A.S.T.M.24, Metallographic and Materialographic Specimen Preparation-2006

Metallographic and
Materialographic Specimen
Preparation, Light Microscopy,
Image Analysis and Hardness
Testing
Kay Geels
In collaboration with Daniel B. Fowler,
Wolf-Ulrich Kopp, and Michael Rckert
ASTM International
100 Barr Harbor Drive
PO Box C700
West Conshohocken, PA 19428-2959
Printed in U.S.A.
ASTM Stock No. MNL46
Library of Congress Cataloging-in-Publication Data
Metallographic and materialographic specimen preparation, light microscopy,
image analysis and hardness testing
Kay Geels; in collaboration with Daniel B. Fowler, Wolf-Ulrich Kopp, and Michael
Rckert
p. cm.Manual; 46
ASTM stock number: MNL 46.
Includes bibliographical references.
ISBN 978-0-8031-4265-7
E-book ISBN 978-0-8031-5691-3
1. Metallography. 2. Metallographic specimens. I. Title.
TN690.G3785 2006
669.95028dc22 2006103391
Copyright 2007 ASTM International, West Conshohocken, PA. All rights reserved.
This material may not be reproduced or copied, in whole or in part, in any printed,
mechanical, electronic, lm, or other distribution and storage media, without the
written consent of the publisher.
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use of specic clients, is granted by ASTM International ASTM provided that
the appropriate fee is paid to the Copyright Clearance Center, 222 Rosewood
Drive, Danvers, MA 01923; Tel: 978-750-8400; online: http://
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The Society is not responsible, as a body, for the statements and opinions expressed
in this publication.
ASTM International does not endorse any products represented in this publication.
Printed in City, State
Month Year
Preface
This book is written both for the experienced and unexperienced metallographer ma-
terialographer who wants specic advice and information. It is also for persons seek-
ing a broader knowledge of metallographic/materialographic specimen preparation
and the examination methods, light microscopy, image analysis, and hardness testing.
Special emphasis has been made on relations between ASTM standards and
metallography/materialography.
The book will be useful for students in courses devoted to practical metallography
andmaterialography.
The scope of the book is to give relevant information, in an efcient and clear way,
covering the daily workina metallographic/materialographic laboratory.
Metallographic/Materialographic Preparation
Kay Geels and Michael Rckert Sections 13.5/6
Part I is a description of sectioning, mounting, grinding, polishing, and etching of
specimens for examination in reected light, enabling the reader to understand the
mechanisms of the entire preparation process. This is combined with practical advice
onspecimenpreparationandanintroductiontoexisting equipment andconsumables.
Part II is a Hands-on Manual guiding the metallographer/materialographer to
the correct preparation method, based on the material to be prepared and the purpose
of examination. More than 150 methods are indicated covering practically all types of
materials, describing the preparation process from sectioning to etching. This part
also includes a section on Trouble Shooting, covering all stages in the preparation pro-
cess andartifacts developedduring the preparation.
Light Microscopy
Wolf-Ulrich Kopp
Part III is a description of the optical reected-light microscope with photomicroscopy
giving the reader both an introduction to the subject and a manual for the daily work.
Also, a short introduction to electron microscopy and scanning probe microscopy can
be foundinthis part of the book.
Quantitative Metallography/MaterialographyAutomatic
Image Analysis
Daniel B. Fowler
Part IV gives an introduction to quantitative microstructural analysis and automatic
image analysis, both theoretically and practically, with emphasis on the examinations
basedonASTMstandards andother types of commonly usedanalyses.
iii
Hardness Testing
Wolf-Ulrich Kopp
Part V gives a description of the hardness testing methods, Brinell, Vickers, Rockwell,
microhardness and instrumented nano indentation testing based on ASTM stan-
dards, boththeoretically andas a practical guide.
The Metallographic/Materialographic Laboratory
Kay Geels
Part VI gives directions on how to establish and maintain a modern metallographic/
materialographic laboratory. The important rules and regulations covering occupa-
tional safety are describedandcommentedon.
The authors of this book, representing more than 100 years experience with prac-
tical metallography and materialography, have tried to make this book a practical tool
and helpful source of information to all who are involved in the noble art/science of
metallography/materialographyKay Geels.
Acknowledgments
The authors wish to acknowledge the four reviewers, who brought forward valuable
insight for improvement. Special thanks to R. C. Nester, for his advice and suggestions
on extension and shortening of the chapters. Thanks to G. Petzow, F. Mcklich and L.
E. Samuels for permission to use a number of illustrations, and to B. Ottesen and W.
Taylor for reading the manuscript and giving good advice. A special acknowledgement
goes to fellow-metallographers/materialographers for support and advice through the
years and directly connected to the book. The list includes U. Tffner, S. Glancy, E.
Weidmann, A. Z. JensenandA. Guesnier. Aspecial thanks to L. Bjerregaardfor her very
important advice on many of the preparation methods, and to H. Hellestad for her in-
valuable support in making the illustrations. Also, thanks go to W. Taylor and Struers
GmbH for providing important micrographs. The authors acknowledge the following
companies for supply of information and illustrations, Buehler Ltd., Carl Zeiss AG,
DoAll Company, Emco-Test GmbH, Leica Microsystems AG, Olympus Optical Co. Inc.,
and Struers A/S. Particular thanks to G. E. Totten and K. Dernoga at ASTM Interna-
tional for establishing and maintaining the project of making this book. Last but not
least, thanks to B. Freiberg and J. Hestehave for support and encouragement during
the years of making the book.
Abbreviations
AFM Atomic Force Microscope
BF Bright Field
CBN Cubic Boron Nitride
DF Dark Field
DIC Differential Interference Contrast
iv
EBSD Electron Backscatter Diffraction
EDS Energy Dispersive Spectroscopy
EPMA Electron Probe Microanalyzer
FIB Focused Ion Beam
MFM Magnetic Force Microscope
PCB Printed Circuit Board
POL Polarized Light
SEM Scanning Electron Microscope
SPM Scanning Probe Microscope
STM Scanning Tunnel Microscope
STEM Scanning Transmission Electron Microscope
TEM Transmission Electron Microscope
v
Contents
Part I: The Metallographic/Materialographic Preparation Process
1 Introduction
1.1 Metallographic/Materialographic PreparationThe True
Microstucture. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.1.1 Henry Clifton Sorby 18261908. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.2 The True Microstructure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.3 Selection of Preparation Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.3.1 Artifacts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.3.2 Preparation Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.4 The Metallographic/Materialographic Specimen. . . . . . . . . . . . . . . . . . . 7
1.4.1 Specimen or Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
1.5 The Preparation Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.5.1 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
1.5.2 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
1.5.3 Preparation of the Surface. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
1.5.4 Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2 Sectioning
2.1 Selection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.1 General Studies or Routine Work. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.2 Study of Failures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.3 Research Studies. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.4 Type of Section. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.5 Reporting of Locations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.2 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3 Wet Abrasive Cutting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3.1 The Cut-off Grinding Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3.2 The Cut-off WheelAbrasives and Bond Materials. . . . . . . . . . . . . . . . 16
2.3.3 Grinding Mechanics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.3.4 Mechanical Damage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
2.3.5 Thermal Damage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
2.3.6 Cut-off Wheel Wear. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.3.7 Cutting Fluids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
2.3.8 The Metallographic/Materialographic Cutting Operation. . . . . . . . . . . 29
2.4 Abrasive Cut-Off Wheels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2.4.1 Consumable Wheels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2.4.2 Slow Consumable Wheels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
2.5 Abrasive Cut-off Machines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
2.5.1 Design Principles of WheelWork Piece Contact. . . . . . . . . . . . . . . . . . 36
2.5.2 Machine Designs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
2.6 Advice and Hints on Wet Abrasive Cutting. . . . . . . . . . . . . . . . . . . . . . . . 43
2.6.1 Cut-off Wheel Selection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
2.7 Other Sectioning Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
2.7.1 Fracturing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
2.7.2 Sectioning by Melting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
2.7.3 Shearing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
2.7.4 SawingTable 2.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
2.7.5 Wire Cutting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
3 Mounting
3.1 Purpose and Criteria. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.1.1 Purpose. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.1.2 Criteria for a Good Mount. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
vii
3.1.3 Surface FlatnessEdge Retention. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.2 Mounting Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
3.2.1 Clamping. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
3.2.2 Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
3.2.3 Cold Castable Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
3.3 Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
3.3.1 Advantages of Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . . . 59
3.3.2 Disadvantages of Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . 59
3.3.3 MSDS Material Safety Data Sheets. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
3.4 Hot Mounting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
3.4.1 Thermoplastic Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
3.4.2 Thermosetting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
3.5 Mounting Presses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
3.5.1 The Heating/Cooling Unit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
3.5.2 The Hydraulic Press. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
3.5.3 The Air-operated Press. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
3.6 Advice and Hints on Hot Compression Mounting. . . . . . . . . . . . . . . . . . 65
3.6.1 Selection of Resins for Hot Compression Mounting. . . . . . . . . . . . . . . . 66
3.7 Cold Castable Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
3.7.1 Advantages of Cold Castable Mounting. . . . . . . . . . . . . . . . . . . . . . . . . 68
3.7.2 Disadvantages of Cold Castable Mounting. . . . . . . . . . . . . . . . . . . . . . . 68
3.7.3 MSDS Material Safety Data Sheets. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
3.8 Cold Mounting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
3.8.1 Acrylics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
3.8.2 Polyesters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
3.8.3 Epoxies. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
3.9 Accessories for Cold Castable Mounting. . . . . . . . . . . . . . . . . . . . . . . . . 70
3.9.1 Mounting Molds. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
3.9.2 Clips. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
3.10 Vacuum Impregnation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
3.10.1 Dyes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
3.11 Special Mounting Techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
3.11.1 Taper Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
3.11.2 Edge Protection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
3.11.3 Mounting of Very Small Parts, Foils, and Wires. . . . . . . . . . . . . . . . . . . . 75
3.11.4 Mounting of Powders. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
3.11.5 Mounting of PCB Coupons. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
3.11.6 Conductive Mounts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
3.12 Recovery of Mounted Specimen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
3.13 Advice and Hints on Cold Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
3.13.1 Selection of Cold Mounting Materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
4 MarkingStoragePreservation
4.1 Marking. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.1 Marking with Waterproof Ink. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.2 Identication Tag. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.3 Engraving. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.4 Stamping. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.2 Storage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
4.3 Preservation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
viii Metallographic and Materialographic Specimen Preparation
5 Cleaning and Cleanliness
5.1 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
5.1.1 Cleaning Before Start of Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
5.1.2 Cleaning During and After Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . 82
5.2 Cleanliness. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
6 Mechanical Surface PreparationGrinding
6.1 GrindingA Basic Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
6.1.1 Plane Grinding PG. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
6.1.2 Fine Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
6.2 Material Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
6.2.1 Rake Angle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
6.2.2 Grain ShapeContacting Points. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88
6.2.3 Grain Penetration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.2.4 Force on Specimens. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.2.5 Grinding/Polishing Fluids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.3 Deformation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.3.1 Metals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.3.2 Brittle MaterialsCeramics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
6.4 Grinding Abrasives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.4.1 Aluminum Oxide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.4.2 Silicon Carbide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.4.3 DiamondDiamond Products. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
6.4.4 Cubic Boron Nitride CBN. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.5 Boron Carbide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.6 Hardness of Abrasives and MaterialsTable 6.1. . . . . . . . . . . . . . . . . . . 97
6.5 Grinding/Polishing FluidsLubricants. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.5.1 Water-Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.5.2 Alcohol-Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.5.3 Water-oil Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
6.5.4 Oil-Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
6.6 Traditional Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
6.6.1 Grinding Stones/Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
6.6.2 SiC Wet Grinding PaperTable 6.2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
6.6.3 AluminaZirconia Alumina Wet Grinding Paper. . . . . . . . . . . . . . . . . . 105
6.7 Contemporary Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
6.7.1 Magnetic Fixation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
6.7.2 Resin-Bonded Diamond Grinding Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . 107
6.7.3 Resin-Bonded SiC Grinding Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
6.7.4 Metal-Bonded Diamond-Coated Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.5 Diamond Pads. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.6 Diamond/CBN/ Al2 O3 /SiC Film. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.7 Rigid Composite Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.8 Fine Grinding Cloths. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
6.8 Grinding/Polishing Equipment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
6.8.1 Plane Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
6.8.2 Fine Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
7 Mechanical Surface PreparationPolishing
7.1 Polishing: Producing the True Structure. . . . . . . . . . . . . . . . . . . . . . . . . . . 120
7.1.1 Rough Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
7.1.2 Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
ix
7.2 Material Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
7.2.1 Inuence of Polishing Abrasive on Removal Rate. . . . . . . . . . . . . . . . . . 121
7.3 Deformation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
7.3.1 The Beilby Layer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
7.3.2 Inuence of Polishing Abrasive, Cloth, and Fluid on Deformation... 123
7.4 Polishing Cloths. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124
7.4.1 Edge RetentionRelief. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
7.4.2 Cloths for Fine Grinding and Rough Polishing. . . . . . . . . . . . . . . . . . . . . 126
7.4.3 Cloths for Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127
7.5 Polishing Abrasives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
7.5.1 Diamond Suspensions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
7.5.2 Diamond Spray. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
7.5.3 Diamond Paste. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
7.5.4 Alumina. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
7.5.5 Silica. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131
7.5.6 Other Oxides. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
7.6 Polishing Lubricants. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
7.7 The Metallographic/Materialographic Preparation Methods
Method Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
7.7.1 RPM of Grinding/Polishing Disk. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133
7.7.2 RPM of Specimen Holder. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133
7.7.3 Direction of Specimen Holder. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
7.7.5 Process Time. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
7.7.6 Stock Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
7.8 Grinding/Polishing EquipmentManual Preparation. . . . . . . . . . . . . . . 135
7.9 Grinding/Polishing EquipmentAutomatic Preparation. . . . . . . . . . . . 135
7.9.1 Machine Design. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135
7.9.2 Polishing Dynamics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139
7.9.3 Semiautomatic and Fully Automatic Systems. . . . . . . . . . . . . . . . . . . . . . 140
7.10 Special Preparation Techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143
7.10.1 PCB Coupons. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143
7.10.2 Microelectronic MaterialsNonencapsulated Cross Sections. . . . . . . . 143
7.10.3 Microelectronic PackagesTable 7.2Target Preparation. . . . . . . . . . 147
7.10.4 EBSD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
7.11 Field Metallography/MaterialographyNondestructive Mechanical
Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
7.11.1 Portable Grinder/Polishers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
7.11.2 Replication. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
7.12 Chemical Mechanical Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151
7.12.1 ProtectionCorrosion at CMP. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
7.13 Thin Sections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
7.13.1 Thin Sections of Petrographic/Ceramic Materials. . . . . . . . . . . . . . . . . . . 152
7.13.2 Thin Sections of Plastics/Polymers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
7.14 MicrotomyUltramilling. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 155
8 Electrolytic Polishing/Etching
8.1 The Electrolytic Polishing/Etching Process. . . . . . . . . . . . . . . . . . . . . . . . . 156
8.1.1 The Polishing Cell. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
8.1.2 Smoothing and Brightening. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
x Metallographic and Materialographic Specimen Preparation
8.1.3 Electrolytic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159
8.1.4 Advantages and Disadvantages. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
8.2 Electrolytes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163
8.3 Electropolishing in Practice. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 164
8.3.1 Factors Inuencing Electrolytic Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . 164
8.3.2 Example of Electrolytic Polishing/Etching. . . . . . . . . . . . . . . . . . . . . . . . . . 165
8.4 Electrolytic Polishing Equipment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
8.4.1 Electropolishers for Laboratory Use. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
8.5 Field MetallographyNondestructive Electropolishing. . . . . . . . . . . . . 166
8.6 Electrolytic Thinning for TEM. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167
8.7 Chemical Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 168
9 Etching
9.1 MicroetchingContrast. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2 Contrast Without Surface ModicationsMicroscope Techniques... 169
9.2.1 Dark-Field Illumination DF. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2.2 Differential Interference Contrast DIC. . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2.3 Polarized Light POL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2.4 Fluorescence. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
9.3 Contrast with Surface ModicationEtching. . . . . . . . . . . . . . . . . . . . . . 170
9.3.1 Grain Contrast Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
9.3.2 Grain Boundary Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
9.3.3 Reproducibility. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
9.3.4 Safety Precautions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4 Classical Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4.1 Chemical Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4.2 Precipitation Color Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4.3 Heat Tinting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.5 Electrolytic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.5.1 Anodic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.5.2 Anodizing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.5.3 Potentiostatic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6 Physical Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6.1 Relief Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6.2 Ion Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6.3 Thermal Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
9.6.4 Vapor Deposition. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
9.6.5 Sputtering. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
9.7 Macroetching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
Part II: Metallographic/Materialographic Specimen PreparationA Hands-On
Manual
10 Introduction
10.1 Specimen Material. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
10.2 Purpose of Examination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
10.3 Specimen Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
11 Specimen MaterialTable 11.1
11.1 Classication of Materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
11.2 How to Use Table 11.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
11.3 Table 11.1Materials/Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182
xi
12 Purpose of Examination
12.1 Purpose in General. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.2 Purpose: ASTM Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.3 Table 12.1: Purpose/ASTM Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.4 ASTM StandardsMetallography. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.4.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.4.2 ASTM Standards in this Book. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 190
12.4.3 ASTM StandardsDocument Summaries. . . . . . . . . . . . . . . . . . . . . . . . . . 193
12.5 Chemical MicroetchingTable 12.2Table 12.3. . . . . . . . . . . . . . . . . . . 194
12.5.1 Etching Practice. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 194
12.5.2 Table 12.2Numerical List of Etchants. . . . . . . . . . . . . . . . . . . . . . . . . . . . 195
12.5.3 Table 12.3Etchant Names. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 217
13 Specimen Preparation
13.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
13.2 Mechanical PreparationThe Traditional and Contemporary
Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
13.2.1 Material/Preparation Tables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
13.2.2 Method TablesGeneric MethodsParameters/Consumables
Table 13.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 219
13.2.3 Material/Preparation TablesMethods C-01/T-01 to C-68/T-68. . . . . . . 222
13.2.4 Manual Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 450
13.3 Electrolytic Polishing and Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 453
13.3.1 Electropolishers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 454
13.3.2 ElectrolytesMethods for ElectropolishingTable 13.2. . . . . . . . . . . . 454
13.3.3 Table 13.2Electrolytes for Electropolishing/Etching. . . . . . . . . . . . . . . 454
13.3.4 Mechanical Preparation for Electropolishing. . . . . . . . . . . . . . . . . . . . . . 456
13.3.5 ElectropolishingMethod Tables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 456
13.3.6 ElectropolishingMethods El-01 To El-25. . . . . . . . . . . . . . . . . . . . . . . . . 456
13.4 Field Metallography/MaterialographyNondestructive
Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.4.1 Mechanical Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.4.2 Electrolytic Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.4.3 Replication. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.5 Trouble ShootingHow to Improve Preparation Results. . . . . . . . . . . 476
13.5.1 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 477
13.5.2 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 479
13.5.4 Electrolytic Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 483
13.5.5 General RulesThe Metallographers Rule of Thumb. . . . . . . . . . . . 483
13.6 Trouble ShootingHow to Overcome Preparation Artifacts. . . . . . . . 484
13.6.1 Preparation ArtifactsFlow Charts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 484
13.6.2 SectioningGeneral ProblemsFlow Charts. . . . . . . . . . . . . . . . . . . . . . 485
13.6.3 MountingGeneral ProblemsArtifacts. . . . . . . . . . . . . . . . . . . . . . . . . . 495
13.6.4 Grinding and Mechanical PolishingFlow Charts. . . . . . . . . . . . . . . . . . 498
13.6.5 ElectropolishingGeneral ProblemsArtifacts. . . . . . . . . . . . . . . . . . . . 521
Part III: Light Microscopy
14 Introduction
14.1 Visible LightTable 14.1Table 14.2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 525
14.2 The Human Eye. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 526
xii Metallographic and Materialographic Specimen Preparation
14.3 Magnifying Lens and Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 527
14.4 Magnication. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 527
15 The Optical Reected Light Microscope
15.1 The Path of Light Rays. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 528
15.2 The Objective. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 528
15.2.1 Numerical ApertureResolution-MagnicationTable 15.1Table
15.2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 528
15.2.2 Aberrations in Image-Formation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 532
15.2.3 Available Objectives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 533
15.3 Eyepieces. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 535
15.4 Illumination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536
15.4.1 Koehlers Illumination System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536
15.5 Microscope Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537
15.6 The Reected-Light Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 538
15.6.1 Upright Type of Reected-Light Microscope. . . . . . . . . . . . . . . . . . . . . . . 538
15.6.2 Inverted Type of Reected-Light Microscope. . . . . . . . . . . . . . . . . . . . . . 538
15.7 Optical Examination Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 540
15.7.1 Bright-Field BF Illumination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
15.7.2 Dark-Field DF Illumination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
15.7.3 Polarization Contrasting POL. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 542
15.7.4 Differential Interference Contrasting DIC. . . . . . . . . . . . . . . . . . . . . . . . 544
15.7.5 Fluorescence in Reected Light. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545
15.8 Practical Use of the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
15.8.1 Setting up the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
15.8.2 Working with the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
15.8.3 Correct Adjustment of the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
15.8.4 Focusing and Practical Use. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
15.8.5 Measurements of Length. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 549
15.8.6 Measurements of Height Differences. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
15.8.7 Maintenance of the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
15.9 Documentation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
15.10 The Confocal Laser Scan Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
15.10.1 Function of Confocal Laser Scan Microscope. . . . . . . . . . . . . . . . . . . . . . 552
15.10.2 Applications of Confocal Laser Scan Microscope. . . . . . . . . . . . . . . . . . . 554
15.11 Stereo Microscopy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 555
16 Electron MicroscopyScanning Probe Microscopy
16.1 The Transmission Electron Microscope TEM. . . . . . . . . . . . . . . . . . . . . . 558
16.1.1 The Scanning Transmission Electron Microscope STEM. . . . . . . . . . . . 558
16.2 The Scanning Electron Microscope SEM. . . . . . . . . . . . . . . . . . . . . . . . . . 558
16.2.1 Energy Dispersive Spectroscopy EDS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 559
16.2.2 Electron Backscatter Diffraction EBSD. . . . . . . . . . . . . . . . . . . . . . . . . . . 559
16.2.3 The Electron Probe Microanalyzer EPMA. . . . . . . . . . . . . . . . . . . . . . . . 560
16.3 Focused Ion Beam FIB. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 560
16.4 Scanning Probe Microscopes SPM. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 560
Part IV: Quantitative Metallography/Materialography Automatic Image Analysis
17 Quantitative Metallography/MaterialographyAn Introduction
17.1 Quantitative Metallography/Materialography. . . . . . . . . . . . . . . . . . . . . 565
17.1.1 StereologyTable 17.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 565
xiii
17.1.2 Specimen Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 567
17.1.3 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 568
17.1.4 Field SelectionBias. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 568
17.2 Volume FractionPoint Count. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 569
17.2.1 ASTM Test Method for Determining Volume Fraction by
Systematic Manual Point Count E 562. . . . . . . . . . . . . . . . . . . . . . . . . . . 569
17.3 Inclusion Rating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 570
17.3.1 ASTM Standard Test Method For Determining the Inclusion
Content of Steel E 45. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 570
17.3.2 ASTM Practice for Obtaining JK Inclusion Ratings Using Automatic
Image Analysis E 1122 withdrawn 2006, replaced by E 45. . . . . . . 570
17.3.3 ASTM Practice for Determining the Inclusion or Second-Phase
Constituent Content of Metals by Automatic Image Analysis
E 1245. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 570
17.4 Grain Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 571
17.4.1 ASTM Test Methods for Determining Average Grain Size E 112. . . 571
17.4.2 ASTM Test Methods for Estimating the Largest Grain Observed in
a Metallographic Section ALA Grain Size E 930. . . . . . . . . . . . . . . . . 573
17.4.3 ASTM Test Methods for Characterizing Duplex Grain Sizes E 1181.. 573
17.4.4 ASTM Test Methods for Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis E 1382. . . . . . . . . . . . 573
17.5 Banding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.5.1 ASTM Practice for Assessing the Degree of Banding or Orientation
of Microstructures E 1268. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.6 Porosity in Thermal Spray Coatings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.6.1 ASTM Test Methods for Determining Area Percentage Porosity in
Thermal Sprayed Coatings E 2109. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.7 DecarburizationCase DepthCoatings. . . . . . . . . . . . . . . . . . . . . . . . . . 575
17.7.2 ASTM Test Methods for Estimating the Depth of Decarburization
of Steel Specimens E 1077. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 575
17.7.3 Case Depth. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 575
17.7.4 ASTM Test Method for Measurement of Metal and Oxide Coating
Thickness by Microscopical Examination of a Cross Section B 487.. 576
17.7.5 ASTM Test Methods for Thickness of Diffusion Coating C 664. . . . . 576
17.8 Other ASTM Standards for Quantitative Materialography. . . . . . . . . . 576
18 Automatic Image Analysis
18.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 577
18.2 Qualitative and Quantitative Metallography/Materialography. . . . . . 577
18.2.1 The Transition to Quantitative Standards. . . . . . . . . . . . . . . . . . . . . . . . . 577
18.2.2 Structure, Stereology, and Statistics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 578
18.3 Principles of Digital Imaging. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 579
18.3.1 What is Digital Image Analysis?. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 579
18.3.2 Image Acquisition. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 579
18.3.3 Image DigitizationGray Scale. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 580
18.3.4 The Histogram. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 581
18.3.5 The Effects of Brightness and Contrast on Illumination
Distribution. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 581
18.3.6 Image Processing and True Microstructure. . . . . . . . . . . . . . . . . . . . . . . . 586
18.3.7 Image Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 595
xiv Metallographic and Materialographic Specimen Preparation
18.4 Image Measurement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 598
18.4.1 Manual Measurements Operator Denes Points, Lines, or Areas... 599
18.4.2 Automatic Measurements Objects Dened by Image
Segmentation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 600
18.5 Digital Imaging Applied to Quantitative Materialography. . . . . . . . . . 602
18.5.1 Percent Area Volume Fraction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 602
18.5.2 Inclusion Rating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 603
18.5.3 Grain Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 606
18.5.4 Degree of Banding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 608
18.5.5 Depth or Thickness Measurements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 608
18.5.6 Graphite in Iron Castings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 610
18.6 Digital Imaging Technology. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 613
18.6.1 Hardware. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 613
18.6.2 Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 616
18.7 Digital Imaging System Implementation. . . . . . . . . . . . . . . . . . . . . . . . . . 617
19 Digital Image Management Archiving
Part V: Hardness Testing
20 Introduction
20.1 Indentation Hardness. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 623
20.2 ASTM Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 625
21 Static Hardness Testing Procedures
21.1 Brinell Hardness Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 626
21.1.1 Calculations and Procedures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 626
21.1.2 Brinell Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 628
21.2 Vickers Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 628
21.2.2 Vickers Hardness Tester. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 632
21.3 Knoop Hardness Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 633
21.4 Rockwell Hardness Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 634
21.4.2 Rockwell Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
21.5 Microindentation Hardness. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
21.5.1 Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
21.5.3 Taking the Measurements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 638
21.5.4 Microindentation Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639
21.5.5 Examples of Indentations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639
21.6 Universal HardnessMartens HardnessInstrumented Indentation
TestingNano Indentation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639
21.6.1 Instrumented Indentation TestingNano Indentation. . . . . . . . . . . . . 641
21.7 Precision of Hardness Values. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 642
21.8 Conversion of Hardness Values. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 642
22 Dynamic Hardness Testing Procedures
23 Special Methods for Hardness Testing
xv
Part VI: The Metallographic/Materialographic Laboratory
24 Introduction
24.1 Establishing a Metallographic/Materialographic Laboratory. . . . . . . . 649
24.2 Running a Metallographic/Materialographic Laboratory. . . . . . . . . . . . 649
24.3 Occupational Safety and Health. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649
25 How to Build a Metallographic/Materialographic Laboratory
25.1 Purpose. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 650
25.1.1 Quality Control QC. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 650
25.1.2 Research and Education. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651
25.1.3 Testing and Inspection LaboratoriesFailure Analysis. . . . . . . . . . . . . . 651
25.2 Rationalization and Automation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651
25.2.1 ReproducibilityStandardsOccupational Safety. . . . . . . . . . . . . . . . . . 652
25.2.2 ProductivityCost Per Specimen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 653
25.3 Planning the Metallographic/Materialographic Laboratory. . . . . . . . . 654
25.3.1 Basic Planning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 654
25.3.2 Detailed Planning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655
25.4 Equipment and Laboratory Layout. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 656
25.4.1 EquipmentTable 25.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 656
25.4.2 LayoutFurnitureInstallations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 660
25.5 Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
25.5.1 Organizing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
25.5.2 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
25.5.3 Servicing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 663
26 Occupational Safety and Health in the Metallographic/
Materialographic Laboratory
26.1 Dangers in the Metallographic/Materialographic Laboratory. . . . . . . 664
26.1.1 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 664
26.1.2 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 664
26.1.4 Electrolytic Polishing/Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 665
26.1.5 EtchingEtchantsElectrolytes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 665
26.1.6 Dust. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 667
26.1.7 Cold Castable Mounting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 667
26.1.8 Standard Guide on Metallographic Laboratory Safety E 2014. . . . . 668
26.2 Safety Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668
26.2.1 Identication. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668
26.2.2 Material Safety Data Sheet MSDS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 670
26.2.3 Standard Operating Procedure SOP. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 672
26.2.4 Job Safety Analysis JSA. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 672
26.3 Disposal of Chemicals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 672
26.4 Occupational Safety in General. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.4.1 Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.4.2 Training. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.4.3 Maintenance and Service. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.5 Standards and RegulationsOrganizations. . . . . . . . . . . . . . . . . . . . . . . 673
26.5.1 Designations and Abbreviations Used to Describe a Chemical
Substance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.5.2 ASTM Standard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674
26.5.3 OSHAOSHA Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674
xvi Metallographic and Materialographic Specimen Preparation
26.5.4 National Institute for Occupational Safety and Health NIOSH. . . . . 681
26.5.5 International Chemical Safety Cards ICSCS. . . . . . . . . . . . . . . . . . . . . . . 682
26.5.6 Environmental Protection Agency EPA. . . . . . . . . . . . . . . . . . . . . . . . . . 683
26.5.7 National Technical Information Service NTIS. . . . . . . . . . . . . . . . . . . . . 683
26.5.8 American Conference of Government Industrial Hygienists
ACGIH. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 683
26.5.9 National Toxicology Program NTP. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 683
26.5.10 Agency for Toxic Substance and Disease Registry ATSDR. . . . . . . . . . 683
26.5.11 National Fire Protection Association NFPA. . . . . . . . . . . . . . . . . . . . . . . 684
26.5.12 National Paint and Coatings Association NPCAHMIS. . . . . . . . . . . . 684
26.5.13 BSIISO. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 684
26.5.14 EU. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 684
26.6 Literature on Laboratory Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 684
27 Literature
27.1 Books. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 685
27.2 Periodicals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 686
Appendixes
Appendix I: Other Standards on Metallography/Materialography . . . . . . . . . . . . . 686
Appendix II: Other Standards on Hardness Testing . . . . . . . . . . . . . . . . . . . . . . . . . . 691
Appendix III: Hardness Conversion Tables for Metals E140 . . . . . . . . . . . . . . . . . . 694
Appendix IV: SI Quick Reference Guide: International System of Units SI . . . . 694
Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 695
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 727
xvii
Part I:
The Metallographic/Materialographic
Preparation Process
1
Introduction
METALLOGRAPHY or MATERIALOGRAPHY? IN MODERN TECHNOL-
ogy and Materials Science we are examining the microstructure of all solid materials;
therefore, materialography seems to be the correct word instead of the traditional met-
allography. In 1968, Crowther and Spanholtz
1
suggested this and it now seems appro-
priate to use the word materialography to cover the examination of the innite num-
ber of existing and future materials. Also, the term metallographer should be
changedtomaterialographer. Changes of this kind, however, take time, andtherefore
the terms metallography and metallographer are used in this book, except in con-
texts where materials other thanmetals are discussed.
G. Petzow
2
denes Materialography metallography as an investigative method
of materials science. It encompasses the optical examination of microstructures, and
its goal is a qualitative andquantitative descriptionof the microstructure.
The term materialography includes ceramography ceramics, metallography
metals, plastography polymers, and mineralogy minerals, in this way covering the
microstructural examinationof most materials.
Metallography/materialography includes a wide eld in material investigation; it
bridges the gap between science in new and existing materials and engineering using
the materials in modern technology. Figure 1.1
3
shows how materialography covers
the examination of parts from the centimetre and metre in and ft range to atomic
dimensions inthe nmandsubnmrange.
The microstructure is characterized through size, shape, arrangement, amount,
type, and orientation of the phases and the defects of these phases, as schematically
Fig. 1.1Metallography/materialography can be described as a bridge between engineering
and science, covering the examination of the part in cm and m to the examination of the
single atom in .
3
shown in Fig. 1.2
3
. Each material contains many millions of microstructural features
per cubic centimetre and these features strongly inuence many of the properties of
the material. As seen in Fig. 1.1, the microstructural features can exist in sizes of at
least ten orders of magnitude. There are many instruments today that visualize nearly
all of the features across this range.
The image we see in the typical microscope is two-dimensional, but we should not
lose sight of the fact that the constituents in a material are three dimensionally ar-
ranged.
A photomontage shows the prepared surface of a silicon nitride alloy superim-
posed on a pile of silicon nitride crystals see Fig. 1.3.
3
It shows that the true size of the
crystals cannot be deduced directly from the microstructure. A statistical extrapola-
tion of the two-dimensional surface shows that approximately 80 %of the crystals are
relatively short and have an equiaxial shape. Stereological calculations, however, show
a much higher variation in crystal length. The average crystal length is larger, corre-
sponding tothe three-dimensional characteristics showninFig. 1.3.
It can be concluded that the analysis of the microstructure plays an important role
in modern materials science and engineering, and consequently, the metallographic/
materialographic preparation. It is important to secure the true microstructure be-
cause without this the best examinations and inspired interpretations will be of no
avail.
As stated in the Preface, this book concentrates on metallographic/
materialographic preparation and the most commonly used examination methods.
For a comprehensive, in-depth coverage of metallurgy and microstructures, including
interpretation of the microstructures, ASM Handbook, Volume 9, Metallography and
Microstructures,
4
is recommended.
This part of the book concentrates on the preparation of the specimen surface for
examination in the reected-light optical microscope. This preparation can also be
used frequently for the scanning electron microscope SEM. The mechanical removal
Fig. 1.2The constituents of a microstructure and the factors affecting them.
4 METALLOGRAPHIC AND MATERIALOGRAPHIC SPECIMEN
of material will be described and discussed rather intensively because it is the central
process inabrasive cutting, sawing, plane/ne grinding, andpolishing, as will the prob-
lems involved in obtaining the true microstructure. The machines and consumables
available will alsobe describedanddiscussed.
Etching, often performed after the specimen preparation process to obtain a con-
trast to highlight or clearly reveal certainfeatures, will be described intheory and prac-
tice.
1.1 Metallographic/Materialographic PreparationThe True
Microstructure
The goal of the metallographic/materialographic preparation is to obtain the true mi-
crostructure or The True Structure, meaning anundisturbed material surface, which
canbe analyzedinanoptical light microscope or anSEM.
The basic problemfor a metallographer preparing a specimen is that the prepara-
tion process itself modies the specimen surface and, theoretically, a true structure
completely without artifacts can never be obtained. Consequently, a preparation pro-
cess should be used that creates the smallest amount of artifacts, making it possible, in
practice, toanalyze a microstructure ina satisfactory way.
1.1.1 Henry Clifton Sorby 18261908
In the 1860s, because he understood that to obtain a true structure he had to remove
the irregularities of the material surface, H. C. Sorby was able to produce what is con-
Fig. 1.3Photomontage of a microsection of silicon nitride alloy superimposed upon a pile of
silicon nitride crystallites.
Chapter 1 Introduction 5
sidered the rst true microstructure. In 1863 he prepared a specimen of Bessemer steel
by using a preparation method with several steps, a method similar to the mechanical
preparation used today. Figure 1.4
5
shows the microstructure, which was prepared in
several steps, a roughpolishing stepanda ne polishing step.
1.2 The True Microstructure
Basedonstudies by Vilella andSamuels,
68
the true structure canbe denedas:
No deformationThe plastically deformedlayer createdby the preparationshould
be removedor be negligible.
No scratchesScratches normally indicate a surface that is not yet sufciently pre-
pared, but small scratches might be allowedif they donot disturbthe examination.
No pull-outsEspecially in brittle materials, particles can be pulled out of the sur-
face leaving cavities that canbe takenfor porosity.
No introduction of foreign elementsDuring the preparation process, abrasive
grains canbe embeddedinthe surface.
No smearingWith certain materials, the matrix or one of the phases might smear
ow, resulting ina false structure or covering of structure details, or both.
No relief or rounding of edgesRelief candevelopbetweendifferent constituents of
the surface, caused by different hardness or other condition. Edge retention is impor-
tant if the edge has tobe examined.
1.3 Selection of Preparation Method
The preparation process will always inuence the prepared surface, creating artifacts.
Artifacts are denedas false structural details introducedduring the preparation.
Fig. 1.4Original specimen prepared by H. C. Sorby, 1863, Bessemer steel 0.2 % carbon. BF,
450:1. Preparation MethodRough grinding: Emery paper from coarse to ne. Fine grinding:
Fine grained water-of-Ayr stone. Rough polishing: Finest grained crocus Fe
2
O
3
used for
industrial polishing. Polishing: Very best and nest washed rouge Fe
2
O
3
, jewelers rouge.
The choice of preparation is usually between using mechanical or electrolytic pol-
ishing, but chemical andchemical-mechanical polishing are alsoused.
1.3.1 Artifacts
Anumber of artifacts are already stated above under the true structure, but a fewmore
can be added. Microcracks, comet tails, pitting, contamination, and lapping tracks are
all causedby the preparationprocess. Artifacts canalso be introducedduring chemical
etching of the surface. Most of these artifacts can be readily observed under the micro-
scope. In some cases, artifacts can be accepted and the metallographer can decide
whether, for example, a scratch is acceptable as it does not disturb the structural analy-
sis, or whether the specimensurface shouldbe reprepared.
In some cases it can be very difcult to establish the true structure, e.g., a smeared
layer can cover pores. It is important that the metallographer pay attention to this pos-
sibility whenanalyzing a structure see Section13.5.
Artifacts of Mechanical Polishing
With mechanical polishing, it is possible to obtain an approximate true structure when
the correct procedures are followed, even with very heterogeneous materials. Figure
1.5 shows the following most commonartifacts: relief betweenphases causedby differ-
ence in hardness; embedded abrasive grain; inclusion protruding it could also be
missing; pull-out looking like a pore; rounding of the edge; and deformation of the
matrix.
Artifacts of Electrolytic Polishing
With electrolytic polishing, the electrolysis might create problems if more than one
phase is present in the structure. Figure 1.6 shows the most common artifacts. Relief
between phases caused by a difference in electrochemical potential: in some cases one
phase will be removed much faster than another phase, in other cases a phase might
not be electrically conductive and, as such, will not take part in the polishing process.
Inclusions might react in the same way; they will often be dug out during the process.
Pitting might develop if the electrolytic process is not controlled correctly. Also, a pro-
nounced rounding of the edge will take place because the current density is always
stronger at the edge.
1.3.2 Preparation Methods
Because most materials are heterogeneous or even nonconductive, the conclusion
must be that mechanical polishing is by far the most commonly used method. For cer-
tainmaterials, however, electrolytic polishing gives very goodresults.
Alternatives to the above-mentioned methods are chemical polishing and
chemical-mechanical polishing. Chemical polishing is not used much, although reci-
pes for polishing of a number of materials are developed. Chemical mechanical polish-
ing or attack polishing can be seen as an extension of mechanical polishing and, when
relevant, recipes will be statedinconnectionwiththe specic material.
For recipes onchemical andchemical mechanical polishing, see Refs. 2, 4, and9.
1.4 The Metallographic/Materialographic Specimen
In practice, the total work piece normally cannot be prepared and examined. For this
reason, a small part of the work piece, the sample specimen must be extracted. For
both specimen preparation and examination, using an optical microscope or an SEM,
the ideal specimensize is 1240 mm0.51.5 in square or cylindrical, witha height of
1230 mm0.51.2 in. There are, of course, exceptions like welds, where larger speci-
mens have tobe prepared.
With the specimen being only a small part of the material to be examined, if the
interpretationis to be valuable, it is very important that the specimenbe representative
of the material to be studied. This usually happens by cutting out the specimen froma
correct location and in the correct direction see Section 2.1. Most ASTM standards
covering examination of a metallographic/materialographic specimen offer guidance
inselectionandsectioning of specimens see Section12.4. The preparationcanbe per-
formedonce the specimenis established.
1.4.1 Specimen or Sample
The two words are often used indiscriminately, describing the object prepared and ex-
amined. The sample can be dened as the piece of material in its raw state, as taken
Fig. 1.5Mechanical polishing: the most common artifacts shown schematically.
from the original material work piece. As soon as the sample is treated prepared
and described, it turns into a specimen, and for this reason only the word specimen
is usedinthis book, except ina fewcases where sample is the correct description.
1.5 The Preparation Process
As mentioned above, several polishing methods are available, but in the diagram, Fig.
1.7, only the two methods used for almost all preparation, mechanical and electrolytic,
are shown. The diagramgives an overviewof the total process, of which each step will
be discussedfurther inthis part of the book.
Fig. 1.6Electrolytic polishing: the most common artifacts shown schematically.
1.5.1 Sectioning
To obtain a specimen, some kind of sectioning from the basic material work piece is
necessary. If this sectioning could take place without disturbing the specimen surface,
the specimen could be examined without further work, but unfortunately all the
known sectioning methods will leave some kind of irregularities on the surface. Abra-
sive wet cutting using a precision cut-off machine is considered as a sectioning method
giving a low deformation of the specimen surface. Figure 1.8 shows a surface from a
specimen cut on a precision cutter and measured with an atomic force microscope
AFM, andthe irregularities of the surface are evident.
Abrasive wet cutting is the most frequently used sectioning method, but other
Fig. 1.7Diagram showing the total preparation process based on mechanical and electrolytic
preparation.
methods, suchas shearing, sawing, andpunching are usedas well see Section2.7.
1.5.2 Mounting
In some cases, the sample taken from the base material can be handled and treated
directly as a specimen, but often a mount must be made to secure the handling and a
satisfactory preparation. The mounting can be made by clamping the specimen be-
tween two pieces of a material compatible to the specimen material. This way of
mounting has a number of drawbacks see Section 3.2.1; therefore mounting mainly
takes place as hot compression or cold castable mounting in a mounting plastic
resin. Figure 1.9a shows three mounts made withhot mounting, giving mounts with
very precise dimensions. Figure 1.9b shows three mounts made with cold mounting;
these mounts, made inmolds, are less exact thanthe hot mounts.
1.5.3 Preparation of the Surface
The goal of the preparationis to obtainthe true microstructure or at least a microstruc-
ture in a condition that makes a satisfactory examination possible. This means that the
number of irregularities artifacts inthe surface must be kept at a minimum.
The preparation is done through a number of steps, either mechanical or electro-
lytical see Fig. 1.7.
Fig. 1.8Surface cut with a precision cut-off machine in a very careful way to avoid
irregularities in the cut surface. Measurements with an atomic force microscope AFM give the
peak-to-valley value of irregularities: higher than 1000 nm 1 m. This shows that even with
the most gentle sectioning technique, the cut surface will have deformations which have to be
removed in the following preparation steps.
Amechanical preparationmethodwill normally containa plane grinding step, one
or more ne grinding steps, andone or more polishing steps.
Electrolytic polishing usually takes place as one electrolytic step, performed on a
mechanically groundor polishedsurface.
Fig. 1.9Mounts made with hot compression mounting a and cold castable mounting b.
1.5.4 Etching
The prepared surface often reacts as a mirror when examined in the microscope, not
showing all phases of the microstructure. For this purpose, the surface can be etched
chemically or electrolytically or treated in other ways to discriminate between phases,
grains, grain boundaries, and other details. Figure 1.10 shows a copper specimen a in
an unetched condition, giving very little information; and b one that is etched, show-
ing the microstructure.
Fig. 1.10Copper unetched a showing a bright, reecting surface and color etched with
Klemm III
45
b, revealing the microstructure.
2
Sectioning
2.1 Selection
ITIS VERYIMPORTANTTHATTHESPECIMENIS SELECTEDCORRECTLYSO
that the specimen material is representative of the material to be studied. The intent or
purpose of the examinationwill usually dictate the locationof the specimen.
With respect to the purpose of the study, metallographic examination may be di-
vided into three classications, as stated in ASTMPractice for Preparation of Metallo-
graphic Specimens E3 see Section12.4.
2.1.1 General Studies or Routine Work
Specimens should be chosen fromlocations that are most likely to showthe maximum
varieties within the material being studied. For example, specimens should be taken
from a casting in the zones wherein maximum segregation should occur, as well as
specimens from sections where segregation should be at a minimum. In the examina-
tionof stripor wire, test specimens shouldbe takenfromeachendof the coils.
2.1.2 Study of Failures
Specimens should be taken as closely as possible to the fracture or to the initiation of
the failure. Before taking the specimens, study of the fracture surface should be com-
plete, or, at the very least, the fracture surface should be documented. In many cases,
specimens should be taken from a sound area for a comparison of structures and
properties.
2.1.3 Research Studies
The nature of the study will dictate the specimen location, orientation, etc. Sampling
usually will be more extensive thaninroutine examinations.
2.1.4 Type of Section
After establishing the location of the specimen to be studied, the type of section to be
examined must be decided. For a casting, a section cut perpendicular to the surface
will show the variations in structure form the outside to the interior of the casting. In
hot-worked or cold-worked metals, both transverse and longitudinal sections should
be studied. Special investigations may at times require specimens with surfaces pre-
pared parallel to the original surface of the product. In the case of wire and small
rounds, a longitudinal sectionthroughthe center of the specimenproves advantageous
whenstudiedinconjunctionwiththe transverse section.
Cross sections or transverse sections taken perpendicular to the main axis of the
material are more suitable for revealing the following information:
Variations instructure fromcenter tosurface
Distributionof nonmetallic impurities across the section.
Decarburization at the surface of a ferrous material, see ASTM Test Methods for
14
Estimating the Depth of Decarburization of Steel Specimens E 1077, Section
12.4.
Depthof surface imperfections.
Depthof corrosion.
Thickness of protective coatings andstructure of protective coating.
Longitudinal sections taken parallel to the main axis of the material are more suit-
able for revealing the following information:
Inclusion content of steel, see ASTM Test Methods for Determining the Inclusion
Content of Steel E45 andother ASTMstandards, Sections 12.4and17.2.
Degree of plastic deformation, as shownby graindistortion.
Presence or absence of banding in the structure, see ASTM Practice for Assessing
the Degree of Banding or Orientation of Microstructures E 1268, Sections 12.4
and17.5.
The quality attainedwithany heat treatment.
2.1.5 Reporting of Locations
The locations of surfaces examined should always be given when reporting results and
in any illustrative micrographs. A suitable method of indicating surface locations is to
make a sketchof the workpiece withanindicationof the location.
2.2 Sectioning
The goal is to extract the specimento be preparedfromthe material to be studiedwork
piece. This should be done so that the specimen is representative of the work piece
material and it should be done with a minimumamount of damage to the surface that
is tobe prepared.
In principle, all methods, including sawing with a hacksaw, shearing, ame cut-
ting, fracturing, etc., can be used to separate a specimen from the work piece. It is,
however, important that the surface being prepared is only inuenced mechanically or
by heat to a degree that is suitable for a rational preparation that follows. This limits
the sectioning methods to wet abrasive cutting and a few other methods that will be
describedinthe following sections.
2.3 Wet Abrasive Cutting
Abrasive cutting is a cut-off grinding process.
2.3.1 The Cut-off Grinding Process
The cut-off grinding abrasive cutting is a special operationfollowing the general prin-
ciples of the machining process, grinding.
Within the spectrumof machining processes, the uniqueness of grinding is found
in its cutting tool. Grinding wheels are generally composed of two materials: abrasive
particles called grains that do the cutting and a softer bonding agent to hold the count-
less abrasive grains together ina solidmass.
During most grinding processes the surface of the work piece is treated to obtain a
given accuracy or surface nish. In cut-off grinding, a very thin grinding wheel nor-
mally the thickness of the wheel is 1/ 100 of the wheel diameter, or less grinds its way
through a work piece. In metallographic/materialographic cutting, this is to separate a
Chapter 2 Sectioning 15
sample suited for further preparation from the work piece. Although there isnt a de-
mand for high accuracy, the surface quality concerning mechanical damage, thermal
damage, andplaneness is important.
Cut-off wheels are made by cementing together abrasive grains with a suitable
bonding material. Each grain is a potential microscopic cutting tool. The grinding pro-
cess uses thousands of abrasive points simultaneously andmillions continually.
By choosing a cut-off wheel with the correct abrasive and bond and using it on a
suitable machine, both the mechanical and thermal damage and the planeness can be
kept inside narrow limits. This will shorten and facilitate the following preparation
process.
Figure 2.1 shows the surface roughness of mild steel after cutting, after grit P220
SiC grinding paper, and after P320 grinding paper. It can be seen that the irregular
scratches fromthe cut-off are removedby the grinding papers, andfor most materials a
grinding withgrit P220 after cutting will give a satisfactory surface for further prepara-
tion; this will be discussed further below. For certain materials P320 paper can be used
as the rst stepafter cut-off, omitting plane grinding withgrit P220.
2.3.2 The Cut-off WheelAbrasives and Bond Materials
The cut-off wheels belong to the category of bondedabrasive tools. Suchtools consist
of hard abrasive grains held in a weaker bonding matrix. Depending on the particular
type of bond, the space between the abrasive particles may only be partially lled, leav-
ing voids and porosity, resulting in an open bond. A dense bond is the result of com-
pletely lled spaces between the grains. Aside from abrasive and bond material, llers
and grinding-aid material may also be added. The correct combination of abrasive and
bondis important toensure the right cut-off process.
Every abrasive particle has a number of cutting points with each removing a tiny
chip fromthe work piece. Eventually the cutting edge becomes blunt and it must bear a
larger force in order to remove the chip from the work piece. The force rises until it
causes the grainto fracture and present a new, sharp edge to the work piece. Inthis way
the grain reduces its size until nally the cutting force see Section 2.3.3 causes it to be
completely torn out of the wheel, exposing new grains. This self-sharpening process
is highly controlled by the combination of abrasive material and bond material see
Fig. 2.2 that schematically shows the abrasive grains in the bond with voids pores in
between.
Depending on how the wheel is breaking down, the wheels are dened as either
Consumable Wheels or SlowConsumable Wheels see Section2.4.
Cut-off Wheel Specications
The basic specication of a consumable cut-off wheel denes the following param-
eters:
1. The type of abrasive, expressed with a number and a letter aluminum oxide: A,
siliconcarbide: S.
2. The size of abrasive grains, expressedwithgrit number see Section6.6.2.
3. The grade hard/soft of wheel bondexpressedwitha letter.
4. The wheels structure expressedwithnumbers.
5. The bondmaterial expressedwitha letter.
6. Acode innumbers toexpress the makers details of manufacture.
Inthe following sections parameters 15will be describedindetail.
Fig. 2.1a Steel after wet abrasive cutting. An abrasive grain arrow, embedded in the
surface during the cutting, can be seen, b after grinding with grit P220 SiC paper, and c
after grinding with P320 grinding paper.
Type of Abrasive
For cut-off wheels four types of synthetic abrasives, aluminum oxide Al
2
O
3
, silicon
carbide SiC, cubic boron nitride CBN, and diamond are used see Table 6.1 and also
Section6.4.
Al
2
O
3
Although this is the softest of the abrasive materials, it is the abrasive used
in most cut-off wheels. This is due to the fact that Al
2
O
3
is best suited for ferrous mate-
rials, frommild steel to high-strength materials, i.e., alloy steels. Al
2
O
3
is not suited for
cast ironsee SiCbelow.
Al
2
O
3
is made synthetically in different types with varying hardness and friability,
andis usedfor cutting of different materials. It is usedinconsumable cut-off wheels.
SiCThis synthetic material is harder and tougher than Al
2
O
3
, but dulls and
glazes rapidly when used with steels. It is well suited for cutting of softer materials like
nonferrous metals, and it is also suited for cast iron. SiCis made in two varieties, black
and green; normally the black type is used in cut-off wheels. It is used in consumable
wheels.
CBNThis very hard, synthetic abrasive superabrasive is used for cutting of
hard materials that are not to be cut with Al
2
O
3
and SiC. CBN is rather expensive; the
price is comparable to the price of diamond, but CBN has the advantage that it cuts
ferrous materials that cannot be cut withdiamond. CBNhas a very highthermal stabil-
ity and will work for a very long time before getting dull and needs little dressing see
Section2.3.6. It is usedinslowconsumable wheels where the wheel consists of a metal
body, andCBNis only part of the rimina very stable bondsee Section2.4. CBNgrains
tend to be blocky shaped with sharp edges and smooth faces, which makes bonding
difcult. Therefore CBN, as diamond, normally is coated before being used in a resin
bondedcut-off wheel.
DiamondDiamond is the hardest abrasive see Table 6.1 and is used for cutting
of the hardest materials. Inspite of its extreme hardness, diamondhas beenfoundtobe
unsuitable for cutting ferrous materials. This is due to graphitizationand carbondiffu-
sion into the iron causing excessive diamond wear.
10
Diamond is found as natural dia-
monds, but mostly synthetic diamonds are used in cut-off wheels. The diamond grains
Fig. 2.2Schematic drawing of cut-off wheel showing abrasive grains and bond material with
voids pores.
are normally coated to improve the xation of the grain in the bond. Diamond is only
usedinslowconsumable wheels as describedunder CBNabove see Section2.4.
Grain Size
The grain size is expressed as a grit number #. This number refers to the number of
openings per linear inch in a mesh screen through which the grain is just able to pass.
The grit sizes are standardized by ANSI American and FEPA European see Table
6.2 and Section 6.6. For cut-off wheels, grit sizes between 50 336 m and 120
125 m are normally used.
Generally speaking, large grains will have a higher material removal rate, but a
rougher nish.
Large grains also allow for a more open bond structure because the pores voids
between the grains can be relatively large see Fig. 2.2 and Structure below. An open
bond structure allows room for the chips created during the cutting process so that
they can be removed without disturbing the process. For this reason cut-off wheels
with large grains, which enable an open structure with large pores, are suited for cut-
ting of large work pieces. This creates a large contact area arc of contact between cut-
off wheel and work piece see l in Fig. 2.3. In the long contact area, chips and bond
particles will be accumulated before they are removed fromthe wheel outside the work
piece, and this accumulation takes place in the large pores. If not accumulated in the
pores, the chips and particles will take room in the interface between wheel and work
piece, reducing the cutting actionandcreating heat.
Fine grains have a lower removal rate, but a better surface nish. Fine grains will
give a relatively dense bond structure small pores, and therefore a ne-grained cut-off
wheel is most suited for brittle materials very small chips and smaller work pieces
Fig. 2.3Schematic drawing of the cut-off process. The rotating cut-off wheel is cutting into
the xed work piece.
witha short arc of contact.
Grade
The grade expresses the degree of retaining grip exerted on each grain by the bonding
material that corresponds to the cutting force needed to dislodge the grain Figure 2.2
shows the grains bonded together with voids pores in between. When the cutting
force has increasedtoa certainpoint, the grainwill be dislodgedfromthe bond.
Wheel grades are expressed with letters fromEvery soft to Xvery hard. Cut-off
wheels are mostly inthe range KtoR.
Asoft grade of bond has a weak hold in the abrasive grain Blunt grains will be torn
away easily, thus the self-sharpening action will be pronounced. This is desirable when
cutting hardmaterials expressedinthe rule: HardMaterialSoft Wheel.
Arelatively soft wheel is used if the arc of contact is very large because the long arc
will normally reduce the force per grainsee Sections 2.3.3and2.3.8.
If the wheel is too soft for a givenmaterial it will inmost cases cut very well, but the
wheel wear will be excessive causing a bad economy. In principle, the hardest possible
wheel for a givenmaterial shouldbe usedtosecure the most economical sectioning.
A hard grade has a stronger hold in the abrasive grain, making it suited for softer
materials expressedinthe rule: Soft MaterialHardWheel.
Ahardwheel is alsousedwitha short arc of contact see Section2.3.6.
A hard bond gives a longer wheel life, but if it is too hard the blunt grains may be
retained for too long, leading to a condition called glazing of the edge of the wheel. In
this conditionthe wheel might stopcutting completely andwill only generate heat.
A wheel may be made to act harder or softer by varying the forces acting on the
grains. Decreasing the wheel speed or raising the feed speed will increase the cutting
forces. This will cause the wheel to shed grains and wear quicker so it will appear to be
acting as a softer grade of wheel. Increasing the wheel speed or reducing the feed speed
will decrease the cutting forces andthe wheel will act as a harder wheel.
This can be used in cut-off machines with variable speeds see Sections 2.3.3 and
2.3.8.
Structure
The structure is a measure of the relationshipbetweenthe grainsize andporosity of the
bond. Wheels can be manufactured to give specic structures ranging fromvery dense
tovery open. Structure is expressedas a numerical value between1 and15, 1 being very
dense and15very open.
The porosity, the voids deliberately built into the wheel see Fig. 2.2, are designed
to take the chips away, to avoid clogging the wheel edge glazing, and to allowgrains to
cut efciently.
A dense structure has closely spaced, relatively small grains and small pores so
that only a small amount of material is removed. An open structure with larger grains
and larger pores can cope with higher rates of material removal as described in Grain
Size above.
Bond Material
The bond material keeps the abrasive grains together. In general, the bond must be
strong enoughtowithstandgrinding forces, hightemperatures, andcentrifugal force.
Consumable abradable cut-off wheels most often have a phenolic bakelite
bond. It is produced by mixing abrasive grains with phenolic thermosetting resin and
plasticizers, molding to shape and baking curing at 150200C 300400F. The
bond hardness and porosity are varied by controlling the amount of plasticizer and by
adding llers.
Phenolics are also used for cut-off wheels of the slowconsumable type, using CBN
and diamond. These wheels are soft compared to the metal bonded wheels see below
and will give a smooth cut on very hard materials, but the wheel wear will be relatively
high.
Bakelite wheels are sensitive toprolongedexposure tocutting uids. The uidlow-
ers the strength of the wheel so that it wears quicker; therefore cut-off wheels must be
kept out of the uidwhennot inuse andstoredina dry place.
Rubber bonds consist of vulcanized natural or synthetic rubber. They are stronger
than phenolics and are often used for extra thin cut-off wheels. Bakelite rubber bond is
a mixture giving a stronger bondthanpure bakelite that allows for a thinner wheel. The
disadvantage with rubber as part of the bond is a strong smell, even with an efcient
cooling during the cutting process.
Metal bonds are used for CBN and diamond wheels. The most common metal
bond is sintered bronze that is produced by powder metallurgy methods. Other metal
bonds that are generally stronger include iron and nickel. Alow-cost diamond wheel is
made with the diamond grains xed through an electroplating process. Metal bonds
andelectroplating are usedfor slowconsumable wheels see Section2.4.2.
2.3.3 Grinding Mechanics
Abrasive cutting is a grinding process where the material removal takes place when the
abrasive grains interact withthe work piece. The mechanics of the process highly inu-
ence the result and the economy of the cut-off process; the most important parameters
will be discussedbelow.
Grinding forces, power, and specic energy forces are developed between the
wheel andthe work piece see Fig. 2.3. The total force against the wheel, F, canbe sepa-
ratedintoa tangential component F
t
anda normal radial component F
n
.
1012
The grinding power Passociated withthe force components inFig. 2.3 canbe writ-
tenas:
P = F
t
v 1
where F
t
is the tangential force andv is the wheel velocity.
An important parameter is the energy per unit volume of material removal spe-
cic energy, u.
u = P/d l b 2
where d is down feed rate (feed speed), l is length of cut (arc of contact), and b is width of
cut (widthof wheel).
The mean force per grain F
t
is another important parameter since it determines

the tendency to cause grain fracture and therefore plays a major role in relation to
wheel wear self sharpening.
F
t
= u d l b/v l b C = d/vu/C 3
where C is the number of active cutting points per square mm/in of the wheel surface.
It can be seen fromEq 3 that the ratio d/v, feed speed, and wheel velocity plays a
major role. At a higher force per grain, F
t
a given wheel should wear faster. It can be

expected that F
t
in a given cut-off operation will increase until the grain fracture

strength is reached, then the worn grain will either be sharpened fractured or forced
fromthe wheel see Section2.3.6.
Chips, Sliding, and Plowing
Some of the energy used in the grinding process is used for creating chips. These very
small chips are comparable to chips made by other cutting processes such as turning
andmilling. The grinding chips are irregular, probably because of the variationinabra-
sive grains andthe negative rake angles see belowandSection6.2.1.
Part of the energy is expended by mechanisms other than chip formation. One
such mechanismcould be attened parts of the abrasive grain sliding against the work
piece surface without removing any material, as shown in Fig. 2.4. Another part of the
energy will be used for plowing, only displacing the material without cutting see Fig.
6.3, Section6.2.
The high energy used for grinding compared to other cutting processes can be ex-
plained with the energy used for sliding and plowing. The specic energy used for
grinding is virtually the same as the melting energy of the removedmaterial.
10
2.3.4 Mechanical Damage
Abrasive cutting generates a surface with scratches that are produced by interaction of
abrasive cutting points with the work piece, as shown in Figs. 2.4 and 2.5. Both gures
showchips being removedfromthe surface of the work piece. Boththe making of chips
and the plowing will create deformation in the specimen surface see Section 6.3 and
the depth of the deformed layer will depend on the material, cut-off wheel, feed speed,
andother factors.
According to the literature
7,1317
the general deformation depth at wet abrasive
cutting will be so that it is easily removed by plane grinding with grit 220 SiC grinding
paper. For annealed polycrystalline 70:30, brass, the damage depth has been measured
to 700 m maximum depth D
d
, see Section 6.3 and signicant deformation depth to
16 m.
7
For carbon steel the damage depth has been measured to 125 mand for elec-
trolytic copper 250 m.
14
Incase of precisioncutting withvery thinwheels, a lowforce
on the wheel and lower cutting speeds, the damage is lower, in the range of 50 m.
14
For annealed steel AISI/SAE4130 deformation of below10 mhas been measured at
conventional wet cutting andless than2 mat precisioncutting.
16
Very often the unplaneness of the cut surface will be in the range of 300500 m
Fig. 2.4Schematic drawing of an abrasive grain producing a chip from a metal work piece.
see below, which means that at least the same amount of material should be removed
to obtain a plane surface. The damaged layer will be removed during this process for
most materials.
WavinessUnplane Surface
It is important to avoidwaviness during the cut. Overloading the cut-off wheel so that it
does not cut straight can cause waviness. This is due to the exibility of the wheel that
allows for cutting without breaking even if the wheel body is curved because of an ex-
cessive force F
n
in Fig. 2.3. The wheel also might cut in a curve if the point of attack
between wheel and work piece is not straight perpendicular, forcing the wheel out of
the line of movement betweenwheel and work piece. The same effect candevelop if the
cooling uid is unevenly distributed to the wheel, causing a chisel-shaped edge of the
wheel see Sections 2.6 and 13.5.1. Correct clamping is also important see Section
2.3.5.
Ina normal routine-cut specimen, the surface might be unplane withvariations up
to several hundred m.
17
The variation is strongest at the entry and the exit of the cut-
off wheel; therefore, the feed speed should be regulated often at the start and the nish
of the cut see Section2.6.
2.3.5 Thermal Damage
As described in Section 2.3.3 the total grinding energy input includes chip formation,
sliding, and plowing. Peak ash temperatures approach the melting point of the ma-
terial being ground. These very high temperatures, however, are of extremely short du-
ration and highly localized on the shear planes of the microscopic grinding chips. Just
beneath the surface the work piece feels nearly continuous heating. This heating, at
cut-off grinding, will mainly take place inthe material under the wheel see below.
Specimen burn can take place if the cut-off conditions are not correct. Visible
burns with steels are characterized by bluish temper colors see Fig. 2.6 and might
Fig. 2.5Schematic drawing of fractures taking place in the abrasive grains and the bond of
the cut-off wheel during cutting.
cause a metallurgical transformationinthe heat-affectedzone see Section13.6.2.
The models developedfor heat transfer at cut-off are for dry cutting usedfor indus-
trial purposes, but materialographic cutting with cooling should follow the same pat-
terns, but with lower temperatures. The heat is developed in the arc of contact and it
will move downwards in the material under the wheel. This means that the heated ma-
terial is continuously removed and only a relatively small part of the heat is transferred
tothe cut surfaces of work piece andspecimen. This process, however, will take place at
the end of the cut when the wheel is about to break through since no work piece mate-
rial remains to conduct the heat downwards. To avoid this it is recommended by
manual cutting to decrease the feed speed a moment before the wheel is through the
work piece. At automatic cutting a suitable low feed speed should be chosen for the
total cutting process.
Heat is also developed through friction between the sides of the wheel and the
work piece/specimen surfaces because of thermal expansion of the material under the
wheel not yet cut. The cutting parameters should be kept so that this expansion is re-
duced to a minimum see Section 2.3.8. Also, a correct clamping can reduce the fric-
tionbetweenwheel andworkpiece see below.
Clamping
It is important that the forces developed by clamping do not inuence the microstruc-
ture of the clamped work piece. This is mostly not the case when using a standard vice
Fig. 2.6Macro photograph of a steel specimen cut with thermal damage. Blue burn can be
seen.
for parts with a stiff cross section, but in the case of sensitive materials, bending and
deformationof the workpiece shouldbe avoided.
Clamping is often made by using two vices and clamping both the work piece and
the specimen, which-avoids a burr. When the wheel is completing the cut, and there is
little stock beneath the wheel, the temperature rises rapidly and the uncut material ex-
pands thermally. This forces the already cut surfaces against the sides of the wheel and
appreciable additional torque is involved. This, combined with internal stresses in the
work piece might cause the disk brake effect inwhichthe two sides of material clamp
the wheel so hard that the rotation stops and most often the wheel breaks see Section
2.6.
Wet Cutting
During materialographic cutting it is important to keep the temperature low. For this
reason the process takes place with a strong supply of a grinding uid, usually water
withanadditive see Section2.3.7.
2.3.6 Cut-off Wheel Wear
The cut-off wheel wear is decisive for the efciency of the wheel. If the wear is too low
the cutting edge will grow dull causing glazing and the cutting will stop. If the wear is
too high, the economy of the process is not correct and the quality of the cut might be
good, but the number of cuts made withone wheel is toolow.
The wheel wear involves three parameters: attritious wear, grain fracture, and
bondfracture see Fig. 2.5.
10
Attritious wear involves dulling of abrasive grains andthe
growth of wear ats by rubbing against the work piece see Fig. 2.4. Grain fracture
refers to the removal of abrasive fragments by fracture within the grain, and bond frac-
ture occurs by dislodging the abrasive fromthe binder see Fig. 2.2.
Both attritious wear and the two types of fracture depend on the tangential force,
F
t
Fig. 2.3. If the force is too low, the process will stop and the grains will be blunt,
resulting in glazing and overheating of the cut. A F
t
that is too high might cause an
increase inthe temperature inthe cut whichleads toanexcessive bondfracture.
Wheel wear is measured by the total weight of abrasive worn away during the pro-
cess. Experiments showthat attritious wear is very little, grain fracture is only a small
part of the total wear, and bond fracture is the dominant part. Attritious wear, alto-
gether negligible, is probably the most important type of wear because it controls the
grinding forces andthus governs the probability of bondfracture andthe overall rate of
wheel wear.
The grinding ratio G is a convenient measure of wheel wear and is expressed as
follows:
G= Volume ground away Q
w
/Volume of wheel consumed Q
s
The G-rationeeds tobe as highas possible tosecure agoodeconomy of acut.

The best G-ratio is obtained when the cut-off wheel and process parameters are
chosen correctly in relation to the material and shape of the work piece. Experiments
12
have shownthat the arc of contact l inFig. 2.3 is important toobtaina highG-ratio. If l
is too high the longer cuts give chip interference, the space pores between the grains
in the cut are not able to accommodate the chips that causes larger lumps to be broken
from the wheel edge, resulting in a lower G-ratio. It seems that the ideal length of l is
around 1220 mm0.50.75 in. If l is smaller, the G-ratio also drops, probably due to
a very high load on the wheel edge due to the very short arc of contact. In practical
work, l can be up to around 1520 %of the wheel diameter without problems, depend-
ing onthe material
11
see Section2.3.8.
Another important factor regarding the G-ratio is the downfeedrate feedspeed d
in Fig. 2.3.
12
It seems that at a too lowd, excessive heat is generated, probably because
of the lack of sufcient chips totake the heat away that causes the wheel towear toofast
because of the high temperature in the bond. At a certain optimumvalue of d the tem-
perature drops and the G-ratio increases. If the feed speed is further increased the
G-ratio drops because there no longer will be sufcient chip clearance to handle the
chips, the temperature increases, andthe wheel edge breaks down, as describedabove.
Inpractical work the G-ratio is inthe range 0.5 to 1.5 depending onthe hardness of
the cut-off wheel and the material to be cut. For a material like medium-carbon steel
40 mm1.50 in diameter cut with a mediumhard wheel 250 mm10 in diameter,
this gives around40to50sectionedspecimens.
Truing and Dressing
Truing and dressing are both connected to wheel wear. Truing is a process to be per-
formed when the grinding wheel is shaped incorrectly because wheel surface is worn.
Cut-off truing is done to an unround wheel, making it run concentrically. This is done
automatically with consumable wheels during the process, but truing might be neces-
sary at slowconsumable wheels.
In metallographic/materialographic preparation using grinding disks having a
plane surface, truing is done to make the disk plane, and it implies that an amount of
the diskis removedtoestablishthe original atness of the disksurface.
Dressing is a process to reinstate the cutting ability of the grains. If the grains are
glazed or the edge/surface of the wheel/disk is clogged, the surface is opened by remov-
ing a small amount of bond material with a dressing stick, normally a piece of ceramic
bonded aluminum oxide or silicon carbide. Dressing should be limited because it
causes wheel/diskwear.
Incut-off, dressing is only done onCBNanddiamondwheels see Section2.4.2.
2.3.7 Cutting Fluids
Materialographic cutting is always performedas wet grinding, using a grinding uidor
coolant. The uid has the following simultaneous functions: cooling the work piece/
cut-off wheel interface; lubrication; ushing away the chips; protecting against corro-
sion of work piece and machine; and preventing development of bacteria and fungi.
Because water is a very good cooling medium, it is used as the main ingredient. How-
ever, an additive that contains a number of components is needed to obtain the men-
tionedfunctions.
Lubrication and Cooling
As described in Sections 2.3.3 and 2.3.5, heat is developed during the grinding opera-
tion due to chip formation and friction forces in the cut. For these reasons it is impor-
tant that a relatively high lubrication takes place, reducing the power required to re-
move a given volume of material and thereby keeping the heat generation as low as
possible, andat the same time cool the workpiece toavoida heat buildup.
Synthetic Grinding FluidsOil-Based Fluids
The so-called synthetic or chemical uids used as additives to water are used for cut-off
grinding. These uids, generally dened as grinding uids contain no mineral oil and
are typically clear, but may be dyed.
The simplest uid only contains some inorganic chemicals that protect against
corrosion and bacterial attack. This uid can be described as water that doesnt make
rust, producing a very goodcooling, but nolubrication.
The most frequently used type of synthetic uid has surface active components
for better wetting of the surfaces and other components that improve the lubrication,
cooling, andcorrosioninhibition. The synthetic uidis mixedas anadditive inratios of
1:30to1:50withwater.
Semisynthetic uids have 330 % oil and give a stronger lubricating action than
the synthetic uid. It can be used instead of emulsions for band sawing and other pro-
cesses withhighfriction.
Emulsions, emulsiable oil in water and typically milky white are not normally
used for cut-off grinding, but are suited for other cutting processes, such as band saw-
ing, hacksawing, etc.
Oil-based uids are, however, often used for cutting with precision cutters using
diamond cut-off wheels. This uid can be used without mixing. Water-soluble emulsi-
able oils, that mix withwater inratios of 1:5to1:20are alsoavailable.
Grinding uids normally have a highpHandcancause skinproblems see Chapter
26 andskincontact shouldbe kept toa minimumsee below.
Application of Grinding Fluid
It is very important that the uid is taken as close as possible to the area of contact
between work piece and wheel. Caused by the rotation of the wheel, a layer of air is
moving along with the sides of the wheel. It is important that the cooling uid pene-
trates this layer and gets in contact with the sides of the wheel so that a laminar stream
of uid is established along the sides of the wheel. In this way the centrifugal force of
the wheel takes the uid into the wheel/work piece contact area. On most cut-off ma-
chines there are two nozzles positioned, one on each side of the wheel, that directs the
uid under a certain pressure towards the wheel sides. In some cases other nozzles will
lead uid to the work piece for extra cooling. Systems with the work piece totally sub-
merged in uid have also been used. These systems should, however, only be used as a
supplement to the nozzles previously described because the coolant covering the work
piece will not be able toget incontact withthe wheel sides due tolackof pressure.
The Cooling System
The most important parts of the cooling system are the pump and tank. The pump
should have a sufcient capacity to supply the uid, normally from 1015 L/ min
2.64 gal / min for tabletopmachines with200250 mm810 in cut-off wheels and
2025 L/ min 5.36.6 gal / min for larger machines with 300500 mm 1220 in
cut-off wheels. The tank should have a sufcient size, containing 2530 L
6.67.9 gal, and 80150 L 21.239.7 gal, respectively. If the tank is too small the
uid might heat up during use, and the tank will ll up too fast with ground-off mate-
rial. The tank should have a number of weirs and bafes so that the swarf and grit settle
on the bottomof the tank and are not circulated in the system. Very long chips may be
oating on the surface of the uid and may eventually clog the pump. Often a simple
lter positioned near the outlet of the machine will collect these chips. This lter
should be cleaned relatively often. Larger lters and lter conveyor swarf removal sys-
tems, originally developedfor industrial machine tools, canbe used.
Maintenance of Cooling System and Grinding Fluid
Considering the importance of a sufcient cooling, both the cooling system and the
uid should be maintained regularly. The ow to the cut-off wheel should be checked
daily toassure that the owis uniformonbothsides of the wheel. Depending onthe use
of the machine, the tank should be emptied and cleaned in regular intervals, at least
yearly. The tank should be emptied regularly for sludge to prolong the lifetime of the
grinding uid. Often the content cannot be taken directly to the sewer because local
environmental restrictions will forbid this see below and Chapter 26. The machine,
cutting chamber, and piping should also be cleaned regularly with a detergent cleaner
toprevent development of bacterial attack see below.
Water Quality
The quality of the water is important to the performance of aqueous grinding uids.
The hardness of the water content of carbonates affects the uid very often and the
amount of additive should be adjusted accordingly based on the advice of the additive
supplier. Water with a high calcium or magnesium content, or both, above 7.0 gpg
120 ppm, is considered to be hard and precautions should be taken. Either a higher
percentage of additive can be used or the water can be softened. Hard water also in-
creases the bacteria/fungi growth see below. Very soft water might cause develop-
ment of foam that often can be suppressed by reducing the amount of additive in the
coolant. Other minerals, such as metal salts also may be present in the water, disturb-
ing the actionof certaincomponents inthe additive.
Concentration of Grinding Fluid
During use, water evaporates and the concentration of additive and minerals will in-
crease see below. This canbe checkedby measuring the pHandusing a refractometer
for exact measurements. According to the advice of the supplier, additive or water, or
both, should be added. Generally straight water should not be added, but always mixed
with additive in a higher or lower concentration so that the correct values are rein-
stated. A rule of thumb is to add water with half of the normal concentration to com-
pensate for evaporation. The concentration of the minerals originating fromthe water
also will rise to maybe three to four times that of the original water during use. There-
fore, the more pure the water used for mixing with the additive and added during use,
the longer the uidcanbe usedbefore problems might develop.
Bacteria and Fungi
Bacterial growth in the cooling system often develops if a machine has not been used
for a period of time or the cleaning has not been done for quite a while. Two types of
bacteria are found in the uid: aerobic, which grow in the presence of oxygen, and
anaerobic, which grow in the absence of oxygen. The anaerobic bacteria that might
develop in the sludge in the bottom of the tank, produce hydrogen sulde that can
cause darkstaining of the workpiece andmachine andhas a strong, unpleasant odor.
The growth of fungus mold in the uid can be a larger problem than bacteria,
depending upon the type of uids used for cut-off. The presence of fungi can be seen in
the formof slimy, semisoliddeposits that cling to the walls of the tank andthe machine.
Development of fungi can be avoided by regular maintenance of the system as men-
tionedabove. Incase of serious attacks the supplier of the additive shouldbe contacted.
In case of strong development of microorganisms, a biocide can be added to the
uid, or in severe cases, the system must be emptied, completely cleaned, and treated
with a biocide germicide before it is lled up with new grinding uid. The choice of
biocide shouldbe done according toinformationfromthe supplier of the original addi-
tive because the biocide added should not be antagonistic to the biocide already in the
formulation.
Disposal of Grinding Fluids
A number of components in a used grinding uid might be dangerous to the environ-
ment and therefore should be treated with special care. These can be: components in
the original uid additive, bactericides, and fungicides used for cleaning, sludge con-
sisting of metal particles, and particles fromcut-off wheels. It is very important that all
these substances are listed and checked with the local authorities regarding their dis-
posal. Since disposal is often very troublesome and expensive, the advantage of good
maintenance is evident; by constantly removing sludge and keeping the uid clean, the
disposal of the uidcanbe done relatively seldom.
Health and Safety Aspects of Grinding Fluids
The operator working with wet abrasive cutting can be affected in one or more of the
following ways: skin contact, oral ingestion, inhalation, and eye contact. The uids
used mostly for cutting are of the water-miscible synthetic chemical type having a
high pH 8.59.5 and a low surface tension. If skin is exposed to this uid for a long
period of time it loses its protective oily layer and, inseldombut some cases, dermatitis
can develop. This can be avoided by careful prevention and the operator should not
come in contact with the uid by using gloves, barrier creams, etc., and by maintaining
the uidsothat it is cleanandthe concentrationis correct.
Inhalation of mist and fumes can be avoided by having the cutting chamber con-
nected to a ventilation system. The operator should use protective glasses to avoid eye
contact.
ASTM Standards
Anumber of ASTMstandards are relatedtogrinding uids, the most important are:
StandardPractice for Selecting Antimicrobial Pesticides for Use inMiscible Metal-
working Fluids E2169
Standard Method for Evaluation of Antimicrobial Agents in Aqueous Metal Work-
ing Fluids E686
Standard Test Method for Evaluating the Bacteria Resistance of Water-Dilutable
Metalworking Fluids D3946
StandardPractice for Safe Use of Water-Miscible Metal Removal Fluids E1497
2.3.8 The Metallographic/Materialographic Cutting Operation
The metallographic/materialographic cutting operationhas the following goals:
1. Produce a specimensurface withlowest possible deformations andscratches.
2. The surface shouldbe without any thermal damage.
3. The surface shouldbe at without waviness andwithout a burr.
4. The cut-off should be done with lowest possible costs, meaning lowest possible
wheel wear highG-ratio andinthe shortest periodof time.
The Parameters
The following parameters are available for the operator when cutting with a normal
cut-off machine see Section2.5andFigs. 2.3and2.7:
Cut-off Wheel rpm
This is normally in the range of 20003000, depending on the diameter of the wheel
see belowandSection2.4.1.
Wheel Velocity
Based on the rpm, the velocity v can be calculated. This should be in the range of
30 to 50 m/ s 600010 000 fpm. On most cut-off machines the rpm, and conse-
quently, the velocity, is a xed value that the operator will not be able to change. The
velocity will decrease withthe decrease of the wheel diameter causedby wear.
On some newer models of cut-off machines the rpm is made variable, making a
variation in wheel velocity possible. This changes the forces on the wheel see Section
2.3.3 and therefore also strongly inuences the wheel wear, meaning that a hard
wheel canbe changedtoa soft wheel by reducing the rpmandvice versa.
Force
The force F is an important parameter relating to wheel grade hard/soft, work piece
material, and length of cut arc of contact. Normally the force is not used as a control-
ling parameter, but made available to accommodate the selected feed speed, even at
long arcs of contact see Section2.3.6.
Feed Speed
The feed d will vary according to material, length of cut, etc. It is usually in the range
of 0.0055 mm/ s 0.0002 to 0.2 in/ s. This parameter can be controlled by the opera-
Fig. 2.7Schematic drawing of wet abrasive cutting process. The cut-off wheel is fed into the
work piece. The work piece being with a circular cross section, the arc of contact between
wheel and work piece, l, will vary from a point when the wheel touches the work piece to
the total diameter of the work piece, when the wheel is half way through.
tor andis very important toobtaina correct cut see below.
Power
The electric motors available in the cut-off machines range from 15 W to 10 kW. The
power consumption expresses the tangential force, F
t
in Fig. 2.3. The operator will of-
ten be able to observe the power consumption on an amp meter, and, if necessary, ad-
just the feed speed up for a higher power consumption and down for a lower
consumption.
Arc of Contact
The contact area l between work piece and wheel plays an important role in the pro-
cess. Preferably the arc should be in the range of 1250 mm 0.52 in, but it is often
longer. As a general rule, the work piece should always be placed so that the arc is the
shortest possible see Fig. 2.8. When cutting large work pieces, it is helpful to use an
oscillating movement of the wheel or work piece, or to rotate the work piece see Sec-
tion2.5.1.
Free Cutting
Based on the relations discussed earlier in this chapter, the expression Free Cutting
can be used as a Rule of Thumb. Free cutting is achieved when the correct balance is
obtained between force wheel against work piece, feed speed, and power consump-
tion, giving a correct cut with the highest G-ratio. The balance is reached at a feed
speed corresponding to the optimumchip removal. If the feed speed and force are too
low, the wheel edge gets blunt and heats up the work piece, stopping the process. On an
automatic machine, if the feedspeedis set toa certainvalue, anda lower feedor nofeed
is obtained, the same will happen because the wheel is too hard for the given material.
If the force is increased without a corresponding increase in feed speed, the cut be-
comes too hot, causing the bond to fracture, and the wheel will start to break down at a
rapidrate or bend.
Fig. 2.8The work piece should be placed correctly to obtain the shortest area of contact
between cut-off wheel and work piece. a This position will give a short area of contact; b
this position will give a longer area of contact and should be avoided.
Free Cutting by Hand
When cutting a work piece by hand, rst a notch is made in the work piece with low
force to secure a straight cut. Then the force is increased until the feed speed is con-
stant, being the free cutting state. Free cutting is when an increase in force does not
increase the feed speed. If a reasonable feed speed is not obtained, even with a rela-
tively strong force, the wheel is too hard for the given material. If a relatively high feed
speedcanbe obtainedwithout a reasonable force, the wheel is probably toosoft.
Free CuttingAutomatic
Cut-off machines often have a hydropneumatic or electric electronic feed system, en-
abling the operator to establish an automatic feed see Section 2.5. To obtain a free
cutting, feed speed and power consumption are compared, the consumption express-
ing the force in the cut. The feed speed is increased, and as long this increase has a
corresponding increase inpower consumption, the situationis correct and free cutting
is made, provided that a sufcient force is available. When adjusting to a higher feed
speed, no increase can be observed but the power consumption goes up, the feed speed
should be reduced because the force in the cut is too high. The wheel will start to break
down at a too high rate or bend. The operation described is assuming that a sufcient
force between wheel and work piece is available. If the force is not adequate for a given
arc of contact, the feedwill, of course, stopor be toolowsee Section2.5.1.
2.4 Abrasive Cut-Off Wheels
Two types of wheels are used for metallographic/materialographic cutting: consum-
able wheels and slow consumable wheels. Consumable wheels are based on inexpen-
sive abrasives, whereas slowconsumable wheels are made withdiamondor CBN.
2.4.1 Consumable Wheels
With consumable cut-off wheels, the whole wheel is made froma resin bond, bakelite
or rubber, or a combination of these, with mixed-in abrasive grains, either aluminum
oxide Al
2
O
3
or siliconcarbide SiC see Fig. 2.9andSection2.3.2.
The consumable wheel functions by wearing down during the cut-off process, the
wear being related to the wheel grade. The wheel grade goes fromsoft to hard, allowing
cutting of hardmaterials upto HV700800 witha soft wheel andsoft materials witha
hard wheel. Al
2
O
3
is used for cutting of most ferrous materials and SiC for nonferrous
andcast iron.
There are normally six to seven different grades available based on either Al
2
O
3
or
SiC. Typically the grades are specied according to material type and hardness, span-
ning from soft nonferrous materials to very hard ferrous materials. When cutting
larger work pieces with a long arc of contact, a wheel with a relatively coarse abrasive
shouldbe usedanda soft grade might be neededsee Section2.3.2.
Wheel Velocity
The consumable wheels, being rather brittle, are not to be used with wheel velocities
higher than stated on the wheel, normally a maximumof 50 m/ s 9800 fpm or 60 m/ s
11 800 fpm.
The wheel velocity depends on the rpm of the wheel and the wheel diameter. The
velocity canbe calculatedfrom:
Velocity =
rpm Diameter of wheel mm
60 1000
m/s
or
Velocity =
rpm Diameter of wheel in
12
fpm
The velocity for consumable wheels is typically 3550 m/ s 69009800 fpm.
Most cut-off machines for general use have a xed rpm except precision cut-off
machines see Section 2.5, setting the wheel velocity. Because the wheel velocity, even
with consumable wheels for general use, has an important impact on the cut-off pro-
cess, newer machines canbe made withvariable rpmsee Section2.5.
Wheel Dimensions
The consumable wheels are normally available in diameters: 100 mm 4 in, 125 mm
5 in, 150 mm 6 in, 175 mm 7 in, 200 mm 8 in, 235 mm 9 in, 250 mm 10 in,
300 mm12 in, 350 mm14 in, 400 mm16 in, 432 mm17 in, 450 mm18 in.
Thickness of the wheels varies from 0.5 mm 0.02 in at the smallest diameters to
3.0 mm0.12 in at the largest.
Arbor shaft diameter is normally 32 mm1.25 in. For small wheels for precision
cutting: 12.7 mm0.5 in.
Storing
Consumable wheels should be stored in a dry atmosphere and laid at on a stiff at
surface to prevent bending of the wheel. To safeguard the wheels it is useful to have a
Fig. 2.9Consumable cut-off wheel. The entire wheel is made of a resin bond with an abrasive
Al
2
O
3
or SiC and will be totally worn down during the process.
vertical shaft protruding from the holes in the wheels and a weight may be placed on
the top. Bakelite wheels especially will deteriorate when stored in a humid
environment.
2.4.2 Slow Consumable Wheels
As indicated in the designation, these cut-off wheels are worn during the process, but
not to the same degree as consumable wheels. The abrasives used in consumable
wheels are the super abrasives, diamond and CBNsee Section 2.3.2. The single grain
is worn very slowly and therefore a very stable bond is used, either metal or resin
bakelite. This secures that the abrasive stays in place and is not torn away from the
wheel, as is the case withconsumable wheels.
The slowconsumable wheels are usually made with a metal body and the abrasive
with the bond is placed around the periphery of the body see Fig. 2.10. The abrasive/
bond layer can be a continuous layer around the periphery continuous rim or in seg-
ments. The metal body allows for very thin wheels, down to 0.15 mm0.006 in suited
for precisioncutting.
In cutting wheels with electroplated abrasives, the abrasives are placed in a band
along the periphery of a metal body and covered with a metal layer. These wheels only
have a thin layer of abrasive; they are less expensive than the wheels described above
andtheir lifetime is shorter.
Truing and Dressing
Because the slow consumable wheels have a very stable bond, the abrasive grain does
not readily break away even when very worn. Also, the edge of the wheel may clog up
Fig. 2.10Slow consumable cut-off wheel, continuous rim. The body of the wheel is metal and
the rim is a bond metal or bakelite with diamond or CBN. The wear is very low, caused by
cutting and dressing.
with abraded material that stops the cutting action. Therefore, truing or dressing must
be done. With truing, the shape of the wheel is corrected see Section 2.3.6 and this is
normally not necessary for a slow consumable cut-off wheel. Dressing is important,
because it exposes newabrasive grains in the edge by removing bond material and to a
certain degree removes worn down grains. Dressing is done with a dressing stick made
fromhard materials such as sintered Al
2
O
3
and SiC that is held against the edge of the
wheel for 510 s.
Attention: Dressing should not be overdone because it wears down the relatively
expensive wheel.
Use
Slow consumable wheels are used frequently when consumable wheels are not suit-
able.
Cut-off in general: For cutting of ferrous metals with hardness higher than ap-
proximately HV 500700 and up to HV 1400, CBN wheels are used. For sintered car-
bides, ceramics, and other very hard materials, diamond wheels are used. Tough duc-
tile materials like sintered carbides are cut with a bakelite bond and most hard and
brittle materials witha metal bond.
Precision Cut-off
This operation, done onprecisioncut-off machines see Section2.5 oftencalls for very
thin wheels belowa thickness of 0.5 mm0.02 in; therefore, slowconsumable wheels
are used. Normally, when cutting hard materials and composites, metal bond is used
with either high or low diamond concentration. High concentrations are used for the
softer materials and lowconcentrations for the hardest materials like ceramics. At low
concentrations the cutting action is high because of the fewer abrasive grains, creating
a higher force on each grain see Section 2.3.3. If possible, ductile materials, like most
metals, should not be cut with slow consumable wheels. The ductile metal will con-
stantly clog up the edge of the wheel, the cutting action will be very low, and the wheel
will wear its way through the work piece. When cutting most metals on a precision
cut-off machine, a thinresinbondedconsumable wheel shouldbe usedif a thickness of
0.5 mm0.02 in canbe allowed.
Wheel Velocity
The wheel speed should be approximately 25 m/ s 4900 fpm. This can be established
withmost precisionmachines see Section2.5, but oftenthe heavier machines for gen-
eral cutting will not be able to accommodate this relatively low wheel velocity. At low-
speed cutting with small precision cutters, very lowwheel speeds in the range of 2 m/ s
395 fpm are usedsee Section2.5.2.
Wheel Dimensions
Slowconsumable wheels for general use are available in diameters from200400 mm
816 in. Thickness from 12.2 mm 0.040.09 in. Shaft diameter arbor is nor-
mally 32 mm1.25 in.
Wheels for precision cutting wafering are available in diameters from
75200 mm38 in. Thickness varies from0.150.9 mm0.0060.035 in. Shaft ar-
bor is normally 12.7or 22 mm0.5or 0.87 in.
Storing
Slow consumable wheels should be stored laid at on a stiff, at surface. Especially
thin wheels should be treated with utmost care because of the risk of bending the
wheel. The boxes inwhichthe wheels were suppliedshouldbe usedfor storage.
2.5 Abrasive Cut-off Machines
Metallographic/materialographic cut-off machines are made for wet abrasive cutting
of a work piece to obtain a sample specimen. The machine is normally built for a cer-
tain size of the cut-off wheel, deciding the power of the electric motor driving the
wheel.
It is important that the cut-off wheel and work piece are sealed off fromthe opera-
tor during the cutting toavoiddamage topersons incase of wheel breakage.
The machine has a systemfor moving either work piece or wheel toestablisha feed
movement see below. It also has a system for adding cooling/lubricating uid to the
cutting area. The work piece is normally placed on a table to allow for xing the work
piece before cutting. The spindle carrying the wheel should be without play and the
machine designshouldbe stable toavoidvibration.
During the cutting, mist andfumes are developed, andthe machine shouldhave an
outlet for anexhaust system.
2.5.1 Design Principles of WheelWork Piece Contact
As described in Sections 2.3.3 and 2.3.8, the arc of contact or contact area between
work piece and cut-off wheel should be kept around ideally 1250 mm 0.52.00 in,
and preferably kept constant during the whole operation. This is often not possible at
direct or chop cutting where the contact area will vary strongly with the shape and
the size of the work piece see below. To avoid this, a number of designs have been
developedtokeepthe contact area constant.
Direct Cutting
The wheel and work piece contact is dependent on the shape of the work piece as
shown in Fig. 2.7 and 2.12a. If a 50 mm 2 in shaft is cut, the length of the contact
area will vary froma point when the wheel rst touches the work piece to more than
50 mm when the diameter of the work piece is reached. This means that the force be-
tweencut-off wheel and work piece canbe very lowat the beginning but has to increase
to ensure a sufcient force on the abrasive grains at the long arc of contact see Section
2.3.6. This is normally solved by operating with a sufciently high force and control-
ling the feed speed, keeping it constant through the whole cut. With the correct cut-off
wheels and machine data, a direct cut can be made on almost all materials, even up to
large sections. A rule of thumb would be that a dimension up to 1520 % of the wheel
diameter canbe cut directly, depending onthe material andthe type of wheel.
Oscillating Cutting
During oscillating cutting, the feed movement between the work piece and the wheel is
combined with a relative movement between the two. This means that the arc of con-
tact is kept low and dependent of the length of the total cut only to a certain degree so
the cutting force can be kept at an optimum value. For metallographic/material-
ographic cutting the oscillating movement also has the advantage of making roomfor
the cooling uid, improving the cooling inthe cut.
Oscillating cutting can be made with an oscillating wheel or an oscillating work
piece as shown in Figs. 2.11 and 2.12b. In most cases, the arbor spindle carrying the
wheel is moved in a circle ellipse or a horizontal lateral movement in the same plane
as the wheel, in this way creating a movement relative to the work piece, as shown in
Fig. 2.12b. Only a small amplitude, 12 mm 0.040.08 in, a in Fig. 2.11, is neces-
sary tolimit the arc of contact.
When oscillating the work piece, the table with work piece is moved in a tilting or
reciprocating movement. Figure 2.12b, shows anoscillating wheel but it caneasily be
imaginedthat the workpiece has a movement giving the same effect.
Oscillating cutting makes it possible to cut very large work pieces even from dif-
cult to cut materials. The short arc also makes it possible to work with harder wheels,
thus reducing the costs.
Fig. 2.12Comparison between direct cutting a and oscillating cutting b. At oscillating
cutting the cut-off wheel can be moved relative to the work piece, as shown, or the table with
the work piece can have a tilting or reciprocating movement, not shown.
Fig. 2.11Principle of oscillating cutting; the cut-off wheel moves relative to the work piece.
Step Cutting
Another way of avoiding the long arc of contact is step cutting Fig. 2.13. In this prin-
ciple the wheel is moved in increments into the work piece, or vice versa, while moving
the wheel back and forth, performing the process in steps. The depth of each step in-
crement dictates the contact arc and this depth can be selected according to the hard-
ness of the work piece material and the hardness of the wheel. The advantage of step
cutting is that very long work pieces can be cut independently of the size of the wheel
andvery hardandtoughmaterials canbe cut.
Fig. 2.13Schematic drawing of step cutting. The cut-off wheel is fed into the work piece in a
step of 15 mm 0.040.2 in and moved along the work piece to the end where a new step is
made.
Rotating Work Piece
In the case of a rotating work piece, the arc of contact is only a point where work piece
and cut-off wheel are touching each other see Fig. 2.14. In some cases this is the only
way to cut very hard materials like sapphire, and by cutting of coatings, the coating is
supported all the way around, avoiding peel-off. This way of cutting also will give
double cutting depth because the cut-off wheel will only reach halfway through the
work piece. Complementary rotation should be preferred see Fig. 2.14. The gure
shows a work piece with a circular cross section, but other shapes can be rotated and
cut. However, this usually causes some cutting in air because the wheel will rst touch
the corners of the workpiece.
A rotating work piece is mostly used at precision cutting but special rotating
chucks are alsoavailable for general use machines.
2.5.2 Machine Designs
Cut-off machines can be designed according to different principles regarding move-
ment of work piece/wheel see Fig. 2.15.
18
The wheel is either moved towards the work
Fig. 2.14Schematic drawing of a rotating work piece showing complementary and
contra rotation. With a rotating work piece, the cut-off wheel and work piece only touch
in a point, and the specimen will be cut off when the wheel reaches the center of the work
piece; this will double the cutting capacity of the machine.
Fig. 2.15Design principles for the metallographic/materialographic cut-off machines. At a, b,
and c, the cut-off wheel is fed into the work piece. At d, e, and f, the work piece is fed into the
cut-off wheel.
piece, a, b, c, or the work piece is moved towards the wheel d, e, f. In the case of the
radial in-feed shown in a, c, d, and f, the depth of the cut is limited to the part of the
wheel outside the ange. At b and e, the work piece is attacked tangentially, and a larger
work piece can be cut if the movement of the cut-off wheel b or the work piece e allows
for it.
Most modern machines are built according to c, where the cut-off wheel is moved
intothe work piece that is xedona stationary table, or e, where the work piece, xedto
a movable table, is moved into the stationary cut-off wheel which in most cases is
placed on the motor shaft. In some machines the two principles are combined, giving
more exibility.
Cut-off Machines for General Use
Smaller machines for wheels of 200250- mm810- in diameter are mostly table top
models with an external recirculation system for the cooling uid. Most of these
smaller machines are hand-operated, and the cut is a direct cut see Section 2.5.1. The
motor power for these machines is in the range of 14 kW. An example of a hand-
operatedtable-topmachine is showninFig. 2.16.
Machines for wheels of 300 mm 12 in and larger are mostly oor models with
recirculation systems included in the machine, with motor power ranging from
410 kW. These machines are usually automatic, meaning that the feed speed is con-
trolled by hydropneumatics or by electric means. In the case of electrically driven feed,
this can be controlled by a microprocessor, allowing for adaptive control so that the
optimum feed speed in relation to motor power is found see Section 2.3.8. An ex-
ample of anautomatic, oor-basedmachine is showninFig. 2.17.
Fig. 2.16Standard manual laboratory cut-off machine for chop cutting with dual vices to
clamp samples on both sides of the cut-off wheel. A 3 kW motor and 254 mm 10 in cut-off
wheels with cut capacity 76 mm 3 in in diameter.
19
Most machines have tables with T-slots for exible positioning of the work piece,
often with quick clamping devices. The cutting compartment should be closed accord-
ing to the rules of safety. It shall not be possible for the operator to open into the com-
partment before the wheel has stopped. The compartment should be easy to clean,
without too many components and corners. It is also an advantage if electrical parts,
suchas the motor, are not placedinthe cutting compartment.
An efcient cooling system is important, taking the grinding uid effectively into
the cut, witheasy access tocleaning.
Large machines should have a system for reducing the arc of contact between
wheel andworkpiece see Section2.5.1.
Precision Cut-off Machines
Precision cut-off machines are dened as machines being able to cut with relatively
high precision, the work piece being placed in a xture, moved with a micrometre
screwor automatically. Where machines for general use are mostly usedfor metals, the
precisionmachines are oftenusedfor other hard materials suchas ceramics andelec-
tronic parts to be cut with diamond cut-off wheels. Most of these cutters have variable
speed, from very low 50 rpm to 5000 rpm. The wheels are from 75 to 200 mm
Fig. 2.17Automatic cut-off machine with oscillating cutting and step cutting for obtaining
the minimum contact area. A 10.5 kW motor and 432 mm 17 in cut-off wheels with cut
capacity 160 mm 6.3 in diameter, cutting length 450 mm.
20
3 to 8 in in diameter and often very thin, securing a very low loss of material kerf
loss which can be important when cutting materials of high value. On most modern
machines both consumable and slow consumable wheels can be used. The work
pieces, electronic parts, optical parts, and other parts where a precision cut is needed,
are normally of a size upto5075 mm23 in.
Fig. 2.18Low speed precision saw for low volume applications. A 15 W motor, 0300 rpm
and up to 125 mm 5 in diamond wheels, 32 mm 1.25 in cutting capacity.
19
Fig. 2.19Precison cut-off machine for automatic precision cutting of larger specimens.
Adjustable vertical position of the cut-off wheel makes use of small wheels, 75 mm 3 in, and
large wheels, 200 mm 8 in, easier to work with. Automatic feed speed adjustment and 5 m
specimen positioning. An 800 W motor, up to 5000 rpm. Cutting capacity 60 mm 2.3 in,
cutting length 190 mm 7.5 in.
20
Precision machines are built according to the same principles as the general pur-
pose machines see Fig. 2.15. The smallest machines are built according to f in Fig.
2.15, with the work piece being fed into the wheel by a weight constant force. These
machines are made for use with slowconsumable wheels diamond because consum-
able wheels cannot be used with the very simple feed systemwithout getting unround.
The speedis low, inthe range corresponding to300 to 600 rpm, andthe motor power is
very low, 15100 W. Anexample of a low-speedcutting machine is showninFig. 2.18.
The larger machines typically have a table with the xed work piece moving linear
into the rotating cut-off wheel, Fig. 2.15, d and e. The motor power is in the range of
5001000 W.
The feed, y-movement, can be hand-operated or automatically controlled by a
microprocessor. The xture, placed on a table carrying the work piece, can be with a
micrometre or with automatic control of the x-movement, positioning the work
piece. An example of an automatic precision cutter is shown in Fig. 2.19. All machines
have a system for cooling uid to be taken into the cut. With machines running more
than approximately 300 r/ min, the cutting compartment is protected by a hood and it
shouldbe securedthat the wheel is stoppedif the hoodis opened.
2.6 Advice and Hints on Wet Abrasive Cutting
When working with cut-off, it is possible to routinely make a number of precautions to
secure a goodcut and, therefore, a goodspecimen.
Fix the work piece securely before cutting. Take care that the cut-off piece the
specimen is not squeezed against the wheel during the cutting. Preferably the
specimenshouldbe lightly clampedtoavoida burr.
When clamping sensitive work pieces, place some soft material, such as plastic,
betweenthe workpiece andthe clamptoavoiddamage.
Whenintroducing the wheel intothe work piece at manual cutting, doit slowly and
stop the feed for 2-3 s to allowa notch kerf to be formed. This secures a straight
cut. This is especially important at tapered or rounded work pieces. If the wheel is
not cutting straight fromthe beginning it will cut sideways andultimately break.
Pay attention at manual cutting when the cut-off wheel is almost through the work
piece. Lower the feed speed to avoid overheating of the edge of the specimen or
pinching of the wheel.
Check the edge of the cut-off wheel. It should be at square whencutting medium
thick sections, at with rounded corners large sections, or concave thin sec-
tions, indicating that the proper cut-off wheel is used and normally giving a burr-
free cut. If the edge is strongly rounded convex or pointed, the wheel is probably
too hard for the material and a softer wheel should be used. Aglazed edge indicates
a wheel that is too hard, which requires a too high force and therefore develops
excessive heat. If the edge is chisel shaped, the ow of cooling uid to the wheel is
uneven, giving a crookedcut possibly causing wheel breakage see Section13.6.2.
Disk brake effect: In some materials having internal stresses the work piece will
tendto pinchthe wheel, very oftenwhenthe cut is almost nished. This cancause a
breakage of the wheel because the pressure betweenthe twoparts of the work piece
is so highthat the rotationstops. This effect might be avoided whenworking witha
very low feed speed, 0.5 mm/ s 0.02 in/ s or lower, and preferably oscillating/step
movement, minimizing the development of heat.
Whencutting a material for the rst time, check that the feedspeedandpower con-
sumption force in the cut are in reasonable balance. If yes, the wheel is free-
cutting see Section 2.3.8. If the force on the wheel increases, shown by an in-
crease in power consumption, without a visible increase in feed speed, the setting
of the feed speed is probably too high and it should be reduced. If the force is al-
lowed to mount, the wheel might bend and a straight cut plane surface is not ob-
tained, or the wheel might break.
Cutting of a work piece with a coating: Take care that the cut-off wheel is moving
through the section of the coating to be examined and into the base material. In
this way the coating is preserved, because it is in compression and not torn away
fromthe base material.
Mounting before cutting: In some cases it is an advantage to mount the specimen
before sectioning to be able to establish a correct cutting plane or avoid breakage.
This can be failure analysis with cracks/corrosion, electronic parts, small speci-
mens of plastic, or very brittle specimens. The mounting is done mostly with a cold
mounting resin, preferable epoxy see Section 3.8. To avoid clogging of the edge
see electronic parts below.
Cutting of electronic parts: Often these parts contain soft copper and very hard
brittle materials ceramics. Use an electroplated diamond wheel precision cut-
ting; this wheel has diamonds on both the edge and the sides, and it will cut
throughductile andbrittle materials without clogging see Dressing below.
Whenthe wheel is too hard glazing, anda softer wheel is not available, try a worn-
down wheel which causes a lower cutting speed and thereby a softer acting wheel,
or use a thinner wheel. In the case of hand cutting, pulse cutting, by beating the
wheel into the work piece will create a wheel wear and the wheel will start cutting;
only the lifetime of the wheel is reduced. Another possibility is to make incisions in
the periphery of the wheel, using a pair of pliers to break out small pieces with
5075 mm23 in indistance. This alsoincreases wheel wear.
Cutting may cause harmful gases derived from the phenolic bond and a rubber
bond will normally develop a strong smell. Therefore, the cut-off machine should
be connectedtoanexhaust system.
The hood of the cutting machine should be left open after use so that the machine
and cut-off wheel can dry out, reducing corrosion of the machine and prolonging
the lifetime of the wheel.
Dressing: Diamond and CBN wheels can have a material build-up on the edge of
the wheel clogging, reducing the cutting ability. The edge is dressed, cleaned,
using a dressing stickof Al
2
O
3
, for about 510 s.
For Trouble Shooting, see Section13.5.
2.6.1 Cut-off Wheel Selection
Rule of thumb: Use a soft wheel for a hard material or a large work piece and a hard
wheel for a soft material or a small workpiece.
Both hardness and ductility of the material must be evaluated. A soft material will
not wear out the abrasive very fast, therefore a hard wheel can be used. A ductile mate-
rial might clog the wheel rimso that a softer wheel must be used. On the other hand, a
ductile material might pull out the grains, causing excessive wear. A hard material will
wear out the grains fast, therefore the wheel shouldbreakdown, releasing newgrains.
General Use
Nonferrous metalsThese are relatively soft up to HV 350. Use a hard bakelite
phenolic resin wheel withSiC.
Soft ferrous metalsUp to HV 350. Use a hard bakelite or rubber-resin wheel
withAl
2
O
3
.
Medium hard ferrous metalsUp to HV 550. Use a medium hard bakelite or
rubber-resinwheel withAl
2
O
3
.
Hard ferrous metalsUp to HV 950. Use a soft bakelite or rubber-resin wheel
withAl
2
O
3
.
Very hard ferrous metalsHarder than HV 950. Use a slow consumable CBN
wheel withbakelite bond.
Sintered carbides/hard ceramics relatively ductileUse a slow consumable
diamondwheel withbakelite bond.
Ceramics/minerals relatively brittleUse a slow consumable diamond wheel
withmetal bond.
PrecisionCutting
Soft and medium hard materialsUse a medium hard bakelite wheel with
Al
2
O
3
.
Medium hard and hard materials, hard, ferrous metalsUse a medium soft
bakelite wheel withAl
2
O
3
.
Very hardferrous metalsUse a slowconsumable CBNwheel with high concen-
tration, metal bond.
Extremely hard ferrous metalsUse a slow consumable CBN wheel with high
concentration, bakelite bond.
Ceramics, minerals, very hard materials, general useUse a slowconsumable
diamondwheel withhighconcentration, metal bond.
Brittle materials ceramics, mineralsUse a slowconsumable diamond wheel
withlowconcentration, soft metal bond.
Electronic parts, hard tough materials, medium to soft ceramics, structural
ceramicsUse a slow consumable diamond wheel with low concentration, metal
bond.
Polymers and other soft materialsUse a slow consumable diamond wheel
withhighconcentrationandmetal bond, or a toothedsawblade.
Soft and ductile nonferrous metalsUse a medium hard bakelite wheel with
SiC.
2.7 Other Sectioning Methods
As described earlier, wet abrasive cutting is the dominating cut-off method for
materialographic specimens. Other methods, however, are used either because they
are simple and effective like fracturing, shearing, punching, and sawing, or because
they give a gentler treatment of the cut surface, like wire cutting, than can be obtained
withwet abrasive cutting.
2.7.1 Fracturing
Fracturing can be done on brittle materials like hardened tool steels, ceramics, etc. Of-
ten a notch is made to control the fracture. Less brittle steels and cast iron can be
cooledinliquidnitrogenbefore fracturing.
2.7.2 Sectioning by Melting
Cutting using methods based on melting the material to be cut is not recommended for
metallographic specimens. The melting process always develops zones affectedby heat
and changes the material, often far fromthe cut surface.
16,21
As some of these methods
are usedinspite of the drawbacks, the most important methods shouldbe mentioned.
Oxyacetylene Torching
This method should only be used when no other method is available and it should only
be used for obtaining a relatively large work piece for further cutting in the laboratory
withother means. Whencutting-off steel specimens it shouldbe consideredthat a zone
of at least 25 mm 1 in has been affected by heat during the torch cutting,
21
but often
the affectedzone is wider see Fig. 13.1.
Plasma Torching
This method also creates a heat-affected zone with material changes and
microcracks,
16
andshouldonly be usedfor cutting a workpiece for further cutting.
Laser Cutting
During laser cutting the heat-affected zone is the range of 0.5 mm 0.02 in for an an-
nealed steel AISI/SAE4130,
16
and care should be taken to remove enough material at
the grinding stage if laser cutting is usedfor the specimen.
Electric Discharge Machining
Electric discharge machining EDM, or spark machining, is a process that uses sparks
in a controlled manner to remove material from a conducting work piece in a liquid
dielectric.
22
The sparks melt the specimenmaterial creating craters inthe surface anda
heat-affected zone belowthe surface. Withcertainmaterials that have beenmelted and
then solidied, the molten material may absorb extraneous alloying elements fromthe
surroundings.
7
A layer containing cracks also may develop immediately beneath the
surface. Both the craters and the heat-affected zone can be several hundred m deep,
and care should be taken, especially in heat-sensitive materials, so that the damaged
layer is removedduring the grinding process.
2.7.3 Shearing
Ashear canbe usedfor cutting of sheets andother at products of not very hardmateri-
als. The edge of the produced specimen will be heavily damaged by cold work and a
burr often develops. The cold work will alter the microstructure in a layer of the speci-
men in most cases, and it is important that this material is removed during the plane
grinding and ne grinding process. For this reason, shearing is not recommended for
materials that are sensitive tomechanical twindeformation.
9
A hand shear can be used for cutting work pieces up to 46 mm 0.150.25 in,
depending on the type of material. For shearing of stock up to 13 mm 0.5 in a power
shear is needed. The power shear is built with a table for placing the work piece and a
lower blade integrated in the table and an upper blade moved mechanically or by hy-
draulics. The work piece is xed during the shearing process by a hold down foot very
close to the lower blade. The upper blade is not attacking the work piece in its full
length, but the blade has a slope called the rake. The rake is given by the design of the
shear. The load required to shear the work piece material depends on the thickness and
type of material and the rake. In normal shearing a portion of the material is sheared
and the rest is broken through due to the shearing action. As an example, in mild steel
upto 6 mm0.25 in, one-half will be shearedandthe rest will break. The shearing load
increases strongly with the thickness of the work piece, although mild steel of 9.5 mm
0.38 in is only approximately 50 % thicker than 6 mm 0.25 in; the load needed is
225 %higher. For this reason, a shear should not be used for cutting of metallographic
material thicker than the rated capacity, even in narrowpieces. On most power shears
the upper blade will move in a plane 0.51 away from vertical, allowing the upper
blade to contact the work piece immediately above the edge of the lower blade. When
the upper blade moves downwards and edge contact is obtained, the correct clearance
is developed and this clearance will increase when the blades overlap. In principle, the
blades should be adjusted according to the thickness of the work piece, but at most
modern shears the blades can be set for a wide range of thicknesses. If shearing of both
thin and thick products are made, the shear should be adjusted to minimumclearance
to avoid thin stock wedging between the blades. It is very important that the clearance
setting is correct and accurate grinding of the blades is maintained. If the edges of the
blades are rounded by wear, or the clearance is too high, the burr mentioned above will
increase.
The shear is a safe tool touse as long the operator follows the givenrules.
The shear is a precision machine tool and should be kept in good working order
according tothe instructions of the supplier.
Punching
Punching is shearing using a die and a punch and it is used for foils and thin plates to
make circular or rectangular specimens. An example of a circular specimen is the
punching of samples for electrolytic thinning see Section 8.6. Rectangular specimens
are used for printed circuit boards PCBs see Section 7.10.1. Rectangular specimens
also are used for steel sheet because the long edge of the specimen can be aligned to the
rolling directionof the sheet.
As with shearing see above, cold work and a burr will be developed in the process
andthis shouldbe removedduring the grinding stage of the preparation.
2.7.4 SawingTable 2.1
Sawing is a machining process using a circular blade or a straight band having a series
of small teeth for cutting of most materials. By sawing, material is removed from the
work piece in chips as described in Section 6.2 and shown in Figs. 6.1 and 6.2. When
sawing, the rake angle see Fig. 6.2 is always neutral 0 or positive, up to 10 for
power hacksawing and bandsawing and 18 for circular sawing. The distance between
adjacent teeth on the saw blade is called the pitch, normally expressed in number of
TABLE 2.1Recommended Band Pitches for Sawing of Work Pieces of Different Thickness.
Work Piece Thickness Band Pitch
Less than 25 mm 1 in 10 or 14
2575 mm 13 in 68
75150 mm 36 in 46
150300 mm 612 in 2 or 3
Over 300 mm 12 in
1
1
2
to 3
teethper inch, andit depends primarily onthe cross sectionarea of the work piece tobe
cut and to a lesser degree on the type of material. As a rule, two or three teeth should be
engaged with the work piece at all times during sawing. Under Bandsawing, below, the
tooth geometry, pitch, etc., are further discussed. Sawing should be performed with a
cutting uidsee Section2.3.7.
The surfaces created by sawing normally are rather rough, but if correctly treated
in the following specimen preparation, sawing can be used for sectioning of
metallographic/materialographic specimens.
Hacksawing
The hand-held hacksawoften can be used for cutting of a work piece froma large part,
maybe placed outside the materialographic laboratory, the work piece later to be sec-
tionedby wet abrasive cutting to produce a specimen. If the hacksawis usedfor cutting
a specimen froma work piece, the surface should be carefully prepared, often with an
extendedplane-grinding steptoremove coldworkanddeformationsee Fig. 13.2.
Power Hacksawing
Power hacksawing is characterized by the reciprocating action of a relatively short,
straight-toothed blade that is drawn back and forth over the work piece in much the
same manner as a handhacksaw.
Hacksawing machines consist of a supported reciprocating frame and saw blade
mounted to a base for supporting the work piece. The machines are made as both hori-
zontal and vertical designs, horizontal machines being the most popular. The blade is
fed into the work piece with a feed mechanism and a ow of cutting uid is led to the
cutting area. Because of the limited possibilities for clamping the work piece, power
hacksawing is well suited for cutting of stock material, tubing, etc., but less suited for
cutting of more complicated parts. The surfaces produced with power hacksawing are
very rough and the problems mentioned above with cold work and deep deformation
are evident. Therefore, this cutting method should only be used for cutting of a work
piece froma larger part, the specimen to be cut later fromthe work piece by wet abra-
sive cutting.
Circular Sawing
Circular sawing is a process using a rotating, continuous cutting blade with teeth on its
periphery to cut most materials under a ow of cutting uid. A circular saw produces
better surfaces than power hacksawing, but the limitations regarding cutting of other
workpieces thanstockmaterial andtubes, etc., are the same.
Bandsawing
Bandsawing uses a long, endless band traveling over two or more wheels in one direc-
tion. The band, with only a portion exposed, produces a continuous and uniform cut-
ting action using a cutting uid to improve the cutting, cool the work piece, and in-
crease bandlife.
In bandsawing the cutting takes place as a continuous, single-direction cutting,
and this, combined with blade guiding and tensioning, gives the possibility of follow-
ing a free cutting path, making contour cutting possible. In this way a specimen can be
cut out from a work piece of odd form, a great advantage compared to other types of
sawing mentionedabove.
A number of saw blade types are available for bandsawing, but only two of them
are suited for cutting of metallographic/materialographic specimens. These types are
conventional sawing with a bandsawblade with teeth, used primarily for cut-off and
contour cutting of most materials, and saw-grinding with a blade with continuous/
segmentededge for the cutting of very hardmaterials andcomposites see below.
The quality of the cut is generally better than hacksawing, but still a relatively
strong deformation caused by cold work is developed.
16,21
At conventional properly
performed bandsawing, the heat developed will not create an altered microstructure
but this could happen if the cooling has not been efcient or the feeding pressure has
been too high. Care should be taken so that cold work and heat-affected zones are to-
tally removedduring the grinding steps of the preparationprocess.
Safety at Bandsawing
The dangerous area when bandsawing is the point of operation where the saw band
traverses to process the work piece. It is very important that the operator is careful to
keep his hands out of the immediate sawing area whenever the band is moving. The
work piece should always be guided into the band with some kind of distance piece so
that the hands will not be close to the band, even when the band has cut totally through
the workpiece.
Bandsaw Blades
It is important to select the correct saw band blade for the given work piece to be
cut.
23
Important factors are:
Type and hardness of the work piece material that determine the tooth form and
compositionof the band.
The size and variation in cross section of the work piece that determine the pitch of
the teethof the band.
Type of cut, is it straight, contoured or both? If cutting in small radii, the width of
the bandshouldbe limited.
Type andconditionof the machine tobe used.
Whether a cutting uidwill be used.
Different bandsaw blades with different width, thickness, and tooth geometries
are available for cutting of different materials, ranging fromrelatively soft carbon steel
bands for cutting of mild steel, cast iron, copper, and other relatively soft materials, to
bi-metal and tungsten carbide-tipped blades for hard, very hard, and tough materials
like work-hardening alloys, high temperature alloys, hastalloy, and titanium. Bandsaw
blades with a grit edge are available with a tungsten grit for cutting hardened tool steel,
titanium, nickel- and iron-based superalloys, glass ber optics, low density ceramics,
and composites. The more expensive diamond edge blades are used for very hard,
brittle materials, suchas minerals andceramics.
Figure 2.20 shows the terminology commonly used for sawbands. The cutting ac-
tion of the band depends on the tooth geometry. There are three main types of tooth
forms: precision, claw, and buttress, as shown in Fig. 2.21. The precision form nor-
mally has a 0 rake angle, but a positive rake angle is alsoavailable. It has a full-rounded
gullet with a smooth radius; the gullet is taking up the chip as long as the tooth is in
contact with the work piece. Bands with precision-form teeth are the most versatile,
have a smooth nish, and are recommended for cutting of most metallographic/
materialographic specimens. The clawformhas the same formas the precision except
the gullet is more shallowwithless chipcapacity but greater backing strengthanda 10
rake angle that requires less feedforce. The clawformis recommendedfor the toughest
materials that demand heavy feed and yield small chips. The buttress form also has a
more shallow gullet and neutral rake angle and is a stronger, less aggressive variant of
the clawformfor cutting of woodandplastics.
The band width should be as high as possible for the given cutting operation see
Fig. 2.20. The wider the band, the greater its beamstrength and the more accurate the
cut. For straight cuts the widest band that the machine can accommodate should be
used. Narrower bands shouldbe usedonly for contour cutting.
The band thickness is important for the strength of the band, especially if the band
widthis small.
The tooth set is the distance between the outer corners of oppositely set teeth, de-
termining the kerf width of the cut. The teeth are set by bending the single tooth to
one side of the band. At straight set the bending alternates all teeth left and right. Raker
set includes one unset tooth raker in each sequence of 3, 5, or 7 teeth. The raker set is
recommendedfor materialographic cutting of ferrous materials.
Fig. 2.20The terminology commonly used for bandsaw blades.
Fig. 2.21The three main types of bandsaw blades.
The band pitch, the number of teeth per inch of length see Fig. 2.21 is primarily
determined by the thickness of the work piece to be cut. A thin work piece requires
bands with a ner pitch more teeth per inch, thick stock a coarser pitch see Table
2.1. The work piece material and the surface nish required also must be considered
whenselecting the optimumpitch. It should, however, be assuredthat at least twoteeth
are incontact withthe workpiece at all times during sawing.
Denitions, tooth formand set, pitch sizes, etc., regarding bandsawblades are dis-
cussed in ASME Standard B94.51M, Specications for Band and Saw Blades Metal
Cutting.
Bandsawing Machines
Bandsawing machines are built as vertical machines and horizontal machines. The
vertical type
23
having a vertical band and a horizontal table on which the work piece is
moved into the band is the most versatile and typically used for cutting of
metallographic/materialographic specimens see Fig. 2.22. The table often can be
tilted to allow for cutting under an angle to the work piece, and the maximum work
height is in the range of 300400 mm 1216 in. Most machines have variable band
speed in the range from 0.228 m/ s 395500 fpm, but most cutting takes place at
speeds in the range of 0.65 m/ s 118985 fpm, the speed varying with the hardness/
ductility of the work piece material and the cross section to be cut see below. Most
metals are cut with speeds in the range of 0.42 m/ s 847394 fpm for a cross section
of 25 mm1 in reducing the speed to half or less at sections above 150 mm6 in. For
soft materials like copper the speedcangoupto5 m/ s 985 fpm.
Cutting Fluids
For cutting uids, semisynthetic or emulsion type uids are used because a relatively
high mechanical lubricity is needed to prevent the chips from bonding to the tooth
faces. A good cooling is also important to keep the teeth cool when they are in the cut,
and the viscosity may also be important depending on the application see Section
2.3.7.
Advice and Hints on Bandsawing
For a higher cutting rate, increase the blade velocity or use a band with a coarser
pitch. Ahigher feeding pressure alsowill give a higher cutting rate.
To increase the life of the blade, the blade velocity shouldbe reducedor a bandwith
a ner pitch should be used. Be careful that the feeding rate feeding pressure is
not toohigh.
To improve the nish of the cut, precision bands 0 rake angle should be used
preferably with a ne pitch. The band velocity may be increased and the feeding
rate feeding pressure may be reduced.
To improve accuracy of the cut, the band velocity may be increased and the feeding
rate may be reduced.
A bandsawis a relatively dangerous machine, and all precautions should be taken
to avoid accidents when the work piece is guided towards the moving band, see
above.
For Trouble Shooting, see Section13.6.2.
2.7.5 Wire Cutting
When sectioning very sensitive materials with relatively small dimensions, wet abra-
sive cutting might be toorough; therefore, other methods have beendeveloped.
Among these, electro-erosive, chemical, and mechanical principles have been
used, but only the mechanical sectioning, based on a wire with embedded diamond
grains, has gainedgroundandis commercially available.
Wire cutting uses a metal wire with diamond particles pressed into the metal, in
this way anchored so that they can remove material froma work piece when the wire is
drawnagainst the work piece under a certainforce. The wire, the lengthup to 1020 m
3060 ft, is rolled on two drums moving in two directions, the wire being rolled from
one drumto the other. This gives a strong wire no welding which can be highly tight-
Fig. 2.22General purpose contour bandsaw machines, Model 2013-V3 and Model 3613-1.
Model 2013-V3 is designed for contour sawing, band ling and band polishing; it cuts metal,
wood, plastics and other materials. It has a 660660 mm 2626 in table that tilts 45 right,
and 10 left and a 330 mm 13 in work height. The band speed can be varied through a two-
speed transmission from 1797 or 2921585 m/ min 55300 or 9605200 fpm. The band
width capacity is 1.527 mm 1/ 161 in and the motor capacity is 2.25 hp.
23
ened, securing a good precision of the cut. The force in the cut, creating the feed move-
ment, is achieved using a weight. The wire is 0.20.5 mm 0.0080.02 in thick and
moves with up to 2.5 m/ s 493 fpm. The process runs without cooling because the re-
moval rate is very low. A uid is used only for cleaning the wire, keeping the diamonds
free fromswarf.
Workpieces upto50 mm2 in canbe cut.
The advantages are a very low deformation of the cut surface and a low material
loss kerf loss. The disadvantage is the long cutting time.
3
Mounting
MOUNTING IS A PROCESS IN WHICH THE SPECIMEN, IN ONE WAY OR AN-
other, is encapsulated to facilitate and often improve the following preparation. The
mounting normally takes place after sectioning for mounting before sectioning, see
Section2.6 andseveral methods are available.
3.1 Purpose and Criteria
3.1.1 Purpose
Mounting is neededfor a number of reasons:
The specimenis small andis difcult tohandle.
The specimen has an awkward shape and mounting is necessary to secure the
preparationof the correct surface.
Edge retentionandatness of the specimenis important for a correct examination.
The specimen is brittle or has cracks or pores, and the mounting impregnation
will stabilize the surface. Also the specimen could be a powder material or in a
shape not t for preparation.
A standard specimen size is required when using semiautomatic or automatic
preparationequipment.
3.1.2 Criteria for a Good Mount
If mounting is done only for handling a small, awkwardly shaped specimen, and the
demands for the quality of the prepared surface are relatively low, a simple mounting,
such as clamping, can be used see Fig. 3.4. In most cases, however, a mounting in
plastic is performed see Fig. 1.9. This is to ensure a certain quality of the mount to
avoid problems when cleaning the specimen see Fig. 3.1. The problem shown in Fig.
3.1 is due to a gap between the specimen and the mounting material, letting uids
etchants or abrasives, or both, from the preparation leak onto the prepared surface
after drying of the specimen. In case of an etchant, the objective of the microscope
might be damaged. The gap develops because the shrinkage of the mounting material
is too high or with a clamped specimen, a gap exists between the specimen and the
clamp material. This gap also spoils the edge retention of the specimen which is one of
the commonadvantages at mounting.
Toobtaina goodmount the following criteria shouldbe fullled:
Nogapbetweenspecimenandmount material.
Rate of removal wear resistance of mounting material should correspond to that
of the specimenmaterial.
Noair bubbles inthe mounting material or along the edge of the specimen.
The mounting material shouldbe resistant tocommonetchants.
The mounting material shouldnot pickupabrasive grains during the preparation.
3.1.3 Surface FlatnessEdge Retention
To obtain a satisfactory examination in a light microscope the specimen surface has to
be relatively at. This is due to the depth of eld of the microscope, the distance along
54
the optical axis over which details of the specimen surface can be observed with ad-
equate sharpness. The depth of eld decreases with increasing magnication, at 100,
250, and 500 the distance is 20, 3, and 1 m, respectively. This means that if a speci-
men should be examined at 250 or higher, special care should be taken to obtain a
plane specimensurface. This canbe obtained by mounting as described belowfor edge
retention, but another important factor is the use of the correct preparation process
see Sections 6.6and6.7.
When examining surface layers, a very good edge retention is denitely needed,
even for lowmagnications. However, also in other cases, a at specimen surface with-
out edge rounding is wanted. Figure 3.2 shows a specimen with a a rounded edge due
to a gap between mounting material and specimen. In b there is contact between
mounting material andspecimen, whichprovides a goodedge retention.
To support the edge of the specimen, the mounting material must be in contact
with the specimen, and ideally, the surface of the mounting material should be in the
same level as the specimen no relief. To obtain this the mounting material should
have the lowest possible shrinkage, good adhesion, and a removal rate wear resis-
tance corresponding tothe specimenmaterial.
Plating the edges of the specimen, mostly with electroless nickel, is used also, but
withmodernpreparationmethods this relatively laborious process canbe avoided.
Attention: Although the edge retention to a high degree depends on a good support
of the edge, the correct preparation process is even more important, using the right
grinding/polishing surfaces see Chapters 6and7.
Shrinkage and Adhesion
All mounting materials typically have a higher shrinkage than the specimen material.
In case of hot mounting materials, using powder of polymers see Section 3.4, the
shrinkage is due to the thermal expansion of the polymer during heating and the con-
traction during cooling. This means that hot mounting resins that usually have a
higher thermal expansion than the specimen material will have a stronger contraction
than the specimen. Therefore, they will squeeze the specimen, making a good con-
tact. This means, however, that a gapwill developina hole or cavity inthe specimen.
Fig. 3.1Fluid leaking from a gap between mounting material and specimen onto the
prepared surface.
Chapter 3 Mounting 55
To ensure a good contact, hot compression mounting materials should always be
cooledunder pressure see Section3.3.
In cold castable mounting resins, the shrinkage takes place during the polymer-
ization of the components see Section 3.7 and a gap will develop if the shrinkage is
high. The shrinkage of cold mounting resins can be reduced by mixing a mineral pow-
der inthe resinIf the polymerizationprocess is accelerated by heating, thenthe shrink-
age is usually increased. High adhesion between the resin and the specimen material
ensures the contact, but only epoxy has a strong adhesion.
Material Removal RateWear Resistance
During the preparation process, the specimen material and the mounting material are
removed fromthe surface, expressed in the material removal rate see Sections 6.2 and
7.2. Ideally the removal rate should be equal for both materials. In most cases, how-
Fig. 3.2Edge retention: a In case of a gap between mounting material and specimen, a
rounding of the specimen edge is developed; b with contact between specimen and
mounting material, edge retention is obtained.
ever, the mounting material resin, being relatively soft, has a much higher removal
rate thanthe specimen. This couldbe critical because a positive relief is developedFig.
3.3a, and the edge of the specimen is not protected. In some cases, if the specimen
material has a higher removal rate than the resin, a negative relief develops, with the
specimenmaterial being ina lower level thanthe resinFig. 3.3b.
The removal rate of the resin, as it pertains to wear resistance, depends to a high
degree on the hardness of the resin Tests have shown that when grinding on a P240 SiC
grinding paper, the removal abrasion rate of anacrylic or phenolic mounting material
is 10 to 15 times as highas for soft metals like copper and brass. At roughpolishing ona
cloth with 46 m diamond, however, the removal polishing rate is only 23 times
higher.
7
It seems that not only the hardness of the mounting material plays a role, but
also the machinability, meaning that at roughpolishing the mounting material to a cer-
taindegree will be removedwiththe same speedas the sample material.
Wear resistance canbe regulatedby adding hardllers to the resin, andthis type of
resinshouldbe usedif a goodedge retentionis wantedsee Sections 3.4and3.7.
See also Sections 3.6.1 and 3.13.1 with indications of the material removal rate for
the single mounting material.
If the wear resistance of a resin is very high, as known from hot mounting epoxy
with ller, it will inuence the preparation process and probably a negative relief will
develop, as mentioned above. The resin will behave like a hard material and if SiC
grinding papers are used, these will wear out the same way as by hard materials. This
also means that if a standard preparation time for a given specimen, mounted in nor-
mal phenolic resin, is 2 to 3 min, it might be doubled if the specimen is mounted in the
epoxy resinwithller.
3.2 Mounting Methods
3.2.1 Clamping
By clamping, the specimen is xed mechanically without using a mounting material.
For automatic preparation, the specimens can be clamped in a holder see Fig. 3.4a
andFig. 3.5a for at specimens andFig. 3.5b for circular specimens.
InFig. 3.4b a clamp, normally usedfor handpreparation, is shown. It has two at
pieces of soft steel or stainless steel which are kept together with two screws and the
Fig. 3.3Relief at mounting: a In case of a mounting material that is too soft, a positive relief
is developed, and the edge of the specimen is rounded. b With a mounting material that is
too hard, a negative relief is developed.
specimen often pieces of sheet metal placed between the two pieces that should have
rounded outer edges to avoid excessive wear of the polishing cloth. If possible, the
clampmaterial andthe specimenmaterial shouldbe compatible.
Common for all clamping: it is difcult to avoid rounding, and often, when clamp-
ing several sheets, gaps will retain abrasives or uids, creating problems during the
examination.
3.2.2 Hot Compression Mounting
Hot compressionmounting or hot mounting indicates that the specimenis placedwith
an amount of resin in a cylinder in a mounting press and heated under pressure for a
speciedperiodof time. The resinpolymerizes aroundthe specimen, andafter cooling,
a mount canbe ejectedfromthe press see Section3.3.
3.2.3 Cold Castable Mounting
Cold mounting typically takes place at room temperature but often the temperature
during the curing will reach30130C82265F peaktemperature.
During cold mounting, the specimen is normally placed in a mold mounting cup
anda mixture of a resinanda hardener is pouredinto the mold. After 5 min to 20 h the
plastic will cure, anda mount canbe takenfromthe moldsee Section3.7.
3.3 Hot Compression Mounting
Hot compressionmounting is based onthe fact that certainplastics, suchas powder, in
the following called resins, can be formed to a given shape, usually cylindrical, when
heated and cooled under pressure in a metallographic/materialographic mounting
press.
Fig. 3.4Clamping of specimens. a Specimen holder for clamping of at specimens for
automatic preparation; b six pieces of sheet metal clamped between two at pieces of steel
for manual preparation.
3.3.1 Advantages of Hot Compression Mounting
The quality andwear resistance hardness is generally superior tocoldmounting.
Fast methodfor making one single mount.
Achoice of diameters from25 mm 1 in 50 mm 2 in.
The diameter of the mount is very exact.
3.3.2 Disadvantages of Hot Compression Mounting
Highinitial cost for mounting press.
Fragile andbrittle specimens canbe damagedby the pressure inthe cylinder that is
from2030 MPa 2.9004.350 psi.
Heat sensitive materials canbe damaged. The temperature is normally 120200C
250400F inthe mounting cylinder.
If mounting large series of specimens, hot mounting is slowbecause usually only a
limitednumber of mounting presses will be available.
3.3.3 MSDS Material Safety Data Sheets
Hot mounting resins are generally not hazardous, but the MSDS should always be ob-
tained from the supplier and studied before use. Vapors from the heated material
might be irritating; especially vapors fromphenolics that might contain formaldehyde
should be avoided. Prolonged skin contact with phenolic and epoxy materials may irri-
tate the skin and cause a skin rash dermatitis, and, of course, all skin contact to very
hot mounts shouldbe avoided.
Fig. 3.5Clamping in specimen holders without mounting: a specimens of a at shape; b
specimens of cylindrical shape.
3.4 Hot Mounting Resins
The resins for metallographic/materialographic mounting are used as powders and
canbe classiedintotwogroups: thermoplastic andthermosetting.
Athermoplastic resin is a polymeric material that can be formed on application of
heat andpressure andis solidiedby cooling.
A thermosetting resin is a polymeric material that can be formed and cured by the
applicationof heat andpressure but cannot be reformedonfurther heat andpressure.
For selection of the correct hot mounting resin for a given purpose, see Section
3.6.1.
3.4.1 Thermoplastic Resins
Thermoplastic materials undergo no permanent change on heating. They ow and
may be molded into a shape which they retain on cooling. The material will owagain
when reheated and can be remolded. Thermoplastic polymers contain linear mol-
ecules that are not cross linked; these are shownschematically inFig. 3.6.
Acrylics
A number of well-known plastics are thermoplastics. For metallography/material-
ography, acrylics polymethylmethacrylate PMMA are used. Acrylics are known as
sheets used instead of glass for many purposes. This transparency often is an advan-
tage for mounting. Acrylics have tobe heatedto150180C300360F toowmelt
and cooled to obtain its shape. The pressure is in the range of 30 MPa 4350 psi like
most other hot mounting resins. The pressure can be omitted or kept very lowduring a
preheating period, and this can be of advantage when mounting porous specimens
when the resin penetrates into the pores. Cooling under pressure should be performed
down to 40C 104F, preferably room temperature, before the mount is removed
from the press. The total time for heating and cooling is 1424 min depending upon
the diameter of the mount.
Acrylics are resistant to water, alcohol when properly cured, solutions of most
salts, diluted alkalies, hydrochloric acid, and sulfuric acid, but soluble in nitric and
acetic acids, some ketones, and esters. Acrylics are notch-sensitive and cracks may de-
velopif stress is toohighsee Section13.6.3.
The shrinkage is relatively high, hardness is medium, compared to other mount-
ing resins, andwear resistance is lowsee Section3.1.3.
Acrylics with Fillers
Acrylics can be made electrically conductive by adding a metal powder, usually Fe or
Cu, and the mount loses its transparency. This is done to create a conductive mount for
electrolytic polishing. This type of conductive mounting material cannot be recom-
mended for use with SEM because the metal powder Fe or Cu can contaminate the
Fig. 3.6Schematic drawing of thermoplastic polymer, not cross-linked.
specimen surface leading to false results. For SEM, a resin with graphite should be
usedsee Section3.4.2.
3.4.2 Thermosetting Resins
Thermosetting resins for hot mounting are capable of a high degree of cross-linking
shown schematically in Fig. 3.7. They are generally molded in a practically polymer-
ized state so that they can ow by the application of heat and pressure. During the
molding process further polymerization occurs, and the plastic becomes highly cross-
linked and can no longer ow or be changed on further application of heat and pres-
sure.
The following three types of thermosetting resins are available for hot mounting:
phenolics bakelite, diallyl phthalate, andepoxy.
Phenolics
The phenolic resin is made fromphenol and formaldehyde and a ller. Formaldehyde,
being a critical solvent, should only be present in very low amounts below 1 % in the
nished resin The ller is important to obtain the right properties of the mount. Gener-
ally wood our is used as a ller giving brown mounts. Added colors provide phenolic
resins with a number of colors. The temperature for a correct polymerization is
150180C 300360F, and although the thermosetting resin need not be cooled for
curing, the mount should be cooled under pressure to approximately 60C 140F to
reduce shrinkage. The pressure in the cylinder should be approximately 30 MPa
4350 psi and the total time for heating and cooling is in the range of 813 min. Phe-
nolics have a number of drawbacks, but being the most inexpensive of the mounting
resins, they are usedfor routine examinations.
Phenolics are resistant to weak acids, organic solvents, hydrocarbons, detergents,
and cleaning uids, but attacked by strong alkalis, oxidizing acids, and hot boiling
etchants.
Phenolics have good mechanical properties. The shrinkage is relatively high, the
hardness is low, andthe wear resistance is lowsee Section3.1.3.
Phenolics with Conductive Filler
Graphite can be added as a ller, making the resin electrically conductive. This resin is
usedfor mounts tobe examinedinanSEM.
Phenolics in Tablet Form
Tablets or premounts are made by pressing phenolic powder to form a mount, with
dimensions slightly smaller than the diameter wanted. It is used for mounting of solid
specimens, which are not inuenced by the pressure, when the tablet is pressed on the
specimen. The advantage is that working witha powder resinis avoided.
Fig. 3.7Schematic drawing of thermosetting polymer with a high degree of cross-linking.
Diallyl Phthalate
The diallyl phthalate DAP resinis a polyester witha ller. The ller strongly inuences
the strength of the resin, and for materialographic mounting, mineral and glass ber
short are used with glass ber-lled resin, the most all-round material. The tempera-
ture for a correct polymerization is 150180C 300360F and the pressure in the
cylinder 2530 MPa 36504350 psi. The total time for heating and cooling is
813 min.
Compared to phenolics, DAP has a number of advantages but it is more expensive
thanphenolics.
DAP is resistant to most chemicals and the mechanical properties are excellent.
The shrinkage is much lower than in phenolics, and the ller causes a relatively high
hardness anda highwear resistance, securing a goodedge retentionsee Section3.1.3.
Epoxy
Epoxy resin for hot mounting is made as a powder with a ller. Epoxy has a number of
properties very suitable for mounting. The ller is a mineral like calcium carbonate
ground to a very ne powder which to a high degree reduces the removal rate and con-
sequently improves the wear resistance of the resin see Section 3.1.3. The tempera-
ture for a correct polymerization is 150180C 300360F, and the pressure in the
cylinder is approximately 10 MPa 1450 psi, considerably less than for other resins.
The total time for heating andcooling is 915 min.
The resistance to all chemicals, even to hot etchants, is very high. The mechanical
properties are excellent and the strong adhesion to the specimen and an extremely low
shrinkage make epoxy resin the best resin for retention of edges. The strong adhesion
cancause problems withadhesionto rams andcylinder walls inthe mounting cylinder.
These parts needtobe treatedwitha release agent see Section3.6.
3.5 Mounting Presses
Heating, pressure, and cooling are needed when making a mount froma hot mounting
resin
The temperature should be in the range of 100200C 210400F and cooling
should take place fromthe maximumtemperature to approximately 60C 140F in a
reasonable time. Cooling is necessary for thermoplastics, but even thermosetting res-
ins should be cooled to around 60C 140F under pressure to secure the lowest pos-
sible shrinkage. The force between the lower and upper ramduring the process should
be in the range of 150 kN22511.235 lbf making it possible to establish a pressure
of 1030 MPa 14504350 psi inthe mounting cylinder at diameters from2550 mm
12 in.
3.5.1 The Heating/Cooling Unit
The heart of the press is the heating/cooling unit consisting of mounting cylinder
mold, lower ram, upper ram, top closure, heating coil, controlled by a thermostat,
and cooling coil water cooling see a schematic drawing in Fig. 3.8. The cylinder can
be typically supplied in diameters of 25 mm 1 in, 30 mm 1.18 in, 31.75 mm
1.25 in, 38.1 mm1.5 in, 40 mm1.57 in, and50 mm1.97 in.
The lower ram is moved up and down in the mounting cylinder by hydraulics or
by air. Before the sample is placed in the cylinder, the lower ramis normally placed in
the top to secure the right position of the sample. After moving down the lower ram, an
amount of resin is put into the cylinder. This amount should cover the sample so that
the upper ramshould not be damaged when the resin is put under pressure, and there-
fore has a volume reduction. The upper ramwithtopclosure is placedandsecured, and
the lower ram is moved upwards, building up pressure. Heating is switched on for a
few minutes, followed by cooling, usually water cooling as shown in Fig. 3.8, but also
air cooling with cooling blocks is used. After about 924 min, depending on the resin
and the diameter, the mount can be pushed out of the top after removing the upper
ram.
Considering that both pressure and heating should be continuously adjusted dur-
ing the process, anautomatizationis a great advantage for the operator see below.
The heating/cooling unit is typically exchangeable sothat one press canbe usedfor
a number of different mount diameters, or the cylinder can be exchanged in the
heating/cooling unit.
If the cylinder has enough space, two mounts can be made at the same time, using
anintermediate rampiston separating the twomounts.
On modern units, the heating and water-cooling coils are totally integrated with
the mounting cylinder, Fig. 3.8. This secures the best heat transfer, saving energy, water,
andtime.
3.5.2 The Hydraulic Press
Hydraulic presses are the most frequently used way of obtaining the relatively high
pressure needed. The rst presses were car jacks operating inside a frame, the jack put-
ting a pressure on the lower ram and the frame holding the cylinder and upper ram in
place. Heating was done with a jacket containing a heating element with a thermostat
placed around the cylinder and exchanged with a cooling block air cooling or a jacket
withwater.
From this simple setup, the hand-operated presses were developed, the pressure
established through a hand pump, and the heating/cooling unit as part of the press see
Fig. 3.8Schematic drawing of heating/cooling unit. The heating and cooling coils can be seen
around the mounting cylinder with upper and lower ram.
Fig. 3.9 which shows a hand-operated mounting press for mold sizes from2538 mm
11.5 in.
Heating is switched on and off manually and the temperature is controlled by a
built-in thermostat. Water cooling is controlled by a water tap, and the operator has to
be careful that the pressure in the mounting cylinder is maintained during the process.
To avoid the requirement for an operator to be present during the whole process, auto-
matic presses are available.
The simplest automatic press uses a motorized hydraulic pump which automati-
cally keeps the pressure controlled by an adjustable pressostat. The operator switches
the heating andcooling onandoff.
Withmore advancedpresses, all parameters, pressure, temperature, cooling cool-
ing rate, and time, are microprocessor-controlled. In some cases, a number of meth-
ods for different mounting materials and mount sizes can be programmed and stored.
Figure 3.10 shows an electrohydraulic, automatic, programmable press with two
heating/cooling units withmolddiameters from2550 mm12 in.
Fig. 3.9Hand-operated mounting press for mold sizes from 2538 mm 11.5 in. The
standard model is with air cooling, and water cooling is optional.
19
3.5.3 The Air-operated Press
Compressed air has been used for establishing the pressure during hot mounting. An
air-operated press could be made at a lower cost than a hydraulic press. The drawback
is the compressibility of the air whichmakes the ejectionof the nishedmount difcult
tocontrol. The air presses seemtohave vanishedfromthe market.
3.6 Advice and Hints on Hot Compression Mounting
Check that the specimen to be mounted is not too brittle, has brittle layers spray
coatings might change the porosity under pressure, or is not suited for compres-
sionmounting or inother ways. If indoubt, use coldmounting.
Checkthat the specimenmaterial canbe treatedat minimum150C300F.
Take care that the specimenis cleananddry, without grease or other residues.
Keepthe mounting cylinder andrams upper/lower clean.
Moldrelease agent: Treat the upper andlower ramwitha thinlayer of agent. This is
especially important for resins, like epoxy, sticking tometal surfaces.
Process time depends upon the amount of resin; therefore, keep the amount low.
On the other hand, the distance from the specimen to the cylinder wall should be
not less than 3 mm 0.12 in, and the resin should effectively cover the top of the
specimensothat the upper ramwill not touchthe specimen.
Save expensive resin: Only use the expensive resin in a thin layer around the speci-
menandll upwitha less expensive back-up resin
Pressure: At phenolics and other thermosetting resins, apply the pressure at the
same time as the heating. At acrylics and other thermoplastic resins, the pressure
may be appliedafter a preheating periodsee below. Never use excessive pressure.
Phenolic mounts: Cool the mount under pressure down to approximately 60C
140F. Do not take out a very hot mount and cool it directly in water; the mount-
ing material might crackor a gapalong the specimenwill develop, or both.
Specimens withlayers requiring a superior edge retention: Use anepoxy resin
Porous specimens: Use a thermoplastic resin acrylics; if possible preheat the
resinor use coldmounting.
Small specimens: These can be supported during the process by using a clip see
below.
Electrolytic polishing: Use a conductive resin but apply a thin layer of nonconduc-
Fig. 3.10Electrohydraulic, automatic, programmable press with two heating/cooling units
with mold diameters from 2550 mm 12 in.
20
tive resinaroundthe specimentoavoidanelectrolytic reactioninthe resin
For Trouble Shooting see Sections 13.5/6.
3.6.1 Selection of Resins for Hot Compression Mounting
Purpose
Specic
Property
Mounting
Resin
Temp.,
CF
Force
KNlbf
Heat./
Cool.
Time
min
Price
Range
Glass clear mounts
Porous specimens
low pressure
Nonconductive
surface for
electropolishing
Thermoplastic
Transparent
Low initial
pressure,
slow cure
Medium
shrinkage
Low hardness
High removal rate
at grinding,
medium at
polishing
Low chemical
resistance
Tendency to
defects
Acrylics,
transparent
without
llers
150180
300360
1550
3375
11250
6/ 8 at
25 mm
1 in
to 12/ 12
at 50
mm
2 in
Medium
Routine
examination
Back-up resin
Color marking
Serial mounting
of uncomplicated
shapes Resin in
tablet form
Thermosetting
Fast cycle
Medium shrinkage
Medium hardness
High removal rate
at grinding,
medium at
polishing
Medium
chemical
resistance
Phenolics
Bakelite
as powder
with wood
our ller,
with or
without
color
Phenolics
Bakelite
in tablet
form
150180
300360
1550
3375
11 250
6/ 3 at
25 mm
1 in
to 11/ 4
at 50
mm 2
in
Low
Low
Good edge retention
Thermal spray
coatings
High planeness
Chemical resistance
Thermosetting
Low shrinkage
High hardness
Low removal rate
Medium/high
chemical
resistance
Diallyl
phthatalate
with glass
ber
or mineral
ller
150180
300360
1550
3375
11 250
5/ 3 at
25 mm
1 in
to 9/ 4 at
50 mm
2 in
High
Purpose
Specic
Property
Mounting
Resin
Temp.,
CF
Force
KNlbf
Heat./
Cool.
Time
min
Price
Range
Very good edge
retention
Thermal spray
coatings,
plated layers
Very high planeness
Thermosetting
Very low
shrinkage
Good adhesion
High hardness
Very low
removal rate
Medium/high
chemical
resistance
Epoxy with
mineral
ller
150180
300360
550
1125
11 250
6/ 3 at
25 mm
1 in
to 11/ 4
at
50 mm
2 in
Medium
Electroytic
polishing,
to be used with a
nonconductive
resin as surface
against electrolyte
Examination in
SEM
Thermoplastics or
thermosetting
Electrically
conductive
Low shrinkage
Acrylics or
phenolics
with metal
or carbon
ller
Phenolics
with
carbon
ller
150180
300360
1550
3375
11 250
6/ 3 at
25 mm
1 in
to 11/ 4
at 50
mm
2 in
High
High
3.7 Cold Castable Mounting
Cold mounting, or castable mounting, is used parallel to hot compression mounting.
Normally cold mounting is not cold room temperature; often temperatures will
reach30150C82265F.
Inmost cases withcoldmounting, two components, either two liquids or a powder
and liquid, are mixed. The components, resin and hardener, are measured either by
weight or by volume with a relatively high precision. In the case of very small quanti-
ties, measurement by weight is recommended. The mixing of the components should
be very careful to secure a total distributionof the hardener. The time after mixing until
the curing starts, the pot life varies for the different resins, but as a rule the mixed resin
should be used immediately, securing the lowest possible viscosity of the mixture. The
mixture is preferably done indisposable paper cups whichcanbe discardedafter use.
Normally the clean, grease-free specimen is placed in a mounting mold see be-
low, and the mixture is poured carefully into the mold, avoiding entrapment of air,
when the mold is lled. The lowviscosity ensures that the resin ows into all irregulari-
ties of the specimen and air bubbles, if any, will be able to move to the top of the mount.
To improve the penetration of the resin into the specimen, vacuum impregnation can
be used see Section 3.10. A pressure chamber that creates a pressure with a small
compressor, 0.20.28 MPa 30 to 40 psi, will help to avoid bubbles and improve the
inltrationof the resinintothe specimen.
During the curing, the temperature increases to the peak temperature, depending
on the type of resin Up to 130C 265F is measured. The temperature can be kept
down if good heat conduction is established. The different resins have different peak
temperatures see Section3.13.1.
3.7.1 Advantages of Cold Castable Mounting
Lowinitial cost.
Brittle andfragile specimens are not damaged.
Specimens withcracks andpores, or both, canbe impregnated.
Large series canbe made simultaneously, using inexpensive mounting molds.
3.7.2 Disadvantages of Cold Castable Mounting
Some of the resins have a relatively highshrinkage.
Some of the resins are relatively soft witha lowwear resistance highremoval rate.
The shape diameter is not very exact.
Riskof bubbles andcracks aroundthe specimen.
Hazardous vapors andriskif skinis incontact withchemicals.
3.7.3 MSDS Material Safety Data Sheets
Some cold mounting resins can be hazardous and special care should be taken during
use. MSDSshould be obtained fromthe supplier and studied carefully. Special precau-
tions tobe takenfor the different resins are mentionedbelow.
3.8 Cold Mounting Resins
Similar to hot mounting resins, cold mounting materials can be both thermoplastic
andthermosetting see Section3.4.
3.8.1 Acrylics
Acrylics are thermoplastic and are supplied as a resin, a powder polyamized methyl
methacrylate MMA with an initiator, and a uid, the hardener MMA monomer,
witha promoter.
The size of the single particles beads of the resin has a specic importance. They
vary from 550 m. Figure 3.11 shows the beads and the grains of a ller. With small
beads, the ow of the mixed resin is more viscous, and better able to penetrate into
microcracks and pores. The peak temperature is 90110C 194240F and curing
time 515 minsee alsoSection3.13.1.
The acrylics without ller are translucent and will cure in down to 510 min
whichmakes it the fastest curing resinIf the systemis expandedwitha ller, the shrink-
age canbe reducedconsiderably see below.
Acrylics being thermoplastic have a tendency to melt during grinding, clogging up
the cut-off wheel andgrinding paper if not efciently cooled.
Acrylic cold mounting materials are not as chemical resistant as the hot mounting
materials see Section3.4.1.
The shrinkage is relatively high and this material should not be used if a very good
edge retention is wanted. The wear resistance is relatively low but both this and the
shrinkage canbe modiedwithllers see below.
Attention: Fumes from methyl methacrylates are considered hazardous and skin
contact shouldbe avoidedsoworkshouldbe done withgloves andunder a fume hood.
Acrylics with Fillers
Withhot mounting materials, the llers usually are establishedduring the manufactur-
ing process, the ller being integrated into the polymer. With acrylics used for cold
mounting, llers like ne ground calciumcarbonate are mixed into the powder and the
grains of the ller will be integratedinthe nishedmount as showninFig. 3.11. Acryl-
ics withllers are opaque.
Combinations of acrylics MMA with styrene see below have been developed
having two liquid components and a powder component consisting mainly of ller ma-
terial. This resinhas a very lowshrinkage andgoodedge retention.
Attention: Grains from the ller can be released from the surface during prepara-
tionandcause scratches inthe nishedspecimen.
3.8.2 Polyesters
Polyester is a thermosetting resin that is supplied as two liquids: an unsaturated poly-
ester resin and styrene acting as an accelerator with peroxide as the initiator. A polyes-
ter mount is transparent.
The amount of accelerator is very small compared to the amount of resin, making
the measurement of the two components relatively difcult, when small amounts
should be used. The peak temperature is 50110C 122240F and curing time is
from45 min to 68 h see alsoSection3.13.1.
The shrinkage is high, and polyester should only be used for mounting of speci-
mens withno needfor edge retention. The price is relatively low, however, andthe resin
is oftenusedfor routine mounts.
Attention: Styrene is considered a dangerous material and all work with measure-
ment and mixing should take place under a fume hood using gloves. Polyester has a
limited shelf life 6 to 12 months; therefore, the container should be marked with the
date of receipt tosecure that the oldest material is usedrst.
3.8.3 Epoxies
Epoxy is a thermosetting resin supplied as two liquids, a resin and a hardener. Epoxy
is the cold mounting resin with the lowest shrinkage and the best grinding and polish-
Fig. 3.11Acrylic-mounting material with ller. The small gray particles between the beads of
the polymer are the ller.
ing properties. Epoxy adheres strongly to the specimen, and if the curing time is rea-
sonably long, more than 68 h, the shrinkage is extremely low. If curing time is short-
ened, either by adding accelerator to the hardener 3045 min or by introduction of
heat 24 h, the shrinkage will be higher. By introduction of heat, the negative effect
can be reduced by letting the epoxy cure in 1 h after mixing at room temperature and
thencomplete the curing at 6070C140158F.
Epoxies are suppliedwitha very lowviscosity anda highboiling point, securing an
efcient impregnationof porous specimens see below.
Epoxies are transparent and cure through an exothermic reaction. The peak tem-
perature varies with the curing time. Curing for periods from 6 to 20 h gives a peak
temperature 4060C 104140F, while curing for 45 min results in peak tempera-
tures from 85100C 185220F. The peak temperature can be kept low by placing
the mold in a fridge. To avoid very high temperatures at mounts larger than the normal
size, cooling with air using a fan is recommended. Epoxies for cold mounting are nor-
mally not supplied with llers for metallographic/materialographic purposes, but ll-
ers canbe mixedinby the user see Section3.11.2.
The two parts, resin and hardener, should be measured in a precise manner be-
cause evena small variationcancause problems after curing see Section3.13.
The good adhesion properties of epoxy can result in problems with removal of the
nished mount from the mounting mold. The mold should be made of a plastic mate-
rial withlowadhesionandcertainexibility, like POMsee Section3.9.
Epoxies are not attacked by weak acids, weak alcohols, and organic solvents.
Strong acids and strong alcohols give a slight attack. Resistance to heat: 90250C
200500F.
Epoxy has good mechanical properties and it is the strongest, most durable of the
cold mounting resins. The shrinkage, as mentioned previously, is very lowif the curing
process is not shortened down. The hardness is relatively high and the wear resistance
is relatively highsee Section3.1.3.
Attention: Epoxies can cause allergies and all work should be done with correct
gloves under a fume hood.
3.9 Accessories for Cold Castable Mounting
In most cases it is important to have a relatively exact shape of the nished mount and
therefore a mounting mold cup is normally used. Clips are other accessories that sup-
port the specimenduring the curing.
3.9.1 Mounting Molds
In most cases these are cylindrical molds, made of a exible plastic like POMor of sili-
cone rubber see Fig. 3.12. The specimen is placed on the bottom of the mold and the
liquid mounting resin is poured into the mold. Some molds have a removable bottom
to allow the mount to be pushed out after curing. Molds made of silicone rubber are
normally in one piece, the high exibility of the silicone rubber allowing the mount to
be removed from the mold. To secure the removal of the mount, the mold can be
smeared with a silicone compound before the resin epoxy is introduced. Reusable
molds of a square or rectangular shape are alsoavailable.
Disposable ring forms often made of phenolics remain as an integrated part of the
mount after curing. The ring is placed on an adhesive lmso that the resin will not leak
during the curing. The specimen is placed inside the ring and, after curing, the ring
withresinandspecimenis takenfor preparation.
Another type of disposable mounting moldis analuminumcupusedfor packaging
of foods, etc. This is especially useful for large specimens of oddshapes.
3.9.2 Clips
If specimens are small andat, it helps tosupport the specimenduring the curing. Plas-
tic and metal clips that squeeze the specimen are available, being an integrated part of
the mount see Fig. 3.12. The clips canbe usedfor bothhot andcoldmounting.
3.10 Vacuum Impregnation
Specimens like sintered materials and ceramics having pores, cracks, etc., are difcult
to prepare without an impregnation inltration of the surface. If not impregnated the
pores will increase in size and cause pullouts, resulting in a microstructure that is not
showing the correct conditions of the material. Also, electronic parts or other parts of a
complicated structure that should be kept in place during the preparation may be en-
capsulatedusing vacuumimpregnation.
Impregnation in depth can only take place in a material with open pores. In the
case of closed pores, only the pores on the surface will be inltrated. Normally the im-
pregnationtakes place after cutting, but tocertain, very brittle materials, impregnation
should be done before cutting. In the case of closed or very narrow pores, the impreg-
nation should take place both after cutting and after plain grinding or even ne grind-
ing.
Impregnation is done in vacuum 80120 mbar using an epoxy resin with a low
viscosity anda boiling point highenoughtoavoidboiling inthe vacuumchamber.
The impregnationtakes place ina vacuumchamber whichcanbe a normal labora-
Fig. 3.12Mounting molds consisting of two parts, a bottom and a cylinder. The specimens are
supported by clips.
tory bell jar or an apparatus made for the purpose see Fig. 3.13. The specimen, care-
fully cleaned and degreased, is placed in a mold in the vacuumchamber and a vacuum
is established for an appropriate time from a couple of minutes for not very porous
specimens up to half an hour for very porous specimens. The impregnation is done by
sucking the mixed epoxy into the mold through a tube until the specimen is covered.
For best results, only a small amount of resin is taken into the mold, just covering the
area of interest and then slowly returning the chamber to atmospheric pressure. The
back pressure will further the penetration of the resin into the specimen. Repeat the
evacuationof the chamber and let inepoxy to completely cover the specimen. Nowthe
mold canbe removed for curing, or curing cantake place inthe vacuumchamber with-
out vacuum.
A simpler method, which can be used for materials with less pores, is to place the
specimen in a mold with epoxy and immediately after pouring in the epoxy, the mold is
placedinthe vacuumchamber andvacuumis established. To obtainthe best result, the
rst methodshouldbe preferred.
Coldmounting canalsobe done under a lowpressure see Section3.7.
3.10.1 Dyes
Dyes can be used in connection with vacuum impregnation of porous materials, the
dye being mixed into a lowviscous cold mounting epoxy resin By using a dye it is pos-
sible to contrast the voids into which the resin has penetrated against the surrounding
structure. The contrast is created through uorescence. Figure 3.14a shows a micro-
structure in bright eld where the pores cannot be identied. In Fig. 3.14b, the same
structure in uorescent light is shown and the pores lled with epoxy can be clearly
identied. To obtain the uorescence, a so-called short-pass lter in the microscope is
neededto excite the areas withdye, anda long pass lter is neededto see the uorescent
light see Section15.7.5. Dyes are commercially available.
3.11 Special Mounting Techniques
For some materials special mounting techniques are necessary, i.e., examination of
very thinlayers, powders, wires, etc.
Fig. 3.13Apparatus for impregnation; the mounting molds are placed in a vacuum chamber
and the epoxy is sucked into the chamber through a tube.
3.11.1 Taper Sectioning
This technique allows the examination of very thin layers and was highly developed by
L. E. Samuels in his work with surface deformation at metallographic/material-
ographic preparationsee Section6.3.
7
TABLE 3.1Taper Sectioning: Enlargement Factor, f, with the Corresponding Taper Angle, .
f f
100:1 0 30 10:1 540
50:1 1 20 5:1 1130
25:1 2 20 3:1 1930
20:1 2 50 2:1 30
15:1 3 50 1.5:1 4150
1:1 90
Fig. 3.14Use of impregnation with epoxy and dye. a Microstructure in bright eld; b and
the same structure in uorescent light revealing the pores lled with epoxy.
The specimen is placed under an angle to the plane of examination, in this way
enlarging the width of the layer, when examined in an optical microscope see Fig.
3.15.
If measured as a normal cross sectioninanoptical microscope, the lower limit of a
layer thickness is approximately 2 m because below this the measurement uncer-
tainty is too big, the limit of the optical microscope being 0.5 m. Very thin layers can
be examined or measured using taper sectioning because, depending on the taper
angle, an enlargement of 1.5 to 100 can be obtained. Table 3.1 shows the enlarge-
ment factor, f, andthe corresponding taper angle, .
If only the layer or the diffusion zone, or both, should be analyzed without mea-
surement of layer thickness, a suitable angle can be established with a spacer, the angle
not being exact.
In case of measurement of the layer thickness, the taper angle should be known
and exact, or the dimension of the specimen should be known. The angle can be estab-
lished with a wedge. If the angle is known, the layer thickness A=B sin , as shown in
Fig. 3.15.
If the dimensions XandYare known, A=X B/ Y, as showninFig. 3.16.
3.11.2 Edge Protection
When examining layers, it is absolutely necessary to have a good edge retention. The
edge retention depends very much on the type of preparation performed; it can to a
very high degree be obtained by using the modern grinding and polishing methods and
automatic polishing see Section6.7.
In some cases, especially if preparation has to take place with SiC grinding paper,
some precautions canbe takentopreserve the edge.
Section 3.1.3 describes the use of the correct mounting resin to protect the edge
andoftenthis will be sufcient.
Fig. 3.15Taper section with taper angle, . The thin layer with thickness A can be analyzed
and measured, B.
Fig. 3.16Taper section with known dimensions X and Y.
If further edge protectionis neededthere a number of methods available.
Plating
During plating a thin layer of metal is deposited on the surface to be analyzed. The idea
is that the edge rounding takes place on the plated layer, leaving the original layer
plane.
Plating can be done electrolytically, placing the specimen as cathode in a bath con-
taining a Cu, Ni, or Fe salt. Electrolytic plating is laborious and the result is not often
satisfactory for metallographic/materialographic examination.
Electroless plating gives better results and is easier to perform. Electroless nickel
is the most commonly used metal for metallographic/materialographic specimens.
Most metals can be plated. Only bismuth, cadmium, tin, lead, and zinc cannot be
plated.
9
Other materials such as plastics, wood, glass, carbide, silicon, and porcelain can
be plated.
Anexample of a formula for electroless nickel:
45 g nickel chloride
11 g sodiumhypophosphite
100 g sodiumcitrate
50 g ammonia chloride
1000 mLdistilledwater
pH8.59
Use the mixture at 90100C 194212F. The plating rate will be in the range of
0.015 mm/ h.
Instead of mixing the solutions yourself, different solutions for electroless plating
are commercially available.
Fillers
Many mounting resins are supplied with integrated llers, in this way improving the
edge protection see Sections 3.4 and 3.8. Fillers can be mounted together with the
specimen, placed in the surface of the mount close to the edge to be protected, and
preferably adjustedtocorrespondtothe hardness of the specimen.
The preferred ller is alumina used together with epoxy cold mounting resin to
avoid shrinkage and increase hardness. The alumina should be made preferably as hol-
low nodules to secure the stability of the alumina grain in the resin If grains fall out
during the nal steps of the preparation this might create scratches in the specimen
surface.
Fillers are commercially available.
Back-up Materials
A relatively simple way of securing the edge is to mount a piece of material similar to
the specimenmaterial close tothe edge of the specimen.
A metal foil can be wrapped around a cylindrical specimen, which, in the case of
hot mounting, is pressed close to the specimen because of the high pressure in the
mounting cylinder.
3.11.3 Mounting of Very Small Parts, Foils, and Wires
Very small parts and foils can be difcult to place correctly for mounting. A solution
wouldbe tomount several at a time placedina piece of tube.
It can be advantageous to use a fast curing glue cyano acrylate to x the parts to
the bottomof a mounting mold before the resinis poured into the mold. Clips for stabi-
lizing the parts are commercially available see Section3.9.
Wires can be examined as cross sections or longitudinal sections. Longitudinal
sections can be done, as mentioned above, but cross sections, especially at thin wires,
can be difcult. If hot mounting is possible, Nelson
24
recommends drilling holes in a
mount made of thermoplastic resin without a specimen. The wires are put into the
holes, the holes are lled with resin and some resin is placed over the top of the mount
toavoiddamage of the upper ram. Thenthe mount is reprocessed. Transparent mounts
are to be preferred when working with small parts and wires, making it possible to ob-
serve the positionof the specimen.
3.11.4 Mounting of Powders
The most common method for mounting of powder is mixing the powder with epoxy
resin The problemcan be the settling of the particles because they either settle around
the periphery of the mounting cup or, if the powder has a lower gravity, the setting is
not efcient, the powder being suspendedinthe liquidepoxy.
Metal powder will settle, but often irregularly, and Glancy
25
suggests a method of
lling a small plastic vial or plastic tube with powder. The vial is placed in a vacuum
impregnationapparatus see Section3.10 under vacuumandepoxy is added, the same
as at a normal impregnation. Once the epoxy has cured, the plastic vial is cut length-
wise using a razor knife. Nowthe slug is mountedby hot or coldmounting. Care should
be takenat coldmounting that the slug does not oat.
For powder with particles sizes under 2 m, Petzow
2
suggests the following: The
powder is placed ina test tube ina lowvacuumlike at impregnation, see Section3.10.
It is then impregnated with a mixture of methacrylic acid methyl ester and 1 % wt %
of benzole peroxide. This mixture cures in 12 h at 50C 122F with the test tube
closed. The test tube is thenbrokenandthe content is mountedas usual.
3.11.5 Mounting of PCB Coupons
A test coupon, normally around 10 by 20 mm0.4 by 0.75 in with two reference holes
of 2 mm 0.079 in is needed if a PCB board should be inspected metallographically/
materialographically with an automatic system. In some cases the coupon is produced
together with the board and it can be removed from the board and taken directly for
mounting.
Very often, the couponhas to be made fromthe nishedboard, inthis way destroy-
ing the board. For handpreparation, the reference holes are not needed.
Test Coupon
According tothe AmericanstandardIPC-TM-650, the plated-throughholes inspection
holes of a PCB board should be inspected metallographically. For this purpose a test
coupon is produced and prepared so that the exact center of the plated holes can be
inspectedina microscope. Toobtainthe exact positionof the couponduring automatic
preparation, two positioning reference holes must be made in an exact distance from
the inspectionholes see Fig. 3.17.
Often the coupon is produced through punching the board, risking deformations
in the areas of the coupon later to be examined. If a router is used, this deformation is
avoidedandthe tworeference holes are made inthe same operation.
Mounting for Automatic Preparation
A preparation system, made according to IPC-TM-650, Method 2.1.1.2, is typically
used. As mentioned earlier, this means that two reference holes are drilled in the cou-
pon. Two or more coupons are placed on two precision pins so that the pins are in a
given distance from the holes to be measured. Now the coupons with pins are
mounted, allowing the ends of the pins to be used as contact surface in a special speci-
men holder. Generally acrylics are used for mounting of PCB coupons but polyester
and epoxy can be used also. It is important that the mounting resin is able to owinto
the holes to be measured. When using acrylics, the coupon can be dipped in the mono-
mere component ensuring a good penetration into the very small inspection holes, of-
tendownto50 mfor preparation, see Section7.10.
3.11.6 Conductive Mounts
Conductive mounts can be necessary for electropolishing and for observation in an
SEM. The simplest way of mounting is using a conductive resin, either thermoplastic
or thermosetting see Section3.13.1.
The conductive resin should only be used to establish conductivity to the top of the
mount. Around the specimen surface contacting the electrolyte, a nonconductive resin
shouldbe used.
If the specimen should be cold mounted, the simplest way is letting the specimen
protrude at the top of the mount. This is only possible if the specimen has a certain
height.
Another effective way is to drill a hole in the cold mount and insert a piece of metal
or a screw to make contact to the specimen. Also, a wire can be soldered to the speci-
menbefore mounting andthe wire takenoutside the topof the mount.
3.12 Recovery of Mounted Specimen
In some cases, the specimen cannot be etched or examined, or both, when mounted in
a mounting resin The resin can be removed mechanically, chemically, or by heating. It
Fig. 3.17PCB test coupon. It can be seen that the distance from the upper edge of the
precision pins, placed in the positioning holes, to the center of the plated inspection holes is
5 mm.
is important that the prepared surface is not damaged. First, as much resin as possible
is removed mechanically by sawing, grinding, and breaking the resin away from the
specimen. When only a small amount of resin is left on the surface of the specimen,
possibly impregnated in the surface, this can be removed chemically or by heating.
M-Pyrol N-Methyl-2-Pyrrolidone is a resin solvent, classied as a combustible liquid,
which is less hazardous than other solvents used for removal of resin The stripped
down specimen is placed in M-Pyrol at room temperature for 24 h and in most cases
the remaining resinis dissolvedor canbe removed.
An alternative is boiling N,N-Dimethyl-formamide approximately 150C
300F or in a laboratory furnace at 500600C 9001100F. Epoxy can be dis-
solvedby submerging the mount inmethylene chloride. Methylene chloride is a strong,
hazardous solvent and is carcinogenic. The mount can also be dipped in boiling glycer-
ine for 1or 2 h, whichwill softenthe epoxy sothat the specimencanbe removed.
All work should be done under a fume hood and with suitable protection. The rele-
vant MSDSs shouldbe studiedcarefully before commencing the work.
3.13 Advice and Hints on Cold Mounting
Check that the specimen material is not being inuenced by the mounting material, if
the material is at all sensitive toheat, use epoxy curing in620 h.
Ensure that the specimenis cleananddry without grease.
If using a mounting mold, take care that the material of the mold is suited for the
mounting material. Relatively exible molds shouldbe usedwhenusing epoxy.
Be careful whenmixing that the exact amount of eachcomponent by volume or by
weight is measured out. Stir for the time stated in the directions for use. It is very
important that the components are totally mixed.
Specimens withlayers requiring a perfect edge retention: Use anepoxy resin
In case of epoxy mounts larger than 50 mm2 in, the heat developed can acceler-
ate the process causing shrinking. To avoid this the amount of hardener can be re-
duced or the mount can be cooled in a refrigerator for the rst period of time, or
both.
If using a ller mixed into the mounting material, this mixture need only be in a
thin layer around the specimen. When this layer is partly cured, ll up with normal
resin
Always use special gloves whenhandling epoxy.
Always use a fume hoodfor all coldmounting resins.
Cold mounting materials, especially polyester have a limited shelf life; take care to
mark the containers upon receipt to ensure that the oldest material is used rst.
For long-termstorage, use a refrigerator.
For Trouble Shooting see Sections 13.5/6.
3.13.1 Selection of Cold Mounting Materials
Purpose
Specic
Properties
Mounting
Material
Approxi-
mate
Curing
Time at 20
C68F
Peak
Temp.
C
F
Price
Range
Serial mounting
Routing
examination
Fast curing
Translucent
Printed circuit
boards
Thermoplastic
Translucent
Medium
shrinkage
Low hardness
High removal rate
Medium chemical
resistance
Acrylics, resin
powder
with one
hardener
Without ller
615 min 90110
194
220
Medium
Good edge
retention
Serial mounting
Fast curing
Thermoplastic
Low shrinkage
High/medium
hardness
Low removal rate
Medium chemical
resistance
Acrylics, resin
powder with
one hardener
and with
mineral ller
815 min 90
194
Medium/
high
Routine
examination
Serial mounting
Thermosetting
Transparent
High shrinkage
Medium hardness
High removal rate
Low chemical
resistance
Polyester, resin
and hardener,
both liquids
45 min to
6 8 h
50110
122
240
Low
Very good edge
retention
Transparent
mounts
Porous
specimens
Impregnation
Plated layers,
thermal
spray coatings
Mineralogy
Thermosetting
Transparent
Low shrinkage
Medium
hardness
Medium removal
rate
Low viscosity
Epoxy, resin
and hardener,
both liquids
620 h 3060
86
140
Medium
Serial mounting
Routine
examination
Transparent
mounts
Thermosetting
Transparent
Medium shrinkage
Low hardness
Medium removal
rate
Epoxy, resin
and
hardener, both
liquids
3045 min 85100
185
220
High
4
MarkingStoragePreservation
4.1 Marking
MARKING OF METALLOGRAPHIC/MATERIALOGRAPHIC SPECIMENS IS
very important because a proper identication of the specimen is the only thing that
ensures that the result of the analysis is correctly used. This is true for both quality
control and research, and it can be said that the specimen must be marked in all cases
where a metallographic/materialographic analysis shouldbe reported.
The marking should not in any way inuence the microstructure of the surface to
be examined; therefore, this risk should be considered before marking is done. It
should also be considered that the marking is placed where it is not disturbed or re-
movedduring the preparationprocess.
The backside of the specimen/mount is usually used for marking. Considering the
limited space, a code expressing job number, material treatment, etc., is used most of-
ten.
If the nal marking is done on the mount, special care should be taken that the
specimen is identied at the stage after sectioning, before mounting, so that correct
marking of the mount is assured.
Anumber of methods for marking are available.
4.1.1 Marking with Waterproof Ink
This cannot be recommended because the treatment of the specimen/mount will in
most cases remove the ink. Marking inkor pencil canbe usedas anintermediate.
4.1.2 Identication Tag
This works well if the tag carton or metal is placed on the backside of the specimen
and mounted in a reasonably transparent resin, the resin protecting the tag. A tag
placed on the outside of the specimen/mount, however, might be removed during
cleaning inwater andalcohol.
4.1.3 Engraving
One of the most widely used methods of marking is vibration engraving. A very hard
vibrating needle induces a visible deformation of the surface of the mount/specimen.
This method will stress the material layer below the surface and it should not be used
for thinspecimens like foils.
Electro engraving gives less damage to the surface, but can only be used on electri-
cally conducting materials. The engraving, on a clean and smooth surface, is done
throughthe melting/evaporationof metal, causedby a hightemperature spark.
Hand engraving, using a hard needle, is also possible in most, not too hard,
materials.
4.1.4 Stamping
Stamping a number or code in the specimen is possible but because of the very strong
deformation below the stamped surface this method should only be used in cases
where it will not disturbthe material tobe examined.
80
4.2 Storage
It is important that the prepared surface of a specimen is not disturbed by attack from
the atmosphere. Therefore, the prepared specimen is placed very often in a dessicator
with moisture-absorbing material. Airtight cabinets are also commercially available.
For long-term storage, often the specimen should be stored for several years, a direct
preservationof the surface is recommendedsee below.
4.3 Preservation
To absolutely protect the prepared surface a lacquer usually from a spray can is used.
The microstructure can be examined through the lacquer, or the lacquer can be re-
movedeasily withacetone andthe specimenresprayedafter examination.
Chapter 4 MarkingStorage 81
5
Cleaning and Cleanliness
TOAVOIDARTIFACTS IT IS VERYIMPORTANT, ESPECIALLYINTHEPOLISH-
ing stage, that the specimen/specimen holder is carefully cleaned between each step. It
is also important that the room in which the process takes place and the operators
hands are cleantoavoidcontaminationof the polishing cloths.
Cross contamination: Considering that the preparation process often includes
abrasives with grain sizes spanning fromgrit 180 82 m grinding paper to 1 mdia-
mond suspension, it is evident that cross contamination, larger grains from an earlier
step, cannot be tolerated. Cross contamination can be caused by an inadequate clean-
ing of the specimen, specimenholder, or by the operators hands.
The polishing disk may become contaminatedfromairborne particles or excessive
debris inthe machine.
5.1 Cleaning
5.1.1 Cleaning Before Start of Preparation
All greases, oils, andother residues onthe specimenshouldbe removedby water witha
detergent or a suitable organic solvent. Failure to clean thoroughly can prevent cold
castable and hot compression mounting resins from adhering to the specimen sur-
face. Also oxidation, etc., should be removed unless these products are to be exam-
ined. As some of the more rough cleaning methods, like shot blasting and wire brush-
ing might damage the surface, it shouldbe consideredwhether this might inuence the
nal result of the preparation. In special cases, where normal procedures are unsuc-
cessful, electrolytic or chemical cleaning can be used see ASTMStandard Practice for
Preparationof Metallographic Specimens E3, Section12.4.
5.1.2 Cleaning During and After Preparation
In principle, the specimen and the specimen holder xed specimens should be
cleaned between every step in the grinding and polishing process, but at wet grinding
on SiC paper, using a constant ow of water, a careful cleaning can be limited to after
the last grinding step. When grinding on other media, like rigid composite disks and at
polishing, a cleaning betweeneachstepis absolutely necessary.
There are, however, some materials or some constituents in materials that will be
preferentially attacked by water zinc coatings on steel, lead inclusions in machining
steels, etc., therefore, water must be avoided completely in the latter preparation
steps.
Cleaning by Hand
For cleaning of most metals and other materials without pores, cracks, etc., manual
cleaning is the most effective method.
The specimen or specimen holder is held under running lukewarm water and
rinsed with a soft brush or cotton ball dipped in water with a detergent. In cases of soft
materials and after the last polishing step, a cotton ball is used to clean the prepared
82
surface. The cleaning is nished with the spraying of ethylene alcohol from a spray
bottle on the prepared surface and possibly wiping the surface before it is taken for
drying. Ethanol containing a denaturation additive can be used as long as the additive
does not leave a lmon the specimen. In case of specimens with pores, cracks, etc., and
mounts with a gap between mounting material and specimen, ultrasonic cleaning is
recommended, except for fragile materials.
In case the standard cleaning methods are inadequate, the cleaning solutions
stated in ASTMStandard Practice for Preparation of Metallographic Specimens E 3,
TABLEX1.1, canbe used.
Ethanol
Although ethanol ethyl alcohol is taken by many persons in different forms, the etha-
nol used in a laboratory has the following Hazards Identication, Human Health: Or-
ganic solvents may be absorbed into the body by inhalation and ingestion and cause
permanent damage to the nervous system, including the brain. The liquid may irritate
the skin, the eyes andthe respiratory tract.
Ultrasonic Cleaning
Ultrasonic cleaning is efcient and relatively fast, removing dirt from pores, gaps,
cracks, etc.
The specimen or specimen holder is placed in a tank with a liquid, water with a
detergent, alcohol, or an organic solvent like acetone. In cases of dirt difcult to re-
move, weakacids andbasic solutions canbe used.
A transducer vibrates under the bottom of the tank, with 2040 kHz creating gas
bubbles cavitation in the liquid. These bubbles implode and a rubbing effect occurs
which removes the dirt. The dirt contaminates the liquid and therefore a specimen
must be rinsed, as mentioned above, before drying. Ultrasound penetrates glass so it is
possible to place one or more beakers in the tank with water with a detergent around
the beakers. When the specimens are only placed in the beakers, in a suitable liquid,
this liquid can easily be exchanged when contaminated. Cleaning usually takes
0.51 min. Some soft, very porous and brittle materials should not be cleaned ultra-
sonically or only for 1030 s. Using specimen holders, the whole holder can be placed
inthe tank.
Ultrasonic Apparatus
Ultrasonic apparatuses are supplied with tanks of different size from 1.510 L
0.42.6 gal U.S. and with capacities from 80 W to 470 W. The ultrasound is pro-
duced mostly from a piezoelectric transducer but magnetostrictive transducers can
alsobe usedwithlarge units. The frequency is 2050 kHz.
Drying
Drying should take place in a streamof mild air. It is important that the layer of alcohol
is not dried on the prepared surface but is blown away and evaporates fromthe sides of
the specimen/mount. Air can be supplied froma xed hair dryer type apparatus allow-
ing bothhands to be free to cleanthe specimenwithsoft cottonwool andalcohol. Com-
pressed air canbe used as well, inwhichcase a clean, dry, oil free air must be secured. A
hair dryer is recommended for the nished specimen to avoid possible oil drops from
the compressedair.
Chapter 5 Cleaning and Cleanliness 83
Cleaning of Grinding Disks and Polishing Cloths
Grinding disks based on diamond usually are used with water as a lubricant and clean-
ing shouldnt be necessary. Rigid composite disks RCD, lubricated by a special lubri-
cant, will be covered with swarf after use. This typically will not disturb the function,
but if the swarf has dried and therefore lled up the openings between the segments of
the disk, the disk should be cleaned. This is done with a brush, detergent, and luke-
warm water. A cloth that has been contaminated can be cleaned in the same way but
different brushes should be used for the grinding disks and the cloths because of the
different grainsizes.
5.2 Cleanliness
It has already been mentioned above that a high level of cleanliness is needed when
preparing metallographic/materialographic specimens. The operator should be aware
that no contamination takes place through transfer of debris fromthe hands of the op-
erator. The roominwhichpolishing takes place shouldbe cleanandshouldnot contain
dust in the air. The room for preparation, when possible, should not be part of a pro-
ductionenvironment.
It is advisable that cutting does not take place in the same room as grinding and
polishing, as the cutting produces large amounts of debris.
The grinding/polishing machines should be kept clean according to a weekly
schedule, securing that no contaminationcantake place fromthe sides of the machine,
splashring, etc. This alsoprolongs the lifetime of the equipment.
6
Mechanical Surface
PreparationGrinding
6.1 GrindingA Basic Process
AFTER SECTIONING AND POSSIBLY MOUNTING, THE METALLOGRAPHIC/
materialographic specimen is nowto be prepared to obtain the true microstructure or
a structure, which, in spite of certain defects artifacts, will give a true examination
result. For a thorough description of artifacts and how to avoid them, see Sections
13.5/6.
The true structure has been dened in Section 1.2, indicating a surface with no or
few artifacts. In practice only two ways are open to obtain this, either mechanical
preparation, grinding and polishing, or grinding, followed by electrolytic polishing
see Fig. 1.7 to get an overview. In some cases a chemical attack can be included in the
mechanical polishing, creating chemical mechanical polishing, and, more seldom,
chemical polishing is used see Sections 7.12 and 8.7, but in all cases one or several
grinding steps are performedbefore the polishing takes place.
In this book, grinding is dened as an abrasive machining process with a xed
abrasive. The abrasive grain might be xed from the start of the process, either by a
bond ceramic, metal, resinoid or placed on a exible backing covered by a coating,
like at SiC grinding paper, or covered by a thin layer of metal on a backing of metal
plate. Also the abrasive grain, normally suspended ina liquid, canbe added to the abra-
sive machining process taking place on a plane, prepared disk. In this case some of the
grains will be forced into the disk surface, be xed in the moment of cutting, and grind-
ing takes place. In case the abrasive grain is not xed but staying loose and rolling be-
tween the work piece and the disk surface a lapping process takes place. Consequently
in this book, a disk to be used with loose abrasive grains is called a grinding disk, if
the majority of the grains are xed when the material removal takes place, producing a
ground surface, and a disk where the majority of the grains are loose, producing a
lappedsurface, is calleda lapping disk see alsoSection6.7.7.
6.1.1 Plane Grinding PG
Plane grinding, alsocalledplanar grinding, may be necessary for three reasons:
1 To plane the surface after sectioning, depending onthe sectioning method, the sec-
tionedsurface might not be plane.
2 To remove the deformation caused by the sectioning and establish a known start
surface of the specimentosecure a reproducible further preparation.
3 When a number of specimens are xed in a specimen holder, the specimen sur-
faces are not inthe same plane, andmaterial has tobe removedtoobtainthis.
Plane grinding is usually performed with relatively coarse abrasive grains and will
be described further under the different grinding methods mentioned below see also
Fig. 13.14.
85
6.1.2 Fine Grinding
Fine grinding is the process used for establishing a specimen surface suited for the rst
polishing step. This means that the relatively rough surface from sectioning or plane
grinding, through one or several steps with ner and ner grain sizes, is changed into a
surface that can be treated by polishing. The ne grinding steps are needed because
the material removal is relatively high, opposite to the polishing steps with a lowmate-
rial removal see below.
Fine grinding is further described under the different grinding methods men-
tionedbelowsee alsoFig. 13.15.
Grinding plays a major role in the preparation process and, therefore, it will be
discussed in depth in the following. The mechanics of the grinding process, being a
cutting process producing chips are the same as in wet abrasive cutting see Chapter
2, andthey are basically the same inmechanical polishing.
In mechanical grinding/polishing, the following two features should be
considered.
Material Removal
Material is removed fromthe specimen surface during the process. The amount of ma-
terial removed can be expressed by the removal rate, often measured as mper minute
or mper a certaintravel inmmetres of the specimenonthe preparationsurface.
The preparation process is controlled mostly by time, assuming that a certain
amount of material is removed from the specimen per time unit. This assumption is
often not correct because a number of parameters that are not totally controlled, such
as preparation surface, abrasive, and lubrication, inuence the removal rate. By the
device, stock removal, sometimes used on grinding machines, the process is not con-
trolled by time but through a constant measurement of the actual removed amount of
material. In this way the process can be stopped when the amount of material planned
for is removedsee Section7.7.6.
Deformation
Deformation can be dened as the nature and depth of the plastically deformed layer
that is producedinthe specimensurface during material removal.
In general, the removal rate should be as high as possible and the deformation as
low as possible. This depends on the interaction between the abrasive grain and the
specimensurface as describedinthe following.
6.2 Material Removal
Grinding is dened as a process with xed abrasive grains, acting like machine tools.
Figure 6.1 shows a schematic drawing of a tool removing a chip froma work piece. The
abrasive grains will remove chips fromthe specimensurface inthe same way.
Using a normal machine tool like a lathe for the cutting process, macroscopic
chips in the form of ribbons or particles having a thickness of from about
0.025 to 2.5 mm 0.0010.1 in are produced. In grinding, the chips produced are
much smaller, ranging in thickness from 0.0025 to 0.25 mm 0.00010.01 in. The
reason for this is the shape and size of the abrasive grains, acting very differently as
tools.
During the cutting process the tool and work piece are forced against each other
and a compressive force is set up which causes the metal to deformin front of the tool
point.
The deformation will take place in a zone along the shear plane see Fig. 6.1 and
the metal is forced to slide over the tool surface. In doing this, the stress will cause the
material to separate as a chip, if the rake angle is correct see below. The cutting pro-
cess is very complex, inuencedby cutting speed, tool geometry, andfeedrate.
Amathematical model has been developed for abrasive machining of a work piece
moving in a linear path across a planar abrasive device like grinding paper under a
constant normal loadL.
7
Inthis model the material removal rate canbe expressedas:
m= fDL/H
m
1
where mis the mass of material removed, f is the fractionof the contactingpoints that cut a
chip, is the density of the work piece material, Dis the distance traveled, Lis the load, His
the indentation value of the surface layers of the work piece material and
m
is a form
factor expressing the shape of the contacting points. The most interesting aspect from a
metallographic/materialographic viewpoint is that the material removal increases within-
creasing load and decreases with increasing hardness of the work piece material. This lat-
ter assumption, however, only covers hard metals where the removal rate can be expected
to be relatively small, but the relative removal rates for metals of low and intermediate
hardnesses are virtually unpredictable.
7
6.2.1 Rake Angle
The rake angle is the angle between the top face of the tool and a plane perpendicular
tothe workpiece, as schematically showninFig. 6.2.
Rake angles may be classed as positive, negative, or neutral tool face perpendicu-
lar tothe workpiece, as showninFig. 6.3.
To create a chip, the rake angle has to be positive, neutral, or to a certain degree
negative. With a positive rake angle, the area under shear decreases, leaving less defor-
mation in the surface of the work piece, and the friction heating is lower than with a
neutral or negative angle.
At a certain negative angle, the critical rake angle, the chip is not produced any-
more anda plowing takes place as showninFig. 6.3.
7
When plowing, the rake angle is so negative that only a groove is made in the work
piece surface. A standing wave bulge forms in front of the tool, and material is dis-
Fig. 6.1Basic model of cutting process indicating shear zone.
Chapter 6 Mechanical Surface 87
placed into a ridge on each side of the groove. The material removal approaches zero
andthe deformationof the surface increases.
6.2.2 Grain ShapeContacting Points
In cutting, using a machine tool like a lathe, the shape of the cutting tool is given with a
xed geometry. In grinding, using the abrasive grains as cutting tools, the shape of the
grain and the number of edges and points vary extremely. Figure 6.13 shows the grains
of a grit 220 SiCgrinding paper. The most effective shape of the grain is a V-formcreat-
ing an efcient chip provided that the rake angle is correct. If the grain is at, the cross
section of the chip is reduced and in the case of at grains of a certain size the specic
pressure between grain and surface will decrease and no cutting will take place, result-
ing inplowing or noactionat all.
It is very important that a high number of contacting points are available to obtain
an efcient grinding. Only a small number of the visible contacting points make con-
tact withthe specimensurface. At coarser SiCpapers like grit 220 only approximately 1
in10points make contact andat ner papers like grit 600only 1in20.
7
Fig. 6.2Basic model of cutting process indicating rake angle.
Fig. 6.3Schematic drawing of possible rake angles with abrasive grains in different positions.
Cutting is shown with a chip being removed from the work piece and plowing is indicated as a
groove with ridges.
7
6.2.3 Grain Penetration
The depth of penetration at the contacting points of an abrasive grain into the work
piece is only a small percentage of its size. At grinding, the maximum value is in the
range of 5 %, meaning that a grit 220 grain with an average size of 68 m using a pres-
sure of 40 kPa 6 psi will penetrate less than 34 m into the specimen surface. In
practice, at grit 220 SiC grinding paper the penetration scratch depth at an annealed
30%Znbrass will be upto5 minthe rst seconds anddropto22.5 m.
7
6.2.4 Force on Specimens
In principle, the material removal increases linearly with the increase in specic pres-
sure between specimen surface and grinding surface. This means that a certain force is
needed to obtain a satisfactory high removal rate. It is, however, a problem with SiC
paper that a too high specic pressure might cause stronger deformation in the speci-
men. This is especially important during the rst fewseconds whenthe paper has a few
large grains causing a very aggressive attack see Section6.6.
At grinding, the force should correspond to a specic pressure from 30100 kPa
4.3514.5 psi depending on the material to be ground. In theory the specic pressure
should be kept regardless of specimen size, but experience has shown that the force on
the single specimen should not exceed 50 N 11 lb
f
, and as compensation, to obtain
the necessary material removal the preparation time is extended. A too high pressure
might cause the grinding paper, in most cases held only by a water layer see Section
13.2.4 to be dragged off the support disk and the more expensive paper with adhesive
backing or a double adhesive foil must be used. If a polishing cloth is used for grind-
ing the clothmay overheat.
6.2.5 Grinding/Polishing Fluids
The uids used for metallographic/materialographic grinding/polishing has no lubri-
cating effect regarding the actual cutting process taking place between the abrasive
grain and the work piece specimen material, creating chips.
7
The uid has a strong
cooling effect andespecially incase of grinding, the uid, usually water, will remove the
swarf. If the debris is not removed the grinding surface becomes clogged and it will
create deformationinthe specimensurface.
At polishing the uid, also called lubricant, is lubricating the surface of the polish-
ing cloth, reducing the friction and heat developed between cloth and specimen, at the
same time removing swarf fromthe cloth surface. For more details on uids and lubri-
cants see Sections 2.3.7and6.5.
6.3 Deformation
6.3.1 Metals
In metals, being ductile materials, the separation of a chip during machining opera-
tions induces complex systems of plastic deformation in both the separating chip and
the specimen material. An inevitable consequence is that a layer, plastically deformed
during machining, is left in the new surface that is produced. In general terms, the
strains inthis layer are very large at the surface anddecrease more or less exponentially
withdepth. See alsoFigs. 13.313.6andFigs. 13.1913.22.
This deformed layer becomes important in metallography when the plastic defor-
mationchanges the microstructure of the specimenina way that canbe detected inthe
microscopic examinationthat is tobe performed. The layer is thenanimportant poten-
tial source of false structures, or preparation artifacts, the avoidance of which is one of
the primary objectives of a metallographic preparationsequence.
As mentioned above, the abrasive grains act as machine tools set at different rake
angles. Whena chipis separatedfromthe surface, the shear strains are concentratedin
the so-called shear zone in front of the tool. A region adjacent to this shear zone, and
extending into the specimen in advance of the tool is also plastically deformed though
toa lesser degree, as showninFig. 6.4.
Samuels
7
has done anexhaustive study of the deformationcreatedinthe specimen
surface of metals, by using taper sections see Section3.11.
A taper section of annealed polycrystalline 30 %Zn brass ground on a 220 grit SiC
paper, etched with different etchants shows the surface of the specimen with scratches
andthe deformationinFig. 6.5.
Samuels
7
splits up the layers into two levels of deformation, the shear-band layer
at the surface that has been subjected to large strains, and the deformed layer beneath
the shear-band layer. The shear-band layer typically extends preferentially beneath in-
dividual polishing scratches for approximately twice the depth of the scratch with
which it associates. In the deformed layer the material has been strained by simple
compression, and the magnitude of the strains decreases with depth until a level is
reached where the material is only elastically strained. This elastic-plastic boundary
denes the lower limit of the deformed layer. An important difference between the
shear-band layer and the deformed layer is that the presence of shear-band layer mate-
rial is always apparent after etching with any etchant suited for the material, whereas
the presence of the less deformed material becomes apparent in light microscopy only
Fig. 6.4Section of a chip cut in 70:30 brass by an orthogonal tool with a highly negative rake
angle.
7
in a rather limited number of materials, and then, perhaps, only after etching by spe-
cic methods.
Samuels splits the deformedlayer into two depths, the total deformedlayer D
d
and
the signicant deformation D
s
. This gives the following three levels of deformation in
anabradedmaterialographic specimen:
Depth of shear-band layer D
sb
: The maximum depth beneath the root of the sur-
face scratches of the shear-bandlayer.
Depth of deformation D
d
: The maximum depth beneath the root of the surface
scratches tothe elastic-plastic boundary.
Depthof signicant deformationD
s
: The maximumdepthbeneaththe root of the
surface scratches of the deformation that would noticeably affect the observations to
be made onthe nishedsurface.
The value of D
s
is the most important one regarding metallographic preparation. It
varies with materials and the etchant used and the level of the nished specimen sur-
face shouldalways be beyondD
s
.
Example: AnnealedPolycrystalline 30%ZnBrass
7
SiCgrinding paper, 220grit, withwater, handabrasion
D
sb
scratches: 2 m
D
d
: 77 m
D
s
: 7.5 m
Fig. 6.5Taper section of the surface of annealed polycrystalline 30 % Zn brass that has been
ground on grit P220 SiC paper. The section has been etched by several methods that have
different threshold strains for revealing deformation as follows. a Ferric chloride reagent
threshold strain: 5 % compression. b Cupric ammonium chloride reagent threshold strain:
0.1 % compression. c Low sensitivity thiosulfate etch threshold strain: 0.1 % compression.
d High-sensitivity thiosulfate etch threshold strain: elastic limit. In each case, the base of the
layer, in which the manifestations of deformation have been developed, is indicated by an
arrow. Taper ratio 8.2, 250:1.
7
6.3.2 Brittle MaterialsCeramics
The above description covers ductile materials like metals, which when stressed, will
plastically deforma signicant amount before fracture occurs. This is not the case with
brittle materials like most ceramics, which deformonly elastically prior to fracture by
propagationof a crack. To understandthe effect oftentaking place at grinding of brittle
materials, it can be seen how the indentation of a sharp point and a spherical point
affects the surface of a specimen. When a sharp point, a in Fig. 6.6, is pressed into the
surface, a pseudo-plastic zone 1 of irreversible deformation is produced beneath the
indentation. This impression stays in the surface, and by increasing force a so-called
medianvent crack invertical direction2 develops, andby further increase of the force
lateral vent cracks develop b 3. When this lateral vent crack develops to the surface,
a relatively large volume of material is removed which can be called a fracture chip,
considerably larger than the chips earlier described under metals.
7
If an indentation is
made with a spherical point, c in Fig. 6.6, rst a pseudo-plastic zone 1 develops, at
increasing force followed by a cone ring crack 2 and by further increase of the force
also a median vent crack develops 3. The circular symmetry of the ring crack will be
lost if the indenter is drawn across the surface as by grinding/polishing, and the crack
might follow grain boundaries and cause pull-outs of whole grains or parts of grains,
d in Fig. 6.6. The same might happen with the crack formation shown in a, Fig. 6.6.
As mentioned above the material removal in brittle materials to a high degree takes
place with fracture chips, leaving cavities in the surface e in Fig. 6.6, but according to
Samuels
7
this is mainly the case at the larger abrasive grain sizes, whereas below grit
P1200approximately 15 m it seems that chipcutting without fracturing takes over.
It can be seen in Fig. 6.6 that beneath the fracture cavities and pull-outs, a crack-
Fig. 6.6Schematic drawing of surface damage to ceramic material. Because of the brittleness
of the material, micro cracks and pull-outs surface fractures are developed in the surface
during the grinding. When a sharp point a is pressed into the surface, a pseudo-plastic zone
1 of irreversible deformation is produced beneath the indentation. A median vent crack 2 in
vertical direction may develop. By increasing force b lateral vent cracks 3 may develop. If an
indentation is made with a spherical point, c rst a pseudo-plastic zone 1 develops, at
increasing force followed by a cone ring crack 2 and by further increase of the force also a
median vent crack 3 may develop. Pull-outs of whole grains or parts of grains, d and smaller
pull-outs e. Crack following grain boundary f.
containing layer develops, f, which extends to considerable depth. This layer must be
removedduring the preparation.
Anormal preparation procedure for ceramics and other hard and brittle materials
is grinding with a bonded diamond grinding disk followed by grinding on rigid com-
posite disks or very hard polishing cloths with diamond and a nal polishing on a me-
diumhard cloth with silica. The most serious problemis the development of pull-outs
and cavities developed during the rst grinding steps with bonded diamond disks.
These artifacts, which as a mistake can be considered to be pores belonging to the true
structure, must be effectively removedduring the grinding onthe rigidcomposite disks
see Sections 3.10, 6.6.1, 6.7.7, and13.5/6.
Preparation of ceramics is stated in Material/Preparation Tables 0206 in Section
13.2.3. For in-depthinformationonceramics and preparationof ceramics, see Refs. 26
and27.
6.4 Grinding Abrasives
The abrasives already described in Section 2.3 for abrasive cutting are also used for
grinding, but belowa further descriptionrelatedtogrinding/polishing is given.
6.4.1 Aluminum Oxide
Hardness: 2500 HV
AlthoughAl
2
O
3
, alumina, has certainadvantages, especially for grinding of steel, it
is not used much for metallographic/materialographic grinding except in ceramic
grinding stones and in connection with zirconia in wet grinding paper for plane grind-
ing.
Very ne alumina is usedfor polishing see Section7.5.
Aluminum oxide was the rst grinding medium found in nature, typically emery
about 50 % Al
2
O
3
with other oxides, principally iron oxide and corundum. Around
1900 a process was found to turn bauxite into Al
2
O
3
and today it is the most used abra-
sive. Al
2
O
3
is available in different crystals with the particles mostly used for grind-
ing. Al
2
O
3
easily forms substitutional solid solutions like the combination Al
2
O
3
and
ZrO
2
mentionedabove.
Being made in many different types, Al
2
O
3
also has very different surface struc-
ture. The types with relatively smooth surfaces are used for rough grinding operations.
Types witha surface withsharpfacets are usedfor ner grinding.
6.4.2 Silicon Carbide
Hardness: 2700 HV
SiCplays animportant role inmetallographic/materialographic grinding withSiC
grinding paper being usedfor bothplane grinding andne grinding see Section6.6.2.
SiC is the rst synthetic abrasive, made in the 1890s. There are two grades of SiC.
The green type is relatively friable and has fewer impurities; the black type has the
same hardness as the green type but is less friable. Most of the SiC used for grinding is
of the blacktype. Siliconcarbide is the secondmost widely usedtype of abrasive.
The surface structure of an SiC grain is rather irregular, resembling fractured
glass. This is anadvantage whencoatedonanSiCgrinding paper because the grainwill
be xedrmly inthe coating cement but the irregular surface combinedwithanirregu-
lar shape will give an increased deformation of the specimen surface see Section
6.6.2.
6.4.3 DiamondDiamond Products
Hardness: 8000 HV
Diamond plays an increasing role in metallographic/materialographic prepara-
tion. A number of products based on diamond are developed using diamond grains as
xedor loose abrasive for bothgrinding andpolishing see below.
Diamond, together with cubic boron nitride CBN, belongs to the superabrasives.
Since the 1940s, natural diamonds have been used for grinding purposes. After many
years of research, methods to make synthetic diamonds were developed in the 1950s
60s and today almost all diamonds used for grinding and polishing are synthetic. Dia-
monds are made withtwocrystal structures: polycrystalline andmonocrystalline.
The polycrystalline grain, having many sharp edges, is relatively friable and will
break down during use, giving a self-sharpening effect, as shown in Fig. 6.7. Polycrys-
talline diamonds are considered the most effective for materialographic preparation
because of a higher removal rate thanmonocrystalline diamonds inmost materials.
7
Monocrystalline grains are stronger, having a blocky formwith relatively fewcut-
ting edges and will not easily break down. If they break down, it takes place along
straight lines, as showninFig. 6.8, not creating many newcutting edges.
Fig. 6.7Schematic drawing of polycrystalline diamond grain before and after grain fracture
creating many new cutting edges.
Fig. 6.8Schematic drawing of monocrystalline diamond grain before and after grain fracture
creating only a few new cutting edges.
Diamond Products with Fixed Grains
Diamond is used in a number of products, all having the diamond grains xed in some
kind of bond. These materials are used for grinding of metallographic/material-
ographic specimens, ranging from plane grinding with relatively coarse grits to ex-
tremely ne grits usedinthe diamondlapping lms see below.
Diamond Grinding DisksThe diamond grains are placed in a metal or bakelite
bond. Primarily used for traditional grinding of very hard materials see Section
6.6.1.
Resin-Bonded Diamond Grinding DisksThe diamonds are placed in a thin layer
in a resin bond not bakelite. This type of disk is used for contemporary grinding of
all materials harder than150 HVsee Section6.7.
Metal-Bonded Diamond DisksThe diamonds are placed in a thin layer xed by a
nickel coating see Section6.7.4.
Diamond PadsThe diamonds are placed in a bond of metal or resin in a dot ma-
trix on a self-adhesive backing. Used for plane and ne grinding of hard materials see
Section6.7.5.
Diamond FilmThe diamonds are coated to a very thin lm lapping lm. This
product is used for grinding/polishing of electronic devices, wafers, etc. see Section
6.7.6.
Diamond Products with Loose Free Grains
A number of products are available with the diamond grains mixed with a carrier, en-
abling grinding or polishing with free grains on the surface of the grinding/polishing
disksee below.
Grain Size
It is very important that the grains for a given grain size are selected with a narrow
tolerance. If the grains are relatively uniform, as showninFig. 6.9 a a very highpart of
the grains are active, securing a high removal rate; Fig. 6.9 b shows diamond grains
with a large difference in grain size and it can be seen that a high number of grains are
present only as ller and with only a few acting grains. This causes the specic pres-
sure on each grain to be high, possibly causing deeper scratches in the specimen
surface.
Fig. 6.9Diamond grains 2, uniform size a and nonuniform size b, between grinding/
polishing disk 3 and specimen 1. The smallest grains b are not active.
Diamond Suspensions
The use of diamond suspensions slurries is increasing because applying the abrasive
in small quantities during the process is an advantage, giving a more constant removal
rate thanother types of diamondproducts.
28
Suspensions are suited for being applied from a dosing unit, in this way making
the charging of the grinding disk/polishing cloth, automatic. The automatic dosing can
be performed as spray, creating aerosols, which are considered dangerous to health, or
by pumps, supplying the suspensions in drops. Also the suspension can be conve-
niently appliedby handfroma pumpspray bottle.
Diamond suspensions can be based on water, alcohol, oil, or other hydrocarbons.
Water-based suspensions are to be preferred, because of the nontoxic nature of water.
To the suspension should be added an ingredient that stabilizes the diamond grains so
that they do not sediment or only sediment very slowly. In case sedimentation takes
place, the bottle with suspension can be placed on a stirring apparatus or in other ways
be stirredduring the process.
Incertaincases, whenthe material to be prepared is sensitive to water, a water-free
suspension based on oil or preferably on alcohol, should be used. Diamond suspen-
sions are available with both polycrystalline and monocrystalline diamonds in the
range 45 m to 0.05 m. The grain sizes most used are 9 and 6 m for ne grinding/
roughpolishing and3, 1, 0.25, 0.1, and0.05 mfor polishing andnal polishing.
The polycrystalline suspension is preferred if the highest removal rate and best
nish is wanted. This is due to the fact that the polycrystalline grains break down dur-
ing the process andinthis way creates newcutting edges. Monocrystalline suspensions
are normally less expensive than polycrystalline, and the removal rate is considered to
be lower.
Normally the suspension is used in combination with a lubricant see Section 6.5.
In this way the adding of new grains and the establishment of a lubricating lm are
separated, making it possible for a more exact dosing of both. Diamond suspensions,
also acting as lubricants, however, are available. Using these, only one product is added
to the grinding/polishing disk, establishing both a sufcient number of active grains
anda lubricating lm.
Diamond Sprays
Both polycrystalline and monocrystalline diamonds are available in spray cans. The
advantage of using spray is the very small amount of other material introduced to the
process that are opposite of suspensions and pastes which contain a high amount of
carrier. Diamond sprays are available in the grain sizes 45, 25, 15, 9, and 6 m for ne
grinding/roughpolishing and3, 1, and0.25 mfor polishing.
Diamond Pastes
This is the original way of distributing the diamond, by rubbing a small amount of dia-
mond paste into the polishing cloth. For this reason diamond cannot be added during
the process and in certain cases, like working with a rigid composite disk RCD, the
paste will disturbthe process.
A variation of paste is the stick, where the diamonds are placed in a harder wax;
this is easier to apply than paste. Pastes are available with both polycrystalline and
monocrystalline diamonds. The grain sizes available are 15, 9, and 6 m for ne
grinding/roughpolishing and3, 1, and0.25 mfor polishing
6.4.4 Cubic Boron Nitride CBN
Hardness: 4500 HV
CBNis made along the same lines as diamond, with high pressures and high tem-
peratures. The main reason why CBN is of interest as an abrasive is that it is much
more chemically stable thandiamondinthe presence of hot ironsee Section2.3.
CBN crystals are relatively smooth which makes bonding difcult. Therefore, the
grains are oftencoatedwithmetal, suckas nickel.
CBNcanbe used ingrinding disks ina metal or bakelite bond for very hard ferrous
metals.
6.4.5 Boron Carbide
Hardness: 2800 HV
Boron carbide B
4
C was developed for grinding purposes, but for different rea-
sons the use is limited. It is used as a suspension for lapping purposes, the grain having
a porous structure with many sharp edges. B
4
C is seldom used in metallographic/
materialographic grinding andpolishing.
6.4.6 Hardness of Abrasives and MaterialsTable 6.1
Table 6.1 gives a comparison between the Vickers hardness of a number of materials to
be preparedandthe abrasive materials usedinthe preparationprocess.
6.5 Grinding/Polishing FluidsLubricants
The most commonly used uid for traditional grinding see Section 6.6, with grind-
ing stones and SiCwet grinding paper, is water with or without an additive. If the water
is recirculated, an additive should be used to prevent corrosion and reduce bacterial
growthinthe water see Section2.3.7.
For contemporary grinding see Section 6.7, using grinding disks with xed
grains, water is also used, but in the case of ne grinding on rigid composite disks
RCDs, lubricants, also called extenders normally used for polishing, are used. They
are describedbelow.
6.5.1 Water-Based Lubricant
This lubricant is to be used if possible because it has no environmental effects. It is
suited for polishing of most materials using polishing cloths. Incase of ne grinding on
rigid composite disks, the water-based lubricant should be dosed in small amounts to
avoid aqua planing where the specimen is planing on the uid layer, not getting into
contact with the surface of the disk. For polishing of certain soft, ductile materials, a
water-oil basedlubricant shouldbe usedsee below.
6.5.2 Alcohol-Based Lubricant
This type of lubricant gives a high removal rate and a good cooling due to the fast
evaporation of the alcohol. For this reason this lubricant can be used as an alternative
for a water-based lubricant for work on rigid composite disks, which shall work dry
to secure that the specimen is in direct contact with the disk surface. An alcohol-based
lubricant shouldbe usedfor materials that are sensitive towater.
Alcohol ethanol is considered dangerous to health by inhalation and ingestion
andfor this reasonthis lubricant shouldbe avoidedif possible.
6.5.3 Water-oil Based Lubricant
This type of lubricant, water with an in-mixed oil forming an emulsion, will give a less
aggressive action between cloth/abrasive and specimen surface than the water- and
alcohol-basedtypes. Anoil lmwill act as a membrane betweenthe polishing clothand
specimen. The lubricant is used for polishing of soft, ductile materials. Because of the
oil, whichmight cause skinproblems, the use shouldbe as limitedas possible.
6.5.4 Oil-Based Lubricant
This lubricant is a lapping oil based on mineral oil heavy petroleum distillate. Like
withthe water-oil basedlubricant mentionedabove, it is usedfor soft, ductile materials
TABLE 6.1Hardness of Abrasives and Materials.
to reduce the formation of deformations. Mineral oil may cause irritation by repeated
skin contact and by inhalation of vapors or aerosols, or both. For these reasons the use
shouldbe limitedor avoided, if possible.
6.6 Traditional Grinding
The expression traditional grinding covers the grinding methods used for a very long
time in metallographic/materialographic preparation: Grinding stones/disks with ce-
ramic or bakelite bonds and silicon carbide SiC, alumina Al
2
O
3
, and zirconium-
alumina wet grinding paper.
6.6.1 Grinding Stones/Disks
Grinding Stones for Plane Grinding of Metals
Grinding stones with aluminumoxide as abrasive and a ceramic bond are used mainly
for plane grinding when a relatively large amount of material shall be removed. The
wheel normally is of the recessed type see Fig. 6.10, the specimen holder being
pressedagainst the topsurface of the stone.
The grinding stones change during the process, the main problems being uneven
wear andclogging of the surface. The stone has to be truedregularly to keepthe surface
plane and dressed to remove material clogging the surface see Section 2.3.6. This is
usually done witha diamondtruing device placedonthe grinding machine.
Diamond Disks for Grinding of Very Hard Materials
Ceramics and other very hard materials have to be ground with diamond. This can be
grinding disks with a metal bond or a bakelite bond. The metal bond gives a relatively
rough surface of the specimen and the wear is relatively low. Bakelite bond produces a
specimen surface with less deformation but the wear is higher than by the metal bond.
Both types of diamond grinding disks are very expensive and only used for grinding of
sintered carbides, ceramics, and other very hard materials. In the past fewyears, a new
type of diamond disk with resin bonded xed grains has been developed. These disks
are considerably less expensive and suited for a wide scale of materials see Section
6.7.
Fig. 6.10Grinding stone for plane grinding, the grinding takes place on the top surface of
the stone.
6.6.2 SiC Wet Grinding PaperTable 6.2
SiC paper is the traditional grinding medium, used since the 1950s, both for plane
grinding and ne grinding. SiC grinding paper is made of a waterproof paper backing
with a layer of SiC abrasive grains. As shown in Fig. 6.11, an adhesive layer called the
make coat is rst applied to the backing before the abrasive grains are applied. As the
backing material passes through a strong electrostatic eld the particles are oriented
with their longest dimension in the vertical direction. This provides good grain reten-
tion and also orients the particles with their sharpest edges upwards. A second layer of
adhesive, calledthe size coat, is thenappliedover the entire assembly.
TABLE 6.2Comparison between Grit Numbers according to
ANSI Standard B74.18 and FEPA P Standard 43-GB.
FEPA
P
Standard
43-GB-
1984 R
1993
Approx. Average Grain
Diameter
FEPA P
m
ANSI
m
ANSI
B74.18-
2006
P60 269 268 60
P80 201 192 80
P100 162 141 100
P120 125 116 120
P150 100 93 150
P180 82 80 180
P220 68 67 220
P240 59
P280 52 52 240
P320 46
P360 41 42 280
P400 35 34 320
P500 30
P600 26 27 360
P800 22 22 400
P1000 18 16 500
P1200 15 13 600
P1500 13
P2000 10
P2500 (P2400) 8.4 6.5 (800)
(P4000) 5 5 (1200)
Fig. 6.11Schematic drawing of cross section of SiC grinding paper.
The paper backing can be of A-type, relatively thin, and C-type, which is somewhat
thicker. Type Cis normally usedfor metallographic/materialographic grinding. The pa-
per is supplied as disks in the diameters 200 mm 8 in, 230 mm 9 in, 250 mm
10 in, and300 mm12 in.
The SiC abrasive is classied according to standards established by ANSI Ameri-
can National Standard Institute and FEPA Federation of European Abrasive Produc-
ers. The grit sizes are split intotwocategories: macrogrits andmicrogrits.
Macrogrits ranging from grit 12 to grit 220 are determined by sieving, the grit
number indicating the number of openings per square inch. Macrogrits are the same in
the ANSI standard and the FEPA standard, the FEPA designation having a P before the
number.
Microgrits ranging from grit 240 to grit 4000 are determined by sedimentation,
and the grit numbers covering a specic grain size are not the same in the two stan-
dards see Table 6.2.
Comparison Between Standard GritsTable 6.2
In practical preparation a selection of grits is used. The suppliers of consumables for
metallographic/materialographic preparation supply both according to the American
and European Standards. In Table 6.2, the most commonly used grits are shown for
comparison P2400 and P4000 are not FEPA designations, 800 and 1200 are not ANSI
designations.
Plane Grinding
For plane grinding the grits 120 P120, 180 P180, 220 P220, or 240 P280 normally
are used. As mentioned above, the nest possible grit should be chosen to limit the de-
formation of specimen surface see below. When using SiC paper, the last plane-
grinding step should be grit 220 or 240 P220 or P280 to be sure of the correct result
reproducibility of the following preparation method. Considering that each sheet of
paper is only grinding efciently in 2060 s, depending on the material to be ground,
often several sheets must be used to secure a totally plane specimen surface co-planar
tothe grinding surface.
Fine Grinding
For ne grinding, three to four steps based onthe following grits are used typically: 280
P320, 320 P360, 360 P500, 400 P600, 500 P1000, 600 P1200, 800 P2400/
P2500, 1200 P4000. A normal ne grinding sequence could be 320400600 using
ANSI-designatedpaper or P320, P500, P1200using FEPAdesignatedpaper.
In the case of soft ductile materials, one or two ne steps can be added, 800, 1200
ANSI or P2400/P2500, P4000FEPA.
Material Removal
The material removal rate for SiC paper is relatively high as long as the paper is not
worn down. This is due to the abrasive grains being rather exposed and having a good
space in between, allowing for the chips to be produced and taken away by the water
ow. This is opposite to dry grinding on emery paper, which will very soon have a
cloggedsurface causing deformations andmaterial owinthe specimensurface.
Because of the brittleness of the SiCand the relatively high load on the grains, they
break down caused by fractioning and wear. In Fig. 6.12 this is shown schematically,
the SiC grains with different rake angles are broken and worn, creating new, negative
rake angles resulting in a loss of cutting action.
29
This develops in 2060 s or longer,
depending on the material to be ground, hard materials strongly reducing the time.
According to tests made by Samuels
7
the removal rate when grinding some metals like
copper and copper alloys, aluminum and aluminum alloys, silver and titanium stays
constant over a long period of time, and for some metals like nickel-chromiumausten-
itic steels, nickel andnickel alloys, titaniumalloys, chromiumandgold, a deterioration
in removal rate occurs in the rst minutes and is followed by a period of relatively high
material removal. These tests were based on a single specimen at a time, whereas in
modern preparation three to six specimens often are ground at the same time, conse-
quently reducing the lifetime of the paper.
In Fig. 6.13, an SEM micrograph shows the single grains of a 220 grit SiC paper
with the different shapes and sizes. Also the large variation in contacting points and
rake angles can be seen. At 220 grit, the median grain size is 63 m and the largest
allowed grain size is 74 m. Because of this large variation in shape and size, only
around 510 %of the many visible contacting points of the grinding paper actually get
in contact with the specimen surface. Only a fraction of these points are able to remove
material from the surface. Samuels
7
estimates that less than 1 in 1000 of the grains
visible can be expected to actually remove material. During the process when the SiC
grains break down, the cutting effect will change into plowing, shown in Figs. 6.3 and
6.14. At certainsoft, ductile materials, grains or parts of fracturedgrains canbe embed-
dedinthe specimensurface see Fig. 2.1andSection13.6.4.
Deformation
As shown in Section 6.3, a 220 grit SiC paper will induce a relatively strong deforma-
tion of the specimen surface. This is mostly because of the single large SiCgrains being
very aggressive in the rst seconds of the grinding process. Figure 6.14 shows a com-
parison between an SiC grinding paper and a grinding disk with diamond abrasive
grains in a resin bond. The situation after 25 s, a Fig. 6.14 shows the introduction of
Fig. 6.12Schematic drawing of grains on a SiC paper with different rake angles, as new and
after 3060 s use, the gray parts are worn away or fractured.
the deep deformations by the paper, whereas the grinding disk with grains embedded
ina bondgives more moderate deformation.
Edge RetentionRelief
In Section 3.1.3 edge retention is discussed, concentrating on mounting. Another im-
portant aspect is the resilience of the substrate, the surface, used for the grinding/
polishing. To totally avoid a rounding of edges, a hard substrate without resilience
must be used. SiC paper has some resilience because the paper backing has a certain
exibility, but in most cases a sufcient planeness can be obtained for most materials.
In more extreme cases, however, where edge rounding or relief, or both, must be abso-
lutely avoided, SiCpaper might have toomuchresilience. InFigs. 6.15 and6.16 grit 220
SiC paper is compared to a diamond grinding disk with the same grain size, having
almost no resilience. In Fig. 6.15, two unmounted, similar specimens are compared.
The specimen on the SiCpaper was rounded due to resilience of the paper backing; the
specimen on the diamond disk is not rounded due to the very lowresilience of the disk.
Even with mounted specimens, SiCpaper in certain extreme cases will create a round-
Fig. 6.13SEM micrograph of a P220 SiC paper. The irregular shapes of the grains and the
variety in grain size can be seen.
ing of the specimen or a relief of the specimen surface. In Fig. 6.16 a drawing of a me-
dium hard, nitrided steel, mounted in epoxy resin, is shown. When prepared on SiC
paper, the SiCparticles grind away the surface irregularly due to the highdifferences in
hardness between the nitrided layer and the core steel. Because of the limited differ-
ence in hardness between the nitrided layer and the SiC particles and the resilience of
Fig. 6.14Comparison of surface deformation using SiC paper and a resin bonded diamond
disk. After 25 s a single large grains of the SiC paper give deep deformations, after 30 s b
the SiC grains are wearing down, and after 60 s c the SiC grains are worn down creating
plowing, causing deformation, see Section 6.2.1. The diamond grinding disk gives less
deformation and remains almost constant during the process.
the paper backing, the layer protrudes above the surface of the specimen due to the
relatively low rate of material removal. The diamond disk cuts all parts of the surface
uniformly due to the extreme hardness of the diamond particles and the lack of
resilience.
EnvironmentEconomy
As mentioned above the efcient grinding time to a high degree depends on the speci-
men material and the number of specimens prepared at the same time. At soft and me-
dium hard materials the total plane and ne grinding might be performed with only
four sheets of paper, but at hard materials, especially with several specimens in a
holder, several sheets of each grain size must be used. In case of a high production of
specimens this is relatively costly and it will cause a relatively high amount of waste. As
a waste substance, the SiCpaper is neutral.
6.6.3 AluminaZirconia Alumina Wet Grinding Paper
Using alumina or zirconia alumina instead of SiC as the abrasive, a longer efcient
grinding time is obtained. The alumina grinding paper is available in grit 120 and the
zirconia alumina papers are available in the grits 60 P60, 80 P80, 120 P120, and
180 P180, and consequently they are only for plane grinding. Due to the longer ef-
cient grinding time they are especially suited for automatic preparation using speci-
menholders withmany specimens.
The inuence onthe specimensurface is as describedunder SiCpaper.
Fig. 6.15Comparison between SiC grinding paper and a resin bonded diamond disk. The SiC
paper has a relatively high resilience, and an edge rounding is introduced on an unmounted
specimen. The diamond disk has no resilience and gives no rounding.
6.7 Contemporary Grinding
Traditional grinding described in the previous section has a number of drawbacks,
especially when used for semiautomatic and fully automatic preparation. For this rea-
son contemporary grinding has been developed, in this way eliminating or reducing
the drawbacks:
Quality of specimensurface: Better edge retention, less deformation.
Constant removal rate: Fewer steps andhigher reproducibility.
Less handling: By using fewer steps, and using automatic preparation systems,
handling is reducedtoa minimumandoperationtime is saved.
Less waste: By using longer lasting consumables, the amount of waste is reduced.
In short it can be said that with contemporary grinding it is possible to prepare
specimens with extreme hardness differences as a routine process. These specimens
could only be prepared with great difculty using the traditional methods. The grind-
ing media used for contemporary grinding are almost all based on diamond as the
abrasive, either as xedbonded inthe surface of a rigidgrinding disk, or addedduring
the process on a rigid composite grinding disk rigid composite disk RCD. The prod-
ucts are supplied as disks in the diameters 200 mm 8 in, 250 mm 10 in, 300 mm
12 in, and350 mm14 in.
6.7.1 Magnetic Fixation
As part of the development of the products for advanced preparation, it was important
also to avoid the relatively troublesome handling of grinding papers and polishing
cloths with adhesive back. For this purpose magnetic systems were developed using a
Fig. 6.16Comparison of edge rounding and relief with a mounted specimen with a hard
surface layer prepared on SiC paper and a resin bonded diamond disk. At the SiC paper a relief
develops between the hard layer and the mounting material/basic material.
supporting disk with a permanent magnet foil on which the substrate, a grinding disk
or polishing cloth, made witha ferromagnetic backing, is xedsee Fig. 6.17. The hold-
ing power is very high in the direction parallel to the supporting disk, in this way keep-
ing the substrate onthe disk, but vertically the holding power is lowenabling the opera-
tor to easily remove the substrate. Afurther advantage is the use of only one supporting
disk for all grinding/polishing steps instead of changing the supporting disk for each
step. Normally the magnetic supporting disk is made especially for that purpose, but it
is possible to convert a normal metal grinding/polishing disk by placing a magnetic foil
with adhesive back on the disk. The drawbacks are an increase in the disk thickness,
and after some time, the foil might loosen due to attack fromliquids during the prepa-
rationprocess.
6.7.2 Resin-Bonded Diamond Grinding Disks
Section 6.6.1 describes conventional diamond disks. These have either a metal or
bakelite bond and because of the high price and careful maintenance truing is impor-
tant to keep the surface plane, they are only used for very hard materials, harder than
600 HV 55 HRC, where SiC and Al
2
O
3
are not hard enough. Diamond as an abrasive,
however, wouldbe ideal for grinding of softer materials.
In the past ve to ten years, a new type of diamond grinding disk has been devel-
oped, taking advantage of the hard diamond, but supplied at a reasonable price, which
matches the SiC grinding paper. The disk is suitable for materials harder than HV150.
The cost is kept lowbecause the diamonds are xed only in a thin layer in a resin bond
andplacedinsegments onthe surface of the diskas showninFig. 6.17
The gure shows howthe disk is xed to the supporting disk by a permanent mag-
net, as described above, but the disk can also be xed by a double adhesive foil placed
ona normal grinding/polishing disk.
The bondkeeping the diamondgrains, Fig. 6.18, is made sothat it allows the grains
to leave the surface when the grain is worn. The disk is used with water like SiC paper.
Using only a thin layer of bond with diamonds, the disk needs not to be trued, when the
layer is worn away at the center of the disk the disk is discarded, see Section 6.7.7 for a
more extensive description of this wear. Only a dressing of the surface with a dressing
stickis neededif the surface is clogged.
Plane Grinding
The disks are used for plane grinding, using the same grain sizes as for SiC paper, grit
80 P80 to 220 P220. Because of the constant removal rate see below the whole
grinding sequence can take place in one operation, even when much material shall be
removedandthe material has a highhardness.
Fig. 6.17Resin bonded diamond disk for magnetic xation on a support disk with a
permanent magnet.
Fine Grinding
The disks canalsobe usedfor ne grinding inthe grit sizes 360 P600 and600P1200.
Material Removal
The disks have a relatively high, constant removal rate securing that the grinding pro-
cess can be nished without interruptions. This is due to the high hardness of the dia-
monds andthe ability of the bondtobreakdown, releasing freshabrasive grains.
Deformation
The diamond grains, being of a more regular shape and with a closer tolerance of the
grain size than SiC grains, will produce less deformation than SiC paper, as shown in
Fig. 6.14. Also the position of the grains, placed in a bond see Fig. 6.18 gives less im-
pact when touching the specimen surface, creating less deformation. The segmented
surface, with grooves to lead away the swarf, is important to avoid smearing of the
specimensurface.
Edge retention, to a high degree depending on the resilience of the disk, is very good.
The resin bond is relatively hard and unexible see Figs. 6.15 and 6.16 and the very
hard diamonds are able to remove material even from very hard phases in the speci-
mensurface, avoiding relief
EnvironmentEconomy
The diamond disk as described above has very little environmental impact when dis-
carded. It only consists of a thin, tinned steel plate as used for canned food and a very
thinlayer of synthetic resin
Depending on the material to be prepared, one disk is equivalent to 100 sheets of
SiCpaper or more, making the cost comparable tothe cost of SiCpaper.
6.7.3 Resin-Bonded SiC Grinding Disks
The diamond disks described above are only suited for materials harder than HV 150.
Therefore, disks have been developed with SiC as an abrasive suited for softer materi-
als. In general, the above description of the diamond grinding disks also covers the SiC
grinding disks.
Fig. 6.18Resin bonded diamond disk. Diamond grains placed in a bond.
6.7.4 Metal-Bonded Diamond-Coated Disks
These types of disks are different from the conventional metal-bonded disks. The dia-
mond abrasive is placed in a very thin layer on a metal surface and bonded coated
witha layer of nickel.
These disks can be used for the softest to the hardest materials, but they are not
usedmuchbecause the cost per preparedspecimenis high.
6.7.5 Diamond Pads
This product, originally developed for grinding/polishing of glass, uses the diamond in
a metal or bakelite bondina dot matrix covering the surface of the pad.
The metal bond is only suited for plane grinding of ceramics, sintered carbides,
and other very hard materials. The grain size varies from 250 m in steps down to
20 m. The bakelite bond can be used for ne grinding of hard materials, being avail-
able ingrainsizes 30, 10, and2 m.
Dressing: It is important that the diamond pads are dressed regularly with a dress-
ing stick, normally Al
2
O
3
or SiC in a ceramic bond. This is to open the surface of the
diskwhenclogging has takenplace see Section2.3.6.
6.7.6 Diamond/CBN/Al
2
O
3
/ SiC Film
Inthe case of preparationof microelectronic devices, wafers, optical bers, andcertain
ceramics where extreme atness and very low deformation is needed, lms lapping
lms coatedwithdiamond, CBN, Al
2
O
3
, or SiCcanbe used.
The very accurately graded abrasive is coated on a thin polyester lm either for
gluing PSA or for adhering only using water plainback. The lms are usedwet or dry
and they are available bothwitha continuous layer of abrasive and withthe abrasive as
dots allowing the swarf to owaway. The lmwith dots ceramic beads gives a higher
material removal, a longer life, and a coarser nish, compared to lms with a continu-
ous layer.
The lms are available insteps from30 mdownto0.05 m.
6.7.7 Rigid Composite Disks
Since the 1970s, the rigid composite disk RCD has been available for materialo-
graphic preparation. The RCDhas the advantage of making very at specimens with a
constant removal rate and relatively little deformation, and this makes the RCD very
well suited for ne grinding of most materials. During the process on an RCD, a dia-
mond suspension is continuously added. This is known from lapping, a very common
abrasive machining process used in the industry to produce at surfaces. Normal lap-
ping takes place on cast iron disks and the surface obtained is not suited for
metallography/materialography see below. The surface of an RCDconsists of a resin
with mixed-in metal powder in different grain sizes, and it seems to be the effect of this
surface which changes the process taking place on an RCD, from lapping to grinding.
To explainthe mechanisms of anRCD, a comparisonwas made betweenlapping loose
grains on a glass disk, grinding on a diamond lm xed grains, and grinding on two
RCDs of different hardness.
30
Experiment: Lapping Versus Grinding
The scratch pattern of the specimen surface created with an RCDis similar to a surface
made with grinding paper, apparently ground, with grinding dened as a process with
xed abrasive grains, each grain acting as a machine tool producing a chip. This seems
strange because when using an RCD, the abrasive, mostly diamond with a grain size of
69 m, is added during the process. Normally these loose grains should create a lap-
ping, dened as a process with loose abrasive grains, rolling and owing in nearly a
single layer between specimen surface and disk, and not a grinding. At lapping, the
corner of the rolling grain digs into the specimen surface, the grain tumbles onto an
edge, and thenanother corner contacts the specimen, and so on. Lapping is considered
less appropriate for metallographic/materialographic preparation because the re-
moval rate is low, andthe specimensurface is rather strongly deformed.
Asteel specimen with a high nish was used for all parts of the experiment. Grind-
ing took place on a diamond lm, 9 m, to secure a perfect grinding. For the lapping a
oated glass disk with an alcohol/water diamond suspension was used with 9 m of
the same type of diamonds used on the lm, added during the process. The RCD pro-
cess was performed on two RCDs, RCD1 and 2, both of the disposable type see below
with the composite placed in segments on the disk surface see Fig. 6.27 below. RCD1
was withmetal powder composite relatively hardandaggressive, andRCD2 was with
a composite without metal powder, whichis relatively soft and withless aggressive ma-
terial removal. For bothRCDs the diamondsuspensionmentionedabove was used.
All the resulting surfaces were analyzedinanSEM.
The results showed that the specimen ground on the lm showed a typical grind-
ing pattern with scratches in all directions Fig. 6.19. To the naked eye the surface was
relatively bright.
The specimen lapped on the glass plate showed a typical lapping pattern with two
distinct features Fig. 6.20. The freely moving rolling diamond grains have made a
relief with cavities in the surface, and a few very large scratches have been produced,
probably due to single grains xedinthe surface of the glass disk. It canbe seenthat the
lapped surface is considerably rougher than the ground surface Fig. 6.19. To the na-
kedeye the surface was dull.
The specimen prepared on RCD 1 Fig. 6.21 has scratches very similar to the
Fig. 6.19Pattern of scratches and deformations after grinding on a diamond lm. SEM.
scratches initiated by grinding Fig. 6.19, only a little larger. The surface is reasonably
plane betweenthe scratches. Tothe nakedeye the surface was relatively bright.
The specimen prepared on RCD 2 Fig. 6.22 has almost the same scratch pattern
as at grinding Fig. 6.19. It is ner thanthe RCD1 patterndue tothe fact that RCD1 is a
more aggressive RCD. This also can be seen fromthe removal rates see belowand Fig.
6.23. Tothe nakedeye the surface was relatively bright.
The conclusion of the SEM analysis is that according to the scratch pattern, the
same process takes place when grinding on a lmwith xed diamond grains and on an
RCDsurface withloose grains addedduring the process.
The removal rate was also measured, dened as material removal inmper 300 m
movement of specimen on the grinding/lapping surface see Fig. 6.23. It can be seen
that the diamond lmis very active during the rst approximately 50 m and wears out
after approximately 250 m. The glass disk has a relatively constant removal rate during
the whole distance and the same is the case with the two RCDs. This is because the
abrasive is added during the whole process. The aggressive RCD 1 shows a higher re-
moval rate thanthe other three surfaces.
Based onthe above experiment, a suggestionfor the mechanisms taking place dur-
ing the processes was made anda model proposed.
Lapping ona hard, homogenous disk: It is beyond doubt that the process withroll-
ing grains makes indentations in the specimen material, in this way breaking particles
out of the surface Figs. 6.20 and 6.24. A fractured, indented, dull surface can be seen
only with a few scratches. A few grains will penetrate into the surface of the disk and
produce a scratchlike grainb inFig. 6.24.
Process on an RCD: On an RCD the surface is very much softer than the sample
material. This means that the abrasive grain is pressed into the disk surface so that a
rolling is prevented and a process, creating chips like at grinding, takes place. Only a
very small number of grains are rolling see Fig. 6.25. According to Samuels
7
it seems
that the abrasive grains embed in the upper regions of the edge faces of the segments
where they cancontact the specimensurface.
Fig. 6.20Pattern of scratches and deformations after lapping on a glass plate. SEM.
At RCD 1, the surface consists to a high degree of metal powder Fig. 6.25. This
gives a variation in surface hardness, and the abrasive will penetrate differently into
the surface, less inthe metal particles. This means that the grainis able tomake a larger
chip, counting for the higher removal rate of RCD1. Inthe case of RCD2 witha consid-
erably softer surface, the abrasive grains penetrate deeper into the disk resulting in a
smaller effective diamondsize, andthe abrasive is heldmore rmly, whichis important
whengrinding ductile materials.
Rigid Composite Disks RCD for Longtime Use
The original RCDs were made as solid disks with a thick layer of composite material,
consisting of a synthetic resin with mixed-in metal powder iron, copper, or a mineral
powder like Al
2
O
3
. The surface can be with segments of different composites and with
grooves of different types toremove the swarf during the process.
The disks can be used for plane grinding with 3045 m, but they are mostly used
for ne grinding with 6 to 9 m diamond suspension added during the process. The
process has to run relatively dry, with a minimum of lubricant added during the pro-
cess. As the disk surface texture turns smooth during use, a dressing is necessary with
intervals toregaina roughsurface andthereby secure the removal rate.
The disks are difcult to use for hand preparation and are normally used with a
semiautomatic specimen mover see Section 6.8. Most specimen movers work with
the specimen holder placed eccentrically on the grinding disk see Polishing Dynamics
Section 7.9.2. This eccentricity causes a wear concentrated around the center of the
disk, making it concave Fig. 6.26. This unevenness will, when exceeding
100200 m, cause an unevenness of the specimens and the effect of the disk will be
reduced. The concave surface must be trued to regain the planeness and this is mostly
done witha truing tool using diamond. Due to this rather laborious truing, many RCDs
were not usedandthe use of SiCpaper was preferred.
The development of the thin, disposable RCDchangedthis situation.
Fig. 6.21Pattern of scratches and deformations after grinding on a hard rigid composite disk
RCD. SEM.
Rigid Composite Disk, Disposable
Taking into consideration the advantages of the RCD, it was evident that an RCDwith-
out the drawbacks mentioned above, and even compatible with SiC paper, should be
developed.
This was done with the disposable RCD, consisting of a tinned steel foil or a steel
plate with segments of composite material. This is xed magnetically to a supporting
disk witha permanent magnet Fig. 6.27. The disposable RCDis made intwo versions,
one relatively aggressive for materials harder than 150200 HV and a softer one for
softer materials inthe 40250 HVrange andfor composite materials.
Plane Grinding
The disposable RCDis normally not suited for plane grinding because it should not be
used with diamond grain sizes larger than 15 m. In some cases, however, when work-
Fig. 6.22Pattern of scratches and deformations after grinding on a soft rigid composite disk
RCD. SEM.
Fig. 6.23Comparison of removal rates of specimens after grinding on a diamond lm,
lapping on a glass plate and grinding on a hard and a soft RCD.
ing with single-specimen preparation, see Section 7.9.1 the amount of material to
remove at this stage is so lowthat grinding with a hard RCDusing 9-m diamond sus-
pensioncanbe considereda plane grinding.
Fine Grinding
The disposable RCDis made for ne grinding with diamond suspension 9, 6, or 3 m.
The total ne grinding stage can be performed usually in only one step in 24 min and
the specimenis ready for the rst polishing step.
Material Removal
The removal rate is considerably higher than at a conventional RCD. This is mostly
because the disposable RCDworks at a higher specic pressure and the removed mate-
rial swarf is efciently removed through the channels between the segments. Also, it
Fig. 6.24Schematic drawing of a lapping process. The abrasive grains are loose and rolls
between the specimen and the lapping disk. A corner of the grain digs into the specimen
surface, and the grain tumbles onto an edge. A track of angular indentations cavities is
produced in the specimen surface.
Fig. 6.25Schematic drawing of a material removal process on a rigid composite disk RCD.
The majority of the abrasive grains are xed in the surface of the disk grinding; only a small
amount is moving lapping.
shall not be dressed during use, but keeps its surface texture during the whole lifetime,
securing a constant removal rate. The material removal varies with material type and
type of RCD. The hard, more aggressive type has the highest removal rate see Fig.
6.23.
Deformation
Using diamonds 96 m with a narrow tolerance on the relatively exible RCD sur-
face, the grain, momentarily xed in the surface, will not have the same damaging im-
pact on the specimen surface as with xed grains SiC paper. Also, by varying the
amount of metal in the composite, the aggressiveness of the surface can be minimized
whichis very important withsoft materials.
The composite material, although microexible, will be rigid and plane as a total sur-
face. This, together with the high cutting capacity of the diamond grains, will give a
very goodedge retentionandpractically norelief.
Wear
As described earlier, an RCD turns concave during use see Fig. 6.26. To avoid the
troublesome truing of the surface, the disposable RCDis discarded when the segments
around the center of the disk are worn away, showing the user that the difference in
planeness between periphery and center is so high that uneven specimens will be
produced.
Fig. 6.26Wear pattern of grinding/polishing disk. Due to the geometry of disk and specimen
holder, the wear around the center of the disk is stronger than at the periphery, causing a
concave disk surface, after a certain preparation time.
EnvironmentEconomy
The disposable RCD can be compared with a piece of tin plate or a thin stainless steel
plate witha layer of paint, andit canbe disposedof like a normal tincanor metal piece.
The price per specimenusing the RCDdepends onthe material to be prepared, but
at normal use more than100specimenholders canbe preparedonone RCD.
6.7.8 Fine Grinding Cloths
When using very hard cloths, absolutely without nap, like nonwoven chemo textiles
and nylon, with diamond suspension or spray/paste of a grain size of 9 m or larger,
the process canbe denedas ne grinding if the pressure onthe specimenis high.
Polishing can be dened as grinding producing very small chips and is explained
further inChapter 7. Inthe above-mentionedcase, however, a material removal similar
togrinding canbe obtained.
The materials used for the ne grinding cloths are stainless steel mesh, woven
polyester, woven silk, woven nylon, and nonwoven synthetics. These are all without
napandusedwith15, 9, 6, or 3 mdiamondsuspensionor spray see Section7.4.
With the introduction of rigid composite disks RCDs for soft materials see Sec-
tion6.7.7, the use of these cloths has beenreduced.
Material Removal
The removal rate is not as high as with an RCD, but higher than at a normal polishing
step.
Deformation
The deformation is much lower than at grinding on a disk with xed abrasives. It is
comparable tothe deformationcreatedby anRCDsee Section6.7.7.
Due to the relatively high resilience of the cloths, except the steel mesh, a certain edge
rounding andrelief might develop.
EnvironmentEconomy
All materials mentioned above can be discarded as normal waste; the cost per speci-
menis comparable toSiCpaper.
6.8 Grinding/Polishing Equipment
Mechanical grinding and polishing are normally performed on the same type of ma-
chines.
Fig. 6.27Disposable rigid composite grinding disc RCD magnetically xed to a support disc
with a permanent magnet.
Only in a few cases machines only for grinding mostly plane grinding are sup-
plied. For this reason only equipment that can be described as grinders are included
inthis section. The grinders/polishers are describedinSections 7.8and7.9.
6.8.1 Plane Grinding
Manual Grinding
Plane grinding using grit 220 240 or coarser can be done by hand on a rotating disk of
a 200- 250- 300 mm 8- 10- 12 in diameter disk with a grinding paper. The paper can
be placed with a plain back in a water-lled disk, and the paper is sucked to the disk
when rotating due to the centrifugal force, which moves the water to the outside of the
paper. The paper may also have a self-adhesive backing or a double-adhesive foil canbe
used.
For the technique of manual hand grinding see Section13.2.4.
Fig. 6.28Polisher/grinder with two disks 200/ 250 mm 4/ 6 in diameter and 300 rpm for
manual preparation.
20
Fig. 6.29Belt grinder with two workstations for coarse grinding. Adjustable water ow and
sink.
19
Machines with one or two disks are available and used for both grinding and pol-
ishing; two disks can be of advantage when using four steps for grinding with SiC pa-
per. Figure 6.28 shows a two-disk grinder/polisher 250 mm10 in disk diameter with
a single speed, 300 rpm, for handgrinding onSiCgrinding paper.
For a more effective grinding by hand, a belt grinder can be used, built with one or
two work stations. The belt grinder works with a belt moving on two rolls and with a
ow of water; it can be used for both plane and ne grinding. Figure 6.29 shows a belt
grinder withtwoworkstations, water owsystemandsink.
Automatic Grinding
Plane grinding of specimen holders with six or more specimens can be done on most
automatic systems, whichare describedinSection7.9.
At very large holders withlarge specimens, it canbe anadvantage toplane grindon
Fig. 6.30Semiautomatic grinding machine grinding stone for plane grinding with specimen
holders. Diameter of grinding stone 356 mm 14 in, 1450 rpm.
20
a grinding stone with a relatively high speed 1450 rpm and a diameter of 356 mm
14 in. The machine, shown in Fig. 6.30, is only for plane grinding and ne grinding/
polishing must take place onanother automatic grinder/polisher.
6.8.2 Fine Grinding
Manual Grinding
Fine grinding by hand takes place on equipment spanning fromsimple apparatus with
four strips of grinding paper Fig. 6.31, to rotating grinder/polisher as mentioned un-
der plane grinding Fig. 6.28. Figure 6.31 shows a four stage hand-grinding apparatus
withfour strips of SiCgrinding paper suppliedfromrolls for plane andne grinding.
Automatic Grinding
Fine grinding of specimen holders either with a number of xed specimens central
force or individually loaded single force takes place on semi- or full-automatic
grinders/polishers describedinSection7.9
Automatic grinding/polishing systems have gained ground because they reduce
the work load on the metallographer and produce an overall better specimen quality.
Also, the reproducibility is improved, securing that if a certain method is followed, the
result always is consistent.
Fig. 6.31Four stage hand-grinder for wet grinding on four strips of grinding paper in rolls.
19
7
Mechanical Surface
PreparationPolishing
7.1 Polishing: Producing the True Structure
AFTER PLANE GRINDING AND FINE GRINDING THE SPECIMEN SURFACE
must be polished to obtain the true microstructure or a structure, which is satisfactory
for a given analysis. In principle, the surface always will have a certain deformation
artifacts, but if not too deep this can often be removed through the etching of the sur-
face see Chapter 9. For a thorough description of artifacts and howto avoid them, see
Section13.5/6.
This chapter covers mechanical polishing and chemical mechanical polishing
CMP. Electrolytical andchemical polishing are describedinChapter 8.
Mechanical polishing is dened as a material removing process with loose abra-
sive grains placed on a substrate like a polishing cloth. The abrasive can be added be-
fore or during the process and normally lubricant is applied during the process for lu-
bricationandcooling.
CMP can be dened as a material removal process where the material removal
takes place chemically andmechanically at the same time see Section7.12.
Mechanical polishing is by far the most usedprocess, anddepending onthe type of
material and the nature of the preceding ne grinding step, one or several polishing
steps are neededsee Fig. 1.7.
7.1.1 Rough Polishing
This step immediately follows the last ne grinding step and is usually done on a hard,
napless clothwith9 or 6 mdiamond. This stepcanbe comparedto the last stepof ne
grinding done on a hard, napless cloth see Section 6.7.8. The rough polishing step is
very important because most of the material, damaged by the grinding, is removed in
this stepsee Table 7.1.
7.1.2 Polishing
The polishing is done in one to three steps with hard, mediumhard, or soft cloths with
diamond30.25 mor ner polishing media, suchas silica andalumina, 0.10.05 m
see Section7.5, depending onthe material tobe polished.
7.2 Material Removal
The process of material removal during polishing, micromachining, is considered to
be the same as it is during grinding see Section 6.2. According to Samuels
7
it seems
that another mechanism, delamination, takes place when polishing with diamond
abrasives below 3 m. Delamination does not produce the elongated chips that result
frommicromachining, but small, plate-shapedequiaxedparticles are produced. Noex-
120
planations have been advanced for the mechanismby which delamination occurs dur-
ing the polishing withthe smallest grainsizes.
At micromachining, the abrasive grain is able to produce a chip, implying that the
grain is, at least momentarily, xed in the polishing cloth, as shown schematically in
Fig. 7.1. The diamondgrainwedges betweenthe clothbers witha rake angle sufcient
to be able to cut a chip from the specimen surface. To obtain a high removal rate at
rough polishing, hard cloths are used, creating a higher load on the grain, giving a
larger chip. Using softer, more resilient cloths for the nal steps, the load onthe grainis
reduced, causing smaller scratches andless deformationof the specimensurface.
7.2.1 Inuence of Polishing Abrasive on Removal Rate
For grinding, the hardness of the abrasive is important. Therefore, diamond is used for
both rough polishing and polishing. For nal polishing, alumina Al
2
O
3
, colloidal
silica SiO
2
, andmagnesia MgO are alsoused.
Likewise, the shape of the grain plays a role. Polycrystalline diamonds give a
higher removal rate than monocrystalline diamonds,
7
probably because the individual
polycrystalline grain contains more angular points of the size needed to provide cut-
ting points thanthose of monocrystalline.
In principle, the removal rate increases linearly with the increase in specic pressure
betweenspecimensurface and the polishing surface once a certainlowthreshold value
has been exceeded. Using a high force causing a high specic pressure might create a
rounding of the specimen, and often the lubrication will not be satisfactory and heat
might develop. Also, an increased wear of the polishing cloth will take place. For nap-
less, hard cloths the specic pressure should be in the range of 30 to 100 kPa
4.35 to 14.5 psi; for softer cloths the pressure should be 15 to 50 kPa 2.2 to 7.25
Fig. 7.1Schematic drawing of an abrasive grain xed in a ber of a polishing cloth.
Chapter 7 Mechanical Surface Preparation 121
psi. Experience has shown that in specimens from 40 mm 1.5 in diameter and up,
the force per specimen should not exceed 50 N 11.5 lbf to avoid overheating of the
cloth and excessive wear. To compensate, the polishing time may be extended
1 to 4 min.
7.3 Deformation
Polishing, as mentioned earlier, in principle being the same process as grinding, will
produce shallower deformed layers. With hard cloths with a low resilience, a stronger
deformation will develop than with softer cloths. The depth of the deformed layers is
an order of magnitude smaller than that on surfaces ground with SiC paper, as shown
by Samuels
7
see Table 7.1. This shows the importance of the rough polishing step
6 mdiamond.
For explanations of D
sb
, D
s
, andD
d
see Section6.3.1.
In theory, even the nest abrasive will create a deformed layer. It is, however, pos-
sible to obtain a surface very close to the true structure with the use of very ne abra-
sives like alumina Al
2
O
3
and silica SiO
2
for the nal polishing step. Silica, having a
carrier liquid with a pHin the range of 8.5 to 11 see Section 7.5.5 and a grain size of a
fraction of a micron, will create a combined mechanical and chemical material re-
moval see Section7.12.
Deformation in the formof smearing can take place with soft metals, the material
being smeared across the surface. For this and other types of deformation, see Section
13.6.
In the literature, the very thin deformed layer left by the last polishing step is often
called the Beilby Layer. The existence of such a layer is not supported by recent re-
searchandthe use of this termshouldbe avoided; however, to give animpressionof the
mechanisms taking place, a short description of the theories by Beilby
31
and Samuels
7
will be giveninthe following section.
7.3.1 The Beilby Layer
At the beginning of the 20th century, Sir George Beilby established the theory of the
so-calledBeilby layer. This layer was proposedtobe of anamorphous nature createdby
a smearedlayer that hadpassedthroughthe liquidstate Fig. 7.2.
31
The layer would ll out the existing scratches and give the surface its mirror-like
character. The layer was thought to have developed due to the very high temperatures
TABLE 7.1Depth of the Plastically Deformed Layer. Annealed Polycrystalline 30 % Zn Brass by Manual
Grinding/Polishing.
Abrasive Grade m/ Grit
Scratches/
Dsb, m Ds, m Dd, m
SiC paper 220 2.0/- 7.5 77
SiC paper 400 1.5/- 6.5 43
SiC paper 600 0.8/- 5.0 22
Diamond 6 0.08/ 0.17 1.0
Diamond 1 0.05/ 0.1 0.7
Alumina, -type 01 2.5
Alumina, -type 00.1 0.03/- 0.7
attained at the points where an abrasive grain touches the specimen surface. This high
temperature, being close to the melting point, would cause the material to melt or be-
come very plastic.
According to Samuels
7
the layer, which Beilby considered amorphous and could
be removed by etching, a phenomenon known to most metallographers, is simply de-
formed material still remaining on the surface see Fig. 7.3. When the original scratch
and most of the deformation below the scratch is removed, the polished surface looks
perfect. After etching, the deformed material is etched preferentially and the original
scratch seems to reappear. This was supposed by Beilby, but what reappears is not the
scratch, but anartifact createdby the scratch. It couldbe calleda scratchtrace.
7.3.2 Inuence of Polishing Abrasive, Cloth, and Fluid on Deformation
Deformation will decrease with a lower abrasive grain size as shown in Table 7.1. The
type of abrasive will play a role, diamond grains, especially on soft materials, will give
more scratches than -type alumina and silica; therefore, the small grain sizes of dia-
mond1, 0, 25 m are not usedfor the nal polishing of softer materials.
Hard polishing cloths, without nap, will normally create more deformation than
napped cloths; however, napped cloths might create other artifacts like relief and
rounding of phases andedges.
The polishing uid is very important for lubrication, cooling, and removal of
swarf. The lubrication is necessary to obtain a reduced friction between the cloth and
Fig. 7.2Beilby layer, diagrammatic section of a calcite plate across the line of ow. The
owed material has completely lled up even the deepest scratches.
31
Fig. 7.3Schematic drawing of Beilby Theory and Local Deformation Theory.
7
the specimen surface. The type of lubricant gives different lubricating effects, the oil-
based lubricants giving the strongest effect, recommended for softer materials. The
water-based type gives a mediumeffect suited for general purpose use, and the alcohol
type gives a low effect suited for brittle materials. The oil-based lubricants also give a
thin surface lm on the cloth that minimizes the damaging effect from the cloth, im-
portant for soft materials. The cooling effect of the lubricant is important when many
specimens at a time under a relatively high pressure are polished. The alcohol- and
water-based lubricants cool most efciently; the water-based type is preferred. In ex-
treme cases, with many specimens with high pressure and a large disk diameter, a spe-
cial disk cooling, usually with water, might be necessary to keep the temperature low
enough. When using rigid composite disks RCD it is important to have an efcient
removal of swarf to prevent it fromdamaging the specimen surface. To a lesser degree,
this is the case withhardcloths andevenless onsoft cloths.
7.4 Polishing Cloths
Polishing cloths can be dened as substrates upon which a polishing medium is ap-
plied to performa polishing process. The polishing cloth is supported by a rigid polish-
ing disk made of metal or a polymer. As described in Section 7.2, the abrasive grain
should, at least momentarily, be xed by the cloth, making material removal possible.
The xing of the abrasive canbe done inseveral ways, depending onthe structure of the
cloth. For hard cloths, the abrasive grains will be placed on the surface of the cloth,
placed in hard bers, securing a more aggressive attack, whereas on a soft cloth, the
grains will penetrate into the nap of the cloth, and a less aggressive material removal
will take place. Consequently, the cloth is a very important factor regarding material
removal, but also the deformationdeveloped during the process and the edge retention
andrelief are strongly inuencedby the cloth.
The termpad is often used for certain polishing cloths made of nonwoven material
see below, but inthe following clothis usedas the general term.
Apolishing clothcanbe characterizedthroughthe following:
Material: All kinds of exible materials can be used. The most used are: Chemotex-
tiles, nonwovenmaterials, wovennylon, wovenacrylates satin, wovensilk, woven
wool, a backing oftencotton withsynthetic ockednap.
Surface Structure: The material can be smooth, porous, perforated, woven, or
ockednap. The ockedcloths always have a nap, but other types also might have
a nappedsurface. The napnormally will give the clotha highresilience see below,
but with certain cloths a high nap will lay down during use and create a compact,
smooth surface with a relatively low resilience. The surface structure might
strongly inuence the polishedsurface see below.
Resilience: The resilience, the elasticity of the cloth in the vertical direction, dic-
tates whether a cloth is hard or soft. All cloths can be compressed when subject to
pressure fromthe specimen. Aclothhaving a lowresilience is hard and a clothwith
a high resilience is soft. A hard cloth, which can only be slightly compressed, will
usually give a high material removal and create deep scratches and more damage
to the specimenthana soft cloth. Two cloths, however, withthe same lowresilience
can perform differently caused by the surface structure of the cloth. Figure 7.4
shows an aluminum/silicon specimen polished on a very hard cloth with an un-
smooth, wovensurface, showninFig. 7.6; the deformations inthe Al / Si surface are
strong. Figure 7.5 shows the same specimen polished on a cloth with the same re-
silience, but with a relatively smooth, woven surface, shown in Fig. 7.8, the defor-
mations are considerably reduced. A soft cloth with nap will normally have a rela-
tively lowmaterial removal and create little deformation and small scratches. The
nap will make an edge rounding. Also, because of the brushing effect the bers of
the nap brushing the specimen surface, a relief might develop if the specimen sur-
face has phases of different hardness; the softer phase being preferably removed.
Polishing cloths are xed to the supporting grinding/polishing disk with a self-
adhesive backing PSA or through magnetism established by a steel foil integrated in
the cloth see Section 6.7.1. Cloths can also be xed by using a retaining ring that
stretches the cloth over the disk. This often causes wrinkles of the cloth and should be
avoided.
Polishing cloths are supplied in the following diameters: 73 mm2.9 in, 102 mm
4 in, 200 mm 8 in, 250 mm 10 in, 300 mm 12 in, 350 mm 14 in, and 400 mm
16 in. For a table of available polishing cloths, see Section13.2.2, Table 13.1.
Fig. 7.4AlSi material after polishing with 3 m diamond suspension on a very hard cloth with
a very irregular surface structure. The surface has deep scratches and strong deformation. The
cloth is shown in Fig. 7.6. BF.
Fig. 7.5The same material as in Fig. 7.4 after polishing with 3 m diamond suspension on a
hard cloth with a smooth surface structure. The surface has considerably less scratches and
deformation although the abrasive is the same. The cloth is shown in Fig. 7.8. BF.
7.4.1 Edge RetentionRelief
As described in Section 3.1.3 and Sections 6.6.2/6.7.7, edge retention is often very im-
portant and development of a relief should be avoided. The sections mentioned earlier
and Figs. 6.15 and 6.16 describe howthe resilience, the vertical exibility of the prepa-
ration substrate, is decisive for the development of edge rounding and relief. It is evi-
dent that when using a cloth with a relatively high resilience as substrate, the risk of
edge rounding and relief will increase strongly. This means that a good ne grinding,
either on SiCgrinding paper or on rigid composite disks, might be spoiled if the polish-
ing cloths used for the following steps have a too high resilience or the polishing times
are too long, or both. It is important that cloths with the lowest possible resilience to
obtain a satisfactory result are used and the times are kept at a minimum. The charac-
teristics regarding edge retention and relief will be discussed further for the single
cloths below.
7.4.2 Cloths for Fine Grinding and Rough Polishing
These cloths are all hard with very lowto mediumresilience. Although primarily used
for ne grinding and rough polishing, some of the cloths can also be used for nal pol-
ishing of medium hard and hard materials. They are typically used with diamonds
from151 m.
Fig. 7.6Napless, very hard, woven, coated polyester cloth for ne grinding/rough polishing.
SEM.
Fig. 7.7Napless, hard, non woven, synthetic cloth for ne grinding/rough polishing. SEM.
All cloths for ne grinding androughpolishing, except the wovensteel cloth, will have a
low, often very low, resilience, which theoretically will cause an edge rounding of the
specimen. In practice, however, if the preparation time is kept inside reasonable limits,
the edge retentionis highwiththese hard cloths, which, used withdiamond as anabra-
sive, give a goodatness without relief.
Cloths
Woven Steel: This is a cloth made of stainless steel wire mesh. The resilience is close to
zero and consequently the edge rounding is very low. The cloth is used for ne grinding
with156 mdiamondfor hardmetals, ceramics, andcomposites.
Woven Coated Polyester Fig. 7.6: A napless, very hard, coated polyester cloth for
use with 153 m diamond for ne grinding/rough polishing of metals, composites,
ceramics, andhardmetals. The resilience is very lowgiving very little edge rounding.
Nonwoven Textile Fig. 7.7: A napless perforated/not perforated nonwoven cloth
for use with 153 m diamond for ne grinding/rough polishing of harder materials
and softer materials depending on the resilience of the cloth. On cloths with a certain
resilience, anedge rounding may take place after prolongedpolishing.
Woven Nylon Fig. 7.8: A napless cloth for use with 91 m diamond. Medium
hard and suited for roughpolishing and polishing of ferrous materials and cast irons to
retain inclusions/graphite and maximize atness. The very low resilience gives very
little edge rounding.
Woven Silk Fig. 7.8: A napless cloth for use with 91 m diamond. Hard and
suited for ne grinding/rough polishing and polishing of most metals, coatings, and
plastics. The lowresilience gives goodatness andvery little edge rounding.
Woven Synthetic Silk Acetate Fig. 7.8: A napless cloth for use with 31 mdia-
mond. Hard and suited for rough polishing of most metals to maximize atness with
very little edge rounding andretentionof hardphases.
7.4.3 Cloths for Polishing
These cloths have medium to high resilience and are used for one or more polishing
steps, an intermediate step or a nal step. They are used with diamond in the
60.25 m, mostly from31 m. Also, some can be used for oxide polishing see Sec-
tion7.5 for the nal step. Some of these cloths are napless; some have naps of different
height andstructure.
Fig. 7.8Napless, hard, woven nylon, silk or acetate cloth for ne grinding/polishing. SEM.
The polishing cloths, having medium to high resilience and often a nap, will cause an
edge rounding of the specimen, depending on the preparation time and force on the
specimen. As a rule the polishing time should be kept as short as possible, with most
time used ona napless cloth, whichgives less rounding, and less time used ona napped
cloth, oftenonly for a short nal polishing. The force onthe specimenshould be kept as
low as possible, especially on napped cloths. In general, the napless polishing cloths
will not develop a relief, but the napped cloth might develop relief if phases of different
hardness are present inthe specimensurface.
Cloths
Woven Wool Fig. 7.9: A napless, soft cloth with medium resilience for use with
61 m diamond. It is suited for polishing and ne polishing of minerals, glass, met-
als, composites, coatings, and polymers. An edge rounding might develop, but it will
usually be acceptable. Norelief will developexcept inextreme cases.
Synthetic Nap on Woven Backing Fig. 7.10: Acloth with a mediumnap of ocked
bers on a cotton backing for use with 60.25 m diamond, alumina, and silica see
Section 7.5. This cloth is for general usage for nal polishing. The nap and backing
give a very high resilience that will cause rounding of the edges of the specimen surface
and often create a relief because of the brushing effect see Section 7.4. For these rea-
Fig. 7.9Napless, medium hard, woven wool cloth for polishing. SEM.
Fig. 7.10Medium napped, soft, with synthetic bers ocked on a backing, cloth for polishing.
SEM.
sons the cloth should only be used for a short time to establish the nal specimen sur-
face.
Synthetic NaponNonwovenBacking: Asoft clothwitha dense napwithhighresil-
ience tobe usedwith31 mdiamond. It is suitedfor one-stepor nal polishing of soft
to hard ferrous and nonferrous metals. The dense nap gives relatively good edge reten-
tioninspite of the highresilience andnorelief.
Synthetic Porous Material Fig. 7.11: A soft, napless cloth with high resilience.
The synthetic material neoprene is chemically resistant and will take up the very ne
alumina and silica suspension in the pores, and it is used with oxide suspensions
0.020.05 msee Section 7.5. The cloth is suited for the nal step for most materials.
The time should be short to avoid edge rounding. The risk for a relief is very little, but a
certain relief might develop because of a chemical mechanical attack from the polish-
ing medium.
Woven Felt: A soft, napless cloth with very high resilience used for 91 m dia-
mond, alumina, and silica see Section 7.5. It is suited for rough and nal polishing of
hard metals, cast iron, and mild steels, preserving inclusions. The high resilience will
cause edge rounding andpossibly relief.
7.5 Polishing Abrasives
The polishing abrasives are usedinconnectionwitha polishing clothfor the steps from
rough polishing ne grinding to the nal polishing step. In general, diamond is used
for all steps except the last step nal polishing step. In case of harder materials, dia-
monds, down to 0.1 malso cover the nal step, but often, especially with softer mate-
rials and composites, a nal cleaning step is made with an oxide, normally silica SiO
2
or alumina Al
2
O
3
.
7.5.1 Diamond Suspensions
Diamondsuspensions are describedinSection6.4.
7.5.2 Diamond Spray
Diamondspray is describedinSection6.4.
Fig. 7.11Napless, soft, porous synthetic cloth for polishing with silica and alumina and for
chemical mechanical polishing. SEM.
7.5.3 Diamond Paste
Diamondpaste is describedinSection6.4.
7.5.4 Alumina
Alumina Al
2
O
3
has been the classic polishing medium in metallographic/material-
ographic preparation. Earlier it was used for all polishing steps, often causing bad re-
sults, because the removal rate is very low. In modern preparation, alumina should
only be usedfor the nal polishing steps ingrainsizes 10.05 m.
Alumina is available as suspensions and powders withtwo crystal types, alpha and
gamma. The alpha crystal has relatively sharp edges giving the highest removal rates,
whereas gamma is more rounded, causing a very small removal rate suited for the last
polishing step.
Both powder and suspension can be supplied in agglomerated and deagglomer-
ated condition. In agglomerated alumina the particles will form agglomerates Fig.
7.12 because of the electric forces between the particles. These agglomerates will give
a higher removal rate and might cause scratches in the specimen surface, although
they are normally broken down during the polishing. In the deagglomerated alumina
the material is treated to avoid the agglomerates so that only the single particles will be
active Fig. 7.13, ensuring anultrane specimensurface.
Alumina is available ingrainsizes from50.05 m.
Fig. 7.12Alumina, agglomerated, the large agglomerates can be seen.
Fig. 7.13Alumina, deagglomerated.
Suspensions
These are ready for use either in diluted or undiluted condition. In some cases the sus-
pension is stabilized so that the alumina does not come out of suspension when not
used. This is anadvantage if usedinautomatic dispensing systems see Section7.9.3.
Alumina can be mixed with silica see below to form special polishing
suspensions.
Powders
Powders have to be mixed with distilled or demineralized water to forma suitable sus-
pension. In special cases, if water is not allowed for the preparation, the powder can be
mixedwithother uids like glycerine or alcohol.
7.5.5 Silica
Originally developed for the preparation of silicon wafers, colloidal silica SiO
2
in a
suspension has gained ground in metallographic/materialographic preparation. The
grain size is very small, 0.10.02 m, and the grains are almost spherical and softer
than alumina, causing a very lowmechanical material removal making SiO
2
very well
suited for the nal polishing step. By comparing the microstructures of an aluminum-
silicon alloy Figs. 7.14 and 7.15, the effect of silica can be recognized. The strong de-
formations from the 3 m diamond polishing as shown in Fig. 7.14 are removed and
bothmatrix andsiliconare perfectly polished, see Fig. 7.15.
For wafers and many other materials, the colloidal silica suspension works ac-
cording to a chemical mechanical polishing CMP process. The suspension, having a
pHbetween 8.5 and 11, plays an important role in the material removal mechanismin
CMP.
32
The CMPgives SiO
2
suspensions and suspensions based on SiO
2
and other oxides,
like iron oxide, an increased removal rate on ceramic materials and metal/ceramic
composites anda number of metals see Section7.12.
A CMP can be established also when mild chemicals like hydrogen peroxide
H
2
O
2
and an ammonia NH
3
solution are mixed into the suspension; this will be de-
scribed under each material in the Material/Preparation Tables, Section 13.2.3. In this
way, very soft andductile materials canbe mechanically polishedtoa deformation-free
Fig. 7.14AlSi surface after polish with 3 m diamond suspension, strong deformations in
both matrix and silicon phase. BF.
nish, avoiding electropolishing. Colloidal silica is available only as suspensions witha
pH8.511andgrainsizes from10.02 m.
Attention: A colloidal silica suspension should not be allowed to dry on the polish-
ing cloth, because it will then be unusable. The polishing cloth shall be carefully
cleaned after use to avoid dried-in crystals which will cause scratching of the specimen
surface. It canbe of advantage to nishthe polishing process by running upto 10 s only
with water to clean the cloth and the specimen; otherwise the chemical attack might
continue, resulting inetching of the specimensurface.
7.5.6 Other Oxides
Magnesium oxide MgO, iron oxide Fe
2
O
3
jewelers rouge, chromium oxide CrO,
and ceriumoxide CeO are all polishing media which noware used very seldom. Al
2
O
3
andSiO
2
will inmost cases dothe same jobandare mucheasier toworkwith.
7.6 Polishing Lubricants
Polishing lubricants are describedinSection6.5.
7.7 The Metallographic/Materialographic Preparation
MethodsMethod Parameters
As described above under sectioning, grinding, and polishing, a deformed or otherwise
damaged layer inevitably is formed during the machining processes. The depth of this
layer decreases with decreasing grain size of the used abrasive, and for this reason the
specimen, in the preparation process, goes through a number of steps with each step
removing the deformations from the previous step. The diagram in Fig. 1.7 shows the
processes of both mechanical preparation and electropolishing. Figure 13.18 shows a
typical process consisting of three stages, sectioning cutting, grinding, and polishing.
The grinding stage and polishing stage both have two steps, plane grinding/ne grind-
ing and rough polishing Polishing 1 and ne polishing Polishing 2. It can be seen
that the deformations from the previous step are removed and the last step ends with
very little or no deformation. The most critical steps are between cutting and plane
Fig. 7.15The same material as in Fig. 7.14 but polished with colloidal silica after 3 m
diamond. The deformations are removed and the true structure can be seen. BF.
grinding and between the last grinding step and rough polishing; this is especially the
case whenusing SiCgrinding paper for the last ne grinding step.
It is important that the method is adapted to the specic material being prepared.
For an overview of available methods refer to the 67 Traditional and Contemporary
Methods covering most materials that is statedinSection13.2.3.
The following contains a brief description of the basic methods for most metals
methods used for ceramics and other very hard materials are described in Section
6.3.2.
The grinding stage: As described in Sections 6.6 and 6.7 this book discriminates
between Traditional grinding based on SiC grinding paper and Contemporary
grinding based on rigid composite disks RCDs. This gives two types of preparation
procedures: The Traditional Methods T-Methods based on grit P220 SiC paper for
plane grinding and grits P320, P500, P1000 for ne grinding, and the Contemporary
Methods C-Methods based on SiC paper grit P220 for plane grinding, and one or two
RCDs with9or 6 mdiamondabrasive for ne grinding.
The polishing stage: At the T-Method the rough polishing step normally is on a
hard, napless cloth with 6 m diamond, a very important step for removal of the
scratches and deformations from the grinding. In the C-Method the rough polishing
step is often on a hard, napless cloth with 3 m diamond for removal of the scratches
and deformations from the RCD. For the T-Method, the rough polishing step is fol-
lowed by a 3 m diamond step on a hard, napless cloth followed by a nal step on a
soft, napped cloth with 1 mdiamond or on a soft, napless, porous cloth with alumina
or silica. In the C-Method, the rough polishing step is followed by a nal polishing as
mentionedfor the T-Method.
The end result is to a highdegree inuenced by the consumables used inthe prepa-
ration, as described earlier in this chapter, but also the parameters of the process play
animportant role.
In the case of automatic polishing with the use of a specimen mover on a grinding/
polishing machine, all parameters, not associated with consumables, are controlled by
the machine see Section 7.9. For manual hand polishing, only the rpmof the polish-
ing diskis a machine parameter.
7.7.1 RPM of Grinding/Polishing Disk
This is typically in the range of 50600 rpm, but for certain machines with continu-
ously variable speed, the rpmcanbe variedfromclose to0upto1200 rpm.
The rpm of the disk will, to a high degree, inuence the relative velocity between
specimen and grinding/polishing substrate. In principle this should be high to secure a
high removal rate, but experiments have shown see Section 7.9.2 that at polishing,
certain limits shall be observed, and for automatic polishing, 150 rpm is recom-
mended. At grinding, however, higher velocities can be allowed corresponding to
300 rpmor more.
7.7.2 RPM of Specimen Holder
To obtain the best results, the rpmof the specimen holder should be approximately the
same as the rpm of the disk see Section 7.9.2. The direction, whether it rotates
complementary to or contra to the direction of the disk is important see below. Most
machines have rpminthe range from3300 rpm.
7.7.3 Direction of Specimen Holder
Most modern grinder/polishers work with the specimen mover rotating in the same
direction as the grinding/polishing disk, complementary comp. This makes synchro-
nous polishing possible see Section 7.9.2 securing the best polishing action, avoiding
certainartifacts. If contra rotationcounter rotation is used, the removal rate is higher,
the specimen mover and the disk rotating in opposite directions, but this can only be
recommended for grinding, not polishing. Contra rotation is also used to keep the ox-
ide suspension on the polishing cloth because then the specimen mover pulls the sus-
pensiontowards the center of the polishing cloth, but according topolishing dynamics,
as described in Section 7.9.2, the contra rotation has certain drawbacks, as mentioned
above.
The force load on the specimens is important to obtain a satisfactory removal rate. At
grinding the specic pressure shall be relatively high, in the range of 3 to 10 N/ cm
2
4.35 to 14.5 psi 30 to 100 kPa, corresponding to a force of 20 to 70 N 4.5 to 15.8
lbf for a 30-mm1.25-in specimen.
The pressure will in certain cases inuence the degree of deformation, especially
for soft, ductile materials. Therefore, the pressure on the specimens shall be lower at
polishing than at grinding, in the range of 14 to 40 kPa, corresponding to a force of
10 to 30 N2.3 to 7 lbf for a 30-mm1.25-in specimen. Inprinciple, the specic pres-
sure shall be the same for large specimens, but experience has shown that a maximum
force of 50 N should be established on specimens of 40 mm 1.5 in in diameter and
larger. This is to avoid an overheating and excessive wear of the polishing cloth. To
compensate for the loss of material removal, the time canbe extendedfrom1 to 4 min.
7.7.5 Process Time
The duration of each step basically depends on the amount of material removed from
the specimen surface stock removal. This, however, cannot normally be measured on
most machines, and therefore the process time is used as an indicator. When grinding,
the amount of material removed is so high that measurement is possible see below,
but the removal rate at polishing is so low that measurement on a polisher is not pos-
sible. Only by measuring the time can a reproducible process be established. It should,
however, be recognized that a specic preparation time does not guarantee that the
necessary material is removed fromthe surface; this is only the case if the consumables
used react like the consumables when the process was established. Also, parameters
suchas force shouldbe correct toensure reproducibility.
7.7.6 Stock Removal
The whole preparation process is based on removal of material from step to step. The
ideal way of working would be to measure the material stock removed and stop the
process when the preselected amount, corresponding to the deformations from the
previous step, is removed. This is possible at the grinding steps, removing stock from
40 to 50 m to several hundred micrometres per step. Grinder/polishers with mea-
surement of stock removal are available in the market. At polishing, the stock removal
is so low for example, 3 to 6 m per 5 min that it cannot be measured without high
precisioninstruments, whichare not usually available ongrinder/polishers.
7.8 Grinding/Polishing EquipmentManual Preparation
The basic polishing machine has a rotating turntable on which an interchangeable
disk, covered with a polishing cloth, is placed. Normally the polishing process will con-
sist of two to four steps, including rough polishing, polishing, and nal polishing. In
some cases, when the ne grinding has been done with the contemporary method see
Section6.7 only one polishing stepmight be sufcient.
As described in Section 6.8, plane grinding, ne grinding, and polishing can take
place onthe same grinder/polisher only by changing the disk/disk surface usedfor each
step. See Section13.2.4for the technique of manual hand polishing.
The grinder/polisher is a standard piece of equipment that is available in many
models and sizes. Most models have one turntable for 200 mm 8 in, 230 mm 9 in
for SiC paper, 250 mm 10 in, or 300 mm 12 in disks, one/two speeds or continu-
ously variable speed, a water supply and a drain Figure 7.16 shows a grinder/polisher
with mineral casting base. It will work with 200 and 254 mm 8 and 10 in disks plat-
ens and is available in different models with one or two wheels turntables. One
model has 150 and300 rpm; another model has 30 to 600 rpm. Agrinder/polisher with
twoturntables is alsoshowninFig. 6.28.
Very often the grinder/polisher is prepared for retrotting of a semiautomatic
specimenmover.
7.9 Grinding/Polishing EquipmentAutomatic Preparation
If we look at the typical specimen mover systemfor automatic polishing, the correct
term would be automatic preparation because polishing is only part of the process.
Also the word automatic needs explanation, taking into consideration that in most
cases it expresses semi- or part-automation, meaning that only the basic process in
each step is mechanized, all handling of specimen holders, change of disk, cleaning,
etc., is done by hand. In some cases, however, the whole process is automated fully
automatic as described below. In the following the word automatic refers only to
the basic process involving manual work. If the systemis fully automatic, this will be
described.
The reason for using automatic equipment is that hand grinding/polishing is hard
and, in the long run, overloads the hand and arm of the metallographer. Automatic
preparation also ensures a better quality of the specimen through a uniform process
that is reproducible. The dependence onthe skill of the operator is reducedas well.
7.9.1 Machine Design
The Englishman I. E. Stead, who continued the work done by H. C. Sorby, already in-
vented a rotating specimen holder in 1900 for four specimens mounted on a movable
armsothat the holder wouldsweepthe rotating polishing disk.
Many other principles have been suggested over the years, but the specimen
mover with a number of specimens placed eccentrically on the grinding/polishing
diskis dominating today. Asupplement is vibratory polishing see below.
The standard specimen mover system is a grinding/polishing machine with a ro-
tating disk and a rotating specimen holder placed eccentrically on the disk see Fig.
7.17. The specimen holder or the individual specimens are pressed against the disk
surface toobtaina grinding/polishing action.
Fig. 7.16Grinder/polisher, with mineral casting base for manual preparation and, as shown,
with a specimen mover for semiautomatic preparation, 200/ 250 mm 8/ 10 in disks,
150300 rpm or 30600 rpm.
19
For a specimen holder with several xed specimens, these are xed in suitable
holes see Fig. 7.18 and during the operation, a central force is established pressing all
the xed specimens against the disk surface. The advantage of this system is a good
atness of the specimens, with the whole holder acting as a large specimen that
avoids the angling of the holder in comparison to the disk surface see below. The dis-
advantage is the work xing involved, and the need for at least three specimens in the
holder to keepthe balance. Inthe event that only one specimenis to be prepared, blind
specimens must be used. Also, the plane grinding may be prolonged to obtain that all
specimens are in the same plane. The microscopic inspection of the specimens during
the preparation process is rather tedious, having to put the whole holder on the micro-
scope.
The alternative is that specimens are placed in a holder plate and individually
loaded and called single specimenpreparation Fig. 7.19. The advantage is easy han-
dling and being able to take out a specimen after every step of the preparation for in-
spection. The disadvantage is a tendency to angling, the specimen being only at-
tacked in one direction, or penciling, the specimen being attacked along the
periphery, especially whengrinding onSiCpaper see Fig. 7.20. Inthe rst moments of
the grinding the SiCgrains will create a very strong pull inthe specimensurface caused
by the grains removing very much material in the rst seconds see Section 6.6. The
tendency will be to remove most material at the edge where the grains move into the
specimen. As soon as an unevenness has been made, the specimen might start rotating
Fig. 7.17Specimen holder placed eccentrically on the grinding/polishing disk.
Fig. 7.18Specimen holder with xed specimens and central load.
around its own axis and penciling will take place, or it might stay without rotation cre-
ating angling. Penciling and angling can be suppressed by working with as low speci-
mens as possible and establish the smallest possible distance, d in Fig. 7.20, between
holder plate and disk surface. Also, an exact guidance of the specimen in the holder
plate will suppress the angling.
The force on the specimens can be established through compressed air or by me-
chanical means. Withcentral pressure the force is transferredthroughthe center of the
specimenholder. By individual load, a pressure foot will be lowered against eachspeci-
mensee Section7.7.4.
Anumber of parameters should be controlled during the process see Section 7.7.
On simpler systems, the operator sets the rpmof the disk and the force. The rpmof the
holder is mostly xed, and in some cases the direction, complementary or contra, can
be set. The operator will stopthe machine after a certainperiodof time.
On more advanced systems all parameters are controlled through a microproces-
sor and programmed before the start of the process. This makes storing of programs
methods possible so that a method, once developed, can be reused whenever neces-
sary. The microprocessor also may control other parameters suchas dosing of abrasive
suspensionandlubricant see Section7.9.3.
The fully automatic systems are based onthe above; only several preparationsteps
including cleaning and drying are programmed as a process. This means either the
disks are changed automatically during the process or a certain number of disks are
available inthe machine see Section7.9.3.
Fig. 7.19Specimen holder plate with specimens placed in holes without xation and
individually loaded single specimens.
Fig. 7.20Schematic drawing of a single specimen placed in the holder plate on a grinding/
polishing disk. If the distance d is too long, angling or penciling will take place at grinding on
surfaces with xed abrasives.
7.9.2 Polishing Dynamics
As described above, the most common way of automatic polishing is placing the speci-
mens in a specimen holder which rotates eccentrically on a polishing disk Fig. 7.21.
As the dynamics between grinding/polishing disk and specimen holder have a certain
inuence on the preparation result, these dynamics shall be briey described. It is evi-
dent that the relative velocity between the surface of the polishing disk and the surface
of the specimen will depend on three factors: rpm of the disk, rpm of the holder and
directionof rotation.
Twosystems that are quite commoncanbe compared.
1 Polishing disk:
150 rpm
Specimen holder:
30 rpm
Complementary comp rotation
2 Polishing disk:
150 rpm
Specimen holder:
149 rpm
Complementary comp rotation
Comparing the velocity vectors in Fig. 7.21, we see that for system 1 the velocity
vectors are one-sided, causing a nonuniform material removal. This phenomenon is
evenmore pronouncedduring contrarotation.
Insystem2 the vectors cover all directions causing a uniformremoval.
This means that certain conditions, the optimum dynamic conditions ODC can
be dened.
33
ODC will be when the relative velocity is constant during a full revolution
of the specimen holder synchronous polishing, as can be seen in 2 Fig. 7.21. If the
rpm of the grinding/polishing disk is higher than the specimen holder, ODC is not ful-
lled and the preparation might result in having artifacts like comet tails see Section
13.6.
Fig. 7.21Polishing dynamics for a specimen holder eccentrically placed on a grinding/
polishing disk. Velocity vectors for two specimen holders, 30 rpm and 149 rpm are shown.
7.9.3 Semiautomatic and Fully Automatic Systems
Considering that automatic preparation is useful, even with an output of very few
specimens, semiautomatic and fully automatic systems can be considered very impor-
tant. They are supplied in different sizes, catering fromone to six specimens or more at
a time.
The tendency is to include as many parameters as possible in the automatic pro-
cess, still maintaining the manual change of the disk and handling cleaning of the
specimenholder withthe semiautomatic systems.
Withthe microprocessor a programming of all parameters is possible.
Small Semiautomatic Systems
The small systems will handle one to three specimens at a time on a 200 or 150 mm 8
or 10 in disk. The load is mostly supplied by a spring or a weight. Insome cases a timer
controlling the process is available.
Figure 7.22 shows a grinder/polisher for low volume semiautomatic preparation,
preparing one specimen at a time. Figure 7.23 shows a specimen mover for lowvolume
Fig. 7.22Automatic grinding/polishing system for one specimen at a time.
19
semiautomatic preparation mounted on a grinder/polisher, preparing up to three
specimens at a time. Specimens withvery lowdeformations especially suitedfor EBDS
see Section7.10 canbe produced.
Medium to Large Semiautomatic Systems
These systems carry the work load in most laboratories. They work with 250, 300, 350,
400 mm10, 12, 14, 16 in disks and specimen holders for six specimens or more, and
mostly rpm, force, andprocess time canbe controlledandpreset see Section7.7.
A dispensing system see below may also be included in the controls so that the
total preparation sequence including dosing of abrasive and lubricant can be pro-
grammed. The possibility of a permanent storage of programs for different materials
might be included as well, and newer systems allowfor connection to a local net LAN
and for establishment of databases with preparation methods. It is even possible to
downloadpreparationmethods fromthe Internet anduse themdirectly.
Figure 7.24 shows a semiautomatic system consisting of a number of grinder/
polishers, specimen movers and a dosing unit. The system is microprocessor con-
trolled allowing for connection to a local network LAN, sharing preparation methods
withother users.
Dispensing Apparatus
Dispensing dosing of abrasive and lubricant is part of the preparation process. Basi-
cally, the operator can perform this before and during the process, but especially add-
ing lubricant during the process that ties the metallographer to the machine is against
the idea of automatic preparation. Therefore, most semiautomatic systems have a
lubricant-dispensing dosing unit connected to the system, in this way adding small
amounts adjustable in regular intervals adjustable to the disk surface during the
process.
To obtain a constant removal rate it is an advantage to apply the abrasive, prefer-
ably as a diamond suspension, during the process. This can be done with dispensing
Fig. 7.23Specimen mover for one to three specimens, 8 rpm and force 220 N.
20
dosing units available for one or several bottles of suspension/lubricants. An oxide
polishing suspension can also be part of the suspensions to be applied, but this needs a
water cleaning systemas part of the dispensing unit.
The more advanced semiautomatic preparation systems include the control of a
dispensing unit.
Stock Removal
Stock removal controlled material removal is sometimes included in the control sys-
tems covering the grinding steps see Section7.7.
Fully Automatic Systems
These systems include all tasks of the preparation process. All parameters for the pro-
cess are programmed and stored permanently before the start, and the automatic pro-
cess includes: grinding, dispensing of abrasive and lubricant, cleaning and drying of
specimen holder after every step, change of grinding/polishing surface, and polishing
in several steps. In some cases stock removal can also be programmed. The goal is to
supply a specimenready for the microscope.
Insome cases the specimenholder withspecimens is plane groundonanother ma-
chine before going into the automatic system. In other systems, the plane grinding is
part of the automatedprocess.
Figure 7.25 shows a fully automatic system that combines the function of a semi-
Fig. 7.24Modular preparation system with single and central pressure, available in three
different disk sizes, 200-, 250-, and 300- mm diameter. Equipped with an automatic dosing unit
and programmable with preparation methods.
20
automatic grinder/polisher, a dispensing system, an ultrasonic cleaner, and specimen
dryer in one compact unit to be placed on a tabletop. It has single and central pressure,
andit is programmable withpermanent storage of methods.
Vibratory Polishing Systems
Vibratory polishing is an alternative to the specimen mover described previously. It
was originally developed for use in the hot cells preparing radioactive materials. The
reasonwas the very simple designwithout rotating parts, cutting maintenance downto
a minimum.
Vibratory polishing is based on the principle of a vibrating plate in the shape of a
bowl. A number of specimens, typically up to twelve, are mounted in weights and
placed face down on the polishing cloth, covering the plate. The bowl shape takes care
that a suspension, mostly Al
2
O
3
or SiO
2
, stays on the cloth. The vibration has both a
vertical and horizontal movement, normally established with an electromagnet. This
means that the single specimen, caused by the inertia, moves slowly along the periph-
ery of the bowl, in this way being polished through the movement between cloth and
specimen. By adjusting the amplitude of the vibratory movement, the speedaroundthe
bowl can be controlled and set according to sample size and weight. The polishing ac-
tion is very low, suited for sensitive materials making a scratch-free surface possible
with very low deformation. Due to the low removal rate, a normal nal polishing step
will take several hours inwhichthe apparatus canbe left unattended.
Figure 7.26shows a heavy duty vibratory polisher withvariable settings.
7.10 Special Preparation Techniques
7.10.1 PCB Coupons
Printed circuit boards PCB are often metallographically/materialographically in-
spected to ensure the quality of the metal layer in the holes of the board. For this pur-
pose a so-calledcouponis made see Fig. 3.17.
PCBcoupons to be tested according to the American standard IPC-TM-650 should
be preparedsothat the preparedsurface is exactly throughthe middle diameter of the
holes to be inspected. This is usually done by mounting several coupons on two preci-
sionpins using tworeference holes see Section3.11.5 andFig. 3.17. The twoprecision
pins canbe usedas contact surface ina special specimenholder sothat the coupons are
placed exactly in relation to the holder. In this way the target the middle of the inspec-
tion holes can be reached by using a number of adjustable stops on the holder. The
stops are calibrated according to the surface on which the pins are resting, in this way
securing that the process stops before the target is reached. Normally a rough SiC
grinding paper is used for the rst step, the grinding being stopped 100 to 200 m
fromthe target. By readjusting the holder the next step with a ner SiC paper will stop
very close to the target. According to the type of PCB, the grinding steps shall be fol-
lowed by one or more polishing steps. These steps are made without stops because the
material removal at polishing is very low, minimizing the risk of removing too much
material fromthe PCB. For a preparationprocess, see MethodT-27inSection13.2.3.
7.10.2 Microelectronic MaterialsNonencapsulated Cross Sections
Microelectronic materials are cross-sectioned to a specic point target for both light
microscopy andscanning electronmicroscope SEM examination.
Cross sections serve twomainfunctions:
34
Cuts through representative structures within an IC show relationships of layers
and features, such as step coverage, interfaces between layers, and possibly em-
beddeddefects or voids.
Precision cross sections through specic defects often lead to the process step or
mechanismthat producedthe defect.
When applicable, nonencapsulated cross-sectioning is simpler and faster than the classi-
cal encapsulated method. Results of nonencapsulated cross-sectioning are more suitable
for viewinginascanningelectronmicroscope.
The passivation layer of the ICprovides sufcient encapsulation of malleable met-
allizationto prevent smearing. Rounding of the front edge is avoidedby using hard, at
grinding andpolishing surfaces.
Tripod FixtureThe Process
Cross sections canbe preparedwiththe relatively simple tripodxture where the speci-
men is the third leg on a xture see Fig. 7.27. Cross sections can also be prepared on
Fig. 7.25Fully-automatic, microprocessor controlled grinding/polishing system, with built-in
dispenser, ultrasonic cleaner, and specimen dryer. Programmable, with permanent storage of
methods.
19
semiautomatic systems andfully automatic systems; bothare commercially available.
In the following only the use of the tripod xture will be described see also
Material/PreparationTables 22, Section13.2.3.
SiC paper 600 grit was used originally to grind to within 20 to 30 m of the tar-
get. Polishing from that point was accomplished solely and slowly on a glass disk.
34,35
However, the need for faster throughput and the introduction of hard tungsten plugs
necessitatednewpolishing media andtechniques.
The procedure described below using a hand-held tripod xture is basic, simple,
and fast. It produces excellent results that can be imaged on either standard or eld
emissionSEMs.
The grinding procedure described involves several short steps with Al
2
O
3
and dia-
mond lapping lm starting with relatively coarse grits. Satisfactory results can be ob-
tainedby grinding longer withfewer steps, but the procedure will be tedious if the over-
all grinding time is increased by using ne grain sizes to remove material slowly.
Additionally, if the grinding time is excessive, the material removal rate may decrease
as grinding/polishing media wear and it is difcult to judge whether enough material
has beenremoved.
Cross sections wider than the 5 by 5 mm 0.20 by 0.20 in in width will require
signicantly longer grinding and polishing times. The use of worn out grinding media
should be avoided; fresh, ner grain size grinding/polishing media may have a faster
removal rate thancoarser, wornmedia.
Even if a cleaved edge is close to the desired nal line such that no grinding is re-
quired, a brief grinding on grit P4000 US grit 1200 is recommended to make a at
surface. Grind only as necessary to create a at surface, even if a part of the surface
remains untouched. Jagged edges on a cleaved sample, if not removed, will scratch
away the Al
2
O
3
or diamondfromthe lm.
Equipment and Consumables
A tripod xture with the specimen mounted on a sample mount paddle see Fig. 7.27
is used by hand on the rotating grinding/polishing disk of a grinder/polisher with a
200 mm8 in diskandvariable speed, preferably 10 to 150 rpmsee Section7.9.
Fig. 7.26Heavy duty vibratory polisher, horizontal vibratory movement, with variable
settings.
19
A stereomicroscope and a metallurgical microscope with measuring abilities are
requiredtocheckthe progress of the preparationprocess.
Sample mounts are used for carrying the sample specimen during the prepara-
tionsteps andfor the analysis inSEM. The process involves grinding paper andlapping
lms, Al
2
O
3
and diamond, and for polishing diamond suspension and a polishing
cloth. Dry nitrogenor a supply of aerosol cans is requiredtoblowthe specimens dry.
Preparation, See also Method C-22, Section 13.2.3
Sectioning can be done on a precision cut-off machine with a diamond wheel see Sec-
tion 2.5. The desired cross section target should be within 50 mof one edge. The sili-
conpiece is thenattached to a sample mount suchthat the edge containing the target is
parallel to and extending over the edge of the sample mount cantilever fashion, plac-
ing the specimen on a hot sample mount 125C 250F using wax, as shown in Fig.
7.28.
Grinding takes place in three to four steps. The purpose of grinding is to rapidly
achieve a surface, 1 m away from and parallel to the desired cross section line tar-
get.
The surface left by grinding, later to be polished, should be at and scratches
should be no greater than those caused by 1 m Al
2
O
3
or diamond particles on
Al
2
O
3
/diamond lms. The grinding procedure typically requires less than 15 min in-
cluding inspectiontime.
In Method C-22 the total preparation process is described. It is important that the
specimen is adjusted so that the ground surface is parallel to the cross section line tar-
get. The time in minutes is not stated at the grinding steps, but the distance remaining
to the target. This is to ensure that all deformation from the previous step is removed
andtoensure that the target is not reachedina tooearly step.
Polishing is used when a very ne nish is wanted. Microelectronics with metal
systems of Al no tungsten or gold no tungsten are polished using a 0.05 m Al
2
O
3
lapping lmor a soft, napped or napless, porous cloth using colloidal silica as the abra-
sive. In case of metal systems with Al / W and Au/ W, polishing is done with a napless,
hard, woven synthetic cloth and 0.1 mdiamond suspension or a napless, soft, porous
clothwith0.1 mdiamondsuspensionmixedina 50:50solutionwithcolloidal silica.
Fig. 7.27Tripod xture, the specimen is placed as one of three legs of the hand
held-holder.
7.10.3 Microelectronic PackagesTable 7.2Target Preparation
Electronic and microelectronic assemblies are complex material composites. The ma-
terials used are dissimilar in their chemical composition, their crystal structure, and
their microstructure. Of technical importance for the qualication of the components
are interfaces, grain boundaries and phase boundaries as well as heterogeneous pre-
cipitations. Imaging and analysis of the microstructure is a prerequisite for estimating
the quality of a component. Further criteria for qualication, from the materialo-
graphic point of view, are inclusions, contaminations, pores, cracks, holes, as well as
the evaluationof contours, e.g., the wetting angle of a soft solder connection.
36
Due to the close packaging of electronic and microelectronic devices with many
various materials within a small volume, microstructural examination is faced with
the problem of simultaneously imaging different materials that have very different
properties. Specimen preparation therefore involves the simultaneous processing of
hard, often brittle materials and soft materials exhibiting plastic deformation. The ma-
terials most used in advanced integrated circuit packaging and interconnection tech-
nology, their use andhardness HU, see Section21.5 are listedinTable 7.2.
37
Each of the materials stated in Table 7.2 has its specic properties and, as can be
seen, the hardness is very different and often the materials are brittle. This must be
taken into consideration during the materialographic preparation; each individual
step from cutting through grinding to the nal polishing step is of signicance. Mis-
takes made in the rst stages of preparation can only be corrected during the subse-
quent steps with considerable difculty or not at all. For each step the rate of material
removal and the deformation layer which remains are important factors. The prepara-
tion parameters used grinding surface, type of abrasive, grain size, lubricant must be
carefully selected on the basis of the physical properties. The general rules for the
preparation of solid materials are that soft and medium-hard materials should be
plane ground using SiCgrinding papers, whereas hard materials require resin-bonded
Fig. 7.28Microelectronic specimen mounted on a sample mount for a tripod xture.
disks withxeddiamondgrains or rigidcomposite disks RCDs withaddeddiamonds.
Very oftenfor the devices describedherein, bothextremely hardandvery soft materials
must be prepared at the same time, and insuchcases the preparationmust be based on
a compromise. The goal of the preparation is to obtain a at specimen without relief
between the different constituents and good edge retention, while at the same time
avoiding deformationand other artifacts of the soft and brittle constituents. If only SiC
grinding papers are used for grinding of hard materials, then edge rounding and relief
will set in at an early stage. Plane grinding and the rst steps of ne grinding should be
done with the hardest possible abrasive suited for the hardest materials in the speci-
menand always using the nest grainsize possible. OftenSiCpaper should not be used
with a grit coarser than P500 to avoid damage to the brittle materials in the specimen,
and during both grinding and polishing the pressure should be kept low to avoid
damage.
36
In the Material/Preparation Tables 1926, Section 13.2.3, eight methods are indi-
cated covering the preparation of different electronic components. To be able to select
the method best suited for a given component, it shall be analyzed before the prepara-
tion starts to be able to decide on the best method and how the preparation shall be
performed.
Inspection and Location of Fail SiteTarget Preparation
Before the preparation starts, the structure of the assembly should be studied by visual
macroscopic methods to decide on the materials involved and to locate critical sites
and the locations of both obvious and possible defects to be marked. Typical fail sites
targets include: poor solder joints, cracks in components, or defects in the circuit
board material. These faults are then investigated more closely using other techniques
TABLE 7.2Materials Used in Electronic and Microelectronic Devices and Interconnections.
Material
Common Applications in
Mounting and Connection
Technology Universal Hardness (HU)
Al
2
O
3
ceramic Carriers (hybrid technology),
body of components
17000
Silicon Semiconductors, transistors, ICs 9300
Nickel-phosphorus (NiP) Resist layer, metallization 4000
Kovar (FeNiCo) Lead frames, circuit board core 1900
Invar (FeNi) Lead frames, lead wires 1800
Aluminum (Al) Housing, heat sinks, capacitor
foils
1300
Copper-silver (CuAg)
solder
Solder (brazing) 1100
Gold (Au) Surface nishing layers,
(connectors, solder, adhesive and
wire bond contacts)
500
Tin-silver (SnAg) solder Soft solder 300
Copper (Cu) Metallization on circuit boards,
lead frames
300
Epoxy-berglass sheet Circuit board material 280
Tin-lead (SnPb) solder Soft solder 230
like radiography, ultrasonic imaging, ne and gross leak testing, and die penetration.
The orientation of the plane of preparation will depend upon the orientation or the
features to be imaged and is often marked on the assembly plan. If the fail site target
has been located then this will determine the plane of preparation, often starting with
the sectioning close to this plane. Special apparatus for target preparation is available
inthe market.
Sectioning and Mounting Encapsulation
Sectioning must be done so that the site of interest is not damaged by deformation or
input of heat. Therefore, very often the device is mounted encapsulated before the
sectioning takes place. Encapsulation shall be accomplished with only a low develop-
ment of heat and the resin shall be able to ll out all cavities without shrinkage. This
means that an epoxy with a low viscosity should be used, preferably under vacuum so
that an impregnation takes place see Section 3.10. It is very important that the speci-
men is cleaned very effectively in acetone, preferably using ultrasonics before the en-
capsulation. After cleaning, the specimen should only be handled with a pair of twee-
zers anddriedwithN
2
or absolutely cleanair, not normal compressedair.
Sectioning and mounting are described in detail in the Material/Preparation
Tables 19to26.
7.10.4 EBSD
Electron backscatter diffraction EBSD has gained ground in recent years as an acces-
sory to a scanning electron microscope SEM. The main advantage of EBSD is the
possibility to link morphology grain size and shape with crystallographic features
phase, orientation, disorientation on the microscopic scale, but still in a representa-
tive specimen area.
38
The preparation is much simpler than for thin foils for TEMsee
Section8.6, but more demanding thanthat for normal SEM.
The information depth of EBSDis very low, in the range of 20370 nmdepending
onmaterial, SEM, etc. This means that the surface of the specimenshall be without the
thin distorted layer that normally exists after a mechanical polishing see Section 7.3.
This can be obtained by etching, but etching should often be avoided for EBSD. For
certain materials electrolytic polishing can give a deformation-free surface, but for
many materials like ceramics, heterogeneous materials, etc., mechanical preparation
is the only possibility toobtaina at anddistortion-free surface.
For this reason the standard grinding/polishing process shall be adjusted, espe-
cially with regard to the last polishing step. In principle, the normal method used for a
specic material can be used with special attention to the last polishing step using
silica, which often is prolonged. A long preparation time using silica as an abrasive
might give an unwanted relief, and therefore polishing cloths must be chosen very
carefully.
Specimen Mover Systems
The most used specimen mover standard system for normal metallographic/mate-
rialographic preparation has a specimen holder rotating eccentrically on the grinding/
polishing disksee Section7.9.
The preparation methods described in Section 13.2.3 are based on the use of this
standard specimen mover, normally operating with 150 rpm grinding/polishing disk
and specimen holder and a force per specimen not lower than 5 N 1.1 lbf. This sys-
tem will give acceptable results for EBSD for very hard materials like ceramics, possi-
bly using chemical mechanical polishing CMP see Section7.12.
For most materials, however, it is not possible to obtain a distortion-free surface
after the last step, and this step either has to be prepared on a special slow moving
specimenmover or by vibratory polishing.
Specimenmovers withvery lowrotationand force per specimenare commercially
available. The rpm of both the disk and specimen holder can be adjusted to a relative
velocity close to zero see Section 7.9.2 and the force on the specimen down to close to
zero. This means that all metals can be prepared for EBSD in a reasonable time, often
using CMP, see under the specic materials in Section 13.2.3. CMP is also needed for
hardmaterials like certainceramics. For specic preparationdata for a highnumber of
materials see Ref. 38.
Vibratory Systems
Vibratory polishing normally gives good results for EBSD; the main drawback being
the very long preparationtimes, althoughthe vibratory polisher canworkunattended.
If vibratory polishing is used for all steps including grinding, a high surface wavi-
ness can be observed and due to the long polishing times a relief can develop. There-
fore, vibratory polishing should be limited to the last step, having done the previous
steps onthe standardspecimenmover or the slowspecimenmover describedabove.
38
Mechanical Preparation
Field metallography is, as the termindicates, used in the eld, often called in situ or on
the spot. It is based on the grinding and polishing processes described above; portable
apparatus is available that is able to prepare a small area nondestructively. Field metal-
lography is usedonlarge parts, steampipes, etc., to be able to check the microstructure
without destructing the work piece. Very oftenit is not possible to analyze the prepared
spot and a replica is taken see below. The preparation methods and etching proce-
dures tobe usedcanbe seenfromTable 11.1andSection13.2.3.
Many materials like steel, aluminum, and titaniumare very well suited for electro-
lytic polishing using a portable electropolisher see Section8.5.
7.11.1 Portable Grinder/Polishers
These are available with a hand piece with a exible rotating disk upon which a small
piece of grinding paper or polishing cloth is placed. This apparatus can be supplied
from the mains or battery operated. The normal preparation process in a number of
steps is employed and normally, after etching, the prepared spot is analyzed with a por-
table microscope to ensure that the microstructure is acceptable for further examina-
tion. Following this, a replica is made. This replica is taken to the laboratory for exami-
nation.
Often the grinder/polisher is used for the preparation of a spot that is nally
electropolished/etchedtoobtainthe microstructure see Section8.5.
7.11.2 Replication
Replication is a very important part of nondestructive preparation. Replication is a
nondestructive procedure that records and preserves the topography of a materialo-
graphically prepared surface as a negative relief ona plastic lmor other mediumrep-
lica. See alsothe ASTMStandardPractice for ProductionandEvaluationof FieldMet-
allographic Replicas E1351 Section12.4.
The replica material shall have a number of characteristics:
All features present on the surface that was replicated shall be accurately repro-
duced.
Simple andreproducible handling.
Highstability andstrength.
Flexibility sothat replica canbe made oncurvedsurfaces.
Replicas should be made either using a piece of plastic acetate lm or a fast cur-
ing silicone rubber-basedmaterial.
Plastic Film
The lm or foil is 12 by 18 mm 0.5 by 0.75 in in size. Two methods can be followed
whichare describedinSection13.4.3.
Silicone Rubber
The silicone rubber-based material used is a two-component silicone rubber that is
available indifferent types according tothe specic purpose.
The compound is supplied in cartridges that are mixed and dispensed on the pre-
pared surface using a special hand-operated gun. The silicone rubber is very exible,
suited for curved surfaces, inside tubes, etc. The material is also very suitable for engi-
neering inspection applications like microcracks, wear marks, corrosion marks, etc.
For use of siliconrubber, see Section13.4.3.
7.12 Chemical Mechanical Polishing
Chemical mechanical polishing CMP has been highly developed for the preparation
of siliconwafers, but CMPis alsousedwithadvantage for other materials.
In CMP, also called etch polishing or attack polishing, the specimen surface is at-
tacked both mechanically by an abrasive and chemically at the same time.
32
Nor-
mally an abrasive suspension with an in-mixed chemical substance is used. Material
removal occurs as a consequence of a combination of the chemical reaction of the
chemical with the specimen surface material and the continuous removal of the reac-
tion materials by the abrasive. Because of the removal of the reaction products, even
chemical solutions that typically would not attack a given material will have an effect
because the passivating layer is constantly removed. CMPis establishedeither by using
suspensions of silica SiO
2
often with a pH between 8.5 and 11 or alumina Al
2
O
3
,
with a pHbetween 3 and 7, or by mixing a chemical solution, often an etchant, with the
oxide suspension.
CMP, using a very ne abrasive like silica with a grain size of 0.02/ 0.05 m, and a
relatively weak chemical attack, will create surfaces almost without deformation and
scratches. This means that CMP is very well suited for the nal polishing step for most
materials, creating a clean surface. Especially in soft and ductile materials this is an
advantage. The polishing will take place ona relatively soft, porous polishing cloth, and
therefore the time shall be limitedto0.5 to 1.5 min.
Aluminum, refractory metals, Ti, and other metals can be polished with silica with
or without an added chemical. Also, ceramics and other materials with high abrasion
resistance are suited for CMP; both acidic alumina suspensions and basic silica can be
used.
For some materials like Ti and most Cu alloys, the nal polishing step can be made
using a silica suspension with the addition of hydrogen peroxide and ammonia solu-
tion. Ferrous metals and Ni-based alloys canbe polished withacidic alumina. If the pH
should be lowered, oxalic acid can be added, and if the pH shall be raised a chemical
like potassiumhydroxide canbe added.
For solutions used for the specic materials, see the Material/Preparation Tables,
Section13.2.3.
With the modern advanced methods of preparation, CMP is mostly limited to the
suspensions and solutions mentioned earlier. CMP, however, can be performed with a
very highnumber of chemical solutions, mostly etchants.
2,9
7.12.1 ProtectionCorrosion at CMP
When using the chemical solutions recommended in this book see Section 13.2.3 the
corrosive attack on equipment and accessories is minimal. In the case of suspensions
mixed with stronger chemicals acids, care should be taken to protect equipment and
persons working with the mixture. Also, only synthetic polishing cloths made for CMP
shouldbe used.
7.13 Thin Sections
For certainmaterials suchas minerals, ores, ceramics, and plastics, the use of reected
light for microscopic examination is not always satisfactory. By using thin sections
with a thickness of 2035 m down to 710 m at plastics and polymers it is pos-
sible to examine the specimen in transmitted light, and if the thin section is polished,
alsoinreectedlight.
To make a thin section a high amount of material must be removed by cutting,
lapping/grinding, and polishing. The process is time consuming and extreme care
shouldbe takennot tomake changes inthe material of the thinsection.
Below follows a short description of thin section preparation for petrographic/
ceramic materials andfor plastics/polymers.
7.13.1 Thin Sections of Petrographic/Ceramic Materials
The preparation of thin sections can be done on machines and consumables available
in the market. In the following a method as shown in Fig. 7.29 is described. Often im-
pregnation of the material is needed before the cutting or the preparation, or both, can
take place. For this and for a further description of the cutting, lapping, and polishing
see Material/Preparation Tables M/P T 39 and 40 for petrographic/mineralogical ma-
terials andM/PT0206for ceramics.
1. The specimentobe sectionedis selectedoftenfroma larger piece.
2. The specimen is sectioned normally with wet abrasive cutting using a diamond
metal bond cut-off wheel. The size of the specimen depends on the size of the glass
slide usedsee below.
3. For minerals, one side of the specimen is lapped in two steps with SiCpowder, grit
P220 and P1000, on a cast iron disk to obtain a plane surface; normally this is done
in a special specimen holder plate on a semiautomatic grinder/polisher. For ce-
ramics, grinding andpolishing of one side are made as describedinM/PT0206.
4/5. A glass slide 27 by 46 mm, 28 by 48 mm or 30 by 45 mm is ground to a given
thickness, e.g., 1.164 mm on a special machine with a diamond grinding wheel
or lappedina holder as describedinNo. 9below.
6. The specimen, with the prepared side towards the glass, is glued to the glass slide
under vacuumusing epoxy.
7. The surplus material of the specimenis removedby cutting witha diamondcut-off
wheel toa thickness of about 0.5 mm0.02 in.
8. The mineralogical thin section is ground down to 80100 m on a special ma-
chine with a diamond grinding wheel, or only lapped as described under No. 9.
Ceramics are ground according to M/P T 0206 to a thickness of approximately
80 m.
9. Mineralogical materials are lapped with SiCpowder on a cast iron disk in a special
holder on a semiautomatic grinder/polisher so that the nished section has a
thickness, including the resin layer, of e.g., 30 m. The holder has built-in sticks of
boroncarbide or diamond so that the process stops whenthe sectionhas the thick-
ness that is wanted. If the thin section has been ground down to 80100 m on a
special machine, lapping only with grit P1000 SiCpowder is needed. If all material
shall be removed by lapping, two steps are used, grit P220 and grit P1000. Ceram-
ics are ne ground and polished down to 530 mdepending on the ceramic. The
preparationprocedure follows M/PT0206.
10. If the thin section is to be polished, this is done in a special holder so that the nal
thickness is inthe range of 2025 m.
The nished thin section can nowbe examined in reected light. For examination
intransmittedlight, a cover glass shall be placedonthe polishedsurface.
7.13.2 Thin Sections of Plastics/Polymers
Thin sections are made when plastics and polymers are required to be examined by
transmitted light or contain hard inclusions. Most often unlled plastics and polymers
canbe examinedinthe formof thinmicrotome slices see below. If carefully prepared,
the thin sections made by grounding/polishing will be less damaged than a thin micro-
tome sectionso it is to a highdegree the purpose of the examinationthat decides which
method to use. In the following a method for preparing thin sections
3941
is described
that is based on the methods stated in Material/Preparation Tables 64 and 65, Section
13.2.3.
1. Aspecimenwithgoodedge retentionis made.
2. A thin slice is cut from the prepared side of the specimen. See Material/
PreparationTables 64and65.
3. The prepared side of the slice is glued to a glass slide with an adhesive while not
disturbing the specimenmaterial andwithout air bubbles.
4. Grinddownmanually or ina holder toabout 20 mfromthe requiredthickness.
5. Fine grindtoabout 5 mfromthe requiredthickness.
6. Polish with 3 m diamond and nish with alumina, step P 3 in Method C-64 to a
thickness of 1015 m.
For examination in transmitted light, a cover glass is placed on the polished sur-
face; this is not neededfor reectedlight.
As mentioned above, thin sliced specimens of plastic and polymers can be made
with a microtome, where the slice is cut in a thickness of 330 m, generally around
10 m. For further information, see Refs. 40, 41andSection7.14.
Fig. 7.29Method for preparation of petrographic/ceramic thin sections. 1. Sampling. 2.
Cutting of a specimen. 3. Lapping of the specimen. 4./5. Grinding/lapping of glass slide. 6.
Cementing of specimen to glass slide using epoxy under vacuum. 7. Cutting of surplus material.
8. Grinding on a special machine of thin section, or lapping as shown in 9 down to 80 m 9.
Lapping of thin section in a special holder down to e.g., 30 m section and resin layer. 10.
Polishing in a special holder down to approximately 25 m. 11. The nished thin section.
7.14 MicrotomyUltramilling
Both microtomy and ultramilling are mechanical preparation processes comparable
to grinding and polishing, and made on relatively sophisticated equipment. In most
cases the specimen, soft metal, or other soft materials canbe examinedwithout further
preparation.
Microtomy is developed for preparation of biological specimens for transmitted
light. In this case the thin section is made by moving the specimen with a controlled
feed into a xed tool knife. In this way a section of a thickness of 0.5 to 60 m can be
made, suited for examination in transmitted light. This method can be used for prepa-
ration of plastics as described in Section 7.13.2 and for preparation of bone, teeth, and
other organic materials.
When used for metals the microtome produces a surface comparable to a plane
grinding or polishing for examination in reected light. To justify the use of a micro-
tome andultramilling see below the nishedsurface shouldbe of a highquality, ready
for the microscope. Soft, nonferrous metals up to a hardness of 150 HV can be pre-
pared on very stable microtomes using special knives with hard metal or diamond
edge.
Microtomes are commercially available.
In ultramilling the specimen surface is prepared not with a knife but with a rotat-
ing milling tool.
The specimen is placed on a sledge traveling underneath the milling head consist-
ing of a vertical, rotating spindle equipped with a diamond cutting tool. The rotational
speed of the spindle is adjustable between 500 and 3000 rpm. The feed between speci-
men and milling tool can be adjusted in steps from 1 m, securing a very ne surface.
Also the speedof the sledge canbe adjustedaccording to the properties of the specimen
material. The process is done in two steps, pre-milling with a special cutter, where the
deformations fromsectioning, etc., are removed, and the nishing step using a milling
tool whichleaves a very smoothsurface ready for investigation.
Ultramilling equipment is commercially available.
8
Electrolytic Polishing/Etching
ELECTROLYTICPOLISHINGORELECTROPOLISHINGANODICPOLISHING
is a polishing methodwhereby the specimenis placedas ananode inanelectrolytic cell
andthe electrolysis establishes a surface suitable for metallographic analysis.
In principle, electropolishing is the ideal polishing method because no deforma-
tions are added to the surface during the process, and most or all deformations intro-
duced before the polishing are removed. Also, the process is done in a very short time,
usually in5 to 20 s.
The electrolysis has some effects that unfortunately limit the use. Most pure met-
als anda vast number of alloys canbe electropolished, withspecial advantage to metals
that are relatively difcult to polish mechanically, such as aluminum/aluminumalloys
and copper/copper alloys. But as soon as the material has several phases with a certain
difference in potential, the results are not satisfying. To limit the negative inuence of
the electrolysis by shortening the process time, the specimen is usually mechanically
groundandsometimes polishedbefore the electropolishing.
An advantage with electropolishing is the possibility of electrolytic etching of the
specimenas part of the process.
8.1 The Electrolytic Polishing/Etching Process
Electrolytic polishing is the anodic dissolution of the specimen surface in an electro-
lytic cell see Fig. 8.1.
42
An electrolytic cell is used very often for depositing a coating
on a work piece, the cathode, removing the material fromthe anode; in this case a pol-
ishing of the anode barely takes place. It is, however, possible to control the conditions
in the cell so that a smoothing, removal of all large-scale irregularities above 1 m,
takes place. This is followed by a brightening which is a removal of all submicro-
scopic irregularities down to approximately 0.01 m, establishing a surface of the an-
ode without irregularities that is suited for microscopical examination. The amount of
Fig. 8.1Schematic drawing of an electrolytic cell, showing the anode, cathode and
electrolyte.
156
material removed is so small that the metal ions stay in the electrolyte without being
depositedonthe cathode.
Anumber of factors play a role for obtaining the right conditions for polishing:
Shape of polishing chamber, positionof anode andcathode.
Voltage.
Anode current density.
Electrolyte compositionandtemperature.
Flowof electrolyte.
Conditionandarea of the specimensurface.
Polishing time.
The process, especially the brightening, is not fully understood, but the supposed
process is describedinthe following.
8.1.1 The Polishing Cell
The specimen surface normally has been ground on SiC grinding paper or on a dia-
mond disk, grit P500 or ner, before electropolishing see Chapter 6. In some cases,
however, it is possible to go straight to electropolishing from the cut-off, but in most
cases a ne grinding, as mentioned, and even a rough polishing is needed. The surface
before electropolishing will in all cases have hills and valleys as shown in Fig. 8.2.
This gure shows the development of the process fromthe rough ground surface to the
nishedsurface see further explanationbelow.
The specimen is placed in an electrolytic cell Fig. 8.3 shown schematically with
the specimen as anode, a thermometer for temperature control, a stirrer to obtain an
electrolyte ow, and a cooling vessel around the cell to keep the temperature constant.
The dc voltage is controlled by a potentiometer, the voltage and amperage can be mea-
suredonmeters, anda timer will control the process time.
8.1.2 Smoothing and Brightening
To explain the theory behind the process, an ideal polishing sequence based on an elec-
trolytic cell using a potentiostat is used. The resulting current-density curve is shownin
Fig. 8.4withthe developments onthe specimensurface as showninFig. 8.2.
When starting the process in the cell shown in Fig. 8.3, by increasing the voltage
from 0 V towards Point B Fig. 8.4, at rst a direct anodic dissolution takes place. At
Point B, a viscous lmis developed and anelectroetching of the specimensurface takes
place, removing very little material see Section 9.5. When the voltage/current density
reaches the level of Point Banunstable conditiondevelops until Point C, where a stable
plateau is established with increasing voltage. At this plateau the previously developed
viscous lm, having a passivating effect, reaches equilibrium, enabling a smoothing of
the specimen surface see Fig. 8.2. The material removal by diffusion through the vis-
cous layer will be higher at the tops of the hills, the current being higher, because the
diffusion path is shorter than at the valleys. This creates a smoothing of the surface.
The best polishing takes place between C and D on the curve. With increasing current
density, D towards E, oxygen bubbles develop and make openings in the viscous layer,
creating pitting in the specimen surface. Close to D the gas development is still rela-
tively low and polishing may take place, but at E the amount of bubbles will totally
destroy the lmandpolishing is not possible.
The presence of the viscous layer, however, cannot explain the brightening of the
submicroscopic irregularities. On many examinations it has been proven that a thin
solid lmwill arise on the surface of the anode, which will play an important part dur-
Chapter 8 Electrolytic Polishing 157
ing the polishing. This lmis considered to have a thickness of a fewatomlayers and is
very difcult to identify with regard to its composition. Some scientists think the lm
consists of metal oxide, but a nal proof of that has not been obtained. The presence of
the lm, however, must be taken for granted. The very thin lmfollows very exactly the
surface of the anode specimen and the decrease of metal ions will be the same every-
where. This will cause a removal of the quite small irregularities.
43
The voltage/current density curve at a cell without potentiostat will not show the
same distinct plateau. Figure 8.5 shows a curve taken frompolishing of mild steel on a
commercial electropolisher.
Fig. 8.2Schematic drawing showing the surface of the specimen during the different steps
developed during the electrolytic polishing and etching. The letters A to E refer to the curve in
Fig. 8.4.
8.1.3 Electrolytic Etching
For many materials, the etching process can take place as a continuation of the polish-
ing but at a lower voltage. The low voltage, usually around one-tenth of the polishing
voltage between A and B on the curve Fig. 8.4 creates a weak attack on the specimen
Fig. 8.3Schematic drawing of an apparatus for electrolytic polishing/etching.
Fig. 8.4Theoretical curve showing current density versus voltage during the process of
electrolytic polishing/etching.
surface, preferably attacking the grain boundaries see Fig. 8.2. In some cases, like
with stainless steel, the polishing electrolyte cannot be used for etching, and etching
must be performed with another electrolyte outside the polishing chamber see Sec-
tion9.5.
8.1.4 Advantages and Disadvantages
At the time when specimen preparation to a high degree was based on manual polish-
ing with alumina, with long polishing times, the quality of the achieved preparation
result was relatively low. Therefore, when electrolytic polishing was commercially de-
veloped around 1950, it gained ground for many years because the quality was higher
than with alumina polishing. Anumber of artifacts developed during electropolishing,
problems with edge retention, etc., were accepted as necessary evils. With the devel-
opment of diamond polishing, rigid composite grinding disks and better polishing
cloths, the quality of mechanical polishing has increased considerably, and the weak
points of electropolishing canhardly be accepted for a number of materials, evenwhen
mechanical polishing normally takes more time thanelectrolytic polishing. Withsofter
materials, relatively difcult to polish mechanically, the electropolishing still has an
advantage.
Electropolishing should be performed on commercially available polishers, spe-
cically developed for that purpose. In principle, electropolishing can be performed in
any electrolytic cell, but because of the risk of re, explosion, spill, etc., the commer-
cially developed apparatus provides better safety and good, reproducible results see
Section 8.4. The following descriptions relate to the use of a commercial
electropolisher.
Advantages
Etching included: For most materials it is possible to include the etching as the last
stepinthe process.
No deformation: The process leaves a clean, undistorted surface, not adding defor-
mation to the specimen surface. This is an important feature when doing research
work which is surface-related, or for preparing surfaces for micro hardness test-
ing, X-ray studies andelectronmicroscopy.
Fast: The method is very fast. The polishing, which takes place after mechanical
grinding and in some cases rough polishing, only takes 5 to 15 s for the polishing
and2 to 10 s for etching if possible. This canbe very important inquality control.
Reproducible: Whenall parameters of a procedure are established, the process can
be exactly repeatedgiving reproducible results.
Fig. 8.5Current density/voltage curve at electropolishing of mild steel.
Automatic: The modern electropolishers are totally automated so that all param-
eters are programmed before the process starts. This secures that the operation is
totally independent of the operator. Also, a number of different methods can be
savedinthe database of the apparatus.
Disadvantages
Nonuniform material removal: The different phases in the specimen surface will
have a different electrochemical potential. This means that the material removal
will be different from phase to phase preferential attack, the more anodic phase
having the biggest removal rate. An example is gray cast iron, where the graphite
will stand in relief relative to the matrix. Also, at inclusions a problem exists. See
Fig. 8.6 showing mild steel polished mechanically a with visible inclusions, and
electropolished b with inclusions partly removed. This takes place because the
Fig. 8.6Mild steel mechanically polished with the inclusions clearly visible a, and elec-
trolytically polished with the inclusions partly removed by the polishing process b.
current density will increase around the inclusion so that material fromthe matrix
is preferably removed which causes a relief or even a dropout of the inclusion see
alsoFig. 1.6.
Lowremoval rate: The removal rate is relatively low, so incase of deepdeformation
in the specimen surface, the polishing time must be long, causing different arti-
facts to develop see below. Caused by the low removal rate, the deformations
fromthe grinding scratches are not removed and they are visible in the surface, as
shown in Fig. 8.7. This can be avoided if the grinding is done with a ner grit up to
P4000, or evena roughpolishing with9or 6 mis performed.
Badedge retention: Evenwhenthe edge of the specimenis protectedwitha lacquer
or mounted, the edge will be preferentially attackedandroundedsee Fig. 8.8.
Limited polished area: Depending on the available amperage restricting the cur-
rent density, the polished area is limited. Short time polishing performed on com-
Fig. 8.7Surface with deformations from grinding still visible after electrolytic polishing.
Fig. 8.8Edge rounding after electrolytic polishing.
mercial electropolishers takes place at 1 to 2 A/ cm
2
0.16 A/ in
2
. In most cases a
polisher is made for a maximumamperage of 10 Asee below.
ArtifactsUnplane Surface: Due to the different potentials mentioned above, all
variations in the specimen material tend to cause artifacts like increasing the size
of pores, preferential attack of differently oriented grains and pitting see Fig. 1.6.
The surface is often not plane but wavy, which causes problems at high magnica-
tions. See alsoSections 13.5.4and13.6.5.
8.2 Electrolytes
The electrolyte is an important factor in the electropolishing process. A good electro-
lyte should have a number of characteristics to support a good polishing and etching.
When choosing an electrolyte for polishing a metal, certain basic principles must be
taken into consideration. The electrolyte must have a low viscosity since the viscosity
determines the quality of the viscous layer that forms on the specimen surface. It must
be a good solvent for the anodic material under the prevailing electrolytic conditions.
The formation of any insoluble reaction products that deposits on the specimen sur-
face interferes with the polishing operation. The electrolyte should, preferably, not at-
tack the metal in the absence of the current, but it is not always possible. Similarly,
preference will be given to an electrolyte that can be used at roomtemperature, and is
little affected by changes in temperature, because in practice it is difcult to control
and maintain an exact electrolyte temperature during the polishing operation. Lastly,
the electrolyte must be stable andsafe tohandle.
The most used electrolytes are based on perchloric, phosphoric, hydrochloric, or
sulfuric acids mixed with ionizing solutions like acetic acid, alcohol, or water. Perchlo-
ric acid HClO
4
is by far the most universal acid suited for polishing of a great number
of metals. Unfortunately HClO
4
is a very dangerous substance that can cause explo-
sions, especially whenmixedwithacetic anhydride CH
3
CO
2
O. It is safe, however, to
use perchloric acid if the correct recommended recipes are used and the necessary pre-
cautions are taken see Section 13.3.2, Table 13.2. Nevertheless, use of perchloric acid
is not permitted in some laboratories. If possible, an electrolyte that is mixed with per-
chloric acid and acetic acid glacial should be avoided. The temperature of a perchlo-
ric acidelectrolyte shouldnot exceed30 to 35C90 to 100F.
It is practical to limit the number of electrolytes used in a laboratory from one to
three, covering most materials. With a general purpose electrolyte based on perchloric
acid covering aluminum/Al alloys, steel, stainless steel, zinc, lead, magnesium, tita-
nium, and other metals, supplemented with an electrolyte based on phosphoric acid
covering copper andcopper alloys, most needs shouldbe covered.
These twoelectrolytes are:
No. 1-1 Table 13.2 78 mL perchloric acid 60 %, 90 mL distilled water, 730 mL
ethanol 96%, 100 mLbutylcellosolve ethylene glycol monobutyl ether.
The perchoric acid which must be shipped and stored separately, should be added
tothe mixture of ethanol, butylcellosolve, andwater immediately before use.
This electrolyte has a lifetime of aroundtwomonths according touse.
Attention: With this and other perchloric acid electrolytes, they should never be
allowed to become more concentrated by evaporation of one or more of the compo-
nents water/ethanol during storage or use.
No. 3-2 Table 13.2 250 mLphosphoric acid, 500 mLdistilled water, 250 mLetha-
nol 96%, 50 mLpropanol n-propanol, 100%, 5 g urea carbamide.
Water, ethanol, and propanol are mixed and the acid is added under constant stir-
ring.
For more electrolytes see Table 13.2, ASTM Standard Guide for Electrolytic Pol-
ishing of Metallographic Specimens E1558 andRefs. 2,4, and9.
For Safety Precautions, see Section26.2.
8.3 Electropolishing in Practice
As already mentioned above electrolytic polishing has some limitations, but also has a
number of advantages. Before deciding on the use of electropolishing for a given mate-
rial a number of factors should be evaluated that are given below. See also Section
13.5.4and13.6.5.
8.3.1 Factors Inuencing Electrolytic Polishing
Material
The material must be electrically conductive and, if mounted, a good electrical connec-
tion should be secured. At the same time, the mounting material around the specimen
shouldnot be conductive see Section3.2.2.
Electrolyte
The right electrolyte compositionfor a givenmaterial shouldbe selected.
The Area to be Polished
When using a commercially available electropolisher see below, the specimen is
placed on a mask, dening the area to be polished. The area should be in relation to the
voltage/amperage current available. The smaller the area, the better, giving the best
polishing conditions and the lowest development of heat. Typically an area of
1 to 2 cm
2
0.16 to 0.32 in
2
is polished.
Voltage/Current
The voltage depends on the type of material and electrolyte. Usually the voltage creat-
ing the necessary amperage current toestablishthe correct current density is set.
The Flow of the Electrolyte
It is important that the reaction products established on the specimen surface during
the process are removed continuously and the temperature in the polishing chamber is
kept low. This is done by circulating the electrolyte through the chamber. At the same
time it is important not to create any air bubbles that are caused by a ow rate that is
toohigh.
The Temperature of the Electrolyte
The temperature should be kept as close to room temperature as possible. This gives
the best polish with high reproducibility. If the electrolyte is heated to temperatures
above 30 to 35C 90 to 100F, the process deteriorates and with electrolytes with
perchloric acid and ethanol, the risk of re and explosion will increase. Therefore, if
more than a few polishings are done in a short period of time, the electrolyte must be
cooled.
Time
The polishing time should be as short as possible to avoid the negative effects of the
electrolysis. For this reason it is important to prepare the specimen before the
electropolishing.
8.3.2 Example of Electrolytic Polishing/Etching
See MethodE1-01, Section13.3.6stating a muchusedmethodfor steel.
8.4 Electrolytic Polishing Equipment
Electropolishers have been commercially available for many years, both for normal
polishing in the laboratory and as portable polishers for polishing on the spot. Also,
apparatus for electrolytic thinning of specimens for TEMis available see Section 8.6.
Only electropolishers for normal polishing for laboratory use will be describedbelow.
8.4.1 Electropolishers for Laboratory Use
These are usually built in two parts: a polishing table, the cell where the actual polish-
ing is done, andanoperating unit containing electronics andsoftware.
The Polishing Table
The main components see Fig. 8.9 are: the polishing chamber with cathode and mask
upon which the specimen is placed, the electrolyte container with a pump circulating
the electrolyte, driven from outside the electrolyte container with a magnet, cooling
coil, anda contact beammaking anodic contact tothe specimen.
The specimen is placed with the surface to be polished against the exchangeable
mask. The mask has a hole of 0.5 to 5.0 cm
2
0.08 to 0.8 in
2
, allowing contact between
the electrolyte and the specimen. The cathode of stainless steel is placed in the bottom
of the polishing chamber and during the polishing/etching the pump circulates the
Fig. 8.9Schematic drawing of a polishing table for electrolytic polishing.
electrolyte through the chamber in a laminar ow. This owcan be adjusted. Often the
pump is driven magnetically as shown to avoid corrosion of metal parts. A cooling coil
of stainless, acid resistant steel is placed around the pump, through which cooling wa-
ter can be circulated to keep the electrolyte temperature constant, normally between
20 to 30C70 to 90F. Incertaincases a cooledliquidis circulatedmaking polishing
at sub 0C 32F temperatures possible. The container is exchangeable, and in this
way the electrolyte can be stored covered with a lid when not in use. This allows for the
least possible handling of the electrolytes.
The Operating Unit
The operating unit has controls for all process parameters and a power supply. Using a
microprocessor, storing of polishing methods is possible that saves time whendifferent
materials are tobe polished.
Electropolishers
Electropolishers are only made by a fewsuppliers; an example is shown in Fig. 8.10. It
has electrolyte temperature control and a load simulation mode for preselection of
polishing/etching voltages. Input topower source is 1 kVA.
8.5 Field MetallographyNondestructive Electropolishing
One of the very rst commercially available electropolishers in the 1940s was made for
nondestructive polishing. Only a spot of 1 mm 0.04 in in diameter was made, allow-
ing the tested product to be sold as new. This was done in the laboratory or at the
manufacturer, but today nondestructive polishing is mostly in the eld, on the spot
insitu, usedfor inspectionof workpieces suchas steampipes still infunction.
For the right type of materials see earlier in this chapter electropolishing is well
suited for nondestructive on the spot polishing because the polishing time is short.
Normally the same electrolytes and data are used as for normal electrolytic polishing
depending on the type of polisher used see Section 13.3.6. In most cases the spot to be
examined is rst treated mechanically see Section 7.11 to secure a deformation-free
Fig. 8.10Electrolytic polisher/etcher with electrolyte temperature control and a load
simulation mode for pre-selection of polishing/etching voltages. Input to power source is
1 kVA.
19
surface after electropolishing/etching. Often a replica is taken after polishing and etch-
ing see Sections 7.11.2and13.4.
Portable polishers consisting of a pencil with a polishing chamber to be pressed
against the work piece and a unit supplying electrolyte and anelectric current are com-
mercially available.
8.6 Electrolytic Thinning for TEM
In a transmission electron microscope TEM, normally a 3-mm 0.118 in diameter
specimen is used. This specimen must be very thin to allow for the TEM analysis, and
electropolishing is suited for thinning of conductive metal specimens. By electrolytic
thinning a hole is made in the specimen, and the edge of this normally is very thin, as
showninFig. 8.11.
The specimenis normally thinnedrst by grinding sothat a 3-mm0.118-in diam-
eter disk with a thickness of 0.5 to 0.1 mm0.02 to 0.004 in can be thinned. The thin-
ning is a normal electrolytic polishing as described above, except the thinning, in most
cases, takes place on both sides at the same time. This can actually be done in a glass
beaker, positioning the specimen as anode, with a lacquer to cover the edges so that
only the center is polished. This window technique is stopped when a hole is estab-
lished in the specimen, and it is quickly taken under water to avoid further attack. This
method is relatively laborious, giving less reproducible results; therefore, the commer-
cial jet thinners have been developed. See Fig. 8.12 which shows a cross section of the
polishing chamber. The specimen is placed in the middle in a movable holder. On each
side of the specimen holder a nozzle holder is placed with a nozzle leading the electro-
lyte owtoward the sides of the specimen. A cathode is placed at each nozzle. The pro-
cess is observed from one side either by watching or with a photocell reacting to the
light which breaks through the hole in the specimen created by the polishing process.
The light comes froma light source placed behind the specimen, and when the photo-
cell is hit the process stops automatically, ensuring a very small hole inthe specimen.
Electrolytes and data from normal electrolytic polishing can often be used, but in
Fig. 8.11Specimen of bronze for TEM. Electropolished with jets from two sides, 87 mA, 7.4 V,
5 min and 50 sec, electrolyte No. 3-2 Table 13.2, electrolyte temperature 5C 41F.
certain cases special electrolytes and temperatures, considerably below room tem-
perature, are needed to be able to effectively control the process. See the literature on
electrolytic thinning.
44
8.7 Chemical Polishing
Chemical polishing is a relatively simple method, comparable to electrolytic polishing,
only without an electric current. It is a process based on the electrolytic action that
takes place when a chemical solution gets into contact with the metal surface see also
Section 9.4.1. The chemical polishing solutions are developed so that material is re-
movedfromthe surface of the specimeninmuchthe same way as inelectrolytic polish-
ing. This means that chemical polishing has the same disadvantages as mentioned
above under electropolishing. The polishing is made by immersing the specimen into
the polishing solutionoftencombinedwitha rubbing toremove reactionproducts.
Due to the disadvantages of the method and the trouble/danger with handling of
chemicals, chemical polishing is not used much. Withcertainsensitive materials, how-
ever, like cadmium, lead, zinc, tin, and zirconium, chemical polishing might be useful
when mechanical polishing or electropolishing are unsuccessful. See the literature,
Refs. 2and9for further informationandfor chemical polishing solutions.
Fig. 8.12Schematic drawing of a polishing cell for electrolytic jet polishing for TEM. The
specimen placed in a holder for quick removal, is attacked from both sides simultaneously,
having two cathodes and the electrolyte in two jets conducted towards the specimen. Using a
photocell instead of an eye, the process can be switched-off immediately when the light
breaks through the specimen, assuring a very small hole in the specimen.
9
Etching
9.1 MicroetchingContrast
MICROETCHINGIS ETCHINGOFMICROSTRUCTURES TOBEOBSERVEDBY
magnicationhigher than2550inEurope. For macroetching, see Section9.7.
In the bright eld illumination BF of the light microscope, a prepared
metallographic/materialographic specimen will only show certain features like inclu-
sions, nonmetallic phases graphite, pores, cracks, etc. It is usually not possible to see
the microstructure because the light is reectedequally fromthe bright surface.
Figure 9.1 shows a steel specimen, unetched a, and chemically etched b, the
etched surface revealing the grains of the microstructure see also Fig. 1.10. To obtain
an image with the structure details, a contrast between the elements in the microstruc-
ture has to be established. The contrast can be caused by a number of methods see the
diagramFig. 9.2. The most important of these methods will be further discussed inthe
following sections. Chemical microetching of metals is covered by ASTM Standard
Practice for Microetching Metals and Alloys E 407, see also Section 12.5. For further
study see the literature, Refs. 2, 4, 9, 21, 26, 27, 4549.
9.2 Contrast Without Surface ModicationsMicroscope
Techniques
In the bright eld illumination BF of the light microscope only structure details that
differ in reectivity from one another can be distinguished from each other. For this
reason special microscope techniques have been developed, making it possible to ob-
serve certaindetails that cannot be observedinBF. See alsoPart III of this book.
9.2.1 Dark-Field Illumination DF
In dark-eld illumination, the light beam is angled to the specimen surface, making it
possible to observe details like inclusions and scratches that stand in relief to the sur-
rounding structure. This can be of advantage when observing some features, such as
lightly etchedgrainboundaries andlight scratches see Fig. 15.10.
9.2.2 Differential Interference Contrast DIC
This illuminationtechnique uses a beamsplitter todirect twobeams towards the speci-
men surface. This makes even very small differences in height relief visible, and DIC
can be used with great advantage using relief polishing see below, in this way avoid-
ing anadditional etching process see Fig. 15.14.
9.2.3 Polarized Light POL
Using polarized light the microstructure of anisotropic metals such as zirconium and
titaniumcan be observed without any treatment of the prepared surface. For isotropic
cubic metals, polarized light can be used when an anisotropic surface lm is estab-
169
lished on the specimen surface. In some cases a chemically etched surface can also be
observedonananisotropic material see Fig. 15.12.
9.2.4 Fluorescence
Some materials emit radiation when illuminated by certain types of light. Fluores-
cence can be used to distinguish pores and other surface details see Section 3.10 and
Fig. 3.14.
9.3 Contrast with Surface ModicationEtching
To obtain the necessary contrast so that a surface can be observed in bright eld in a
reected light microscope, a treatment, often called etching must take place. The
most used method is chemical etching based on an electrochemical attack of the sur-
face, but electrolytic etching and other methods such as physical etching are also
usedsee Fig. 9.2.
9.3.1 Grain Contrast Etching
To obtain grain contrast etching, certain grains in the specimen surface are inuenced.
Figure 9.3
18
shows 1 a grain in relief caused by relief polishing which could also be
established by ion etching see below; 2 grains which are differently attacked by the
Fig. 9.1Unetched steel specimen. a Only the inclusions can be seen. b Etched in 3 % Nital
100 mL ethanol 96 %, 3 mL nitric acid 65 % revealing the grains.
etchant; 3 a grain covered by an interference layer lm that is selectively deposited;
4 a layer deposited independently of the grains; and 5 the lm deposited according
tothe orientationof the grains.
9.3.2 Grain Boundary Etching
In this type of etching the grain boundaries only are attacked see Fig. 9.3. Figure 9.3
shows: 6 a grain boundary attacked by chemical etching; and 7 a grain boundary
after treatment under heat andvacuum.
9.3.3 Reproducibility
During the preparation of the specimen, the process of making a contrast shall be re-
producible. It is important that the etching process does not introduce artifacts, but
Fig. 9.2Diagram showing the methods to create surface contrast.
Fig. 9.3Schematic drawing of grain contrast etching. 1 Relief polishing, 2 grains
differently attacked, 3 grain covered with interference layer, 4 layer deposited
independently of the grains, 5 lm deposited according to the orientation of the grains, 6
grain boundary etch, 7 grain boundary treated under vacuum and heat.
Chapter 9 Etching 171
ensures that the true structure is revealed. This is particularly important when image
analysis is tobe performedonthe specimeninquestionsee Part IV.
Typical artifacts developed during etching are stains if the specimen surface was
not properly cleaned after the last polishing step. Also pitting and other artifacts can be
developedat over-etching.
9.3.4 Safety Precautions
Especially in chemical etching it is important to take necessary safety precations. Be-
fore using or mixing any chemical, all product labels and pertinent Material Safety
Data Sheets MSDS should be read and undertood concerning all of the hazards and
safey precautions tobe observedsee Section26.2.
9.4 Classical Etching
9.4.1 Chemical Etching
The most commonly used method for creating the necessary contrast in the specimen
surface is chemical etching, alsocalleddissolutionetching.
2,4,9,21,26,4547
Chemical etching is a process based on the electrolytic action that takes place
when a chemical solution etchant is in contact with a metal surface. The etchant, nor-
mally having a reduction component that is usually an acid, an oxidizer compo-
nent, and a modier component, causes an electric potential between differently ori-
ented grains, different phases, grains and boundaries, inclusions, and matrix, etc. The
difference in attack, which is the amount of material removed from the single details,
reveals the structure. For electrolytic etching, where the specimen is placed as an an-
ode inanelectrolytic cell, the appliedcurrent acts as the oxide component.
Anumber of etchants for chemical etching are statedinTable 12.2.
9.4.2 Precipitation Color Etching
This etching method, also called color etching or tint etching, uses a chemical etchant
that reacts with the specimen surface and deposits a very thin insoluble lm. The lm
acts as aninterference layer producing colors inbright eld illuminationand polarized
light. Variations in the grains inuence the observed colors. Precipitation etching re-
quires a high quality of the prepared specimen; even small scratches or deformations
will be visible whenthe lmis established.
46,47
9.4.3 Heat Tinting
Oxidizing will take place on the surface of metal specimens that are heated to tempera-
tures in the range 250 to 700C 500 to 1300F in air. The oxidized lm will vary in
thickness according to the variations in the specimen material. If the layer is thicker
than 30 nm, interference colors can be seen in the bright eld of the microscope. Heat
tinting is not suited for carbon steels and low-alloy steels, but works well with high-
alloy steels, tool steels, stainless steels, titanium, andother metals.
9.5 Electrolytic Etching
9.5.1 Anodic Etching
Anodic etching, also known as electrolytic etching, is in principle the same as chemical
etching, except in this case the specimen is placed as an anode in a galvanic cell. This
means that material is removed fromthe specimen surface, causing an etching and not
a polishing as with electrolytic polishing see Fig. 8.1. The etching takes place because
the voltage andcurrent density are lowsee Fig. 8.4.
Frequently, electrolytic etching can be performed as the second step of the
polishing-etching process, using a voltage of approximately 1/ 10 that used as the pol-
ishing voltage. In many cases, however, the electrolyte suited for polishing cannot be
used for etching. In this case, electrolytic etching often takes place using a stainless
steel vessel connected as a cathode containing the etchant. The specimen is handled
with a pair of tongs, connected as an anode, and a suitable low direct current is estab-
lished between the cathode and anode. An example is etching of stainless steel that can
be electrolytically etched inanelectrolyte etchant of 10 g oxalic acid in100 mLwater,
using a voltage of 6 V in 10 to 15 s. A number of etchants for electrolytic etching are
statedinTable 12.2.
9.5.2 Anodizing
During this process that is closely relatedtoelectrolytic etching/polishing, a layer, often
an oxide lm, is established on the surface of the specimen see Fig. 9.335. This in-
terference layer will produce a colored image in bright eld illumination and with po-
larized light. The layers can be related to the layers created at precipitation etching,
heat tinting, andvapor deposition.
9.5.3 Potentiostatic Etching
A reproducible, selectively working electrolytic etching is made with an electronic po-
tentiostat and a reference electrode. With the potentionstat it is possible to establish a
constant potential at the specimensurface anode.
Because of the controlled etching process, potentiostatic etching is very well
suited for selective etching of desired microstructural constituents with high repro-
ducibility.
9.6 Physical Etching
9.6.1 Relief Polishing
Insome cases it is possible to establisha contrast by relief polishing that creates a small
relief betweenthe grains or the grainboundaries, or bothsee 1 inFig. 9.3.
Relief polishing is oftendone witha relatively resilient clothsee Section7.4 and a
very ne polishing mediumlike colloidal silica or alumina see Section 7.5. Relief can
alsobe establishedthroughchemical mechanical polishing see Section7.12.
Relief polishing should only establish a very small relief between the single grains
or other constituents, not to disturb the microstructure; therefore, often DIC is used
whenexamining relief polishedsurfaces see Section9.2.2.
9.6.2 Ion Etching
This method, also called ion beametching, uses an ion bombardment of the specimen
to remove material fromthe single grains, depending onorientationand phase compo-
sition. Ion beam etching can be used for thinning of specimens for transmission elec-
tron microscopy TEM as an alternative to electropolishing see Section 8.6. It is,
however, also suited for etching microstructures, especially of nonconductive materi-
als for materialographic examination.
48
The ions, often argon, are supplied in a strong
vacuum104 mbar by an ion gun towards the specimen which is often placed so that
the surface is bombardedunder anangle.
9.6.3 Thermal Etching
Thermal etching takes place at high temperatures in an oven with an inert atmosphere
or vacuum. Both metals and ceramics can be thermally etched. During the process
grooves are formed in the grain boundaries/phase boundaries and grain surfaces are
curved. The method can be used at high-temperature microscopy for metals, but ther-
mal etching is mostly used for etching of ceramics taking place at temperatures be-
tween1000and1400C1800and2500F.
26
9.6.4 Vapor Deposition
Interference lms can be established on the specimen surface by vacuumdeposition of
a suitable material. This method Pepperhof will enhance the irregularities in the pol-
ished surface and the structure will be visible through the interference between the
light reected from the top of the lm and the specimen surface. The lm materials
shall have a high refractive index; ZnS, ZnTe, ZnSe, and TiO
2
are often used. The pro-
cess takes place ina chamber witha vacuumof about 105 mbar.
49
9.6.5 Sputtering
SputteringCathodic Discharge
Interference layers lms can be produced by sputtering. In sputtering, materials like
carbon, gold, or gold-palladium alloys are atomized by bombarding a surface target
withhighenergy particles. Positively chargedgas ions producedby electrical discharge
1 to 5kV dc are accelerated by a potential difference between the anode specimen
and cathode target so that they bombard the cathode, thereby dislodging atoms that
leave the surface in all directions. These atoms settle on the specimen surface where
they form the desired layer. If undesirable reactions with the target material shall be
avoided, the process shall take place at 0.03 to 0.05 mbar inaninert gas like argon.
49
Reactive Sputtering
At reactive sputtering, not an inert gas, but an atmosphere of oxygen is used. This
means that the atomized target material is oxidized, forming oxidic layers on the
specimen.
49
9.7 Macroetching
Macroetching can be dened as revealing the macrostructure for examination with the
naked eye or at a magnications up to 10, either direct or by using sulfur prints Bau-
mannprints.
Macroetching is consideredoutside the scope of this book.
Macroetching is described in great detail in the three following ASTM standards
see alsoSection12.4.
Standard Test Method for Macroetching Metals and Alloys E 340. This standard
is very comprehensive covering a wide range of materials.
Standard Methods for Macrotech Testing Steel Bars, Billets, Blooms, and Forging
E381
Standard Practice for Preparing Sulfur Prints for Macrostructural Examination
E1180
References Part I
1 Crowther, D. S. and Spanholtz, R. B., ANew Name for Metallography? Try Materialogra-
phy, Metal Progress, September 1968, p. 21.
2 Petzow, G., Metallographic Etching, ASMInternational, Materials Park, Ohio, USA, 1999.
3 Petzow, G. and Mcklich, F., Microstructure-Fascinating Variety in Stringent Rules, Practi-
cal Metallography, Vol. 33, 1996, pp. 6482.
4 ASM Handbook, Metallography and Microstructures, Volume 9, ASM International, Materi-
als Park, Ohio, USA, 2004.
5 Edyvean, R. G. I. andHammond, C., Journal of Historical Metallurgy, October 1998.
6 Vilella, J. R., Metallographic Technique for Steel, American Society for Metals, Cleveland,
Ohio, USA, 1938.
7 Samuels, L. E., Metallographic Polishing by Mechanical Methods, ASMInternational, Materi-
als Park, Ohio, USA, 2003.
8 Bjerregaard, L., Geels, K., Ottesen, B., and Rckert, M., Metalog Guide, Struers A/S, Copen-
hagen, Denmark, 2000.
9 Vander Voort, G. V., Metallography Principles and Practice, ASM International, Materials
Park, Ohio, USA, 1999.
10 Malkin, S., Grinding Technology, Ellis HorwoodLtd., Chichester, UK, 1989.
11 Shaw, M. C., Principles of Abrasive Processing, ClarendonPress, UK, 1996.
12 Shaw, M. C., Farmer, D. A., and Nakayama, K., Mechanics of the Abrasive Cut-Off Opera-
tion, Journal of Engineering for Industry, August 1967.
13 Nelson, J. A. and Westricht, R. M., Abrasive Cutting in Metallography, Metallographic
SpecimenPreparation, PlenumPress, PlenumPublishing.
14 Wellner, P., Investigations on the Effect of the Cutting Operation on the Surface Deformation
of Different Materials, Practical Metallography, Vol. 17, 1980, p. 525.
15 Geels, K., Andersen, A. T., and Damgaard, M., An Analysis of Two Principles of Abrasive
Cutting in Materialographic Cut-Off Machines, Proceedings, MC95 International Metal-
lography Conference, ASMInternational, Materials Park, Ohio, 1996, p. 251.
16 Cloeren, H. H., Thermische und mechanische Probenentnahme und deren Einuss auf das
wahre Gefge, Fortschritte in der Metallographie, Vol. 33, Werkstoff-
Informationsgesellschaft mbH, Frankfurt, Germany, 2002, p. 309.
17 Geels, K., Mller, G., and Sorensen, J. I., Oberchenphenomene beimmaterialographischen
Nasstrennschleifen, Fortschritte in der Metallographie, Vol. 34, Werkstoff-
Informationsgesellschaft mbH, Frankfurt, Germany, 2003, p. 93.
18 Waschull, H., Prparative Metallographie, Wiley-VCHVerlag, Weinheim, Germany, 1993.
19 Courtesy of Buehler, Ltd.
20 Courtesy of Struers A/S.
21 Bramtt, B. L. and Benscoter, A. O., Metallographers Guide, Practices and Procedures for Iron
andSteels, ASMInternational, Materials Park, Ohio, USA, 2002.
22 Barrett, J., Electric Discharge Machining, Metallographic Specimen Preparation, Ple-
numPress, PlenumPublishing Corporation, NewYork, USA, 1974, p. 69.
23 Technical documents fromDoALLCompany, Des Plains, Illinois, USA, 2004.
24 Nelson, J. A. andSlepian, R. M., Practical Metallography, Vol. 7, 1970, p. 510.
25 Glancy, S., Structure, Vol. 22, 1990, p. 14.
26 Carle, V., Schfer, U., Tffner, U., Predel, F., Telle, R., and Petzow, G., Ceramography of High
Performance Ceramics: Description of the Materials, Preparation, Etching Techniques, and
Description of the Microstructure, Practical Metallography, Part I, Ceramographic Etch-
ing, Vol. 28, 1991, pp. 359377; Part II, Silicon Carbide, Vol. 28, 1991, pp. 420434; Part III,
Zirconium Oxide, Vol. 28, 1991, pp. 468483; Part IV, Aluminum Nitride, Vol. 28, 1991, pp.
542552; Part V, Silicon Nitride, Vol. 28, 1991, pp. 592610; Part VI, High-Temperature Su-
perconductor YBa
2
Cu
3
O
7
, Vol. 28, 1991, pp. 633648; Part VII, Boron Carbide, Vol. 31, 1994,
pp. 218233; Part VIII, AluminumOxide, Vol. 32, 1995, pp. 5476.
27 Elssner, G., Hoven, H., Kiessler, G., and Wellner, P., Ceramics and Ceramic Composites: Mate-
rialographic Preparation, Elsevier Science Inc., NewYork, USA, 1999.
28 Exner, E. andKuhn, K., Practical Metallography, Vol. 8, 1972, pp. 453469.
29 Bouseld, B., Surface Preparation and Microscopy of Materials, John Wiley & Sons, Chi-
chester, UK, 1992.
30 Damgaard, M. J., Bjerregaard, L., and Geels, K., Practical Metallography, Vol. 8, 2001, pp.
466476.
31 Beilby, G., AggregationandFlowof Solids, MacMillanandCo. Ltd., London, UK, 1921.
32 Luo, J. and Dornfeld, D. A., Material Removal Mechanism in Chemical Mechanical Polish-
ing: Theory and Modeling, IEEE Transactions on Semiconductor Manufacturing,
2000.
33 Geels, K. andGillesberg, B., Practical Metallography, Vol. 37, 2000, pp. 150159.
34 Burgess, D. and Blanchard, R. A., Wafer Failure Analysis for Yield Enhancement, Accelerated
Analysis, Half MoonBay, California, USA, 2001.
35 Ross, Boit, and Staab, Eds., Microelectronics Failure Analysis, ASM International, Materials
36 Wulff, F. W. andArens, T., Structure, Vol. 32, 1998, p. 9.
37 Reiter, K., Reiter, M., andArens, T., Structure, Vol. 34, 1999, p. 12.
38 Katrakova, D., Damgaard, M., andMcklich, F., Structure, Vol. 38, 2002, p. 19.
39 Kopp, W.-U. andLinke, U., Practical Metallography, Vol. 17, 1980.
40 Trempler, J., Practical Metallography, Vol. 5, 2001, pp. 231269.
41 Trempler, J., Practical Metallography, Vol. 10, 2003, pp. 481531.
42 McG. Tegart, W. J., The Electrolytic and Chemical Polishing of Metals inResearchand Industry,
PergamonPress Ltd., London, 1956.
43 Knuth-Winterfeld, E., Korttidsmetoder til metallogrask elektropolering ved stuetemperatur,
C. A. Reitzel, Copenhagen, Denmark, 1952.
44 Thompson-Russell, K. C., and Edington, J. W., Monograph Five, Electron Microscope Speci-
men Preparation Techniques in Materials Science, N. V. Philips Gloeilampenfabrieken, Eind-
hoven, Holland, 1977.
45 Beckert, M. and Klemm, H., Handbuch der metallographischen tzverfahren, Deutscher Ver-
lag fr Grundstofndustrie, Leipzig, Germany, 1984.
46 Beraha, E. and Shipgler, B., Color Metallography, American Society for Materials, Materials
47 Weck, E. and Leistner, E., Metallographic Instructions for Colour Etching by Immersion, Part
I 1982, II 1983 and II 1986, Deutscher Verlag fr Schweisstechnik GmbH, Dsseldorf,
Germany.
48 Grff, I., Practical Metallography, Vol. 36, 1999, pp. 669684.
49 Bhler, H. E. and Hougardy, H. P., Atlas of Interference Layer Metallography, Deutsche Gesell-
schaft fr Materialkunde, Oberursel, Germany, 1980.
Part II:
Metallographic/Materialographic
Specimen PreparationA Hands-On
Manual
10
Introduction
THE GOAL FOR ANY METALLOGRAPHIC/MATERIALOGRAPHIC PREPARA-
tion is a true microstructure, or at least a structure that makes a correct analysis of a
structure detail possible. It should be stressed that an examination with a subsequent
interpretation, using a light microscope or other method, is of no use if the prepared
microstructure is not correct.
This part of the book is made to guide the reader directly towards the correct
preparation of the microstructure for most materials and material groups. To obtain
more information on the true structure, a more detailed description of the total prepa-
rationprocess andthe theories behindit, see Part I of this book.
Before starting a preparation process, two facts must be considered: Specimen
Material andPurpose of Examination.
10.1 Specimen Material
The specimenmaterial, inthe following material, is decisive for the choice of a prepara-
tion process. It is evident that soft, hard, ductile, brittle, homogenous, heterogeneous,
etc., materials cannot be treatedthe same way toobtaina correct result.
To ndthe correct preparationmethodfor a givenmaterial, the reader shall review
Table 11.1 and nd the material or group of materials corresponding to the given mate-
rial see below.
10.2 Purpose of Examination
Before a preparation method is selected, the purpose of examination, in the following
the purpose, should be considered. A given material can be prepared often electrolyti-
cally in a relatively short time for one purpose, and for another purpose, a longer me-
chanical preparation sequence should be performed. An example is medium carbon
steel. If the purpose of examination is the study of grain size, the electrolytic polishing
method El-01, Section 13.3.6, can be used, having a total preparation time of approxi-
mately 3 min, including grinding less than 3 min and polishing/etching 1012 s. If
the purpose is examination of inclusions, the mechanical methods, C-28 and T-28, Sec-
tion13.2.3, are recommendedwitha total preparationtime of 1012 min.
Based on the purpose, the user will select the correct process/method stated in the
Material/Preparation Tables. Other information connected to the purpose, such as
etchants, will be statedalso.
10.3 Specimen Preparation
Modern specimen preparation is based on a systematic approach, and in this way se-
curing the reproducibility that is a must in both research and quality control. In the
Material/Preparation Tables, Section 13.2.3, the total preparation process is stated, in-
179
cluding sectioning, mounting, grinding/polishing methods mechanical and electro-
lytical, andetching. Mechanical polishing canbe done by handandis alsodescribedin
this part of the book, but for the indicated methods, a semiautomatic grinder/polisher
is recommended.
A section covering trouble shooting of all stages of the preparation process, and
how to analyze the used preparation method to avoid or overcome artifacts is also in-
cludedinPart II.
11
Specimen MaterialTable 11.1
THE SPECIMENMATERIAL, COMBINEDWITHTHE PURPOSE OF EXAMINA-
tion, is decisive for the choice of preparation process/method. Two physical properties,
hardness and ductility, are important in selecting a specic preparation method, but
conditions suchas coatings or composites alsoplay animportant role.
In Table 11.1, Section 11.3, most materials and the most common material combi-
nations are indicated to guide the reader to a preparation process/method best suited
for a specic material statedinthe Material/PreparationTables, Section13.2.3.
11.1 Classication of Materials
A classication of all available materials is needed to guide the reader to a specic ma-
terial in an efcient way. This is done by dening twelve main groups partly based on
material composition, such as ceramics, ferrous metals, etc., and on other impor-
tant features like coatings, electronic components, etc. The twelve main groups are
statedalphabetically see below.
The main groups are split into a number of subgroups. An example is the main
group Ceramics, which has ve subgroups: Carbides, Nitrides, Oxides, Traditional Ce-
ramics, andOther Ceramics.
These subgroups leadtothe specic material or material group, e.g., under Ceram-
ics, Oxides: Al
2
O
3
, BaTiO
3
, CaO, CeO
2
, Cr
2
O
3
, MgO, SiO, ZnO, ZrO
2
, andOther Oxides.
The twelve maingroups alphabetic:
Ceramics
Coatings
Composites andReinforcedMaterials
Electronic Components
Ferrous Metals
Mineralogical Materials
Nonferrous Metals
Organic Materials
Polymers
Powder Metals
SinteredCarbides
11.2 How to Use Table 11.1
When a given material or material group should be found in the table, the main group
most likely will be evident such as Ceramics, Coatings, Ferrous Metals, Polymers, etc.
If in doubt, a look at the subgroups will often lead the way to the material or material
group. Inthe case of analloy, the material shouldbe foundaccording to the component
with the highest content. Example: The superalloy: 48 %Ni, 25 %Co, 19 %Cr, 7.5 %Fe,
0.5 % Ti, is classied under the main group Nonferrous Metals, subgroup Nickel and
Nickel Alloys.
181
When the material material group is found, two or more Methods with Method
Numbers are indicatedinthe same row. Nowgo to Section13.2.3 andndthe Material/
Preparation Tables with the same number. A number of purposes with corresponding
preparation methods are indicated here see Chapter 12, and the method correspond-
ing tothe correct purpose is selected.
11.3 Table 11.1Materials/Methods
TABLE11.1Materials/Methods.
Material Group/Material (Alphabetical)
Method
(SeeSection13.2.3/3.6)
Ceramics Bioceramics Hydroxyapatite Coating T-01, C-01
Bioceramics, Others T-05, C-05, T-06, C-06
Carbides B
4
C T-02, C-02
CrC T-03, C-03
SiC T-02, C-02
TaC T-03, C-03
TiC T-03, C-03
WC T-03, C-03
Nitrides CBN T-03, C-03
Si
3
N
4
T-04, C-04
TiN T-03, C-03
Other Ceramics T-03, C-03
Oxides Al
2
O
3
T-05, C-05
BaTiO
3
T-06, C-06
CaO T-06, C-06
CeO
2
T-06, C-06
Cr
2
O
3
T-05, C-05
MgO T-06, C-06
SiO T-06, C-06
UO
2
T-68, C-68
ZnO T-06, C-06
ZrO
2
T-06, C-06
Oxides, Others T-05, C-05, T-06, C-06
Borides T-06, C-06
Traditional Glasses, Optical Fibers T-07, C-07
Ceramics Porcelain T-06, C-06
Slag T-06, C-06
Tile T-06, C-06
Other Traditional Ceramics T-06, C-06
Coatings Electrolytically Anodized Coatings T-08, C-08
Deposited GalvanizationPlated Coatings T-09, C-09
Other Electrolytically Deposited T-09, C-09
Other Coatings CVD T-08, C-08
Diffusion Coatings T-09, C-09
Hot Dip Zn-Coating T-10, C-10
Other Zn-based Coatings T-10, C-10
PVD T-08, C-08
TABLE11.1(Continued.)
Method
Paint Layers T-11, C-11
Other Coatings T-09, C-09
Thermal Spray Flame T-12, C-12
Coatings HVOF (High Velocity Oxygen
Fuel)
T-12, C-12
Plasma Spray Coatings
Metallic Layers
T-13, C-13
Ceramic Layers
T-14, C-14
Composite Layers
T-15, C15
Other Thermal Spray Coatings T-12, C-12
Composites SiC Fibers in Ti Matrix T-16, C-16
and Glassber Reinforced Plastic T-17, C-17
Reinforced Other Composite Materials T-18, C-18
Electronic Ceramic Capacitors T-19, C-19
Components Components Resistors T-19, C-19
Diodes T-19, C-19
YBCO Ceramic Super
Conductors
T-20, C-20
Metallic Germanium, Silicon, Si Wafers T-21, C-21
Components Microelectronic Material C-22
(Semiconductor Device)
Resistors T-23, C-23
Solderballs T-24, C-24
Other Metal Components T-23, C-23
Polymer Capacitors, Other Electronic T-25, C-25
Components Components
Microelectronic Packages,
Integrated
T-24, C-24
Circuits, Transistors T-26, C-26
PCB Coupon T-27, C-27
Other Microelectronic Devices T-26, C-26
Ferrous Carbon Steels High Carbon Steels T-28, C-28, E1-01
Metals Low Carbon Steels T-29, C-29, El-02
Medium Carbon Steels T-28, C-28, El-01
Cast Irons Gray Cast Iron, T-30, C-30, El-03
Lamellar
Cast Iron, T-30, C-30, El-03
Malleable
Cast Iron, T-31, C-31, El-03
Nodular
Cast Iron, White T-32, C-32, E1-03
Cast Iron, others T-28, C-28, El-03
Heat Treated Heat Treated, High-Alloy Steels T-33, C-33, El-04
Chapter 11 Specimen Material 183
Method
Steels Heat Treated, Low-Alloy Steels T-33, C-33, El-04
High-Alloy Stainless Steels T-34, C-34, El-05
Steels Super Alloys, Fe-Based T-35, C-35, El-06
Other High-Alloy Steels T-33, C-33, El-05
Low-Alloy High Strength Low-Alloy Steels T-36, C-36, El-04
Steels Other Low-Alloy Steels T-34, C-34, E1-04
Other Ferrous T-33, C-33, E1-02
Metals
Pure Iron T-34, C-34, El-07
Surface Treated Carbonitrided Steels T-37, C-37
Steels Carburized Steels T-37, C-37
Nitrided Steels T-37, C-37
Other Surface Treated Steels T-37, C-37
Tool Steels High Speed Steels T-38, C-38, El-08
Low-Alloyed Tool Steels T-38, C-38, El-09
Tool Steels, Others T-38, C-38, El-09
Mineralogical Constructed Portland Cement Clinker,
Concrete
T-39, C-39
Materials Materials
Natural Minerals T-40, C-40
Ores T-40, C-40
Nonferrous Aluminum and Pure Aluminum T-41, C-41, El-10
Metals Al Alloys Cast AluminumAlloys T-41, C-41
Wrought AluminumAlloys T-43, C-43, El-10
Other AluminumAlloys T-42, C-42, El-10
Americium See Material/
Preparation
Tables 68
Antimony and Pure Antimony T-44, C-44, El-10
Sb Alloys Antimony Bearing Alloys T44, C-44, El-10
Other Sb Alloys T-44, C-44, El-10
Beryllium and T-45, C-45, El-10
Be Alloys
Bismuth and Bi T-44, C-44, El-10
Alloys
Cadmium See Material/
Preparation
Tables 68
Chromium and T-46, C-46, E1-11
Cr Alloys
Cobalt and Co Pure Cobalt, Cobalt Alloys T-47, C-47, El-12
Alloys Super Alloys, Cobalt-Based T-48, C-48, El-12
Copper and Cu Pure Copper T-50, C-50, El-13
Alloys Brass T-49, C-49, El-13
Bronze T-49, C-49, El-14
Method
Copper Bearings Alloys T-50, C-50, El-14
Other Copper Alloys T-49, C-49, E1-13
Germanium T-21, C-21
Gold and Au T-51, C-51
Alloys
Hafnium and
Hf Alloys
T-62, C-62, El-11
Indium See Material/
Preparation
Tables 68
Iridium and Ir T-57, C-57
Alloys
Lead and Pb T-52, C-52, E1-15
Alloys
Magnesium
and
T-53, C-53, E-16
Mg Alloys
Manganese and T-54, C-54, El-01
Mn Alloys
Mercury and
Amalgams
See Material/
Preparation
Tables 68
Molybdenum
and Mo Alloys
T-55, C-55, E1-01
Neptunium See Material/
Preparation
Tables 68
Nickel, Ni T-56, C-56, El-17
Alloys and Ni-
Based Super
Alloys
Niobium and T-55, C-55
Nb Alloys
Osmium and
Os Alloys
T-57, C-57
Palladium and T-57, C-57
Pd Alloys
Platinum and
Pt Alloys
T-57, C-57
Plutonium See Material/
Preparation
Tables 68
Rare Earth
Metals
See Material/
Preparation
Tables 68
Rhenium and T-55, C-55
Method
Re Alloys
Rhodium and T-57, C-57
Rh Alloys
Ruthenium and T-57, C-57
Ru Alloys
Selenium See Material/
Preparation
Tables 68
Silicon T-21, C-21
Silver and Ag T-58, C-58, E1-18
Alloys
Tantalum and T-55, C-55
Ta Alloys
Tellurium See Material/
Preparation
Tables 68
Thallium See Material/
Preparation
Tables 68
Thorium See Material/
Preparation
Tables 68
Tin, Sn
Bearing
T-59, C-59, E1-19
Alloys and
Other Sn
Alloys
Titanium and
Ti Alloys
T-60, C-60, E1-20
Tungsten and
WAlloys
T-55, C-55, E1-21
Uranium and T-68, C-68
Uranium
Dioxide
Vanadium and
VAlloys
T-55, C-55, E1-22
Zinc and Zn T-61, C-61, E1-23
Alloys
Zirconium and T-62, C-62, E1-24
Zr Alloys
Zircalloy
Organic Biological T-63, C-63
Materials Materials
Bone
Teeth
Tissue
Method
Carbon, Coal, T-63, C-63
Graphite
Paper, T-63, C-63
Wood
Other Organic T-63, C-63
Materials
Polymers Elastomers Elastomers, Others T-64, C-64
EPDM Polymers T-64, C-64
Silicone T-64, C-64
Thermoplastics Acrylic (CS) T-64, C-64
Acrylonitril Butadicne Styrene T-65, C-65
(ABS)
Polyamid (PA) T-64, C-64
Polycarbonate (PC) T-65, C-65
Polyester, Saturated T-65, C-65
Polyethylene (PE) T-64, C-64
Polymethylmethacrylate
(PMMA)
T-65, C-65
Polyoxymethylene (POM) T-65, C-65
Polypropylene (PP) T-64, C-64
Polystyrene (PS) T-64, C-64
Polyvinylchloride (PVC) T-64, C-64
Thermoplastics, Others T-64, C-64
Thermosetting Epoxy T-65, C-65
Plastics Phenolic Resins (PF) T-65, C-65
Polyester, Unsaturated T-65, C-65
Polyurethane (PUR) T-65, C-65
Other Thermosetting Plastics T-65, C-65
Powder
Metals
Ferrous Powder
Metals
Nonferrous T-66, C-66
Powder Metals
Sintered Cemented T-67, C-67, E1-25
Carbides Carbides,
(Cemented
Carbides)
(Hard metals),
Coated
Sintered
Carbides and
Other Sintered
Carbides
12
Purpose of Examination
12.1 Purpose in General
FOR A GIVEN MATERIAL SEVERAL PREPARATION METHODS WILL USU-
ally be available, however, the correct method should be chosen based on the purpose
of examination. For this reason, a number of relevant purposes are stated with each
material/methodinthe Material/PreparationTables, see Section13.2.3.
Table 12.1 shows a number of the most common purposes of examination. It is
expressedinthe following text andinthe table as purpose. Most of these purposes are
coveredby one or more ASTMstandards and, inthis case, the standards is indicated.
For a given material also microetching is performed in accordance with the pur-
pose of the examination, and therefore also chemical microetching with a list of
etchants Table 12.2 is statedinthis chapter.
12.2 Purpose: ASTM Standards
A preparation is made very often to be able to make an examination according to an
ASTM standard. Section 12.4 lists all ASTM standards commonly used in metallogra-
phy and materialography and a Document Summary of each standard is indicated in a
CD-ROMincludedwiththis manual.
Other relevant standards ISO, BSI, DIN, etc. are stated in Appendixes I and II. In
Table 12.1, the ASTMstandards are shownrelating topurpose.
12.3 Table 12.1: Purpose/ASTM Standards
Table 12.1indicates a number of common purposes of examination with the most im-
portant ASTM standards, if any. Not all applicable standards are listed in this table,
only some of the more pertinent ones.
As part of each Material/Preparation Tables Section 13.2.3, a similar table will be
stated, but only the purposes and the ASTM standards, relevant for the material de-
scribedinthe Material/PreparationTables, will be indicated.
12.4 ASTM StandardsMetallography
12.4.1 Introduction
The metallographic eld is covered by ASTM with a number of documents of the fol-
lowing types:
Guidea compendium of information or series of options that doesnt recom-
menda specic course of action.
Practicea denitive set of instructions for performing one or more specic op-
erations or functions that does not produce a test result.
188
Specicationan explicit set of requirements to be satised by a material, prod-
uct, system, or service.
Terminologya document comprising denitions of termsexplanation of sym-
bols, abbreviations, or acronyms.
Test Methoda denitive procedure that produces a test result.
Most of the standards covering metallography and materialography are published
in the Annual Book of ASTM Standards, Volume 03.01, MetalsMechanical Testing;
Elevated and Low-Temperature Tests; Metallography ASTM Stock Number:
S030100.
The standards covering metallography, including Microindentation Hardness
Testing, are under the jurisdiction of ASTMCommittee E4. Those covering other types
of hardness testing are under ASTMCommittee E28.
Designation
Each standard has a serial designation prexed to the following title, the number fol-
lowing the dash indicates the year of original adoption as a standard or, in the case of
revision, the year of the last revision. Thus, standards adopted or revised during the
year 2003 have as their nal number, 03. A letter following this number indicates more
than one revision during that year, that is, 03a indicates the second revision in 2003,
03b, the third revision, etc. Standards that have been reapproved without change are
indicated by the year of last reapproval in parentheses as part of the designation num-
ber, for example, 2003. A superscript epsilon indicates an editorial change since the
last revisionor reapproval-1 for the rst change, 2 for the secondchange, etc.
TABLE 12.1Purpose/ASTM Standards.
Purpose (alphabetic): ASTM Standard (See Section 12.4)
Case or coating thickness/hardness B 487, B 578, B 748, B 931, B 933, B 934, C 664,
Surface layers E 1077
Perfect edge retention
Graphite in cast iron A 247
Grain size, grain boundaries B 390, E 112, E 930, E 1181, E 1382
Heat-inuenced zone E 1077
Heat treatment
Image analysis, rating of inclusion content E 45, E 562, E 768, E 1077, E 1181,
High planeness E 1245, E 1268, E 1382, E 2109
Inclusions in steel B 796, E 45, E 768, E 1245
Microhardness, hardness B 578, C 730, C 849, C 1326, C 1327, E 10,
E 18, E 92, E 103, E 110, E 140, E 384, E 448
Microstructure A 247, A 892, B 657, B 665, E 3, E 45, E 112, E
407, E 562, E 768, E 883, E 930, E 1077, E 1122, E
1181, E 1245, E 1268, E 1351, E 1382, E 1558, E
1920, E 2015, E 2109, E 2283
Phase identication A 247, B 657
Porosity B 276, E 2109, F 1854
Structure changes (forging)
Thermal sprayed coatings: Distribution, porosity,
unmelted particles
E 1920, E 2109
Chapter 12 Purpose of Examination 189
In this manual, only the serial designations are indicated because the following
numbers are continuously changed.
12.4.2 ASTM Standards in this Book
All ASTM standards mentioned under METALLOGRAPHY in Volume 03.01 and oth-
ers, relating to the subjects covered by this book, are listed below. Most of these will be
stated as DOCUMENT SUMMARY in Section 12.4.3. The listed standards should not
be considered as a complete list of standards covering the subject of metallography/
materialography and related subjects. Also, a fewspecications covering materials are
shownas examples.
The standards listed are based on the situation as per October 2006, and this situa-
tion will change due to the development of new standards and the revision or deletion
of oldstandards.
ASTM Standards Listed by Subject Alphabetically
Coatings
Test Methods for:
B 487 Measurement of Metal and Oxide Coating Thickness by Microscopical Ex-
aminationof a Cross Section
B578Microhardness of ElectroplatedCoatings
B 588 Measurement of Thickness of Transparent or Opaque Coatings by Double-
BeamInterference Microscope Technique
B 748 Measurement of the Thickness of Metallic Coatings by Measurement of
Cross Sectionwitha Scanning ElectronMicroscope
C664Thickness of DiffusionCoating
Criteria for Metallographic Laboratory Evaluation, Safety, and
Management
Guide for:
E1578Laboratory InformationManagement Systems LIMS
E2014Metallographic Laboratory Safety
Grain Size
Test Methods for:
E1181Characterizing Duplex GrainSizes
E112Determining Average GrainSize
E 930 Estimating the Largest Grain Observed in a Metallographic Section ALA
GrainSize
Practice for:
B 390 Evaluating Apparent Grain Size and Distribution of Cemented Tungsten
Carbides
Guides for:
E1951Calibrating Reticles andLight Microscope Magnications
Inclusions
Test Methods for:
B 795 Determining the Percentage of Alloyed or Unalloyed Iron Contamination
Present inPowder Forges P/F Steel Parts
B 796 Nonmetallic Inclusion Content of Powders Intended for Powder Forging
P/F Applications
E45Determining the InclusionContent of Steel
Indentation Hardness Testing
Specications for:
E 140 Hardness Conversion Tables for Metals. Relationship Among Brinell Hard-
ness, Vickers Hardness, Rockwell Hardness, Supercial Hardness, Knoop Hardness,
and Scleroscope Hardness. Please refer to ASTM E 140 in the CD-ROM included with
this manual.
Test Methods for:
C730KnoopIndentationHardness of Glass
C849KnoopIndentationHardness of Ceramic Whitewares
C1326KnoopIndentationHardness of AdvancedCeramics
C1327Vickers IndentationHardness of AdvancedCeramics
D785Rockwell Hardness of Plastics andElectrical Insulating Materials
D1415Rubber Property-International Hardness
D2240Rubber Property-Durometer Hardness
E10Brinell Hardness of Metallic Materials
E110IndentationHardness of Metallic Materials by Portable Hardness Testers
E103RapidIndentationHardness Testing of Metallic Materials
E18Rockwell Hardness andRockwell Supercial Hardness of Metallic Materials
E92Vickers Hardness of Metallic Materials
Practice for:
E448Scleroscope Hardness Testing of Metallic Materials
Microindentation Hardness Testing
Test Methods for:
B578Microhardness of ElectroplatedCoatings
B931 Metallographically Estimating the Observed Case Depth of Ferrons Powder
Metallurgy P/M Parts
B933MicroindentationHardness of Poweder Metallurgy P/M Materials
B 934 Effective Case Depth of Ferrous Poweder Metallurgy P/M Parts Using Mi-
croindentationHardness Measurements
E384MicroindentationHardness of Materials
Practice for:
WK382InstrumentedIndentationTesting
Porosity
Test Methodfor:
B276Apparent Porosity inCementedCarbides
See alsounder Quantitative Metallography
Quantitative Metallography
Test Methods for:
D629Quantitative Analysis of Textiles
D1030Fiber Analysis of Paper andPaperboard
D 2798 Microscopical Determination of the Reectance of Vitrinite in a Polished
Specimenof Coal
E562Determining Volume Fractionby Systematic Manual Point Count
E 1382 Determining the Average Grain Size Using Semiautomatic and Automatic
Image Analysis
E1077Estimating the Depthof Decarburizationof Steel Specimens
E2109Determining Area Percentage Porosity inThermal SprayedCoatings
F1854Stereological Evaluationof Porous Coatings onMedical Implants
Practices for:
C-856Petrographic Examinationof HardenedConcrete
E1268Assessing the Degree of Banding or Orientationof Microstructures
E1245 Determining the Inclusion or Second-Phase Constituent Content of Metals
by Automatic Image Analysis
E 2283 Extreme Value Analysis of Nonmetallic Inclusions in Steel and Other Mi-
crostructural Features
Sampling, Specimen Preparation and Photography
Test Methods for:
A247Evaluating the Microstructure of Graphite inIronCastings
B 328 Density, Oil Content, and Interconnected Porosity of Sintered Metal Struc-
tural Parts andOil-ImpregnatedBearings
B 657 Metallographic Determination of Microstructure in Cemented Tungsten
Carbides
E381MacroetchTesting Steel Bars, Billets, Blooms, andForgings
E340Macroetching Metals andAlloys
E3Preparationof Metallographic Specimens
Practices for:
B665Metallographic Sample Preparationof CementedTungstenCarbides
E 122 Calculating Sample Size to Estimate, with a Specied Tolerable Error, the
Average for Characteristic of a Lot or Process
E178Dealing withOutlying Observations
E407Microtching Metals andAlloys
E1180Preparing Sulfur Prints for Macrostructural Examination
E 768 Preparing and Evaluating Specimens for Automatic Inclusion Assessment
of Steel
E1351ProductionandEvaluationof FieldMetallographic Replicas
Guides for:
A892Dening andRating the Microstructure of HighCarbonBearing Steels
E1558Electrolytic Polishing of Metallographic Specimens
E1920Metallographic Preparationof Thermal SprayedCoatings
E 2015 Preparation of Plastics and Polymeric Specimens for Microstructural Ex-
amination
E883Reected-Light Photomicrography
Terminology
Terminology for:
E7Metallography
X-Ray and Electron Metallography This subject is not included in this
Book.
Test Methods for:
E82Determining the Orientationof a Metal Crystal
E2142 Rating and Classifying Inclusions in Steel Using the Scanning Electron Mi-
croscope
Practices for:
E766Calibrating the Magnicationof a Scanning ElectronMicroscope
E963 Electrolytic Extraction of Phases fromNi and Ni-Fe Base Superalloys Using
a Hydrochloric-Methanol Electrolyte
E81Preparing Quantitative Pole Figures
E 986 Scanning Electron Microscope Beam Size Characterization Performance
Characterization
E 975 X-Ray Determination of Retained Austenite in Steel with Near Random
Crystallographic Orientation
Guides for:
E1508Quantitative Analysis by Energy-Dispersive Spectroscopy
ASTM SpecicationsExamples
StandardSpecicationfor:
A1CarbonSteel Tee Rails
A3Steel Joint Bars, Low, Medium, andHighCarbonNon-Heat-Treated
A36CarbonStructural Steel
A47Ferritic Malleable IronCastings
A48Gray IronCastings
A126Gray IronCastings for Valves, Flanges, andPipe Fittings
A159Automotive Gray IronCastings
A197Cupola Malleable Iron
A220Pearlitic Malleable Iron
A242High-StrengthLow-Alloy Structural Steel
A 338 Malleable Iron Flanges, Pipe Fittings, and Valve Parts for Railroad, Marine,
andOther Heavy Duty Service at Temperatures Upto650F345C
A377Ductile-IronPressure Pipe
A439Austenitic Ductile IronCastings
A532Abrasion-Resistant Cast Irons
A536Ductile IronCastings
A572High-StrengthLow-Alloy Colombium-VanadiumStructural Steel
A602Automotive Malleable IronCastings
A 656 Hot-Rolled Structural Steel, High-Strength Low-Alloy Plate with Improved
Formability
12.4.3 ASTM StandardsDocument Summaries
For Document Summaries on the above mentioned standards please refer to the CD-
ROMincludedwiththis manual.
12.5 Chemical MicroetchingTable 12.2Table 12.3
The prepared specimen surface typically must be etched to reveal the microstructure
depending on the purpose of examination. Mostly this is done with chemical solutions,
etchants, developedfor a specic material andoftenfor a specic purpose.
InASTMPractice for Microetching Metals andAlloys E407 see Section12.4.3 a
large number of etchants for metals are stated withthe purposes uses. Based onTable
1 of the newest version of this practice ASTM E 40799 and other sources, Refs. 2, 4,
and 9, Part I, etchants are stated according to their purpose on each Material/
Preparation Tables, Section 13.2.3. The etchant is identied with a number. This num-
ber is taken to Table 12.2, which states the composition and procedure for the etching
process. Table 12.2 is based on Table 2 of ASTM E 40799 covering metals etchants
1226 with additions etchants 901950, mainly covering ceramics and plastics,
taken from Petzow, Ref. 2, Part I, ASM Handbook, Vol. 9, Ref. 4, Part I, and Vander
Voort, Ref. 9, Part I.
Attention: The ASTMPractice E 407 mentioned above is updated at different time
intervals and the reader should consult with the latest published version of the stan-
dard which can be found in Annual Book of Standards, Volume 03.01 see Section
12.4.1.
For etchants not mentioned in this book, see references in Section 9.1, and Litera-
ture, Chapter 27.
Etchant Names: Some etchants have special names, like Beraha. These names
are stated in Table 12.3, indicating the etchant number so that the composition can be
foundinTable 12.2. Table 12.3is basedonTable 3of ASTME407.
Theory of Microetching: For chemical etching theory, different types of etching
andliterature onetching see Chapter 9.
12.5.1 Etching Practice
Chemical etching is a straightforward, reasonably simple process. In most cases a rela-
tive small quantity of the etchant is placed in a shallow beaker, and the carefully
cleaned and dried specimenis immersed into the reagent. The specimenshould always
be held with a pair of tongs, and preferably with the surface turning upwards to be able
to see the progress of the process. The specimen is moved gently to remove reaction
products on the surface. In some cases a swabbing with a saturated piece of cotton can
be recommended, but the cotton might scratch the surface and care should be taken
that the cottonis regularly rechargedwithreagent.
Safety Precautions: See Sections 9.3.4 and 26.2 and ASTM Guide for Metallo-
graphic Laboratory Safety E 2014. Please refer to E 2014 in the CD-ROM included
withthis manual.
12.5.2 Table 12.2Numerical List of Etchants
TABLE12.2Numerical list of etchants. (This table contains etchants mentioned in the Material/
Preparation Tables andother etchants, seeASTME407.)
Etchant Composition Procedure
1 1 mL HF
200 mL water
(a) Swab with cotton for 15 s.
(b) Alternately immerse and polish several
minutes.
(c) Immerse 35 s.
(d) Immerse 10120 s.
2 3 mL HF
100 mL water
(a) Swab 10 s to reveal general structure.
(b) Immerse 15 min, wash 10 min in water to form
lm with hatching
which varies with grain orientation.
3 2 mL HF
3 mL HCl
5 mL HNO
3
190 mL water
(a) Immerse 1020 s. Wash in stream of warm
water. Reveals general structure.
(b) Dilute with 4 parts water-colors constituents
mix fresh.
4 24 mL H
3
PO
4
50 mL Carbitol (diethylene glycol
monoethyl ether)
4 g boric acid
2 g oxalic acid
10 mL HF
32 mL water
Electrolytic: Use carbon cathode raising d-c
voltage from 030 V in 30 s. Total
etching time 3 min with agitation. Wash and cool.
Repeat if necessary.
5 5 g HBF
4
200 mL water
Electrolytic: Use Al, Pb, or stainless steel cathode.
Anodize 13 min,
2045 V d-c. At
30 V, etch for 1 min.
6 25 mL HNO
3
75 mL water
Immerse 40 s at 70C 160F. Rinse in cold
water.
7 1020 mL H
2
SO
4
80 mL water
Immerse 30 s at 70C 160F. Rinse in cold
water.
8 10 mL H
3
PO
4
(a) Immerse 13 min at 50C 120F.
90 mL water (b) Electrolytic at 18 V for 510 s.
9 34 9 sulfamic acid
5 drops HF
100 mL water
Use just prior to the last polishing operation.
It is not intended as a nal etchant.
The specimen is examined as polished even under
polarized light.
10 10 mL HF
90 mL methanol (90 %)
Immerse 1030 s.
11 2 mL HF
100 mL water
Immerse or swab few seconds to a minute.
12 20 mL HNO
3
60 mL HCl
Use hood. Do not store. Immerse or swab 560 s.
13 10 g oxalic acid
100 mL water
Electrolytic at 6 V:
(a) 1015 s.
(b) 1 min.
(c) 23 s.
Use stainless steel cathode and platinum or
Nichrome connection to specimen.
Preparation Tables andother etchants, seeASTME407.)(Continued.)
14 10 mL HNO
3
Immerse few seconds to a minute.
15 15 mL HNO
3
15 mL acetic acid
60 mL HCl
15 mL water
Age before use. Immerse 530 s. May be used
electrolytically.
16 510 mL HCl
100 mL water
Electrolytic at 3 V for 210 s.
17 5 mL HCl
10 g FeCl
3
100 mL water
Electrolytic at 6 V for few seconds.
18 210 g CrO
3
100 mL water
19 A
8 g NaOH
100 mL water
B
Saturated aqueous solution of KMnO
4
Immerse in freshly mixed Solutions A+B (1:1) for
510 s.
If surface activation is necessary, rst use Etch
#18, then rinse in water.
While still wet, immerse in Solutions A+B (1:1).
Mixture of solutions A+B has 15 min useful life.
20 5 mL H
2
O
2
(30 %)
100 mL HCl
Use hood. Mix fresh. Immerse polished face up for
few seconds.
21 1 g CrO
3
140 mL HCl
Use hood. To mix, add the HCl to CrO
3
.
22 100 mL HCl
0.5 mL H
2
O
2
(30 %)
Use hood. Do not store.
(a) Immerse or swab 1/ 23 min. Add H
2
O
2
dropwise to maintain action.
(b) Electrolytic, 4 V, 35 s.
23 5 mL HCl
95 mL ethanol (95 %) or methanol
(95 %)
24 5 mL HNO
3
200 mL HCl
65 g FeCl
3
Use hood. Immerse few seconds.
25 10 g CuSO
4
50 mL HCl
50 mL water
Immerse or swab 560 s. Made more active by
adding few drops of H
2
SO
4
just before use.
26 5 g FeCl
3
10 mL HCl
50 mL glycerol
30 mL water
Swab 1660 s. Activity may be decreased by
substituting glycerol for water.
27 1 g KOH
20 mL H
2
O
2
(3 %)
50 mL NH
4
OH
30 mL water
Dissolve KOH in water, then slowly add NH
4
OH
to solution. Add 3 % H
2
O
2
last. Use
freshimmerse few seconds to a minute.
28 1 g FeNO
3
100 mL water
Swab or immerse few seconds to a minute.
29 1 g K
2
Cr
2
O
7
4 mL H
2
SO
4
50 mL water
Add 2 drops of HCl just before using. Swab few
seconds to a minute.
30 25 mL NH
4
OH
25 mL water
50 mL H
2
O
2
(3 %)
Mix NH
4
OH and water before adding H
2
O
2
. Must
be used fresh. Swab 545 s.
31 10 g ammonium persulfate
100 mL water
(a) Swab or immerse to 5 s.
(b) Immerse to 2 min to darken matrix to reveal
carbides and phosphides.
(c) Electrolytic at 6 V for few seconds to a minute.
(d) Immerse 360 s. Can be heated to increase
activity.
32 60 g CrO
3
100 mL water
Saturated solution.
Immerse or swab 530 s.
33 10 g CrO
3
24 drops HCl
100 mL water
Add HCl just before use. Immerse 330 s. Phases
can be colored by Nos. 35, 36, 37.
34 5 g FeCl
3
50 mL HCl
100 mL water
(a) Immerse or swab few seconds to few minutes.
Small additions of HNO
3
activate solution and minimize pitting.
(b) Immerse or swab few seconds at a time. Repeat
as necessary.
35 20 g FeCl
3
5 mL HCl
1 g CrO
3
100 mL water
Immerse or swab few seconds at a time until
desired results are obtained.
36 25 g FeCl
3
25 mL HCl
100 mL water
37 1 g FeCl
3
10 mL HCl
100 mL water
desired results are obtained
38 8 g FeCl
3
25 mL HCl
100 mL water
Swab 530 s.
39 5 g FeCl
3
10 mL HCl
1 g CuCl
2
0.1 g SnCl
2
100 mL water
40 5 gFeCl
3
16 ML HCl 60 mL
ethanol (95 %) or methanol
(95 %)
Immerse or swab few seconds to few minutes.
41 2 g K
2
Cr
2
O
7
8 mL H
2
SO
4
4 drops HCl
100 mL water
Add the HCl just before using. Immerse 360 s.
42 10 g cupric ammonium chloride
100 mL water
NH
4
OH
Add NH
4
OH to solution until neutral or slightly
alkaline. Immerse 560 s.
43 20 mL NH
4
OH
1 g ammonium persulfate
Immerse 530 s.
44 50 mL NH
4
OH
2050 mL H
2
O
2
(3 %)
050 mL water
Use fresh. Peroxide content varies directly with
copper content of alloy to be etched.
Immerse or swab to 1 min. Film on etched
aluminum bronze removed by No. 82.
45 1 g CrO
3
100 mL water
Electrolytic at 6 V for 36 s. Use aluminum
cathode.
46 15 mL NH
4
OH
15 mL H
2
O
2
(3 %)
15 mL water
4 pellets NaOH
When mixing, add NaOH pellets last.
For best results use before pellets have dissolved.
47 5 g NaCN or KCN
5 g NH
4
2
S
2
O
2
100 mL water
Use hoodCan give off extremely poisonous
hydrogen cyanide.
PrecautionAlso poisonous by ingestion as well
as contact.
48 10 g NaCN
100 mL water
hydrogen cyanide.
as contact. Electrolytic at 6 V:
(a) 5 s for sigma.
(b) 30 s for ferrite and general structure.
(c) to 5 min for carbides.
49 3 g FeSO
4
0.4 g NaOH
10 mL H
2
SO
4
190 mL water
Electrolytic at 810 V 0.1 A for 515 s.
50 5 mL acetic acid
10 mL HNO
3
85 mL water
Use hood. Do not store. Electrolytic at 1.5 V for
20 to 60 s. Use platinum wires.
51 2 g FeCl
3
5 mL HCl
30 mL water
60 mL ethanol or methanol
Immerse few minutes.
52 1 g sodium dichromate
1 g NaCl
4 mL H
2
SO
4
250 mL water
Swab few seconds.
53 15 mL NH
4
OH
100 mL water
Immerse 560 s.
54 1 g ammonium acetate
3 g sodium thiosulfate
7 mL NH
4
OH
1300 mL water
Electrolytic at 0.3 A/ cm
2
for 530 s.
55 1 mL H
2
SO
4
15 mL HNO
3
10 mL acetic acid
5 mL H
3
PO
4
20 mL lactic acid
Swab gently 1015 s. Rinse with methanol and
blow dry. Helps to chemically polish.
If nal etch is too even mild, follow with No. 98.
56 30 mL HNO
3
10 mL H
3
PO
4
20 mL acetic acid
10 mL lactic acid
Swab gently 515 s. Rinse with ethanol or
methanol and blow dry.
57 75 mL acetic acid
25 mL H
2
O
2
(30 %)
Immerse 615 s.
58 25 mL HF
25 mL HNO
3
5 mL water
Swab 320 s.
59 2 g AgNO
3
40 mL water
40 mL HF
20 mL HNO
3
Mix AgNO
3
and water, then add HF and HNO
3
.
Swab 1/ 22 min.
60 25 mL HNO
3
15 mL acetic acid
15 mL HF
57 drops bromine
Use hood. Let stand 1/ 2 h before using. Swab
320 s.
61 60 mL HCl
40 mL HNO
3
Use hood. Immerse few seconds to a minute.
62 15 g CrO
3
100 mL HCl
Vary composition of reagent and aging of reagent
after mixing to suit alloy.
Swab or immerse few seconds to a minute.
63 0.1 g CrO
3
10 mL HNO
3
100 mL HCl
Swab few seconds to a minute.
64 5 mL HNO
3
25 mL HCl
30 mL water
(a) Immerse 15 min.
(b) Use hot. Will form chloride lm on gold alloys
if much silver is present.
Ammonia will remove lm.
65 A
100 mL water
B
10 g KCN
100 mL water
hydrogen cyanide.
as contact. Mix 1+1 mixture of Solutions A and B
just before use. (A mixture of 5 drops of each will
cover the surface of a 1 in. dia. mount.)
Immerse 1/ 22 min.
66 30 mL HF
15 mL HNO
3
30 mL HCl
Swab 310 s or immerse to 2 min.
67 10 mL perchloric acid
10 mL 2-butoxyethanol
70 mL ethanol (95 %)
10 mL water
PrecautionKeep cool when mixing and use.
35 mL 2-butoxyethanol
60 mL methanol (absolute)
80 mL acetic acid
Electrolytic at 2060 V for 15 min.
70 5 mL HF
2 mL AgNO
3
(5 %)
200 mL water
Swab for 560 s.
71 5 mL HF
95 mL water
Add 510 drops of this solution on the nal
polishing wheel which has been charged
with the polishing solution. The specimen is
polished on this wheel until the surface
turns black. Distilled water is then slowly added to
the wheel and polishing continued
until the surface is bright. At this time the
specimen should be ready for examination
via polarized light.
NoteUse inert substance between cloth and
wheel to prevent attack of the wheel.
Wear gloves.
72 10 mL HF
45 mL HNO
3
45 mL water
Swab for 520 s.
73 20 mL HCl
25 g NaCl
65 mL water
Electrolytic etchuse carbon cathode and
platinum wire connection to specimen.
(a) 6 V ac for 1 min.
(b) 5 V20 V ac for 12 min.
(c) 20 V ac for 12 min.
For etch-polishing, use shorter times. After etching,
water rinse, alcohol rinse, and dry.
74 15 mL HNO
3
(95 %)
Etching rate is increased, sensitivity decreased with
increased percentage of HNO
3
.
(a) Immerse few seconds to a minute.
(b) Immerse 540 s in 5 % HNO
3
solution. To
remove stain, immerse 25 s in 10 %
HCl-methanol solution.
(c) For Inconels and Nimonics, use 5 mL HNO
3
solutionelectrolytic at 510 V for 5
20 s.
(d) Swab or immerse several minutes.
(e) Swab 560 s. HNO
3
may be increased to
30 mL in methanol only depending on
alloy. (Ethanol is unstable with over 5 % HNO
3
).
Do not store.
75 5 g picric acid
8 g CuCl
2
20 mL HCl
(95 %)
Immerse 12 s at a time and immediately rinse
with methanol. Repeat as often as
necessary. (Long immersion times will result in
copper deposition on surface.)
76 4 g picric acid
(95 %)
Composition given will saturate with picric acid.
Immerse few seconds to a minute or
more. Adding a wetting agent such as zepherin
chloride will increase response.
77 10 g picric acid
5 drops HCl
(95 %)
Composition given will saturate the solution with
picric acid. Immerse few seconds to
a minute or more.
78 10 g potassium metabisulte
100 mL water
Immerse 115 s. Better results are sometimes
obtained by rst etching lightly with
No. 76 or 74.
79 40 mL HCl
5 g CuCl
2
30 mL water
(95 %)
Swab few seconds to a minute.
80 5 mL HCl
1 g picric acid
(95 %)
Immerse or swab few seconds to 15 min. Reaction
may be accelerated by adding a
few drops of 3 % H
2
O
2
. Optional (for prior
austenite grain boundaries)temper
specimen at 600900F prior to preparation.
81 2 g picric acid
1 g sodium tridecylbenzene sulfonate
100 mL water
Composition given will saturate the should with
picric acid.
(a) Immerse few seconds to a minute.
(b) Immerse to 15 min with occasional swabbing
for heavy grain boundary attack.
82 5 g FeCl
3
5 drops HCl
100 mL water
Immerse 510 s.
83 10 g CrO
3
100 mL water
(a) Electrolytic at 6 V for 560 s. Attacks
carbides.
(b) Electrolytic at 6 V for 35 s.
84 10 mL H
2
SO
4
10 mL HNO
3
80 mL water
PrecautionAdd H
2
SO
4
slowly to water and cool,
then add HNO
3
. Immerse 30 s.
Swab in running water. Repeat three times and
repolish lightly.
85 2 g picric acid
25 g NaOH
100 mL water
Immerse in boiling solution for 5 min. Precaution
Do not boil dryanhydrous picric
acid is unstable and highly explosive. Alternative:
Electrolytic at 6 V for 40 s (room
temperature). Use stainless steel cathode.
86 3 g oxalic acid
4 mL H
2
O
2
(30 %)
100 mL water
Solution should be freshly prepared. Immerse
1525 min when specimens or parts
cannot be given usual metallographic polish.
Multiple etching may be required.
87 10 mL HNO
3
2050 mL HCl
30 mL glycerol
Use hoodCan give off nitrogen dioxide gas.
PrecautionMix HCl and glycerol
thoroughly before adding HNO
3
. Do not store.
Discard before solution attains a dark
orange color. Immerse or swab few seconds to few
minutes. Higher percentage of
HCl minimizes pitting. A hot water rinse just prior
to etching may be used to activate
the reaction. Sometimes a few passes on the nal
polishing wheel is also necessary
to remove a passive surface.
88 10 mL HNO
3
20 mL HCl
30 mL water
PrecautionDiscard before solution
attains a dark orange color. Immerse few seconds
to a minute. Much stronger reaction
than No. 87.
89 10 mL HNO
3
10 mL acetic acid
15 mL HCl
25 drops glycerol
Use hood. Do not store. Immerse or swab few
seconds to few minutes.
90 10 mL HNO
3
20 mL HF
2040 mL glycerol
Immerse 210 s.
91 5 mL HNO
3
5 mL HCl
1 g picric acid
(95 %)
This etchant is equivalent to a 1+1 mixture of No.
80 and No. 74 (5 % HNO
3
). Swab
for 30 s or longer.
92 10 mL HCl
(95 %)
Immerse 530 min or electrolytic at 6 V for
35 s.
93 concentrated HNO
3
Use hood. Electrolytic at 0.2 A/ cm
2
for few
seconds.
94 2 g CuCl
2
40 mL HCl
(95 %)
Submerged swabbing for few seconds to several
minutes. Attacks ferrite more readily
than austenite.
95 2 g CuCl
2
40 mL HCl
(95 %)
40 mL water
Immerse or swab few seconds to few minutes.
96 85 g NaOH
50 mL water
97 45 g KOH
60 mL water
Composition of solution is approximately 10 N.
Electrolytic at 2.5 V for few seconds.
Stains sigma and chi yellow to red brown, ferrite
gray to blue gray, carbides barely
touched, austenite not touched.
98 10 g FeCN
4
10 g KOH or NaOH
100 mL water
hydrogen cyanide. PrecautionAlso
poisonous by ingestion as well as contact. Use
fresh.
(a) Immerse or swab 1560 s. Stains carbides and
sigma. (To differentiate, No. 31
electrolytic at 4 V will attack sigma, but not
carbides. If pitting occurs, reduce voltage.)
(b) Immerse in fresh, hot solution 220 min.
Stains carbides dark, ferrite yellow,
sigma blue. Austenite turns brown on overetching.
(c) Swab 560 s. (Immersion will produce a stain
etch.)
Follow with water rinse, alcohol rinse, dry.
99 25 mL HCl
3 g ammonium biuoride
125 mL water
few grains potassium metabisulte
Mix fresh. (For stock solution, mix rst three items.
Add potassium metabisulte just
before use.) Immerse few seconds to a few
minutes.
100 10 g FeCl
3
90 mL water
Immerse few seconds.
101 2 g CrO
3
20 mL HCl
80 mL water
Immerse 560 s. (CrO
3
may be increased up to
20 g for difcult alloys. Staining and
pitting increase as CrO
3
increased.)
102 concentrated NH
4
OH Use hood. Electrolytic at 6 V for 3060 s. Attacks
carbides only.
103 20 mL HNO
3
4 mL HCl
Immerse 1060 s.
104 5 mL HNO
3
45 mL HCl
50 mL water
Immerse 10 min or longer.
105 5 mL H
2
SO
4
3 mL HNO
3
90 mL HCl
Use hood. Precautionadd H
2
SO
4
slowly to HCl
with stirring, cool; then add HNO
3
.
Discard when dark orange color. Swab 1030 s.
106 7 mL HNO
3
25 mL HCl
Use fresh to avoid pitting. Immerse or swab
1060 s.
107 10 mL H
3
PO
4
50 mL H
2
SO
4
40 mL HNO
3
Use hood. PrecautionMix H
3
PO
4
and HNO
3
thoroughly, then add H
2
SO
4
slowly
with stirring. Use fresh, but allow to cool.
Electrolytic at 6 V for few seconds. Brown
discoloration will form at edges of specimen. To
slow reaction, add water (to 100 mL)
very carefully with stirring. Attacks bakelite
mounts.
108 310 mL H
2
SO
4
100 mL water
Electyrolytic at 6 V for 510 s. Tends to pit with
longer times.
109 50 mL HCl
25 mL HNO
3
1 g CuCl
2
150 mL water
Make fresh but allow to stand 30 min to avoid
plating out copper. Immerse few
seconds to a few minutes.
110 10 mL HCl
5 mL HNO
3
(95 %)
Immerse to several minutes until deeply etched.
Follow with light repolish.
111 5 mL H
2
SO
4
8 g CrO
3
85 mL H
3
PO
4
Electrolytic at 10 V 0.2 A/ cm
2
for 530 s.
Reveals Ti- and Cb-rich areas at a faster
rate than grain boundaries.
30 mL H
2
O
2
(30 %)
Immerse 815 s.
15 mL HNO
3
60 mL glycerol
Do not store. Use fresh solution at 80C 176F.
20 mL HNO
3
80 mL water
Use fresh solution at 4042C 104108F.
Immerse 430 min depending on depth of
worked metal layer. Clean with cotton in running
water.
10 mL H
2
O
2
(30 %)
Immerse 1030 min depending on depth of
worked metal layer. Clean in HNO
3
if
necessary.
116 510 g AgNO
3
90 mL water Swab.
117 10 mL HCl
90 mL water
(a) Immerse for 1/ 25 min. Follow with
electrolytic etch at low current density in same
solution. If specimen has considerable surface ow,
immerse in concentrated HCl for
a few seconds, then follow above procedure.
(b) Immerse for 1/ 22 min.
118 1 mL HNO
3
75 mL diethylene glycol
25 mL water
Swab 35 s for F and T6, 12 min for T4 and O
temper.
119 1 mL HNO
3
20 mL acetic acid
60 mL diethylene glycol
20 mL water
Swab 13 s for F and T6, 10 s for T4 and O
temper.
120 10 mL HF
90 mL water
Immerse with gentle agitation 330 s.
121 0.7 mL H
3
PO
4
4 g picric acid
(95 %)
Composition critical.
(a) Immerse with gentle agitation 1030 s.
(b) To increase staining immerse and withdraw
with a meniscus layer. Lightly apply
etchant over surface until dark stain develops.
122 2 g oxalic acid
100 mL water
Swab.
123 60 mL H
3
PO
4
Electrolytic: Use stainless steel cathode. Space
electrodes 2 cm apart. Start at 3 V dc.
After 30 s maintain at 11/ 2 V.
10 mL water
6 g picric acid
(95 %)
6 g picric acid
(95 %)
15 mL water
6 g picric acid
(95 %)
20 mL water
3 g picric acid
(95 %)
128 8 mL HF
5 mL HNO
3
200 mL water
129 10 mL HF
30 mL HNO
3
60 mL lactic acid
Swab 1020 s. Vary HF to increase or decrease
activity.
130 25 mL HCl
75 mL methanol
CautionKeep below 24C 75F. Electrolytic
at 30 V for 30 s.
131 5 mL H
2
SO
4
1 mL HF
132 5 mL HF
10 mL HNO
3
50 mL lactic acid
Use fresh.
(a) Swab with heavy pressure for 510 s. Water
rinse, alcohol rinse, dry, then etch
with No. 98c.
(b) Swab for 530 s.
133 50 mL HNO
3
50 mL acetic acid
Use hood. Do not store. Mix fresh. Immerse or
swab 5 to 30 s. Will chemically polish
with longer times. Suldized grain boundaries
etched before normal grain boundaries.
134 70 mL H
3
PO
4
30 mL water
Electrolytic 510 V for 560 s. (Polishes at high
currents.)
135 80 mL HNO
3
3 mL HF
Use hood. Warm specimen in boiling water prior to
immersion for 10 to 120 s.
136 20 mL H
3
PO
4
80 mL water
137 10 g NaNO
3
100 mL water
Electrolytic, 0.2 A/ cm
2
, 1 min.
138 5 g FeCl
3
2 mL HCl
100 mL ethanol (95 %) or
methanol (95 %)
Swab 1060 s.
139 5 g (95 %) KCN
100 mL water
0.5 mL H
2
O
2
(3 %)
poisonous by ingestion as well as contact. Immerse
10100 s.
50 mL HNO
3
50 mL acetone
Use hood. Do not store. Decomposes with possible
explosion on standing. Immerse
1030 s.
141 3 g NH
4
Cl
3 g CrO
3
10 mL HNO
3
90 mL water
Swab 530 s. Do not store.
142 5 mL HF
10 mL glycerol
85 mL water
144 A
100 mL water
B
10 mL HCl
90 mL water
Electrolytic in Solution A: specimen is cathode,
10 V, 510 s. Then electrolytic in
Solution B: specimen is anode, 10 V, 510 s.
145 2 mL H
2
SO
4
100 mL water
Electrolytic at 310 V for 515 s. Use platinum
wires. H
2
SO
4
may be increased to 20
mL for deeper attack.
146 10 mL HF
100 mL HNO
3
Immerse 30 s- 3 min.
147 20 mL HNO
3
80 mL HCl
Immerse 530 s.
148 5 mL HNO
3
100 mL water
Immerse 1030 s.
149 50 mL HCl
2 mL H
2
O
2
(30 %)
50 mL water
Immerse 1030 s. Do not store.
150 60 mL HCl
20 mL HNO
3
40 mL glycerol
Use hood. Do not store. Swab few seconds to a
minute. Discard when solution turns
dark yellow.
151 10 mL HF
25 mL HNO
3
150 mL water
Swab 530 s.
152 85 mL NH
4
OH
15 mL H
2
O
2
(30 %)
Immerse 515 s. Do not storeDecomposes.
153 10 mL HNO
3
50 mL HCl
60 mL glycerol
Use hood. Do not store. Add HNO
3
last. Discard
when dark yellow. Immerse 1060 s.
Preheating specimen in boiling water hastens
reaction.
154 50 mL HCl
(95 %)
Immerse 10100 s.
155 3 mL selenic acid
10 mL HCl
100 mL ethanol (95 %)or methanol
(95 %)
Immerse 115 min. (Up to 30 mL of HCl may be
used for more vigorous action.) Stable
for 390 days, depending on HCl concentrations.
158 1 g thiourea
1 mL H
3
PO
4
1000 mL water
Electrolytic, 0.0050.01 A/ cm
2
, 12 min.
157 25 g CrO
3
150 mL HCl
50 mL water
Immerse 520 s.
158 10 mL HF
10 mL HNO
3
20 mL glycerol
Swab 515 s.
159 5 mL HF
20 mL HNO
3
50 mL acetic acid
Swab 1030 s.
160 20 mL HF
15 mL H
2
SO
4
5 mL HNO
3
50 mL water
Immerse to 5 min.
161 25 mL HNO
3
5 mL HF
Immerse 5120 s.
162 A
50 mL lactic acid
30 mL HNO
3
2 mL HF
B
30 mL lactic acid
10 mL HNO
3
10 mL HF
Swab 13 min in Solution A (acts as etch polish).
To etch, swab with Solution B for 5 s.
Repeat if necessary. The HF may be varied to give
more or less etching.
163 30 mL H
2
SO
4
30 mL HF
35 drop H
2
O
2
(30 %)
30 mL water
Immerse 560 s. Use this solution for alternate
etch and polishing.
164 50 mL HNO
3
20 mL water
Use hood. Swab 310 s.
165 10 mL HCl
90 mL ethanol
(a) Electrolytic at 10 V for 30 s. Use carbon
cathode and platinum wire connection to
specimen. For etch-polishing, use shorter time.
(b) Electrolytic at 6 V for 10 s. Use stainless steel
cathode and platinum or Nichrome
wire contact to specimen.
166 A
90 mL water
B
20 g KCN
90 mL water
poisonous by ingestion as well as contact. Mix 1
+1 ratio of Solution A and B just
before use. (A mixture of 5 drops of each will
cover the surface of the 1 in. dia mount.)
Immerse to several minutes.
167 5 g NaCN
100 mL water
Use hoodCan give of extremely poisonous
poisonous by ingestion as well as contact.
Electrolytic at 15 V ac for 12 min. Use
platinum cathode.
168 20 mL HCl
35 g NaCl
80 mL water
Composition given will saturate the solution with
NaCl. Electrolytic at 11/2 V ac for 1
min.
169 5 mL HNO
3
50 mL ethylene glycol
(95 %)
2
for 2 min. Use stainless
steel cathode.
170 1 mL HF
30 mL HNO
3
(a) Swab 530 s. Follow with water rinse, alcohol
rinse, dry.
30 mL lactic acid (b) Swab for 10 s intervals. Increase HF to
exaggerate grain boundaries.
171 concentrated HCl Use hood. Electrolytic at 5 V ac for 12 min. For
etch-polishing, use shorter times.
Follow with water rinse, alcohol rinse, and dry.
172 A
10 mL water
B
5 g KCN
100 mL water
poisonous by ingestion as well as contact. Prepare
1+1 mixture of Solutions A and B just before use.
(A mixture of 5 drops of each will cover the
surface of a 1 in. dia
mount.) Immerse 12 min.
173 50 mL NH
4
OH
1030 mL H
2
O
2
(50 %)
Immerse few seconds to a minute.
174 A
25 mL HNO
3
1 g K
2
Cr
2
O7
1000 mL water
B
40 g CrO3
3 g Na
2
SO
4
200 mL water
Prepare 1+1 mixture of Solutions A and B. Apply
with camels hair brush.
Nonadherent lm of silver chromate should form.
If lm adheres, add more of solution
A, if none forms, add Solution B.
175 1 g CrO
3
1 mL H
2
SO
4
100 mL water
Immerse to 1 min.
176 2 g FeCl
3
100 mL water
Immerse 530 s.
177 10 g NaOH
100 mL water
Swab or immerse 515 s.
178 20 mL HF
20 mL HNO
3
60 mL lactic acid
Swab for 520 s.
179 A
10 mL HF
10 mL HNO
3
30 mL lactic acid
B
10 mL HF
10 mL HF
90 mL H
2
SO
4
Use hoodMix Solution B very slowly. Solution
A is used as a chemical polish, though
some etching will occur. Swab 2 or more minutes
for desired surface. If surface is
insufciently etched use Solution B electrolytically
at 1/ 21 V/ in.
2
of specimen. Use
carbon cathode and platinum wire connection to
specimen. Discard Solution B after 1
h.
180 10 mL HNO
3
30 mL acetic acid
50 mL glycerol
Immerse for 1/ 210 min at 38 to 42C
100108F.
181 2 mL HCl
(95 %)
Swab for 13 min.
182 10 mL HNO
3
10 mL acetic acid
80 mL glycerol
Immerse for 1/ 210 min at 38 to 42C
100108F
183 2 drops HF
1 drop HNO
3
25 mL glycerol
Immerse for 1 min.
184 10 g FeCl
3
2 mL HCl
100 mL water
Immerse for
1
2
5 min.
185 10 mL HF
10 mL HNO
3
Swab for few seconds.
186 10 mL HF
5 mL HNO
3
Swab 32 s.
85 mL water
187 10 mL HF
30 mL HNO
3
50 mL water
Swab 320 s.
188 1 mL HF
50 mL HNO
3
50 mL H
2
O
2
(30 %)
50 mL water
Swab until stain is removed.
189 10 mL HF
25 mL HNO
3
45 mL glycerol
20 mL water
Swab 320 s.
190 8 g KOH
10 mL H
2
O
2
(30 %)
60 mL water
Swab 320 s.
191 25 mL HF
18 g benzalkonium chloride
40 mL glycerol
Swab 320 s.
192 13 mL HF
26 mL HNO
3
100 mL water
Swab 310 s or immerse 1030 s. (HF attacks
and HNO
3
brightens the surface of
titanium. Make concentration changes on this
basis.)
193 2 drops HF
1 drop HNO
3
3 mL HCl
25 glycerol
Swab 320 s.
194 20 mL HF
20 mL HNO
3
60 mL glycerol
Immerse 530 s.
195 30 mL H
3
PO
4
30 mL ethylene glycol
Electrolytic at 1820 V 0.03 A/ cm
2
for
515 min.
196 18 g CrO
3
75 mL acetic acid
20 mL water
Dissolve CrO
3
in hot water and cool before adding
acetic acid. Keep solution below
2C 35F during use. Electrolytic at 80 V for
530 min. Do not store.
197 5 g oxalic acid
100 mL water
198 30 mL HF
30 mL HNO
3
30 mL glycerol
Swab for 60 s.
199 2 mL HF
5 g AgNO
3
100 mL water
Swab for 5 s
200 A
40 g CrO
3
3 g Na
2
SO
4
200 mL water
B
40 g CrO
3
200 mL water
Immerse in Solution A with gentle agitation for
several seconds. Rinse in Solution B.
201 A
40 g CrO
3
1.5 g Na
2
SO
4
200 mL water
B
40 g CrO
3
200 mL water
Immerse in Solution A with gentle agitation for
several seconds. Rinse in Solution B.
202 A
10 g CrO
3
1 g Na
2
SO
4
200 mL water
Immerse in Solution A for 25 s. Rinse in
Solution B.
B
40 g CrO
3
200 mL water
203 20 g CrO
3
100 mL water
2
for 5 s.
10 mL glycerol
10 mL water
205 5 mL HF
2 mL AgNO
3
(5 %)
100 mL water
Swab vigorously for 1060 s. Wet cotton
frequently.
206 5 mL HF
10 mL HNO
3
10 mL glycerol
PrecautionDiscard after use. Solution
decomposes on standing. Electrolytic at 912
V for 110 min.
207 30 mL HNO
3
30 mL acetic acid
30 mL water
Swab for 530 s.
208 1 mL NH
4
OH
10 mL water
Immerse or swab few seconds to a minute.
209 15 mL HNO
3
3 mL HF
80 mL water
Immerse 560 s.
210 50 mL water (cold) saturated with
sodium
thiosulfate
1 g potassium metabisulte
First ingredient in stock solution. Add potassium
metabisulte before use. Solution
good for several days, or longer. Immerse face up,
gently agitate until coloration
begins, allow to settle. Stop etch when surface is
red-violet. Etch time varies with
material. Colors matrix phases.
211 3 g potassium metabisulte
100 mL water
Use fresh solution. Immerse specimen face up,
gently agitate solution until coloration
begins, allow to settle. Stop etch when surface is
red-violet. Etch time varies with
material. Colors matrix phases.
212 1050 % HCl in water
0.51.0 g potassium metabisulte per
100 mL of aqueous HCl solution
Optional: 1 g CuCl
2
13 g FeCl
3
For more corrosion resistant alloys. Increase the
HCl and potassium metabisulte
contents. Use optional ingredients to improve
coloration, if needed. Colors matrix
phases. Use by immersion only.
213 210 mL HCl
0.53 mL selenic acid
100 mL ethyl alcohol (95 %)
For more corrosion resistant alloys, increase the
HCl and selenic acid content. For highly
corrosion-resistant alloy, use 2030 mL HCl.
Colors second phase
constituents. Use by immersion only.
214 1 g sodium molybdate
100 mL water
Add nitric acid to lower the pH to 2.53. Add
0.10.5 g ammonium biuoride for carton
steels. Use by immersion only. Colors carbides.
Immerse about 15 s.
215 240 g sodium thiosulfate
30 g citric acid
24 g lead acetate
1000 mL water
Mix in order given. Store in a dark bottle at least
24 h before use at 20C. Lightly pre-
etch specimen before use. Use small portion of
stock solution for 4 h max. Pre-etch
steel specimens with nital before tinting the MnS
(add 0.2 g sodium nitrite to 100 mL
of etch) white. Colors phosphides in cast iron.
Colors matrix of Cu alloys.
216 815 g sodium metabisulte
100 mL water
Do not store. Mix fresh. Immerse specimen face
up. Agitate solution gently until
coloration begins, allow to settle. Stop when
surface is dark. use crossed polarized
light and sensitive tint to improve coloration.
217 5 g ammonium biuoride
100 mL water
Mix fresh, use plastic coated tongs and
polyethylene beaker. Immerse until surface is
colored.
218 3 g ammonium biuoride
4 mL HCl
100 mL water
Mix fresh, use plastic coated tongs and
polyethylene beaker. Immerse until surface is
colored. Works best with attack-polished
specimens.
219 60 mL HNO
3
40 mL water
Electrolytic etch, does not reveal twins in
stainless steel. Excellent grain boundary
etch for ferritic stainless steels. Use at 1 V dc,
120 s, with stainless cathode; 0.6 V dc
with platinum cathode.
220 20 g NaOH
100 mL water
Electrolytic etch, colors -ferrite in stainless steel.
Use at 220 V dc, 520 s,
stainless steel cathode. If is not colored, increase
NaOH to 40 g.
221 50 mL water
50 mL ethyl alcohol
Use by immersion. Will not attack suldes in
stainless steels.
50 mL methyl alcohol
50 mL HCl
1 g CuCl
2
2.5 g FeCl
3
2.5 mL HNO
3
222 8 g Na
2
SO
4
100 mL water
(a) Few seconds to 1 minute.
(b) Pre-etch 2 s in No. 74, rinse, and etch 20 s.
223 A
8 g oxalic acid
5 mL H
2
SO
4
100 mL water
B
H
2
O
2
(30 %)
Mix equal volumes of Solutions A and B just
before use. Etch 23 s; 3 s pre-etch in
No. 74 may be needed.
224 10 mL H
2
O
2
(30 %)
20 mL 10 % aqueous NaOH
Immerse 10 s at 20C 68F.
225 4 g NaOH
100 mL saturated aqueous KMnO
4
Immerse 10 s at 20C 68F.
226 15 mL HCl
10 mL acetic acid
5 mL HNO
3
2 drops glycerol
PrecautionMix HCl and glycerol
thoroughly before adding HNO
3
. Do not store.
Discard before solution attains a dark
orange color. Use fresh or age up to 1 min.
Immerse or swab few seconds to few
minutes. Can increase HNO
3
to increase strength.
Sometimes a few passes on the
nal polishing wheel is also necessary to remove a
passive surface.
901 1 g KOH
100 mL water
Electrolytic: Use stainless steel cathode. 40 V
DC at 3 A/ cm
2
in 3060 s
902 Plasma etching with CF
4
gas and O
2
gas (1:1)
35 min, 6080 W
903 See etchant 98 (Murakamis reagent) Use hot, 3040 min for SiC with 1 % B
4
C or
boiling for B-doped SiC
904 30 g K
3
FeCN
6
3 g NaOH
60 mL water
Immerse 530 min at 110C 230F
905 10 g K
3
FeCN
6
10 g NaOH
20 mL water
Immerse 510 min
906 10 g K
3
FeCN
6
10 g NaOH
80 mL water
Immerse 1020 min
907 10 mL HNO
3
(65 %)
10 g K
3
FeCN
6
100 mL water
908 30 g K
3
FeCN
6
3 g NaOH
60 mL water
Immerse 815 min. Use boiling
909 10 mL HNO
3
(65 %)
10 mL HF (40 %)
10 mL water
Immerse seconds to min
910 10 mL HF (40 %)
50 mL lactic acid
30 mL HNO
3
(65 %)
911 10 mL HF (40 %)
30 mL HNO
3
(65 %)
Immerse 2 min
912 10 mL HCl (32 %)
10 mL H
2
O
2
(30 %)
Immerse seconds to min
913 Plasma etching
CF
4
gas and O
2
gas (2:1)
15 min, 6080 W
914 H
3
PO
4
(85 %) Use boiling up to 15 min
915 Molten NaOH (free of water) 20 s to 3 min at 300350C 570660F, 23
samples per melt
916 10 mL 10 % aqueous NaH solution
10 mL 10 % aqeous potassium
ferricyanide solution
50 mL water
(Modied Murakami, see etchant 98)
Immerse 30 min at 100C 212F)
917 Thermal etch in air 11001500C 1520 min at 13001400C 23702550F
(Etch temperature is approximately 150C
300F below sintering temperature
918 H
3
PO
4
(85 %) 5 s to 3 min at 250C 480F
919 HCl (32 %) Immerse 36 min
920 Sat. aq. Na
2
S Immerse up to 1 min
921 20 mL HNO
3
(65 %)
10 mL HF (40 %)
20 mL water
Immerse up to 15 min
922 45 mL HNO
3
(65 %)
5 mL HF (40 %)
50 mL water
Immerse up to 15 min agitate
923 KHSO
4
, molten Immerse 1520 s at 300C
924 15 mL HNO
3
(65 %)
100 mL water
925 10 g NaOH
10 g K
3
FeCN
6
100 mL water
Immerse seconds to minutes
926 Thermal etch in air Minutes to 1 h at 13001400C 23702550F
(according to sintering temperature)
927 H
3
PO
4
(85 %) Immerse 3 s to 2 min at 250C 480F
928 Thermal etch in air 3060 min at 1200C 2190F 5 s to 2 min
929 3 mL HCl (32 %)
2 mL HF (40 %)
95 mL water
Immerse 5 s to 2 min
930 2 mL HF (32 %)
98 mL water
Immerse 1015 min
931 5 mL HNO
3
(65 %)
5 mL HF (40 %)
90 mL water
Immerse, up to 20 s
932 10 mL HNO
3
(65 %)
10 mL HF (40 %)
Immerse up to a few min
933 50100 g NaOH
100 mL water
934 15 mL HCl (32 %)
10 mL HF (40 %)
90 mL water
935 30 mL HCl (32 %)
5 mL H
2
O
2
(32 %)
70 mL water
936 30 mL CH
3
COOH (glacial acetic acid)
10 mL H
2
O
2
(30 %)
937 30 mL HCl (32 %)
2 g FeCl
3
100 mL water
938 25 mL HCl (32 %)
8 g FeCl
3
100 mL water
939 15 mL HCl (32 %)
50 mL aq. sodium thiosulfate (16 %)
3 mL aq. CrO
3
(10 %)
30 mL water
Add CrO
3
just before use
940 50 mL HCl (32 %)
50 mL water
Immerse 110 min
941 25 down to 9 mL
HNO
3
(65 %)
25 down to 9 mL CH
3
COOH (glacial
acetic acid)
100 mL glycerol (87%)
Immerse s to min
942 200 mL acetyl acetone
12 mL nitric acid (65 %)
Immerse 218 min in ultrasonic bath to break up
the oxide layer
943 100 mL HNO
3
(65 %)
100 mL H
2
SO
4
+CrO
3
(chromosulfuric acid)
(Variable concentration)
Immerse in 2 min at 70C, time varies
944 60 g CrO
3
(chromium (VI)oxide)
100 mL water
Immerse several hours at 70C
945 HNO
3
(65 %) Polyethylene (PE): Immerse in seconds to
minutes
Polyoxymethylene (POM) and polypropylene
(PP): Immerse in 10 min
946 C
6
H
4
CH
3
2
(xylol) (99.8 %) Polyethylene, polypropylene: Immerse 3 days at
70C
Polyamid, polyethylene: 70C
for 60 s. Nylon 6: 6570C for 23 min. Nylon
6,6: 75C for 34 min
947 C
6
H
15
N (triethylamine (99 %) Immerse seconds to minutes
948 30 mL HCl (32 %)
100 mL distilled water
Immerse 20 s
949
ASTM
Standard
B 657,
Etching
Technique
1
A: Freshly prepared mixture of equal
quantities of 10 % (mass/mass)
aqueous solutions of K
3
Fe CN
6
(III)
(potassium ferricyanide and
potassium or sodium hydroxide)
Etch in mixture A at approx. 20C for 210 s.
Flush the test-piece section with water
immediately, without removing the oxide layer.
Dry the surface carefully with acetone or alcohol
without wiping
950
ASTM
Standard
B 657,
Etching
Technique
2
A: same as A (949)
B: A mixture of equal volumes of
concentrated hydrochloric acid and
water
Etch at approx. 20C in mixture A for 34 min..
then wash in water and etch in mixture B for
approx. 10 s. Next wash in water, then in alcohol
and dry the test-piece section. Finally, etch in
mixture A for approx. 20 s
951
ASTM
Standard
B 657,
Etching
Technique
3
A: same as A (949) Etch in mixture A at approx. 20C for 36 min
12.5.3 Table 12.3Etchant Names
TABLE12.3Etchant names. (This tablewas takenfromASTME407.)
CommonName No. CommonName No.
Acetic glyceregia 89, 226 Groesbecks 19
Alkaline Sodium Picrate 85 Hatch 2
Aqua regia 12 Howarths 84
Barkers 5 Kallings 1 95
Berahas 99, 155, 211215 Kallings 2 94
Carapella 138 Kellers 3
Chrome regia 101 Klemms 210
Contrast 141 Krolls 192, 187
CP 4 60 Marbles 25
El-1R 107 Marshalls 223
Flat 133 Murakamis 98
Flouregia 90, 158 Nital 74
Franks 104 Palmerton 200
Frys 79 Phoschromic 111
G 107 Picral 76
Glyceregia 87 Ralphs 221
Gorsuch 75 Super Picral 77
Grards No. 135 Vilellas 80
Green contrast 94 92-5-3 105
13
Specimen Preparation
13.1 Introduction
THIS CHAPTER COVERS THE PRACTICAL PREPARATION OF THE MATER-
ials stated in Table 11.1 for each material two different methods of the mechanical
preparation process are stated in 68 Material/Preparation Tables. These tables also
containspecic informationonASTMstandards andetching describedinChapter 12.
Electropolishing is coveredby 25methods.
At the end of the chapter, Section 13.5 covers Trouble Shooting regarding the pro-
cess andthe results.
The background for the preparation process, including general advice and hints
for wet abrasive cutting and mounting can be found in Part I. Advice and hints for the
total preparation process covering specic materials will be stated on each Material/
PreparationTable andinSection13.5.
13.2 Mechanical PreparationThe Traditional and
Contemporary Methods
As described in Part I, two basic methods are available for the metallographer, one is
based on SiC grinding paper or other traditional grinding media, referred to as the
traditional method with a T-number, and another method, based on rigid composite
disks RCDs, referredtoas the contemporary method, witha C-number.
Both methods will be stated side-by-side in the Material/Preparation Tables, Sec-
tion13.2.3.
13.2.1 Material/Preparation Tables
Each sheet of Material/Preparation Tables has a number starting with 168. The two
MethodTables, one for the C-Methodandone for the T-Methodare part of the Material/
PreparationTables andhave the same number as the sheet, for example, C-01 andT-01.
Each sheet with tables can be fromthree to six pages, depending on the amount of text.
The tables include as far as possible all relevant information for the preparation pro-
cess of the givenmaterial or material group.
The text is inthe following order:
Material or Material Group, see Section11.2andTable 11.1.
Material Properties: For most materials, four basic properties are stated: Crystal
Structure, Density in g/ cm
3
, Melting Point in C F, and Hardness, for nonferrous
metals the gures for hardness are taken fromASMHandbook, Vol. 02, Properties and
Selection: Nonferrous Alloys and Special-Purpose Materials, ASMInternational, Materi-
als Park, Ohio, USA, 1990. The hardness canbe inHB, HK, HRC, HV, andMohinsome
cases, nohardness is indicated.
Comments on Material: Basic information on the material and the preparation
of the material.
General Comments on:
218
Sectioning
Mounting
Grinding
Polishing
Etching
Purpose: A table indicating relevant methods relating to the purpose of examina-
tionandASTMstandards see Section12andTable 12.1.
PreparationProcess:
Sectioning: Specic indications.
Mounting: Specic indications. Attention: In most cases several types of mount-
ing materials can be used. In these cases only examples, bakelite hot mounting and
acrylics coldmounting are stated.
Grinding: Specic indications.
Polishing: Specic indications.
Contemporary Method: MethodTable.
Traditional Method: MethodTable.
Etchants: Table withrelevant etchants.
13.2.2 Method TablesGeneric MethodsParameters/Consumables
Table 13.1
Generic Methods
The Method Tables covering the C- and T-methods contain a number of parameters
and consumables. The methods should be considered generic, and state a basic pro-
cedure for a given material, using a standard semiautomatic grinder/polisher with ex-
changeable grinding/polishing disks. The specimens are either single specimens or
xed specimens in a holder on a 300 mm 12 in grinding/polishing disk. If material
or equipment/consumables vary, the data must be changed accordingly see belowun-
der Forceper Specimen andTime.
The time stated for each step can in some cases be shortened with the stated times
being to the safe side. This is because the preparation time normally is the only indi-
cation we have of material removal. During the preparation a certain amount of ma-
terial should be removed. The best would be a direct measurement, but innormal prac-
tice only the process time can be measured, giving an indication of material removal
based on experience. Variation in polishing cloths, abrasives, etc., justies the rela-
tively long times indicated to secure a sufcient material removal, but often the metal-
lographer withexperience will be able toshortenthese times.
Steps
The methodis dividedintoa number of steps:
PGplane grinding. This is the rst step and is usually performed with one or sev-
eral sheets of 220 grit SiC grinding paper. In the row, Time see below normally Until
plane is stated, indicating that a sufciently prepared surface, coplanar to the surface
of the paper and with a regular 220 scratch pattern covering the whole specimen sur-
face is obtained.
In some cases a coarser grain like grit 180 can be used before grit 220, but 220
should always be used as the last paper for PG. This ensures the reproducibility of the
method.
For some materials very hard or soft, grit 220 grinding paper is not stated for PG;
Chapter 13 Specimen Preparation 219
in these cases, PG, possibly made in several steps, shall end with the Disk/Cloth stated
inthe MethodTable.
See alsoTimebelow.
FGne grinding. This canbe inseveral steps indicatedwitha number, e.g., FG1.
P polishing. This can be in several steps, indicated with a number, e.g., P 1. In
most methods, the last step indicated is with silica/alumina. Often this step can be
omitted, depending onthe purpose of the preparation.
Parameters
Eachstepcontains a number of parameters:
Disk/Cloth: The surface covering the rotating disk of the grinding/polishing ma-
chine.
AbrasiveType: The abrasive usedfor grinding andpolishing.
Grit/GrainSize: Grit, indicatedwitha P- number corresponding tothe FEPAstan-
TABLE 13.1Comparison Between Surfaces for Grinding and Polishing from a Number of Suppliers with
Abbreviations Used in Method Tables.
Suppliers Buehler Struers Leco
Allied
High
Tech
Mark
V
Lap-
master
Abbreviations in
Method Tables
Dia, pad, bak or
met
Ultra-Prep Diamond
Pad
Diamond
Spot
Pattern
Bonded
Diamond
Disk
Flex
Diamond
Disk
Dia, disk, xed,
res
Apex DGD MD-Piano Cameo
Platinum
RCD, hard ApexHerculesH MD-
Allegro
Cameo
Silver
RCD, soft ApexHercules S MD-Largo Cameo
Gold
Cloth, napless,
v. hard, wov,
syn
Ultra-Pad DP/MD-
Plan
Plan
Cloth
Cloth, napless,
hard, nonwov
syn
Texmet 2000
Texmet 1000
DP/MD-
Pan
Leco Pol
Pan-W
Kempad
Pan-B
Met-X Pan-W
Cloth, napless,
hard, wov, silk
Ultra-Pol DP/MD-
Dur
Silk Silk Silk Silk
Cloth, napless,
hard, wov, syn
Trident
Nylon
DP/MD-
Dac
Gold
Technotron
Nylon
Gold
Label
Nylon
RAM
Nylon
ASR
Nylon
Cloth, napless,
med hard, wov,
wool
DP/MD-
Mol
Broad
cloth
Micro
LP
Cloth, med nap,
soft, syn
Microcloth DP/MD-
Nap
Lecloth Spec-
Cloth
Alpha
A
NTR
Cloth, napless,
soft, porous, syn
Chemomet OP/MD-
Chem
Black
Technotron
Chem-Pol Supreme
dard see Table 6.2 for comparison to American standard. In case of diamond or an-
other abrasive, the grainsize is indicatedinm.
Lubricant Type: The type of mediumusedfor lubricationduring the process.
Rotation Disk/Holder, Comp/Contra: rpm of grinding/polishing disk and speci-
men holder. Comp means complementary: The disk and holder rotates in the same
direction. Contra means counter rotation: The disk andthe holder rotates inopposite
directions.
Force per Specimen: The force in N and lb per specimen. Attention: The force is
based on a 30 mm 1.25 in mounted specimen with the specimen totaling approxi-
mately 50 %of the mount. At 25 mm1 in specimens the force should be reduced with
the factor 0.7. At 40 mm 1.50 in only increase the force up to a maximum of 50 N
11 lb and as compensation, to obtain the necessary material removal, extend the
preparation time with 14 min. This is to avoid a possible overheating of the polishing
cloth that can take place at a force on each specimen of more than 50 N 11 lb. With
SiC grinding paper, a very high force might create heavy damage to the specimen see
Section6.6 andthe paper, if not gluedtothe disk, might be tornaway.
Be aware that the values indicated are for a single specimen. When using a holder
withsay six xedspecimens, the value shouldbe increasedwitha factor 6.
Time: The number of minutes the specimens are in contact with the disk. Atten-
tion: For specimens larger than 30 mm 1.25 in the time should be extended see
Force per Specimen above. Also, if the grinding/polishing disk is smaller than
300 mm 12 in, the time should be extended. At PG, until plane indicates that the
specimensurface shouldbe uniformly coveredwitha regular scratchpattern. The time
used depends on the quality of the sectioning and the alignment of the specimens if a
specimenholder withseveral xedspecimens is used.
ConsumablesAbbreviationsTable 13.1
The methods are based on the use of a number of consumables which are described in
the Method Tables with abbreviations. These consumables have different names from
the different suppliers. For this reason a description is given below for each type of
consumable. Based on this, the user should be able to choose the correct consumable
fromany supplier.
The surfaces used for grinding and polishing can be difcult to describe. For this
reason, a list of surfaces froma number of suppliers is statedinTable 13.1.
The descriptions are given according to the abbreviations used in the Method
Tables, statedalphabetically.
For a more detaileddescriptionof consumables see Part I.
Abbreviations Used in Method TablesDescription of Consumables
Alco: Alcohol-based lubricant. This lubricant should be phased out if possible and re-
placed with water-based lubricant because ethyl alcohol ethanol is considered a dan-
ger tohealthincertaincountries.
Alumina: Al
2
O
3
suspensionas abrasive.
Bak: The abrasive is xedina bakelite bond.
Cloth: A surface made of a textile or other exible material xed to the polishing
diskwithadhesive backing or magnetically.
Disk: A surface for grinding/polishing made of a material with a rigid surface
normally xed to the polishing disk like a cloth, or in some cases a solid disk taking the
place of the polishing disk.
Dia: Diamondas abrasive. This is followedby spr or susp, or bothsee below.
Diamond: Diamondas abrasive.
Fixed: The abrasive is xedinthe surface of the disk.
Hard: A hard rigid composite disk RCD or polishing cloth with a relatively hard,
aggressive surface. A hard cloth could be satin woven, very thin or compact see V.
hard without napandwitha very lowresilience.
Low nap: Polishing cloth with a very short nap could be synthetic material. Low
resilience.
Medium hard: Polishing cloth, napless, witha lowresilience.
Medium nap: Polishing cloth with a medium nap could be a ocked cloth with
relatively highresilience.
Met: The abrasive is xedina metal bond.
Napless: Polishing clothwithout napsee Hardabove.
Nonwov: Polishing clothmade of a nonwovenmaterial.
Oil: Oil-based suspension or lubricant. This type should be avoided because oil-
based products are considered dangerous to health in certain countries. Oil-based dia-
mondsuspensions are only statedinthe T-methods. Lubricants basedonoil emulgated
withwater see below.
Pad: Diamondpaddisk witheither metal or bakelite bond.
Porous: Polishing clothwitha porous surface mostly usedfor oxide polishing.
RCD: RigidComposite Disk.
Res: The abrasive is xedina resinbondlike epoxy, different frombakelite.
SiC paper: SiC wet grinding paper, normally with a C weight backing, and nor-
mally used with plain backing see Section 13.2.4. In certain cases it is an advantage to
use paper withanadhesive backfor heavy automatic grinding.
Silica: Colloidal silica SiO
2
as abrasive.
Silk: Polishing clothmade of silk.
Soft: A soft RCDor cloth with a relatively soft, less aggressive surface. For a cloth,
soft indicates a certainrelative resilience, andcanbe withNap or Napless.
Spr: Diamondspray.
Susp: Diamondsuspension.
Syn: Polishing clothmade of synthetic material.
V.hard: A very hard cloth with an aggressive surface mostly used for ne grind-
ing see Hard above.
Wat: Water-based suspension or lubricant. This type should be preferred because
alcohol- and oil-based products are considered dangerous to health in certain coun-
tries.
Water: Normal tapwater or recirculatedwater, withor without anadditive.
Wat-oil: Lubricant basedonwater withanin-mixedoil forming anemulsion.
Wool: Polishing clothmade of wool.
Wov: Polishing clothmade of a wovenmaterial.
13.2.3 Material/Preparation TablesMethods C-01/T-01 to C-68/T-68
This section contains 68 numbered sheets with Material/Preparation Tables M/PT
that include material/process informationandtwoMethodTables.
Tondthecorrect M/PTuseTable11.1
Using these tables should guide the user to obtaining a satisfactory preparation
result basedonthe material andthe examinationpurpose.
The data stated in the Method Tables are based on a specimen of 30 mm 1.25 in
diameter, clamped in a specimen holder on a 300 mm 12 in grinding/polishing disk.
Using a smaller disk diameter might prolong the preparation time. The specimen area
shouldbe approximately 50%of the mount.
The force indicated is per specimen and should be multiplied with the number of
xedspecimens inthe holder.
The dosing levels for lubricant and abrasives are to be adjusted individually be-
cause temperature, humidity, etc., has a signicant inuence on the preparation pro-
cess. Take care that the surface of the polishing cloth/RCDis just moist whentouched
witha ngertip, not wet.
For manual preparation see Section 13.2.4; often the data indicated in the
T-methods andsome of the C-methods are suitedfor preparationby hand.
For electrolytic polishing see Section13.4.2.
Material/Preparation Tables 01
Material: Hydroxyapatite HA coating
Material Properties: HA: Ca
10
PO
4
6
OH
2
Comments on Material: Ceramic materials that are specially developed for use as
medical and dental implants are called bioceramics. They include alumina and
zirconia, bioactive glasses, glass-ceramics, coatings and composites,
hydroxyapatite HA, tricalcium phosphate TCP and other calcium phosphates
and radiotherapy glasses. The most used bioceramics are calcium phosphate
compounds, especially HA and TCP. This is because they have almost the same
compositions as the skeleton 69 % of bone is HA and they have excellent
biocompatibility. When these ceramics are implanted into the living body in vivo
for a range of time, it is found that they have a strong chemical bond with bone
tissue and nally become a rm attachment. Ceramics are brittle and they are less
suited for load-bearing applications. Therefore, a calcium phosphate like HA is
used as a coating on materials such as titanium alloys or stainless steel where it
can contribute its bioactive properties, while the metallic component bears the
load. Also the coating gives a relatively rough surface that increases the
mechanical xation of the component. The accepted method of applying HA
coatings to metallic implants is plasma spraying. The coatings with HA and TCP
are made with a controlled porosity. This porosity and other features like the
contact between base material substrate and coating should be
materialographically examined.
For preparation of other bioceramics see Material/Preparation Tables M/PT 05
and 06, and for other ceramic coatings see M/PT 14.
Sectioning: HA/TCP are very sensitive materials and should be kept free of
contamination during the cutting. This can be done by masking the areas of
concern using plastic lm and tape. It is important that the specimen is mounted
and vacuum impregnated before sectioning takes place to avoid damaging the
brittle ceramic layer see below. The sectioning should be done on a precision
cutter with a cut-off wheel suited for the base material substrate. The specimen
should be oriented so that the coating is compressed into the substrate during the
cutting see also M/PT 08. The thinnest possible cut-off wheel should be used and
the feed speed should be low.
Mounting: Before sectioning a careful vacuum inltration of the specimen should
take place see M/PT 02 and Section 3.10. It is important that all open pores are
lled with epoxy so that the coating cannot be contaminated or damaged during
the following preparation. The sectioned specimen should possibly be vacuum
impregnated after the sectioning and carefully mounted in epoxy to secure a good
edge retention.
Grinding: In Methods C-01 and T-01 it is an assumption that the base material
can be ground with SiC grinding paper. For grinding surfaces for the harder
ceramics see M/PT 0206.
Grinding times should be kept at a minimum.
Polishing: Also, polishing times should be as short as possible to secure a good
edge retention.
Etching: Normally the HA/TCP layer is not etched, but relief polishing, creating a
physical etching can be used see Section 9.6. For other ceramics see M/PT 02
to 06.
Purpose ASTM Standard See Section 12.4 Method
Case or coating thickness/hardness,
surface layers
C-01
Grain size, grain boundaries E 562, E 1245,
E 1268, E 1382
C-01
Image analysis, rating of inclusion
content
E 562, E 1245,
E 1268, E 1382
C-01
High planeness
Microhardness, hardness C 730, C 849, C 1326,
C 1327, E 384
C-01,
T-01
Microstructure E 3, E 562, E 883,
E 1245, E 1268, E 1382
C-01,
T-01
Phase identication C-01,
T-01
Porosity C-01
Thermal spray coatings: Distribution,
porosity, unmelted particles
C-01
Preparation Process 01
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC, backlite bond or diamond, metal bond
Mounting
Hot
Compression
Mounting
Resin Cold Mounting Resin Epoxy
Time
Minutes
Time
Minutes/Hours
612 h
Grinding
Attention: In C-methods when using RCD: The disk turns concave during use.
When the difference is more than 100150 m between the center and the
periphery, the disk is either discarded or trued.
Polishing
C-01: In some cases a step with a napless, hard, wov, silk cloth and 1 m
diamond, other parameters like step P 2 in method T-01, can be added as P 1,
making the shown P 1 to P 2.
Contemporary Method C-01 For denitions of parameters and consumables see
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 P 1
Disk/Cloth SiC paper SiC paper RCD,
soft
Cloth, napless
soft, porous, syn
Abrasive Type SiC SiC Dia, spr
or susp
Silica
Grit of Grain
Size m
320 500 9 0.04
Lubricant Type Water Water Alco/wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp Contra
Force per
Specimen
N lb
30 7 30 7 40 9 15 3.3
Time
Minutes
Until plane 1 56 24
Traditional Method T-01 For denitions of parameters and consumbles see
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 P 1 P 2 P 3
Polishing
Disk/Cloth SiC
Paper
SiC
Paper
SiC
Paper
SiC
Paper
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC SiC SiC Dia, spr or
susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1000 6 3 0.04/ 0.05
Lubricant
Type
Water Water Water Water Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Comp
or
contra
Comp
or
contra
Comp Comp Contra
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 6 3 12
Material: Boron carbide, B
4
C. Silicon carbide, SiC. Other carbides
Material Properties: B
4
C: Rhombohedral, 2.52 g/ cm
3
, 2450C 4442F, HV
34003800
SiC: Hexagonal/cubic, 3.21 g/ cm
3
, 2300C 4172F, HV 28003600
Comments on Material: High-performance ceramics can roughly be characterized
by structure and function. They can be divided roughly into two categories,
structural and functional ceramics. For those structural ceramics like silicon
nitride, silicon carbide, some types of zirconium dioxide, and a number of mixed
ceramics based on Al
2
O
3
, the properties are directed towards mechanical strength
and other mechanical properties. For those functional ceramics like barium
titanate, zinc oxide, and titanate the properties are directed towards electric,
magnetic, dielectric, and optical properties. Some ceramics like aluminum oxide
the most important high-performance ceramic and zirconium dioxide can be
optimized towards either structural or functional properties. For in-depth
information on ceramics and preparation of ceramics see Carle et al. Ref. 26, Part
I and Elsner et al. Ref. 27, Part I.
In contrast to metals, the evaluation of ceramic materials with light microscopy
can be carried out both by reected light and with some exceptions on thin
sections by transmitted light. For economic reasons, however, the more simple
preparation of specimens for reected light is preferred for routine examination.
For preparation of thin sections see Section 7.13.1.
Compared to metals, ceramics have a high to very high hardness, a low ductility,
and a high brittleness. The high hardness inuences the preparation to a high
degree, but other factors like porosity and brittleness also makes the preparation
difcult.
Brittleness: This might cause pull-outs during cutting and grinding, the ceramic
grains being removed by the abrasive. Pull-outs are especially critical in materials
with a vitreous amorphous phase between the grains. Also cracks and surface
stress can develop during sectioning and grinding see Sections 6.3.2 and 13.6.
Porosity: Often the following should be determined: Total porosity, pore type,
shape, size, and pore size distribution. Pull-outs are often made during the rst
stages of the preparation. These pull-outs can be observed as pores and often will
disturb the analysis of grains, etc. Also, the edges of the original pores will be
damaged and rounded after grinding and ne grinding. In case of differences in
hardness between phases, material can be smeared into the original pores see also
Section 13.6.
Preparation methods: Due to the large variations in ceramic materials, ve Material/
Preparation Tables, 0206, with ten methods, are stated in the following.
Preparation times: A wide variation in time is provided in the method tables. This
is due to the large variations in ceramic materials which in some cases call for
long times, especially in the case of a high porosity.
Sectioning: The bond of the diamond cut-off wheel, its thickness and also the
type, size, and concentration of the abrasive grains are mainly responsible for the
quality of the cut surface. Both metal bond bronze and bakelite bond can be
used. Bakelite bond will give the least damage to the surface and should be used
on brittle/porous materials. Depending on the material properties, feed rate and
rotational speed of the cut-off wheel should be adjusted. The higher porosity and
risk of pull-outs of a material, the slower the feed rate. The rotational speed
should not exceed 2000 rpm and often a lower speed should be used. The surface
quality can normally be improved by using a cut-off wheel with small grain size,
giving a drawback when cutting large specimens as the cutting time is prolonged.
The concentration of diamonds in the bond should not be too high, causing the
wheel to press and pinch, which will create pull-outs and micro and
macrocracks see Section 2.4.2. The same types of material damage develop with
a very hard bond. As a rule the cutting should be made with a thinnest possible
wheel with a grain size around 94 m. Special care should be taken when
clamping specimens. Pressure spots induce high stress which might fracture the
material prior to cutting. In case of very brittle and porous materials, an
impregnation before cutting can be necessary see below and also Section 13.6.
Mounting: Vacuum impregnation: If the porosity is higher than 5 % it is advisable
to impregnate under vacuum in a special apparatus using epoxy of low viscosity
and possibly a dye see Section 3.10. Impregnation should often be repeated after
grinding to close pores that have been opened.
Mounting: Dense ceramic specimens with porosity under 5 % can be prepared
unmounted, clamped in a holder, if the shape permits. Ceramics with a porosity
over 5 % should be impregnated as described above and mounted in a cold
mounting material, preferably epoxy having an addition of hard ller to increase
the hardness of the mounting material. For very stable ceramics that will not be
damaged by the pressure, hot compression mounting in a mineral lled epoxy is
preferred because it provides a mount with a hardness matching the ceramic. In
certain cases hot mounting can be made with acrylic that can be used virtually
without pressure see Section 3.4.
Grinding: Plane grinding PG is normally done with grinding disks with diamond
see Sections 6.6.1 and 6.7.2. PG is causing relatively heavy damage to the
specimen surface; for this reason the nest possible grain size should be chosen. If
using diamond pads, the metallic bond will be the most aggressive, giving short
times but with strong damage. For sensitive ceramics the less aggressive bakelite
bond should be used. If the ceramic is not too hard functional ceramics, SiC
grinding paper might be used.
Fine grinding FG normally takes place using diamond but in relatively soft,
brittle materials, sensitive to pull-outs, SiC paper can be used down to P4000.
Fine grinding FG can be done on different surfaces stated in the Method Tables.
In case of brittle materials the pressure when using RCDs should be kept at 25 N
5.7 lb. On materials with many pores the swarf from the RCD might be forced
into the pores, making examination very difcult. In this case a napless very hard,
woven, synthetic cloth is used for FG.
Polishing: The 6 m and 3 m diamond steps are very important for most
ceramics, removing the heavy deformations from grinding. In the case of pores a
1 m diamond step can be useful to establish the edges of the pores. Oxide
polishing gives chemical mechanical action on ceramics. The effect can often be
increased by adding small quantities of H
2
O
2
32 % and ammonia solution 25 %
to the colloidal silica. This polishing can be used for relief polishing see Section
9.6.
Etching: Ceramic materials may often be difcult to examine under the
microscope since reection differences in the structure are very slight. Various
etching and contrast methods can be used. Oxide materials are often contrasted by
thermal etching in air, vacuum, or various gases. The temperature range is usually
between 1200 and 1650C 2200 and 3000F Approximately 150C 300F
below sintering temperature in air. Etching time can be from 15 minutes to
several hours. Chemical etching mostly takes place only with hot boiling acid
mixtures or molten metal salts. All etching shall take place under a fume hood
with extreme care. Often optical etching like dark eld and DIC can be used on the
specimen surface taken directly from the preparation relief polishing. Also
plasma etching and ion etching are used see Chapter 9.
Purpose ASTM Standard See Section 12.4 Methods
surface layers
C-02
E 1181, E 1382
C-02, T-02
content
E 562, E 1245,
E 1268, E 1382
C-02
High planeness
C 1327, E 384
C-02, T-02
Microstructure E 3, E 562, E 883, E 1245,
E 1268, E 1382
C-02, T-02
Phase identication C-02, T-02
Porosity C-02
Sectioning
Cut-Off Wheel Diamond, metal bond, or bakelite bond
Mounting
Hot Compression
Mounting
Resin Epoxy with
Mineral Filler
Cold Mounting Resin Epoxy
Time Minutes 9 Time
Minutes/
Hours
68 h
Grinding
C-02: Often the FG2 step can be omitted.
T-02: Often the PG step can be omitted.
T-02: PG and FG1: Often both steps or only FG1 should be changed to
bakelite bond. Also, conventional diamond disks, preferably with bakelite bond
can be used see Section 6.6.1.
Attention: In C-methods, when using RCD: The disk turns concave during use.
Polishing
C-02: Often P 2 can be changed to a napless, hard, silk cloth or be omitted.
C-02, T-02: Final polishing step: Chemical mechanical polishing can be used by
adding small quantities of H
2
O
2
32 % and ammonia solution 25 % to the
colloidal silica.
Etching
Etchants for oxides see Material/Preparation Tables 05/06.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 P 1 P 2 P 3
Polishing
Disk/Cloth Dia. disk,
xed, res
Dia. disk
xed, res
RCD,
soft
Cloth,
napless,
hard,
wov, syn
Cloth, med
nap, syn
Cloth,
napless,
soft,
porous
Abrasive Type Diamond Diamond Dia.spr
or susp
Dia.spr
or susp
Dia.spr
or susp
Silica
Grit or Grain
Size m
P220 P1200 9 3 1 0.04/ 0.05
Lubricant Type Water Water Alco or
wat
Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp Comp Contra
Force per
Specimen
N lb
25 6 25 6 30 7 30 7 25 6 15 3.4
Time
Minutes
Until
plane
2 815 10120 210 16
Traditional Method T-02 For denitions of parameters and consumables see
Section 13.2.2.
Polishing
Disk/Cloth Dia
pad,
met
Dia
pad,
met
Cloth,
napless,
v. hard,
nonwov/
wov,
syn
Cloth,
napless,
v. hard,
non
wov/
wov,
syn
Cloth,
napless,
hard,
non
wov,
syn
Cloth,
napless,
hard
wov,
silk
Cloth,
napless,
soft,
porous
Abrasive
Type
Diamond Diamond Dia,
spr or
susp
Dia,
spr or
susp
Dia,
spr
or susp
Dia,
spr
or susp
Silica
Grit or
Grain
Size m
125 40 15 9 6 3 0.04/ 0.05
Lubricant
Type
Water Water Alco/wat Alco/wat Alco/wat Alco/wat
Rotation
Disk/
Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp Comp Comp Comp Comp Comp Contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 30 7 20 4.5 10 2.2
Time
Minutes
Until
plane
210 615 615 530 1060 110
Etchants
Material Etchants see Table 12.2 Uses
B
4
C 901 General structure
SiC with 515 %
oxide additions
902 Secondary phase
remain
SiC with 1 % B
4
C 903 Grain boundaries
SSiC 904 Alpha/alpha /
grain boundaries
Alpha/beta /
phase boundaries
SSiC doped
with B
905 Grain boundaries
SSiC doped
with Al
SiC with B
4
C 907 Grain boundaries
SiSiC 908 Grain boundaries
Material: Chromium carbide, CrC. Titanium carbide, TiC.
Titanium nitride, Tin Cubic boron nitride, CBN. Tungsten
carbide, WC. Other ceramics
Material Properties:
TiC: Face-centered cubic, 4.93 g/ cm
3
, 3140C 5684F, HV 28003500
TiN: Face-centered cubic, 5.4 g/ cm
3
, 2950C 5342F, HV 2450
CBN: Face-centered cubic, 3.48 g/ cm
3
, 1700C 3092F, HV 4500
WC: Hexagonal, 15.7 g/ cm
3
, 2780C 5036F, HV 2400
Comments on Material: See Material/Preparation Tables 02.
Preparation times: A wide variation in time is provided in the Method Tables. This
long times, especially in the case of high porosity.
Sectioning: See Material/Preparation Tables 02.
Mounting: See Material/Preparation Tables 02.
Grinding: See Material/Preparation Tables 02, and directions for specic materials
below.
Polishing: See Material/Preparation Tables 02, and directions for specic materials
below.
Etching: See below and Material/Preparation Tables 02.
surface layers
C-03
E 1181, E 1382
C-03,
T-03
Image analysis, rating of
inclusion content
E 562, E 1245,
E 1268, E 1382
C-03
High planeness
C 1327, E 384
C-03,
T-03
E 1245, E 1268, E 1382
C-03,
T-03
T-03
Porosity C-03
Sectioning
Cut-Off Wheel Diamond, metal bond, or bakelite bond
Mounting
Hot Compression
Mounting
Resin Epoxy with
Mineral Filler
Time
Minutes
9 Time
Minutes/Hours
68 h
Grinding
C-03: PG: If the surface is very rough, start with Dia, disk, xed res, P120.
T-03: The PG step can often be omitted.
T-03: PG and FG 1: Often both steps or only FG 1 should be changed to bakelite
bond. Also conventional diamond disks, preferably with bakelite bond can be
used see Section 6.6.1.
Polishing
Tungsten carbide: C-03: FG 2 can be omitted, P 1 can be changed to a napless,
hard, wov silk cloth and a P 2 step from Method C-02 can be included before the
nal step see also Method C-67.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 P 1 P 2
Polishing
Disk/Cloth Dia, disk,
xed, res
RCD, hard RCD,
soft
Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamond Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 3 0.04/ 0.05
Lubricant Type Water Alco or wat Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp Contra
Force per
Specimen N lb
35 8 35 8 35 8 25 5.5 10 2.2
Time
Minutes
Until plane 56 1015 810 2
Section 13.2.2.
Grinding/ FG 3 P 1 P 2 P 3
Polishing PG FG 1 FG 2
Disk/Cloth Dia,
pad,
met
Dia,
pad,
met
Cloth,
napless,
v. hard,
wov,
syn
Cloth,
napless,
v. hard,
wov,
syn
Cloth,
napless,
hard,
non
wov,
syn
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
Diamond Diamond Dia,
spr/
susp
Dia,
spr/
susp
Dia,
spr/
susp
Dia,
spr/
susp
Silica
Grit or
Grain
Size m
125 40 15 9 6 3 0.04/ 0.05
Lubricant
Type
Water Water Alco Alco Alco Alco
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
30 7 30 7 40 9 40 9 40 9 25 5.5 10 2.2
Time
Minutes
Until
plane
2 68 68 56 56 2
Etchants
CrC, HfC, TiC, VC 909 General structure
TaC 910, 911 General structure
WC 912 General structure
Material: Silicon nitride, Si
3
N
4
Material Properties: Si
3
N
4
: Hexagonal, 3.18 g/ cm
3
, 1900C 3452F, HV 800
1900
Grinding: See Material/Preparation Tables 02.
Polishing: See Material/Preparation Tables 02.
Case or coating
thickness/hardness,
surface layers
C-04
Grain size,
grain boundaries
E 112, E 930,
E 1181, E 1382
C-04, T-04
inclusion content
E 562, E 1245,
E 1268, E 1382
C-04
High planeness
C 1327, E 384
C-04, T-04
E 1268, E 1382
C-04, T-04
Porosity C-04
Sectioning
Cut-Off Wheel Diamond, metal bond
Mounting
Hot Compression
Mounting
Resin Epoxy
with Filler
Time
Minutes
9 Time
Minutes/Hours
68 h
Grinding
C-04: PG: If the surface is very rough, start with Dia, disk, xed, res, P120.
T-04: PG with 125 m diamond can often be omitted.
Polishing
C-04: P 1 can often be omitted so that FG 3 is the last step. In some cases also
FG 3 can be omitted.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 P 1
Polishing
xed, res
RCD, soft RCD, soft RCD, soft Cloth,
napless,
soft, porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit/Grain
Size m
P220 9 3 0.25 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
35 8 50 11 40 9 25 5.5 10 2.2
Time
Minutes
Until
plane
78 78 68 1
Section 13.2.2.
Polishing
Disk/Cloth Dia, pad,
met
Dia, pad,
met
Cloth,
napless,
v. hard,
non wov,
syn
Cloth,
napless,
hard,
non
wov,
syn
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless.
soft,
porous,
syn
Abrasive Type Diamond Diamond Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or
Grain
Size m
125 30 9 6 3 0.04/ 0.05
Lubricant
Type
Water Water Alco or
wat
Alco or wat Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 30 7 40 9 40 9 30 7 15 3.4
Time
Minutes
Until
plane
4 810 56 56 2
Etchants
Si
3
N
4
913 General structure
Si
3
N
4
Si
3
N
4
AlN-Al
2
O
3
Material: Aluminum oxide, Al
2
O
3
. Chromium oxide, Cr
2
O
3
Material Properties: Al
2
O
3
: Trigonal rhombohedral, 4.0 g/ cm
3
, 2050C
3722F, HV 25002800
Cr
2
O
3
: Hexagonal, 5.12 g/ cm
3
, 2340C 4244F, HV 2900
Grinding: See Material/Preparation Tables 02 and directions for specic materials
below.
Polishing: See Material/Preparation Tables 02 and directions for specic materials
below.
surface layers
C-05
E 1181, E 1382
C-05, T-05
inclusion content
E 562, E 1245,
E 1268, E 1382
C-05
High planeness
C 1327, E 384
C-05, T-05
E 1245, E 1268, E 1382
C-05, T-05
Porosity C-05
Sectioning
Mounting
Hot Compression
Mounting
Resin Epoxy with Filler Cold Mounting Resin Epoxy
Time
Minutes
9 Time
Minutes/
Hours
68 h
Grinding
T-05: The PG step with 125 m diamond and FG 2 can often be omitted.
Very hard oxides: Use C-03.
Polishing
C-05: Cr
2
O
3
: The steps FG 1 and P 2 can be omitted.
Section 13.2.2.
Polishing
xed, res
Dia, disk,
xed, res
RCD,
soft
Cloth,
napless,
hard,
wov,
syn
Cloth, med
nap,
soft,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamond Diamond Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or sup
Silica
Grit or
Grain Size m
P220 P1200 9 6 1 0.04/ 0.05
Lubricant Type Water Water Alco
or wat
Alco
or wat
Alco
or wat
Rotation
Disk/Holder
150/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Force per
Specimen
N lb
35 8 35 8 35 8 30 6.6 25 5.5 25 5.5
Time
Minutes
Until
plane
1 910 8 23 12
Section 13.2.2.
Polishing
Disk/Cloth Dia
pad,
met
Dia
pad,
met
Cloth,
napless,
v. hard
wov,
syn
Cloth,
nap-
less,
v. hard,
wov, syn
Cloth,
napless,
hard,
non
wov,
syn
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
Diamond Diamond Dia, spr/
susp
Dia, spr
or
susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
125 40 15 9 6 3 0.04/ 0.05
Lubricant
Type
Water Water Alco or
wat
Alco or
wat
Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
30 7 30 7 40 9 40 9 40 9 20 4.7 15 3.4
Time
Minutes
Until
plane
2 67 67 56 56 2
Etchants
Material Etchants see Tables 12.2 Uses
Al
2
O
3
and small grains
Al
2
O
3
Cr
2
O
3
Material: Barium titanate, BaTiO
3
. Calcium oxide, CaO. Cerium
oxide, CeO
2
. Magnesium oxide, MgO. Silicon oxide, SiO
2
.
Zirconium dioxide, ZrO
2
. Zinc oxide, ZnO. Other oxides. Borides.
Porcelain Tile. Slag. Other traditional ceramics
CeO
2
: Cubic, 7.28 g/ cm
3
MgO: Cubic, 3.5 g/ cm
3
, 2800C 5072F, HV 1130
SiO
2
: Hexagonal, 2,2-2,65 g/ cm
3
, 1710C 3100F, HV 10001250
ZrO
2
: Monoclinic, 5.76 g/ cm
3
, 2690C 4874 F, HV 15001900
Grinding: See Material/Preparation Tables 02 and directions for the specic
materials below.
Polishing: See below and Material/Preparation Tables 02 and directions for the
specic materials below.
surface layers
C-06
E 1181, E 1382
C-06, T-06
inclusion content
High planeness
E 562, E 1245,
E 1268, E 1382
C-06
C 1327, E 384
C-06, T-06
E 1245, E 1268, E 1382
C-06, T-06
Porosity C-06
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
9 Time
Minutes/
Hours
68 h
Grinding
Borides: T-06: FG 4 can be changed to grit 4000 SiC paper and P 1 can be
changed to FG 3 in C-06.
Calcium oxide: C-06: PG can be done with SiC paper grit 500, FG 1 and FG 3
can be omitted by changing FG 2 to 9 m diamond.
Zirconium dioxide: The methods C-02 and C-05 can also be used. Often the step
P 3 in C-05 can be omitted.
Porcelain and traditional ceramics: The step FG 2 can be omitted and FG 3
can be prolonged to 10 min
Tile, slag: Method C-02 can be used with SiC paper grit 220 for PG and FG 1
and P 3 omitted.
T-06: FG 3 and FG 4 can be omitted if a 6 m step is performed see below.
Polishing
T-06: In some cases a P 1 step with 6 m diamond and a napless, hard, wov, silk
cloth should be added with further data like P 1 indicated below. In this case FG
3 and FG 4 may be omitted.
T-06: Often the step P 2 can be omitted.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 P 1 P 2
Polishing
xed, res
RCD,
hard
RCD,
soft
RCD, soft Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
Diamond Dia, spr or
susp
Dia, spr or
susp
Dia, spr
or susp
Dia, spr or
susp
Alumina
Grit or
Grain
size m
P220 9 6 3 3 0.02/ 0.05
Lubricant
Type
Water Alco or
wat
Alco or
wat
Alco or
wat
Oil-wat
Rotation
Disk/
Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Force per
Specimen
N
lb
30 7 40 9 35 8 35 8 20 4.4 15 3.4
Time
Minutes
Until
plane
56 56 56 56 35
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 FG 4 P 1 P 2 P 3
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC SiC SiC SiC Dia,
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 3 1 0.04
/ 0.05
Lubricant
Type
Water Water Water Water Water Alco
or wat
Alco
or wat
Rotation
Disk/
Holder
100/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 20 4.5 25 5.5 25 5.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 58 515 35
Etchants
CaO 919, 920, 921, 922, 923 General structure
MgO 919, 924 General structure
Porcelain 930 General structure
ZnO 925 Grain boundaries
ZrO
2
926, 927 Grain boundaries
Ba TiO
3
Material: Glasses. Optical bers
Comments on Material: There are many different types of glass with different
chemical and physical properties. Glass can be dened as an amorphous solid. A
material is amorphous when it has no long-range order, that is, when there in no
regularity in the arrangement of its molecular constituents on a scale larger than a
few times the size of these groups. For example, the average distance between
silicon atoms in vitreous silica SiO
2
is about 3.6 , and there is no order between
these atoms at distances above about 10 . A solid is a rigid material that does not
ow when it is subjected to moderate forces. This denition is not totally agreed
upon. In the ASTM standard for glass, the material is described as glass is an
inorganic product of fusion which has been cooled to a rigid condition without
crystallization. This description is based on the fact that most glass is made by
cooling a liquid in such a way that it does not crystallize. The difculty with this
view is that glasses can be prepared without cooling from the liquid state. Glass
coatings are deposited from the vapor or liquid solution, sometimes with chemical
reactions. Sodium-silicate glass made by evaporation and baking is
indistinguishable from sodium-silicate glass made by cooling from the liquid.
The main types of glass and their used are: Soda lime containers, windows, lamp
bulbs, pyrex borosilicate headlamps, cookware, laboratory ware vitreous silica
semiconductor crucibles, lamps, optical components, optical bers, alkali lead
lamp tubing, sealing, E lime aluminosilicate bers, lime magnesia
aluminosilicate high temperatures, cookware.
Optical bers are coated strands of optically pure glass with a thickness of
962.5 m that carry digital information over long distances. They are also used
in medical imaging and mechanical engineering inspection.
Preparation of glass is not difcult; if planeness is important, the use of Method
C-07 should be preferred. Glass being a very brittle material can be prepared by
lapping see Section 6.7.7 and Method T-39. As the surface of glass is softened by
water, this liquid should be used to carry the lapping abrasive to obtain the highest
removal rate. Also at polishing a hydrated layer is formed by chemical reaction
and the process can be described as chemical mechanical polishing CMP, the
polishing abrasive only removing the soft reaction layer see Section 7.12.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel
preferably on a precision cut-off machine. Because of the brittleness of the glass,
the feed rate should be low and the use of a thin cut-off wheel should be
preferred. In the case of examination of a coating, the area to be examined should
be under compression when the cut-off wheel enters the work piece see also
Material/Preparation Tables 0810.
Mounting: In general, hot compression mounting cannot be recommended due to
the risk of cracking because of the pressure and thermal cycle in the mounting
press. If considered possible, the hot compression mounting should be with epoxy
with a ller to obtain a high hardness of the mounting material. Cold mounting
can be with acrylics with a ller, epoxy, and polyester.
Grinding: Most glasses can be ground with SiC grinding paper. As an alternative,
diamond disks with xed abrasives in a resin bond should be used combined with
an RCD see Method C-07 if a very plane surface is needed. Also lapping see
Method T-39 and diamond lapping lm can be used see Section 6.7.6.
Polishing: Polishing can be done with diamond, silica, and alumina. The methods
mentioned below may be extended as indicated. To increase the CMP, an acidic
suspension can be used for the nal polishing step by adding a few drops of nitric
acid.
Etching: Normally glasses are not etched.
Purpose alphabetic: ASTM Standard See Section 12.4 Methods
Case or coating
thickness/hardness,
surface layers
C-07
inclusion content
High planeness
C-07
Microhardness, hardness C 730 C-07, T-07
Microstructure C-07, T-07
Porosity C-07
Sectioning
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Acrylics/Epoxy
Time
Minutes
Time
Minutes/Hours
610 min/ 68 h
Grinding
C-07: FG 1 can be omitted and FG 2 changed to 9 m diamond. In this case two
polishing steps are added see below.
Medium hard materials: C-07: PG can be changed to SiC paper grit 500
followed by the three steps mentioned above and below.
Polishing
C-07: A polishing step like P 1 in Method T-07 can be added. If FG 1 is omitted
and FG 2 is changed as mentioned above, two polishing steps, P 1 from C-06 and
P 1 from T-07 are added.
T-07: A step like P 2 in Method T-06 can be used between FG 4 and P 1 to secure
a good edge retention. A few drops of HNO
3
can be added to the nal polishing
step see above.
Section 13.2.2.
Grinding/ PG FG 1 FG 2
Polishing
xed, res
Dia, disk
xed, res
RCD, soft
Abrasive Type Diamond Diamond Dia, spr, or susp
Grit or Grain size m P220 P1200 1
Lubricant Type Water Water Wat
Rotation Disk/Holder 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp
Force per Specimen N lb 30 7 30 7 35 8
Time
Minutes
Until plane 35 7
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 FG 4 P 1
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper SiC paper Cloth,
napless,
soft,
porous
syn
Abrasive Type SiC SiC SiC SiC SiC Silica
Grit or
Grain Size
m
P320 P400 P800 P1000 P4000 0.04/
0.05
Lubricant
Type
Water Water Water Water Water
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp Contra
Force per
Specimen N
lb
20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 2
Material: Anodized coatings. CVD coatings. PVD Coatings
Material Properties: See below.
Comments on Material: Anodizing is used for surface treatment of aluminum
products. The work piece is placed as an anode in an electrolytic bath, and an
aluminum oxide layer is developed. It consists of a solid layer of typically
0.0050.04 m towards the work piece and further a layer with pores 525 m
thick.
Solid aluminum oxide has a hardness in the range of 2000 HV, the hardness of the
porous layer is normally higher than 1000 HV. Hard anodizing is performed at low
temperatures around 5C 41F and gives a coating with few small pores and
thickness up to 50100 m. Anodizing is mainly used for decorative nishing and
protection against wear and corrosion. Metallographic/materialographic
examination is mainly made for measurement of the thickness, microhardness,
and the quality of the coating.
Chemical vapor deposition CVD is a method of forming dense structural parts or
coatings using the decomposition of relatively high vapor pressure gases. Coatings,
which are the most common application of CVD, generally fall into one of two
categories, electronic materials or protective coatings, and are applied either as
conversion coatings or as deposited coatings. Conversion coatings involve the
surface formation of a compound where one of the elemental components is
already present on the surface. At deposited coatings all the elemental constituents
of the coating comes from the vapor phase Protective coatings are deposited onto
a work piece substrate to provide wear, corrosion or erosion protection, or both.
A high number of materials, metals, and ceramics can be used for coatings.
Metallographic/materialographic examination includes the purposes mentioned
above and the adhesion between coating and work piece substrate.
Physical vapor deposition PVD is a method of depositing a coating using a
vacuum chamber and an electric current between the material source and the
work piece. The material source can consist of any electrically conductive metal.
The coating has a thickness of 35 m and the hardness can go up to 5000 HV
using AlTiN as the coating material. Used coating materials are Cr, CrN, Ni, Ag, Ti,
TiAlCN, TiCN, AlTiN, TiO, TiN, and ZrN. The coatings are made for corrosive
protection, decoration, high hardness, improved wear resistance, and reduced
friction.
The metallographic/materialographic examination includes the purposes
mentioned above.
Sectioning: It is important that the cutting takes place perpendicular to the
surface to be prepared. If the plane of the cross section is not perpendicular to the
plane of the coating, the measured thickness will be greater than the true
thickness. For example, an inclination of 10 will contribute a 1.5 % error.
The cutting should preferably take place on a precision cut-off machine using the
thinnest possible cut-off wheel with a bakelite bond, the wheel suited for the work
piece material, not the coating material. The wheel speed should be in the range of
25 m/ s 82 ft/ s. Diamond cut-off wheels should only be used for very hard work
piece materials like ceramics. It is very important that the cut-off wheel is entering
the work piece through the coating at the area later to be examined so that the
coating is compressed into the work piece. This reduces the risk that the true
condition of the coating adherence to substrate material is disturbed. For this
reason also the feed speed should be low.
If shearing is used for sectioning of plate material, the grinding time should be
prolonged to remove damaged material and possible cracks between base material
and coating caused by the shearing see Section 2.7.3
Mounting: It is very important that edge rounding and gaps between sample and
mounting material are avoided. Therefore, a mounting material without shrinkage
should be used, preferably epoxy. On very hard coatings hot mounting with epoxy
with a ller should be preferred if heat and pressure can be tolerated.
Also a phenolic resin with carbon bers can be of advantage. In hot mounting a
special application can be made to secure the edge: Tightly wrap up the specimen
in Al-foil household type. This gives a good separation between mounting
material and coating. Choose a mounting material with hardness as close as
possible to the hardness of the coating. As an alternative cold mounting with
epoxy can be used, and in case of porosity, vacuum impregnation can be an
advantage see Section 3.10.
Grinding: The preparation process should secure the highest possible edge
retention. This means that all grinding, either on SiC grinding paper or rigid
composite disks RCDs, should be as short as possible.
Polishing: Also the polishing steps should be kept as short as possible.
Etching: For most examinations no etching is needed.
Case or coating
thickness/hardness,
surface layers
B 487, B 578, B 681, B 748 C-08
Grain size, grain boundaries B 390, E 112, E 930,
E 1181, E 1382
C-08, T-08
Heat inuenced zone C-08, T-08
Image analysis, rating
of inclusion
content
E 562
E 1245, E 1268, E 1382
C-08
High planeness
Microhardness, hardness B 578, C 730, C 849,
C 1326, C 1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
C-08, T-08
Microstructure E 3, E 407, E 883 C-08, T-08
Porosity C-08, T-08
Sectioning
Cut-Off Wheel Bakelite, Al
2
O
3
or SiC depending on the work piece
substrate material 0.5 mm 0.019 in thickness
Mounting
Hot Compression
Mounting
Time
Minutes
9 Time
Minutes/
Hours
68 h
Grinding
C-08, T-08: If possible make PG step with SiC paper grit 500.
C-08: FG 1 and FG 3: Often these two steps can be omitted.
C-08: For CVD coating and PVD coatings on a hard substrate change PG and FG
1 to PG from Method C-09.
C-08: For preparation of CVD and PVD coatings, use shortest times stated.
Polishing
C-08: For preparation of anodized coatings, the P 1 step can be changed to a
napless, hard, wov, silk cloth.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper Sic paper RCD, soft RCD, soft Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC Dia, spr or
susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit/Grain
Size m
P320 P500 9 3 3 0.04/ 0.05
wat
Alco or
wat
Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 25 4.5 20 4.5 10 2.3
Time
Minutes
Until
plane
0.51 38 37 1.55 0.51
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
non
wov,
syn
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC SiC SiC Dia,
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 1200 6 3 0.04/ 0.05
Lubricant
Type
wat
Alco or
wat
Rotation
Disk/
Holder
r/min/r/min
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
25
5.7
25
5.7
25
5.7
25
5.7
20 4.3 20 4.3 10 2.3
Time
Minutes
Until
plane
0.51 0.51 0.51 35 25 0.51
Material: Electrolytically deposited coatings: Galvanization,
plated coatings, other coatings. Diffusion coatings. Other
coatings
Comments on Material: Electrolytically deposited coatings are produced by
electrolysis, the work piece substrate placed as a cathode in an electrolyte with
an anode of the coating material. In galvanization, zinc is used as the coating
material and in electroplating plating other metals like chrome may be used. For
Zn coatings also see Material/Preparation Tables 10.
Diffusion coating is a process in which the work piece is either coated with
another material and heated to a sufcient temperature in a suitable environment
or exposed to a gaseous or liquid medium containing the other material, causing
diffusion of the coating material into the work piece surface resulting in a change
of the composition and properties of the surface see also Material/Preparation
Tables 37.
An example of other coatings is electroless plating in which metal ions in a dilute
aqueous solution are plated out on the work piece by means of an autocatalytic
chemical reduction.
Typical examples of metallographic/materialographic examination of coatings are
the layer thickness, porosity of coating, cracks, adherence to base material, and
the diffusion zone between substrate work piece and coating.
Mounting: See Material/Preparation Tables 08. As an alternative to epoxy for cold
mounting, acrylics with a ller can be used.
Polishing: See Material/Preparation Tables 08. For zinc coatings, see Material/
Preparation Tables 10.
Etching: For most examinations, etching is not needed, but an etchant for Sn
coating on steel is stated below and etchants for Zn coatings are stated in Material/
Case or coating
thickness/hardness
surface layers
B 487, B 587, B 748, B 931, B 933, B 934 C-09
Grain size, grain boundaries B 390, E 112, E 930, E 1181, E 1382 C-09, T-09
of inclusion
content
E 562, E 1245, E 1268, E 1382 C-09
High planeness
Micohardness, hardness B 578, C 730, C 849, C 1326,
C 1327, E 10, E 18, E 92, E 103,
E 110, E 140, E 384, E 448
C-09, T-09
Porosity C-09, T-09
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC according to base material, bakelite
bond, 0.5 mm 0.019 in thickness
Mounting
Hot Compression
Mounting
Resin Epoxy Cold Mounting Resin Epoxy
Time
Minutes
810 Time
Minutes/Hours
68 h
Grinding
Plated coatings: C-09: Use SiC paper grit 500 for PG.
Diffusion coatings: C-09: FG 1: RCD, soft can be changed to a napless v. hard,
wov, syn cloth.
C-09: PG: SiC paper grit 220 or grit 320 can be used instead of a diamond disk.
C-09: For some Zn coatings where water sensitivity is suspected, diamond spray
and alcohol-based lubricants are preferred at the step FG 1 and P 1. If silica in P
2 is too alkaline use alumina, pH 7-7.5.
C-09: P 2: For sensitive layers this step can be changed to a napless, hard, wov,
silk cloth with 1 m diamond spray and alcohol-based lubricant.
When the difference is more than 100150 m
between the center and the periphery, the disk is either discarded or trued.
Polishing
C-09: A step like P 3 in Method T-17 can be added before the nal step.
Section 13.2.2.
Grinding/ PG FG 1 P 1 P 2
Polishing
xed, res
RCD,
soft
Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamond Dia, spr
or susp
Dia, spr
or susp
Silica
Grit/Grain Size m P220 9 3 0.04/ 0.05
Lubricant Type Water Alco or wat Alco or wat
Rotation Disk/Holder 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Contra
Force per Specimen N lb 25 5.7 25 5.7 25 5.7 15 3.4
Time
Minutes
Until plane 35 35 0.51
Section 13.2.2.
Grinding/ PG FG 1 Fg 2 FG 3 P 1 P 2
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC SiC Dia, spr
or
susp
Silica
Grit or Grain Size m P220 P320 P500 P1200 3 0.04/ 0.05
Lubricant Type Water Water Water Water Wat-oil
Rotation Disk/Holder
rpm/rpm
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Comp/Contra Comp
or
contra
Comp
or
contra
Comp
or
contra
Comp Comp Contra
Force per Specimen
N lb
30 7 30 7 30 7 30 7 30 7 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 23 1
Etchants
Material Etchants see Table
12.2
Uses
Sn coating on steel 183 General structure
Zn coatings, see M/PT-10
Material: Hot dip zinc coatings. Other Zn coatings
Comments on Material: In hot dipped zinc coating the work piece is dipped into
molten zinc. This is a very efcient way to apply a sufcient thickness of zinc to
obtain a very good corrosion protection.
Other Zn coatings include electrolytically deposited coatings mentioned in Material/
Preparation Tables 09, and the below stated methods should be seen as
alternatives to Methods C/T-09.
The metallographic/materialographic examination of Zn coatings includes
thickness measurement of the coating, adhesion of coating to base material,
microstructure of base material, and coating and failure analysis like cracks in the
coating.
Mounting: See Material/Preparation Tables 08. It is very important that mounting
is done without gaps between sample and mounting material because the water
sensitive zinc is strongly inuenced by water bleeding from the gap. Degrease the
specimen in acetone before mounting. Place the specimen in clips to keep it
upright. Use epoxy for cold mounting or bakelite with a carbon ller for hot
mounting. In case of having many pieces of coated sheets in the same mount,
gluing the sheets together with instant glue and hot mounting give good results
without bleeding of liquid from the gaps between the sheets.
Grinding: Pure zinc is very soft and sensitive to water. The purer the zinc of the
coating is, the softer and the more water-sensitive it becomes. Therefore, plain, hot
dipped, and electrolytically deposited coatings are soft and prone to mechanical
deformation and they cannot be cleaned with water. Ethanol or isopropanol
should be used for cleaning. It is important that the grinding steps are properly
performed to avoid excessive damage that is very difcult to remove during the
polishing.
Polishing: Water-free suspensions and lubricants should be used for polishing of
zinc coatings. The polishing can be nished with a cleaning step see below.
Etching: Etching times should be short and concentration of etchant low to avoid
over-etching see below.
surface layers
B 487, B 578, B 748 C-10
Grain size, grain boundaries E 112, E 930, E 1181, E 1382 C-10, T-10
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1268, E 1382 C-10
High planeness
Microhardness, hardness B 578, C 730, C 849, C 1326,
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384,
E 448
C-10, T-10
Porosity C-10, T-10
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC according to base material, bakelite
Mounting
Hot Compression
Mounting
Resin Bakelite with
Carbon Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
Polishing
C-10: P 1 can be changed to a hard silk cloth as used in P 2 and P 3 can be
omitted.
C-10 and T-10: The polishing can be nished with a cleaning step see P 3 in
Method C-10. This is to avoid contact with water to the nished surface. For all
other cleaning alcohol should be used.
In the case of very sensitive Zn coatings, water free suspensions and lubricants
should be used with Method C-10.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 P 1 P 2 P 3
Disk/Cloth SiC paper RCD, soft Cloth
napless,
hard,
wov, syn
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
See
above
Grit/Grain Size m P320 9 3 1
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp Comp
Force per
Specimen N lb
30 7 30 7 25 5.7 20 4.5 10 2.2
Time
Minutes
Until plane 4 46 46 1520 s
Section 13.2.2.
Grinding/ PG FG 1 Fg 2 FG 3 P 1 P 2
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
med
hard,
wov,
wool
Abrasive Type SiC SiC SiC SiC Dia, spr or
susp
Dia,
spr or
susp
Grit or
Grain
Size m
P220 P320 P500 P1200 3 1
Lubricant
Type
Water Water Water Water Alco Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp
Force per
Specimen
N lb
20 4.3 20 4.3 20 4.3 20 4.3 20 4.3 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 46 12
Etchants
Zn-Fe 74a Structure of galvanized sheet
Material: Paint layers
Comments on Material: Paint layers can be very different, either charged directly
on the base material of the work piece or on a coating.
The metallographic/materialographic examination includes measurement of layer
thickness, adhesion to work piece surface, and failures in the paint.
Sectioning: Sectioning shall take place as mentioned for coatings, see Material/
Grinding: See Material/Preparationn Tables 08.
Polishing: See Material/Preparation Tables 08. The paint coat normally is very soft
compared to the base material. This increases the risk of edge rounding and the
polishing times should be kept to a minimum, depending on the base material.
Etching: For etching, an etchant suited for the base material should be used.
Case or coating
thickness/hardness,
surface layers
B 487, B 578, B 748 C-11
E 1181, E 1382
C-11, T-11
of inclusion content
E 562, E 1245,
E 1268, E 1382
C-11
High planeness
C 1326, C1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
C-11, T-11
Porosity C-11, T-11
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC, bakelite bond, 0.5 mm 0.019 in
thickness
Mounting
Hot Compression
Mounting
Resin Bakelite or Epoxy
with Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
T-11: FG 1: This step with grit 320 is only needed at hand preparation.
Attention: In C-methods, when using RCD: The disk concave during use. When
the diffenence is more than 100150 m between the center and the periphery,
the disk is either discarded or trued.
Polishing
C-11: P 2 can changed to step P 2 in Method T-11.
T-11: P 2 can be changed to P 2 in Method C-11.
Contemporary Method C-11 For denitions of parameters and consumable see
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 P 1 P 2
Disk/Cloth SiC paper SiC paper RCD, soft Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft, porous,
syn
or susp
Dia, spr
or susp
Silica
Grit or Grain
Size m
220 500 9 3 0.04/ 0.05
wat
Alco or wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
35 8 35 8 20 4.5 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 46 26 1
Traditional Method T-11 For denition of parameters and consumables see
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 P 1 P 2
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
med
hard,
wov,
wool
Abrisive Type SiC SiC SiC SiC Dia, spr
or susp
Dia, spr
or susp
Grit or Grain Size m P320 P500 P1200 P4000 3 1
Lubricant
Type
Wat
Wat-oil
Rotation Disk/Holder 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
contra
Comp Comp Comp Comp Comp
Force per Specimen
N lb
20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 25 13
Material: Thermal spray coatings: Flame, HVOF High Velocity
Oxygen Fuel and other coatings
Comments on Material: Thermal spraying is a group of processes in which nely
divided metallic or nonmetallic surface materials are deposited in a molten or
semimolten condition on a substrate to form a spray deposit. The surfacing
material may be in the form of powder, rod, cord, or wire. A common feature of
all thermal spray coatings is their lenticular grain structure resulting from the
rapid solidication of small globules, attened from striking a cold surface at high
velocities.
Flame spraying or the combustion wire thermal spray process is basically the
spraying of molten metal ceramics and cements can be used in rod or composite
form onto a surface to provide a coating.
Material in wire form is melted in a ame and atomized using compressed air to
form a ne spray. This ame spray process is called a cold process relative to
the work piece material being coated, as the substrate work piece temperature
can be kept low during the processing, avoiding damage, metallurgical changes,
and distortion to the substrate material. Flame spraying is used for improvement
of wear resistance, etc., at machine elements and for anticorrosion coatings.
HVOF/HVAF high velocity oxygen fuel/high velocity air fuel and LVOF low
velocity oxygen fuel are spraying processes using material in powder form which
is melted in a ame to form a ne spray. In HVOF the spray velocity is extremely
high and the coatings are very dense, strong, and show low residual tensile stress
or in some cases compressive stress. This enables very much thicker coatings to be
applied than possible with other spray processes.
Metallography/materialography is used for examination of a number of features,
decisive for the quality of the coating, described below.
Bond: The bonding at the thermal spray coating/substrate interface and between
the particles in the spray coating should be such that both mechanical interlocking
and diffusion bonding occur. A number of factors like cleanliness, temperature,
time, velocity, and physical/chemical properties inuence the bonding.
Microstructure: The coatings show lamellar or attened grains appearing to ow
parallel to the substrate. The structure is heterogeneous that is due to the
variations in the condition of the individual particle on impact. An important
feature is the presence of unmelted particles and also whether the coating contains
some porosity.
Porosity: This is present in most thermally sprayed coatings due to a lack of fusion
between sprayed particles or the expansion of gases generated during the spraying
process. A porosity of 1 to 25 % is normal but can be inuenced by changes in
process and materials.
Linear detachment: Cooling and solidication of most materials is accompanied by
contraction or shrinkage. This generates a tensile stress within the particle and a
compressive stress within the surface of the substrate. As the coating is built up,
so are the tensile stresses in the coating. At a certain point the thickness will be
reached while the tensile stresses will exceed that of the bond strength or cohesive
strength and linear detachment will occur.
Oxides: Most metallic coatings suffer oxidation during normal thermal spraying in
air. The products of oxidation are usually included in the coating. Oxides are
generally much harder than the coating metal. Oxides in coatings can be
detrimental towards corrosion, strength, and machinability. During metallographic/
materialographic examination it is important to be able to discriminate between
oxides and pores voids. Other features to be examined are coating thickness,
hardness, and microhardness.
Metallographic/materialographic preparation: Preparation of thermal spray
coatings is more difcult than the average specimen. This is due to the difference
in coating material and substrate work piece material, the complicated nature of
the coating, etc. All stages in the preparation process should be carefully executed
to obtain a sufcient result; a special problem is to reveal the true porosity see
Section 13.6.4, Pull-OutsFalse Porosity. As the preparation process has this
very important inuence on the microstructure, it is important that a systematic
and reproducible process is maintained. The preparation process is described
below, and two ASTM standards cover specically the preparation and
examination of thermal sprayed coatings:
Standard Guide for Metallographic Preparation of Thermal Sprayed Coatings E
1920 and Test Method for Determining Area Percentage Porosity in Thermal
Sprayed Coatings E 2109.
Sectioning: Care must be exercised to avoid affecting the soundness of the coating
and the interface between the coating and the substrate. Friable, porous, or brittle
coatings may be vacuum impregnated with epoxy before sectioning to protect the
specimen see Section 3.10. Specimens should always be sectioned such that the
coating is compressed into the substrate. If the coating or interface is placed under
tension, it may cause the coating to be pulled away from the substrate or result in
delamination of the coating. If a part of the specimen has been under stress, this
part should not be included in the examination of the specimen. Sectioning
methods creating strong damage to the specimen, even wet cutting with a normal
cut-off wheel, should be avoided. Preferably precision cutting should be used with
the thinnest possible cut-off wheel, using Al
2
O
3
or SiC in a bakelite bond
according to the substrate material. Only in case of very thick ceramic layers a
diamond wheel should be used. The cut-off wheel speed should be in the range of
25 m/ s 82 ft/ s and the feed speed should be low to minimize the damage.
should be used, preferably epoxy. At very hard coatings hot mounting with epoxy
with a ller should be preferred if heat and pressure can be tolerated. Also, a
phenolic resin with carbon bers can be an advantage. However, only cold
mounting with epoxy should be used in the initial determination of the true
characteristics of a coating before considering the use of any other mounting
material because hot mounting might inuence the microstructure. As a rule hot
mounting should only be used for mounting of dense, nonfriable coatings with
substrates a minimum of 1.5 mm 0.06 in thick. Choose a mounting material with
hardness as close as possible to the hardness of the coating. In case of porosity,
vacuum impregnation can be required see Section 3.10 and often the use of a dye
can be of advantage see Section 3.10.1.
Grinding: Grinding may have a strong inuence on the edge retention and a
number of artifacts like false porosity and smearing see below. Due to the many
different types of thermal coatings and substrate materials, the grinding sequence
will vary, but it should be possible to nd a useable method among the methods
described in the Material/Preparation Tables 1215.
Polishing: It is very important to evaluate the type of coating and substrate before
the start of the preparation because of the high variety of coatings and substrate
materials. Two important features are whether one or more of the components in
the microstructure are brittle or ductile. In case of a brittle component, often
pull-outs will take place during the grinding, causing a false porosity that can
only be removed with a prolonged polishing. In case of a ductile component this
might be smeared into the existing pores voids and a too dense microstructure
might appear. To avoid this the use of SiC grinding paper should be reduced and
grinding on rigid composite disks RCDs or very hard cloths followed by at least
two polishing steps should be used. See Section 13.6.4, Pull-OutsFalse Porosity,
where a number of thermal spray coatings are shown.
Etching: The thermally sprayed coating is usually not etched, but etchants for the
substrate material can be used, mentioned under this material.
Case or coating
thickness/hardness,
surface layers
B 487, B 748 C-12
Grain size, grain
boundaries
E 112, E 930, E 1181 C-12, T-12
of inclusion
content
E 45, E 562, E 768,
E 1245, E 1382, E 2109
C-12
High planeness
Microhardness,
hardness
B 578, C 730, C 849,
C 1326, C 1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384, B 448
C-12, T-12
E 768, E 883, E 1245,
E1920
C-12, T-12
Porosity E 2109 C-12
Thermal spray coatings:
Distribution, porosity,
unmelted particles
E 1920, E 2109 C-12, T-12
Sectioning
Cut-Off Wheel Al
2
O
3
thickness
Mounting
Hot Compression
Mounting
Resin Epoxy or Bakelite
with Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
Polishing
C-12: At certain thermal spray coatings where longer polishing times are needed,
the P 1 step can be changed to diamond with grain size 6 m and the P 1 and P
2 steps shown will be P 2 and P 3.
Section 13.2.2.
Polishing
xed, res
Dia, disk
xed, res
RCD,
soft
Cloth,
napless,
hard, wov,
syn
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Alumina
Grit/Grain Size m P220 P1200 9 3 0.02/ 0.05
Lubricant Type Water Water Alco or wat Alco or wat
Rotation Disk/Holder 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N lb
25 5.7 30 7 30 7 25 5.7 10 2.2
Time
Minutes
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 FG 4 P 1 P 2
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, syn
Cloth,
med.
nap,
soft,
syn
Abrasive
Type
SiC SiC SiC SiC SiC Dia, spr
or susp
Dia, spr
or susp
Grit or
Grain Size
m
P220 P320 P500 P1200 P2400 3 1
Lubricant
Type
Water Water Water Water Water Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 20 4.5 20 4.5
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 3 0.51
Material: Plasma spray coatings: Metallic layers
Comments on Material: Plasma spraying is a thermal spraying process in which a
nontransferred arc is utilized as the source of heat that ionizes a gas that melts
and propels the coating material to the work piece substrate. Compared to
combustion ame spraying the plasma spraying provides rapid heating, low
particle ight time, more inert ame and higher velocity, resulting in a ner,
denser microstructure with less oxide inclusions. For further information see
Etching: See Material/Preparation Tables 12.
Case or coating
thickness/hardness,
surface layers
B 487, B 748 C-13
Grain size, grain boundaries E 112, E 930, E 1181 C-13, T-13
Image analysis,
rating of inclusion
content
E 45, E 562, E 768, E 1245,
E 1382, E 2109
C-13
High planeness
Microhardness,
hardness
B 578, C 730, C 849, C 1326,
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384, E 448
C-13, T-13
E 768, E 883, E 1245,
E 1920
C-13, T-13
Distribution, porosity,
unmelted particles
E 1920, E 2109 C-13, T-13
Sectioning
Cut-Off Wheel Al
2
O
3
thickness
Mounting
Hot Compression
Mounting
with Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
C-13: PG: Grit 320 should be used if possible.
Polishing
C-13: P 2: Can be changed to P 2 from Method T-12.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper RCD, soft RCD,
soft
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC Dia,
spr or
susp
Dia,
spr or
susp
Dia,
spr or
susp
Silica
Grit/Grain
Size m
P220 9 3 3 0.04/ 0.05
Lubricant
Type
Water Alco or wat Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N
lb
25 5.7 25 5.5 25 5.5 25 5.5 10 2.3
Time
Minutes
Until
plane
46 57 34 0.51
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Alumina
Grit or
Grain Size
m
P220 P320 P550 P1200 P4000 3 0.02/ 0.05
Lubricant
Type
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 15 3.4 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 34 0.51
Material: Plasma spray coatings: Ceramic layers
Comments on Material: See Material/Preparation Tables 12 and 13.
Sectioning: Depending on the substrate an Al
2
O
3
or SiC, bakelite bond, or
diamond metal bond, 0.5 mm 0.019 in thickness cut-off wheel should be used. In
case of very brittle coatings a diamond wheel with bakelite bond should be used,
see Material/Preparation Tables 12.
Grinding: Remove at least 500 m during the PG step to ensure that all damage
from the cutting is removed. Pull-outs will be developed during the grinding,
resembling pores see below.
See also Material/Preparation Tables 12.
Polishing: Polishing must be performed until the pull-outs made during the
grinding are removed. Check the porosity and go on polishing with the P 1 step
until the porosity level is constant.
See also Material/Preparation Tables 12.
Case or coating
thickness/hardness,
surface layers
B 487, B 748 C-14
of inclusion
content
E 45, E 562, E 768,
E 1245, E 1382, E 2109
C-14
High planeness
C 1326, C 1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
C-14, T-14
E 768, E 883, E 1245,
E 1920
C-14, T-14
Distribution,
porosity, unmelted particles
E 1920, E 2109 C-14, T-14
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC, bakelite bond, or diamond metal or
bakelite bond, 0.5 mm 0.019 in thickness
Mounting
Hot Compression
Mounting
Resin Epoxy or
Bakelite
with Filler
Cold Mounting Resin Epoxy vacuum
impregnation
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
The PG step is very important see above.
C-14, T-14: PG: At thin or brittle layers, or both, change to PG from Methods
T-13.
C-14: FG 1: For very hard ceramic layers, the disk should be changed to RCD,
hard.
Polishing
C-14, T-14: The time for the step, P 1 depends on the porosity level see M/PT 12.
Section 13.2.2.
Polishing
xed, res
RCD,
soft
RCD,
soft
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit/Grain Size m P220 9 3 3 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N lb
30 7 40 9 35 8 35 8 15 3.4
Time
Minutes
Until
plane
45 3 34 1
Section 13.2.2.
Polishing
Disk/Cloth Dia, pad, met Cloth, napless,
v. hard, non
wov/wov, syn
Cloth, napless,
hard,
non-wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamond Dia, spr or susp Dia, spr or susp Alumina
Grit or Grain Size m 40 9 3 0.02/ 0.05
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Contra
Force per
Specimen N lb
25 5.7 25 5.7 25 5.7 20 4.5
Time
Minutes
Until plane 67 34 12
Material: Plasma spray coatings: Composite layers
Material Properties: See Material/Preparation Tables 12 and 13.
Comments on Material: See Material/Preparation Tables 12 and 13.
Sectioning: See Material/Preparation Tables 12 and 14.
Grinding: See Material/Preparation Tables 12 and 14.
Polishing: See Material/Preparation Tables 12 and 14.
Case or coating
thickness/hardness,
surface layers
B 487, B 748 C-15
Grain size, grain
boundaries
E 112, E 930, E 1181 C-15,
T-15
Heat inuenced zone C-15,
T-15
Image analysis,
rating
of inclusion
content
E 45, E 562, E 768, E 1245,
E 1382, E 2109
C-15
High planeness
Microhardness,
hardness
B 578, C 730, C 849, C 1326,
C 1327, E 10
E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-15,
T-15
E 768, E 883, E 1245,
E 1920
C-15,
T-15
T-15
Thermal spray
coatings:
Distribution,
porosity, unmelted
particles
E 1920, E 2109 C-15,
T-15
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC, bakelite bond, or diamond metal bond,
0.5 mm 0.019 in thickness
Mounting
Hot Compression
Mounting
with Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
C-15: PG: For softer composites this can be changed to PG or FG 1 in Method
T-15
C-15: FG 2 and FG 3: It is important that the true level of pores is obtained at
these steps.
C-15: FG 1: If the composite layer is very hard ceramic, the disk can be
changed to RCD, hard. During the FG 2 step the level of porosities should be
evaluated, and FG 2 shall go on until the level stays constant.
T-15: If the composite layer contains hard ceramics 800 HV, SiC paper
should be changed to diamond pads. PG: 40 m, met, FG 1: Diamond pad
10 m, bak. See also Method T-14.
Polishing
C-15 and T-15: The last step can be changed to P 2 from Method T-12.
T-15: P 1 and P 2: It is important that the true level of pores is obtained at these
steps. During the P 2 step the level porosities should be evaluated, and P 2 shall
go on until the level stays constant.
Section 13.2.2.
Polishing
Disk/Cloth Dia, disk
xed, res
RCD, soft RCD,
soft
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
soft, porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit/Grain
Size m
P220 9 3 3 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 35 8 35 8 25 5.7 10 2.3
Time
Minutes
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
v.
hard,
nonwov/
wov,
syn
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
spr,
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1000 6 3 0.04/
0.05
Lubricant
Type
Water Water Water Water Alco
or
wat
Alco
or
wat
Rotation
Disk/Holder
300/
150
300/150 300/150 150/150 150/
150
150/
150
150/
150
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp Comp Comp Comp Comp Contra
Force per
Specimen
N lb
30 7 25 4.5 25 4.5 25 4.5 20
4.5
20
4.5
10
2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 1520 10 0.51
Material: Composites: SiC bers in Ti matrix
Comments on Material: A composite material is characterized as consisting of
two or more different components. Depending on the bonding component used, a
distinction is made between metal matrix composites, ceramic matrix composites,
and plastic matrix composites. The intention behind a composite material is to
combine the favorable properties of various materials and, at the same time,
compensate for less favorable properties. The required combination of properties
determines the choice of materials. Another vital factor in achieving a material
with favorable properties is whether the various components work together. For
example, good bonding between the components is important and no
unintentional component alterations may occur during the production process. In
the area of metal matrix composites, cermets, the high hardness of ceramic
particles or the extreme strength of ceramic bers, will typically be combined with
the toughness of the metal.
Metallographic/materialographic examination includes separation between
components, porosity, and transitions between components. Due to the very wide
variety of composite materials it is only possible to indicate six basic methods in
the Material/Preparation Tables 16 to 18, and these should be changed according
to the given material following the comments stated for each stage/step in the
preparation process.
The most common problems with the preparation of composites are related to
relief and unplaneness between the different components, often combined with
smearing of material from a soft component covering pores, etc., of the other
components.
Sectioning: Depending on the hardness of the components of the composite,
sectioning should be made as wet abrasive cutting with an Al
2
O
3
/ SiC, bakelite
bond cut-off wheel or a diamond wheel. If the bond between the components in
the composite is sufciently high, a diamond wheel with metal bond can be used.
If the bond is not adequate or one of the components is very hard and brittle, or
both, bakelite bond should be used. The sectioning should be performed with
great care, and often it is an advantage to use a precision cutting machine for the
cutting using thin wheels see Material/Preparation Tables 12. A band saw should
only be used for cutting of a large piece, later to be cut with a cut-off wheel.
Mounting: As composite materials often have very high differences in hardness,
mounting in a relatively hard mounting material is of advantage. In the case of
porosity in one or more of the components, vacuum impregnation may be needed
see Section 3.10.
Grinding: In case of very high differences in hardness, SiC grinding paper may be
less suited for grinding, removing too much material from the soft component
creating relief. In case of ceramic components, diamond disks should be used for
grinding.
Polishing: As a general rule, both grinding and polishing times should be kept as
short as possible to secure the planeness. It is important, however, that the hardest
component is correctly ground/polished at each step before going on to the next
ner step.
Etching: Etching is performed according to the components of the composite.
Case or coating
thickness/hardness,
surface layers
C-16
E 562, E 1245, E 1382 C-16
High planeness
C 1326, C 1327, E 10,
E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-16, T-16
E 1245, E 1382
C-16, T-16
Porosity C-16
Sectioning
Mounting
Hot Compression
Mounting
with Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
The material is relatively difcult to prepare because of the very hard SiC and
the relatively soft and tough Ti. It is important that the SiC phase is nished in
each step, before going to the next ner step.
Polishing
Ti may be chemically-mechanically polished: C-16: P 2 and T-16: P 3: Use the
solution: 96 mL silica, 2 mL H
2
O
2
30 %, 2 mL NH
3
solution 25 %.
Section 13.2.2.
Polishing
xed, res
Dia, disk
xed, res
RCD,
soft
RCD,
soft
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamond Diamond Dia, spr
orsusp
Dia, spr
or susp
Dia, spr
orsusp
Silica
See note
Grit/Grain
Size m
P220 P600 9 3 1 0.04/ 0.05
Lubricant
Type
Water Water Alco or
wat
Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N
lb
30 7 30 7 30 7 20 4.5 20 4.5 10 2.3
Time
Minutes
Until
plane
2 4 5 3 1
Section 13.2.2.
Grinding/ PG FG 1 P 1 P 2 P 3
Polishing
Disk/Cloth Dia,
pad,
met
Dia,
pad,
bak
Cloth,
napless,
v. hard,
nonwov/
wov, syn
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamon Diamond Dia, spr or
susp
Dia, spr or
susp
Silica
See note
Grit or Grain
Size m
40 10 6 1 0.04/ 0.05
Lubricant Type Water Water Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 25 4.5 20 4.5 20 4.5 10 2.2
Time
Minutes
Material: Composites: Glass ber reinforced plastic
Comments of Material: See Material/Preparation Tables 16. No contemporary
method is developed for this kind of material, instead, Method C-17 describes a
method using SiC grinding paper. See also the Material/Preparation Tables 64 and
65 covering polymers.
Case or coating
thickness/hardness,
surface layers
C-17, T-17
of inclusion
content
E 45, E 562, E 768,
E 1245, E 1382
C-17, T-17
High planeness
Microhardness, hardness B 578, C 730, C849, C 1326,
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384,
E 448
C-17, T-17
Microstructure E 3, E 45, E 407, E 562, E 768,
E 883, E 1245
C-17, T-17
Porosity C-17, T-17
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC, bakelite bond or diamond, metal bond
or bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
68 h
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
Cloth,
napless,
hard, wov,
syn
Cloth,
napless,
medium
hard,
wov, wool
Cloth,
napless,
soft,
porous,
syn
orsusp
Dia, spr
orsusp
Silica
Grit/Grain
Size m
P220 P1200 3 1 0.04/ 0.05
Lubricant
Type
Water Water Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 30 7 20 4.5 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 35 3 1
Section 13.2.2.
Grinding/ PG FG 1 FG 2 P 1 P 2 P 3 P 4
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
P220 P320 P500 9 3 1 0.04/ 0.05
Lubricant
Type
Water Water Water Alco or
wat
Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 25 4.5 25 4.5 20 4.5 20 4.5 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 4 4 4 23
Material: Composites. Other composite materials
Case or coating
thickness/hardness,
surface layers
C-18
Grain size, grain
boundaries
E 112, E 930, E 1181 C-18, T-18
of inclusion
content
E 45, E 562, E 768,
E 1245, E 1382
C-18
High planeness
Microhardness, hardness B 578, C 730, C 849, C 1326,
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384,
E 448
C-18, T-18
E 883, E 1245
C-18, T-18
Porosity C-18
Sectioning
Cut-Off Wheel Al
2
O
3
or SiC, bakelite bond or diamond, metal bond
or bakelite bond
Mounting
Hot Compression
Mounting
with Filler
Time
Minutes
810 Time
Minutes/
Hours
68 h
Grinding
T-18: At composites with ceramics, SiC grinding paper may not be used; use
diamond for grinding see Method T-16 or use Method C-18.
Polishing
C/T-18: Polishing step with silica: Depending on the matrix of the material,
alumina is used instead of silica. See under the actual material. Also the silica
step can be changed to P 2 from Method T-12.
T-18: P 2: Can be changed to step P 2 from Method T-12 as nal step.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 P 1 P 2
xed, res
RCD,
soft
Cloth,
napless, hard,
wov, syn
Cloth,
napless,
soft, porous,
syn
susp
Dia, spr or
susp
Silica
Grit/Grain Size m P220 9 3 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra
Comp or
contra
Comp Comp Contra
Force per Specimen N lb 30 7 40 9 40 9 10 2.2
Time
Minutes
Until plane 46 35 1
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 3 1 0.04/ 0.05
Lubricant
Type
or
wat
Alco
or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra
Comp
or
contra
Force per
Specimen
N lb
30 7 25 5.5 25 5.5 25 5.5 20
4.5
20
4.5
10
2.3
Time
Minutes
Until
plane
0.51 0.51 0.51 45 3 0.51
Material: Ceramic capacitors. Ceramic resistors. Diodes
Comments on Material: In ceramic capacitors, ceramic resistors, and diodes we
have the hard, brittle ceramic or glass phases combined with softer materials like
silicon and metals. Delamination, voidage, and cracks are typical processing
defects which can be assessed by materialography/metallography. Also
materialography/metallography can be used for dimension analysis.
The monolithic ceramic capacitor consists of ceramic plates, often barium
titanate, coated with layers of a silver-palladium alloy and with terminations in
silver. The barium titanate being very brittle and sensitive to mechanical stress
must be prepared very carefully with Method T-19 below; only the two grinding
steps PG and FG 1 should be omitted so that the preparation starts with grit P500
grinding paper.
Ceramic resistors are normally made with a less brittle and harder ceramic
alumina and Method C-19 can be recommended.
Glass and silicon of the diodes are very brittle materials and very careful
preparation is necessary. Method T-19 is considered the most suitable.
A number of artifacts can be developed during the preparation, like pull-outs,
cracks, delaminations, and relief see Section 13.5. The correct mounting
encapsulation is important; uncorrect mounting may create voids and gaps
between mounting material and the single constituents, leaving the constituent
unsupported causing rounding and possibly cracking.
Methods C-19 and T-19 may also be used for preparation of other electronic/
microelectronic devices like integrated circuits see also Material/Preparation
Tables 26.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel as thin
as possible. This should preferably take place on a precision cut-off machine, both
to obtain the smallest possible stress to the specimen and to be able to cut
reasonably precise in the correct distance from the site target to be investigated.
This distance should be so that neither the damages from the cutting and from the
rough grinding steps will inuence the surface at the site of interest target.
In case the part capacitor is relatively small, the part can be encapsulated
mounted see below and a sectioning is not necessary; the inspection plane
target can be reached by grinding.
Mounting: The lowest possible heating of the specimen should take place during
mounting, so hot mounting should be avoided. Cold mounting in epoxy is
recommended because of the low viscosity, the low peak temperature, and the
possibility of vacuum impregnation see Section 3.10.
Grinding: It is important that the very brittle materials are not damaged too much
by the rough grinding papers and often, as mentioned above, the grinding should
start with the grits P320 or P500. If a relief between areas with a high difference
in hardness should be avoided, Method C-19 should be used if possible.
Polishing: Polishing times should be kept as short as possible to avoid relief, but
often long times are needed to remove deformation and other artifacts developed
during the grinding. Often a water-oil based lubricant should be used for the nal
diamond steps.
Etching: Normally no chemical etching takes place, but physical etching, like
relief polishing can be used see Section 9.6.
surface layers
C-19
Grain size, grain boundaries E 112, E 1382 C-19, T-19
content
High planeness
E 562, E 1245, E 1382 C-19, T-19
Microhardness, hardness E 92, E 384 C-19, T-19
1245, E 1382
C-19, T-19
Porosity C-19, T-19
Sectioning
Cut-Off wheel Diamond, metal bond, 0.5 mm 0.019 in thickness
Mounting
Hot Compression Mounting Resin Cold Mounting Resin Epoxy
Time
Minutes
Time
Minutes/Hours
1224 h
Grinding
C-19 and T-19: For very sensitive materials it is recommended not to use the PG
step with grit P220 grinding paper, but start with grit P320 or P500.
Diodes: C-19: It is recommended to use SiC paper grit P220 for PG and grit
P500 for FG 1 so that FG 1 RCD, soft is changed to
FG 2.
Polishing
C-19: P 2: At materials with less tendency for relief, the cloth can be changed to
med nap, soft, syn.
Diodes: C-19: The cloth for the step P 1 is changed to napless, hard, wov, syn,
and the cloth for P 2 is changed to med nap, soft, syn.
C-19: In case of sensitive materials like constituents of soft metals diodes, the
lubricant for 3 m and 1 m diamond-polishing steps should be water-oil based.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 P 1 P 2 P 3
res
RCD,
soft
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft,
porous,
syn
Abrasive Type Diamond Dia,
spr or
susp
Dia,
spr or
susp
Dia,
spr or
susp
Silica
Grit/Grain
Size m
P220 9 3 1 0.04/ 0.05
Lubricant Type Water Alco or
wat
Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra
Comp or
contra
Force per
Specimen
N lb
30 7 30 7 20 4.5 20 4.5 10 2.2
Time
Minutes
Until plane 46 12 12 0.51
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 P 1 P 2 P 3 P 4
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
soft,
porous
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
size m
P220 P320 P500 P1200 9 6 1 0.04/ 0.05
Lubricant
Type
or wat
Wat-oil Wat-oil
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp Comp Comp Comp Comp Comp Comp Contra
Force
per
Specimen
N lb
15 3.4 20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 1015 510 2 0.51
Material: YBCO ceramic super conductors
Comments on Material: A superconductor is an element, intermetallic, or
compound that will conduct electricity without resistance below a certain
temperature, Tc. However, this applies only to direct current dc electricity and to
nite amounts of current. All known superconductors are solids, and all require
extreme cold to enter a superconductive state. Once set in motion, current will
ow forever in a closed loop of superconducting materialmaking it the closest
thing to perpetual motion in nature. Tc is the critical transition temperature below
which a material begins to superconduct, and research is going on to nd the
material with the highest Tc. Superconductors are categorized in Type 1 and Type
2. Type 1 category is mainly comprised of metals and metalloids that require
extremely low temperatures, Tc, up to a few K, to become superconductive. The
Type 2 category is comprised of metallic compounds and alloys, of which the
perovskites, metal-oxide ceramics like the so-called YBCO compounds composed
of yttrium, barium, copper, and oxygen, are important because they have a Tc
higher than 90 K.
In general, YBCO materials are very brittle and porous, so pull-outs and
microcracks can be introduced during the sectioning and grinding stages. The
Method T-20 is developed for YBa
2
Cu
3
O
7
+, and in case of materials too hard for
SiC grinding paper, or an extremely plane specimen is wanted, Method C-20 can
be used.
Sectioning: Sectioning should take place with utmost care because of the brittle
and porous material. Wet abrasive cutting can be done with a thin diamond cut-off
wheel, metal bond, or, if damage should be reduced, with bakelite bond on a
precision cut-off machine. The cut-off wheel should be as thin as possible and for
some softer materials, a thin SiC bakelite bond wheel, 0.5 mm 0.02 in can be
used. The feed rate should be low and the wheel speed in the range of 1000 rpm.
If the porosity is high, it can be recommended to vacuum impregnate the
specimen before cutting see below. The clamping of the specimen during cutting
should be so that pressure spots are avoided, as these can cause fractures in the
material. Very sensitive materials can be glued to a piece of nonmetallic base
material which is then clamped in the machine.
When water is used for cutting, place the cut specimen in alcohol for one hour if
the material is water sensitive.
Mounting: If the porosity is above 5 % it is advisable to vacuum impregnate the
sectioned specimen with epoxy possibly using a dye see Section 3.10. The
material should not be hot mounted, but mounting after impregnation should be
with a slow curing epoxy. To balance the hardness of the epoxy a ller can be
added see Section 3.11.2.
Grinding: As grinding with rough grinding papers causes pull-outs and
microcracks, the PG step with grit P220 grinding paper may be changed to grit
P320 if the surface after cutting seems relatively little damaged. Water should be
avoided for water sensitive materials see below.
Polishing: To remove pull-outs and microcracks polishing may be carried out at
low pressure over relatively long times see methods below.
Etching: No etchants are stated below, but contrast can be developed as indicated.
Case or coating
thickness/hardness,
surface layers
C-20
High planeness
E 562, E 1245, E 1268, E 1382 C-20
Microhardness, hardness E 384 C-20, T-20
E 1268, E 1382
C-20, T-20
Porosity C-20, T-20
Sectioning
Cut-Off Wheel Diamond, metal bond bakelite bond, or SiC bakelite
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Epoxy with ller
Time
Minutes
Time
Minutes/Hours
1224 h
Grinding
C-20: FG 1 and FG 2: If material is highly sensitive to water use a water-free
diamond suspension.
T-20: If the material is not water sensitive, water should be used as a cooling
uid for the steps PG and FG 1 to FG 4.
Polishing
C-20: P 1: If the material is water sensitive, use P 1 and P 2 from T-20.
T-21: If material is water sensitive, use water-free diamond suspension or spray
for P 1 and P 2 as indicated.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 P 1
Polishing
Disk/Cloth SiC paper RCD, soft RCD, soft Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC Dia, spr
or susp
Dia, spr
or susp
Silica
Grit or Grain Size m P220 9 3 0.04/ 0.05
Lubricant Type Water/dry Alco, water-free Alco, water-free
rpm/rpm
Comp/Contra Comp Comp Comp Contra
Force per Specimen N lb 15 3.4 25 5.7 25 5.7 20 4.5
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, silk
Abrasive Type SiC SiC SiC SiC SiC Dia, spr
or susp
Dia, spr
or susp
Grit and
Grain Size
m
P220 P500 P1200 P2400 P4000 1 0.25
Lubricant Type Dry Dry Dry Dry Dry Alco,
water
free
Alco,
water-
free
Rotation
Disk/Holder
rpm/rpm
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Comp/Contra Comp Comp Comp Comp Comp Comp Comp
Force per
Specimen
N lb
15 3.4 15 3.4 15 3.4 15 3.4 15 3.4 1015
2.3.4
1015
2.33.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 420 515
Etchant
YiBa
2
Ca
3
O
7+
Contrast can be made by:
a vapor depositing of interference layer e.g., iron oxide
b Observation of the polished specimen in polarized light
Material: Germanium. Silicon. Si wafers. Other semiconductors
Material Properties: Germanium: Face-centered cubic, 5.3 g/ cm
3
, 937.4C
1719F.
Silicon: Face-centered cubic, 2.42 g/ cm
3
, 1420C 2588F.
Comments on Material: Germanium and silicon are metalloids and belong to the
group of materials, semiconductors. Silicon is the most commonly used material
and is often prepared as a chip see Material/Preparation Tables 22 and 26 or as a
wafer/solid piece, which is discussed here. It is, however, only the preparation for
metallographic/materialographic examination, the polishing thinning, which is
part of the production process, is outside the scope of this book. The
semiconductors are brittle materials that fracture easily, and especially as thin
wafers, the specimens should be handled with great care.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel,
0.5 mm 0.02 in thick or thinner. The cutting should be done on a precision
cut-off machine to obtain the most controlled cutting with a low feed speed. The
clamping should not be directly on the specimen, but with elastic material as
spacers. Often it can be of advantage to encapsulate the specimen before cutting.
Sectioning for production of wafers is outside the scope of this book.
Mounting: For preparation of the at side of a wafer, the wafer or a piece of the
wafer is temporarily glued with wax to a support disk which can be placed in the
specimen holder. In the case of a cross section of the wafer, the specimen is cold
mounted and placed in the mounting mold supported by clips to hold it in an
upright position see Section 3.9. Due to the brittle nature of the semiconductors
these should not be hot mounted, but cold mounted, preferably with epoxy.
Grinding: The rough grits of SiC grinding papers will damage silicon and other
semiconductors rather strongly, and therefore the grits P220 and P320 should only
be used if relatively much material should be removed. If the cut surface is of a
good quality, the plane grinding should be done with a grit P500 grinding paper if
possible. To avoid SiC grinding paper for ne grinding, use Method C-21. As an
alternative to SiC grinding papers, Al
2
O
3
/diamond lapping lms can be used see
Section 6.7.6 and Material/Preparation Tables 22.
Polishing: Polishing times should be as short as possible to avoid edge rounding.
The semiconductor materials respond very well to chemical mechanical polishing
with colloidal silica, but also here the time should be as short as possible.
Etching: See Etchants below.
surface layers
C-21
Grain size,
grain boundaries
E 112, E 930, E 1382 C-21, T-21
High planeness
E 562, E 1245, E 1382 C-21
E 1382
C-21, T-21
Porosity C-21, T-21
Sectioning
Cut-Off Wheel Diamond, metal bond, 0.5 mm 0.02 in or thinner
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
1224 h
Grinding
C-21 and T-21: Plane grinding with grit P220 or P320, or both, should be
avoided if possible.
C-21: PG: Grit P500 SiC paper can be used.
Polishing
C-21 and T-21: Polishing times should be kept as short as possible.
C-21 and T-21: P 1: This step can be changed to step P 2 in Method T-21.
Section 13.2.2.
Polishing
xed, res
RCD, soft RCD, soft Cloth,
napless,
hard, wov,
syn
Cloth, nap-
less, soft,
porous, syn
Abrasive
Type
Diamond Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or
Grain Size
m
P500 9 3 3 0.04/ 0.05
Lubricant
Type
Rotation
Disk/
Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Force per
Specimen
N lb
15 3.4 20 4.5 20 4.5 20 4.5 10 2.3
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous
or susp
Dia, spr
or susp
Silica
Grit or Grain
Size m
P500 P1000 P2400 P4000 3 1 0.04/ 0.05
Lubricant Type Water Water Water Water Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/150 300/150 300/150 300/150 150/150 150/150 150/150
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp Comp Contra
Force per
Specimen
N lb
1525
3.45.7
20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 1015
2.23.4
Time
Minutes
Until
plane
1.52 1.52 1.52 4 3 13
Etchants
Material Etchants see Table
12.2
Uses
Si, Si alloys 931 General structure
Si, Si alloys 932 General structure
Si 933 General structure
Si 934 To reveal SiO
2
Material: Microelectronic material semiconductor device
Preparation of cross section of a semiconductor device using a tripod xture for
hand preparation on a grinder/polisher with a 200 mm 8 in polishing disk and
variable speed 0150 r/ min.
Comments on Material: Nonencapsulated cross sections through microelectronic
material semiconductor devices serve two main functions. Cuts through
representative structures within an IC show relationships of layers and features,
such as step coverage, interfaces between layers, and possibly embedded defects or
voids. Precision cross sections through specic defects often lead to the process
step or mechanism which produced the defect see Section 7.10.2.
The preparation of a nonencapsulated cross section of microelectronic material is
described below. The method is considered a C-Method, using a combination of
SiC grinding papers and Al
2
O
3
/diamond lapping lms see Section 6.7.6, and no
T-Method is stated.
Sectioning: The specimen should be a piece of silicon roughly 5 mm 0.20 in
square. The desired cross section target should be within 50 m from the edge.
The specimen can be cut out with a thin diamond cut-off wheel on a precision
cut-off machine medium speed or cleaved. Determine the desired cross section line
target. If suitable landmarks do not exist, create visible marks with a laser or
mechanical probe.
Mounting: Heat up a sample mount to approximately 125C 250F. Apply a dot
of wax and mount the specimen in cantilever fashion on the sample mount. The
target cross section line must extend beyond the end of the sample mount see
Section 7.10.2. Place the sample mount with specimen in the tripod xture.
Grinding: The purpose of grinding is to rapidly achieve a surface 1 m away from
and parallel to the desired cross section line. If more than 40 m of material
should be removed to reach the nal cross section line, begin grinding with SiC
paper grit P1200 see step PG below. If the distance to line is 20 m or less, start
with step FG 1 below.
FG 3 and FG 4 uses Al
2
O
3
and diamond lapping lm plane back, placed with
water as a glue on a plane, smooth surface glass/metal plate on the polishing
disk.
Diamond lapping lm can be used as an alternative to SiC paper, and Al
2
O
3
lapping lm in the steps PG and FG 1, 2, 3, and 4; this is stated in the Method
Table below. Step FG 5 shall always be with diamond lapping lm. Attention:
Always let the grinding/polishing disk rotate into the edge containing the target,
except at the last polishing step reverse position.
Polishing: The completed cross section should be exactly centered on the contact,
via, or other feature in the target. Polishing will only remove very little material
2 m or less and cannot remove deep scratches or damage created by grinding
too close to the desired nish with coarse abrasives. Polishing is most important
when the cross section is to be viewed in a high-resolution eld emission SEM.
Type of polishing depends on the composition of the specimen: Si, SiO
2
, and Al
with/without thin barrier layers: Repeat step FG 4 after step FG 5, only with
0.05 m Al
2
O
3
lapping lm in 0.5 min or longer until the diamond scratches are
removed. Finish with 0.5 min holding the xture in reverse position see Section
7.10.2.
Si, SiO
2
, and metallization including tungsten plugs or layers: Use step P 1 below,
holding the xture in reverse position see Section 7.10.2.
Etching: Normally no etching is used.
Sectioning
Cut-Off Wheel Diamond wheel metal bond 0.5 mm 0.019 in
thickness or by cleaving
Mounting
Hot Compression
Mounting
Resin See above Cold Mounting Resin See above
Time
Minutes
Time
Minutes/Hours
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 FG 4 FG 5 P 1
Polishing
Disk/Cloth SiC
paper
or
diamond
lapping
lm
SiC
paper
or
diamond
lapping
lm
SiC
paper
or
diamond
lapping
lm
Al
2
O
3
or
diamond
lapping
lm
Al
2
O
3
or
diamond
lapping
lm
Diamond
lapping
lm
Cloth,
napless,
hard,
wov, syn
Abrasive
Type
SiC or
diamond
SiC or
diamond
SiC or
diamond
Al-
oxide
Al-oxide Diamond Dia, susp
Grit/Grain
Size m
P1200
or 15
P2400 or
8
P4000 or
3
1 0.3 0.1 0.1
Lubricant
Type
Water Water Water Water Water Water Alco
Rotation
Disk/
Holder
60/ 100 60/ 100 60/ 100 60/ 100 30 30 70/ 100
rpm/
rpm
Comp/
Contra
Force per
Specimen
N lb
Weight
of
xture
Weight
of
xture
Weight
of
xture
Weight
of
xture
Weight
of
xture
Weight
of xture
Weight
of xture
Time
Minutes
Until
within
22 m
from
target
line
Until
within
12
m
from
target
line
Until
within 7
m
from
target
line
Until
within 3
m
from
target
line
Until
within 2
m
from
target
line
Until
within 1-
1.5 m
from
target
line
0.51,
until
target
Material: Resistors. Other electronic metal components
Comments on Material: Metal lm resistors and other metal-based electronic
components often consist of several very different types of material that range
from a very soft metal to a very hard ceramic. The methods stated below should
be considered as supplement to the methods stated in Material/Preparation Tables
19 and 26.
Sectioning: See Material/Preparation Tables 19 and 26.
Mounting: See Material/Preparation Tables 19 and 26.
Grinding: See Material/Preparation Tables 19 and 26.
Polishing: See Material/Preparation Tables 19 and 26.
surface layers
C-23
content
E 562, E 1382 C-23, T-23
High planeness
E 1245, E 1382
C-23, T-23
Porosity C-23, T-23
Sectioning
Cut-Off Wheel Diamond wheel metal bond or SiC bakelite bond,
0.5 mm 0.019 in thickness.
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Acrylics with a
Filler/Epoxy
Time
Minutes
Time
Minutes/Hours
615 min/ 1224 h
Grinding
C-23: In the case of a high amount of ceramics in the specimen, PG may be
changed to a diamond pad, 30 m, bakelite bond. See also Methods C/T-19.
Polishing
T-23: The step P 1 can be followed by a step like P 1 in Method C-23.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper RCD, soft RCD, soft Cloth, nap-
less, soft,
porous, syn
or susp
Dia, spr
or susp
Silica
Grit or Grain Size m 320 9 3 0.04/ 0.05
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Contra
Force per Specimen N lb 35 8 35 8 35 8 20 4.5
Time
Minutes
Until
plane
34 3 0.51
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper Cloth,
napless,
hard,
wov, syn
Abrasive Type SiC SiC SiC SiC Dia,
spr or
susp
Grit or Grain
Size m
P220 P320 P500 P1200 3
Lubricant Type Water Water Water Water Alco
or wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
Contra
Comp or
Contra
Comp or
Contra
Comp Comp
Force per
Specimen N lb
30 7 30 7 30 7 30 7 30 7
Time
Minutes
Until plane 0.51 0.51 0.51 3
Material: Solder balls. Microelectronic packages
Comments on Material: The tin-lead solders used for solder balls often have to be
prepared together with other components like printed circuit boards PCBs,
ceramics, plastics, etc. see Section 7.10.3. This means that the ideal preparation
of the soft solder is not possible if the other components also should be prepared
in an acceptable way. For soft solders the main problem is embedding of abrasive
grains and particles from the preparation process see below and Section 13.5/6.
In case of soldered joints, cracks may develop after the preparation due to stress,
and for this reason the specimen should be examined and documented
immediately after preparation. For preparation of PCBs see Material/Preparation
Tables 27. For microelectronic packages see also Material/Preparation Tables 19
and 26.
Sectioning: Sectioning often involves cutting through components of very
different hardness. Wet abrasive cutting should be done with a diamond metal
bond cut-off wheel if the sectioning involves ceramics, and a SiC bakelite wheel if
cutting involves only softer materials see also Material/Preparation Tables 26.
Cutting should be done on a precision cut-off machine to secure a precise cut and
make the use of a thin wheel, 0.5 mm 0.02 in or thinner, possible. In case of
component-mounted boards, take care that all specimens are properly identied
before they are sectioned from the PCB. The cut should be in a certain distance
from the level of investigation so that damage from the cutting can be removed at
grinding and polishing.
Often the section to be investigated should be encapsulated mounted in epoxy
prior to cutting to ensure the integrity of delicate joints/components.
Mounting: The specimen should be carefully cleaned in acetone and preferably
ultrasonics before mounting. Hot mounting cannot be recommended. Cold
mounting with epoxy and vacuum impregnation is recommended so that all voids
are lled with epoxy see Section 3.10.
Grinding: For specimens containing ceramics the Method C-24 should be used
with Method C-19 as an alternative.
Polishing: In case of embedded abrasive grains, the use of diamond paste can be
tried out for the 3 and 1 m steps; also the use of only small amounts of lubricant
may prevent embedding of particles.
Etching: Normally no etching is made, but in case of etching, see Material/
Case or coating
thickness/hardness,
surface layers
C-24
Grain size, grain boundaries C-24, T-24
C-24, T-24
High planeness
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond, thinnest
possible
Mounting
Time
Minutes
Time
Minutes/Hours
1224 h
Grinding
C-24: FG 1 and T-24: FG 3: Grind until solder balls are visible, being close to
target.
Polishing
C-24, T-24: In case of embedded diamonds, diamond paste may be used instead
of spray/suspension for the 3 m and 1 m steps.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, nap-
less, medium
hard,
wov, wool
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
220 320 9 3 0.04/ 0.05
Lubricant Type Water Water Alco or wat Wat-oil
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp Comp Contra
Force per Specimen
N lb
20 4.5 15 3.4 20 4.5 20 4.5 15 3.4
Time
Minutes
Until plane To target 2 12 1
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
nonwov,
syn
Cloth,
napless,
hard,
wov, silk
Cloth,
nap-
less, soft
porous,
syn
Abrasive
Type
SiC SiC SiC SiC Dia, spr
or susp
Dia, spr
or susp
Silica
Grit or Grain
Size m
P220 P320 P500 P1200 3 1 0.04/ 0.05
Lubricant
Type
Water Water Water Water Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 20 4.5 20 4.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 4 2 0.51
Material: Capacitors. Other polymer electronic components
Comments on Material: Film capacitors often incorporate two layers of dielectric
lm that have each been metallized on one side; these strips are stacked and
rolled. The assembly may be packaged in a polymeric conformal coating or in a
molded polymeric housing.
Grinding: If the specimen contains phases of very different hardness, Method C-25
should be preferred.
Polishing: Polishing times should be kept as short as possible to avoid relief.
Etching: Normally no etching is done.
surface layers
C-25
Grain size, grain boundaries E 112, E 1382 C-25,
T-25
content
E 562, E 1245, E 1382 C-25,
T-25
High planeness
Microhardness, hardness E 92, E 384 C-25,
T-25
E 1245, E 1382
C-25,
T-25
T-25
Porosity C-25,
T-25
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond, 0.5 mm
0.02 in thick
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
610 min/ 812 h
Grinding
C-25: PG step: In the case of little or no ceramic material, SiC paper can be
used.
Section 13.2.2.
Polishing
res
RCD, soft Cloth, nap-
less, hard,
wov, silk
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or
Grain Size m
P220 9 6 1 0.04/ 0.05
Lubricant
Type
Water Alco or wat Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per
Specimen N lb
25 5.7 25 5.7 20 4.5 20 4.5 15 3.4
Time
Minutes
Until plane 5 12 0.51 0.5
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
v. hard,
wov, syn
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft
porous,
syn
or susp
Dia, spr
or susp
Silica
Grit or Grain
Size m
P320 P500 P800 P1200 6 3 0.04/ 0.05
Lubricant
Type
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 30 7 20 4.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 3 2 0.51
Material/Preparation Table 26
Material: Microelectronic packages. Integrated circuits.
Transistors. Other microelectronic devices
Comments on Material: As an introduction to preparation of microelectronic
packages Section 7.10.3 should be studied to get an impression of the problems
involved.
Electronic and microelectronic devices and packages are complex material
composites. Imaging and analysis of the various material microstructures, layered
structures, and interfaces are necessary for a number of reasons, including
package qualication, monitoring of the manufacturing process, incoming quality
control, and failure analysis. The dimensions of the individual features range from
fractions of a micron to several cm fraction of an in. Due to the close packing of
the various materials within a small volume, all materials having very different
properties; materialographic preparation faces the problem of making all the
materials suited for proper analysis. It is essential to have a general understanding
of the physical properties of all materials used in the construction of the package
see Table 7.1. As a rule the preparation is tailored to the predominant component
material to be analyzed, but often all materials must be considered to obtain a
satisfactory result. Ignoring the unique interfaces that are present in a
microelectronic package will likely result in artifacts induced during the
preparation process. Such artifacts may be edge rounding, relief, embedding of
abrasive grains, smearing and fracturing, and introduction of microcracks. Several
of these artifacts could be misinterpreted as defects in the package developed
during the production or in other ways.
Making a cross section of a microelectronic package is a destructive test; it is
important that as much information as possible about the device is gathered
before the preparation starts. Such information is important to decide on the
target of the preparation and may be important to be able to decide whether a
defect was pre-existing or induced during the preparation. Also, this information is
important in case of failure analysis. The information can be obtained through a
number of analysis techniques like radiography, ultrasonic imaging, and
macrophotography. Based on the available information, the
preparation process is decided upon as either one of the two methods indicated
below or other methods stated in Material/Preparation Tables 19, 22, 23, and 25,
with the Methods C-19 and T-19 as the rst choice.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel,
0.5 to 1 mm 0.02 to 0.04 in thick on a precision cut-off machine with
1500 to 2000 rpm. Often an electroplated diamond wheel can be used with
advantage, and in the case of very hard components a diamond wheel with
bakelite bond should be used. In certain cases depending on the materials, SiC
bakelite bond cut-off wheel can be used.
Cutting before encapsulation: In some cases the package should be opened to be
able to make the encapsulation mounting. This can be done with wet abrasive
cutting as mentioned or with grinding away the material or by other means. It is
important that this process takes place at a safe distance to the site to be
investigated.
Cutting after encapsulation: Wet abrasive cutting as stated above is recommended.
It is important that the specimen is oriented, with respect to wheel rotation, such
that the brittle material in the specimen, like silicon, is cut in compression. Doing
this will minimize delamination or fracturing, or both, of the brittle component
material. Also the specimen should be positioned so that the wheel cuts into the
smallest dimension of the critical parts in the package. To shorten the following
preparation process, the cutting should be done in a plane relatively close to the
site of investigation with this under the condition that the damage caused by the
cutting is under control.
Mounting: Microelectronic packages cannot be subjected to pressure and heat, so
only cold mounting, most often as an encapsulation in epoxy under vacuum, is
recommended.
Encapsulation: It is very important that the package is carefully cleaned to secure
a complete adhesion by the epoxy during the encapsulation. This can be done in
acetone, preferably in a beaker in an ultrasonic bath. Drying should be done with
N
2
gas or absolutely pure compressed air; normal compressed air should
be avoided. The cleaned part should be handled with a pair of tweezers and dried
in an oven at 50C 122F. The package is placed in the mounting mold so that
the plane of interest will ultimately be parallel to the cutting wheel. If needed, the
specimen is supported with clips or by other means. It is important that the
mounting material adheres to all constituents and that all topographical features
of the package is lled with mounting material. This can best be provided with an
epoxy with a low viscosity and impregnation under vacuum see Section 3.10.
Also a pressure vessel can be used for securing a good encapsulation see Section
3.7.
Grinding: Considering the often very brittle materials in the specimen, plane
grinding with rough SiC grinding papers should be avoided. In the methods stated
below plane grinding is with grit P320 grinding paper, but this paper should only
be used if the plane grinding is in a plane relatively far from the site of interest
target. If possible, depending on the surface established by the sectioning, the
plane grinding should be done with an RCD stated in Method C-26, step FG 2,
below. In case of packages with many soft, ductile materials, Method T-26 below
may have the best grinding steps.
Polishing: It is very important that the deformation and other damage developed
during the grinding is removed during the rough polishing step. Often step P 2 in
Method T-26 can be omitted. For packages containing predominantly soft
materials plastics, it can be of advantage to use a mixture of 50 % colloidal silica
and 50 % deagglomerated alumina 0.05 m for the nal polishing step.
Etching: Normally no chemical etching takes place, but physical etching, like
relief polishing and methods like deposition of layers can be used see Section 9.6.
surface layers
C-26
content
E 562, E 1245, E 1382 C-26, T-26
High planeness
E 1245, E 1382
C-26, T-26
Porosity C-26, T-26
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond,
0 to 1 mm 0.02 to 0.04 in thick, see also above.
Mounting
Time
Minutes
Time
Minutes/Hours
1224 h
Grinding
C-26, T-26: Only use rough grits of SiC grinding paper, when not close to target.
Polishing
C-26: P 2: Often the cloth can be changed to a med nap, soft, syn, if the
difference in hardness of the components materials is not high.
C-26 and T-26: For predominantly soft materials use a mixture of 50 % colloidal
silica and 50 % deagglomerated alumina 0.05 m for the nal polishing step.
C-26 and T-26: For the steps with 6, 3, and 1 m diamond, colloidal silica can
be used as lubricant.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, nap-
less, hard,
wov, syn
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
220 320 9 3 1 0.04/ 0.05
Lubricant
Type
Water Water Alco or
wat
Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Force per
Specimen
N lb
25 5.7 25 5.7 20 4.5 20 4.5 20 4.5 1015
2.23.4
Time
Minutes
Until
plane
0.51 215
Close to
target
15 14 0.51
Section 13.2.2.
Grinding/ FG 3 P 1 P 2 P 3 P 4
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
hard,
wov,
syn
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
soft,
por-
ous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P320 P500 P800 P1200 6 3 1 0.04/
0.05
Lubricant
Type
Water Water Water Water Wat-oil Wat-oil Wat-oil
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 20 4.5 20 4.5 20 4.5 1015
2.2
3.4
Time
Minutes
Until
plane
0.51 0.51 0.5 1
Close
to
target
515 12 14 0.51
Material: PCB coupon
Comments on Material: For a description of PCB coupons with reference holes
and their preparation, see Section 7.10.1.
A contemporary method is not developed for this type of preparation; therefore,
Method C-27 is a traditional method using SiC grinding paper.
Sectioning: The coupon is normally cut out with a router or punched out. A
precision cut-off machine with a diamond cut-off wheel, metal bond, can also be
used.
Mounting: Two to six coupons are mounted with a cold mounting material like
acrylics in a special mounting mold to be placed in a special holder, with reference
pins, to obtain a controlled material removal.
Grinding: Grinding is done in two steps against adjustable stops mounted on the
specimen holder to stop material removal before the center of the holes to be
inspected.
Polishing: The polishing steps P 3 and even P 2 in Methods C-27 and T-27 may be
omitted according to the type of PCB and the purpose of examination.
Etching: If an etching is wanted this can be done in the polishing step P 3: Use
96 mL colloidal silica, 2 mL H
2
O
2
30 % and 2 mL ammonia solution 25 %.
Sectioning
Cut-Off Wheel Diamond, metal bond, if not routed or punched, see
above.
Mounting
Hot Compression Mounting Resin Cold Mounting Resin Acrylics
Time
Minutes
Time
Minutes/Hours
810 min
Grinding
C-27, T-27: Grinding is performed against adjustable stops see above.
Polishing
C-27, T-27: Etching can be done through chemical mechanical polishing with
96 mL colloidal silica, 2 mL H
2
O
2
30 % and 2 mL ammonia solution 25 %.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
hard, wov,
wool
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Silica
Grit or Grain Size m P220 P1200 3 1 0.04/ 0.05
Lubricant Type Water Water Water Water
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per Specimen N lb 20 4.5 20 4.5 20 4.5 15 3.4 10 2.2
Time
Minutes
See above See above 2 2 0.5
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 P1200 6 1 0.04/ 0.05
Lubricant Type Water Water Water Water
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N lb
20 4.5 20 4.5 20 4.5 15 3.4 10 2.2
Time
Minutes
See above See above 2 2 0.5
Material: High carbon steels. Medium carbon steels
Material Properties: Alpha iron ferrite: Body-centered cubic, gamma iron
austenite: Face-centered cubic, 7.85 g/ cm
3
, 1528C 2782F, HV 70 ferrite.
Low carbon steel: 0.2 % C, medium carbon steel: 0.20.5 % C, high carbon steel:
0.5 % C weight %.
Comments on Material: The plain carbon steels are characterized by their
composition, having only carbon as the important alloying element. A typical
medium carbon steel SAE-AESI 1042 has the composition: 0.40.47 % carbon,
0.600.90 % manganese, maximum 0.040 % phosphorus, maximum 0.05 % sulfur.
The plain carbon steels and other steels are classied according to their
composition by the American Iron and Steel Institute AISI and the Society of
Automotive Engineers SAE. ASTM also has a classication system built on the
steel product and its application. The ASTM standards are specications for
specic products; a few examples are: A 1, A 3, A 36 see Section 12.4.2. The
microstructure of plain carbon steels is a mixture of ferrite and pearlite, with an
increase in pearlite corresponding to the increase in carbon content. At 0.8 %
carbon, only pearlite is present and above 0.8 % carbon, cementite will develop.
Medium and high carbon steels are relatively easy to prepare. The problem is to
obtain a true ferrite without deformation. At higher carbon contents with small
amounts of ferrite, the preparation can be cut down to three or four steps for
routine examination see below. These materials are well suited for electrolytic
polishing.
Sectioning: The correct selection of the specimen is important, especially on
rolled material see Section 2.1. In wet abrasive cutting an Al
2
O
3
cut-off wheel
should be used. Overheating should be avoided because martensite can be
developed. Cutting pressure should be moderate and cooling should be efcient on
both sides of the cut-off wheel. If shearing or band sawing is used, the increase in
deformation should be taken into consideration, prolonging the plane grinding
step, or possibly use of a rougher grinding paper before grit 220.
Mounting: For routine examination bakelite as powder or tablets is sufcient. In
the case of examination of coatings, other mounting materials should be used see
Material/Preparation Tables 0815. For mounting for electrolytic polishing, see
Section 3.11.6.
Grinding: Grinding normally will give no problems with these materials. Care
should be taken that the deformations from plane grinding are effectively removed
before the polishing. If not, the deformed ferrite can be seen after etching, and the
process must be repeated from FG 1. In the case of water sensitive inclusions,
mineral spirits or kerosene can be used for grinding with SiC grinding paper see
also Material/Preparation Tables 36.
Polishing: The problem can be to obtain a perfect ferrite phase as mentioned
above. In the case of only small deformations, prolong the 3 m step for 12 min.
For medium carbon steels the nal step could be with diamond see below.
A common test on steels is nonmetallic inclusion identication; often SEM and
EDAX analysis is used. As Si may be contained in the indigenous inclusions, silica
SiO
2
should be avoided for the last polishing step. Therefore this step should be
changed to diamond see below.
Electrolytic polishing can be recommended.
Etching: A high number of etchants are available for steels. In most cases a
relative small selection will cover the need in a given laboratory see below.
Electrolytic etching is possible.
Case or coating
thickness/hardness
surface layers
B 487, E 1077 C-28
Grain size, grain boundaries E 112, E 930, E 1181, E 1382 C-28, T-28,
El-01
Heat inuenced zone E 1077 C-28
Heat treatment C-28, T-28,
El-01
High planeness
E 45, E 562, E 768, E 1077,
E 1245, E 1268, E 1382, E 2283
C-28
Inclusions in steel E 45, E 768, E 1245 C-28, T-28
Microhardness, hardness E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-28, T-28
Microstructure A 892, E 3, E 45, E 407, E 562, E
768,
E 883, E 1077,
E 1181, E 1245, E 1268,
E 1351, E 1382, E 1558
C-28, T-28,
El-01
Phase identication C-28, T-28,
El-01
Structure changes forging C-28, T-28,
El-01
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Resin Bakelite Cold Mounting Resin Acrylics
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
T-28: In some cases, at high C content, FG 1 can be omitted.
Polishing
C-28 and T-28: In case of SEM and EDAX analysis of inclusions, the nal
polishing step is changed to diamond 1 m, see step P 2 in Method C-29. Also,
0.25 m diamond can be used as a step after 1 m diamond, using the same
cloth and same data.
C-28: P 1: The cloth can be changed to napless, hard, wov, silk.
C-28: P 2: This step can be changed to diamond 1 m, see P 2 in C-29, and the
silica step will be P 3 or it may be omitted.
T-28: P 3: Often the alumina suspension can be diluted with water 1:1. In some
cases this step can be omitted.
Section 13.2.2.
Polishing
xed, res
RCD, hard Cloth,
napless,
hard, wov,
syn
Cloth,
napless,
soft, porous, syn
or susp
Dia, spr
or susp
Silica
Grit or Grain Size m P220 9 3 0.02/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Contra
Force per
Specimen N lb
30 7 25 5.5 20 4.5 10 2.2
Time
Minutes
Until plane 46 3 14
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
porous,
syn
Abrasive
Type
SiC SiC SiC Dia, spr or
susp
Dia, spr or
susp
Alumina
Grit or
Grain
Size m
P220 P320 P500 6 3 0.02/ 0.05
Lubricant
Type
Water Water Water Alco or wat Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N
lb
40 9 40 9 40 9 30 7 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 3 3 14
Etchants
Fe+C and 76, 74a, 77, 78, 79 General structure
Fe+ 1 C 74a, 77, 31a, 223 Ferrite grain boundaries
+4% additions 80, 81, 82 Prior austenitic grain boundaries in
martensitic and bainitic steels
78, 222a Untempered martensite
31b, 78 Carbides and phosphides matrix
darkened carbides and phosphides
remain bright
83 Cementite attacked rapidly, sustenite
less, ferrite and iron phosphide least
84 Overheating and burning stains
carbides
85 Stains carbides
86 Chemical polish-etch
210, 211 Colors ferrite
213, 214 Colors carbides
216
222b
Color latch martensite in low carbon
high-alloy grades for dual phase steels;
reveals pearlite, darkens martensite
and outlines austenite
Material: Low carbon steels
3
, 1528C 2782F, HV 70 ferrite.
Low carbon steel: 0.2% C, medium carbon steel: 0.20.5 % C, high carbon steel:
0.5%C weight %
Comments on Material: Low carbon steels are relatively easy to prepare. The
problem is to obtain a true ferrite without deformation. This depends on the
carbon content and often, at higher carbon contents, a ne grinding step can be
omitted for routine examination see Material/Process Tables 28.
Case or coating
thickness/hardness
surface layers
B 487, E 1077 C-29
Grain size, grain
boundaries
E 112, E 930, E 1181, E 1382 C-29, T-29,
El-02
Heat inuenced
zone
E 1077 C-29
Heat treatment C-29, T-29,
El-02
High planeness
E 45, E 562, E 768, E 1077,
E 1245, E 1268, E 1382, E 2283
C-29
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-29, T-29
Microstructure A 892, E 3, E 45, E 407, E 768, E 883,
E 1077, E 1181, E 1245,
E 1268, E 1351, E 1382, E 1558
C-29, T-29,
El-02
El-02
Structure changes
forging
C-29, T-29,
El-02
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Resin Bakelite Resin Acrylics
Cold Mounting Time
Minutes
89 Time
Minutes/Hours
810 min
Grinding
C-29: P 2: This step can be changed to SiC paper grit P220/320.
T-29: In some cases, at a relatively high carbon content, FG 1 can be omitted.
Polishing
C-29 and T-29: In case of SEM and EDAX analysis of inclusions, the nal
polishing step is changed to diamond 1 m, see step P 2 in Method C-29 and
step P 3 in T-29. Also 0.25 m diamond can be used as a step after 1 m
diamond, using the same cloth and same data.
C-29: P 2: For certain materials cast iron this step can be omitted or P 3 can be
omitted.
C-29 and T-29: Silica can be used instead of alumina.
T-29: A ne polishing step, P 3, from C-29 can be added.
Section 13.2.2.
Polishing
xed, res
RCD, soft Cloth,
napless,
hard, wov,
syn
Cloth,
med. nap, soft,
syn
Cloth, nap
less, soft,
porous, syn
Abrasive
Type
Diamond Dia,
spr or
susp
Dia, spr
or
susp
Dia, spr
or
susp
Alumina
Grit or Grain
Size m
P220 9 3 1 0.02/ 0.05
Lubricant
Type
Water Alco
or wat
Alco
or wat
Alco
or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N lb
25 5.5 30 6.6 25 5.5 25 5.5 10 2.2
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, syn
Cloth,
med
nap,
soft,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Dia, spr
or susp
Grit or
Grain Size
m
P220 P320 P500 P1200 6 3 1
Lubricant
Type
wat
Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp Comp Comp Comp
Force per
Specimen
N lb
40 9 40 9 40 9 40 9 40 9 35 8 35 8
Time
Minutes
Unit
plane
0.51 0.51 0.51 34 34 1
Etchants
See Material/PreparationTables 28.
Material: Gray cast iron, lamellar. Malleable cast iron
3
, 1528C 2782F, HV 70 ferrite.
Gray cast iron: Carbon 2.54.0 %, silicon: 0.53.5 %, manganese: 0.21.3 %,
phosphorus 0.0021.0 %, sulfur: 0.20.15 % weight %.
Comments on Material: Gray cast iron is by far the most used cast iron. The
microstructure consists of ferrite or pearlite with graphite in akes lamellar, or
both, or in other shapes. The name refers to the color of a fresh fractured surface,
which is grayish because of the graphite. Gray cast iron has a relatively high
silicon content because silicon promotes the formation of graphite during
solididation. The microstructure of lamellar cast iron contains 510 volume % of
graphite, and the lamellar size and distribution are important for the strength of
the cast iron, but in general lamellar cast iron has a relatively low strength
because of the graphite. The type, size, and distribution are standardized in the
ASTM Standard Test Method for Evaluating the Microstructure of Graphite in Iron
Castings A 247. Also, a number of other specications are described in ASTM
standards; some examples covering gray cast iron and malleable cast iron are: A
47, A 48, A 126, A 159, A 197, A 220, A 338, and A 602 see Sections 12.4.2.
Malleable cast iron, also called TG temper graphite iron, is made by heat
treatment of white cast iron. During this treatment, up to 20 h, the carbides of the
white cast iron are changed into graphite which will be separated into irregularly
shaped nodules in a ferritic or ferritic/pearlitic matrix. This condition makes
malleable cast iron comparable to steel regarding strength, but the importance of
this material has been reduced because of the development of nodular cast iron
ductile cast iron see Material/Preparation Tables 31.
As the microstructure strongly inuences the mechanical properties of cast iron,
metallographic/materialographic examination is important. The examination is
supported by standard reference comparison charts or image analysis techniques,
or both, to determine the morphology, size, and distribution of the graphite on an
unetched specimen.
During the metallographic/materialographic preparation, the retention of the free
graphite in a ferrite/pearlite matrix causes a problem. The difference in hardness
between the two phases and the relative brittleness of the graphite may cause
pull-outs of the graphite and development of a relief between the phases. To obtain
a correct result of a running analysis, it is important that the same high number of
graphite lamellars/nodules are satisfactorily present in the structure without
missing parts of the graphite. The pull-outs to a high degree take place during the
rougher steps of the grinding and therefore it is important that the graphite is
re-established during the ne grinding and polishing steps.
SiC paper may cause a pull-out of graphite even at the ne grain sizes. In that case
Method C-30 should be used.
In the case of a matrix containing much ferrite this may cause problems with
deformations see Material/Preparation Tables 28. For certain cast irons,
electrolytic polishing can be used.
Method C-29 and T-29 can also be used for cast iron.
Sectioning: These materials are normally sectioned with wet abrasive cutting
without problems using an Al
2
O
3
, bakelite bond cut-off wheel. If band sawing is
used, the increase in deformation should be taken into consideration, prolonging
the plane grinding step, or possibly use of a rougher grinding paper before grit
220. Standards test bars are to be preferred, reducing the amount of sectioning,
only it should be considered, whether the microstructures of the test bar truly
represent the structure of the casting.
Mounting: Normally a mounting is not needed except for establishing a suitable
shape for automatic preparation. Often the preparation and examination shall take
place as part of a production process and the time for preparation is very short. In
that case the shape of the test bar coming from the production should be so that it
ts into a specimen holder or specimen holder plate without mounting.
If graphite close to the edge shall be examined, mounting in a suitable mounting
material with a hardness corresponding to the cast iron is recommended.
Grinding: In Method T-30 the high number of grinding papers is due to the
development of the correct graphite at the nest papers. In case of problems with
retaining of graphite, the steps FG 3 and FG 4 may be used without water. Often
the number of steps can be reduced see also Method T-31. Always use fresh
paper, as worn down paper may create pull-out of the graphite.
Polishing: In case of routine examination without image analysis, polishing may
stop after the P 1 step for Method C-30 and after the P 2 step in Method T-30.
Electrolytic polishing cannot be recommended, but it may be used for routine
examination of certain materials.
Case or coating
thickness/hardness,
surface layers
C-30
Graphite in cast iron A 247 C-30, T-30
El-03
Heat treatment C-30, T-30
of inclusion
content
E 562, E 1077, E 1245, E 1382 C-30
High planeness
E 140, E 384, E 448
C-30
Microstructure A 247, E 3, E 407, E 562, E 883,
E 1245, E 1351, E 1382, E 1558
C-30, T-30,
El-03
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/
Hours
810 min
Grinding
Polishing
C-30: A P 3 step from T-30 can be added.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper RCD, soft Cloth,
napless,
hard, wov, syn
Cloth, short
nap,
soft, syn
Abrasive Type SiC Dia, spr or susp Dia, spr or
susp
Dia, spr or susp
Grit or Grain
Size m
P220 9 3 1
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per
Specimen N lb
30 7 30 7 30 7 25 5.7
Time
Minutes
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
silk or
nonwov,
syn
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 6 1 0.04/
0.05
Lubricant
Type
or
wat
Alco
or
wat
Rotation
Disk/
Holder
300/150 100/150 300/150 300/150 300/150 150/150 150/150 150/150
rpm/
rpm
Comp/
Contra
Comp or
contra
Force per
Specimen
N lb
40 9 30 7 30 7 30 7 30 7 30 7 25
5.7
10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 45 23 1
Etchants
Material: Nodular cast iron ductile iron
3
, 1528C 2782F, HV 70 ferrite.
Nodular cast iron: Carbon 3.04.0 %, silicon: 1.82.8 %, manganese: 0.11.0 %,
phosphorus: 0.010.1 %, sulfur: 0.010.03 % weight %.
Comments on Material: Nodular cast iron, also called ductile iron and spheroidal
graphite SG cast iron, is a cast iron with the graphite in the form of nodules or
spheres. Unlike malleable cast iron see Material/Preparation Tables 30, the
nodules are developed during the solidication due to small additions of
magnesium and cerium. The advantage of nodular cast iron is the considerable
increase in toughness, caused by the spheroidal graphite, which makes it
comparable to steel for many purposes. The type, size, and distribution are
standardized in the ASTM Standard Test Method for Evaluating the
Microstructure of Graphite in Iron Castings A 247. Also a number of other
specications are described in ASTM standards; some examples are: A 377, A 439,
A 536, and A 439 see Sections 12.4.2.
The metallographic/materialographic examination of the microstructure is as
described in the Material/Preparation Tables 30. Also Methods C-30 and T-30 can
be used for nodular cast iron.
Grinding: Fine grinding with the ner grades of SiC paper in Method T-31 is
important to re-establish the graphite after pull-outs with the coarser grades.
Polishing: At routine examinations, not using image analysis, the specimen
surface after the 3 m polishing step might be satisfactory. Electrolytic polishing
cannot be recommended, but it may be used for routine examination of certain
materials.
Case or coating
thickness/hardness,
surface layers
C-31
Graphite in cast iron A 247 C-31, T-31
of inclusion
content
E 562, E 768, E 1245, E 1382 C-31
High planeness
E 140, E 384, E 448
C-31, T-31
E 1245, E 1351, E 1382, E 1558
C-31,
T-31,
El-03
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/Hours
810 min
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/
Hours
810 min
Grinding
C-31: SiC grinding paper P220 can be used for PG.
When the difference is
more than 100150 m between the center and the periphery, the disk is either
discarded or trued.
Polishing
C-31 and T-31 Both methods can be nished with a ne polishing step with
silica see Method T-30
step P 3.
Section 13.2.2.
Polishing
xed, res
RCD, soft Cloth, napless,
hard,
nonwov, syn
Cloth, nap-
less, hard, wov,
syn
or susp
Dia, spr
or susp
Dia, spr
or susp
Grit or Grain
Size m
P220 9 3 1
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per
Specimen N lb
25 5.7 25 5.7 25 5.7 20 4.5
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
med
hard,
wov,
wool
Abrasive
Type
or susp
Dia, spr
or susp
Dia,
spr
or
susp
Grit or Grain
Size m
P220 P320 P500 P1000 6 3 1
Lubricant
Type
wat
Alco or
wat
Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp Comp
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 30 7 25 5.7 20 4.5
Time
Minutes
Until
plane
0.51 0.51 0.51 5 34 34
Etchants
Material: White cast iron
3
, 1528C 2782F, HV 70 ferrite.
White cast iron: Carbon 1.83.6 %, silicon: 0.51.9 %, manganese: 0.250.8 %,
phosphorus: 0.0060.2 %, sulfur: 0.060.2 % weight %.
Comments on Material: If the liquid iron-carbon is solidied relatively fast, the
carbide is not formed as graphite like in gray cast iron, but as cementite in a
network. This makes the white cast iron very hard and wear resistant, and the
cementite gives the fractured surface the white appearance. If white cast iron is
heated over a period of time, the cementite will break down to form graphite see
Material/Preparation Tables 30. White cast iron is often alloyed with nickel,
chromium, or molybdenum or combinations thereof, to improve the wear
resistance. The different types of white cast irons are standardized in the ASTM
Specication for Abrasion-Resistant Cast Irons A 532 see Sections 12.4.2.
Materialographic preparation of white cast iron is relatively easy because of the
very hard cementite.
Sectioning: Wet abrasive cut-off should be done with a soft Al
2
O
3
, bakelite bond
cut-off wheel. White cast iron may be difcult to cut because of internal stresses
and the feed speed should be low. For very hard materials a CBN wheel resin bond
may be needed see Section 2.4.2.
Mounting: Normally mounting is not needed except in the case of examination of
surface layers see Material/Preparation Tables 0815, or in the case of obtaining a
shape of the specimen suited for automatic preparation. If possible, the specimen
should be sectioned so that it can be placed in a specimen holder without
mounting.
Grinding: Because of the high hardness, the SiC grinding papers will be worn very
fast, and especially at the PG step several sheets may be needed.
Polishing: The polishing step with silica may be omitted for routine examinations
see below.
Etching: See below and Material/Preparation Tables 28, 33, and, 34.
Case or coating
thickness/hardness,
surface layers
C-32
of inclusion
content
E 562, E 768, E 1245, E 1382 C-32
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-32, T-32
E 1351, E 1382, E 1558
C-32, T-32
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond. For very hard materials HV
500700 a CBN wheel resin bond may be
needed see Section 2.4.2..
Mounting
Hot Compression
Mounting
Resin Epoxy with Filler Cold
Mounting
Resin Acrylics
with Filler
Time
Minutes
810 Time
Minutes/
Hours
615 min
Grinding
C-32 and T-32: The PG step may start with SiC grinding paper grit P120 or
P180, if a high material removal is needed.
Polishing
C-32: P 3. This step can often be omitted.
T-32: A step like P 2 in Method C-32 can be added.
Section 13.2.2.
Polishing
xed, res
RCD, hard Cloth,
napless,
hard, wov,
silk
Cloth, med
nap, soft,
syn
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 1 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N
lb
30 7 30 7 30 7 25 5.7 15 3.4
Time
Minutes
Until
plane
4 4 3 1
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Cloth,
v. hard,
wov, syn
Cloth,
napless,
hard
nonwov,
syn
Cloth,
napless,
hard,
wov, syn
Abrasive Type SiC SiC SiC Dia, spr or
susp
Dia, spr or
susp
Dia,
spr or
susp
Grit or Grain
Size m
P220 P320 P500 9 6 3
Lubricant Type Water Water Water Alco or
wat
Alco or
wat
Alco
or wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp
Force per
Specimen N lb
40 9 40 9 40 9 40 9 35 8 30 7
Time
Minutes
Until
plane
0.5 0.5 4 4 3
Etchants
White cast iron 210 General structure
See also Material/Preparation Tables 28, 33,
and 34
Material: High-alloy steels. Heat-treated, low-alloy steels. Heat-
treated, High-alloy steels. Other ferrous metals
austenite face-centered cubic, 7.85 g/ cm
3
, 1528C 2782F, HV 70 ferrite.
High-alloy steels: 8 % total alloying elements weight %.
Comments on Material: High-alloy steels have been developed to obtain special
characteristics like resistance to corrosion, heat, and wear. The corrosion resistant
steels, stainless steels, are described in Material/Preparation Tables 34. The heat
resistant steels can be low- or high-alloyed depending on the temperature range.
The high-alloyed steels may contain chromium, molybdenum, nickel, cobalt, and
titanium to obtain highest heat resistance. For iron-based super alloys, see
Material/Preparation Tables 35. The wear resistant high-alloy steels, tools steels,
may contain a high percentage of chromium and manganese, molybdenum, and
vanadium see Material/Preparation Tables 38.
High-alloy steels can be difcult to prepare because of the often relatively soft
matrix. It can be difcult to conserve all inclusions and carbides, especially if the
specimen should be examined by image analysis. Also hardened alloy steels can be
difcult to prepare; they often have different hardness within the microstructure
and contain a high amount of very hard and brittle carbides. For problems with
smearing, loss of inclusions, etc., see Section 13.6. Often electrolytic polishing can
be used.
Sectioning: Wet abrasive cutting with an alumina, bakelite bond cut-off wheel
with an effective cooling should be without problems. For very hard materials a
CBN wheel resin bond may be needed see Section 2.4.2. Cutting with a band saw
may give deformations and possible work hardening in steels with an austenitic
structure that should be removed at a prolonged plane grinding, or only used for
initial cutting followed by wet abrasive cutting.
Mounting: Normally mounting is not needed except in case of examination of
surface layers see Material/Preparation Tables 0815 or in case of obtaining a
shape of the specimen suited for automatic preparation. If possible the specimen
mounting.
Grinding: In case of water-sensitive inclusions or carbides Method C-33 should be
preferred without the nal polishing step.
Polishing: Electrolytic polishing can be recommended for steels not having a too
heterogenous microstructure.
Etching: For observation of certain phases, like carbides, in the microstructure, a
minimal relief can be developed during the last polishing step so that these can be
seen in the microscope without chemical etching see Section 9.6. A number of
etchants are stated below see also Material/Preparation Tables 34.
Case of coating thickness/
hardness, surface layers
E 1077 C-33
Grain size, grain
boundaries
E 112, E 930, E 1181, E 2283 C-33,
T33,
El-04
Heat treatment C-33,
T-33
inclusion content
E 45, E 562, E 768, E 1077,
E 1122, E 1245, E 1268, E 1382,
E 2283
C-33
High planeness
Inclusion in steel E 45, E 768, E 1122, E 1245 C-33,
T-33
E 140, E 384, E 448
C-33,
T-33
E 768, E 883, E 1077, E 1181,
E 1245, E 1268, E 1351,
E 1382, E 1558
C-33,
T-33,
El-04
T-33,
El-04
Structure changes forging C-33,
T-33,
El-04
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond. For very hard materials HV
500700 a CBN wheel resin bond may be
needed see Section 2.4.2..
Mounting
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/
Hours
610
Grinding
C-33: PG: For low-alloyed steels SiC paper grit P220 should be used.
C-33: FG 1: For low-alloyed steels an RCD soft can be used.
Section 13.2.2.
Polishing
xed, res
RCD, hard Cloth,
napless,
hard, wov,
silk
Cloth, med.
nap, soft, syn
susp
Dia, spr or
susp
Dia, spr or
susp
Grit/Grain Size m P220 9 6 1
Lubricant Type Water Alco or wat Alco or
susp
Alco or wat
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per
Specimen N lb
30 7 30 7 35 8 25 5.7
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov, silk
Cloth,
nap-
less,
hard,
wov, syn
Cloth,
nap-
less,
soft,
porous,
syn
or susp
Dia, spr
or susp
Alumina
Grit or
Grain
Size m
P220 P320 P500 P1200 6 3 0.02/ 0.05
Lubricant Type Water Water Water Water Alco or
wat
Alco or
wat
Rotation Disk/
Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 30 7 25 5.7 10 2.2
Time
Minutes
Until
plane
0.5 0.5 0.5 34 3 1
Etchants
Fe+412 Cr 80, 87, 88, 89, 90, 91, 79, 210 General structure
Fe+1230 Cr+ 6Ni
400 Series
80, 87, 88, 89, 34, 40, 92, 93,
94, 95, 91, 226
General structure
96, 97, 98 Sigma phase
31c Carbides
86 Chemical polish etch
219 Grain boundary
220 Darkens delta ferrite
High temperature 89, 25, 105, 106, 97, 212, 221 General structure
107, 108, 213, 86 precipipate chemical
polish etch
Nonstainless maraging
steels
109, 89, 99, 100, 221 General structure
Nonstainless maraging
steels
83b, 86 Grain boundaries,
chemical
polish etch
Material: Stainless steels. Pure iron
3
, 1528C 2782F, HV 70 ferrite.
Austenitic stainless steels: 1524 % chromium, 322 % nickel.
Ferritic stainless steels: 10.527 % chromium.
Martensitic stainless steels: 11.518 % chromium.
Duplex stainless steels: 2328 % chromium, 2.55.0 % nickel, 1.02.0 %
molybdenum.
Precipitation-hardening stainless steels: 12.2518 % chromium, 7.58.5 % nickel
weight %.
Comments on Material: The stainless steels are corrosion resistant steels
classied according to the type of microstructure, austenitic, ferritic,
austenitic-ferritic, martensitic, duplex, and precipitation-hardening. The austenitic
stainless steels have a microstructure of austenite at room temperature because of
a high nickel content, and they are nonmagnetic. The steels are chromium-nickel
steels, and a typical alloy is the steel 18 % chromium, 8 % nickel. The ferritic
stainless steels are basically chromium steels without nickel, therefore, the ferritic
microstructure. Martensitic stainless steels are chromium steels with a higher
carbon content than other stainless steels making hardening possible. Duplex
stainless steels have a mixed microstructure of ferrite and austenite.
Precipitation-hardening stainless steels are alloyed with elements as copper and
aluminum to establish the precipitation hardening. They can have either a ferritic
or martensitic microstructure.
Pure iron Fe has a ferritic microstructure.
Most stainless steels having an austenitic or ferritic microstructure give difculties
in metallographic/materialographic preparation because these structures are
relatively soft and ductile. Austenite may work harden during cutting and grinding.
It can be difcult to remove all deformation and scratches and obtain a true
structure preserving all inclusions, often brittle carbides and oxides. The
martensitic microstructure is easier to prepare, but in case of brittle carbides,
these can easily be damaged. For advice on smearing, inclusions, etc., see Section
13.6.
The ferrite of pure iron may give problems with deformations see Material/
Sectioning: Wet cut-off cutting with a correct Al
2
O
3
, bakelite bond cut-off wheel
will be without problems. Cutting with a band saw and shearing may give
deformations and cold work that should be removed at a prolonged plane
grinding. For deformation sensitive austenitic steels these methods should be
avoided.
Mounting: Normally mounting is not needed except in the case of examination of
surface layers see Material/Preparation Tables 08 to 15 or in case of obtaining a
shape of the specimen suited for automatic preparation. If possible, the specimen
mounting.
Grinding: Due to deep deformations and possible cold work in the austenite, it is
important that the ne grinding steps are carefully performed to secure that all
deformations and cold work from the sectioning and plane grinding are removed.
Using new SiC grinding paper there is a risk that retained austenite is transformed
into martensite due to mechanical deformation. Also very rough papers and high
grinding forces should be avoided, as deep deformation, introduced in the rst
grinding steps may not be removed by the ne grinding.
Polishing: It can be a problem to obtain a perfect ferrite phase as mentioned
Often electrolytic polishing can give very good results see Section 13.3.
Etching: For stainless steels, observation of inclusions can normally be done
without etching. Chemical etching is relatively difcult, often electrolytic etching
gives good results. A much used electrolytic etching is with 10 g oxalic acid,
100 mL water, using 68 volts for 2030 s, in a stainless steel beaker, using the
beaker as cathode see Section 9.5. For etchants, see below and Material/
Etchants for pure iron, see Material/Preparation Tables 28.
Case or coating
thickness/hardness
surface layers
E 1077 C-34
El-05
E 45, E 562, E 768, E 1077
E 1245, E 1268, E 1382, E 2283
C-34
High planeness
E 140, E 384, E 448
C-34, T-34
E 768, E 883, E 1077,
E 1181, E 1245, E 1268, E 1351,
E 1382, E 1558
C-34, T-34,
El-05
El-05
Structure changes forging C-34, T-34,
El-05
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/Hours
610 min
Grinding
C-34: PG: Use SiC paper grit P320 for pure iron.
Polishing
T-34: P 1: This step can be changed to an FG 4 step with SiC paper grit P4000,
same data as FG 3.
C-34 and T-34: The nal step can be done with alumina 0.02/ 0.05 m.
Section 13.2.2.
Polishing
napless,
hard, wov, syn
Cloth,
napless,
soft, porous, syn
susp
Silica
Grit/Grain
Size m
P220 9 3 0.04/ 0.05
Rotation
Disk/Holder
rpm/rpm
300/ 150 150/ 150 150/ 150 150/ 150
Comp/Contra Comp or
contra
Comp Comp Contra
Force per
Specimen N lb
25 5.5 30 7 25 5.5 15 3.3
Time
Minutes
Traditional Method T-34 For denitions of parameters and consumable see
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
napless,
soft,
porous
Abrasive
Type
or susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 6 3 0.04/ 0.05
Lubricant
Type
wat
Alco or
wat
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
20
4.4
20
4.4
20
4.4
20
4.4
30 7 25 5.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 4 35 12
Etchants
Fe+1220 Cr+410 Ni+ 7 % 80, 31c, 89, 99, 100, 91 General
other elements structure
controlled
transformation,
precipitation
hardening,
stainless
maraging
alloys
31c Carbides
86 Chemical polish-
etch
220 Darkness delta
ferrite
Fe+1530 Cr+640
Ni+ 5%
other elements 300
series
13b, 89, 87, 88,
83a, 80, 94, 95,
91, 101, 212, 221,
226
General structure
13 a, 102, 31 c,
48 c, 213
Carbides and
sensitiza-
tion
Fe+16- 25 Cr+36
Ni+510
48, 96, 97, 98 Stains sigma phase
Mn 200 series 103, 104,
98
Delineates sigma
phase and welds
of dissimilar
metals
86 Chemical
polish-etch
219 Grain boundary
etch no
twins
220 Darkens delta
ferrite
Pure iron 74a Grain boundaries
75 Substruc-
ture
210 Colors ferrite
grains
Material: Super alloys, iron based
3
, 1528C 2782F, HV 70 ferrite.
Super alloys Fe based: 26 to 55 % nickel, 13 to 23 % chromium, 1 to 2.5 %
titanium, 1 to 9 % molybdenum weight %.
Comments on Material: The Fe based super alloys are closely related to the high
alloy steels described in Material/Preparation Tables 33.
Etching: See below and Material/Preparation Tables 33 and 34.
Case or coating
thickness/hardness,
surface layers
C-35
Grain size.
grain boundaries
E 112, E 930, E 1382 C-35, T-35,
E1-06
Heat inuences zone C-35
Image analysis,
rating of inclusion
content
High planeness
E 45, E 562, E 768, E 1245, E 1382, E 2283 C-35
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384
C-35, T-35
E 448
E 768, E 883
E 1245, E 1351, E 1382, E 1558
C-35, T-35,
E1-06
E1-06
Sectioning
Cut-off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/Hours
610 min
Grinding
C-35: PG: SiC paper grit P220 can be used.
C-35: FG 1: Very often this step can be omitted. In that case the step FG 2 RCD,
soft is prolonged to seven minutes.
Polishing
C-35: P 2: Often this step can be omitted.
C-35: P 3: Alumina 0.02/ 0.05 can be used.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 P 1 P 2 P3
Polishing
xed, res
RCD,
hard
RCD,
soft
Cloth,
napless,
hard,
wov,
silk
Cloth, short
nap,
soft, syn
Cloth,
napless,
soft,
porous,
syn
or susp
Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit/Grain size
m
220 9 9 6 1 0.04/ 0.05
Lubricant
Type
Water Alco or
wat
Alco or
wat
Alco or
wat
Alco or
wat
Rotation Disk/
Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 25 5.7 15 3.4
Time
Minutes
Until
plane
3 3 4 3 12
Traditional Method T-35 For denitions of parameters and consumable see
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, syn
Cloth,
med.
nap,
soft,
syn
Abrasive
Type
spr
or susp
Dia,
spr
or susp
Dia,
spr
or susp
Grit or Grain
Size m
P220 P320 P500 P1000 6 3 1
Lubricant
Type
wat
Alco or
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp Comp
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 30 7 30 7 20 4.5
Time
Minutes
Until
plane
0.51 0.51 0.51 45 4 12
Etchants
Super alloys
Fe based
86, 87, 94, 221, 226 General etch
111 depletion
Material: High strength low-alloy steels
3
, 1528C 2782F, HV 70 ferrite.
High strength low-alloy steels: Low and medium carbon steels with small amounts
of alloying elements, vanadium, niobium, titanium.
Comments on Material: High strength low-alloy HSLA steels are a group of low-
and medium-carbon steels with small amounts of alloying elements to improve the
yield strength. The steels are classied by SAE according to yield strength and by
ASTM according to composition, mechanical property requirements, and
application. Examples of the ASTM specications are: A 242, A 572, and A 656 see
Section 12.4.2.
The microstructure of HSLA steels is a mixture of ferrite, pearlite, bainite, and
martensite, and the problems regarding preparation are the same as with medium-
and low-carbon steels see Material/Preparation Methods 28 and 29. In some
cases, water sensitive inclusions should be examined; for this reason the polishing
steps in Methods C-36 and T-36 are stated with water-free lubricants.
Sectioning: At wet abrasive cutting with an Al
2
O
3
cut-off wheel, overheating
should be avoided because martensite can be developed. Cutting pressure should
be moderate and cooling should be efcient on both sides of the cut-off wheel. If
shearing or band sawing is used, the plane grinding should be prolonged to
remove possible deformation or a rougher grinding paper should be used before
grit P220.
Mounting: For routine examination bakelite as powder or tablets is sufcient. In
the case of examination of coatings, other mounting materials should be used see
Material/Preparation Tables 0815. For mounting for electrolytic polishing, see
Section 3.11.6.
Grinding: Grinding normally will give no problems with these materials. Care
should be taken that the deformations from plane grinding are effectively removed
before the polishing. If not, the deformed ferrite can be seen after etching and the
process must be repeated from FG 1.
Polishing: The problem can be to obtain a perfect ferrite phase as mentioned
Electrolytic polishing can be recommended for certain alloys.
Etching: A high number of etchants are available for steels. In most cases a
relative small selection will cover the need in a given laboratory see Material/
Preparation Tables 28 and 33.
surface layers Perfect edge retention
B 487, E 1077 C-36
Grain size, grain boundaries E 112, E 930, E 1181,
E 1382
E-36,
T-36
El-04
Heat treatment C-36,
T-36,
El-04
content
High planeness
E 45, E 562, E 768,
E 1077, E 1245,
E 1268, E 1382, E 2283
C-36
Inclusion in steel E 45, E 768, E 1245 C-36,
T-36
E 110, E 140, E 384, E 448
C-36,
T-36
E 768, E 883, E 1077, E 1122,
E 1181, E 1245, E 1268, E 1351,
E 1382, E 1558
C-36,
T-36,
El-04
T-36,
El-04
Structure changes forging C-36,
T-36,
El-04
Sectioning
Cut-Off-Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/Hours
610 min
Grinding
C-36: PG: SiC paper grit P220 can be used.
Polishing
C-36 and T-36: Steps P 1 and P 2 are stated with water-free diamond
suspensions. These can be changed to normal water-based suspensions.
C-36: P 2: This step can be followed by a nal step with silica like step P 3 in
Method C-35.
Section 13.2.2.
Polishing
xed, res
hard, wov, syn
Cloth, med. nap,
soft, syn
Abrasive Type Diamond Dia, spr or susp Dia, spr or
susp, water-free
Dia, spr or
susp, water-free
Grit or Grain
Size m
P220 9 3 1
Lubricant Type Water Alco or wat Alco or oil,
water-free
Alco or oil,
water-free
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per
pecimen N lb
25 5.5 30 6.6 25 5.7 15 3.4
Time
Minutes
Traditional Method T-36 For denitions parameters and consumables see
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
silk
Cloth,
naplesss,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Alumina
Grit or
Grain
Size m
P220 P320 P500 P1200 6 3 0.02/ 0.05
Lubricant
Type
oil,
water-
free
Alco or
oil,
water-
free
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
35 8 35 8 35 8 25
5.7
25 5.7 25 5.7 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 3 3 12
Etchants
See Material/PreparationTables 28and33.
Material: Carbonitrided steels. Carburized steels. Nitrided steels.
Other surface treated steels
3
, 1528C 2782F, HV 70 ferrite.
Comments on Material: Case hardening is a term that covers the process of
changing the surface layer of steel by absorption of carbon or nitrogen, or both.
The process can be done in different ways as carbonitriding, carburizing,
cyaniding, nitriding, and nitrocarburizing. With or without further heat treatment
a hard surface layer is created.
Mostly low carbon steels are used for carburization, often a case with a carbon
content of 0.71 %, and a hardness of approximately 60 HRC HV 700. The case
depth varies from 0.3 to 3 mm depending on processing time and temperature.
For nitriding low carbon steels and steels alloyed with Al, Cr, and V are used. The
hardness of the diffusion layer may be up to 70 HRC HV 1000 and the thickness
0.010.5 mm depending on process time and temperature.
The metallographic/materialographic examination normally covers layer thickness,
diffusion zone, and defects in the layer. For this reason it is very important to
obtain the highest degree of edge retention see also the Material/Preparation
Tables 0815.
Sectioning: Cutting, often of a test piece treated along with the work piece, should
be wet abrasive cutting with an Al
2
O
3
, bakelite bond cut-off wheel. It is important
that excessive heat and deformation is avoided. When cutting nitrided layers that
are very hard, a relatively soft wheel is used and cooling should be very effective.
If shearing or band sawing is used, the plane-grinding step should be prolonged to
remove possible deep deformation. It is important that the cutting takes place
perpendicular to the surface to be prepared. If the plane of the cross section is not
perpendicular to the plane of the surface layer, the measured thickness will be
greater than the true thickness. For example, an inclination of 10 will contribute
a 1.5 % error.
should be used, preferably epoxy. For very hard coatings hot mounting with epoxy
with a ller should be preferred. Also, a phenolic resin with carbon bers can be
of advantage. For hot mounting a special application can be made to secure the
edge: Tightly wrap up the specimen in Al foil household type. This gives a good
separation between mounting material and surface layer. Also, a copper foil can be
used on nitrided and carburized layers giving an excellent edge denition and
contrast. Choose a mounting material with hardness as close as possible to the
hardness of the coating. As a less ideal alternative, cold mounting with epoxy or
an acrylic material with ller can be used.
Grinding: The preparation process should secure the highest possible edge
retention. This means that all grinding, either on SiC grinding paper, diamond
pads, or rigid composite disks RCDs, should be as short as possible.
In Method T-37 the grinding is suggested with diamond pads, considered for very
hard surface layers. In case of softer layers these pads can be changed to SiC
grinding paper, as stated in Method T-32 see below.
It has been found that the use of xed diamonds for plane grinding of certain
nitrided and carburized layers may introduce ne cracks in the hard layer,
therefore, SiC paper should be used see below.
Polishing: Also the polishing steps should be kept as short as possible.
Etching: See Material/Preparation Tables 28, 33, and 34.
Case or coating
thickness/hardness,
surface layers
C-37, T-37
Prefect edge retention
High planeness
E 45, E 562, E 768, E 1077
E 1245, E 1268,
E 1382, E 2283
C-37, T-37
Microhardness, hardness E 10, E 18, E 92, E 103,
E 140, E 684, E 448
C-37, T-37
768,
E 883, E 1077, E 1245, E 1268,
E 1351, E 1382, E 1558
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Resin Expoxy
with Filler
with ller
Time
Minutes
9 Time
Minutes/
Hours
68 h
Grinding
C-37 and T-37: PG: For certain nitrocarburized/nitrided layers, disks/pads with
xed diamonds should be avoided see above. SiC paper grit P220 should be
used. Also FG 1 in Method T-37 shall be changed to SiC paper grit P320/P500
see Method T-32.
C-37: Very often FG 1 can be changed to RCD, soft and FG 2 can be omitted.
T-37: In case of relatively soft surface layers, the diamond pads in PG and FG 1
can be changed to SiC grinding paper see Method T-32.
Polishing
T-37: To improve edge retention, the step P 2 can be changed to P 2 from
Method C-37.
Section 13.2.2.
Grinding PG FG 1 FG 2 P 1 P 2
Polishing
xed, res
RCD, hard RCD, soft Cloth,
napless,
hard, wov,
syn
Cloth, med
nap, soft, syn
Abrasive
Type
Diamond Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Grit or
Grain
Size m
220 9 3 3 1
Lubricant
Type
Water Alco or wat Alco or wat Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp Comp Comp
Force per
Specimen N
lb
35 8 25 5.5 25 5.5 40 9 25 5.5
Time
Minutes
Until
plane
5 45 45 12
Section 13.2.2.
Polishing
Disk/Cloth Dia, pad
met
Dia, pad met Cloth nap-
less, v. hard
nonwov or
wov, syn
Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous, syn
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
125 40 9 3 0.04/ 0.05
Lubricant Type Water Water Alco or wat Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp Comp Contra
Force per
Specimen N lb
35 8 35 8 40 9 40 9 15 3.4
Time
Minutes
Etchants
See Material/PreparationTables 28, 33, and34.
Material: High-speed steels. Low-alloyed tool steels. Other tool
steels
3
, 1528C 2782F, HV 70 ferrite.
Comments on Material: The tool steels cover a wide range from the highly
alloyed high-speed steels to low-alloy steels with small amounts of a few alloying
elements. Most tool steels contain molybdenum or tungsten, or both. Often other
elements like vanadium, cobalt, nickel, and chrome are added. The tool steels are
classied by the American Iron and Steel Institute AISI using a letter to represent
each class of steel. Tool steels are metallographically/materialographically
examined for inclusion content, decarburization, degree of spheroidization, grain
size, hardness, etc., and they are often difcult to prepare because of the hardness
and the brittle carbides. For advice on artifacts developed during the preparation,
see Section 13.6.
Sectioning: In the case of nontempered tool steels, it is important that the
sectioning takes place without excessive heat because this will introduce localized
tempering effects. Cutting should take place as wet, abrasive cutting with an
efcient cooling, preferably using a thin cut-off wheel, or a relatively soft wheel, or
both. The feed speed should be low with a low force in the cut. For high-hardness,
high-alloy steels, precision cutting with a thin CBN cut-off wheel may be of
advantage, producing a cut surface with very little damage. Steels with a hardness
below 35 HRC may be cut using a band saw, but in this case, because of the
considerable deformation, the plane grinding should start with SiC grinding paper
rougher than grit 220. In case of as-quenched high-alloy steels, the specimen may
be sectioned by fracture.
Mounting: For routine examination bakelite as powder or tablets is sufcient if
heat degredation is not anticipated. In the case of examination of coatings, other
mounting materials should be used see Material/Preparation Table 0815. For
mounting for electrolytic polishing, see Section 3.11.6.
Grinding: The often very hard material will wear out the SiC grinding papers in a
very short time, and often several sheets of each grain size should be used. In case
of pull-outs of carbides at high-alloy steels, Method C-38 should be preferred.
Polishing: For routine examination, the number of steps may be reduced see
below.
Etching: A number of etchants are stated below.
Case or coating
thickness/hardness,
surface layers
B 748, C 664 C-38
Image analysis,
rating of inclusion
content
E 45, E 562, E 768, E 1077
E 1245, E 1268, E 1382, E 2283
C-38, T-38
High planeness
Inclusions in steel E 45, E 768, E 1245 C-38
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-38, T-38
768,
E 883, E 1077, E 1245, E 1268, E
1351, E 1382, E 1558
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/Hours
610 min
Grinding
C-38: For certain tool steels, the step P 1 can be changed to an RCD, soft.
T-38: For routine examination the step FG 3 may be omitted.
Polishing
C-38: For certain tool steels, the step P 2 can be changed to P 3 from Method
T-38 or P 3 Method T-38 can be added.
T-38: In case of routine examinations, the step P 2 can be changed to step P 1
from Method C-38, as the last step.
Section 13.2.2.
Grinding/ PG FG P 1 P 2
Polishing
xed, res
RCD, hard Cloth,
napless,
hard, wov,
syn
Cloth, med.
nap,
soft, syn
susp
Dia, spr or
susp
Dia, spr or
susp
Grit or Grain Size
m
P220 9 3 1
Rotation Disk/
Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per Specimen
N lb
35 8 35 8 35 8 40 9
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless
soft
porous,
syn
or susp
Dia, spr
or susp
Alumina
Grit or Grain
Size m
P220 P320 P550 P1200 6 3 0.02/ 0.05
Lubricant
Type
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp Comp
Force per
Specimen
N lb
40 9 40 9 40 9 40 9 40 9 30 7 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 5 4 12
Etchants
Tool steels 74a, 80, 14 General structure
110 Grain boundaries in tempered tool steel
210, 211 Colors ferrite, lower alloy grades
214 Colors cementite
224, 225 Carbides attacked and colored
Material: Cement clinker. Concrete
Material Properties: Portland cement clinker, mineralogical composition: Alite
C
3
S 3575 %, Belite C
2
S 040 %, Aluminate C
3
A 110 %, Ferrite C
4
AF 215
%, Periclase MgO 03 %, Free lime CaO 05 %, Arcanite K
2
SO
4
03 %,
Ca-Langbeinite 2CaSO
4
03 %.
Comments on Material: Portland cement clinker is a raw material for cement
production consisting of several mineral phases with different physical properties,
as mentioned above.
Hardened concrete consists of cement paste mixed with aggregates like sand and
stone.
Cement clinker and concrete can be examined in reected light and in transmitted
light. The preparation of cross sections for reected light is stated below. Thin
sections for transmitted light is described in Section 7.13.
Both cement clinker and concrete often are very sensitive to water used during the
preparation and, consequently, this should be avoided, especially during the last
steps of the preparation.
Sectioning: The material being brittle should be treated carefully to avoid
damage. Often it can be of advantage to impregnate the specimen before cutting
see below. Cutting is preferably done with a precision cut-off machine with a
thin cut-off wheel, diamond, metal bond or SiC, bakelite bond and with a
water-free coolant.
Mounting: Very often the specimen is porous so that impregnation with epoxy is
needed to stabilize the material. Also, often the examination, especially at
concrete, is done to determine pores air voids and microcracks, and therefore it
can be recommended to add uorescent dye to the epoxy see Section 3.10.
Grinding: The traditional method, T-39, stated below is based on lapping on cast
iron disks, as known from preparation of mineralogical materials. Often the
lapping can be changed to the use of SiC grinding paper, as indicated under
Preparation Process 39 below.
Polishing: The two methods stated below have a 3 m step as the last polishing
step. If needed, this step can be followed by ner steps, as indicated under
Preparation Process 39 below.
Etching: Normally these materials are not etched.
Case or coating
thickness/hardness,
surface layer
Cement clinkers and concrete are covered
by a number of ASTM standards. These are
not stated here, as it is considered outside
the scope of this book.
C-39
Grain size, grain
boundaries
C-39, T-39
C-39
High planeness
Microhardness,
hardness
C-39, T-39
Porosity C-39
Sectioning
0.019 in thickness
Mounting
Time
Minutes
Time
Minutes/Hours
812 h
Grinding
C-39: PG, if material is very water sensitive use alcohol or glycerol instead of
water.
C-39: PG and FG: For clinker, lower force on specimens to 15 N.
C-39: In some cases clinker FG 1 can be omitted.
T-39: In some cases the lapping on cast iron disks can be changed to SiC paper,
P220, P320, P500 and P1000 using glycerol as cooling uid.
Polishing
C-39: P 1: For clinker, lower force per specimen to 10 N.
C-39 and T-39: If needed, P 1 can be followed with one or two steps, see
P 2 in Method C-38 with water-free lubricant, followed by P 2 in Method T-37.
Section 13.2.2.
Grinding/ PG FG 1 FG 2 P1
Polishing
Disk/Cloth Dia, disk, xed,
res
Dia, disk, xed,
res
hard, wov, syn
Abrasive Type Diamond Diamond Dia, spr or susp,
water-free
Dia, spr or
susp,
water-free
Grit or Grain
Size m
P220 P1200 9 3
Lubricant Type Water/
glycerol
Water/glycerol Alco,
water-free
Alco, water-
free
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or contra Comp Comp Comp
Force per
Specimen N /lb
35 8 35 8 35 8 20 4.5
Time
Minutes
Until plane 5 5 5
Section 13.2.2.
Polishing
Disk/Cloth Cast iron
disk
Cast iron
disk
Cast iron
disk
Cast iron
disk
Cloth,
napless,
hard,
wov, syn
Abrasive Type SiC powder SiC powder SiC powder SiC powder Dia, spr or
susp, water-
free
Grit or Grain
Size m
P220 P400 P800 P1200 3
Lubricant Type Glycerol Glycerol Glycerol Glyecerol Alco or oil,
water-free
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Contra Contra Contra Contra Comp
Force per
Specimen N
lb
5 1.1 5 1.1 5 1.1 5 1.1 20 4.5
Time
Minutes
23 23 23 23 5
Material: Minerals. Ores
Comments on Material: Minerals, ores, and rocks cover a wide eld of materials
with a high variety of phases. Most often minerals are brittle and hard, but often
with a very different hardness of the different phases. This makes preparation of
minerals relatively difcult, both because of the risk of deformation, the
brittleness, pores, and cracks, creating the risk of pull-outs, and the tendency for
relief between the phases.
Minerals are prepared as polished sections for reected light examination and as
thin sections for transmitted light examination. Below the preparation of polished
sections is described; thin sections are described in detail in Section 7.13 see also
Sectioning: It is important that the often very hard and brittle material is not
damaged too much during the sectioning. Often the cutting of an intermediate
piece is cut with a large machine specially built for cutting of minerals, using a
diamond cut-off wheel, metal bond. For the actual specimen, wet abrasive cutting
is often done with a thin diamond, metal bond cut-off wheel on a precision cut-off
machine to ensure a good surface. In case of very brittle materials, with pores and
cracks, an impregnation before the cutting is recommended see below. For softer
minerals an SiC bakelite bond cut-off wheel can be used.
Mounting: Often the specimen, being brittle and with pores and cracks, should be
impregnated under vacuum with an epoxy see Section 3.10. To easily distinguish
pores and cracks, the epoxy resin can be added as a dye see Section 3.10. Also,
an impregnetion with a dye makes it possible to distinguish between original pores
and pores, pull-outs, caused by the preparation process see Section 13.6.
Grinding: The traditional grinding of minerals is made as a lapping with loose
grains see Section 6.7.7. This method is stated in Method T-39, however, below,
the two methods stated are with xed grains considered the most useful for
polished sections. Some phases in minerals are very sensitive to deformation like
certain soft and ductile metals. For this reason the ne grinding step with 9 m
diamond in Method C-40 and the steps with 9 m and 6 m in Method T-40 are
very important to create a deformation free surface, and these steps should be
prolonged if the deformation is not reduced to a satisfactory level that can be
removed by the 3 m step.
Polishing: In the case of phases with very different hardness, the polishing time
should be kept as short as possible and the force as low as possible to reduce
relief.
Etching: Etching of minerals can be done for identication of the single phases in
a mineral based on the reaction of a specimen material to a standard set of
reagents. Another approach is to use the reagents for revealing the microstructural
details, as it is known from etching of metals. Both approaches are relatively
complicated and fall outside the scope of this book.
Case or coating
thickness/hardness,
surface layers Perfect edge
retention
ASTM standards covering
minerals and ores are
not stated here, as it is
considered outside the
scope of this book.
C-40
content
C-40
High planeness
Microhardness, hardness C-40, T-40
Porosity C-40
Sectioning
0.019 in thickness
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
812 h
Grinding
C-40: For soft/brittle materials, SiC paper grit P320 can be used.
C-40: FG: For hard materials a step like FG 1 in Method C-39 can be added.
Attention: In C-methods, when using RCD: the disk turns concave during use.
Polishing
C-40: P 1 and P 2: For hard materials a step like P 2 in Method C-38 can be used
between the steps P 1 and P 2.
T-40: P 1 can be followed by a P 2 step like in Method C-40
Section 13.2.2.
Polishing
xed, res
RCD, soft Cloth,
napless,
hard,
wov, syn
Cloth
napless,
soft,
porous, syn
Abrasive Type Diamond Dia, spr, or susp Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp
Force per
Specimen N lb
20 4.5 20 4.5 20 4.5 10 2.2
Time
Minutes
Until plane 36 35 1
Section 13.2.2.
Grinding/ FG 3 P 1
Disk/Cloth Dia, pad
bak
Cloth,
napless,
v. hard,
nonwov/
wov
Cloth, napless,
v. hard
nonwov/
wov
Cloth,
napless,
v. hard
nonwov/
wov
Cloth,
napless,
hard,
wov, silk
or susp
Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or susp
Grit or Grain
Size m
30 9 6 3 1
Lubricant Type Water Alco
or wat
Alco
or wat
Alco
or wat
Alco
or wat
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp
Force per
Specimen N lb
25 5.7 30 7 3040 79 3040 79 1030 2.37
Time
Minutes
Until
plane
5 5 5 2
Material: Pure aluminum. Cast aluminum alloys
Material Properties: Aluminum: Face-centered cubic, 2.699 g/ cm
3
, 660.2C
1220F, HV 150.
Cast alloy: Aluminum-silicon: 12.5 % Si eutectic composition. Other cast alloys:
Aluminum-silicon-magnesium, aluminum-silicon copper, aluminum
silicon-copper-magnesium, aluminum-magnesium, aluminum-zinc-magnesium,
aluminum-copper-titanium-magnesium weight %.
Comments on Material: Commercially pure aluminum has an aluminum content
higher than 99 % for wrought alloys and 99.5 % for cast alloys. Cast alloys can be
alloyed with a number of elements as mentioned above. Aluminum and its alloys
are classied through a number of systems, the most important is the system
established by the Aluminum Association see below. Another important system
uses the chemical symbols of the most important alloying elements combined with
a number stating the content in weight %. AlMg3MnCr describes an alloy with 3 %
magnesium and amounts of manganese and chromium, normally but not always
below 1 % each. Less important alloying elements are not mentioned.
Aluminum Association has developed a system for wrought and cast alloys
consisting of four numbers followed by a with a letter and a number. For
wrought alloys the four numbers are like: nnnn, at cast alloys the numbers have a
dot: nnn.n. For wrought alloys the rst number expresses:
1nnn Commercially pure aluminum 99 %
2nnn Copper as most important alloying element
3nnn Manganese
4nnn Silicon
5nnn Magnesium
6nnn Magnesium and silicon.
7nnn Zinc
8nnn Other alloying elements
9nnn Is not used
For cast alloys the rst number expresses:
1nn.n Commercially pure aluminum 99.5%
2nn.n Copper
3nn.n Silicon with copper or magnesium
4nn.n Silicon
5nn.n Magnesium
6nn.n Is not used
7nn.n Zinc
8nn.n Tin
9nn.n Other alloying elements
The letter following the expresses heat treatment and the number will express
further specication of the alloy.
ASTM has specied a high number of aluminum alloys and a number of test
methods for aluminum.
Pure aluminum is a very soft and ductile metal that can be difcult to prepare
mechanically. It is important that deformations developed during sectioning and
grinding are removed through the polishing steps. Also, there is a risk of
embedded grains see Section 13.6.4. Electrolytic polishing can be done with a
perchloric acid electrolyte and often gives very good results. Cast aluminum alloys
and wrought alloys are easier to polish mechanically and they are normally not
suited for electropolishing.
Sectioning: Wet abrasive cutting with an SiC bakelite bond cut-off wheel should
be recommended. To avoid solid state transformation in certain materials, an
efcient cooling is important. If shearing or band sawing are used, it is important
that the induced heavy deformation is removed during the plane grinding step.
Mounting: Both hot and cold mounting materials can be used. In the case of
heat-sensitive alloys cold mounting is recommended. For examination of pores
castings, vacuum impregnation may be of advantage see Section 3.10.
Preferably the mounting material should be a little harder than the hardest
constituent in the specimen material. In the case of examination of thin layers it
can be recommended that the specimen is tightly wrapped in thin metal foil e.g.,
household aluminum foil or nickel foil and then hot mounted. In this way the
surface layer can be easily distinguished from the mounting material.
Grinding: It is important that the deformation from sectioning and the rough
grinding steps are removed. If the grinding steps give too high deformation, the
force per specimen should be reduced.
Polishing: The rough polishing steps with 6 and 3 m are important. If strong
deformation can be seen after 3 m, the process should be repeated from FG 1.
With only small deformation the time can be prolonged or the force increased, or
both. If relief develops between matrix and a second phase, Method C-41 should
be used.
Electrolytic polishing can be used for pure aluminum and for not too
heterogenous alloys.
Etching: It can be difcult to etch the surface of aluminum due to a thin oxide
lm. Also, it is difcult to etch the matrix and several intermetallic phases and
precipitates with the same etchant, making the use of several ecthants necessary. It
is, however, possible to avoid this for a number of alloys by using a color etchant
based on potassium permanganate Weck, see Ref. 47, Part I: 100 mL distilled
water +4 g potassium permanganate, after dissolving: +1 g sodium hydroxide.
Immersion in 15 s at room temperature with a freshly prepared solution. The
drawback with this etchant is that the specimen surface must be absolutely free
from deformation. This can be obtained by pre-etching the surface with 100 mL
distilled water +2 g sodium hydroxide. Immersion in 30 to 60 s at room
temperature. For other etchants, see below, and Material/Preparation Tables 42/43.
Case or coating thickness/
hardness,
surface layers
B 487 C-41
Grain size, grain
boundaries
E 112, E 930, E 1181, E 1382 C-41, T-41
El-10 pure
Al
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-41, T-41
High planeness
E 110, E 140, E 384,
E 448
C-41, T-41
E 1181, E 1245, E
1351, E 1382, E 1558
C-41,
T-41,
El-10 pure
Al
Sectioning
Cut-Off Wheel SiC, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
C-41: PG: If possible use SiC paper grit P320.
T-41: Very often FG 4 can be omitted.
Polishing
C-41: P 2: This step can often be omitted.
Pure Al: Electrolytic polishing will give good results.
Section 13.2.2.
Polishing
napless,
med hard,
wov, wool
Cloth, med
nap, soft, syn
Cloth,
napless,
soft, porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 1 0.04/ 0.05
Lubricant Type Water Water Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp Comp Contra
Force per
Specimen N lb
25 5.7 30 7 25 5.7 20 4.5 15 3.3
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
med
hard,
wov,
wool
Cloth,
nap-
less,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 6 3 0.04/
0.05
Lubricant
Type
wat
Wat-
oil
Rotation
Disk/
Holder
rpm/
rpm
300/150 300/150 300/150 300/150 150/150 150/150 150/150 150/150
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N
lb
25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 20 4.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 4 34 12
Etchants
Pure aluminum 1a, 2, 3 General structure
Cast aluminum 2000 series 3, 2, 1a General structure
8a, 6, 7 Phase identications
Cast aluminum 4000 series 3, 1a General structure
Material: Other aluminum alloys
3
, 660.2 C
500F, HV 150.
Etching: See Material/Preparation Tables 41/43 and below.
surface layers
B 487 C-42
El-10
content
E 562, E 1245, E 1382 C-42, T-42
High planeness
E 110, E 140, E 384, E 448
C-42, T-42
E 1181, E 1245, E 1351,
E 1382, E 1558
C-42, T-42,
El-10
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
Polishing
C-42: P 1: For harder alloys this step can be changed to a napless, hard, wov, silk
cloth.
C-42: For softer alloys the step P 1 from Method T-42 can be added, between FG
1 and P 1.
T-42: P 3 can be followed by a step with silica, see C-42. Also at harder alloys the
step P 3 can be omitted.
Often electrolytic polishing can be recommended for the examination of the
microstructure.
Section 13.2.2.
Polishing
napless, med
hard, wov,
wool
Cloth, napless,
soft, porous, syn
susp
Silica
Grit or Grain
Size m
P220 9 3 0.04/ 0.05
Lubricant Type Water Water Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Contra
Force per
Specimen N lb
25 5.7 30 7 25 5.7 15 3.3
Time
Minutes
Until
plane
5 3 12
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov, syn
Cloth,
med.
nap,
soft,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Dia, spr
or susp
Grit or
Grain
Size m
P220 P320 P500 P1200 6 3 1
Lubricant
Type
wat
Alco or
wat
Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp Comp
Force per
Specimen
N lb
25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 4 4 1
Etchants
Al alloys 3, 1a, 2 General structure
7000 series 4, 5 Grain structure under polarized light
3b, 6 Phase identication
Material: Wrought aluminum alloys
3
, 660.2C
500F, HV 150. Wrought aluminum alloys: Manganese. Magnesium.
Magnesium-manganese-chrome. Magnesium-silicon. Copper. Copper-manganese
and copper-silicon-manganese. Zinc-magnesium. Zinc-magnesium-copper.
Lithium-copper-magnesium.
Polishing: Alloys containing magnesium may be sensitive to water and should be
polished with water-free lubricants see also Material/Preparation Tables 41.
Etching: See Material/Preparation Tables 41/42 and below.
Case or coating
thickness/hardness,
surface layers
B 487 C-43
El-10
E 562, E 1245, E 1382 C-43, T-43
High planeness
E 140, E 384, E 448
C-43, T-43
E 1245, E 1351, E 1382, E 1558
C-43, T-43,
El-10
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
C-43: FG 2: Very often this step can be omitted.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper RCD, soft RCD, soft Cloth,
napless,
med hard,
wov, wool
Cloth, nap-
less, soft,
porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
ize m
P220 9 3 3 0.04/ 0.05
Lubricant Type Water Alco or wat Alco or wat Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
20 4.4 30 6.6 25 5.7 15 3.4 15 3.4
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Alumina
Grit or Grain
Size m
P220 P320 P500 P1200 P2400 3 0.02/
0.05
Lubricant
Type
Water Water Water Water Water Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Comp Comp Contra
Force per
Specimen
N lb
25
5.7
25
5.7
25
5.7
25
5.7
25
5.7
20 4.5 15 3, 4
Time
Minutes
Unit
plane
0.51 0.51 0.51 0.051 34 12
Etchants
1000 series 1a, 2, 3, General structure
4, 5 Grain structure under
polarized light
6, 7 Phase identications
3000 series 3, 1a General structure
polarized light
8a, 6, 7 Phase identications
5000 series 3, 1a, 2, 6, 8a General structure
polarized light
6000 series 3, 1a, 2, 6, 8a, 222 General structure
polarized light
1a, 2, 7, 6, 8a Phase identications
Material: Pure antimony. Sb alloys, and Sb bearing alloys. Pure
bismuth. Bi alloys
Material Properties: Antimony: Hexagonal, 6.691 g/ cm
3
, 630.5C 1167F.
Bismuth: Hexagonal, 9.78 g/ cm
3
, 271.3C 520F, HB 70.
Comments on Material: Both antimony and bismuth are seldomly used as pure
metals, but mostly used as alloying elements. Antimony is used for bearing alloys.
Pure antimony is relatively hard and pure bismuth is soft. Both metals are very
brittle.
Sectioning: Care should be taken that the brittle materials are not damaged too
much during the cutting. At wet abrasive cutting, a thin SiC cut-off wheel bakelite
bond should be used. To avoid cracking during cutting it may be useful to mount
the specimen in epoxy before cutting.
Mounting: Both hot and cold mounting can be used. Be careful that the high
pressure during hot mounting doesnt damage the brittle specimen.
Grinding: During grinding with SiC grinding paper, the paper may be loaded with
the material because this is not taken away by the water ow. A loaded paper
should not be used as it will give stronger damage to the specimen. The water ow
should be strong and the aggressiveness of the paper can be dampened by adding
a small amount of hard wax to the paper surface before use, or the new paper can
be run-in with a hard material in a few seconds.
Polishing: It is important that all deformations from the grinding are removed
after the rough polishing step P 1. For polishing of pure antimony and pure
bismuth, a solution of 3 % nitric acid in glycerol can be added to the silica used
for the last step. At polishing of Sb alloys containing lead, the last polishing step
can be with a 0.3 alumina suspension with added ammonium tartrate, 1 g per 1 L
distilled water. At polishing of Bi, the 6 m step can be omitted see below.
Both pure antimony and bismuth are well suited for electrolytic polishing.
Etching: See below.
Case or coating
thickness/hardness,
surface layers
B 487 C-44
Grain size, grain
boundaries
E 112, E 930, E 1181, E 1382 C-44, T-44
El-10
E 562, E 1245, E 1382 C-44, T-44
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-44, T-44
E 1245, E 1351, E 1382, E 1558
C-44, T-44,
El-10
Sectioning
Mounting
Hot Compression
Mounting
Resin Bakelite Cold Mounting Resin Acrylics/Epoxy
Time
Minutes
89 Time
Minutes/
Hours
610 min/ 68 h
Grinding
T-44: For harder alloys, FG 4 can be omitted.
Polishing
C-44 and T-44: P 1: At polishing of bismuth and Bi alloys this step can be
omitted.
C-44: P 3: At polishing of bismuth and Bi alloys the time may be increased to
several minutes.
For the nal step chemical mechanical polishing can be recommended see
above.
Section 13.2.2.
Polishing
napless,
hard,
wov, silk
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
nap-
less,
soft,
porous,
syn
or susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit or Grain
Size m
P220 P320 9 6 3 0.04/ 0.05
wat
Wat-oil
Rotation
Disk/
Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp or
contra
Force per
Specimen
N lb
25 5.7 25 5.7 30 7 25 5.5 25 5.7 15 3.3
Time
Minutes
Until
plane
0.51 5 4 3 1
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
med.
hard,
wov,
wool
Cloth,
nap-
less,
soft,
por-
ous,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 6 3 0.04/
0.05
Lubricant
Type
Water Water Water Water Water Wat-oil Wat-oil
Rotation
Disk/
Holder
300/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 20 4.5 15 3.4 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 45 3 1
Etchants
Sb, lean,
Sb alloys
Sb 938 Grain contrast
Sb, Sb alloys 936, 937, 940 General structure
Sb-Pb alloys 938, 941 General structure
Bi, Bi alloys 937, 940 General structure
Bi-Sn alloys, Bi-Ca alloys 938 General structure
Material: Pure beryllium. Be alloys
Material Properties: Beryllium: Hexagonal close-packed, 1.8 g/ cm
3
, 1350C
2462F, HRB 80.
Comments on Material: Beryllium is a light metal which is mostly used as an
alloying element, improving the strength of the alloy. Pure beryllium is toxic to
inhale which means that the preparation process, when dust is developed, must
take place in a glove box or under an efcient fume hood, or both.
Pure beryllium resembles magnesium see Material/Preparation Tables 53 it
deforms and fractures easily and preparation must be done with great care.
Sectioning: For wet abrasive cutting a thin SiC bakelite bond cut-off wheel should
be used. For alloys based on copper, a medium hard wheel is recommended. For
nickel-based alloys a softer wheel should be used. The cooling should be efcient
to avoid thermal damage. When cutting pure beryllium and alloys with a high Be
content, it is important that the sludge, metal dust, and particles from the wheel
are correctly disposed of because of the toxicity.
Mounting: Both hot mounting and cold mounting can be used.
Grinding: When wet grinding pure beryllium and alloys with a high Be content
the dust is bound by the water, but care must be taken to have the correct disposal
of the sludge. For pure beryllium the force on the specimen should be reduced and
often it can be of advantage to make the grinding on a stationary paper in one
direction.
Polishing: For pure beryllium and certain alloys electrolytic polishing is
recommended. Also a chemical mechanical polishing can be used see below.
Etching: Pure beryllium can be examined in polarized light. For etchants, see
below.
Purpose ASTM Standard See Section 12.4. Method
Case or coating
thickness/hardness,
surface layers
B 487 C-45
El-10
E 562, E 1245, E 1382 C-45, T-45
High planeness
E 110, E 140, E 384,
E 448
C-45, T-45
Microstructure E 3, E 407, E 562, E 883, E 1181, E 1245,
E 1351, E 1382, E 1558
C-45, T-45,
El-10
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
T-45: Pure Be is relatively brittle and grinding should be performed with Method
T-45, but with lower force than indicated.
Polishing
C-45, T-45: For the last step with silica, one part of hydrogen peroxide 30 %
can be added to ve parts of silica suspension.
Section 13.2.2.
Grinding PG FG 1 P 1 P 2
Polishing
xed, res
RCD, soft Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft,
porous, syn
or susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 0.04/ 0.05
Lubricant Type Water Water Water
rpm/rpm
Comp/Contra Comp or contra Comp Comp Contra
Force per Specimen
N lb
20 4.4 30 6.6 25 5.5 15 3.4
Time
Minutes
Until plane 5 45 12
Traditional Method T-45 For denitions of parameters and consumables
see Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1200 6 3 0.04/ 0.05
Lubricant
Type
Water Water Water Water Alco-wat Wat-oil
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
25 5.7 25 5.7 25 5.7 20 4.5 20 4.5 20 4.5 15 3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 45 34 12
Etchants
Pure Be 9, 10 General structure via polarized light
Be alloys 11 General structure
Material: Pure chromium. Cr alloys
Material Properties: Chromium: Body-centred cubic, 7.17 g/ cm
3
, 1875C
3407F, HB 125.
Comments on Material: Chromium belongs to the refractory metals and pure
chromium is soft and ductile. The alloys, which are commercially available, often
used for plating, are hard and relatively brittle.
The machinability of chromium is low and cold working is easy which makes
chromium relatively difcult to prepare mechanically.
Sectioning: Wet abrasive cutting can be made with an SiC bakelite bond cut-off
wheel. Due to the poor machinability a relatively soft wheel, as thin as possible,
should be used.
Mounting: Both hot and cold mounting can be used.
Grinding: Because of the poor machinability the grinding papers should only be
used as long as they are cutting efciently, if not, cold work and deformation will
develop.
Polishing: It is important that the deformations from grinding are removed during
the rough polishing step. It can be difcult to remove all deformation by
mechanical polishing and often chemical mechanical polishing can be an
advantage see below. Also electrolytic polishing can be recommended.
Etching: Chromium is difcult to etch, two etchants are stated below.
Purpose ASTM Standard
See Section 12.4
Method
Case or coating
thickness/hardness,
surface layers
B 487 C-46
Grain size, grain
boundaries
E 112, E 930, E 1181, E 1382 C-46, T-46,
El-11
E 562, E 1245, E 1382 C-46, T-46
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110, E 140,
E 384, E 448
C-46, T-46,
El-11
E 1351, E 1382, E 1558
C-46, T-46,
El-11
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
T-46: Very often FG 3 can be omitted.
Polishing
C-46 and T-46: The last polishing step can be with alumina 0.020.05 m in
distilled water 100 mL with sodium hydroxide 5 g, or alumina 300 mL with
hydrogen peroxide H
2
O
2
20 mL 30 %.
C-46: If needed the step P 1 from T-46 can be used between FG 1 and P 1
expanding the method with one step.
C-46: P 2: This step can often be omitted.
Section 13.2.2.
Polishing
xed, res
RCD, soft Cloth,
napless,
hard, wov,
silk
Cloth, med.
nap, soft, syn
Cloth, nap-
less, soft,
porous, syn
Abrasive
Type
Diamond Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 1 0.04/ 0.05
Rotation
Disk/
Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Force per
Specimen
N lb
30 7 30 7 30 7 25 5.7 15 3.39
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Alumina
Grit or
Grain
Size m
P220 P320 P500 P1200 6 3 0.02/ 0.05
Lubricant
Type
wat
Wat-oil
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Force per
Specimen
Nlb
15
3.4
15
3.4
15
3.4
15
3.4
30 7 20 4.5 10 2.3
Time
Minutes
Until
plane
0.51 0.51 0.51 45 3 1
Etchants
Cr 12, 13c General structure
Material: Pure Cobalt. Co Alloys
Material Properties: Cobalt: Above 417C 783F: Face-centred cubic. Below
417C 783F: Hexagonal close packed, 8.8 g/ cm
3
, 1495C 2723F.
Comments on Material: Cobalt is a metal with characteristics close to iron and
nickel; it is tough and the machinability is relatively low. Cobalt is very magnetic
and used for magnets and for alloying element to improve strength. For super
alloys based on cobalt, see Material/Preparation Tables 48. For cobalt in cemented
carbides, see Material/Preparation Tables 67.
Pure cobalt being tough and with a tendency to cold work and deformation is
relatively difcult to prepare. Cobalt alloys are less difcult. Preparation is similar
to the refractory metals see Material/Preparation Tables 55.
Sectioning: Wet abrasive cutting is done with an SiC bakelite bond cut-off wheel.
A thin and relatively soft wheel is recommended to secure a cut with the lowest
deformation possible.
Mounting: Hot mounting and cold mounting can be used.
Grinding: Due to the toughness of cobalt the SiC grinding papers shall not be
used for too long of a time to avoid smeared layers.
Polishing: It is important that the rough polishing step has removed the
deformation from the grinding. If this cannot be obtained with the 3 m step, a
6 m step is used see below. Electrolytic polishing can be recommended.
Etching: See below.
Case or coating thickness/
hardness, surface layers
B 487 C-47
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-47, T-47,
El-12
E 562, E 1245, E 1382 C-47, T-47
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
C-47, T-47,
El-12
E 1181, E 1245, E 1351,
E 1382, E 1558
C-47, T-47,
El-12
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
Polishing
C-47: The step P 1 from Method T-47 can be used between the FG 1 step and the
P 1 step see above.
C-47: P 2: Often this step can be omitted.
T-47: The method can be expanded with P 3 from C-47.
Section 13.2.2.
Polishing
xed, res
RCD, hard Cloth,
napless,
hard,
wov, syn
Cloth, med
nap, soft,
syn
Cloth,
napless,
soft,
porous, syn
or susp
Dia, spr
or susp
Dia, spr
or susp
Alumina
Grit or Grain
Size m
P220 9 3 1 0.02/ 0.05
Lubricant
Type
Water Alco or
wat
Alco or
wat
Alco or wat
rpm/rpm
Force per
Specimen N lb
25 5.7 30 7 30 7 30 7 10 2.2
Time
Minutes
Until
plane
56 4 2
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
hard,
wov,
silk
Cloth
med.
nap,
soft,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Dia, spr
or susp
Grit or Grain
Size m
P220 P320 P500 P1200 6 3 1
Lubricant
Type
or
wat
Alco
or
wat
Alco
or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Comp Comp
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 15 3.4 25 5.7 30 7 30 7
Time
Minutes
Until
plane
0.51 0.51 0.51 45 4 2
Etchants
Pure Co 14, 15, 17 General structure
Hard-facing and tool metals 18, 19, 20 General structure
High temperature alloys 20, 18, 16, 21, 22b, 24, 25 General structure
19 Phase identication
Material: Cobalt-based super alloys
Material Properties: Cobalt: Above 417C 783F: Face-centered cubic. Below
417C 783F: Hexagonal close packed, 8.8 g/ cm
3
, 1495C 2723F.
Super alloys Co based: Heat-resistant casting alloys: 2032 % chromium, 713 %
tungsten, 111 % nickel and molybdenum, niobium, zirconium, titanium,
aluminum, tantalum, boron, silicon and manganese.
Wrought heat-resistant alloys: 115 % iron, 335 % nickel, 2030 % chrome, 710
% molybdenum, carbon, manganese, tungsten, niobium weight %.
Comments on Material: The cobalt-based super alloys are high-temperature
resistant materials. They are hard and tough, relatively easy to prepare. Stellite is a
special cobalt-based alloy with 4565 % Co, 2535 % Cr, and 520 % W. This alloy
is very wear resistant used only as casting alloy. It is hard and brittle. Cobalt is
also used in cemented carbides see Material/Preparation Tables 67.
Sectioning: Wet abrasive cutting is done with an SiC bakelite bond cut-off wheel.
Very often shearing or other more rough sectioning methods should be avoided, as
serious distortions and cold work could be introduced. Use only these methods for
sectioning of large pieces, later to be sectioned by wet cutting.
Mounting: Both hot mounting and cold mounting can be used. In case of edge
retention a hot mounting material like bakelite or epoxy with a ller should be
used.
Grinding: For the harder alloys, like stellite, Method C-48 should be preferred.
Polishing: For the nal step with alumina, the pH should be lowered to around 4.
Electrolytic polishing is recommended.
Case or coating
thickness/hardness
surface layers
B 487 C-48
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-48,
T-48
E-12
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-48,
T-48
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-48,
T-48
El-12
E 1245, E 1351, E 1382, E 1558
C-48,
T-48
El-12
T-48
Sectioning
Mounting
Hot Compression
Mounting
Resin Bakelite/
Epoxy
Cold Mounting Resin Acrylics
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
C-48: FG: Very often FG 1 can be changed to RCD, soft, and FG 2 and FG 3 can
be omitted.
Polishing
C-48 and T-48: The P 3 step: Use alumina with a pH around 4.
Contemporary Method C-48 for denitions of parameters and consumables see
Section 13.2.2.
Polishing
xed, res
RCD, hard RCD, soft RCD, soft Cloth, nap-
less, hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrashive
Type
Diamond Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or susp
Alumina
Grit or Grain
Size m
P220 9 6 3 3 0.02/ 0.05
Lubricant
Type
Water Alco
or wat
Alco
or wat
Alco
or wat
Alco
or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Force per
Specimen
Nlb
30 7 30 7 30 7 25 5.7 30 7 15 3.4
Time
Minutes
Until
plane
45 4 5 24 12
Traditional Method T-48 For denitions parameters and consumables see
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth
napless,
hard,
wov, silk
Cloth
napless,
hard,
wov,
syn
Cloth
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Alumina
Grit or Grain
Size m
P220 P320 P500 P1200 6 3 0.02/
0.05
Lubricant
Type
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 30 7 30 7 30 7 10 2.3
Time
Minutes
Until
plane
0.51 0.51 0.51 5 23 1
Etchants
See Material/Preparation Tables 47.
Material: Copper and copper alloys. Brass. Bronze. Other copper
alloys
Material Properties: Copper: Face-centered cubic, 8.93 g/ cm
3
, 1083C 1981F,
HRB 37.
-brass: Body-centered cubic, up to 38 % zinc.
--brass: Body-centered cubic, 38 to 47 % zinc.
Bronze: Up to 30 % tin
Comments on Material: Copper makes alloys with a high number of other
metals. In alloys improving the characteristics of pure copper, small amounts of
alloying elements like silver, cadmium, sulfur, tellurium, chromium, beryllium, and
cobalt are used. The alloys with zinc, brasses, are numerous, often with lead as a
further alloying element. In special brasses further elements like aluminum, tin
12 % manganese nickel and iron are used. Brass can be obtained as wrought
and cast alloys. The alloys with tin, bronzes are supplied as wrought bronzes with
up to 6 % tin and cast bronzes with up to 30 % tin Often zinc is added up to 2 %
and other elements like phosphorous and lead. Aluminum bronze is a group of
bronzes with 511 % aluminum, up to 6 % nickel, 6 % iron, and 2 % manganese.
Manganese bronze contains 515 % manganese. Copper-nickel alloys have a nickel
content of 4.545 % nickel with small amounts of iron and manganese.
Copper and copper alloys are specied in a number of systems by a number of
organizations. The most important are:
UNS System, Standard Designations for Copper and Copper Alloys, by Copper
Development Association CDA.
AMS System, Aerospace Material Specications, by Society of Automotive
Engineers SAE.
ASME System, by American Society of Mechanical Engineers ASME.
ASTM System by ASTM.
AWS System by American Welding Society AWS.
Ingot No System by Brass and Bronze Ingot Manufacturers.
Federal System and Military System.
SAE System by American Society of Mechanical Engineers ASME.
Metallographic examination is often used for the determination of grain size,
evaluation of the distribution of second phase, and control of heat treatment.
Copper alloys are soft and ductile, making them difcult to prepare without
deformation. Care should be taken to keep the deformation low at sectioning and
grinding and to remove deformation from previous steps. See also the Material/
Preparation Tables 50 covering the preparation of pure copper and copper bearing
alloys.
Sectioning: Wet abrasive cutting with an SiC bakelite bond cut-off wheel. Use an
efcient cooling to avoid recrystallization of cold-worked lean alloys. When using
shearing or band sawing, care should be taken that the strong deformation
developed is removed during the plane grinding.
Mounting: Hot and cold mounting can be used.
Grinding: Sectioning and the rough grinding steps introduce deep deformation so
it is important to remove this during the ner grinding steps.
Polishing: It can be very difcult to remove the last deformation and obtain a
scratch-free surface with mechanical polishing. Using chemical mechanical
polishing at the last polishing step is an efcient way to obtain a correct surface
see below. Electrolytic polishing gives very good results with a number of brasses
and bronzes.
Etching: See below.
Case or coating
thickness/hardness,
surface layers
B 487 C-49
Grain size,
grain boundaries
E 112, E 930,
E 1181, E 1382
C-49, T 49,
El-13
Brass, El-
14 Bronze
Image analysis,
rating of inclusion
content
E 562, E 1245,
E 1382
C-49, T-49
High planeness
Microhardness, hardness E 10, E 18, E 92, E 103, E 110, E 140,
E 384, E 448
C-49, T-49
E 1351, E 1382, E 1558
C-49, T-49,
El-13
Brass, El
14 Bronze
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
Attention: In C-method, when using RCD: The disk turns concave during use.
Polishing
C-49 and T-49: For Cu and Cu-alloys a chemical mechanical polishing can be
obtained in the last polishing step by mixing 98 96 mL colloidal silica with
1 mL 2 mL H
2
O
2
30 % and 1 mL 2 mL ammonia solution 25 %.
Electrolytic polishing: Brass: El-13. Bronze: El-14
Section 13.2.2.
Polishing
napless,
hard, wov,
syn
Cloth,
napless,
soft,
porous,
syn
or susp
Dia, spr
or susp
Silica
See note
Grit or Grain
Size m
P220 9 3 0.04/ 0.05
Lubricant Type Water Alco or wat Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or Contra Comp Comp Contra
Force per
Specimen N lb
25 5.7 30 7 25 5.5 15 3.3
Time
Minutes
Until plane 4 4 23
Section 13.2.2.
Grinding/ PG FG 1 FG 2 FG 3 FG 4 FG 5 P 1 P 3
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
med
hard,
wov,
wool
Cloth
nap-
less,
soft,
por-
ous,
syn
Abrasive
Type
SiC SiC SiC SiC SiC SiC Dia,
spr
or
susp
Silica
See
note
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 P4000 3 0.04
/ 0.05
Lubricant
Type
Water Water Water Water Water Water Wat-oil
Rotation
Disk/
Holder
300
/ 150
300
/ 150
300
/ 150
150
/ 150
150
/ 150
150
/ 150
150
/ 150
150
/ 150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 20 4.5 25
55.7
10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 0.51 3 1
Etchants
Cu-Al aluminum,
bronze
44, 31d, 34 b, 35, 36,
37, 38, 39, 40, 45, 215
General structure
Cu-Be 46, 41, 45 General structure
Cu-Cr 41 General structure
Cu-Mn 41 General structure
Cu-Ni 34, 47, 48, 40, 49, 50 General structure
Cu-Si 41 General structure
Cu-Sn tin
bronze
51, 52 General structure
Admirality metal 8b General structure
Gilding metal,
cartridge metal,
free
cutting brass,
nickel silver
31d, 32, 33, 41, 42, 49 General structure
Cu alloys 26, 27, 28, 29, 30, 44,
41, 31d, 32,
33, 34b, 35, 36, 37, 38,
39, 210, 215
General structure
53, 43, 28, 49 Chemical polish
and etch
42, 49, 210 Darkens beta in
alpha-beta brass
54 Etching of cold
worked brass
Material: Pure copper. Copper-bearing alloys
Material Properties: Copper: Face-centered cubic, 8.93 g/ cm
3
, 1083C 1981F,
HRB 37.
Copper bearing alloys: 3.525 % lead, 3.511 % tin, 0.54 % zinc, small additions
of antimony, nickel and iron weight %.
Comments on Material: Commercially pure copper, 99.999.99 %, can be
obtained as oxygen-free electronic copper and as tough pitch copper containing
very small amounts of oxide. Copper bearing alloys have high contents of lead and
tin, as mentioned above.
Pure copper is very ductile and soft making the preparation difcult. Copper
bearing materials, having the very soft phases of lead and tin is difcult to prepare
without smearing of these phases. The methods described in Material/Preparation
Tables 49 can also be used for pure copper. For further information see Material/
Sectioning: Wet abrasive cutting with an SiC bakelite bond cut-off wheel. When
using shearing or band sawing, care should be taken that the strong deformation
developed is removed during the plane grinding.
Grinding: Sectioning and the rough grinding steps introduce deep deformation so
it is important to remove this during the ner grinding steps.
Polishing: It is important that the deformation developed during the grinding is
removed after the step with 9 m or 6 m. For pure copper it can be very difcult
to remove the last deformation and obtain a scratch- free surface with mechanical
polishing. Using chemical mechanical polishing at the last polishing step is an
efcient way to obtain a correct surface see below. Electrolytic polishing gives
good results with pure copper using Method El-13. Electrolytic polishing of
bearing alloys can be done with Method El-14 if the amount of phases is not too
high.
Etching: Etching can take place between preparation steps to remove deformation
see below. See etchants below.
Case or coating
thickness/hardness,
surface layers
B 487 C-50
Perfect edge
retention
Grain size,
grain boundaries
E 112, E 930,
E 1181, E 1382
C-50, T-50,
El-13 Pure
copper, El-14
Bearing
alloys
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-50, T-50
High planeness
E 140, E 384, E 448
C-50, T-50
E 1245, E 1351, E 1382, E 1558
C-50, T-50,
El-13 Pure
copper, El-14
Bearing
alloys
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
T-50: FG 4: This step can often be omitted.
Polishing
C-50 and T-50: To remove deformation after the last FG step etch with 100 mL
water mixed with 100 mL ethanol and 10 g iron III nitrate before the P 1 step.
C-50 and T-50: For Cu and Cu alloys a chemical mechanical polishing can be
obtained in the last polishing step by mixing 98 96 mL colloidal silica with
1 mL 2 mL H
2
O
2
30 % and 1 mL 2 mL ammonia solution 25 %. An
alternative is adding a few drops of the nitrate etchant mentioned above to the
colloidal silica during the polishing.
Electrolytic polishing: Pure copper: El-13. Copper bearing alloys: El-14.
Section 13.2.2.
Polishing
napless,
med hard,
wov, wool
Cloth, nap-
less, soft,
porous,
syn
susp
Dia, spr or
susp
Silica
See note
Grit or Grain
Size m
P220 P320 9 3 0.04/ 0.05
Lubricant Type Water Water Alco or wat Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per Specimen
N lb
20 4.4 20 4.4 30 7 2.5 5.7 15 3.3
Time
Minutes
Until plane 0.51 34 5 12
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
med
hard,
wov,
wool
Cloth,
nap-
less,
soft,
por-
ous,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Silica
See
note
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 6 3 0.04/
0.05
Lubricant
Type
Rotation
Disk/
Holder
300/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Comp
or
contra
Comp
or
contra
Force per
Specimen
N lb
20
4.5
20
4.5
20
4.5
20
4.5
20
4.5
25
5.7
25
5.7
15
3.3
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 34 34 1
Etchants
Material Etchants
see Table 12.2
Uses
Pure Cu 26, 27, 28, 29,
30, 31d, 32, 33,
34b, 35, 36, 37,
38, 39, 40, 41,
42, 8b, 210, 215
General structure
43, 28 Chemical polish and etch
Material: Pure gold. Au alloys
Material Properties: Body-centered cubic, 19.3 g/ cm
3
, 1063C 1945F
Comments on Material: Gold belongs to the precious metals which include the
platinum-group metals see Material/Preparation Tables 57, gold and silver, Pure
gold, 99.99 % is seldomly used, most often gold is alloyed with silver, copper,
nickel, or the platin-metals. Gold is the most ductile metal; it can be rolled to a
thickness of 1/ 12 000 mm. Gold is used for jewelry and has a number of industrial
applications. Often gold is used as a coating on other materials, and for electronic
parts gold is used as coatings for certain components see Section 7.10.3 and
Material/Preparation Tables 22 and 26. Pure gold, being very soft and ductile, is
very difcult to prepare; deformation and smearing are difcult to avoid. Also,
there is a risk of embedded abrasive grains in the specimen surface. Some alloys
are harder and therefore easier to prepare.
Sectioning: Because of the high price of gold, the wet abrasive cutting should be
with a thin cut-off wheel to reduce the kerf loss. Cutting is best done on a
precision cut-off machine using SiC bakelite bond cut-off wheels 0.5 mm 0.02 in
thick and with an efcient cooling. In the case of examinations of coatings, the
cutting should be done correctly see Material/Preparation Tables 0810. Also, it
can be of advantage to mount the specimen in epoxy before cutting to stabilize the
coating see below. If using shearing, the strong deformation of the edge should
be taken care of when plane grinding the specimen.
Mounting: Hot and cold mounting can be used. Very often coatings should be
examined and the correct hot mounting material, with a ller, should be used.
Also, cold mounting with epoxy may be satisfactory see Sections 3.1.3 and 3.11.
Grinding: If following a proper cutting, grit P220 grinding paper should be
avoided, starting with grit P320. To reduce the induction of deformation in the
material, the grinding paper can be covered with a thin layer of wax, or the paper
can be worn-in with a hard specimen for a few seconds. It is important that all
deformation from the previous step is removed. In the case of embedded SiC
grains in the specimen surface, use Method C-51. To avoid embedded abrasive
grains see Section 13.6.4, a softer grinding/polishing surface should be used. In
the case of embedded grains the FG 2 step of Method C-51 can be changed to a
hard, nonwoven, synthetic cloth. Also diamond paste, xing the grains in the cloth,
can be used. As an alternative to C-51, Method C-58 for silver can be used. For the
softest materials, Method C-51 should be used.
Polishing: For pure gold and alloys with a high gold content chemical mechanical
polishing can be used for the last polishing step see below.
Etching: See etchants below.
Case or coating
thickness/hardness,
surface layers
B 487 C51
Grain size, grain
boundaries
E 112, E 930, E 1181, E 1382 C-51,
T-51
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-51,
T-51
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-51,
T-51
E 1245, E 1351, E 1382, E 1558
C-51,
T-51
T-51
Sectioning
Cut-Off Wheel SiC, bakelite bond, 0.5 mm 0.02 in thick
Mounting
Hot Compression
Mounting
Resin Bakelite/Bakelite
with a Filler
Cold
Mounting
Resin Acrylics/
Epoxy
Time
Minutes
89 Time
Minutes/
Hours
610 min/
68 h
Grinding
C-51: The step FG 2 can be changed to a hard, nonwoven, synthetic cloth if
embedded abrasive grains are a problem using the RCD.
Polishing
C-51 and T-51: Both methods can be nished with chemical mechanical
polishing: Step P 3 in C-51 with alumina 0.05 m added a few drops of etchant
62: 15 g CrO
3
, 100 mL HCl see Etchants below.
C-51: For certain alloys the step P 1 can be changed to 3 m diamond, followed
by P 2 from Method T- 51 for 28 min so that P 2 and P 3 are omitted.
T-51: Can be nished with P 3 from C-51.
T-51: Steps FG 3 and FG 4 can be changed to P 1 from C-51. In some cases P 1
can be omitted, and P 2 changed to 1 m diamond.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper RCD,
soft
Cloth,
napless,
hard,
wov, silk
Cloth, nap-
less, med
soft,
wov, wool
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC Dia,
spr or
susp
Dia,
spr or
susp
Dia,
spr or
susp
Alumina
see note
Grit or Grain
Size m
P220 P320 9 6 3 0.02/ 0.05
Lubricant
Type
Water Water Alco or
wat
Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
20 4.5 20 4.5 25 5.7 20 4.5 20 4.5 10 2.3
Time
Minutes
Until
plane
0.51 5 5 3 1
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
med
nap,
soft,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Grit or Grain
Size m
320 500 1000 2400 4000 3 0.25
Lubricant
Type
Water Water Water Water Water Wat-
oil
Wat-
oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
contra
Force per
Specimen
N lb
20
4.5
20
4.5
20
4.5
20
4.5
20
4.5
20 4.5 15
3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 1 4 28
Etchants
Pure Au 61, 62 General structure
63 Chemical polish and etch
Au alloys 64b, 62 General structure
90 % noble metals 61 General structure
Material: Pure lead. Pb alloys. Pb bearing alloys
Material Properties: Lead: Face-centered cubic, 11.34 g/ cm
3
, 327C 621F, HV
2540.
Lead bearing alloys: 0.911.0 % tin, 316 % antimony, 0.10.7 % copper, arsenic,
bismuth, zinc, aluminum, cadmium weight %.
Comments on Material: Lead is a very soft and ductile metal with a low melting
point and a recrystallization temperature around 20C 68F. Lead and most lead
alloys are toxic both when inhaled and ingested. Pure lead is difcult to prepare,
whereas bearing alloys are less difcult. After cold working lead rapidly
recrystallizes. The cold work developed during sectioning and grinding should be
kept at a minimum to avoid development of a pseudostructure through
recrystallization. Also, abrasive grains are easily embedded in the specimen
surface.
No contemporary C-method for lead is available. C-52 describes a method
based on etching between steps. T-52 is a normal traditional method. Method
C-52 with etching between steps is recommended for pure lead.
Sectioning: Abrasive wet cutting of pure lead and lead alloys can be done with a
thin SiC bakelite cut-off wheel, preferably on a precision cutting machine. Also, a
toothed cut-off wheel can be used. Pure lead also can be cut by using a sharp knife
or a band saw or hand saw with ne teeth. If a microtome is available, very good
surfaces can be obtained so that grinding is not needed see Section 2.7.6. In the
case of examination of corrosion products batteries, the specimen should be
impregnated before sectioning see Section 3.10.
Mounting: As a rule pure lead and lead alloys should not be hot compression
mounted, both because of the low recrystallization temperature and because of
voids and pores in the alloys that possibly may collapse under the high pressure of
hot mounting. To obtain the lowest possible temperature during cold mounting,
epoxy should be used see Section 3.8.3.
Grinding: To minimize the risk of embedded SiC grains in the specimen surface,
the grinding paper can be treated with wax and a low pressure is used. Also
parafn can be used instead of water. In both cases an abundant ow of liquid
should be used to secure the removal of loose grains. In Method C-52 the
specimen is etched after the last grinding step FG 2 to remove deformation from
grinding see below.
Polishing: It is important that the deformation from the grinding is removed
during the rough polishing step. For pure lead chemical mechanical polishing is
recommended for the last polishing step see Method C-52 below. Lead and some
lead alloys are suited for electrolytical polishing.
Etching: See below.
Case or coating
thickness/hardness,
surface layers
B 487 C-52, T-52
Grain size, grain boundaries E 112, E 930, E 1181, E 1382 C-52, T-52, El-15
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-52, T-52
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-52, T-52
E 1245, E 1351, E 1382, E 1558
C-52, T-52,
El-15
Sectioning
Cut-Off Wheel SiC bakelite bond cut-off wheel, 0.5 mm 0.02 in
thick, low speed, very careful, see also above.
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Acrylics/epoxy w.
lowest possible
peak temp.
Time
Minutes
Time
Minutes/Hours
68 min/ 1224 h
Grinding
T-52: PG, FG 1 and FG 2: Charge SiC papers with wax or use parafn instead of
water.
C-52: Instead of water, parafn is used for SiC steps.
C-52: After FG 2 the specimen is etched in Solution 1: 15 mL acetic acid, 15 mL
nitric acid 65 %, 60 mL glycerol. Do not store, use fresh solution at 80C
176F. The solution is etchant 113 below.
See also alternative below.
C-52: As an alternative to Solution 1, Solution 2 can be used: 100 mL hydrogen
peroxide 30 % mixed with 139 mL ammonia 25 %.
Polishing
C-52 and T-52: For pure lead use chemical mechanical polishing with last step,
P 3: Solution 3: 84 mL glycerol, 8 mL acetic acid 96 %, 8 mL ammonia 25 %.
10 mL of Solution 3 is added to 90 mL colloidal silica. Also a mixture of 90 mL
silica and 10 mL hydrogen peroxide 30 % can be used. A third possibility is
adding a few drops of ammonium tartrate to the silica.
T-52: P 2: This step can often be omitted.
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
med.
nap,
soft,
syn
Cloth,
napless,
soft,
porous,
syn
or susp
Dia, spr
or susp
Silica,
see note
Grit or Grain
Size m
P320 P500 P1200 P2400 3 1 0.04/ 0.05
Lubricant
Type
Parafn Parafn Parafn Parafn Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
Nlb
15
3.4
15
3.4
15
3.4
15
3.4
20 4.5 15 3.4 10 2.2
Time
Minutes
0.51 0.51 0.51 0.51 34 3 12
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
med hard,
wov, wool
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC Dia,
spr or
susp
Dia,
spr or
susp
Silica
Grit or Grain
Size m
320 500 1200 9 3 0.04/ 0.05
Lubricant
Type
Water Water Water Alco or wat Wat-oil
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
1020
2.24.5
1020
2.24.5
1020
2.24.5
1520
3.44.5
1520
3.44.5
10
2.2
Time
Minutes
Until
plane
0.51 0.51 45 3 2
Etchants
Material Etchants
see Table 12.2
Uses
Pure Pb 57, 112 General structure
Pure Pb, Pb+ 2Sb, Pb+ 2Sb,
Pb+Ca
113 For alternate polishing
and etching
Pb+ 2Sb 114, 115, 57, 74b General structure
Pb+ 2Sb 114, 57, 74b General structure
Pb+Ca 112 General structure
Pb alloys 116, 117b General structure
Babbitt 74b General structure
Material: Pure magnesium and Mg alloys
Material Properties: Magnesium: Hexagonal close-packed, 1.74 g/ cm
3
, 650C
1202F, HBB 35.
Magnesium alloys: 1.210 % aluminum, 0.151.5 % manganese, 0.23.0 % rare
earths, 1.83.0 % thorium, 0.55.7 % zinc, 0.60.7 % zirconium weight %.
Comments on Material: Magnesium is the light metal with the lowest specic
gravity in practical use. Pure magnesium is rarely used because of the low
strength, but in form of alloys based on the ve alloying elements mentioned
above. Magnesium alloys are normally available as low-pressure casting alloys,
high-pressure casting alloys, and wrought alloys. Magnesium alloys are not
universally classied, but in ASTM Practice for Temper Designation of
Magnesium Alloys, Cast and Wrought B 296 a designation is stated.
Magnesium is soft and will easily cold-work making it difcult to prepare. As the
dust from grinding may ignite, all sectioning and grinding should be with a
cooling uid. Pure magnesium and many alloys are sensitive to water.
The preparation of Mg cast and wrought alloys vary considerably, and therefore a
number of suggestions are stated below. For harder alloys use Method C-53.
Sectioning: At examination of die castings it should be recognized that the
microstructure varies strongly through the casting. This should be considered
when selecting the sample. Wet abrasive cutting with an SiC cut-off wheel. Care
should be taken to avoid excessive deformation of the cut surface and the xing of
the work piece should be as gentle as possible. As mentioned above the
magnesium swarf/dust may ignite and even development of hydrogen may take
place at the contact with water, and special precautions should be made. If cutting
with a shear or a band saw, at least 1 mm of the cut surface should be removed
during the plane-grinding step.
Mounting: The pressure that is needed for hot mounting may cause cold-work in
the specimen, and cold mounting should be preferred. In case of heat-sensitive
alloys only epoxy should be used for cold mounting, keeping the peak temperature
low see Section 3.8.3.
Grinding: The plane grinding should be performed with the nest possible grit. If
the sectioned surface is not very rough, the rst grinding step can be with grit
P320 or P500 as deep deformations are very difcult to remove at the later steps.
For water-sensitive materials use a mixture of glycerol and ethanol, 1:3, instead of
water, or pure ethanol for the ner grits. In case of embedded SiC particles in the
specimen surface, charge the surface of the grinding paper with wax.
Polishing: For most materials water should be totally avoided for polishing.
Ultrasonic cleaning in ethanol between polishing steps is recommended. During
the polishing a relief may develop between the matrix and hard particles; to avoid
this use Method C-53. Also this method should give the smallest amount of
embedded abrasive grains in the specimen surface. By the nal cleaning, water
should be avoided for most alloys. Use soap and ethanol, and avoid using cotton
after the last polishing step because new scratches may be introduced.
Pure magnesium and most alloys can be electrolytically polished.
Etching: Magnesium having a hexagonal close-packed crystal structure can be
examined in polarized light. For enchants, see below.
Case or coating
thickness/hardness,
surface layers
B 487 C-53
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-53, T-53,
El-16
Image analysis,
rating of inclusion content
E 562, E 1245, E 1382 C-53, T-53
High planeness
E 140, E 384, E 448
C-53, T-53
E 1351, E 1382, E 1558
C-53, T-53,
El-16
Sectioning
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Acrylics
Time
Minutes
Time
Minutes/Hours
6/ 10 min
Grinding
C-53 and T-53: If the material is very water sensitive use ethanol or a mixture
1:3 of glycerol and ethanol instead of water.
C-53: FG 1: For water-sensitive materials use water-free lubricant.
Polishing
Cleaning: For most alloys cleaning between polishing steps should be done
without water.
C-53 and T-53: If the specimen material is sensitive to water use water-free
polishing media and lubricants.
C-53 and T-53: The nal cleaning can be done on a rotating polishing cloth, med
nap, soft, syn, only with ethanol.
C-53: P 3: This step can be changed to step P 2 in Method T-53, only with 1 m
diamond in 2 min.
C-53: Polishing step, P 3: Mix silica 1:1 with ethanol.
T-53: P 1: This step can be changed to a step like FG 3 with SiC paper grit 2400.
T-53: P 2: The cloth can be changed to napless, med hard, wov, wool.
T-53: P 3: For pure Mg: Use same data as P 2 except grain size: 1 m.
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
RCD,
soft
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
med hard,
wov, wool
Cloth,
napless, soft,
porous, syn
Abrasive
Type
SiC Dia, spr or
susp
Dia, spr or
susp
Dia, spr or
susp
Silica, see
above
Grit or Grain
Size m
P500 9 6 3 0.04/ 0.05
Lubricant
Type
Water Alco or wat Alco or wat Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
2030 4.57 2030
4.5 7
30 7 15 3.3 10 2.2
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
med.
nap
soft, syn
Cloth,
napless,
soft,
porous,
syn
or susp
Dia, spr
or susp
Silica
Grit or
Grain Size
220 320 500 1200 15 3 0.04/ 0.05
Lubricant
Type
oil
Alco or
oil
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
2030
4.57
2030
4.57
2030
4.57
1020
2.34.5
30 7 25 5.7 15 3.4
Time
Minutes
Until
plane
0.51 0.51 12 34 34 0.51
Etchants
Pure Mg 118, 119, 74a,
120, 121, 122
General structure
123 Stainfree polish-etch
Mg-Mn 119, 74a, 124, 122 General structure
Mg-Al, Mg-Al-Zn
Al +Zn5 %
118, 119, 74a, 125,
124, 123, 122
General structure
120, 125, 126, 127 Phase identication
124, 126, 127 Grain structure
Mg-Al, Mg-Al-Zn
Al +Zn5 %
118, 119, 74a, 125,
124, 121, 122
General structure
120, 125, 126, 127 Phase identication
Mg-Zn-Zr and Mg-Zn-Th-Zr 118, 119, 74a, 1d, 128,
124, 126, 127, 121, 122
General structure
120, 121 Phase identication
Mg-Th-Zr 118, 119, 74a, 1d, 124,
127, 121, 122
General structure
Mg-rare earth-Zr 120, 121 Phase identication
Material: Pure manganese. Mn alloys
Material Properties: Manganese: Body-centered cubic or body-centered
tetragonal, 7.2 g/ cm
3
, 1260C 2300F, HRC 35.
Comments on Material: Manganese is a metal resembling iron, but it is harder
and very brittle. It is primarily used as an alloying element, examples are with
steel, where 0.22 % manganese is used, brass with up to 3 % and bronze with
515 % Mn.
Pure manganese and alloys with high manganese content are not difcult to
prepare. In the case of most alloys, the Material/Preparation Tables covering the
base metal should be followed.
Sectioning: Wet abrasive cutting with an Al
2
O
3
bakelite bond cut-off wheel.
Grinding: No special precautions are needed.
Polishing: Pure manganese and some alloys can be electrolytically polished.
Etching: See below.
Case or coating
thickness/hardness,
surface layers
B 487 C-54
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-54, T-54,
El-01
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-54, T-54
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-54, T-54
E 1181, E 1245, E 1351,
1382, E 1558
C-54, T-54,
El-01
Sectioning
Cut-Off Wheel Al
2
O
3
, bakelite bond
Mounting
Hot Compression
Mounting
Time
Minutes
810 Time
Minutes/Hours
610 min
Grinding
C-54: PG: For pure Mn use SiC paper grit P220.
Section 13.2.2.
Polishing
xed, res
RCD, hard Cloth, napless,
hard, wov, syn
Cloth, napless,
soft, porous, syn
Abrasive Type Diamond Dia, spr or susp Dia, spr or
susp
Alumina
Grit or Grain
Size m
P220 6 3 0.02/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or contra Comp Comp Contra
Force per
Specimen
N lb
30 7 40 9 30 7 15 3.4
Time
Minutes
Until plane 4 4 2
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC SiC Dia, spr or
susp
Alumina
Grit or Grain
Size m
P220 P320 P500 P1200 3 0.02/ 0.05
Lubricant Type Water Water Water Water Alco or wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Contra
Force per
Specimen
Nlb
35 8 35 8 35 8 35 8 35 8 15 3.7
Time
Minutes
Until
plane
0.51 0.51 0.51 4 12
Etchants
Mn-Fe, Mn-Ni,
Mn Cu, Mn alloys
Pure Mn, Mn-Cu,
and small additions
of Ni, Cu, Fe, Ge
Material: Pure molybdenum. Mo alloys. Pure
niobiumColumbium. Nb Cb alloys. Pure rhenium. Re alloys.
Pure tantalum. Ta alloys. Pure tungsten. W alloys. Pure
vanadium. V alloys
Material Properties: Molybdenum: Body-centered cubic, 10.2 g/ cm
3
, 2620C
4748F, HV 200.
Niobium Columbium: Rhombohedral, 8.4 g/ cm
3
, 1950C 3542F.
Rhenium: Hexagonal close packed, 20.53 g/ cm
3
, 3000 C 5432F, HK 200.
Tantalum: Body-centered cubic, 16.6 g/ cm
3
, 2996C 5425F, HV 110.
Tungsten: Body-centered cubic, 19.3 g/ cm
3
, 3410C 6170F, HV 350.
Vanadium: Body-centered cubic, 5.96 g/ cm
3
, 1710 C 3110F, HB 72.
Comments on Material: Molybdenum, niobium, rhenium, tantalum, tungsten,
and vanadium all having high melting points belong to the refractory metals. They
are seldomly used pure but mostly as alloying elements. Pure niobium, rhenium,
tantalum, and vanadium are soft and ductile, difcult to prepare. Pure
molybdenum and tungsten are harder and more brittle. All metals have a low
machinability and this combined with development of deformation and cold-work
makes it difcult to obtain a true microstructure by mechanical polishing; often it
must be combined with chemical mechanical polishing.
Sectioning: Wet abrasive cutting can be made with a SiC bakelite bond cut-off
wheel. Due to the poor machinability and to minimize the deformation, a
relatively soft wheel, as thin as possible, should be used.
Mounting: Both hot and cold mounting can be used. In case of examination of
porosity, a vacuum impregnation with epoxy may be useful see Section 3.10. For
mounting of wires, see Section 3.12. Foils and wire samples should preferably be
cold mounted to avoid induction of deformation at hot compression mounting.
Grinding: Because of the poor machinability the SiC grinding papers should only
be used as long they are cutting efciently; if not, cold work and deformation will
develop. In case of alloys with hard nonmetallic precipitates, it may be of
advantage to use Method C-55 to avoid relief and pull-outs. Variation regarding
specic materials, see below.
Polishing: It is important that the deformations from grinding are removed during
the rough polishing step, and if needed this step must be prolonged. It can be
difcult to remove all deformation by mechanical polishing and often chemical
mechanical polishing can be an advantage see below. Also electrolytic polishing
can be recommended see below for methods covering the different metals.
Etching: See etchants below. Molybdenum may be electrolytically etched see
Method El-01.
Case or coating
thickness/hardness,
surface layers
B 487 C-55
Grain size,
grain boundaries
E 112, E 930,
E 1181, E 1382
C-55, T-55,
El-
methods,
see below
of inclusion
content
High planeness
E 562, E 1245,
E 1382
C-55, T-55
E 110, E 140, E 384,
E 448
C-55, T-55
E 1181, E 1245, E 1351,
E 1382, E 1558
C-55, T-55
El-
methods,
see below
Sectioning
Cut-Off Wheel SiC, bakelite bond, a thin wheel
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
Niobium: T-55: An extra step with P4000 SiC paper can be added after FG 4.
Rhenium: Method C-55 can be recommended.
Tantalum and other very soft metals: C-55: A grinding step with P320 SiC
paper can be used between PG and FG 1 steps.
Polishing
Tungsten: C-55, T-55: The polishing step P 1 may be prolonged.
Molybdenum: C-55 and T-55: To remove deformed layers, the P 2 step can be
used with 0.05 m alumina dispersed in a small amount of a 30 % K
3
Fe CN
6
aqueous solution.
Molybdenum, niobium, tantalum, tungsten: C-55, T-55: To remove deformed
layers, the P 2 step can be used with colloidal silica 95 mL added 5 mL of a 20
% aqueous solution of chromium VI oxide 20 g CrO
3
in 100 mL distilled
water.
Molybdenum: C-55 and T-55: For last step mix 96 mL of colloidal silica with
2 mL of ammonia 25 % and 2 mL of hydrogen peroxide 30 %.
Niobium, pure vanadium: C-55, T-55: The last polishing step can be done as
chemical mechanical polishing: Mix 80 mL of colloidal silica with 20 mL of
hydrogen peroxide 30 %.
Tungsten, vanadium: C-55 and T-55: For last step mix 95 mL of colloidal silica
with 5 mL of hydrogen peroxide 30 %.
Rhenium: C-55, T-55: The last polishing step can be done as chemical
mechanical polishing: 15 g potassium ferricyanide K
3
FeCN
6
, 2 g sodium
hydroxide NaOH, 100 mL distilled water and equal part of silica.
Electropolishing: Molybdenum: El-01, Vanadium: El-22, Tungsten: El-21
Section 13.2.2.
Polishing
xed, res
RCD, soft Cloth,
napless,
hard, wov,
silk
Cloth, nap-
less, soft,
porous, syn
or susp
Dia, spr
or susp
Silica,
see above
Grit or Grain
Size m
P220 9 3 0.04/ 0.05
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
Contra
Comp Comp Contra
Force per
Specimen
N lb
2030
4.57
2030
4.57
30 7 1015
2.33.4
Time
Minutes
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Silica,
see
above
Grit or Grain
Size m
P220 P320 P500 P1200 P2400 3 0.04/ 0.05
Lubricant
Type
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/contra Comp or
contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
2030
4.57
2030
4.57
2030
4.57
2030
4.57
2030
4.57
20 4.5 20 4.5
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 35 25
Etchants
Mo base 98c, 129, 130, 131 General structure
As cast 132 a Chemical polish prior to etching
Nb and Nb
alloys
129, 66, 158, 159, 160, 161,
162, 163
General structure
164, 129, 160 Grain boundaries
Re base 13b, 98c, 132b, 170a General structure
Pure Ta 177 General structure
Ta alloys 159, 66, 178, 163, 161, 179 General structure
164 Grain boundaries and inclusions
158 Grain boundariesretains carbide
precipitate
Pure W 98c, 131 General structure
As cast 132a Chemical polish prior to etching
W-Th 209 General structure
Pure V 170b, 165b General structure
V alloys 199, 198 General structure
Material: Pure nickel. Ni alloys. Ni Based super-alloys
Material Properties: Nickel: Face-centered cubic, 8.89 g/ cm
3
, 1452C 2646F.
Nickel-copper alloys: 2834 % copper, 1 % manganese, 1 % iron, carbon,
aluminum.
Nickel-iron alloys: 0.1 % carbon, 0.2 % manganese, 0.2 % iron.
Super alloys nickel based: Heat resistant casting alloys: 815 % chromium, 228
% molybdenum 0.52 % niobium, 0.84.7 % titanium, 0.56 % aluminum, 118.5
% iron, 0.110 % tungsten, 0.31 % tantalum, 2.518.5 % cobalt, carbon,
zirconium, boron.
Wrought heat resistant alloys: 18 % iron, 219 % cobalt, 550 % chromium, 0.45
% titanium, 325 % molybdenum, carbon, tungsten, niobium, aluminum,
zirconium, boron, tantalum weight %.
Comments on Material: Pure nickel and nickel-copper alloys are mostly used for
the good resistance to corrosion, also for this purpose nickel is used for coatings.
Nickel being somewhat magnetic, it makes special magnetic alloys with iron. The
superalloys are very heat resistant.
Nickel is a metal with characteristics close to iron and cobalt; it is tough and the
machinability is relatively low. Pure nickel being tough and with a tendency to
cold-work and deformation is relatively difcult to prepare. Nickel alloys are less
difcult.
Sectioning: Wet abrasive cutting is done with an SiC bakelite bond cut-off wheel
with an efcient cooling. A thin and relatively soft wheel is recommended to
secure a cut with the lowest deformation possible. Very often shearing or other
more rough sectioning methods should be avoided, as serious distortions and
cold-work could be introduced. Use only these methods for sectioning of large
pieces later to be sectioned by wet cutting.
Mounting: Hot mounting and cold mounting can be used. In the case of
examination of nickel coatings, see Material/Preparation Tables 0810.
Grinding: Due to the toughness of nickel the SiC grinding papers shall not be
used for a too long time, to avoid smeared layers.
Polishing: It is important that the rough polishing step has removed the
deformation from the grinding. In case of pure nickel and soft alloys, it may be
necessary to add a silica step to the methods see below. Electrolytic polishing can
be recommended. Often a very short electrolytic polishing after mechanical
polishing will remove smeared material see Method El-17.
Etching: Nickel is relatively difcult to attack, strong solutions are needed see
etchants below.
Case of coating
thickness/hardness,
surface layers
B 487 C-56
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-56, T-56,
El-17
Image analysis,
rating of inclusion
content
High planeness
E 562, E 1245, E 1382 C-56, T-56
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-56, T-56,
El-17
E 1181, E 1245, E 1351, E 1382,
E 1558
C-56, T-56,
El-17
Sectioning
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
C-56: PG: For pure nickel and the most ductile alloys SiC paper grit P220/ 320
should be used.
Polishing
Pure Ni and Ni-Cu alloys: T-56: P 3 can be followed by or replaced by a step
with silica, see P 2 in Method C-56.
C-56: P 2: Alumina 0.02/ 0.05 m can be used instead of silica.
T-56: In some cases FG 3 can be omitted.
Section 13.2.2.
Polishing
xed, res
RCD, soft Cloth,
napless,
hard, wov,
syn
Cloth,
napless, soft,
porous,
syn
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P220 9 3 0.04/ 0.05
Rotation
Disk/Holder
300/ 300 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Contra
Force per
Specimen
Nlb
30 7 30 7 30 7 15 3.3
Time
Minutes
Until plane 46 45 2
Section 13.2.2.
Grinding/ PG FG1 FG 2 FG 3 FG 4 P 1 P 2 P 3
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
med
nap,
soft,
syn
Abrasive
Type
spr or
susp
Dia,
spr or
susp
Dia,
spr
or
susp
Grit or
Grain
Size m
P220 P320 P500 P1000 P1200 6 3 1
Lubricant
Type
or wat
Alco
or wat
Alco
or wat
Rotation
Disk/
Holder
300/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
rpm/
rpm
Comp/
Contra
Comp Comp Comp Comp Comp Comp Comp Comp
Force per
Specimen
N lb
25 5.7 25 5.7 25 5.7 25 5.7 25 5.7 30 7 30 7 20 4.5
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 4 3 12
Etchants
Pure Ni and
high Ni alloys
133, 134, 47, 135, 136, 25, 108, 31c General structure
137 Grain boundary suldation
Ni-Ag 38, 138, 50, 139 General structure
Ni-Al 50, 140, 141, 142, 89, 143 General structure
Ni-Cr 144, 50, 83, 134, 145,
98, 146, 147, 13a
General structure
Ni-Cu 38, 138, 50, 133, 140, 25,
134, 47, 48b, 94, 108, 34
General structure
Ni-Fe 50, 140, 141, 83, 134, 148, 40,
107, 149
General structure
74e, 25, 150 Orientation pitting
Ni-Mn 74e General structure
Ni-Mo 143 General structure
Ni-Ti 143, 151, 50, 133 General structure
Ni-Zn 152 General structure
Superalloys 94, 105, 138, 153, 12, 87, 89, 212,
226, 25, 94
General structure
Grain size
107, 111, 13a Reveals microstructural
inhomogneity
133 Grain boundary suldation
154 Fine precipitation structure
19b, 155, 156 Differential matrix and
nonmetallic staining
22a For passive alloys for
example, UNS Alloy N06625
157 Specic for UNS Alloys
N10004
107 Submicroscopic structure in
aged super alloys particularly
for electron microscopy
Stains the matrix when
precipitates are present
154 banding
18 Pre-etch activation for passive
specimens electrolytic etchant
213 Colors carbide and
Material: Pure palladium. Pd alloys. Pure platinum. Pt alloys.
Pure iridium. Ir alloys. Pure osmium. Os alloys. Pure rhodium. Rh
alloys. Pure ruthenium. Ru alloys
Material Properties: Palladium: Face-centered cubic, 12.16 g/ cm
3
, 1553C
2827F.
Platinum: Face-centered cubic, 21.37 g/ cm
3
, 1773.5C 3224F.
Iridium: Face-centered cubic, 22.42 g/ cm
3
, 2350C 4262F, HV 220.
Osmium: Hexagonal, 22.48 g/ cm
3
; 2700C 4892F.
Rhodium: Face-centered cubic, 12.5 g/ cm
3
, 1985C 3605 F, HV 122.
Ruthenium: Hexagonal, 12.2 g/ cm
3
, 2450C 4442F.
Comments on Material: The above-mentioned metals belong to the so-called
platinum metals that belong to the precious metals with gold and silver. Platinum
is used as base metal in a number of alloys used for jewelry and technical
purposes. The other metals are to a high degree used as pure or as alloying
elements in materials for the electronics, medical, and other industries.
Palladium and platinum are soft ductile metals, difcult to prepare because of
deformation and smearing. Iridium and rhodium, and especially the hexagonal
close-packed ruthenium and osmium are harder and less difcult to prepare.
Because of the high ductility, embedded abrasive grains in the specimen surface is
a risk see below.
No contemporary method is available for these metals, and C-57 is a variation of
T-57. In case of harder alloys the C-methods, C-51 se also Grinding below and
C-58 may be used.
Sectioning: Because of the high price of the platinum metals, the wet abrasive
cutting should be with a thin cut-off wheel to reduce the kerf loss. Cutting is best
done on a precision cut-off machine using SiC bakelite bond cut-off wheels
0.5 mm 0.02 in thick with efcient cooling. In the case of examinations of
coatings, the cutting should be done correctly see Material/Preparation Tables
0810. Also, it can be of advantage to mount the specimen in epoxy before cutting
to stabilize the coating see below. If using shearing, the strong deformation of
the edge should be taken care of when plane grinding the specimen.
Mounting: Hot and cold mounting can be used. If coatings should be examined
the correct hot mounting material, with a ller, should be used. Also cold
mounting with epoxy may be satisfactory see Sections 3.1.3 and 3.11.
avoided, starting with grit P320. It is important that all deformation from the
previous step is removed. Wax can be used to reduce the aggressiveness of the SiC
paper, or the paper can be dulled by grinding a hard material in 15 s before
use. In the case of embedded SiC grains in the specimen surface, use Method C-51
or C-58 to reduce the use of SiC grinding paper. To avoid embedded abrasive
grains see Section 13.6.4, a softer grinding/polishing surface should be used. In
the case of embedded grains the FG 2 step of Method C-51 or the FG 3 step of
C-58 can be changed to a hard, nonwoven, synthetic cloth. Also diamond paste can
be used to improve the xation of the diamond grains.
Polishing: Methods C-57 and T-57 both use diamond for the last polishing step.
For use of silica for the last step see Methods C-51 and C-58.
For chemical mechanical polishing etch-polishing of ruthenium and osmium
alloys see Etchants below.
Etching: See below.
Case or coating
thickness/hardness,
surface layers
B 487 C-57
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-57, T-57
Image analysis,
rating of inclusion
content
High planeness
E 562, E 1245, E 1382 C-57, T-57
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-57, T-57
E 1245, E 1351, E 1382, E 1558
C-57, T-57
Sectioning
Mounting
Hot Compression
Mounting
Resin Bakelite Cold
Mounting
Resin Acrylics/epoxy
Time
Minutes
89 Time
Minutes/Hours
610 min/ 68 h
Grinding
See above.
Polishing
C-57: For pure metals use wat-oil lubricant in P 1 and P 2.
T-57: P 2: This step can be changed to P 3 in C-57.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 FG 4 P 1 P 2 P 3
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
med
nap,
soft,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Dia,
spr
or
susp
Grit or
Grain
Size m
P220 P320 P500 P1200 P2400 6 1 0.25
Lubricant
Type
wat
Alco or
wat
Wat-oil
Rotation
Disk/
Holder
300/
150
300/
150
300/
150
150/
150
150/
150
150/
150
150/
150
150/
150
rpm/rpm
Comp/
Contra
Comp
or
contra
Conmp
or
contra
Force per
Specimen
N lb
1520
3.44.5
1520
3.44.5
1520
3.44.5
1520
3.4
4.5
1520
3.4
4.5
1520
3.44.5
15 3.4
4.5
1015
2.3
3.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 4 2 12
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 FG 4 P 1 P 2
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
med hard,
wov,
wool
Cloth,
med
nap,
soft, syn
or susp
Dia, spr
or susp
Grit or Grain
Size m
P320 P500 P1000 P2400 P4000 3 1
Lubricant Type Water Water Water Water Water Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
contra
Force per
Specimen
N lb
1520
3.4
4.5
1520
3.4
4.5
1520
3.4
4.5
1520
3.4
4.5
1520
3.4
4.5
1520
3.44.5
1015
2.33.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 4 2
Etchants
Pure Pd 61, 166, 62, 165a General structure
Pd alloys 166, 64a, 62, 165a General structure
90% noble metals 61 General structure
Pure Pt 64a, 73a General structure
167 Electrolytic polish and etch
Pt alloys 64b, 73a General structure
Pt-10 % Rh 168 General structure
Os base 165a General structure
165a Etch-polish for viewing grains
for polarized light
Rh base 171 General structure
Ru base 73b General structure
73b Etch-polish for viewing grains
for polarized light
Material: Silver. Ag alloys
Material Properties: Silver: Face-centered cubic, 10.5 g/ cm
3
, 961C 1762F, HV
25.
Comments on Material: Silver is used for jewelry and in the electronics and
chemical industries. Pure silver, like the other precious metals see Material/
Preparation Tables 51 and 52, is soft and ductile and therefore has a strong
tendency to deformation and smearing during the preparation. Also, abrasive
grains can be embedded in the specimen surface see Section 13.6.4. Silver alloys,
like Ag-Cu, Ag-Pd, and Ag solders are harder and therefore easier to prepare. Often
silver is used as a coating and if this coating should be examined the methods
stated in Material/Preparation Tables 0810 may be used.
Sectioning: Because of the relatively high price of silver, the wet abrasive cutting
should be with a thin cut-off wheel to reduce the kerf loss. Cutting is best done on
a precision cut-off machine using SiC bakelite bond cut-off wheels 0.5 mm
0.02 in thick with an effective cooling. In the case of examination of coatings, the
cutting should be done correctly see Material/Preparation Tables 0810. Also, it
can be of advantage to mount the specimen in epoxy before cutting to stabilize the
coating see below. If using shearing, the strong deformation of the edge should
be taken care of when plane grinding the specimen.
Mounting: Hot and cold mounting can be used. If coatings should be examined,
the correct hot mounting material,with a ller, should be used. Also, cold
mounting with epoxy may be satisfactory see Sections 3.1.3 and 3.11.
avoided, starting with grit P320. Wax can be used to reduce the aggressiveness of
the SiC paper, or the paper can be dulled by grinding a hard material in 15 s
before use. It is important that all deformation from the previous step is removed.
In the case of embedded SiC grains in the specimen surface, use Method C-58. To
avoid embedded abrasive grains see Section 13.6.4, a softer grinding/
polishing-surface should be used. For this reason the FG 3 step of Method C-58
can be changed to a hard, nonwoven, synthetic cloth and possibly the FG 2 step
can be omitted. Also diamond paste, xing the grains in the cloth, can be used. As
an alternative to C-58, Method C-51 for gold can be used.
Polishing: For pure silver and alloys with a high content of silver, chemical
mechanical polishing can be used for the last polishing step see below.
Electrolytic polishing can be used for pure silver and certain alloys.
Case or coating
thickness/hardness,
surface layers
B 487 C-58
Grain size, grain
boundaries
E 112, E 930, E 1181, E 1382 C-58, T-58,
El-18
of inclusion
content
E 562, E 1245, E 1382 C-58, T-58
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-58, T-58
E 1181, E 1245, E 1351, E 1382, E 1558
C-58, T-58,
El-18
El-18
Sectioning
Mounting
Hot Compression
Mounting
Resin Bakelite or
bakelite w. ller
Cold
Mounting
Resin Acrylics/
Epoxy
Time
Minutes
89 Time
Minutes/
Hours
610 min/
68 h
Grinding
See above.
Polishing
C-58: P 2: Chemical mechanical polishing of silver alloys can be done by adding
a solution of 25 mL distilled water, 25 mL ammonia solution 32 % and
1020 mL hydrogen peroxide 30 % to 1000 mL of colloidal silica.
C-58: P 2: This step can be changed to P 2 from Method T-58.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 P 1 P 2
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
RCD,
soft
Cloth,
napless,
hard, wov,
silk
Cloth,
napless,
soft,
porous, syn
Abrasive Type SiC SiC SiC Dia, spr
or susp
Dia, spr
or susp
Silica, see
note above
Grit/Grain
Size m
P220 P320 P500 9 3 0.04/ 0.05
wat
Wat-oil
Rotation Disk/Holder 300/ 150 300/ 150 150/150 150/150 150/150 150/150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Force per
Specimen N lb
20 4.5 20 4.5 20 4.5 25 5.7 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 5 5 1
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 FG 4 P 1 P 2
Disk/Cloth SiC
paper
SiC
paper
SiC paper SiC
paper
SiC
paper
Cloth,
napless,
med hard,
wov,
wool
Cloth,
med
nap,
soft,
syn
Abrasive
Type
or susp
Dia,
spr
or
susp
Grit or
Grain
Size m
320 500 1000 2400 4000 3 0.25
Lubricant
Type
Water Water Water Water Water Wat-oil Wat-
oil
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp
or
contra
Force per
Specimen
N lb
1520
3.44.5
1520
3.44.5
1520
3.44.5
1520
3.44.5
1520
3.44.5
1520
3.44.5
1015
2.33.4
Time
Minutes
Until
plane
0.5 0.5 0.5 1 4 2
Etchants
Pure Ag 172 173, 62 General structure
Ag alloys 65, 61, 174, 175, 62 General structure
Ag-Cu alloys 130 General structure
Ag-Pd alloys 173 General structure
Ag solders 173, 176 General structure
Material: Tin, Sn bearing alloys and other Sn alloys
Material Properties: Body-centered tetragonal 13.2C 56F, 7.29 g/ cm
3
,
232C 450F, HV 25.
Tin bearing alloys: 7 to 8 % antimony, 0.5 % lead, 3 to 4 % copper, iron, arsenic,
bismuth, zinc, aluminum.
Other tin alloys: Tin-lead, tin-copper, tin-zinc weight %.
Comments on Material: Pure tin is a soft metal, with a recrystallization
temperature close to room temperature. Pure tin is often used for coating to
obtain a reduced corrosion tinned steel plate and on electric parts to make
soldering easier. Tin-lead alloys are used for solders and tin-antimony alloys for
bearing materials.
Tin and tin alloys being soft and having a low recrystallization temperature makes
the preparation very difcult, and all steps in the preparation process must be
performed with great care. For the softest alloys use Method T-59.
Sectioning: Abrasive wet cutting of pure tin and tin alloys can be done with a thin
SiC bakelite cut-off wheel, preferably on a precision cutting machine with an
efcient cooling. Pure tin also can be cut by using a sharp knife or with a band
saw or hand saw with ne teeth. In the case of sawing the very deformed zone
must be carefully removed during grinding. For cutting of tinned steel plate, see
Mounting: As a rule pure tin and tin alloys should not be hot mounted, both
because of the low recrystallization temperature and because of voids and pores in
the alloys which possibly may collapse under the high pressure of hot mounting.
To obtain the lowest possible temperature during cold mounting, epoxy with a low
peak temperature should be used see Section 3.8.3. In the case of examination of
thin coatings see Material/Preparation Tables 0810.
Grinding: To minimize the risk of embedded SiC grains in the specimen surface,
the grinding paper can be treated with wax and a low pressure is used. For water
sensitive alloys parafn kerosene can be used instead of water.
Polishing: It is important that the deformation from the grinding is removed
during the rough polishing step. Chemical mechanical polishing can be used at the
last step see below. For pure tin and certain alloys, the specimen surface can be
cleaned by electrolytic shock-polishing, using Method El-19 in only 12 s. Tin
and some tin alloys are suited for electrolytical polishing.
Water sensitive alloys: use water-free lubricants and clean between steps without
water see below.
surface layers
B 487 C-59
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-59, T-59,
El-19
Image analysis,
rating of inclusion
content
E 562, E 1245, E 1382 C-59, T-59
High planeness
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-59, T-59
E 1245, E 1351, E 1382, E 1558
C-59, T-59,
El-19
El-19
Sectioning
Cut-Off Wheel SiC bakelite bond cut-off wheel, 0.5 mm 0.02 in
thick, low speed, very careful see also above
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Epoxy, lowest
possible peak
temp.
Time
Minutes
Time
Minutes/Hours
1224 h
Grinding
T-59: The cutting action of SiC papers P1000 and P1200 can be reduced by using
wax before grinding, or making the paper dull by rst grinding a hard material
in 10 s.
Polishing
C-59 and T-59: P 3: Mix 96 mL of colloidal silica with 2 mL ammonia 25 %
and 2 mL of hydrogen peroxide 30 %.
T-59: P 1: This step can be changed to a step like FG 4, only with SiC paper grit
P4000.
C-59 and T-59: To remove deformed layers and scratches, electrolytic polishing
in a short time, 12 s shock-polishing, can be recommended to follow the P 3
step see Method El-19.
Water sensitive alloys: C-59: The step P 1 can be omitted and the step P 3 is
changed to a diamond step like P 2 in Method T-57 using a water-free lubricant.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 P 1 P 2 P 3
Disk/Cloth SiC
paper
RCD,
soft
Cloth,
napless,
hard, wov,
silk
Cloth, nap-
less, med
hard, wov,
wool
Cloth, napless,
soft, porous,
syn
Abrasive
Type
SiC Dia, spr
or susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit or Grain
Size m
320 9 6 3 0.04/ 0.05
Lubricant
Type
Water Alco or wat Alco or
wat
Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
20 4.5 25 5.5 25 5.5 25 5.5 1015
2.33.3
Time
Minutes
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 FG 4 P 1 P 2 P 3
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
hard,
wov,
silk
Cloth,
nap-
less,
med
hard,
wov,
wool
Cloth,
nap-
less,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grain
Size m
P220 P320 P500 P1000 P1200 6 3 0.04/
0.05
Lubricant
Type
or
wat
Wat-oil
Rotation
Disk/
Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Force per
Specimen
N lb
20
4.5
20
4.5
20
4.5
20
4.5
20
4.5
20
4.5
25
5.5
1520
3.3
4.4
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 5 5 12
Etchants
Pure Sn 74d, 180, 151 General structure
Sn-Cd 74d General structure
Sn-Fe 74d, 177a General structure
Sn-Pb 182, 183, 74b General structure
116 Darkens Pb in Sn Pb
eutectic
Sn coatings on steel 183 General structure
Babbitts 184 General structure
Sn-Sb-Cu 74b General structure
Material: Titanium and Ti alloys
Titanium: allotropic: more than one crystallographic form: -titanium:
Close-packed hexagonal, -titanium: Body-centered cubic, 4.5 g/ cm
3
, 1670C
3038F, HB 70.
Titanium alloys: alloys: Alloying elements: Aluminum, gallium, germanium,
carbon, oxygen, and nitrogen. alloys: Alloying elements: Isomorphous group:
Molybdenum, vanadium, tantalum, and niobium. Group forming eutectoid
systems: Manganese, iron, chromium, cobalt, nickel, copper, and silicon.
Comments on Material: Titanium is a relatively new metal that is expensive to
produce, but nevertheless is gaining ground for applications in the aerospace
chemical, and medico-technical industries. Titanium has a high strength to weight
ratio, and it has a self-healing oxide layer that provides an effective barrier against
incipient corrosion. Commercial titanium grades and alloys are divided into four
groups: 1 commercially pure titanium, 2 and near alloys such as
Ti-6Al-2Sn-4Zr-2Mo, 3 - alloys like Ti-6Al-4V, and 4 alloys that have a high
content of vanadium, chromium, and molybdenum.
Commercially pure titanium and most of the alloys are soft and ductile with a low
machinability, difcult to prepare because of development of a deformed layer.
Also, titanium can be sensitive to hydrogen and high temperatures during the
preparation. Heat-treated alloys are harder and consequently easier to prepare.
Sectioning: Due to the high ductility and toughness of titanium it has low
machinability. Consequently it can be very difcult to cut with wet abrasive cutting
using the standard cut-off wheels because the edge will clog-up with abraded
material.
Titanium should be cut with a special SiC, bakelite bond wheel with a strong ow
of cooling uid to obtain a cool and burr-free cut. Sectioning with a shear or with
a band saw cannot be recommended, but if they are used, care should be taken
with prolonged plane grinding to remove the heavy deformation cold work
developed during cutting.
Mounting: Generally hot and cold mounting can be used. Because of the low
machinability of titanium a mounting material with a high wear resistance should
be used see Section 3.1.3. Still it can be experienced that the mounting material
is removed at a much higher rate than the sample. This can be dampened by
placing two or more samples in the same mount, not only one in the center of the
mount.
If the specimen should be etched with a strong etchant, a mounting material with
a high chemical resistance should be used. In the case of examination of surface
layers, special mounting materials should be used see Material/Preparation Tables
0810. If the examination involves the hydride phase, it may be of advantage to
leave the specimen unmounted or use an epoxy which cures slowly at a
temperature not much above room temperature.
Grinding: As rough SiC papers will leave deep deformation in the specimen, the
plane grinding should be performed with the nest grinding paper possible. Plenty
of water should be used. In the two methods below grit 220 is stated for plane
grinding, but if the sectioned surface is not very rough, grit 320 should be
preferred. New papers should be used. Often the paper can only be used in
2025 s to avoid smearing and development of cold work.
Polishing: Using ner and ner diamond grades as is normally done develops
deformed layers in titanium, very difcult to remove. Therefore, the deformation
from the grinding is removed by chemical mechanical polishing see below.
Both pure titanium and a number of alloys can be electrolytically polished.
Etching: A microstructure of titanium can be examined in polarized light without
etching. For Etchants, see below.
Case or coating
thickness/hardness,
surface layers
B 487 C-60
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-60, T-60,
El-20
Image analysis,
rating of inclusion
content
High planeness
E 562, E 1245, E 1382 C-60
Microhardness,
hardness
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-60, T-60
E 1245, E 1351, E 1382, E 1558
C-60, T-60,
El-20
El-20
Sectioning
Cut-Off Wheel SiC, bakelite bond, specially developed for titanium
Mounting
Hot Compression
Mounting
Resin Bakelite/Epoxy
with Filler
Cold
Mounting
Resin Epoxy
Time
Minutes
89 Time
Minutes/Hours
824 h
Grinding
C-60 and T-60: Use a grit 320 grinding paper for the PG step if possible, for pure
titanium and soft alloys.
Polishing
C-60: For the step P 1 use one of the following solutions: 90 mL silica with
10 mL hydrogen peroxide 30 % or 96 mL silica, 2 mL hydrogen peroxide 30 %
and 2 mL ammonia solution 25 %.
T-60: For the steps P 1, P 2, and P 3 use the solution: 260 mL silica, 40 mL
hydrogen peroxide 30 %, 1 mL nitric acid 65 % and 0.5 mL hydrouoric acid
40 %.
Section 13.2.2.
Grinding/ PG FG 1 P 1
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, napless,
soft,
porous,
syn
Abrasive Type SiC Dia, spr or susp Silica,
see note above
Grit or Grain
Size m
220 9 0.04/ 0.05
Lubricant Type Water Alco or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or Contra Comp Contra
Force per
Specimen
N lb
25 5.7 30 7 2030 5.76.6
Time
Minutes
Until plane 5 810
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
soft,
porous,
syn
Cloth,
napless,
soft,
porous,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC SiC SiC Silica,
see
note
above
Silica,
see
note
above
Silica,
see
note
above
Grit or Grain
Size m
P220 P320 P500 P1200 0.04/ 0.05 0.04/ 0.05 0.04/
0.05
Lubricant
Type
Water Water Water Water
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
contra
Comp
or
contra
Comp
or
contra
Comp Contra Contra Contra
Force per
Specimen
N lb
20
4.5
20
4.5
20
4.5
20
4.5
35 8 20 4.5 10 2.2
Time
Minutes
Until
plane
0.251 0.251 0.251 10 2 2
Etchants
Pure Ti 186, 187, 67, 68, 69, 217 General structure
188 Removes stain
Ti-5Al-2.5Sn 189 Reveals hydrides
Ti-6Al-6V-2Sn 190 Stains alpha and transformed
beta, retained beta remains
white
Ti-Al-Zr 191 General structure
Ti-8Mn 192 General structure
Ti-13V-11Cr-3Al aged 192 General structure
Ti Si 193 General structure
Ti alloys 186, 187, 192, 194, 158,
132b, 1c, 67, 68, 69, 3a, 218
General structure
11, 1c Reveals alpha case
72, 192, 178 Chemical polish and etch
170a Outlines and darkens hydrides
in some alloys
188 Removes stain
Material: Zinc and Zn alloys
Material Properties: Zinc: Close-packed hexagonal, 7.14 g/ cm
3
, 419C 786F.
Zinc alloys: Zn is mainly alloyed with aluminum, 1 to 15 % and copper up to 4 %.
Other alloying elements are lead, cadmium, iron, titanium, magnesium, and tin
weight %.
Comments on Material: Zinc is to a high degree used for die-casting and for
coating of steel sheet see Material/Preparation Tables 0810.
Zinc is very difcult to prepare because of the tendency to form layers of plastic
deformation with smearing and twins when being ground and polished. Also,
embedding of abrasive grains during grinding and polishing is a risk.
Sectioning: Abrasive wet cutting of pure zinc and zinc alloys can be done with a
thin SiC bakelite cut-off wheel, preferably on a precision cutting machine with an
efcient cooling. Zinc also can be cut by shearing or with a band saw or hand saw
with ne teeth. In the case of shearing and sawing the very deformed zone must
be carefully removed during grinding. For cutting of zinc coated steel sheet, see
Mounting: Cold mounting should be preferred because hot compression mounting
may cause deformation and recrystallization in the material. In the case of
mounting of zinc coated steel sheet, see Material/Preparation Tables 0810.
Grinding: If the sectioned surface is not very rough, plane grinding should be
done with grit 320 SiC grinding paper. To minimize the risk of embedded SiC
grains in the specimen surface, the grinding paper can be treated with wax and a
low pressure is used. Also, parafn can be used instead of water. For pure zinc it
can be of advantage to extend the time for the last FG steps to ensure that
deformation from earlier steps is removed.
Polishing: Only use a polishing cloth for zinc, do not mix with copper or lead. It
is important that the deformation from the grinding is removed during the P 1
polishing step. Pure zinc and some zinc alloys are suited for electrolytic polishing.
Cleaning: Avoid water for cleaning between the polishing steps; use alcohol for
cleaning and nish the polishing with a very brief polish with pure alcohol
followed by rinsing and drying.
Etching: A microstructure of zinc can be examined in polarized light without
etching. For Etchants, see below.
Case or coating
thickness/hardness,
surface layers
B 487 C-61
El-23
inclusion content
E 562, E 1245, E 1382 C-61
High planeness
E 110, E 140, E 384,
E 448
C-61, T-61
E 1183, E 1245, E
1351, E 1382, E 1558
C-61, T-61,
El-23
El-23
Sectioning
Cut-Off Wheel SiC bakelite bond, thin wheel
Mounting
Hot Compression
Mounting
Time
Minutes
89 Time
Minutes/Hours
610 min
Grinding
T-61: Cutting action of SiC papers can be dampened with wax. If possible, use
grit P320 for the PG step.
Polishing
C-61: In some cases P 2 can be omitted. Also, the cloth in P 2 can be changed to
a medium nap, soft, synthetic.
T-61: A step like P 2 in Method T-57 can be added between steps P 1 and P 2.
Cleaning: Avoid water for cleaning between polishing steps, use alcohol for
cleaning and nish the polishing with a very brief polish with pure alcohol
followed by rinsing and drying.
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
RCD,
soft
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr
or susp
Dia, spr
or susp
Silica
Grit/Grain
Size m
P320 9 3 1 0.04/ 0.05
Lubricant Type Water Alco or wat Wat-oil Alco or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
25 5.7 30 7 25 5.7 20 4.5 1015
2.23.3
Time
Minutes
Until
plane
4 46 35 12
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
med
hard,
wov, wool
Cloth,
napless,
soft,
porous,
syn
or susp
Silica
Grit or Grain
Size m
P220 P320 P500 P1200 3 0.04/ 0.05
Lubricant Type Water Water Water Water Wat-oil
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Comp Comp Contra
Force per
Specimen
N lb
20 4.3 20 4.3 20 4.3 20 4.3 20 4.3 10 2.2
Time
Minutes
Until
plane
0.51 12 12 46 12
Etchants
Pure Zn 200a General structure
Zn-Co 177 General structure
Zn-Cu 201 General structure
203 Distinguishes gamma
and epsilon
Zn-Fe 74a Structure of galvanized sheet
Die castings 202 General structure
Material: Zirconium. Zr alloys. Zircalloy. Hafnium. Hf alloys
Material Properties: Zirconium: Close-packed hexagonal, 7.14 g/ cm
3
, 1490C
2714F.
Hafnium: Close-packed hexagonal, 13.3 g/ cm
3
, 1700C 3092F. Zircalloy:
Zirconium with tin, oxide, iron, chromium, and nickel.
Comments on Material: Pure zirconium and zircalloy are mainly used for
cladding of uranium fuel elements for nuclear power plants. Hafnium also is used
in the nuclear reactors. Both pure zirconium and hafnium are soft and ductile,
difcult to prepare, they deform easily and mechanical twinning may develop. Also
the machineability is low.
Sectioning: Sectioning should take place with great care to avoid excessive
deformation. Wet abrasive cutting can be done with an SiC bakelite bond cut-off
wheel. Preferably the cutting should take place with a precision cut-off machine
using a thin wheel 0.5 mm 0.02 in. It is important that the cooling is very
efcient so that over-heating is avoided. If shearing or band sawing is used, plane
grinding should be extended to remove the strong deformation caused by these
cutting methods.
Mounting: Hot mounting and cold mounting can be used. If the specimen is to be
studied for hydrogen content, or in the case of a risk for mechanical twinning by
the pressure at hot mounting, cold mounting should be preferred. As the specimen
may be attacked by rather strong acids for chemical mechanical polishing and
etching, a mounting material with good chemical resistance, like epoxy, should be
used see Sections 3.6.1 and 3.13.1.
Grinding: To avoid excessive deformation, the plane grinding should preferably be
done with a grit P320 grinding paper. The grinding should always be wet because
Zr and Hf dust may generate re. The cutting action of the ner grinding papers
may be dampened with wax.
Polishing: To obtain a surface free from deformation, the nal mechanical
polishing step can be turned into chemical mechanical polishing. The chemical
solutions contain strong acids and precautions should be taken to avoid attack of
the grinding/polishing disk and the machine see below. In the case of hard
particles in the specimen surface, use Method C-62 to avoid relief. For pure metals
use Method T-62 because SiC paper has a better cutting action than diamond.
Etching: Both zirconium and hafnium can be examined in polarized light. For
Etchants, see below.
Case or coating
thickness/hardness,
surface layers
B 487 C-62
Grain size,
grain
boundaries
E 112, E 930,
E 1181, E 1382
C-62, T-62,
El-24
Zirconium,
El-11
Hafnium
Heat
treatment
C-62, T-62
Image analysis,
rating of inclusion
content
E 562, E 1245,
E 1382
C-62
High
planeness
Micro-
hardness,
hardness
E 10, E 18, E 92, E 103,
E 110, E 140, E 384, E 448
C-62, T-62
Micro-
structure
E 3, E 407,
E 562, E 883,
E 1181, E 1245, E 1351,
E 1382, E 1558
C-62, T-62,
El-24
Zirconium,
El-11
Hafnium
Phase
identication
C-62, T-62,
El-24
Zirconium
El-11
Hafnium
Preparation Process
Sectioning
Cut-Off Wheel SiC bakelite bond, a thin wheel
Mounting
Hot Compression
Mounting
Resin Bakelite/Epoxy Cold
Mounting
Resin Acrylics/
Epoxy
Time
Minutes
89 Time
Minutes/Hours
610 min
/ 68 h
Grinding
C-62 and T-62: Avoid grit P220 if possible for PG.
T-62: The cutting action of the SiC papers can be damped with wax.
Polishing
C-62 and T-62: The step P 2: A chemical mechanical polishing can be obtained
by using 96 mL colloidal silica with 2 mL hydrogen peroxide 30 % and 2 mL
ammonia solution 25 % or 95 mL colloidal silica with 5 mL chromium trioxide
solution 20 g CrO
3
to 100 mL distilled water. Another solution is 75 mL
distilled water, 10 g oxalic acid, 5 mL acetic acid glacial, 6 mL nitric acid 70
% and 2 mL hydrouoric acid 4852 % Caution!. One part of the solution is
mixed with four parts of silica for the purer zirconium materials and 1 to 1 for
zircalloys and hafnium materials.
Also, a mixture of 90 mL colloidal silica and 10 mL of hydrogen peroxide 30 %
can be used. Zirconium can be electropolished with Method El-24 and hafnium
with El-11.
Section 13.2.2.
Polishing
Disk/Cloth SiC paper RCD,
soft
Cloth, napless,
hard, wov, syn
Cloth, napless
soft, porous, syn
Abrasive
Type
SiC Dia, spr or susp Dia, spr or
susp
Silica, see note
above
Grit/Grain
Size m
P320 9 3 0.04/ 0.05
Rotation
Disk/
Holder
300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or contra Comp Comp Contra
Force per
Specimen
N lb
20 4.5 30 7 25 5.5 15 3.3
Time
Minutes
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC paper Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Silica
see note
above
Grit or
Grain
Size m
P320 P500 P1200 P2400 P4000 3 0.04/ 0.05
Lubricant
Type
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/
Contra
Comp or
contra
Force per
Specimen
N lb
20 4.3 20 4.3 20 4.3 20 4.3 20 4.3 20 4.3 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 46 310
Etchants
Zr base 66, 67, 204, 68, 69, 205 General structure
206 Electrolytic polish and etch
71 Grain structure under polarized light
Material: Bones. Carbon. Coal. Graphite. Paper. Teeth. Tissue.
Wood. Other organic materials
Comments on Material: Common to the preparation of organic materials is the
grinding steps on SiC grinding paper to the nest grit. For this reason no
contemporary method is developed, and both Methods C-63 and T-63 stated
below are traditional methods. Often organic materials, having pores, cracks,
and voids should be impregnated to obtain a surface that can be satisfactorily
prepared see below.
Sectioning: Many organic materials like paper and wood can be cut with a scissor
or a ne toothed saw. Other materials like teeth, bones, and coal should be cut on
a precision cut-off machine with a thin cut-off wheel, either with SiC bakelite
bond, diamond in a metal bond, or with ne teeth. In some cases the material
should be impregnated before cutting see below. For some materials like coal,
the selected sample is crushed and the particles are mounted in a transparent
mounting material see Section 3.11.4.
Mounting: Often the material contains pores, cracks, and cavities, or it is very
brittle. In this case a vacuum impregnation with epoxy should be done see
Section 3.10. An example of an organic material, difcult to prepare without
impregnation is paper. It is important that the paper bers are totally wetted. This
is done with an epoxy with a low viscosity, which, to obtain the best wetting, is
thinned with acetone or another thinner. A method is to briey soak the paper
specimen in acetone to wet it, soak the specimen in a 50 % acetone/epoxy mixture
for several minutes with abundant stirring. Then transfer the specimen to a 10 %
acetone/90 % epoxy mixture for several minutes, followed by transfer to a bath
with 100 % epoxy for several minutes and nally transfer to a second bath of 100
% epoxy in the mounting cup in which the specimen should be hardened. Several
specimens can be mounted in the same mounting cup, using clips to keep the
specimens upright and separated.
Grinding: In the two methods stated below grinding to P4000 is stated. For some
materials the steps FG 3 and FG 4 can be omitted.
Polishing: Diamond polishing generally is not suited for organic materials;
therefore, diamond is only used for one polishing step in Method T-63. The
polishing step, with silica in Method C-63 can vary considerably in time,
depending on the material being prepared.
Etching: Normally no etching is done.
Case or coating
thickness/hardness,
surface layers
C-63, T-63
Grain size,
grain boundaries
C-63, T-63
inclusion content
C-63, T-63
High planeness
Microstructure E 883 C-63, T-63
Sectioning
Cut-Off Wheel Thin wheel, SiC bakelite bond or diamond with metal
bond or with ne teeth
Mounting
Hot Compression
Mounting
Resin Cold Mounting Resin Epoxy/Acrylics
Time
Minutes
Time
Minutes/Hours
612 h/ 610 min
Grinding
C-63, T-63: Carbon and similar materials: Step FG 3 and FG 4 can be omitted,
when followed by a step with 3 m diamond see below.
periphery, the disk is either discarded trued.
Polishing
Carbon and similar materials and paper: C-63 and T-63: Establish a P 1 step
with a napless, hard cloth with 3 m diamond, see step P 1 in Method C-62,
followed by P 1 in C-63 or T-63. To improve planeness a napless, hard, wov, silk
cloth can be used in P 1 of T-63, possibly followed by P 1 in C-63.
Bones and teeth: T-63: The step P 1 from Method C-64 can be added as nal
step.
Paper: C-63: The step FG 4 can be changed to the step P 1 in Method C-62 using
wat-oil lubricant.
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC SiC SiC Silica
Grit or Grain
Size m
P320 P500 P1200 P2400 P4000 0.04/ 0.05
Lubricant Type Water Water Water Water Water
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen
N lb
30 7 30 7 30 7 20 4.3 20 4.3 10 2.2
Time
Minutes
Until
plane
2 2 2 12 110
Section 13.2.2.
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper SiC paper Cloth,
med nap,
soft, syn
or susp
Grit or Grain
Size m
P320 P500 P1200 P2400 P4000 1
Lubricant Type Water Water Water Water Water Wat-oil
Rotational
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp Comp Comp Comp Comp
Force per
Specimen
N lb
30 7 30 7 30 7 20 4.3 20 4.3 15 3.4
Time
Minutes
Until
plane
2 2 2 12 16
Material: EPDM polymers. Silicone. Other elastomers.
Polypropylene PP. Polystyrene PS. Polyvinylchloride PVC.
Other thermoplastics
Comments on Material: Plastics and polymers cover a very wide range of
materials with different characteristics, rigid, semi-rigid, and nonrigid. The plastics
and polymers are classied in ASTM Classication System for Specifying Plastic
Materials D 4000.
A basic reason for making materialographic examinations of plastics and polymers
is to gain a more complete understanding of the relationships between the
manufacturing processes, the microstructure and texture of the material, and the
products performance. The microstructures of plastics and polymers visible in the
light microscope are affected to a considerably greater extent by their chemical
composition and method of production than is the case with metals.
Plastics and polymers can be examined in different ways, as cross sections
polished in reected light, or as thin sections and microtome sections in
transmitted light see Section 7.13. The cross sections can be prepared by
grinding and polishing and by ultramilling; only the preparation by grinding and
polishing is described below.
Plastics and polymers are normally soft and very often the material is sensitive to
heat and possibly also to the type of cooling uid used during the preparation. It is
important that the correct uid is used in sufcient amounts both at sectioning,
grinding, and polishing to avoid thermal damage. Heat developed may cause a
softening of the material resulting in embedding of abrasive grains in the
specimen surface. It can be advised to test the cooling uids water, alcohol, etc.
and mounting material acrylics, etc. on the specimen material before the
preparation to check the resistance of the material.
The preparation of plastics and polymers is described in the ASTM Standard
Guide for Preparation of Plastics and Polymeric Specimens for Microstructural
Examination E 2015.
No contemporary method is developed for these materials, so Method C-64
below is a variant of the traditional method, T-64 by Trempler, Ref. 40, Part I.
Also, Methods C-65 and T-65 can be used for these materials. For further
information on preparation of plastics and polymers see Refs. 40 and 41, Part I.
Sectioning: Selection: The selection of the test specimen is extremely important
and dependent upon the purpose of the examination, the material, and the
microscopical technique to be used. It should be decided whether the specimen
should be taken as a cross section, longitudinal, or inclined. The selection criteria
must include the following considerations: The size and scale of homogeneity/
heterogeneity of all structures, textures, and other features within the work piece
being studied, the size or scale and distribution of the structures to be studied,
and the need for control/reference specimens. In general, sectioning should
produce a at, relatively damage-free surface near to the region of interest.
Depending on the type of material, the sectioning can be made by cutting with a
sharp knife, a pair of scissors or a scalpel. This technique will introduce a strain
typically dominated by ductile deformation in the region near the cut face. The
width of the strain region can be minimized by properly securing the specimen
during cutting, using a sharp instrument, making the cut with uniform speed and
force, and making the cut at the appropriate temperature often below room
temperature. The cut face from a cryogenically microtomed specimen is often
ready for microstructural examination with minimal nal polishing or without
additional preparation. Sawing either manually or by precision cut-off machine
can be done with a sharp, ne short-toothed saw blade with an efcient cooling.
The surface after sawing is rather rough and the region with nonuniform strain
must be removed by the following grinding and polishing. Also, wet abrasive
cutting with a precision cut-off machine using a wheel with electroplated
diamonds or an abrasive wheel with SiC in a bakelite bond may be used. Abrasive
wheels tend to clog when cutting certain materials and a diamond wheel should be
preferred, using a low feed rate. The cutting should take place with an efcient
cooling using a cooling uid which is nonreactive with the specimen material.
Often small specimens or parts, or both, with the plane of interest not parallel to a
at surface may require mounting prior to sectioning to facilitate sectioning of the
specimen parallel to the desired plane to be polished. Also, laminated, friable, or
very ductile materials may be mounted prior to sectioning to minimize damage
during the process.
Mounting: The specimen can be clamped between plates of the same or similar
type of material as the specimen. Also, the specimen can be cold mounted using a
mounting material that does not react with the specimen material, and generally
with a peak temperature sufciently below the softening temperature of the
specimen material. The softening temperature being in the range from
70 to 125C 158 to 257F for most plastics and polymers limits the use of cold
mounting materials to acrylics having a peak temperature of 90C 194F and
slow curing epoxy with a peak temperature of 30 to 60C 86 to 140F. It can be
recommended to work with a temperature not above 40C 104F. This limits the
cold mounting material to a slow curing epoxy that also can be used for vacuum
impregnation in case of porous or cracked specimen materials see Section 3.10.
To discriminate between the mounting material and the specimen material, the
epoxy should be added to a dye. To slow down the curing to keep the temperature
low, the smallest amount of mounting material should be used, and curing can
take place in a refrigerator. Also, cooling can be obtained by placing metal heat
sinks into or around the mount. In the case of the mounting of small parts,
powder or particles, see Section 3.11. In the case of a very sensitive specimen
material, the specimen can be sputter coated with a 20 to 60 nm thick metal lm
of gold or gold/palladium to form a barrier towards the mounting material. Also, a
100 nm lm will make a good contrast between the specimen-mounting material.
In the case of examination of materials with hard bers an acrylic mounting
material with a ller should be used.
Hot mounting cannot be recommended for plastics and polymers because of the
high temperatures and high pressure.
Grinding: In Methods C-64 and T-64 four grinding steps are indicated, but often
the step FG 4 and in fewer cases both FG 3 and FG 4 can be omitted. The force on
the specimens should be low and the rotational speed of the grinding/polishing
wheel should not be higher than indicated in the methods. The specimen surface
should be inspected after every 15 to 30 s of grinding to ensure that material
removal does not go beyond the area of interest; this is especially important at
mounted and impregnated specimens. Water is normally used as cooling uid and
the cooling must be effective. In case the specimen material reacts with water,
another uid must be chosen.
Peruorinated liquids, such as those used as diffusion pump oil or as cooling
liquids for active electronic circuits, are often appropriate for use with
water-soluble plastics and polymers. In the case of embedded SiC grains, use more
cooling uid, lower the force on the specimen and briey move a blind specimen
across the new grinding paper before it is used for the specimens.
Polishing: When using the grinding papers grit P2400 and P4000 as indicated in
Methods C-64 and T-64, the rough polishing, step P 1, can be done with 3 m
diamond. It is important to ensure a good cooling during the polishing. Use water,
or in special cases glycerol, as lubricant. Care must be taken not to embed the
abrasive in the specimen which can easily occur with softer plastics and polymers.
The use of a lubricant that contains a surfactant or wetting agent can minimize
the embedding of the abrasive. Also, a polish only with distilled water in a few
minutes may remove embedded grains. If after the step P 1, only a few ne
scratches are visible, then proceeding to the nal polish, as indicated in Method
T-64, is appropriate. If numerous scratches are visible, then repeat the step P 1 or
follow Method C-64, going to a step with 1 m diamond.
Cleaning: Cleaning is very important when preparing plastics and polymers. The
specimen should be cleaned between each step in an aqueous solution of dish soap
if the material is not water sensitive. The use of ultrasonic baths cleaning is
usually an acceptable practice. However, materials such as partially cured resins
may be damaged by excessive cavitation in ultrasonic cleaning. When drying,
avoid hot air.
Etching: Relief polishing may be sufcient to establish a good examination of the
specimen in dark eld illumination DF or in differential interference contrast
DIC see Section 9.2. For Etchants, see below.
Case or coating
thickness/hardness,
surface layers
C-64, T-64
Image analysis,
rating of inclusion content
C-64, T64
High planeness
Microhardness, hardness D 785, D 1415, D 2240, E 384 C-64, T-64
Sectioning
Cut-Off Wheel SiC bakelite bond, thin, a thin electroplated diamond
wheel or a ne toothed saw blade
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
615 min/ 1224 h
Grinding
C-64, T-64: For some materials the steps FG 4 and even FG 3 can be omitted.
Polishing
C-64, T-64: Check that the specimen material is not damaged by the lubricant.
For water sensitive materials use glycerol. Clean in distilled water.
C-64 and T-64: Colloidal silica can be used instead of alumina.
Section 13.2.2.
Polishing
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
nap-
less,
med
hard,
wov,
wool
Cloth,
med
nap,
soft,
syn
Cloth,
nap-
less,
soft,
porous,
syn
Abrasive
Type
spr
or
susp
Dia,
spr
or
susp
Alumina
Grit or
Grain
Size m
P320 P500 P1200 P2400 P4000 3 1 0.02/
0.05
Lubricant
Type
Rotation
Disk/
Holder
150/150 150/150 150/150 150/150 150/150 150/150 150/150 150/150
rpm/
rpm
Comp/
Contra
Force per
Specimen
N lb
1020
2.2
4.5
1020
2.2
4.5
1020
2.2
4.5
1015
2.2
3.4
1015
2.2
3.4
20 4.5 20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 45 3 Up to
10
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC SiC SiC Dia,
spr or
susp
Alumina
Grain or
Grain
Size m
P320 P500 P1200 P2400 P4000 3 0.02/ 0.05
Lubricant
Type
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Force per
Specimen
N lb
1020
2.24.5
1020
2.24.5
1020
2.24.5
1015
2.23.4
1015
2.23.4
20 4.5 10 2.2
Time
Minutes
Until
plane
0.51 0.51 0.51 0.51 5 Up to 10
Etchants
Polypropylene PP 943, 942, 945, 946 General structure
Polyethylene PE 945 Reveals lamellar structure
946 Reveals spherolites
Polyamid PA 946, 947 General structure
Material: Acrylics. Acrylonitrile butadiene styrene ABS.
Polyamid PA. Polycarbonate PC. Polyethylene PE.
Polymethyl methacrylate PMMA. Polyester saturated.
Polyoxymethylene POM. Epoxy EP. Phenolics. Polyester un
saturated. Polyurethane PUR. Other thermosetting plastics
Comments on Material: See Material/Preparation Tables 64. Also Methods C-64
and T-64 can be used for these materials.
Mounting: ASTM E 2015 recommends: For polyurethanes PUR: Sputter coat
with 40 nm of gold, and encapsulate in a moderately soft epoxy 70 to 75 Shore D
hardness under vacuum and cure at room temperature for 24 h. For
polycarbonates: Sputter as for PUR and encapsulate in acrylic or hard epoxy 80
Shore D hardness or greater under vacuum; cure acrylic at less than room
temperature; cure epoxy at room temperature for 24 h. For polymethyl
methacrylate PMMA the same procedure as for polycarbonates is recommended
only a hard setting epoxy resin should be used since PMMA may react with acrylic
mounting resin For polyester thick lms and sheets: Sputter as for PUR and
encapsulate in moderately hard 75 to 80 Shore D hardness epoxy under vacuum
for contrast, and cure epoxy at room temperature for 24 h.
Grinding: ASTM E 2015 recommends: For grinding of PMMA and polycarbonates:
The FG 3 step in Methods C-65 and T-65 are changed to a rough polishing step
with 6 m diamond or to 9 m diamond for polyester thick lms and sheets see
below.
For preparation of soft and ductile materials, use T-65.
Polishing: ASTM E 2015 recommends: For nal polishing of urethanes, PMMA
and polycarbonates: The P 3 step in Methods C-65 and T-65 are changed to
0.05 m gamma alumina see below.
Etching: See etchants below and Material/Preparation Tables 64.
Case or coating
thickness/hardness,
surface layers
B 487 C-65, T-65
inclusion content
High planeness
C-65, T-65
Microhardness, hardness D 785, D 1415, D 2240, E 384 C-65, T-65
Microstructure E 3, E 2015 C-65, T-65
Phase identication C-65, T65
Sectioning
Cut-Off Wheel SiC bakelite bond, thin wheel or wheel with ne teeth
or a thin electroplated diamond wheel
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
615 min/ 1224 h
Grinding
C-65 and T-65: For PMMA and polycarbonates: Change the step FG 3 to a rough
polishing step with a soft napless nonwoven synthetic cloth, 6 m diamond,
lapping oil, 150/ 150 r/ min, Comp, 1827 46 N lb, 30 s, repeat as needed. For
polyester thick lm and sheets: Change the step FG 3 to a rough polishing step
with a perforated hard nonwoven chemitextile pad, 9 m diamond, distilled
water, 120/ 120 r/ min, Comp, 13 3 N lb, 30 s, repeat as needed.
C-65: Often a step with SiC paper grit P2400 should be added between FG 2 and
FG 3.
Polishing
C-65 and T-65: For urethanes, PMMA and polycarbonates: Use 0.05 m alumina
for nal polishing, step P 3, instead of the stated silica. For polyester thick lm
and sheets: Use 0.05 m alumina mixed with colloidal silica in high pH aqueous
suspension for step P 3.
C-65: Often the steps P 1 and P 2 can be omitted.
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
med nap,
soft, syn
Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC SiC Dia,
spr
or
susp
Dia,
spr
or
susp
Silica
Grit or
Grian
Size m
P320 P500 P1200 P4000 3 1 0.04/ 0.05
Lubricant
Type
Water Water Water Water Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
Contra
Force per
Specimen
N lb
2030
4.57
2030
4.57
2030
4.57
2030
4.57
30 7 2030
4.57
1020
2.24.5
Time
Minutes
Until
plane
0.51 0.51 0.51 34 23 0.51
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
med
hard,
wov,
wool
Cloth,
med
nap,
soft,
syn
Cloth,
napless,
soft,
porous,
syn
or susp
Dia, spr
or susp
Silica
Grit or
Grain
Size m
P320 P500 P1200 P2400 3 1 0.04/ 0.05
Lubricant Type Water Water Water Water Wat-oil Wat-oil
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp
or
contra
Force per
Specimen
N lb
2030
4.5
7
2030
4.5
7
2030
4.5
7
2030
4.5
7
30 7 2030
4.57
1020
2.24.5
Time
Minutes
Until
plane
0.51 0.51 0.51 34 23 0.51
Etchants
Material Etchants
see Table 12.2
Uses
Polyoxymethylene POM 945 Reveals spherolite spherolite
cores and growth direction
Polycarbonate of styrene 947 General structure
Material: Powder Metals. Ferrous. Nonferrous
Material Properties: Iron-graphite mixtures: Up to 0.8 % carbon. Iron-copper: 2
to 20 % copper. Iron- copper-carbon: 2.0 to 5.0 % copper, 0.8 % carbon.
Iron-phosphorous: Phosphorous less than 1 %. Iron- nickel: 2 to 4 % nickel, 0.4 to
0.8 % carbon, up to 2.0 % copper.
Stainless steels: Compositions that approximate AISI designations 303, 304, 316,
for austenitic stainless steels and 410 for martensitic stainless steels.
Copper-base: Bronzes with 10.0 % tin Brasses with 10, 20, and 30 % zinc. Nickel
silver with 18 % zinc and 18 % nickel. Some alloys may contain 2.0 % lead.
Titanium-based: 6.0 % aluminum, 4.0 % vanadium.
Aluminum-based: 0.25 to 4.4 % copper, 0.6 to 0.8 % silicon, 0.4 to 1.0 %
magnesium weight %.
Comments on Material: Powder metal is one of the four major methods of
forming metals casting, machining, and plastic forming. It is the process of
producing metal shapes from metallic powders. The metal powder is blended,
pressed compacted into shape, and sintered to temperatures just below the
melting point. The process offers a wide variety of alloys and material properties.
The main production of powder metal parts is small to medium sized parts for the
auto and manufacturing industry. The advantage is that the parts have a good
surface nish with close dimensional tolerances so that machining is reduced or
avoided. Other alloys are made for cutting tools with tungsten carbide and other
carbides see Material/Preparation Tables 67. Powder metals are classied with a
prex and a code, an example is: CNZ181613, where C means copper base
element, N means nickel minor element #1, Z means zinc minor element #2, 18
means percentage of minor element #1, 16 means percentage of minor element #2,
and 13 means minimum yield strength.
During the sintering, recrystallization and grain growth occur between the
particles in a contact area, and a grain and lattice structure such as known from
solid metals is developed. Voids and pores between the particles are still present,
depending on the amount of compression and the time of sintering. When doing
metallographic/materialographic examination, the major difference between solid
metals and powder metals is the amount of porosity. Sintered materials generally
exhibit 0 to 50 % porosity which affects mechanical properties and strongly
interferes with the preparation and interpretation of the microstructure. Careful
preparation is important because the shape of the porosity is as important as the
amount in judging sintered strength and the degree of sintering. The main
problem during the preparation is the smearing of the pores during grinding and
rough polishing that may occur even when the pores are lled with a resin see
below.
For mounting of uncompacted powder, see Section 3.12.4. Preparation of mounted
specimens with uncompacted powder is in principle done as for the base material,
but often the preparation times should be reduced to avoid over-polishing of the
powder particles embedded in the epoxy.
Sectioning: Selection: As the density and other features can vary considerably, it
is important that the specimens are selected from the surface and interior of the
part and from top and bottom. Wet abrasive cutting with an SiC or Al
2
O
3
bakelite
bond cut-off wheel, depending on the base material of the powder metal.
Preferably a precision cut-off machine with an effective cooling and a thin wheel
0.5 mm 0.02 in should be used to reduce material damage.
In the case of band sawing, the relatively large deformed layer of the cut surface
should be removed through a careful plane grinding.
Mounting: Before mounting it may be necessary to remove uids absorbed in the
pores of the material during the manufacture and cutting. If the specimen can be
heated, the uids water and oil can be removed by heating the specimen in a
short time on a hot plate under a fume hood. If the specimen material cannot be
heated an extractor-condenser like the Soxhlet apparatus may be used. The
apparatus consists of a ask, a siphon cup, and a condensing-coil unit that ts on
the top of the ask. A solvent, such as toluene or acetone, is placed in the ask,
and the specimen to be cleaned is placed in the siphon cup. Six cycles, requiring a
total of 1 h, will usually ensure removal of the oil. The method is described in
ASTM Standard Test Method for Density, Oil Content, and Interconnected Porosity
of Sintered Metal Structure Parts and Oil-Impregnated Bearings B 328. Also,
ultrasonic cleaning under a fume hood for one h in 1-1-1 trichloroethane and a
hot ultrasonic bath has been recommended. The residual entrapped solvent should
be evaporated from the specimen.
Mounting of specimens, which should be examined for porosity, should be done
with a low viscosity epoxy, ensuring an effective vacuum impregnation see Section
3.10. If edge retention is important, the epoxy should be mixed with a ller see
Section 3.11.2. Other specimens can be hot mounted or cold mounted with
acrylics.
Grinding: For materials with high porosity and which are relatively soft and
ductile it may be of advantage to extend Method T-66 with a step using grit 2400
grinding paper see below.
Polishing: It is important that the porosity is clean, all pores must be opened,
after the 3 m diamond step. If this is not the case, the step should be prolonged.
For the nal polishing step a chemical mechanical polishing may be of advantage
see under the Material/Preparation Tables covering the base material.
Etching: Often the specimen is examined in unetched condition to evaluate the
number and distribution of the particle boundaries.
Etchants used for the base metal may be used; these can be found under the
relevant Material/Preparation Tables.
Case or coating
thickness/hardness,
surface layers
B 487 C-66
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-66, T-66
Image analysis,
rating of inclusion
content
High planeness
E 562, E 1245, E 1382 C-66, T-66
Microhardness, hardness B 931, B 932, B 933,
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
C-66, T-66
Microstructure B 328, E 3, E 407, E 562, E 883, E 1181,
E 1245, E 1382, E 1558
C-66, T-66
Sectioning
Cut-Off Wheel SiC or Al
2
O
3
, bakelite bond, thin wheel
Mounting
Hot Compression
Mounting
Resin Bakelite Cold
Mounting
Resin Epoxy/Acrylics
Time
Minutes
810 Time
Minutes/Hours
612 h/ 610 min
Grinding
T-66: In case of soft, ductile materials a grinding step, FG 4, with grit P2400
grinding paper can be added.
Polishing
C-66 and T-66: For nal polishing chemical mechanical polishing may be used
see the relevant Material/Preparation Tables for the base material.
C-66: Often the step P 2 can be omitted.
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
RCD,
soft
Cloth,
napless,
hard,
wov,
syn
Cloth,
med
nap,
soft,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
SiC SiC Dia,
spr
or
susp
Dia,
spr
or
susp
Dia,
spr
or
susp
Alumina
Grit/Grain
Size m
P220 P500 9 3 1 0.02/ 0.05
Lubricant
Type
Water Water Alco or wat Alco or wat Alco or wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Comp or
contra
Force per
Specimen
N lb
2030
4.57
2030
4.57
2030
4.57
2030
4.57
2030
4.57
1015
2.23.4
Time
Minutes
Until plane 1 5 4 3 1
Section 13.2.2.
Polishing
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Cloth,
napless,
hard,
wov,
silk
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Alumina
Grit or Grain
Size m
P220 P320 P500 P1200 6 3 0.02/ 0.05
Lubricant
Type
wat
Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Comp or
contra
Force per
Specimen
N lb
2030
4.57
2030
4.57
2030
4.57
2030
4.57
2030
4.57
2030
4.57
1015
2.23.4
Time
Minutes
Until
plane
0.51 0.51 0.51 4 3 12
Etchants
See under the relevant Material/Preparation Tables covering the base material of
the powder metal.
Material: Sintered cemented tungsten carbides. Hard metals.
Other coated sintered carbides
Comments on Material: Cemented carbides sintered carbides, hard metals are
sintered materials consisting of tungsten carbide or a mixture of tungsten carbide,
titanium, or tantalum carbide in powder form, sintered in a matrix of cobalt or
nickel. Cemented carbides, being very hard and tough with a high wear resistance,
are suited for cutting tools, metal forming tools, rock drilling, and other purposes
where a high wear resistance is needed. To improve the wear resistance of the
cutting tool, often the cemented carbide insert is coated by chemical vapor
deposition CVD with one or more hard materials like titanium carbide, titanium
nitride, titanium carbonitride, and aluminum oxide, the coating being
0.2 to 10 m thick.
Cemented carbides are covered by a number of ASTM standards regarding
specimen preparation B 665, determination of microstructure B 657, apparent
grain size B 390, and apparent porosity B 276 see below and Section 12.4.
The high hardness of cemented carbides makes only metallographic/
materialographic preparation with diamond possible. The relatively soft cobalt can
be smeared over the carbides and lack of adequate pressure on the specimen
during polishing may result in pull-outs material being torn from the surface of
the specimen. This condition may erroneously be interpreted as porosity see
Section 13.6.4.
Sectioning: The carbides, being very hard, the wet abrasive cutting should be
done with a diamond metal bond cut-off wheel preferably on a precision cut-off
machine so that a thin wheel can be used, reducing the damage to the cut surface.
The cutting, with an efcient cooling, should be performed with a suitable low
feed speed to avoid fracturing of the relatively brittle material, especially at the
end of the cut.
Mounting: Due to the high hardness, cemented carbides should always be
mounted in a mounting material with a ller. For hot mounting, epoxy with a ller
is recommended and for cold mounting acrylics with a ller or epoxy with an
in-mixed ller may be used see Sections 3.1.3 and 3.11.2. In the case of
examination of coatings, an epoxy mounting material should be used see also
Grinding: If the sectioning has been without excessive deformation, the PG step in
Method T-67 can be omitted.
Polishing: It is important that all deformation from the previous steps are
removed after the 3 m diamond step, P 1 in Method C-67 and P 2 in T-67. Often
the surface after this step is satisfactory for routine examination. Alumina should
not be used for cemented carbides with cobalt matrix because the surface may
corrode. Also, the cleaning should be with alcohol only because water may corrode
the cobalt matrix.
Etching: See etchants below. A physical etching by relief polishing can be made if
a napped cloth is used for the nal polishing step, a relief between carbides and
matrix will develop see below Also, vapor deposition of interference layers may
give good results see Section 9.6.
Case of coating thickness/
hardness, surface
layers
B 487 C-67
Grain size, grain boundaries B 390, E 1382 C-67, T-67
High planeness
E 562, E 1245 C-67, T-67
Microhardness, hardness E 10, E 18, E 92, E 140, E 384 C-67, T-67
Microstructure B 657, B 665, E 3, E 562,
E 1245
C-67, T-67
Porosity B 276 C-67, T-67
Sectioning
Mounting
Hot Compression
Mounting
Resin Epoxy
with Filler
Cold
Mounting
Resin Epoxy with Filler/
Acrylics with Filler
Time
Minutes
Time
Minutes/
Hours
612 h/ 610 min
Grinding
C-67: Very often the FG 2 step can be omitted.
T-67: Very often the PG step can be omitted.
Polishing
C-67: In case of pull-outs developed during the grinding, the time of step P 1
should be prolonged.
T-67: In case of pull-outs developed during the grinding, the time of step P 2
should be prolonged.
C-67 and T-67: The nal polishing step can be changed to 1 m diamond on a
medium napped cloth
see Method T-65, step P 2.
Section 13.2.2.
Polishing
xed, res
RCD, hard RCD,
soft
Cloth,
napless,
hard, wov,
syn
Cloth,
napless,
soft, porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
P120 9 3 3 0.04/ 0.05
Lubricant
Type
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per
Specimen N
lb
40 9 35 8 35 8 30 6.6 15 3.4
Time
Minutes
Until
plane
5 510 58 12
Section 13.2.2.
Polishing
Disk/Cloth Dia
pad, met
Dia pad,
bak
Cloth,
napless,
v. hard
wov, syn
Cloth,
napless,
hard,
non-
wov, syn
Cloth,
napless,
hard,
wov,
syn
Cloth,
napless,
soft,
porous,
syn
susp
Dia, spr or
susp
Dia, spr or
susp
Silica
Grit or Grain
Size m
125 30 15 6 3 0.04/ 0.05
Lubricant
Type
Water Water Alco or
wat
Alco or wat Alco or
wat
Rotation
Disk/Holder
300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Comp or
contra
Force per
Specimen N
lb
30 7 30 7 40 9 40 9 30 7 15 3.4
Time
Minutes
Until
plane
35 6 5 5 2
Etchants
Cemented tungsten
carbides according to
ASTM Standard B 657
Etching Technique 1
951 Identication
of phase
Cemented tungsten
ASTM Standard B 657
Etching Technique 2
949 in combination with
950
Identication
of phase
Cemented tungsten
ASTM Standard B 657
Etching Technique 3
951 Identication
of phase
Material: Uranium and Uranium dioxide. Americium. Cadmium.
Indium. Mercury and amalgams. Neptunium. Plutonium. Rare
earth metals. Selenium. Tellurium. Thallium. Thorium
Material Properties: Uranium: Body-centered cubic, 238.07 g/ cm
3
, 1689C
3010F, HV 190. For all other materials mentioned above, see below.
Comments on Uranium: Uranium U belongs to the rare earth metals radioactive
group. It is the most important of the rare earth metals see below because it has
been used as a metallic fuel in producing atomic energy. The metallic fuels have
been superceded by oxide fuels, and the information below covers preparation of
uranium dioxide UO
2
. Uranium dioxide is normally used in the form of pellets
that are made through a process where the raw material in powder form is
sintered at a high temperature. In this state the uranium dioxide can be
considered a ceramic material of cubic crystal structure with a very high melting
point.
U and UO
2
are radioactive materials and a health hazard so that all handling shall
take place in hot cells or glove boxes through manipulators so that human contact
with the radioactive material is avoided.
The metallographic/materialographic preparation process follows the same lines as
normal preparation, only as mentioned in a shielded environment and with special
precautions regarding the disposal of the used consumables. The preparation
process stated below is for uranium dioxide, and two methods, a C-method and
a T-method are indicated.
Comments on Other Materials:
Americium Am, neptunium Np, plutonium Pu, and thorium Th are
radioactive metals and will not be discussed further.
Cadmium Cd, indium In, and thallium Tl are very soft metals that are seldom
used. Cd and Tl are toxic. These metals will not be discussed further.
Mercury Hg and amalgams: Amalgams are mercury alloys consisting of Hg
mixed with powders of silver, tin, copper, and zinc. Only amalgams can be
metallographically prepared, and these alloys will not be discussed further.
Rare earth metals: This group of 15 metals are very rarely prepared and will not
be discussed further. For yttrium Y see Material/Preparation Table 20.
Selenium Se and tellurium Te are semiconductors and very toxic and will not
be discussed further. For preparation of the semiconductors silicon and
germanium see Material/Preparation Tables 21.
Sectioning: The uranium dioxide, in pellet form, is normally encapsulated in
epoxy mounted prior to cutting. This is to minimize fragmentation of the
material and thereby reduce the waste and contamination issues. The cutting is
done on a special cutting machine made for the special conditions in a hot
cell/glove box, using a diamond wheel with resin or metal bond. A wheel with
electroplated diamonds may also be used, especially when cutting encapsulated
material. When working with radioactive material the volume of liquid in any hot
cell/glove box is strictly controlled to a minimum. Consequently, cutting is carried
out with a low rotational wheel speed, controllable feed rate, and wheel cooling by
dip transfer of the coolant to the wheel so that splashing is avoided and the
consumption of coolant is kept very low.
Mounting: Cold mounting with epoxy is used. Vacuum impregnation is used on
some applications see Section 3.10.
Grinding: Grinding and polishing are carried out on special semiautomatic
machines, often with modications of standard machines so that all handling can
take place through manipulators.
When using SiC grinding paper, as indicated in Method T-68 below, a large
amount of low level contaminated waste is generated which involves costly
disposal.
Polishing: For the nal step both alumina and colloidal silica can be used, often
with addition of hydrogen peroxide see below.
Etching: See below.
Case or coating
thickness/hardness,
surface layers
C-68
Grain size,
grain boundaries
E 112, E 930, E 1181, E 1382 C-68, T-68
High planeness
E 562, E 1245, E 1268, E 1382 C-68
Microhardness,
hardness
C 730, C 849, C 1326, C 1327,
E 384
C-68, T-68
E 1268, E 1382
C-68, T-68
Porosity C-68
Sectioning
Cut-Off Wheel Diamond, metal/resin or electroplated,
see above.
Mounting
Hot Compression
Mounting
Time
Minutes
Time
Minutes/Hours
68 h
Grinding
C-68 and T-68: When using water for cooling this shall be only as drops to
reduce contaminated waste see above.
Polishing
C-68 and T-68: P 3: Mix 90 mL of alumina or colloidal silica with 10 mL of
hydrogen peroxide 30 %.
Section 13.2.2.
Grinding/
Polishing
PG FG 1 P 1 P 2 P 3
xed, res
RCD,
hard
Cloth,
napless,
hard,
nonwov,
syn
Cloth,
napless,
hard, wov,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
Diamond Dia,
spr or
susp
Dia,
spr or
susp
Dia,
spr or
susp
Silica
see
note
Grit/Grain
Size m
P220 6 6 3 0.04/ 0.05
Lubricant
Type
Water
drip
Wat
drip
Wat
drip
Alco
or wat
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or
contra
Force per Specimen N lb 30 6.6 30 6.6 35 8 30 6.6 30 6.6
Time
Minutes
2 5 5 4 1.5
Section 13.2.2.
Grinding/
Polishing
PG FG 1 FG 2 FG 3 P 1 P 2 P3
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
SiC
paper
Cloth,
napless,
hard,
nonwov,
syn
Cloth,
med.
nap,
soft,
syn
Cloth,
napless,
soft,
porous,
syn
Abrasive
Type
or susp
Dia, spr
or susp
Alumina
see
note
Grit or
Grain
Size m
P220 P320 P500 P1000 6 3 0.02/ 0.05
Lubricant
Type
Water
drip
Water
drip
Water
drip
Water
drip
Alco Alco
Rotation
Disk/
Holder
150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
rpm/
rpm
Comp/
Contra
Force per
Specimen
N lb
25 5.5 25 5.5 25 5.5 25 5.5 20 4.4 20 4.4 20 4.4
Time
Minutes
31 min 41 min 61 min 101 min 8 6 5
Etchants
UO
2
924 General
structure
13.2.4 Manual Preparation
The methods stated in Section 13.2.3 are based on semiautomatic preparation. It is
possible, however, to use the data stated inthe Method Tables for manual hand prepa-
rationalso.
The T-methods are most suited for preparation by hand, both the methods based
on SiC grinding paper, and the methods based on diamond disks/pads, but also the
C-methods, often using resin bonded diamond disks and rigid composite disks RCDs
for grinding, can in some cases be transferred to manual hand preparation see be-
low.
As manual hand preparation is less uniform, to a high degree depending on the
operator, the times indicated in the Method Tables should only be taken as guidelines
see below.
Manual grinding/polishing should preferably be done on two machines, a grinder
with one or two disks especially designed for SiC paper see below, rotating with
300 rpm, and a polisher 150 and 300 rpm with one or two interchangeable disks for
mounting of several polishing cloths or one magnetic disk see Section 6.7.1. For
manual grinding and polishing, disks for 230 mm 9 in grinding paper and for
200 mm 8 in polishing cloths should be preferred. Separating the grinding and pol-
ishing on two machines reduces the risk of contamination, but both processes can also
be done onthe same machine.
Before starting on manual preparation, it is recommended to read relevant sec-
tions inChapters 6and7.
Grinding
SiC Grinding Paper
In the Method Tables, P220 grit is usually stated as the rst step. If the original surface
of the specimen is very rough it might be necessary to start with P120 or P180 grit be-
fore grinding with a P220 grit. In general, paper with plain back should be used, the
paper being xed by a thin layer of water between the paper and the disk. For this pur-
pose the disk has a raised edge, allowing water to stay on the disk when not rotating,
and water is added to the disk before the sheet of paper is placed. Aring is often used to
keep down the edge of the paper, but this ring is not xing the paper, the xation takes
place through the suction between disk surface and sheet, because most of the water is
slung away by the centrifugal force when the disk starts rotating. The paper should not
be storedinwater betweenuses because this weakens the bondof the paper. Paper with
adhesive back canalso be used, but generally the force onthe paper at manual grinding
is so lowthat a plain backed paper can be used. Also, paper with adhesive back is con-
siderably more expensive than plain backed paper. As a middle solution a double ad-
hesive foil can be placed between disk and paper and the foil can be used for many
sheets. Water should be supplied in a constant ow to the center of the rotating disk
securing that all debris is washedaway.
When grinding, hold the specimen in a rmgrip, with a relatively strong pressure,
both hands can be used, and move it fromperiphery to center of the paper surface and
back in a slowmovement. Be careful that the specimen is held so that the scratches are
in the same direction on a given paper. Also, be careful that the specimen is not tilting,
making facets onthe surface. Whengoing tonext ner grit paper, turnthe specimen90
so that the new scratch pattern can be seen perpendicular to the scratches from the
previous step. Continue grinding until all scratches from the previous step are re-
moved, and as a rule go onfor at least the same period of time to remove possible defor-
mation. This rule covers harder materials with limited deformations introduced, but
for softer, more sensitive materials grinding shall go on for a longer period of time. In
some cases it might be necessary to use several sheets of the same grit. Do not use the
paper for too long, depending on the hardness of the material, the paper is worn after
20120 s. If the paper is worn out it is not removing material but creating deformation
in the specimen surface see Chapter 6. The specimen surface ground correctly is dull
with parallel scratches. If the surface is bright, the paper has been worn and newpaper
shouldbe used.
All grinding steps can be done without cleaning in between, but after the last n-
est stepthe specimenshouldbe cleanedanddriedsee below.
Diamond DisksDiamond Pads
Diamond disks with xed diamond grains are in the form of diamond in a metal/
bakelite bond on a solid disk, as diamond pads or as resin epoxy bonded diamonds,
both on a thin backing, to be xed by adhesion or magnetically to a grinding/polishing
disk. They are all usedwitha owof water andinthe same way as SiCpaper.
Rigid Composite Disks RCD
A disposable RCD is placed on a disk magnetically as described for polishing cloths
below, or a solid disk is used see Section 6.7.7. Also, the diamond is charged as stated
below, only spray andsuspensioncanbe used. The diskshall rotate with150 rpm.
It can be difcult to use an RCD for hand preparation because the RCD normally
works with relatively little lubrication to avoid aqua planing. This process drags
strongly in the specimen and it might be difcult to hold it by hand. The effect is not
very strong on less aggressive soft RCDs, and hand preparation can easily be per-
formed. The specimen is rotated around the disk, as described belowunder polishing;
take care that the whole surface of the diskis usedtoavoidanunplane surface.
A rm pressure is applied during grinding with RCD; both hands are often used,
like for SiCpaper.
The disk should be cleaned regularly to avoid swarf closing the openings between
the segments onthe surface.
Diamond Polishing
If using polishing cloths with adhesive back, take care that a number of disks, corre-
sponding to the number of polishing steps, including the step with silica or alumina, is
available. In this way, the cloths charged with different grain sizes can easily be
changed during the process and should only be removed fromthe disk when worn out,
securing the highest degree of cleanliness and avoiding contamination from disk to
disk. If cloths withmagnetic backing are used, the clothcanbe removedeasily fromthe
magnetic diskwhichcanstay inthe machine, andonly one diskis needed.
In the case of a newcloth, charge the cloth with a reasonable amount of diamond,
at paste, use approximately 1 g for a 200 mmdisk and recharge regularly with 0.5 g. At
diamond spray, spray one round on the cloth for a start and respray every 23 min
during the process. At suspension, charge the newcloth with a reasonable amount and
recharge during the process every 23 min froma spray bottle. If a product with dia-
mond and lubricant in one is used, it is added as stated belowfor lubricant. According
to Samuels Ref. 7, Part I, diamond paste should give the highest removal rate at
manual polishing.
In the case of a used cloth, take care that the cloth can be used for the material in
question. Normally a cloth should only be used for the same group of materials; this
gives three sets of disks with cloths in an all-round laboratory: for ferrous metals, non-
ferrous metals, andfor ceramics.
Starting witha dry cloth, the clothis wetted witha reasonable amount of lubricant
sothat the total surface is moist, but not swimming, see below. It is preferable touse
a water-based lubricant because alcohol- and oil-based lubricants may be dangerous to
health.
The polishing disk should rotate with 150 r/ min and the specimen is rotated
slowly in a circle against the direction of the disk. The specimen is moved slowly from
the periphery to the center of the disk and back to secure a uniformwear of the polish-
ing cloth. By rotating the specimen, all phases in the specimen surface are uniformly
treated, ensuring a minimum of artifacts in the surface. Charge the cloth RCD with
small amounts of lubricant at the center of the disk inshort intervals so that the surface
is just moist whentouchedwitha ngertip, not wet.
The pressure during polishing is rmat the roughsteps andlower at the nal steps.
Also, at all steps, the pressure is reducedduring the last approximately 30 s.
Important: The times indicated in the Method Tables are based on semiautomatic
preparation, therefore the times for manual preparation could be longer. Until experi-
ence with a given material is developed, take care that deformations and scratches
from the previous step are removed by looking at the specimen surface in the micro-
scope see the Metallographers Rule of Thumb andTrouble Shooting Section13.5.
Silica and Alumina Polishing
Be careful, especially with silica SiO
2
polishing, that the cloth is absolutely clean be-
fore starting the process, not having dried-in particles from previous polishing; these
particles might scratch the specimen surface. Circulate the specimen as described
above, adding the polishing medium to the center of the cloth from a spray bottle in
small amounts at short intervals.
When nished, clean the specimen and the cloth by further polishing in approxi-
mately 10 s withplenty of water addedtothe center of the cloth. Silica canbe especially
difcult to remove and at certain, not too sensitive materials, the specimen surface can
be rubbedwitha wadof cotton. To cleana porous clothuse the edge of a piece of plastic
as a scraper on the rotating cloth to remove remaining polishing media to avoid par-
ticles that will later dry-inonthe cloth.
Cleanliness and Cleaning
It is important that a step is not contaminated with abrasive grains from the previous
step. The specimen should be washed and cleaned with cotton in lukewarmwater and
nally rinsed with ethanol and dried in a stream of warm air or cleaned dry com-
pressedair see alsoChapter 5. The hands of the operator shouldalsobe washed.
13.3 Electrolytic Polishing and Etching
In electrolytic polishing, or electropolishing, the specimen is placed as an anode in an
electrolytic cell. Material is removed fromthe specimen surface through the electroly-
sis, and because of this, the prepared surface often has a number of artifacts see Chap-
ter 8. If the specimen has two or more phases, with different potential, like cast iron
and contains nonmetallic nonconductive inclusions, or both, the prepared surface
will not usually showa true or acceptable microstructure.
Electropolishing has, however, a number of advantages. The surface created is
usually scratch-free and without deformation, an advantage for soft metals, difcult to
polish mechanically. Also electropolishing is very effective for routine polishing, the
polishing time is very short, andoftenthe etching cantake place as part of the process.
In certain cases like in stainless steel, the etching cannot be done with the electro-
lyte used for polishing, and external etching can take place using a lowvoltage and a
special electrolyte see Section9.5.
Trial and Error: To develop a new method, start with a relatively low voltage and
increase with 5 V for each trial until the correct voltage current density is found.
Grind with relatively ne SiC paper between trials to remove traces from the previous
electropolishing. Newer electropolishers see below have a built-in scan function that
indicates the correct voltage/current level for a givenmaterial.
Trouble Shooting: See Section13.6.5.
Electrolytic polishing is described in the ASTMGuide for Electrolytic Polishing of
Metallographic Specimens E1558 see Section12.4.
13.3.1 Electropolishers
The methods stated in this book are based on the use of an apparatus in which the
specimen is placed as an anode on top of a polishing chamber with a mask dening a
specic area to be polished, the chamber containing a cathode anda owof electrolyte.
The area is usually from 0.55 cm
2
0.080.8 in
2
. A number of parameters, voltage,
polishing/etching current amperage, ow rate of electrolyte, polishing/etching time,
andelectrolyte temperature, are controlledby the apparatus see Chapter 8.
13.3.2 ElectrolytesMethods for ElectropolishingTable 13.2
A number of electrolytes have been developed for most metals, mainly based on per-
chloric, perchloric/acetic, phosphoric, and sulfuric acids. The composition of a num-
ber of electrolytes covering most materials is stated in Table 13.2. To obtain the formu-
las of a very high number of electrolytes, see Table 2 in the ASTMStandard E1558 see
Section12.4.
To nd the correct electrolyte for a specic material, go to Table 11.1 and nd the
Electropolishing Method El-Method number. These methods are stated in Section
13.3.5. The El-Method numbers are also stated in the Material/Preparation Table, Sec-
tion 13.2.3. In the El-Method, the Electrolyte number is stated. This number is taken to
Table 13.2, andthe compositionis found.
When mixed, the electrolytes often have a relatively short shelf life, around two
months for the most used perchloric acid type. Life also depends on the number of pol-
ishings performed. Often an electrolyte only works best after a few polishings when a
number of metal ions are established.
Attention: Perchloric acid is very dangerous explosion when in contact with or-
ganic material at high concentrations. For this reason, only authorized electrolytes
containing perchloric acid should be used, and care should be taken that the concen-
tration of perchloric acid is not increased by evaporation of other ingredients in the
electrolyte, like ethanol.
General Safety Precautions: Work with acids and other chemicals is potentially
dangerous. Before using or mixing any chemicals, all product labels and pertinent Ma-
terial Safety Data Sheets MSDS should be read and understood. All general precau-
tions shouldbe takenregarding protectionof persons. For specic informationonhan-
dling electrolytes, see Chapter 26.
13.3.3 Table 13.2Electrolytes for Electropolishing/Etching
Comments to Table 13.2:
The electrolytes are split intove groups. The groupnumber is the rst digit inthe Elec-
trolyte Number.
Group1: Perchloric AcidandAlcohol WithandWithout Organic Additions
Group2: Perchloric AcidandGlacial Acetic AcidinVarying Proportions
Group3: Phosphoric AcidinWater or Organic Solvent
Group4: MixedAcids or Salts inWater or Organic Solvent
Group5: Alkaline Solutions
TABLE 13.2Electrolytes for Electropolishing/Etching.
Electrolyte
Number Use Formula Remarks
1-1 Steel, cast iron, Al, Al
alloys, Ni, Sn, Ag, Be,
Ti, Zr, U, heat resisting
alloys
Ethanol (95 %) 700 mL
2-butoxy ethanol 100 mL
Perchloric acid (30 %) 200 mL
One of the best formulas for
universal use.
Add the perchloric acid to the
mixture of the other two
components.
12 Iron and steel in
general, stainless steel,
Al, Al alloys, Ni, Sn,
Ag, Mo, Ti, Zr, Pb, Pb-
Sa, Zn, Zn-Al-Cn, Mg
and high Mg alloys
Distilled water 90 mL
Butylcellosolve 100 mL
Universal use.
Add the perchloric acid to the
mixture of the other three
components. Shelf life around
two months.
13 Carbon, steels, alloyed
steels, stainless, steels,
martensite, high temp.
alloys, Pb, Al-Cu
alloys, Mn, Mo, Sn, Ti,
Ti-alloys, Zr, V
Methanol (100 %) 600 mL
Vogels Sparbeize 2 mL
Vogels Sparbeize is an inhibitor
used in industrial electrolytic
polishing. The electrolyte can
be used without this.
Attention: Methanol is a poison,
use fume hood.
14 Cast iron, low alloyed
C-steels, stainless
steels, Be, Mg, Ni
Propanol (100 %) 100 mL
Sodium thiocyanate dihydrate
Mix in the following way:
Propanol and ethanol are mixed
and hydroxychinolin is dissolved.
After dissolution the sodium
60 g
Citric acid 75 g
Hydroxychinolin ortho 10 g
thiocyanate is added and after
dissolution the citric acid. When
the citric acid is added, the liquid
turns muddy, but turns clear when
all is dissolved and the perchloric
acid is added.
2-1 Austenitic steels, Cr,
Hf, Ni, Pb, Th, Ti
Acetic acid (glacial) 950 mL
Alternative to Group 1 electrolytes
for certain materials.
3-1 Alpha, alpha+beta
brass, Cu-Fe, Cu-Co,
Co, Cd
Distilled water
600 mL
Ortho phosphoric acid (84 %)
400 mL
Alternative to electrolyte No. 3-2
for Cu alloys.
3-2 Cu, brass, Au Distilled water
Ortho phosphoric acid (84 %)
250 mL
Urea 5 g
Vogels Sparbeize 2 mL
Vogels Sparbeize is an inhibitor
used in industrial electrolytic
baths; this or another similar
inhibitor improves the electrolyte,
but can be omitted.
4-1 Cd, Mg, Zn, Pb Ethanol (95 %) 800 mL
Distilled water 20 mL
Sodium thiocyanate dihydrate
160 g
The sodium thiocyanate is
dissolved in the mixture of water
and ethanol. When in solution the
butylcellosolve is added.
4-2 Bronzes, brasses,
examination of
inclusions, materials
with strongly varying
structural elements,
steels with inclusions
Methanol (100 %) 900 mL
Acetic acid (glacial) 120 mL
Cobalt nitrate (II) 400 g
Iron (III) nitrate 40 g
Tartaric acid 140 g
Urea 4 g
Methanol and propanol are
mixed and tartaric acid is
dissolved in the mixture, then
the cobalt nitrate, the iron nitrate
and the urea is dissolved. At
last the acetic acid and butylcellosolve
are added.
Attention Methanol is a poison,
use fume hood.
5-1 W Distilled water 1000 mL
Sodium hydroxide 20 g
The NaOH content can be
increased to 100 g
13.3.4 Mechanical Preparation for Electropolishing
To shorten the polishing time and thereby improve the quality of the electropolished
surface, the specimen is normally ground on a number of SiC grinding papers before
polishing. In the Method Tables Section 13.3.6 only three grinding steps are stated. If
only ne grinding FG is indicated, often a plane-grinding step should be performed
before the FGsteps. If the polishing time should be reduced, it is recommended to use
ner grits of SiC paper, a rigid composite disk, or a hard polishing cloth both with dia-
mond for ne grinding and rough polishing see the Method Tables for the given mate-
rial inSection13.2.3.
Short Time Shock Polishing
In case of materials difcult to electropolish, the polishing time can be reduced to
12 s, in some cases repeated two to three times, when a mechanical preparation, in-
cluding the 3 m and even 1 m diamond steps are performed. In this way only an
electrolytical cleaning of the surface takes place.
13.3.5 ElectropolishingMethod Tables
In Section 13.3.6 a number of Method Tables are stated, containing the parameters for
electropolishing of a number of metals. The methods are calledEl-01toEl-25.
The user will nd the method for a specic material by using Table 11.1. The meth-
ods are alsostatedinthe Material/PreparationTables Section13.2.3.
Parameters
Preparationbefore the electrolytic polishing is statedwitha number of parameters ab-
breviations similar to the Method Tables of mechanical preparation see Section
13.2.2.
The electrolytic polishing andetching is statedwiththe following parameters:
Electrolyte. Anelectrolyte number will be stated. This number is takento Table 13.2,
whichindicates the formula of the electrolyte.
Area. The polished area in cm
2
, always 1 cm
2
0.16 in
2
. The current stated corre-
sponds tothis area.
Temp. The electrolyte temperature during the process in C F. The temperature
should not increase more than 10C above room temperature during the polishing
process. If polishing large areas or many specimens withshort intervals, the electrolyte
must be cooledsee Chapter 8.
Voltage. Voltage between specimen anode and cathode in V see Area above. Two
values are indicated: polishing andetching.
Current. Current amperage in A passing between the cathode and the specimen. The
process depends onthe correct current density, A per cm
2
in
2
.
FlowRate. The owof electrolyte throughthe polishing chamber. The rate is indicated
as low, medium, andhigh.
Time. Polishing and etching time in seconds, indicating the period of time the voltage
is on.
13.3.6 ElectropolishingMethods El-01 To El-25
This section contains 25 Method Tables for electrolytic preparation. The tables include
the data regarding preparation before the electropolishing, and the data for electropol-
ishing andetching.
The data for electropolishing are based on the use of a commercial available elec-
tropolisher see Section 8.6 that is able to control the stated data. The values indicated
refer to an area of 1 cm
2
0.16 in
2
. In the case of mounted specimens, the mounting
resininthe surface of the mount shouldnot be conductive see Section3.11.6.
Attention: Amixed electrolyte will often have a limited shelf life, the most used per-
chloric acidbasedelectrolyte No. 12 only approximately twomonths.
Trouble Shooting: See Section13.6.5.
Method TableElectrolytic Polishing Method El-01
Material: High carbon steels. Medium carbon steels. Manganese
and Mn alloys. Molybdenum and Mo alloys
Method El-01
Grinding/
Polishing
FG 1 FG 2 FG 3 Electropolishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
13 13
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
P220 P320 P500 Temperature
C F
2030
6886
2030
6886
Lubricant
Type
Water Water Water Voltage V 40 23
Rotation
Disk/Holder
300/ 150 300/
150
300/
150
Current A 1.82 0.20.3
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp
Force per
Specimen
N Ib
30 7 30 7 30 7 Flow Rate Medium Medium/
high
Time Minutes 0.51 0.51 0.51 Time s 68 25
Comments
Electrolytes: 12 or 11 can be used as alternatives. In case of inclusions, use elec-
trolyte 42.
Matherial: Low carbon steels
Method El-02
Grinding/
Polishing
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12 12
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Gri/Grain
Size m
C F
2030
6886
2030
6886
Lubricant
Type
Water Water Water Voltage V 3540 1,5
Rotation
Disk/
Holder
300/
150
300/
150
300/
150
Current A 1.82 0.20.3
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp Comp
Force per
Specimen
N Ib
30
7
30
7
30
7
Flow Rate Medium Medium/
high
Time
Minutes
0.51 0.51 0.51 Time s 8 5
Comments
Steels withvery lowcarboncontent couldbe ne groundwithP1000SiCpaper.
Electrolyte: Incase of inclusions, use 4-2.
Material: Gray cast iron. Malleable cast iron. Nodular cast iron
Method El-03
Grinding/
Polishing
FG 1 FG 2 FG 3 Electro-
polishing/
Etching
Electrolytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
Cloth,
napless,
hard,
wov, silk
Electrolyte No.
Table 4.4
14
Abrasive
Type
SiC SiC Dia,
spr or
susp
Area cm
2
1
Grit/Grain
Size m
P500 P1200 6 Temperature
C F
2030
6886
Lubricant
Type
Water Water Alco or
wat
Voltage V 80
Rotation
Disk/Holder
300/ 150 150/
150
150/
150
Current A 1.82
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp
Force per
Specimen
N lb
30 7 20 4.5 30 7 Flow Rate Low/medium
Time Minutes 0.51 0.51 45 Time s 46
Comments
Ingeneral, cast ironis not suitedfor electrolytic polishing.
If performed, the process should be short and etching should be chemical with
etchant No. 74 Nital Table 12.2.
The result can be improved by introducing a polishing step before the electropol-
ish, see stepP2inMethodT-30, andcut downthe electrolytic polishing to34 s.
Material: Heat treated steels
Method El-04
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte
No.
Table 13.2
13 13
Abrasive Type SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size
m
C F
2030
6886
2030
6886
Lubricant
Type
300/
150
300/
150
Alco
or
water
Voltage V 80
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 Current A 2 0.20.3
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp
or
Contra
Comp
Force per
Specimen
N lb
30
7
30
7
30 7 Flow Rate Medium Medium
Comments
Electrolyte: 1-2or 1-1canbe usedas alternatives.
Steels with a high CrNi content might not be electrolytically etched as part of the
process see MethodEl-05.
Material: Stainless steels. High alloy steels
Method El-05
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte
No. Table 13.2
12 12,
see below
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Sizem
C F
2030
6886
2030
6886
Lubricant
Type
Rotation
Disk/Holder
300/ 150 300/ 150 300/ 150 Current A 1.9 0.20.3
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp
Force per
Specimen
N lb
30 7 30 7 30 7 Flow Rate Low/medium High
Time
Minutes
0.51 0.51 0.51 Time s 12 up to 120
Comments
Etching: For stainless steels external electrolytic etching in oxalic acid 10 % at
6 Vin1015 s, canbe recommended.
Electrolytes: 13canbe usedas analternative. 2-1is suitedfor austenitic steels.
Insome cases FGcanbe reducedtogrit P500SiCpaper.
Material: Super alloys, Fe based
Method El-06
Grinding/
Polishing
polishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
aper
SiC
paper
Electrolyte No.
Table 13.2
11 11
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
C F
2030
6886
2030
6886
Lubricant
Type
Water Water Water Voltage V 4050
Roation
Disk/Holder
300/ 150 300/ 150 300/ 150 Current A 1.52 0.20.3
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp
Force per
Specimen
N lb
30 7 30 7 30 7 Flow
Rate
Medium High
Time
Minutes
0.51 0.51 0.51 Time s 1012 510
Comments
Electrolyte: 12and13canbe usedas alternatives.
Material: Iron, pure
Method El-07
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte
No. Table 13.2
11 11
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size
C F
2030
6886
2030
6886
Lubricant
Type
Water Water Water Voltage V 3035 1.5
Rotation
Disk/Holder
300/ 300 150/ 300 150/ 150 Current A 1.52 0.2
rpm/rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Comp
Force per
Specimen
N lb
30 7 30 7 20 4.5 Flow Rate Medium Medium/
high
Comments
Electrolyte: 12and13canbe usedas alternatives. Incase of inclusions, use 4-2.
Material: High-speed steels
Method El-08
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/
Cloth
SiC paper SiC paper SiC
paper
Electro-
lyte No.
Table. 13.2
12 See
below
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
P220 P320 P500 Temper-
ature
C F
2030
6886
Lubricant
Type
Rotation
Disk/
Holder
300/ 150 300/ 150 150/ 150 Current A 2
rpm/rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Comp
Force per
Specimen
N lb
30 7 30 7 30 7 Flow Rate Medium
Times
inutes
0.51 0.51 0.51 Time s 610
Comments
Etching: External electrolytic etching withoxalic acid10% at 510 Vin1015 s.
Electrolytes: 1-1and13canbe usedas alternatives.
Material: Low-alloyed tool steels
Method El-09
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12 12
Abrasive Type SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
C F
2030
6886
2030
6886
Lubricant
Type
Rotation
Disk/ Holder
300/ 150 300/ 150 300/ 150 Current A 1.82 0.3
rpm/rpm
Comp/
Contra
Comp or
contra
Comp or
contra
Comp
Force per
Specimen
N lb
30 7 30 7 30 7 Flow Rate Medium Medium/
high
Time
Minutes
0.51 0.51 0.51 Time s 610 510
Comments
Electrolytes: 1-1and13canbe usedas alternatives.
Material: Aluminum and Al alloys. Antimony and Sb alloys.
Beryllium and Be aloys. Bismuth and Bi alloys
Method El-10
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12 12
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
P500 P1200 P2400 Tempera-
ture
C F
2030
6886
2030
6886
Lubricant
Type
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 Current A 1.52 0.20.4
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 Flow Rate Low/medium High
Time
Minutes
0.51 0.51 0.51 Time s 515 1020
Comments
Cast Al with Si is not suited for electrolytic polishing. Al alloys with a low Si con-
tent canoftenbe polishedas Al alloys.
Electrolytes: 11and13canbe usedas alternatives.
Al-Cualloy shouldbe polishedwiththe electrolyte 13.
Etching: Often electrolytic etching is not satisfactory, chemical etching is recom-
mendedsee the Material/PreparationTables, Section13.2.3.
Fine grinding: By introducing grit P4000 SiC paper before electropolishing the
polishing time canbe shortenedanda possible relief reduced.
Antimony: The electrolyte 21canbe analternative.
Beryllium: The electrolytes 11and14canbe alternatives.
Material: Chromium and Cr alloys
Method El-11
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/
Cloth
SiC
paper
SiC
paper
SiC
paper
Electrolyte
No.
Table.
13.2
21
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/
Grain
Size
m
C F
2030
6886
Lubricant
Type
Rotation
Disk/
Holder
300/ 150 150/ 150 150/ 150 Current
A
1.82.2
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp
Force
per
Specimen
N lb
20
4.5
20
4.5
20
4.5
Flow
Rate
Medium
Time
Minutes
0.5
1
0.5
1
0.51 Time s 1015 510
Comments
Etching: Chemical etching is recommendedsee Material/PreparationTables 46.
Fine grinding: By introducing grit 4000 SiC paper and a rough polishing step see
MethodT-46, stepP1, the polishing time canbe shortenedor deformations inthe elec-
tropolishedsurface canbe avoided.
Material: Cobalt and Co alloys
Method El-12
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table. 13.2
31 31
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
C F
2030
6886
2030
6886
Lubricant
Type
Rotation
Disk/
Holder
150/ 150 150/ 150 150/ 150 Current A 1.82.5 0.10.2
rpm/rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
15
3.4
15
3.4
15 3.4 Flow Rate Medium Medium/
high
Time
Minutes
0.51 0.51 0.51 Time s 1015 510
Comments
Electrolyte: As analternative use phosphoric acid85%.
Material: Brass. Copper alloys. Pure Cu
Method El-13
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte
No. Table 13.2
32 32
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
C F
2030
6886
2030
6886
Lubricant Type Water Water Water Voltage V 1530 34
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 Current A 1.82.5 0.10.2
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp Comp
Force per
Specimen
N lb
20 4.5 20 4.5 20
4.5
Flow Rate Medium Medium/
high
Comments
brass: Having more than one phase, further ne grinding with SiC paper grit
4000 is recommended to shorten the electropolishing time. Also a mechanical polish-
ing stepwith3 mdiamondcanbe recommendedsee MethodT-49.
Copper alloys: See alsoEl-14.
Copper withoxides: See brass above.
Material: Bronze. Copper bearing alloys
Method El-14
Grinding/
Polishing
polishing/
Etching
Electro-
lytic
Polishing
Electro-
lytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte
No. Table 13.2
42 42
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
C F
2030
6886
2080
6886
Lubricant
Type
Rotational
Disk/Holder
rpm/rpm
300/ 150 150/ 150 150/ 150 Current A 1.52 0.10.2
Comp/Contra Comp or
contra
Comp Comp
Force per
Specimen N lb
20 4.5 20 4.5 20 4.5 Flow Rate Medium High
Time
Minutes
0.51 0.51 0.51 Time s 1015 1015
Comments
Bronze and other alloys with several phases see Method El-13 regarding prepara-
tionbefore electropolishing.
Material: Lead and Pb alloys
Methods: El-15
Grinding/
Polishing
polishing
Etching
Electrolytic
Polishing
Electroytic
Etching
Disk/Cloth SiC
paper
SiC
paper
Cloth,
napless,
hard
wov,
sil
Electrolyte No.
Table 13.2
11
Abrasive
Type
SiC SiC Dia spr
or
susp
Area cm
2
1
Grit/Grain
Size m
P500 P1200 6 Temperature
C F
2030
6886
Lubricant
Type
Water Water Wat-oil Voltage V 4060
Rotation
Disk/
Holder
rpm/rpm
150/ 150150/ 150 150/ 150 Current A 1.52
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
20
4.5
20
4.5
20
4.5
Flow Rate Low
Time
inutes
0.51 0.51 5 Time s 35
Comments
Etching: Chemical etching see Material/PreparationTables 52.
Electrolytes: 12, 21, and41canbe usedas alternatives.
Electrolytic polishing of Pb should only be last step in a mechanical preparation
process see MethodT-52.
Material: Magnesium and Mg alloys
Method El-16
Grinding/
Polishing
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
41
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/
Holder
150/ 150 150/ 150 150/ 150 Current A 1.52
rpm/rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 Flow Rate Low
Time
Minutes
0.51 0.51 5 Time s 1015
Comments
Etching: Often the surface is etched by the electrolyte. Chemical etching is recom-
mendedsee Material/PreparationTable 53.
Electrolytes: 12and14canbe usedas analternative.
Material: Nickel and Ni alloys. Ni-based super alloys
Method El-17
Grinding/
Polishing
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/
Holder
150/ 150 150/ 150 150/ 150 Current A 22.5
rpm/
rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 Flow Rate Low
Time
Minutes
0.51 0.51 0.51 Time s 10
Comments
Electrolyte: 21canbe usedas analternative.
Preparationbefore electropolishing: See MethodEl-13andT-56.
Short time shock polishing: Often a specimen, prepared according to M/PT 56
canbe cleaned by electrolytic polishing in12 s.
Material: Silver and Ag alloys
Method El-18
Grinding/
Polishing
FG 1 FG 2 FG3 Electropolishing
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12 12
Abrasive
Type
SiC SiC SiC Area cm
2
1 1
Grit/Grain
Size m
C F
2030
6886
2030
6886
Lubricant
Type
Rotation
Disk/
Holder
300/
150
150/
150
150/150 Current A 1.7
rpm/rpm
Comp/
Contra
Comp
or
contra
Comp Comp
Force per
Specimen
N lb
10
2.3
10
2.3
10
2.3
Flow Rate Medium Medium
Time
Minutes
0.51 0.51 0.51 Time s 10 510
Comments
Electrolyte: 11canbe usedanalternative.
Material: Tin and Sn alloys
Method El-19
Grinding/
Polishing
polishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/
Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 Current A 1.52
rpm/rpm
Comp/
Contra
Comp or
contra
Comp Comp
Force per
Specimen
N lb
20 4.5 20 4.5 20 4.5 Flow Rate Medium
Time
Minutes
0.51 0.51 0.51 Time s 10
Comments
Etching: Use chemical etching see Material/PreparationTables 59.
Preparation before electropolishing: To avoid deformation, a rough polishing step
canbe performedbefore electropolishing see MethodT-59.
See alsoMethodEl-10for antimony alloys.
Material: Titanium and Ti alloys
Method El-20
Grinding/
Polishing
polishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
12
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/Holder
300/ 150 150/ 150 150/ 150 Current A 2
rpm/
rpm
Comp/
Contra
Comp
or
contra
Comp Comp
Force per
Specimen
N lb
25 5.7 25 5.7 25
5.7
Flow Rate Medium
Time
Minutes
0.51 0.51 0.51 Time s 2030
Comments
Electrolytes: 1-1, 12, and21canbe usedas alternatives.
Material: Tungsten and W alloys
Method El-21
Grinding/
Polishing
polishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Area cm
2
1
Abrassive
Type
SiC SiC SiC
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 Current A 22.5
rpm/rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
20
4.5
20
4.5
20
4.5
Flow Rate Low
Time Minutes 0.51 0.51 0.51 Time s 1520
Comments
Material: Vanadium and V Alloys
Method El-22
Grinding/ FG 1 FG 2 FG 3 Electropolishing/ Electrolytic Electrolytic
Polishing Etching Polishing Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Tables 13.2
13
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/Holder
150/150 150/150 150/150 Current A 22.5
rpm/rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
15 3.4 15 3.4 15 3.4 Flow Rate Medium
Time
Minutes
0.51 0.51 0.51 Time s 10
Comments
Fine grinding: See MethodEl-11.
Material: Zinc and Zn alloys
Method El-23
Grinding/
Polishing
polishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
41
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/Holder
150/150 150/150 150/150 Current A 22.5
rpm/rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
15 3.4 15 3.4 15 3.4 Flow Rate Medium
Time
minutes
0.51 0.51 0.51 Time s 2025
Comments
Etching: Chemical etching can be recommended see Material/Preparation Tables
61.
Preparation before electropolishing: A rough polishing step can be performed to
avoiddeformationsee MethodT-61.
Electrolytes: 12canbe usedas alternative.
Material: Zirconium and Zr alloys
Method El-24
Grinding/
Polishing
polishing/
Etching
Electrolytic
Polishing
Electrolytic
Etching
Disk/Cloth SiC
paper
SiC
paper
SiC
paper
Electrolyte No.
Table 13.2
13
Abrasive
Type
SiC SiC SiC Area cm
2
1
Grit/Grain
Size m
C F
2030
6886
Lubricant
Type
Rotation
Disk/Holder
150/ 150 150/ 150 150/ 150 Current A
rpm/rpm
Comp/
Contra
Comp Comp Comp
Force per
Specimen
N lb
15 3.4 15 3.4 15 3.4 Flow Rate Medium
Time
Minutes
0.51 0.51 0.51 Time s 10
Comments
For preparationbefore electropolishing: See MethodT-62.
Material: Hard metals. Sintered carbides
Method El-25
Grinding/ FG 1 FG 2 FG 3 Electropolishing/ Electrolytic Electrolytic
Polishing Etching Polishing Etching
Disk/Cloth See
below
See
below
See
below
Electrolyte No.
Table 13.2
51
Abrasive Type Area cm
2
1
Grit/Grain
Size m
Temperature
C F
2030
6886
Lubricant Type Voltage V 1524
Rotation
Disk/Holder
rpm/rpm
Comp/
Contra
Force per
Specimen
N lb
Flow Rate Medium
Time Minutes Time s 1
Comments
Electropolishing can only be done as a shock polishing. The specimen is prepared
according to Material/Preparation Tables 67 except for the last step, which is done as
electropolishing, shownabove.
Preparation
Nondestructive preparation is used for metallographic/materialographic examination
in the eld on steampipes, boilers, etc., and for inspection of large structures like drop
forgings, weldings, etc. The preparation of the surface is along the same lines as for a
normal specimen; both mechanical and electrolytic preparation can be used. Portable
apparatus are available for mechanical grinding/polishing and electropolishing, either
cable- or battery-driven. A portable microscope is needed to check the prepared sur-
face before, inmost cases, a replica is made sothat the microstructure canbe examined
inthe laboratory. The process, apparatus, andconsumables are describedinPart I.
13.4.1 Mechanical Preparation
The same grinding and polishing media are used as stated in the T-methods see Sec-
tion 13.2.3. A surface of approximately 25 mm 1 in diameter is prepared to be sure
that a replica of 12 by 18 mm 0.5 by 0.75 in can be made. The prepared surface is
normally chemically etched before the replica is made. The preparation should be
done very carefully and the prepared area cleaned between polishing steps and before
replicationsee alsoManual Preparation, Section13.2.4.
Trouble Shooting: See Section13.5/6.
13.4.2 Electrolytic Polishing
Normally grinding before electropolishing is made mechanically by handor witha por-
table grinder. Often also a rough mechanical polishing is performed to shorten down
the electropolishing time and thereby improving the result. For electropolishing, the
data stated in Section 13.3.6 are used only the polished area and corresponding
voltage/current should be calculated. Etching can often be done electrolytically as part
of the polishing process.
Trouble Shooting: See Sections 13.5.4and13.6.5.
13.4.3 Replication
The prepared surface is controlled with a portable microscope to ensure that the sur-
face expresses a microstructure that canbe acceptedfor further examination.
The replica can be made either with a piece of plastic acetate lm or with an
amount of silicon rubber-based material positioned on the prepared spot see Section
7.11.2.
Plastic Film
The plastic lm, 12 by 18 mm0.5 by 0.75 in, normally made of methyl acetate, can be
used in two ways. It can be wetted on one side with a suitable solvent such as mono
methyl acetate and after a moment 510 s to dissolve the surface, pressed against the
prepared spot, or the spot can be wetted with the solvent, and the lm pressed against
the spot. It should be held against the work piece with stable, high pressure with a n-
ger, and it should be placed very carefully to avoid a movement parallel to the work
piece surface. It is important that the lm adheres to the work piece before it is re-
moved; usually a time of 1020 s is needed.
Incase the plastic lmis transparent, it may be difcult todistinguishthe details of
the microstructure. This can be improved by coating the backside with black paint or
tape. Another more complicated, but better type of enhancement is to place the replica
ina sputtering device producing aninterference layer onthe replica see Section9.6.5.
Silicone Rubber
The silicone rubber material is dispensed with a hand-operated dispensing gun di-
rectly on the prepared spot. The material will cure in 515 min and can be used at tem-
peratures from10C15F to180C350F.
When the replica is made it is placed on a glass slide with double adhesive tape to
improve the handling bothfor microscopy andfor ling together withthe report.
See also Section 7.11 and ASTM Practice for Production and Evaluation of Field
Metallographic Replicas E1351 inSection12.4.
13.5 Trouble ShootingHow to Improve Preparation Results
The goal of metallographic/materialographic specimen preparation is to produce a
specimen that gives a true picture of the microstructure, reecting the inuence of the
previous manufacturing process or any other process intended to inuence or change
the properties of the material.
If the material has inany way beentreatedwithaninuence onthe microstructure
as a result, either thermally, mechanically, or chemically, this change has to be visible
so it may be classied or graded. In many cases the purpose of the metallographic/
Fig. 13.1Part after torching, heavy thermal damage.
materialographic examination is the validation of the quality of the involved process.
Therefore, it is of utmost importance that the nished specimen, after metallographic/
materialographic preparation, displays the changes introduced during the manufac-
turing, nomore andnoless.
The preparationmust inno way change the structure whichmeans it must not add
any characteristics that have not been there before and, as important, it must not re-
move any of the characteristics that have been introduced during manufacturing. Oth-
erwise the metallographer may misinterpret the result shown in the microscope that
might result in either faulty parts being classied as being satisfactory, or good parts as
being scrap.
To illustrate the above here are a couple of examples: If a specimen is coated with a
thin layer of a soft material this coating can be smeared over the base material, indicat-
ing a thicker layer than actually exists. Thus the layer can be measured and accepted
evenif the actual layer thickness is insufcient.
More often it will happen that correctly manufactured parts are rejected because
of incorrect specimen preparation. If hardened materials are cut using insufcient
cooling the reached temperature might anneal the material, resulting in a lower hard-
ness. Thus, a complete batch of correctly treated parts might be scrapped only because
of faulty specimenpreparation.
The rst case, accepting faulty parts as correct ones, might be the most critical, but
the other, scrapping goodparts, canalsobe very costly.
Therefore it is essential that the prepared specimen shows what can be described
as the True Structure.
As shown previously, the entire preparation process can be divided into a series of
preparation steps, from cutting over mounting to grinding and polishing. All these
steps canintroduce preparationartifacts if they are not carriedout correctly.
In the following the individual preparation steps are listed and possible failures
that can occur during these steps are explained. Afterwards these preparation artifacts
andhowtoavoidor overcome themare discussedindetail.
13.5.1 Sectioning
There are several possible reasons for sectioning:
Toreduce the size of the workpiece andturnit intoa manageable sample.
Fig. 13.2Part after sawing, heavy mechanical damage.
Tobe able tomeasure or examine layers, coatings, hardenedzones, or welds.
Tobe able toexamine a part indifferent orientations or angles.
In all cases it is important to ensure that a representative part of the work piece is
taken out for further examination. Especially important when sectioning a part with a
surface treatment or some sort of layer is the correct angle of the cut. If the cut is not
carried out in an angle of 90 to the surface, the layer, coating, or hardened zone will be
enlarged, and the result is a kind of taper section, something used quite often on pur-
pose when mounting samples for easier measurement of layer thickness see Section
3.11.1.
Apart from that, the most important consideration to take when sectioning is to
avoid any mechanical or thermal inuence that could alter the structure. As previously
described, wet abrasive cutting is the most appropriate way of sectioning when also
time andeconomy are considered.
Most of the other sectioning techniques introduce either heavy thermal damage
such as after torching as shown in Fig. 13.1, or mechanical damage as is the case after
hacksawing to be seen in Fig. 13.2. In case of bandsawing, however, an acceptable re-
sult often can be obtained when the correct machine, saw blade, speed, pressure, and
cutting uidare used.
For this reason the following examples are concentrating on wet abrasive cutting
and bandsawing. However, also with these two methods, thermal or mechanical, dam-
age canoccur if care is not taken.
Thermal Damage
Thermal damage is a result of excessive heat generated in the cut. Either because of
insufcient cooling due to an insufcient amount of cutting uid in the actual cut or
because the feed speed is too high and thus too much heat is introduced see Section
2.3. Thermal damage can change the structure of the material to be examined which
especially is critical withheat treatedparts where these structural changes canresult in
wrong readings in the following microhardness tests. To avoid thermal damage make
sure that there always is plenty of cooling uid in the cut and that the feed speed is set
correctly, i.e., not toohighsee Figs. 13.7and13.8.
In wet abrasive cutting, also the selection of cut-off wheels is important. Wheels
with a hard bond release abrasive grains slower. That makes them more economical
but also less suited for cutting of harder materials, as blunt abrasive particles will not
cut properly, but instead introduce heat and result in thermal damage see also Section
2.3.5. At bandsawing, the type of sawblade is important see Section2.7.4.
Mechanical Damage
Wet Abrasive Cutting
Mechanical damage mostly occurs when cutting brittle materials or materials with
brittle or fragile coatings. In many cases damage rst occurs when the cut-off wheel is
exiting the part to be sectioned. If the force or the selected feed speed is too high, the
sample fractures easily. If it is not possible to use a lowpre-set constant feed-speed and
thus avoid the damage, it usually helps to support the sample with some similar mate-
rial or bondit ontoanother material using wax.
Whencutting coated materials it is very important to cut throughthe layer or coat-
ing into the base material as this then acts as a support. Otherwise the layer might be
pushed away from the base material resulting in cracks or delamination. During the
nal examination in the microscope it can be impossible to tell if this kind of fault is a
real fault from production or if it has been introduced during cutting. Cylindrical,
coated samples can, if possible, be rotated during cutting, thus securing support of the
coating over the entire circumference.
Bandsawing
Bandsawing, as a rule, always leaves more mechanical damage than wet abrasive cut-
ting. For most materials this damage, if all sawing parameters are correct, can be re-
moved through an effective plane grinding, but in case of a too low band velocity or a
too coarse pitch of the band, or both, an unacceptable mechanical damage can be de-
veloped. Also, feedspeedthat is toohighor a cutting uidthat is not enoughor is wrong
may give a very roughsurface withdeepmechanical damage.
13.5.2 Mounting
There are several reasons for mounting samples. The most commonreasonis simply to
get specimens withuniformsize andshape to facilitate future preparation. Inthis case,
requirements to the mounting techniques are limited. However, a few matters should
be considered.
If the sample to be mountedis sensitive to heat, coldmounting shouldbe preferred
to hot mounting, because the temperature during hot mounting can get as high as
180200C 350400F. Cold mounting is not really cold but temperatures seldom
exceed100C210F for a normal-sizedmount of 30 mm1.25 in diameter.
If the temperature is really critical then only slowcuring epoxy resins can be used.
To keep temperatures as lowas possible epoxy resins can sometimes even be cured in a
refrigerator. That takes a longer time but the temperature of the mount does not exceed
roomtemperature.
Some materials and fragile samples are sensitive to pressure. In this case, hot
mounting cannot be usedandcoldmounting must be utilizedinstead.
Impregnation
Porous materials are usually impregnated under vacuum and here epoxy resins are
used; most of the other resins will start boiling when exposed to a pressure below the
atmospheric pressure. Vacuumimpregnationhas several advantages:
Vacuum impregnation acts as a reinforcement of the sample because the resin
works as a bonding agent in the pores. This facilitates the following specimen
preparationas pull-out of material is eliminatedor at least reduced. Pull-out of par-
ticles during the nal polishing steps is very often the cause of deep scratches re-
sulting inlengthy reruns of the preparationmethod.
Colored dyes can be added to the epoxy resin to help distinguish between porosity
and pull-out. Very often uorescent dyes are used as these show up more brightly
than normal colors. This dye is added to the epoxy resin before impregnation. Dur-
ing impregnation all pores connected to the surface are lled with the dyed epoxy
resinandafter the preparationis nishedall the lledpores canbe identiedeasily.
Areas that are not lled can then be either unlled pores or pull-outs. The trained
metallographer canoftendetermine pull-outs frompores by looking at the circum-
ference of the hole. Pull-outs leave a more jagged edge than real pores see also
Section3.10.
Shrinkage
A general rule when cold mounting is that the faster a resin cures or the higher the
caring temperature gets, the higher the shrinkage. Shrinkage of the resincanresult ina
variety of preparationartifacts see alsoSection3.1.
Staining
Water, cleaning agents, alcohol, and etchants are trapped in the gap between specimen
and resin Cleaning is almost impossible and the different liquids will continue seeping
out of the gap and staining the specimen. This can produce problems both when exam-
ining the specimen, but also when etching the specimen, as some other liquid might
cover part of the surface, which then will not be attacked correctly see Fig. 3.1. When
hydrouoric acid is used for etching, this can even ruin the objective of the microscope
because the acid seeping out of the gap during examinationof the specimenmight etch
the glass.
Fig. 13.3Deformation after grinding on SiC grinding stone, grit 150.
Fig. 13.4Deformation after grinding on ZrO
2
/ Al
2
O
3
paper, grit 120.
Scratching
If the gap is large enough, coarse abrasive grains from an earlier preparation step can
be transferred to one of the nal steps, ruining the preparation result and contaminat-
ing the polishing cloth.
Edge Rounding
Gaps can also result in edge rounding of the sample, as the resin cannot support the
edge of the sample. However, when using modern preparation methods, this risk is
quite limitedsince the consumables usedtoday provide very goodedge retention.
Delamination
When resins with relatively high shrinkage are used for mounting of samples with po-
rous coatings, the coating can be pulled away from the substrate during the polymer-
izationof the resinThis is quite rare andnot explainedinthe section: HowtoOvercome
PreparationArtifacts.
Fig. 13.5Deformation after grinding on SiC paper, grit P1000.
Fig. 13.6Deformation after grinding on rigid composite disk RCD using 6 m diamonds.
As cutting or mounting, or both, not always are necessary operations the real speci-
menpreparationprocess usually is denedas grinding andpolishing.
Preparationtime shouldbe kept as short as possible. Inproductioncontrol, time is
important and the faster the specimens are nished the earlier production can con-
tinue. The secondimportant point is that shorter preparationtimes usually also reduce
costs for consumables andlabor.
The rst preparationstepis grinding.
Grinding
There are twoconsiderations whenthe grinding process is started.
Howis the surface nishfromthe previous cutting?
Are the specimens prepared as single specimens or are they clamped in a specimen
holder?
If cutting has been carried out correctly the surface nish is in many cases suf-
cient for immediate ne grinding. However, if the specimens are clamped together in a
holder, plane grinding has to be carried out rst to level all specimens in the specimen
holder at the same height.
In this case the correct grit/grain size of abrasive has to be selected to have a re-
moval rate high enough to achieve short grinding times, but on the other hand, not too
coarse to avoid unnecessary deformationwhichthenmust be removed inthe following
steps. Figures 13.3 and 13.4 showthe deformation after plane grinding with a grinding
stone, 150 grit and a ZrO
2
/ Al
2
O
3
grinding paper, grit 120, respectively, and the heavy
deformation is evident. Figures 13.5 and 13.6 show the much smaller deformation at
SiCgrinding paper grit P1000anda rigidcomposite disk RCD using 6 mdiamonds.
Especially with soft materials, very coarse grit sizes should be avoided. The defor-
mation introduced can be very deep and might take a very long time to be removed in
the following steps. It can even happen that fractured abrasive grains become embed-
dedintothe soft material during the preparationandmay disturbfuture preparation.
Like with cutting, sufcient cooling is required to avoid thermal damage of the
specimens. Water is in most cases sufcient but for water-sensitive materials other u-
ids like water-free oil can be used to avoid attack of the sensitive phases. Recirculation
cooling systems are advantageous in these cases because the uid is reused continu-
ously. However, in many cases even water-sensitive materials can be ground using wa-
ter as a lubricant during the rst step since plenty of material still is removed after-
wards andmaterial is removedbeyondthe damagedarea.
Polishing
After grinding to a sufciently ne nish the preparation is continued with polishing.
During polishing the last deformation is removed and a reective surface is produced.
A reective surface is necessary for examination in an optical microscope. Addition-
ally, the surface should be plane without height differences betweendifferent phases or
rounded edges. Otherwise a correct evaluation of the specimen might be difcult or
even impossible. Especially when working with very thin coatings, edge rounding can-
not be tolerated.
There are several ways to avoid edge rounding and unplaneness. Using the correct
mounting technique was already mentioned, but also the choice of polishing cloths is
very important for the result. Soft cloths usually give a better reectivity but can easily
generate unplane samples androundededges.
During polishing, a lubricant must be used to avoid any thermal damage. Espe-
cially during the nal stages of the preparation, water-free products must be used if the
material to be prepared is water sensitive. Otherwise certain phases might be attacked
or evendissolvedanda correct assessment is nolonger possible.
13.5.4 Electrolytic Polishing
As described in Section 8.3, electrolytic polishing is well suited for the preparation of
homogeneous materials whereas it is difcult, in most cases impossible, to get accept-
able results with heterogeneous materials. The most common artifacts are relief, miss-
ing inclusions see Fig. 8.6 andedge rounding see Fig. 8.8.
In any case, like with mechanical preparation, it is important that the consum-
ables used are in perfect condition. Take care that the correct electrolyte for the given
material is available see Section 13.3. The electrolyte must not be too old since impu-
rities in the electrolyte may cause phenomena that might lead to a wrong interpreta-
tion of the prepared specimen. Used electrolytes may be heavily loaded with metal ions
fromthe specimens. These ions can act as catalysts and reduce the lifetime of the elec-
trolyte which in turn will have a negative inuence on the following preparation.
Therefore the electrolytes must be discardedindue time.
13.5.5 General RulesThe Metallographers Rule of Thumb
Before the actual preparation process is started it is important to dene the purpose of
the specimenpreparation: Why amI going toprepare this specimen; what doI want to
evaluate?
If you are working with the inspection of incoming materials and have to check a
certain type of steel for a certain heat treatment, e.g., normalized, a short preparation
of an unmounted sample will in most cases be sufcient. A slight rounding of the edge
or a fewscratches will not inuence the examination. Inthis case it is important to get a
result ina very short time andinmany cases alsoat lowcost. Therefore a short prepara-
tionmethodwithfewsteps is selected.
However, specimens with very specic characteristics, such as a very thin coating
that has to be measured accurately, must be treated in a completely different way. Al-
ready during cutting great care has to be taken to avoid damage of the coating. The
sample should be mounted in a resin with lowshrinkage to prevent any edge rounding
and also the preparation method has to be selected carefully with regards to planeness
and edge retention. The entire preparation process will take longer, as in the previous
example, and the cost will be higher, but it is the only way to ensure that the correct
result is obtained.
When the purpose is established, use the Metallographers Rule of Thumb, when
a newpreparationprocedure shall be developed:
Put Up a Goal for Each Preparation Step
When following this rule, the result of every step is checked in the microscope. This is
to avoid that one of the early steps are not correctly made, a fact that often is not real-
izedbefore the nal polishing step, causing a repetitionof the whole process.
The above also means that you request as much information as possible if you are
askedtoprepare a newmaterial or a different kindof sample. Without having sufcient
information about the type of material, mechanical, chemical, or thermal treatment,
service history and request to the nal examination, it is very difcult to choose the
correct preparationmethodandtoput upacceptable goals for the preparationprocess.
13.6 Trouble ShootingHow to Overcome Preparation Artifacts
In the following sections the most important preparation artifacts are described in
some detail andsolutions onhowtoavoidor overcome themare presented.
Whenever a new method is established for a specic material, the specimens
should be checked under the microscope after every step to ensure that the
scratches, deformation, and other possible damage from the previous step have
beenremovedbefore continuing withthe next step.
The preparation times should be kept as short as possible without sacricing the
quality of the preparation. This usually results in specimens with better planeness
andedge retentionandsaves time andconsumables.
When utilizing fresh consumables like RCDs or polishing cloths where abrasive
has to be added, they have to be used for a while before they reach maximum per-
formance. Allowfor a slightly longer preparationtime inthe beginning.
The rst part of the preparation process, sectioning, does by and large not cause
very high requirements to the equipment used. But generally it can be said that at wet
abrasive cutting the more automatic cut-off machines can produce better or at least
more repeatable results thanmanual equipment.
Mounting depends much more on the correct choice of consumables than on the
equipment used, especially with cold mounting where no equipment except maybe a
vacuumchamber for the impregnationis employed.
With the grinding and polishing procedures it is a completely different situation.
To be able to achieve the best possible preparation results and to use the guidelines
stated in the following sections, the specimen preparation has to be carried out on ei-
ther semiautomatic or automatic equipment. Otherwise it is not possible to control
force, time, dosing levels, polishing dynamics and other preparation parameters and
consistent results canonly be accomplishedwithgreat difculty.
13.6.1 Preparation ArtifactsFlow Charts
The following artifacts are described both in words and pictures, and a ow chart is
used to show ways to improve the quality of the prepared specimen and avoid the
artifacts.
Sectioning
Thermal damage
Mechanical damage
Cracks
Delamination
Mounting
Staining
Scratching
Edge rounding
Grinding and Polishing
Scratching
Lapping tracks
Deformation
Smearing
Pull-outsFalse porosity
Embeddedabrasive
DestroyedinclusionsPull-outs
Edge rounding andrelief
Comet tails
Flow Chart Symbols
The symbols usedinthe owchart indicate the following:
13.6.2 SectioningGeneral ProblemsFlow Charts
Wet Abrasive Cutting
General Problems
As anintroductionto the owcharts for the specic artifacts connected to wet abrasive
cutting, a number of general problems with suggested solutions are indicated in the
table below.
Problem Cause Solution
Wheel does not cut
or stops cutting
after some time
Incorrect wheel, the
abrasive has
become blunt, or the
rim of the wheel
has been clogged
Use a softer wheel,
or in case of
very hard material
use diamond or
CBN as abrasive
Arc of contact too large Increase the force,
if possible
Use oscillating cutting
Wheel wears very fast Wheel is too soft Use a harder wheel
Wheel wobbles or
vibrates
Wheel is not straight Change wheel
Wheel is not clamped
correctly
Clamp the wheel
correctly
Wheel is too hard Use a softer wheel
or reduce the
speed of the wheel
Bearings of machine are defect Have machine repaired
Wheel breaks Feed speed too high Reduce the feed speed
Work piece has moved Clamp the work piece
correctly
Wheel bends while cutting Did the wheel attack a
tilting surface? Take care
that a notch is made
before the cutting starts
Check xation of work
piece
Disk brake effect,
the wheel is
pinched in cut
Internal stress in work
piece, lower feed speed
or preferable use
oscillating/step cutting,
clamp sample downwards on both sides
Wheel does not
cut straight
Wheel bond varies Change wheel
Work piece not clamped
correctly
Realign and clamp work
piece
Attack of wheel not
perpendicular
Change position of work
piece or
take care that the wheel
makes a notch before the
cutting starts
Feed speed too high Reduce feed speed
Signs of overheating
of specimen surface
Wheel is too hard or
too thick
Use a softer wheel or
a thinner wheel
Feed speed too low Increase feed speed
Wheel is clogged Used a softer wheel
Feed speed too high Reduce feed speed
Arc of contact too large Change position of
work piece or
use a softer wheel
Cooling not efcient Check the cooling system, the
level of the cooling liquid and the
positioning of the nozzles
Foam and smell from the
cooling liquid, or both
Additive to cooling
liquid is not active,
bacteria might have
developed
Check that the cooling liquid has
the correct additive content or
clean system using bacterial killer, or both.
Wet Abrasive CuttingFlow Charts
Thermal Damage
There can be different reasons for thermal damage of the sample during cutting.
Mostly thermal damage is directly visible as discoloration on the cut surface, as shown
in Fig. 13.7. A cross section through the discolored area shows how deep the thermal
damage extends, see Fig. 13.8. A correctly cut sample does not display any discolora-
tion and is free from any thermal damage, as shown in Fig. 13.9. The most common
reason is the lack of cooling uid during cutting. A relatively large amount of cooling
uid is needed to remove the heat generated during cutting. Therefore the
recirculation-cooling unit has to be monitored and the level of cooling liquid checked
regularly andrelledif necessary.
Another reason might be the wrong selection of the cut-off wheel. As described in
Section 2.6.1, different cut-off wheels are available for different materials. If a wheel is
used which is too hard for the material to be cut, free cutting cannot be obtained,
the specic pressure in the cut rises and overheating will take place. To avoid overheat-
Fig. 13.7Thermal damage after cutting with insufcient cooling.
Fig. 13.8Cross section of part shown in Fig. 13.7, deep thermal damage can be seen.
ing a softer wheel must be used. A softer wheel will break down faster, releasing more
abrasive grains andconsequently cut more efciently throughhardmaterials.
The same behavior can be achieved by reducing the speed of the cut-off wheel. If it
is possible to adjust the spindle speed on the cut-off machine the hardness of the
wheel can be modied. Lower speed makes the wheel act softer and higher speed pro-
duces harder wheels see Section2.3.8. Insteadof changing wheels whendifferent ma-
terials have to be cut, an adjustment of the wheel speed can simply compensate for the
variationinhardness of the different materials.
The third reason for thermal damage is very often a too high feed speed. Material
from the sample cannot be removed as fast as the wheel is moved into the cut. Free
cutting is not achieved and overheating is taking place see Sections 2.3.5 and 2.3.8.
Often the reason for using high feed speed is to save time. This is usually not a good
idea, since the time saved during cutting has to be used again in the grinding process to
remove the thermal damage. In many cases more time has to be spent than was saved
in the rst place. Therefore it cannot be recommended to go too fast during cutting; it
usually prolongs the total preparationtime insteadof reducing it.
Thermal damage during cutting can usually be avoided if these three guidelines
are followed:
Check and maintain the correct cooling uid in the recirculation-cooling unit. Di-
rect the cooling uidintothe cut.
Select the correct cut-off wheel for the material to be cut. If a variable wheel speed
is available it canbe usedinsteadof changing the cut-off wheel.
Adjust the feedspeeddepending onsample material andsize.
Fig. 13.9No thermal damage after cutting.
Abrasive Wet Cutting, Thermal Damage
Mechanical Damage
When cutting correctly, the total amount of applied energy can be transformed into
removal of material. If the feed speed is too high more energy is applied than can be
transformed. The excess energy has to be consumed somehow, and where it often is
transformed into heat resulting in thermal damage with metallic materials, it can re-
sult in the initiation of cracks in brittle materials as shown in Figs. 13.10 and 13.11.
Fig. 13.10Plasma sprayed coating with crack.
With solid materials we very often get cracks extending fromthe surface into the mate-
rial whereas we oftensee delamination, the separationof layers, withcoated materials.
Therefore special care has to be taken with ceramics and other brittle materials and
with coated materials. In Fig. 13.12 a delamination is seen; the coating is not in contact
withthe base material.
In many cases thermal damage is restricted to the area around the cut, whereas
cracks propagate deepintothe material.
Often materials are examined to see whether cracks or delamination have been
introduced during the manufacturing process. This means that cracks or delamination
that have been introduced during cutting might cause the entire series to be scrapped
or at least lead to a lot of extra work, because the production process will be suspected
to be faulty. This can be avoided by impregnation of the specimen before cutting using
an epoxy with a uorescent dye. In Fig. 13.11 a specimen is shown that has been
vacuum impregnated before grinding and polishing so when examined in the micro-
Fig. 13.11Prior to grinding and polishing, the sample was vacuum impregnated using an
epoxy resin with a uorescent dye showing up green when examined using uorescent light.
As the crack is completely lled with resin it was there before the grinding and polishing were
started. Whether it was there before cutting or created during cutting cannot be said.
Fig. 13.12Delamination between coating and base material.
scope it can be seen whether a crack existed before the preparation. The same type of
impregnationcanbe done before cutting.
To reduce the risk of introducing cracks during cutting a few simple rules should
be followed.
Always use moderate feedspeed.
Use the correct cut-off wheel for the material to be cut. In the case of coatings the
cut-off wheel should be selected to suit the majority of the material, e.g., a thin ce-
ramic coating on a steel bar should be cut using an abrasive Al
2
O
3
wheel suitable
for the steel bar instead of using a diamond cut-off wheel that would suit the ce-
ramic coating only.
Thin cut-off wheels should be preferred to thicker wheels because they remove less
material andthus introduce less energy.
With very brittle and fragile materials, vacuum impregnation prior to the cut can
reinforce the samples andprevent cracking.
With coatings: always cut through the coating into the base material. Thus the
coating is supportedall the time andthe riskof cracking is reduced.
Abrasive Wet Cutting, Mechanical Damage
Bandsawing
General Problems
When working with a vertical bandsawa number of problems can be experienced, and
belowthe most important of these are listed with suggested solutions see also Section
2.7.4.
Problem Solution
Premature dulling of teeth Decrease band velocity.
Use band with ner pitch.
Apply proper cutting uid when cutting ferrous
and nonferrous materials.
Keep teeth engaged. Do not allow the teeth to
idle through cut.
Increase feeding pressure.
Apply cutting uid at point of cut, saturating the
teeth evenly when cutting ferrous and
nonferrous alloys.
Be sure that band is running with teeth pointing
down.
Band vibrating in the cut Increase or decrease band velocity.
Increase band tension.
Hold work piece rmly.
Band teeth ripping out Use ne-pitch bands on thin work piece
sections.
Eliminate vibration by holding work piece
rmly while it is fed into the band.
Use cutting uid on ductile materials.
If gullets are loading, use heavier duty cutting
uid.
Reduce feed pressure.
Surface of nished cut too
rough
Increase band velocity.
Use slower feeding rate.
Apply correct amount of proper cutting uid.
Premature band breakage Change to band with gage that is not too heavy
for diameter of wheels and speed of the
machine.
Decrease band velocity.
Check periphery of wheels for defects.
Cracking at weld. Try longer annealing period,
decrease unit load by using ner pitch.
Decrease feeding pressure.
Decrease band tension.
Properly adjust band tool guides.
Apply cutting uid.
Band making belly-shaped cut Increase band tension.
Adjust guides close to work piece.
Use band with coarser pitch.
Decrease feeding pressure.
Gullets loading Use band with coarser pitch.
Apply cutting uid.
Lower band velocity.
Band not running true against
saw guide backup bearing
If clicking against saw guide backup bearing,
remove burr on back of band where joined.
If hunting back and forth against saw guide
backup bearing, re-weld with back of band in
true alignment.
Check alignment of band carrier wheels.
Check saw guide backup bearing, if worn or
unbalanced, replace same.
Negative camber developing in
band
Band riding too heavy on saw guide backup
bearing. Adjust band for alignment on top and
bottom wheels.
Cutting rate too slow Increase band velocity.
Use band with coarser pitch.
Apply cutting uid.
Band leading in cut Unbalanced set or partial dullness caused by
striking hard inclusion in material being cut.
Apply cutting uid.
Saw guides out of adjustment. Carefully readjust
guide inserts or rollers. If worn, replace same.
In the case of brush-equipped cut-off machines,
make sure brushes are properly adjusted, if
worn, replace with new.
Reduce feeding pressure.
Premature loss of set Band too wide for radii being cut.
Decrease band velocity.
Apply cutting uid.
Positive camber developing in
band
Reduce feeding pressure.
Use band with coarser pitch to permit greater
tooth penetration.
Saw guides too far apart, adjust closer to work
piece.
Band developing twist Band binding in cut, decrease feeding pressure.
Side inserts or rollers of saw guides adjusted too
close to band.
Wrong width of band for radii.
Decrease band tension.
13.6.3 MountingGeneral ProblemsArtifacts
General ProblemsHot Mounting
In the following overview some of the general problems that can arise during hot
mounting are shown and both cause and the possible solution are described see also
Section3.6.
General ProblemsCold Mounting
In the subsequent overviewsome of the problems that can arise during cold mounting
are shown and both cause and the possible solution are described see also Section
3.13.
Problem Cause/Solution
The surface of the mount is
sticky after normal curing time.
The components are not mixed in the correct
quantities, the mixing has not been correct or
the room temperature has been too low.
Mix carefully with the exact portions of each
component and check that the room
temperature is approx. 2022C 6872F.
Also cover the mounting cup so as to prevent
any reaction between the surface of the mount
and the air.
The mount is brown after
curing, too rapid curing.
The temperature during curing has been too
high.
Mix carefully with the exact portions of each
component and check that the room
temperature is approx. 2022C 6872F.
When using large amounts of resin make sure
that the mount is cooled during curing. Use
either a stream of cool air, a water bath or a
refrigerator.
It is very difcult to remove the
mount from the mounting mold.
The mounting resin epoxy has very little
shrinkage and good adhesion to all materials.
Use a more exible mounting mold or coat the
inner surface with a thin layer of silicone mold
release agent.
The mount is soft after curing,
not cured completely.
The components are not mixed in the correct
quantities or one of the components is too old.
Check the expiry date of the components and
make sure to measure the correct quantities of
each component. The mount can maybe be
saved by placing it in an oven at 4050C
100120F.
Specimen moves, turns, falls or
oats in the mounting mold.
The specimen is very light.
Coat the bottom of the mounting mold with
spray lacquer and position the specimen before
the lacquer is dry or use double adhesive tape
to secure the specimen.
Staining
Staining is the discoloration of the specimen surface through residues of liquids used
during preparation, cleaning, or etching of the specimen.
Sometimes staining is used to purposely contrast the specimen surface in order to
identify different phases, but here we are only talking about unintendeddiscoloration.
Staining usually occurs when the sample is not mounted correctly and there is a
gap between the sample and the mounting material. This gap is often lled with lubri-
cant that is accumulated there during polishing or with cleaning liquid or etchant that
has been used during the preparation process. Very often the gap is rather narrow, but
the capillary action lls the gap easily with liquid. Figure 3.1 Section 3.1.2 shows a
specimen surface with staining caused by a gap, and in Fig. 3.2b a correct mount is
seenwithout gapandconsequently without staining.
Toavoidstaining the subsequent rules canbe followed:
Always cleanand degrease the samples prior to mounting; this will provide a better
adhesionof the resintothe sample.
Select a resin with very low shrinkage; these usually are hot mounting resins con-
taining a ller material or epoxy resins for coldmounting. The epoxy resins provide
the best result, especially with vacuum impregnation; however, the long curing
time oftenprohibits their use.
Cleanthe specimencarefully after eachstep, possibly using ultrasonic cleaning.
Dry the specimen very thoroughly to avoid bleeding out of liquids during examina-
tionwiththe microscope.
Use a piece of soft tissue together with a hair dryer to make sure that all liquid is
removed from the gap. Be careful with soft materials that the tissue does not
scratchthe material.
After etching the specimen make sure that all etchant is removed from the speci-
men or the gap in the specimen, otherwise the specimen might start bleeding on
the microscope. This can destroy the specimen, or, if hydrouoric acid was used,
eventhe objective of the microscope.
Scratching
Scratching is usually not related to mounting; however, under certain circumstances a
poor quality of the mount might result inscratching of the specimensurface.
As with the previous example, incorrect mounting can result in a gap between the
sample and the mounting material. During preparation some of the abrasive particles
canbe trappedinthe gapandcarriedontothe following preparationstage, as shownin
Fig. 13.13. If the particles are falling out of the gap and stay on the polishing cloth they
will result infewbut distinct scratches.
Toavoidscratching because of poor mounting quality, followthese rules:
Fig. 13.13Abrasive grains in the gap between sample and mounting resin When these fall
out during preparation they will result in scratching.
Always cleanand degrease the samples prior to mounting; this will provide a better
adhesionof the resintothe sample.
Select a resin with very low shrinkage; these usually are hot mounting resins con-
taining a ller material or epoxy resins for coldmounting. The epoxy resins provide
the best result, especially with vacuum impregnation; however, the long curing
time oftenprohibits their use.
Cleanthe specimencarefully after eachstep, possibly using ultrasonic cleaning.
If abrasive particles are carried from one preparation step to a following step, it
will not only damage the specimen and require at least part of the preparation method
to be repeated, it will also require the contaminated polishing cloth to be exchanged.
The result is bothlonger preparationtime andincreasedcost see alsoSection13.6.4.
Edge Rounding
Mounting is often carried out to protect the edges of the sample, especially when the
sample is coated with very thin layers of another material. To be able to measure the
thickness of these layers accurately it is crucial that they are absolutely plane without
any rounding. The same is valid when microhardness testing has to be carried out very
close tothe edge; alsohere perfect planeness of the sample is required.
Todays selection of consumables for grinding and polishing has made the prepa-
rationeasier and faster as previously stated. Still, whenthe maximumedge retentionis
required it is usually not possible to avoid mounting the samples. The correct mount-
ing resin has to be selected carefully to avoid a gap between sample and mounting ma-
terial, and usually there are not so many choices. The best option when mounting
samples with porous or fragile coatings is epoxy resin because this can be used under
vacuumand will provide both a reinforcement of the coating and a mount without any
gap. For mounting of samples withvery hard coatings or the mounting of surface hard-
ened materials it can be advantageous to use hot mounting. In this case resins with
different ller materials are available. This makes it possible to select a mounting resin
that has similar wear characteristics as the material to be prepared. Thus a uniform
removal of material across the entire specimen surface is obtained and perfect plane-
ness and edge retention will be the result see Section 3.1.3. Figure 3.2a shows a
mount with a mounting material not in contact with the sample, causing edge round-
ing. InFig. 3.2b the correct mounting material adhering tothe sample is used.
13.6.4 Grinding and Mechanical PolishingFlow Charts
Scratching
The mechanical removal of material fromthe surface is carried out step-by-step using
continuously ner grain sizes of abrasive. The abrasive particles act as machining
tools, removing small chips of material. As a result, the surface is covered with unidi-
rectional grinding scratches getting smaller after every step of the preparation, disap-
pearing totally at the end, or at least being so small that they are no longer visible in an
optical microscope. The unidirectional pattern is achieved when the specimen is pre-
pared using some kind of automatic or semiautomatic preparation equipment as de-
scribed in Section 7.9. To avoid scratches on the nished sample, the specimen has to
be examined after every preparation step to ensure that all scratches fromthe previous
step have been removed completely before continuing to the following step. Otherwise
steps fromone of the early grinding steps might still be visible after nal polishing. It is
crucial that the specimen is checked carefully after every step because the removal rate
of smaller abrasives is much less than that of larger abrasives causing the polishing
times needed to be extremely long if a nal polishing step should remove scratches
from an initial grinding step. Figure 13.14 shows the very rough scratch pattern with
heavy deformations after plane grinding, in contrast to the pattern developed during
the ne grinding showninFig. 13.15.
It is also very important to clean the specimens carefully after every step as con-
taminationof a polishing clothquite easily canoccur. Scratching because of mounting
gaps has beendescribedinSection13.6.3.
Fig. 13.14Scratched and deformed surface after plane grinding.
Fig. 13.15Uniform scratching after ne grinding.
Scratching
Lapping Tracks
During mechanical preparationthe abrasive particles should act as small cutting tools,
machining chips from the surface of the specimen. This requires the abrasive grain to
be held rmly on the polishing cloth while the specimen is passing over it as the abra-
sive grainotherwise will start rolling.
Since we use loose abrasives that are added during preparation, this presents a
challenge to the polishing cloth used. The polishing cloth must be selected carefully
depending on the grain size of abrasive it is going to be used with and especially in
relation to the hardness of the material to be prepared. If the polishing cloth is too soft
the abrasive will disappear into the fabric and will not remove any material. If the pol-
ishing cloth is too hard the abrasive cannot be pressed deep enough into the cloth and
the abrasive may start rolling, resulting in lapping tracks. If the cloth is even harder, or
a rigid ne grinding disk withtoo highof a hardness is used, the abrasive might evenbe
pressed into the sample material and become rmly embedded see the section below
onembeddedabrasives.
Lapping on softer materials does not remove any material, it only introduces deep
deformation. The lapping tracks are easy to identify, they follow a straight line, like a
grinding scratch; however, it is interrupted as the abrasive grain is tumbling across the
surface, as shown in Figs. 13.16 and 13.17 in bright eld BF and differential interfer-
ence contrast DIC, respectively.
For informationonpolishing cloths see Section7.4.
Fig. 13.16Specimen with lapping tracks, BF.
Fig. 13.17Specimen with lapping tracks, DIC.
Lapping Tracks
Deformation
The entire mechanical preparationprocess is basedonthe removal of material through
grinding and polishing as described earlier. Any mechanical treatment will result in a
certain amount of plastic deformation of the surface of the specimen. It is the purpose
of metallographic/materialographic specimen preparation to remove the deformation
from the surface to allow for the examination of the true structure. Therefore,
metallographic/materialographic specimen preparation is carried out in steps to
gradually remove the deformation from the previous steps; see Fig. 13.18 that shows
the preparation process schematically fromthe surface left after cutting through plane
grinding, ne grinding, and polishing to a surface to be examined on the microscope
see also Section 7.7. However, very often some residual deformation is left after the
preparation is nished and that can lead to wrong conclusions; see Fig. 13.19 that
shows the remaining deformation from an earlier grinding step. Therefore, it is
Fig. 13.18The preparation process. Deformation is removed step-by-step.
Fig. 13.19Remaining deformation from preparation, following early grinding scratches.
important to follow certain preparation routines and to check the specimens fre-
quently during preparation.
Generally eachstep has to remove the material deformed during the previous step,
while at the same time only introducing a limited amount of new deformation. With
todays modern consumables the preparation of most materials can be reduced to
about four steps resulting in a deformation free sample surface. If these steps are not
carried out correctly deformation may be visible after preparation. Very often the de-
formation is rst visible after etching. Especially color etching will reveal even the
smallest amount of remaining deformationas showninFig. 13.20.
Fig. 13.20Color etched specimen, remaining deformation can clearly be seen.
Fig. 13.21Smearing on a soft type of steel.
Deformation
Smearing
Smearing is not as common as many of the other artifacts; however, it is important to
be aware of the possibility and the inuence smearing can have on the nal result.
Smearing usually happens with very soft materials, as shown in Fig. 13.21, and often
when soft materials are contained in layers. Instead of being cut cleanly the material is
pushed across the surface. Especially when the thickness of layers has to be measured,
e.g., copper and solder layers on a PCB, the correct thickness must be obtained, other-
wise the part might be not acceptable. As can be seen in Fig. 13.22 the soft solder mate-
rial has been deformed and dragged across the copper layer following a coarse grind-
ing scratch. The exact measurement of the different layers in this case is not possible.
Therefore, smearing is not acceptable and has to be avoided. Also, smeared material
may hide the pores inthe surface see Pull-OutsFalse Porosity, below.
Mostly the occurrence of smearing is due toone of the following reasons:
Wrong type of abrasive used. Abrasives that are too blunt cannot cut properly and
may result in smearing. Therefore diamond is the best choice of abrasive for the
rst, relatively coarse polishing steps. Diamond is the hardest known abrasive and
consequently will produce a clean cut over a long period of time. Polycrystalline
diamonds are superior for specimenpreparation.
Insufcient lubricant level during polishing. When the amount of lubricant added
to the polishing cloth is too low, the lubricant lmbetween specimen and cloth can
be imperfect and thus smearing can occur. The lubricant level should be main-
tained on a stable level throughout the entire preparation step in a way that the
polishing clothis moist but not wet.
Polishing cloths that are too soft. With soft polishing cloths the abrasive can be
pressed too deep into the textile and thus not create any cutting action. Change to a
harder polishing clothor increase the abrasive grainsize see below.
Abrasive grain size that is too small. This is similar to the above reason; small abra-
sive grains can also be pressed so deep into the fabric of the cloth that their cutting
action is nonexistent. Either increase the size of the abrasive used or change to a
harder polishing cloth to avoid the condition that the abrasive is pressed too deep
intothe fabric.
Fig. 13.22Smearing on a PCB. The solder material is smeared over the copper layer, following
a grinding scratch.
Smearing
Pull-OutsFalse Porosity
As stated earlier, the goal of metallographic/materialographic preparation is to show
the true structure. For most solid materials that is a relatively easy task, but porous
materials quite often produce a challenge, even to experienced metallographers. De-
pending on the type of material, the preparation process can produce either a too high
porosity level or a toolowlevel.
Porous, brittle materials usually display a higher porosity level than what is actu-
ally in the material due to fracturing of the material during cutting and plane grinding.
This fracturing creates pull-outs, cavities in the surface, and cracks see Section 6.3.2,
see alsopull-outs inconnectionwithinclusions inthe following section.
Ductile materials oftendisplay a too lowporosity since the softer metallic material
canbe smearedintothe pores during plane grinding, covering these up.
The following examples are taken from the same type of application, thermal
spray coatings, using two different types of materials where the above can be seen very
clearly. To reach the correct result, displaying the accurate porosity level with the same
routine can be used with both types of material. When preparing such a specimen for
the rst time it is important to monitor the porosity level throughout the entire prepa-
ration and rst continue to the following preparation step when the porosity level stays
constant. With brittle materials it will get smaller and smaller until it reaches the cor-
rect level as shown in Figs. 13.2313.26. At ductile materials the porosity level will in-
crease with ner and ner preparation steps until the nal, correct level is reached, as
showninFigs. 13.2713.32.
In both sections on false porosity the use of an RCD is recommended. Experience
shows that the constant supply of abrasive during preparation on an RCD gives the
most constant removal of material and thus is best suited for ne grinding of both soft
and hard porous materials when the correct porosity level has to be obtained. If the use
of an RCD is not possible the correct type of abrasive for the material in question
shouldbe selected.
Onhard, brittle materials diamondgrinding disks or diamondpads insuccessively
ner grainsizes shouldbe usedtoremove the damage fromplane grinding.
For soft materials ne grained SiC paper can be selected; however, it is important
to change the paper frequently to allowfresh, still sharp grains to remove material and
thus avoidsmearing.
Fig. 13.23Ceramic plasma sprayed coating after plane grinding, the porosity level is very high
due to many pull-outs.
Fig. 13.24Same specimen as in Fig. 13.23 after ne grinding, pull-outs are reduced.
Fig. 13.25Same specimen as in Fig. 13.23 after diamond polishing, pull-outs are further
reduced.
Fig. 13.26Same specimen as in Fig. 13.23 after nal polishing, correct porosity level.
Fig. 13.27WC/Co plasma sprayed coating after plane grinding. The surface is completely
smeared and the pores are not visible.
Fig. 13.28Same specimen as Fig. 13.27 after ne grinding. Most of the pores are still smeared
over.
Fig. 13.29Same specimen as Fig. 13.27 after 6 m polishing. Pores start to open up.
Fig. 13.30Same specimen as Fig. 13.27 after 3 m polishing. More pores are opening up.
Fig. 13.31Same specimen as Fig. 13.27 after 1 m polishing.
Fig. 13.32Same specimen as Fig. 13.27 after nal polishing on colloidal silica. Correct porosity
level.
Pull-Outs, False Porosity, Hard, Brittle Materials
False Porosity, Soft, Ductile Materials
Destroyed Inclusions
Many materials contain different types of nonmetallic inclusions. They are naturally
contained in the material or added to improve machinability. These inclusions have
different mechanical behavior than the base material; they can be harder or softer and
often they have other thermal expansion values resulting in relatively bad adhesion of
the inclusions tothe base material.
During metallographic/materialographic preparation these inclusions can be
crushed if they are very brittle see Fig. 13.33, or removed by a long napped polishing
cloth if they are soft, but the result is the same, partly or completely missing inclusions
in the base material. Apart from misleading results in the following microscopic ex-
amination, these inclusion particles, pulled out during the preparation can also result
inother preparationartifacts suchas scratching.
There is, however, another important group of inclusions, the water-sensitive in-
clusions. If not treatedcorrectly, the result after preparationwill be the same withthese
inclusions as with those described above; they will simply be missing when examining
the specimen see Fig. 13.34. This takes place if the polishing consumables used, espe-
cially during the last steps of the preparation, containwater.
Fig. 13.33Brittle inclusion, removed during polishing.
Fig. 13.34Missing water-sensitive inclusions.
Destroyed Inclusions
Embedded Abrasives
Contrary to pull-outs, no material is removed from the specimen, but during prepara-
tion, abrasive grains are embedded into the specimen surface. Also, this is unwanted
because the foreign matter will make interpretation much more difcult or even im-
possible. Embedded abrasives are only seen with relatively soft materials, and mostly
because they are prepared on preparation disks that are quite hard; this can be rigid
composite disks RCDs or hard polishing cloths, but even from SiC grinding paper
grains canbe embeddedinthe specimenmaterial.
This can pose a problem with certain composite materials. If they consist of both
hard and soft phases, RCDs and hard polishing cloths are recommended to keep the
specimens plane and avoid edge rounding. Therefore, a way has to be found to fulll
both requirements at the same time, plane specimens without embedded abrasive
grains. Figure 13.35 shows embedded abrasive particles after 3 mdiamond polishing
ina PbSnsolder, andFig. 13.36shows the same specimeninSEM.
To resolve the problem with embedded abrasive it is essential to know when the
abrasive particles became embedded. Therefore, the specimens have to be checked af-
ter every preparationsteptobe certain
Fig. 13.35Embedded abrasive 3 m diamonds in PbSn solder.
Fig. 13.36Same specimen as Fig. 13.35, SEM image of diamonds in the solder phase.
Embedded Abrasive
Edge Rounding and Relief
The goal of specimen preparation is to produce specimens showing the true structure.
This usually requires perfect edge retention and absolutely plane specimens. With
composite materials containing phases of very different hardness or materials with
thin, sometimes multiple coatings, this canpresent a serious challenge to the metallog-
rapher. Figures 13.37 and 13.38 showa composite material with relief and without re-
lief, respectively. Figures 13.39 and 13.40 show a coated material with rounded edge
andwithperfect edge retention, respectively.
Fig. 13.37Composite material with relief between bers and matrix.
Fig. 13.38Same specimen as Fig. 13.37 after correct preparation, perfect planeness.
Fig. 13.39Coated material with rounded edge.
Edge rounding has already been touched upon in connection with mounting in
Section 3.1.3; however, it is not always possible to mount the sample and in the follow-
ing some tips are provided to get good edge retention without mounting. Basically the
same rules are validtoavoidrelief betweenthe different phases inthe specimen.
Use rigid composite disks RCDs for ne grinding and relatively hard cloths for
polishing tokeepthe specimenat.
Use diamondas the abrasive because it cancut equally throughall phases.
Use polishing times as short as possible.
Use as fewpolishing steps as necessary, e.g., go directly from6 to 1 m polishing,
omit the 3 mstep.
Use a lubricant withhigher viscosity for the ner polishing steps.
Fig. 13.40Same specimen as Fig. 13.39 after correct preparation, perfect edge retention.
Fig. 13.41Specimen after unidirectional polishing with comet tails around the inclusions.
Edge Rounding and Relief
Comet Tails
Comet tails owe their name to their characteristic shape. They are found adjacent to
inclusions or pores and are the result of unidirectional polishing see Fig. 13.41. By
adjusting the polishing dynamics, comet tails canbe avoidedeasily see Section7.9.2.
As with the other artifacts we also assume here that the preparation process is car-
riedout onsome kindof semiautomatic or automatic equipment. Toachieve anaccept-
able polishing result it is necessary that the specimenis movedacross the entire surface
of the polishing disk andthat the specimenholder at the same time is rotatedaroundits
center. This is difcult to carry out manually, but most modern machines are designed
toutilize the entire preparationsurface andtorotate the specimens at the same time.
One reason to move the specimen across the entire preparation surface is to wear
the polishing cloth symmetrically, thus increase the lifetime and as result reduce the
cost of specimen preparation. But more important is that the specimen is subjected to
a unidirectional inuence from the polishing cloth. This is important as different
phases or constituents in the specimen react differently to metallographic/material-
ographic specimen preparation. If we are polishing a material with hard inclusions,
the inclusions will be polished slower thanthe rest of the material, and after a while the
inclusions will stick slightly out of the base material. As a result, less of the base mate-
rial will be removed in the shadow of the inclusion. When examined in the micro-
scope this characteristic feature will look like a comet tail. Apart from disturbing the
examination it will also make, for instance, correct automatic inclusion rating using
image analysis impossible, since the inclusions will seemlarger thanthey actually are.
To avoid comet tails it is important that the speed of the polishing disk and the
speed of the specimen holder or specimen mover disk in which the specimens are lo-
cated are almost the same. They must not be identical because the specimens other-
wise would run in exactly the same track over and over again, but they should be simi-
lar. As a rule of thumb the speed of the specimen holder should not differ more than
510 %fromthe speedof the preparationdisk.
This is only relevant during polishing where the removal rate is limited and the
relative softness of the cloths contributes to unevenremoval betweensofter and harder
phases. Grinding is carried out on hard supporting disks and the removal rate is much
higher. Here comet tails will not occur and therefore the speed of the grinding disk can
be much higher than the speed of the specimen holder to achieve a higher removal rate
andthus a shorter preparationtime.
13.6.5 ElectropolishingGeneral ProblemsArtifacts
In the following overviewsome of the problems and artifacts that can be observed dur-
ing electrolytic preparation are indicated and both cause and the possible solution are
displayed.
General Problems and Artifacts
Surface not polished
or only partly
polished
Current density insufcient
Electrolyte too old
Insufcient quantity
of electrolyte
Adjust the voltage
Renew electrolyte
Add electrolyte
Reduce the ow rate
Spots that have not
been polished
Gas bubbles Adjust ow rate
Check the electrolyte
temperature
Decrease the voltage
Etching of the
polished surface
Chemical attack of
grain boundaries
after switching off
the current
Remove the specimen
immediately when the
current is switched off
Choose a less corrosive
electrolyte
Phases in relief Polishing lm is
inadequate
Increase the voltage
Improve the mechanical
preparation
of the specimen
Polishing time too long Reduce the polishing time
Pitting Polishing time too long Improve the mechanical
preparation
Decrease the time
Voltage too high Lower the voltage
Insufcient anodic layer Reduce ow rate
Use a different electrolyte
Attack at the edge
of the specimen
Film too viscous or too thin Decrease the voltage
Increase ow rate
The center of the
specimen is
deeply attacked or not
polished at all
Polishing lm did not form
in the center of the
specimen
Reduce the ow rate
Add more electrolyte
Deposits on the
surface
Insoluble reaction products Renew electrolyte or try a
different one
Wavy surface or
residual
deformation
Polishing time too short
Flow rate too high or too
low
Rough surface after
grinding
Increase the time
Change the ow rate
Improve the preparation
prior to electrolytic
polishing
Electrolyte too old Renew electrolyte
Selective polishing because
of potential differences in
surface
heterogeneous material
Other electrolyte with
other polishing data or use
mechanical
preparation instead
Part III: Light Microscopy
14
Introduction
METALLOGRAPHY/MATERIALOGRAPHYCOMPRISES THEOPTICAL EXAMI-
nation of a material for the purpose of giving a qualitative and quantitative description
of that materials structure. The structure is characterized by size, shape, distribution,
density, orientation, andtype of phases, as well as microstructural defects see Fig. 1.2.
In this context, the light microscope is an important tool. In the following chapter,
the basic physical principles of reected light microscopy and the most important
methods of microscopic examination will be described in more detail. In Chapter 16 a
short introductiontoelectron-microscopy andscanning probe microscopy is given.
The optical effect of enlargement that occurs when one looks through the rounded
glass of a convex lens magnifying lens or loupe was known to the ancient Egyptians,
Greeks, and Romans. Today, a convex lens still serves as a magnifying glass for observ-
ing small objects, the useful magnicationis limitedto1015.
The rst microscope, consisting of two lenses, was probably built by either Hans
andZacharias Janseninabout 1590 inthe Netherlands or by Cornelius Drebbel around
1600. In connection with the growing signicance of the natural sciences in the 19th
century, microscopic observations in the elds of medicine, biology, and geology be-
came ever more important.
H. C. Sorby in England 1864 and A. Martens in Germany 1878 were the rst to
prepare metallographic polished sections of steel and cast iron, examine them by mi-
croscope, andsketchor photographtheir visible structure.
Microscopes used today are still built according to the old principle of a systemof
lenses placed together. Their essential elements are source of light, lens, eyepiece or
ocular, prism, mirror, andshutter andltering systems.
14.1 Visible LightTable 14.1Table 14.2
Light that can be seen by the human eye is an electromagnetic light wave with wave-
lengths of between 350 and 780 nm. Depending on the wavelength, the human eye sees
different colors see Table 14.1.
White light consists of a mixture of all the colors in the spectrum. Light of an even
wavelengthis monochromatic.
When wavelengths of a particular range are missing from a beam of polychro-
matic light, we see a mixedcolor Table 14.2.
TABLE 14.1Range of Wavelength of Visible Light and Color.
Range of Wavelength, nm Color
360440 violet
440495 blue
495580 green
580640 yellow/orange
640780 red
525
14.2 The Human Eye
The construction of the human eye is similar to that of a camera Fig. 14.1. Thanks to
the muscles in our eyes, the focal distance of their exible lenses 1 can be varied to
enable us to focus on any object at a distance between approximately 20 cmand inn-
ity. The inner diameter of the iris 3 can be varied to change the amount of light falling
into it. This variationproduces a sharp image onthe retina 2, the gray values of which
are received by receptor-rods, and the color values of which are received by the cones
and transformed into electrical impulses. These impulses are in turn transmitted via
the optical nerve 4 tothe brainwhere they are thenprocessed.
For example, let us look at a 160 m 490 ft high tower from a distance of about
300 m915 ft. If we imagine two lines that extend fromthe middle of our eye, one to
the foot of the tower and one to the top, we get what is called the visual angle. In this
example, the visual angle is about 30 degrees. We are not able torecognize the faces of
people on the tower because the visual angle is too small for our eye to process. But if
we go closer to the tower, then we can better recognize the details of the building and
the people. This means that the closer we bring an object to our eye, however, thereby
increasing the visual angle, the more details we are able todiscern.
Normally, we are able to read the text on a page of a book froma distance of 25 cm
10 in. This distance is called the conventional visual range, or visual range of refer-
ence. It enables us tocompare the magnicationdata of different optical systems.
To make out the details of the individual letters on that page of text, we must de-
crease the visual angle. If we bring the text closer to our eyes, in order to increase the
TABLE 14.2Spectral Color Filtered Out and Visible Mixed Color.
Spectral Color Filtered Out Mixed Color
Violet Green-yellow
Ice blue Orange
Yellow Ultramarine blue
Red Blue-green
Fig. 14.1Light path of the human eye, with lens, cornea 1, retina 2, iris 3, optical nerve
4.
1
visual angle further, the text begins to blur because the ability of our lenses to adjust to
the visual angle is limited.
14.3 Magnifying Lens and Microscope
Magnifying glasses and microscopes are optical devices that enable us to increase the
visual angle between the eye and objects that are small and near so that details that
cannot be seenwiththe unaidedeye nowbecome visible.
If we place a convex lens magnifying glass between our eyes and the page of text,
the visual angle is increased and the details of individual letters as well as the surface
structure of the paper become visible.
A magnifying glass produces an enlargement by means of a single imaging step.
The object lies in the center of focus and the eye is accommodated ad innitum. The
smaller the focal point of the magnifying lens, the greater the magnication. Practi-
cally speaking, a magnication of the object of 10 up to a maximum of 15 times its
actual size remains inthe useful range.
By using several lenses arranged one after the other, the magnication effect can
be increasedconsiderably.
The construction of the classical microscope consists of a two-lens system. The
magnication takes place in two image-forming steps. First, an enlarged image of the
object is projected by the objective in the intermediate image plane. This image is then
magniedby the ocular, or eyepiece.
14.4 Magnication
Magnication, M, as the functionof anoptical instrument is denedas:
M=
Visual angle with optical instrument
1
Visual angle without optical instrument
2
1
or
M= tan
1
/tan
2
2
Magnification by a compound microscope results as a product of the magnification of the
objective andthe magnificationof the eyepiece
M= M
objective
M
eyepiece
3
15
The Optical Reected Light
Microscope
15.1 The Path of Light Rays
FIGURE 15.1 SHOWS THE COURSE OF LIGHT RAYS IN A MODERN THREE-
lens transmitted light microscope with innity optics the ICS principle, which
means Innity Color-corrected System. Let us follow the light rays that emanate
from an object 1. From these rays the objective 2 projects an image to innity. The
intermediate lens 3 that also intervenes in the progress of the light rays creates a mag-
nied intermediate image 4 from the rays that are now running parallel. This inter-
mediate image is further magnied by the eyepiece 5. As the illustration shows, the
visual angle
1
that results whenthis optical systemis used is considerably greater than
it is when the object is viewed by the naked eye at the same distance of 25 cm10 in,
visual angle
2
.
15.2 The Objective
The objective consists of a combination of lenses, both converging and diverging, that
are precisely adjusted to one another. This makes a correction of any part of the image-
forming process possible whereby something has been lost, e.g., missing color, and a
at intermediate image is projected.
The angle of opening 2, the aperture of the objective lens system, is crucial for the
quality of a microscopic system Fig. 15.2. An effective aperture is one that is as large
as possible so that as many diffraction spectrum maxima as possible of the rays re-
ected by the object can be captured and an image rich in detail consequently ren-
dered.
If, withregardtothe illumination, one uses a condenser lens systemFig. 15.2 that
concentrates the initially parallel rays intoa cone, the objective canthencatchrays that
are even more diffracted. This means a greater optical resolving power and, conse-
quently, more detail.
For technical reasons, the angle at which a ray of light can enter into the objective
is maximally =72.
15.2.1 Numerical ApertureResolution-MagnicationTable 15.1Table
15.2
The numerical aperture, by means of which a comparison can be made between two
objectives, is denedas follows:
NA= n sin 1
Inthis equation, is half of the aperture angle of the objective.
If air is present betweenthe objective andthe object, the refractive index, n1 see
Table 15.1.
528
Under comparable conditions, maximum achievable image brightness is propor-
tional toNA
2
.
The greater the aperture of the objective and the shorter the light wavelength
the better one can distinguish two adjacent image points fromone another. The short-
est distance d
o
is a measure of the resolving power of the microscope. This is shown
schematically inFig. 15.3.
According to the laws of wave optics, one has achieved this distance d
o
when a
maximumdegree of refraction is emitted fromeach of two image points that are sepa-
ratedfromone another by a minimumof refraction.
Ernst Abbe has dened this relationship mathematically with the following equa-
tion:
Fig. 15.1Optical path A in a three-lens transmitted light microscope with innity optics with
the visual angle
1
compared to the visual angle
2
, when the object is viewed by the naked
eye in beam path B. With object A and B 1, objective 2, tube lens 3, magnied
intermediate image 4, eyepiece 5, eye 6.
1
Chapter 15 The Optical Reected 529
d
o
=

NA
Objective
+ NA
Condensor

2NA
2
Example: If we assume that the aperture of the objective and the condenser is 1.25
and a wavelength in the middle range of 0.5 m, respectively, we receive, as the
smallest distance possible between two object points that can just be distinguished, a
d
o
value of 0.2 m.
TABLE 15.1Immersions Agents, Their Refractive Index, and the Possible Numerical Aperture.
Medium Refractive Index (n) Numerical Aperture NA
Air 1 to 0.95
Water 1.333
Immersion oil 1.515 to 1.4
Monobromonaphtalene 1.66
Methylene iodide 1.740
Fig. 15.2Optical path of a condenser lens system with object in transmitted light 1, light
beam 2, objective 3, condenser 4.
1
The resolving power can be improved by using light of shorter wavelength and a
larger aperture inthe objective. Withthe use of white light, if one takes a mediumwave-
length of 0, 56 m and an immersion objective with an aperture of 1.4 and with k
=0.61, a resolving power of 0.25 m results. For blue light with a wavelength of
=0, 49 m, one gets a resolving power, under otherwise identical conditions, of about
0.2 m. Table 15.2 shows some values of resolutions that are theoretically possible for
various objectives and for a wavelength of 0, 55 m. Here, d
o
is the distance between
twopoints onthe object andD
o
is the point distance onthe intermediate image.
In actual practice, the attainable resolution is usually less than the theoretical val-
ues stated in Table 15.2. It is dependent on the quality of the objective, the optimal set-
ting of the aperture diaphragm, use of the right immersion oil and, naturally, the speci-
men. One gets the best results with dust-free microscope systems and clean objectives
andwell preparedspecimens.
The overall magnicationof a microscope is the product of the scale magnication
of the objective multipliedby the ocular magnication.
The magnication number indicates how many times larger the intermediate im-
age producedby the objective is thanthe object itself.
M= M
objective
M
eyepiece
3
With a 50 objective and a 10 eyepiece the overall magnication of the micro-
scope is 500.
Commonly usedare 5, 10, 20, 50, and100-objectives.
Additional magnications gained through the use of between-lenses or zoom-
devices are tobe borne inmind.
M= M
objective
M
eyepiece
M
between-lens or zoom-device
4
Fig. 15.3The shortest distance d
0
between two adjacent image points. The shortest distance
is a measure of the resolving power of the microscope.
The magnications achieved individually by the objective, the intermediate lens,
and the eyepiece must be attuned to one another. One obtains optimal image quality
with an objective of a high scale number in combination with an eyepiece of lowmag-
nication. For example, the combination 50-objective and 5-eyepiece is preferable
tothe combination10-objective with25-eyepiece.
The total magnicationof a microscope shouldbe from500 to a maximumof 1000
times the aperture of the objective. This is the maximum useful magnication that al-
lows the objective to reproduce tiny details in which the intermediate image can then
be magniedfurther by the eyepiece.
The numerical aperture of an objective increases with the objective magnication,
while the depth of eld decreases. It is possible to increase the depth of focus, within
limits, by lowering the aperture diaphragm. But this is done at the cost of resolution.
Setting the aperture diaphragmtoo lowresults in empty enlargements and blurred im-
ages inasmuchas one thereby leaves the range of useful magnication.
In the case of dry objectives, there is air between the front lens and the object. A
maximum aperture of 0.95 is possible. In the case of immersion objectives, use of cer-
tain immersion agents with a higher refraction index between the front lens and the
object makes possible an increase of the numerical aperture to 1.7. This is shown in
Fig. 15.4.
Table 15.1 shows some values of immersions agents, their refractive index and the
possible numerical aperture.
The numerical aperture NA is of essential signicance for:
Maximumimage brightness
Resolving power
Useful total magnication
Depthof focus
15.2.2 Aberrations in Image-Formation
Geometric and chromatic aberrations in image-formation are possible with uncor-
rectedoptical systems.
Geometric aberrations in the imaging process can occur even with monochro-
matic light. These include:
Aperture errors: With light beams on a plane parallel to the axis, the convergence
on the image side occurs not in the ideal image plane but rather either in front of it in
the case of converging lens or behindit inthe case of dispersing lens.
Coma: Off-axis point objects appear as asymmetrical areas witha comet-like tail.
Astigmatism: Point objects appear not as point images but rather as line images.
Curvature of eld: The image points of a larger object do not lie on a plane but
TABLE 15.2Values of Resolutions that are Possible for Various Objectives and for a Wavelength of 0, 55 m.
Objective NA d
o
/ m D
o
/ m
5 0.15 2.2 11.2
10 0.30 1.1 11.2
40 0.75 0.45 17.9
40 1.3 oil 0.26 10.3
63 1.4 oil 0.24 15.1
100 1.3 oil 0.26 25.8
instead on a curved surface. With uncorrected optical systems one can therefore focus
sharply either onthe center of the image or else onperipheral zones.
Distortion: The image scale is dependent on the distance of the image point from
the optical axis. Increasing that scale leads to a pillow-shaped distortion. Decreasing
the scale results inbarrel-shapeddistortions.
With the polychromatic light used in microscopy, chromatic aberration can also
occur.
Since the refractive index decreases with an increase in wavelength, the focal
lengthof a lens for these light rays increases. The image of anobject point, produced by
short-wave light violet lies in front of the image produced with long-wave light red.
Undesirable color fringes are the result.
The chromatic difference of spherical aberration manifests itself in blue and yel-
lowfringes.
With an appropriate combination of converging and dispersing lenses made of op-
tical glass with varying dispersive and refractory properties, these aberrations can be
correctedandobjectives withvarying optical properties canbe produced.
15.2.3 Available Objectives
Depending on the purpose for which they are used and the quality that is required of
the microscopic image, various corrected objective lens systems are available for selec-
tion.
The objectives most often used are achromats. They are inexpensive because they
consist of relatively few lenses. Spherically they are corrected for one wavelength and
chromatically for only two wavelengths, usually red and green. This may lead to red
and blue color fringes around the object, but this can be avoided to a large extent
through the use of a green lter. Because the atness of eld is limited, they are appro-
priate for visual elds of up to approximately 18 mmin diameter. These objectives can
be used for routine tasks, including those as in polarized light. They are less useful for
Fig. 15.4Improved resolution by use of an immersion liquid 6 between object, over slip 5
and objective 3.
1
microscopy in darkeld and for color photography, especially when there is a high de-
gree of magnication.
Withuorite or semiapochromatic objectives, spherical and chromatic aberration
is more strongly corrected. Flatness of eld is also improved. For these reasons such
objectives can be used for elds of vision of up to 23 mmin diameter and are appropri-
ate for color microphotography in reected light and transmitted light as well as for
darkeldandDIC.
With apochromats, spherical aberration is corrected for two colors and chromatic
aberration for three colors. Because of their even further improved atness of eld,
these objectives can be used for elds of vision of up to 25 mm in diameter. And be-
cause color fringes hardly ever occur, these high-quality objectives are well suited for
color photography and for microscoping in dark eld. Because of the better image cor-
rection, higher numerical apertures are possible and consequently a better resolution.
These objectives are therefore appropriate for the upper range of magnication to dif-
ferentiate the nest details precipitations, grainboundaries andcapture themintheir
true colors. This means, however, less depth of eld and a smaller working distance
betweenobjective andobject incomparisonwithachromats.
Plan apochromats and epiplan apochromats exhibit an outstanding atness of
eld and can therefore be used for large elds of view. Furthermore, since they possess
color correctionfor four wavelengths, the color rendering is optimal. The highnumeri-
cal aperture makes a maximum of resolution power possible. These objectives in the
upper price range satisfy the highest demands inresearchandtechnology.
Objectives are usually marked with color rings corresponding to their magnica-
tions: red-5, yellow-10, green-20, blue-50, white-100.
The most important technical data are also inscribedonthe barrel of the objective.
For example,
Epiplan-Neouar
10/ 0, 30HDDIC
/ 0
provides the following information:
Epiplan means that this is an objective for a reected light microscope that ren-
ders a attened intermediate image. Fluar refers to the uorite glass with which the
objective has beenconstructed.
The indicated scale number 10 means that the intermediate image is 10 times
larger thanthe object.
0.30 is the numerical aperture of the objective.
Using a light with an assumed wavelength of =500 nm, a resolving power of
1 mcanbe calculated.
HDDIC means that this objective can be used for bright-eld BF illumination,
dark-eldilluminationDF, anddifferential interference contrast DIC illumination.
On most microscopes, objectives of varying scale number are exchangeable with
the rotatory nosepiece. To keep the focus essentially unchanged, the distance between
the screw-onsurface of the objective andthe eyepiece headis animportant mechanical
dimension. It is calledthe mechanical tube lengthandis engravedonthe objective.
If is indicated there, this means that the object is imaged to innity by the ob-
jective andthat anadditional tube lens produces a real intermediate image.
With a transmitted light microscope, objects are placed on a glass stage and pro-
tected by a cover glass. Consequently, transmitted light objectives are calculated and
correctedfor a cover glass thickness of 0.17 mm.
In our example we are looking at an objective for reected light microscopy. Be-
cause one usually examines uncovered specimens, the cover glass thickness is repre-
sentedas a 0.
15.3 Eyepieces
The simplest eyepieces consist of a convergent lens that acts as a magnifying glass.
Goodeyepieces are equippedwitha correctedlens systemincluding aneye lens above
and a eld lens below. Figure 15.5 shows a schematic cross section of an eyepiece
with the position of the intermediate image plane 1, the boundaries of the visible eld
of vision 2, the eyepiece optical system 3, the pupil of the observers eye 4, and the
focusing ring for the diopter adjustment 5.
Although eyepieces magnify the intermediate image that is produced by the objec-
tive, they do not bring about any further improvement inresolving power. But since the
angle of visionis nowlarger, the humaneye is able todiscernmore detail.
If aberrations are still present in the intermediate image, they can be corrected
withthe appropriate eyepieces.
Many eyepieces are designed for people who wear eyeglasses. They are usually
equipped with eyecups. The eyecups can be attached or they can be folded up to get the
right visual distance if the individual wants touse the microscope without eyeglasses.
The area of the intermediate image that can be examined, the eld of view, is re-
stricted by the eld lens and the aperture diaphragm. The value S is the measure of the
eldof visionandis indicatedonevery eyepiece.
The diameter of the eld of visioncanbe calculated fromthe eld of visionvalue of
the objective together withthe objectives scale number:
Fieldof visionvalue S/Mobjective
An example: If M objective =40 and S eyepiece =18 mm, the result is a viewing
eldof 0.45-mmdiameter.
Wide-eld eyepieces should be used only in combination with corrected plane ob-
jectives that produce a well attenedintermediate image.
Micrometer eyepieces have a glass plate with a scale situated on the plane surface
of the diaphragm. After the systemhas been calibrated, linear measurements as well as
Fig. 15.5Schematic cross section of an eyepiece, with the position of the intermediate image
plane 1, the boundaries of the visible eld of vision 2, the eyepiece optical system 3, the
pupil of the observers eye 4 and the focusing ring for the diopter adjustment 5.
1
measurement of angles goniometric eyepiece can be made. The corresponding stan-
dardguides for calibrating are cited.
A tip: The eyepiece can also be used as a magnifying glass. Simply turn the eye-
piece, trainthe eye lens onthe object, andlookthroughthe eldcondensing lens.
15.4 Illumination
Illuminationsource andlight pathare important elements of a microscope.
Halogenlamps are oftenused, as are xenonhigh-pressure lamps.
Halogen lamps of between 25 and 100 watts emit light with a color temperature of
about 3000 K. This must be kept in mind when colored photographs are being taken
andconversionlters must be usedfor correction.
Xenonhigh-pressure lamps that produce between100 and500 watts are available,
and they produce a light that is more like natural light. Spectral response of the radi-
atedlight andcolor temperature are about 5000 K.
Amicroscopes illuminationshould
Be adaptedtothe illuminatedobject eld.
Illuminate completely andevenly the object eldtobe observed.
Be such that the illuminated object eld is adapted to the eld of vision of the mi-
croscope.
Be adjustable according tothe aperture angle.
15.4.1 Koehlers Illumination System
The illumination system proposed by August Koehler in 1893 is still used today with
many optical systems using transmitted- andreected-light microscopy.
The Koehlers illumination method produces images that are illuminated with
evenly distributed light using three lenses placed between the light source 1 in Fig.
15.6 and the reector 2. This type of illumination also contributes to the enhance-
ment of the resolution power. On reected-light microscopes used for metallography/
materialography the Koehler illumination system is adjusted by the microscope fac-
tory and should not be changed by the user, for transmitted light, the system shall be
adjusted regularly. The three lenses of the Koehler system are part of the illumination
elements A in Fig. 15.6. As the rst lens in front of the light source 1, the collector
lens forms an image of the light source at the second lens, the rst condenser lens. The
third lens, the second condenser lens, reproduces the image of the light source in the
back focal plane of the objective 3 after passing the reector 2. In this way the sur-
face of the specimenis uniformly illuminated.
Inthe pathof the illuminating light rays there are twoimportant diaphragms.
The centering radiant eld diaphragm makes it possible to adjust the illuminated
object eld to the microscopes actual eld of view. This diaphragm is correctly set
when the image of the edges of the diaphragmdisappear behind the border of the eld
of vision. Stray light is avoided and contrast is heightened. With reected-light micro-
scopes a one-time setting of the elddiaphragmis sufcient; it does not have tobe read-
justedeachtime the objective is changed.
By means of the aperture diaphragm, the cone of light is adjustedtothe aperture of
the objective. It has an optimal setting when that part of the light rays that is not dia-
phragmed out covers about two-thirds of the objectives entrance pupil. This dia-
phragm must be reset whenever the objective is changed to meet the requirements of
the desired image. This means that a compromise must be made between resolution,
contrast, anddepthof focal eld.
15.5 Microscope Options
The optical elements of a microscope, i.e., the objective, tube lens, eyepiece or projec-
tive, illuminators withlight source, aperture and light eld diaphragmare assembled
ina mechanical device, the microscope body.
Depending on the expandability and capability of the built-in optical and me-
chanical assembly parts, one differentiates between student microscopes, laboratory
microscopes, andresearchmicroscopes.
Student microscopes are the most simply built and therefore the most limited in
their uses. The interchangeability of the individual optical elements is limited. Because
of their ease of use these microscopes are appropriate for the beginner or are used for
the preselectionof specimens.
Laboratory or working microscopes are equipped in such a way that they can be
Fig. 15.6Bright eld BF illumination in reected light and components in the optical path
for establishing contrast: Light source 1, beamsplitter, color neutral 2, objective 3, object
4, lens 5 and contrast components on the side of the lamp A, on the side of the eyepiece
B and components for both light paths C.
1
used without problem for many routine tasks. The stage can be rotated or can be ad-
justed in an x-y-direction, or both, and the focusing of the objective occurs through a
coarse andne focusing mechanism.
As an illumination source, a halogen bulb is mostly used. Koehler illumination as
well as interchangeable objectives and lters make it possible to perform all the usual
examination procedures. Attachment possibilities for further xtures, as for example
analogue or digital cameras, are present.
Research microscopes belong to the top class of instruments. With these micro-
scopes all the essential parts, such as lamp-housing, condenser turret, object holding
stage, objective rotator, and tubes are interchangeable and can be adapted to special
tasks. Specimens can be viewed in either reected or transmitted light. All known
methods of microscopic examinationare possible.
The motorizedvariants are especially convenient because they make it possible for
change of objective, focusing, and movement of the mechanical stage to occur auto-
matically. Moreover, with the appropriate software all the important data such as ob-
jective, illumination, magnication, coordinates of the object, and the digital photo-
graphing of the image canbe savedandlater retrieved.
In a metallographic/materialographic laboratory, reected-light microscopes of
either the upright or inverted type are used. If other materials are also examined, for
example, ceramic, stone, glass, or synthetics, a microscope with reected-light as well
as transmitted-light beamprojectionis necessary.
15.6 The Reected-Light Microscope
In metallography/materialography, ground and polished surfaces of materials are the
mainobjects that are examinedwithreectedincident light.
The essential parts of a reected-light microscope are: light source, condenser,
aperture- and radiant-eld diaphragm, lter holder, reector, rotating nosepiece with
reected-light objective, stage, intermediate optic, body tube, andeyepiece.
15.6.1 Upright Type of Reected-Light Microscope
With the reected-light microscope of the upright type that is customarily used in ma-
terials research, the top surface of the specimen is illuminated fromabove through the
objective. Here the light rays are reected or scattered. These rays are collected by the
objective. The tube lens projects an enlarged intermediate image that is caught by the
eyepiece andfurther magnied.
Figure 15.7 shows a modern upright type, reected-light microscope, for routine
purposes.
The specimen lies on a movable stage. Direct observation of the fully lit position is
possible.
For the area being examined to be positioned absolutely perpendicular to the opti-
cal axis, the specimen must be correspondingly orientated with a leveling device. The
thickness of the specimen is limited by the working distance between objective and
stage.
15.6.2 Inverted Type of Reected-Light Microscope
In the eld of metallography/materialography, reected light microscopes of the in-
verted type are also used often. Following the suggestion of Le Chatellier, the specimen
is placed on a movable specimen stage with a hole above the microscope column and
the objective.
Figure 15.8shows a modernresearchmicroscope, invertedtype, reected-light.
The inverted type has the following advantages: 1 The specimen is simply placed
with the prepared surface facing down on the stage and over the hole; 2 There is no
need for cumbersome manipulation of a leveling device in order to get the prepared
surface of the specimen perpendicular to the light path; 3 Larger, irregularly shaped
specimens can be easily examined microscopically as well, inasmuch as the working
distance object-objective is not affected by the size of the specimen. One disadvantage
is that the prepared surface can become scratched when it is placed on the stage. Fur-
thermore, one may not be able tosee the illuminatedarea very clearly.
The objective of a reected-light microscope differs from that of a transmitted-
light microscope. Optical calculations must take into account the fact that surfaces like
polished specimens are examined without a cover glass. In addition, reected-light ob-
jectives are especially well dereected so that no disruptive false ashes are superim-
posedonthe image of the specimen.
With both systems, all the necessary construction elements are integrated in the
microscope. With a rotating nosepiece, different objectives can be inserted into the
beampathand the magnicationthereby changed. Exchangeable slide-incomponents
permit quickandsimple change toother types of illuminationor lters.
Fig. 15.7Upright type reected-light microscope.
2
A camera connection makes documentation of the magnied image of the object
possible.
15.7 Optical Examination Methods
The prepared specimen normally has a plane surface. The ground and polished metal-
lic surface reects light very well, therefore, usually shine brightly. The surface is either
silver or slightly colored, depending on the composition of the material. However, we
can differentiate individual portions of structural constituents only when they show
different contrast. If the reection difference between two structural constituents is
greater than 10 %, they can be distinguished from each other. If that difference is less
than10%, contrast must be heightenedusing methods suitedtothat purpose.
Before contrasting, either by chemical or physical means, can be undertaken on a
ground and polished specimen, the specimen should rst be observed in a polished
condition. To this end it is advisable to begin with the lowest degree of magnication
and then proceed to greater magnication. This enables one to check the quality of the
specimenpreparation. Moreover, ssures, shrinkage and pores, inclusions, impurities,
corrodedareas, thinoxide lms, peripheral layers, andtheir adhesionto the base mate-
rial can already be detected. If the contrast between individual structural constituents
is sufciently high, they canbe distinguishedas well.
With most metallographically/materialographically prepared specimens, how-
ever, the reectiondifferences betweenthe individual structural constituents or phases
are sosmall that the contrast must be heightenedby using carefully selectedmethods.
One process used to effect a change in the specimen surface, and which is con-
nected with contrast-heightening, is the electrochemical etching method. This process
includes the classical chemical as well as electrolytic etching.
In addition, physical contrasting methods, including thermal etching, ionic etch-
ing, and the application of interference coating are used to bring about a change in the
Fig. 15.8Inverted type reected-light microscope for research.
3
surface of the specimen see Figs. 9.1 and 9.2. These methods are described in more
detail inChapter 9.
Our task here is to consider in greater detail various optical methods of producing
contrast that donot cause any change inthe specimensurface.
The four mainoptical contrast methods used for the purpose of examining the tex-
tures and structures of metallographically/materialographically prepared specimens
with a microscope are the following: bright-eld illumination, dark-eld illumination,
polarizationcontrast, anddifferential interference contrast.
15.7.1 Bright-Field BF Illumination
Reected light bright-eld illumination is the most important method used in
reected-light microscopy. In this process, the light that is reected into the light path
of the microscope passes throughthe objective directly onto the specimensurface. Fig-
ure 15.6 shows the light path when bright-eld illumination is used. An integrated ver-
tical illuminator 1 emits a light that travels through the reected-light aperture dia-
phragm and the radiant-eld diaphragm. The light beam is then reected by a color
neutral beamsplitter 2, which is set at 45 to the optic axis, and through the objective
3 the beam strikes the surface of the specimen 4. There, the reected or scattered
beams again pass through the objective 3 and traverse the beamsplitter 2. The tube
lens 5 then projects the intermediate image. The image is further enlarged by the eye-
piece. Half-translucent mirrors may be usedas beamsplitters, but a higher light yieldis
obtainedby using prismilluminators.
Figure 15.6 also shows the location of all possible contrasting components ar-
rangedina small area above the objective with
A: Contrasting element of the illuminationside,
B: Contrasting element of the observationside, and
C: Space for components for bothlight paths.
The reecting capacity of the individual structural constituents depends on their
refraction number n. More important, however, is the varying absorption power of in-
dividual phases and diffuse reections. Differences in absorption of individual phases
and the presence of diffuse reections create contrasts. If this contrast is sufcient, the
differences canbe visible tothe eye.
Accordingly, the polished specimen of a single-phase gold alloy, as well as those of
many multiphase metal alloys, showhardly any contrasts. If the material has constitu-
ent parts of widely varying reection power, e.g., cast iron with laminated graphite,
steel with slag inclusion or suldes, those individual constituent parts are already mi-
croscopically detectable immediately after the material has beenpolished.
Diffuse reection occurs when there are rough surfaces, grain boundaries, and
scratches. But the presence of these things may also give some indication, inindividual
cases, of the materials structure.
For microstructures inbright eldBF, see Figs. 7.15and15.10a.
In other methods of achieving optical contrast, the light rays emanating from the
light source are diverted or else altered. Various reectors that are built into the reec-
tor slide of the microscope are usedfor this purpose. To gaina particular kindof micro-
scopic illumination or to observe the specimen in a particular way, one simply inserts
the reector inthe corresponding position.
15.7.2 Dark-Field DF Illumination
In the case of reected-light dark-eld illumination Fig. 15.9, the light that is emitted
by the reected-light illuminator 1 does not fall directly on the specimen surface. By
means of a reector staircase 2 and 3, the light is conducted around the actual ob-
jective and into a second housing case 4 where it strikes a ring-shaped concave reec-
tor. This device reects the rays at a very at angle of illumination onto the specimen
surface 5. Only scattered light returns for observation in the microscopic beampath.
For this reason, the at surface of a well-polishedspecimenappears dark.
Reected-light dark-eld illumination is well suited to show the quality of a pol-
ished surface inasmuch as the oblique light rays allow lapping tracks, scratches, and
ne cracks to show up bright. Unevenness and rough surfaces are easily detected as
well. Hard phases that stand out, deeper-lying soft phases, as well as contraction cavi-
ties and pores display bright edge seams relief. Half-opaque phases may show their
inherent color.
Figure 15.10 shows a carbon steel in bright eld a and dark-eld b. The struc-
ture and texture as well as surface details can be clearly seen with dark-eld
illumination.
15.7.3 Polarization Contrasting POL
When contrast is achieved using polarization, a polarizer P is inserted into the illumi-
nation beam pathway and an analyzer A into the observation beam pathway Fig.
Fig. 15.9Dark eld DF illumination in reected light, with light source 1, mirror step
assembly 2, mirror with an oval hole 3, light, directed in a second housing case towards the
objective 4, sample surface 5.
1
15.11. The direction of transmission of the analyzer 6, A is at a right angle to the po-
larizer 2, P. Only the depolarized portions of the rays can reach the tube lens 7. In
this polarizedlight a lambda plate 6a, changes the gray contrast intocolor contrast.
Interference reection can be prevented by using a rotating / 4-plate antiex-
plate betweenthe object andthe objective.
In the case of substances that are optically isotropic, e.g., cubic or amorphous, the
specimen always appears dark because reection fromthese materials does not lead to
a change in the state of polarization. The polarized light is, consequently, not let
throughby the analyzer.
Structural constituents that are optically anisotropic, as for example zinc, tita-
nium, spheroidal graphite, some nonmetallic inclusions or minerals onthe other hand,
do change the polarization state of a ray of light when reected. Then the depolarized
portions of the light canpenetrate the analyzer.
Fig. 15.10Microstructure of carbon steel in bright eld a and dark eld b.
Observationof a metallographic/materialographic polishedspecimeninpolarized
light is therefore useful for differentiating between isotropic cubic and anisotropic
noncubic phases. Ferromagnetic phases can be identied as well inasmuch as the
plane of polarization, affected by the magnetization, is turned. For this reason, the do-
mainboundaries of the magnetic zones appear invarying degrees of brightness.
The gray contrasts that occur in anisotropic phases can be transformed into color
contrasts through the use of a lambda plate 6a in the observation beampathway. Iso-
tropic phases can likewise be contrasted in polarized light by applying an optically an-
isotropic layer. For example, an oxide layer applied by anodization to aluminum pro-
duces color contrasts. With slag, minerals, ceramic, and glass that show half-opaque
behavior, the use of polarized light results in less scattered light. This makes a better
contrast possible and the structural constituents can be delineated better one froman-
other.
The microstructure in Fig. 15.12 shows titanium with deformed areas made vis-
ible withpolarizationcontrast POL.
15.7.4 Differential Interference Contrasting DIC
When Nomarskis differential interference contrast method is used, the polarized ray
of light is split into two beams of different oscillationdirections Fig. 15.13 by a doubly
Fig. 15.11Polarization contrast POL in reected light, with polarizer 2 P, analyzer 6 A,
lambda plate 6a .
1
refracting prism 4. These two rays are out of phase with each other when they strike
the specimen 6. If the specimen surface is not completely at, path differences are the
result. Ina reverse direction, the reectedor scatteredbeams, or both, nowtraverse the
DIC-prism 4 and the analyzer 7, thereby acquiring the same oscillation direction
and nowcapable of interfering with the intermediate image. The path differences that
are caused by the specimen surface are converted to gray values. Unevenness becomes
visible as relief. Witha lambda plate, color contrasts canbe obtained.
Figure 15.14 shows a microstructure of a soldering in bright eld BF a and in
differential interference contrast DIC b. In BF the solder can only be seen as a gray
phase in the lighter matrix, but in DICthe solder can be clearly discriminated fromthe
matrix.
15.7.5 Fluorescence in Reected Light
Specic areas of a microstructure can be marked with a uorescence dye see Section
3.10.1. These areas will absorb light of a specic wavelength in a short period of time,
and then emit the light. The wavelength of the emitted light is always around
2050 nmlonger than the incoming light. If blue light is absorbed, green light is emit-
ted, fromUV-light visible light is emitted.
Especially at the examination of medical and biological samples, uorescence is
often used, as specic dyes are suited for specic phases in the sample. In this way an
exact microscopic examinationcanbe performed.
In metallography/materialography the use of a dye can give important informa-
tion on size and distribution of pores, cracks, gaps between basic material and surface
layers, etc. see Section3.10.1.
At the reected uorescence microscopy Fig. 15.15 a short pass lter A is placed
in the light path, only allowing light of a narrowwavelength to pass to the specimen. In
between is placed a beamsplitter B, which reects the short waved reected light and
only let throughthe long wavedemittedlight. The reectedlight that is not absorbedby
the specimen surface is stopped by a long pass lter C; this lter only lets the long
waveduorescence light pass.
Lamps with a high degree of red or infrared light are less suited for uorescence
Fig. 15.12Microstructure of titanium in polarized light. Cold work is visible.
microscopy; mercury vapor lamps witha line type spectrumare tobe preferred.
For a microstructure impregnated with a dye and examined with uorescence see
Fig. 3.14.
15.8 Practical Use of the Microscope
15.8.1 Setting up the Microscope
If possible, the microscope should be set up in a roomof its own on a stable worktable.
There should be sufcient space to the right and to the left of the apparatus for the
depositing of specimens and supplemental equipment. If no separate roomis available
for microscopic or measurement work, the instrument should be located in a place re-
moved from all sectioning, grinding, and polishing equipment to avoid any transfer-
ence of vibrations or abrasion particles. Moisture, especially alkaline and acid vapors
from electrolytic polishing or chemical etching, can also damage important parts of
the microscope after just a short time. Such chemical procedures should be performed
under a fume hoodina separate room.
Fig. 15.13Differential interference contrast DIC in reected light, with doubly refracting
prism 4, objective 5, specimen 6 and analyzer 7.
1
15.8.2 Working with the Microscope
Inthis sectionandthe following twosections, a number of points are statedthat should
be followedwhenworking withthe microscope.
Adjust the height of your chair in such a way that you are sitting erect but comfort-
ably as you look into the eyepiece and can reach all the operating parts of the in-
strument effortlessly.
Turnonthe source of light.
Place a specimenonthe microscope stage focus plane.
Look into the distance, then, without changing the focus of your eyes, look into the
eyepiece.
Adjust the distance between the eyepieces according to the distance between your
eyes.
If you do not wear glasses, put rubber eyecups on the eyepieces to get the right eye
distance tothe eyepiece.
Fig. 15.14Microstructure of a soldering in bright eld BF a and differential interference
contrast DIC b.
If you do wear glasses, check to see whether the eyepieces are designed accord-
ingly. If you have done everything right you will have a clear view of everything in the
whole eldof vision.
15.8.3 Correct Adjustment of the Microscope
Begin by using an objective of a lowscale number and bring the specimen into fo-
cus.
Open the eld diaphragmand center this and the condenser in such a way that the
viewing eldis illuminatedevenly.
Close the elddiaphragmand, throughcentering, bring the little fuzzy eck of light
that is still present intothe middle of the viewing eld.
This eck of light can be brought into sharp focus by vertically adjusting the con-
denser.
Open the centered eld diaphragmin such a way that the diaphragmleaves extend
out over the eldof vision.
Open the aperture diaphragm and close it again carefully until the image has be-
come darkenoughtoshowsufcient contrast.
With transmitted-light microscopes, a change of objective requires each time a re-
adjustment to accommodate the settings of the eld and aperture diaphragms. Such
readjustments are not necessary with reected-light microscopes. With the latter it is
sufcient toadjust the aperture diaphragmtothe object andthe objective.
15.8.4 Focusing and Practical Use
The task of getting a sharpfocus onshiny polishedspecimens of metal canbe facili-
tated by partially closing the radiant-eld diaphragm. After that, focus sharply on
the image of the radiant-eld diaphragm. Because this diaphragmis imaged in the
Fig. 15.15Fluorescence: Short pass lter A, beamsplitter B and long pass lter C.
1
object plane, it is easy tondthe image of the specimensurface.
As an alternative move the eld of viewto the edge of the sample. The contrast be-
tweenthe sample andthe mounting material or air allows for a simple focus.
Infocusing the microscope, use at rst anobjective of weak magnicationandlook
for the area of interest. Then change to objectives with a higher magnication, as
necessary.
With unfamiliar specimens it is advisable to experiment with all the different illu-
mination possibilities optical contrasting methods. Often structural details can be
identiedbetter inthis way anddistinguishedfromone another.
If anoil immersionobjective is used onanupright type microscope, the area of the
object that is of interest is rst of all locatedwithanobjective of a lowmagnication10
. Thenone focuses withthe oil immersionobjective e.g., 100. After that, using the
objective revolver, this objective is turned to the side and the one with the lower magni-
cation is again swung into position. Now one applies a drop of immersion oil to the
illuminated area on the object, trains the objective with the higher magnication on
the specimen, and refocuses with ne focusing. Proceeding in this way can avoid
dampening other objectives with oil. In case of an inverted microscope, rst focus with
the oil immersion objective without oil. The specimen is removed then fromthe micro-
scope, and a very small drop of immersion oil is placed on the center of the objective.
Nowthe specimenis replacedanda ne focusing is done.
After work with the microscope is nished, the oil on the objective and on the
specimen is removed immediately and carefully with ne tissue paper and then
cleanedwithethanol.
15.8.5 Measurements of Length
The microscopic image can be measured with eyepiece crosses on which there are
scales, squared grids, or reference samples. This canbe inthe formof a reticle, whichis
a systemof lines, circles, dots, cross hairs, or wires, or some other pattern, placedinthe
eyepiece or at an intermediate plane on the optic axis which is used as a measuring
reference, focusing target, or todene a camera eldof view. Alsoa graticule, whichis a
scale onglass or other transparent material placedinthe eyepiece or at anintermediate
plane on the optic axis can be used. The scale of the reticle or the graticule serves as a
reference gage. The distance betweengradationmarks onthis scale is very precise, e.g.,
0.1 mm.
Let us suppose that we want to measure the length of an integral part of a micro-
structure that we are examining with an objective with a scale number of 100. If its
apparent length amounts to 1.2 mmin the intermediate image of the eyepiece, its true
length can be determined by dividing by the scale number on the objective. The length
is 1.2 mmdividedby 100, i.e., 12 m. It is not necessary totake the magnicationof the
eyepiece intoconsideration.
A calculated magnication, using the manufacturers supplied ratings, as men-
tionedearlier, is only anapproximationof the true magnication, since individual opti-
cal components may vary from their marked magnication. For a precise determina-
tion of the magnication calibration observed through an eyepiece, a stage micro-
metre is used. This is a graduated scale, placed like a specimen on the stage of a micro-
scope andusedfor calibration.
It is very important that the measuring devices used are precise, and it is recom-
mended that these should be traceable to the National Institute of Standards and Tech-
nology NIST or a similar organization.
Measurements should be performed according to ASTMStandard Guide for Cali-
brating Reticles and Light Microscope Magnications E 1951. This guide covers
methods for calculating and calibrating microscope magnications, photographic
magnications, video monitor magnications, grain size comparison reticles, and
other measuring reticles.
15.8.6 Measurements of Height Differences
Occasionally it is of interest to measure height differences of layers of differing hard-
ness or the depth of scratches. To do this, an objective of a high numerical aperture is
used because its depth of focus is very slight. One narrows the eld diaphragm to a
small circle and focuses on the highest plane. On the ne-focusing knob scale a value
can be read. Then one focuses on the deepest place and again reads off the appropriate
value. If one knows the level difference obtained from the instruction manual that
corresponds to the distance between two scale-marks on the ne focus mechanism,
one can easily calculate the measurement. Use of a dial gage that is connected to the
microscope stage or of anelectric positionencoder is more convenient.
15.8.7 Maintenance of the Microscope
Microscopes are precisioninstruments that should serve their purpose for many years.
For this reasonthey shouldbe handledwithcare.
Dust particles or smoke are especially a problem. Always cover your microscope
with a protective dust cover after you have nished working and turned it off. The front
lenses of the objective are especially sensitive. Avoid letting the objective come into
contact with the specimen or the stage when you are focusing. The most minute
scratches that can occur when these touch one another can cause blurred areas in the
image.
Etched specimens should be thoroughly cleaned and dried before they are used in
the microscope. Acids and residual moisture can not only leave ecks on the specimen
but also have an adverse effect chemically on the front lenses of the objective, as for
example canhappenwithhydrouoric acid.
If youmust remove dust fromthe objective, eyepiece, or lter, blowthemoff witha
rubber dust blower. Fingerprints, traces of grease, andresidues of immersionoil canbe
removedwitha cottonball dippedingrease-free benzene if necessary.
It is a good idea to have the service department of the manufacturer check the de-
vice at least once a year and make any adjustments or calibrations that may be neces-
sary. Leave repair worktothe service department of the manufacturer also.
15.9 Documentation
The documentation of microscopic images can be done in different ways. In the early
days of microscopy, the viewer sketchedthe image details that interestedhim.
Today either reex cameras for photos in various formats or video or digital cam-
eras, or both, are used.
Modern microscopes are equipped accordingly. They have their own photograph/
television connection. One can change over to this connection from the ordinary bin-
ocular tube via a beamsplitter.
Figure 15.16 shows the light path. Through a photo-ocular 3, the intermediate
image 2, coming from the tube lens 1, is magnied and projected to innity. The
photo-objective produces from this an intermediate image on the lm plane in the
camera 6 if the central shutter 4 is openedfor exposure. The size of this intermediate
image must be adjusted to the format of the lm. With microphotography lm, for ex-
ample, a magnication with the factor 2.5 must be effected when the original inter-
mediate image has a diameter of 20 mm. This means that the entire image cannot be
capturedonlmof microphotography format.
The housing of a reex camera can be joined to the photo/TVconnection by means
of an adapter with a built-in objective. The reex camera should be equipped with an
electric motor for lmtransport and a remote control switch. One disadvantage is that
the ipping upof the mirror at the moment of exposure may cause boththe microscope
andthe camera tovibrate, resulting inblurredimages.
For professional documentation, microscope cameras are to be preferred. All the
important camera settings can be regulated electronically from a control desk. The
camera itself works witha vibration-free shutter. Depending onthe model, the lmcas-
sette may be exchangeable.
For several years now, video cameras and digital cameras have been increasingly
used for image documentation. Because semiconductor sensors can be used with the
modern CCD-cameras that have very small active surface areas, the enlarged interme-
diate image in the microscope must be reduced again. For this purpose, TV-adapters
with special optics and a xed reduction factor are necessary. With a TV-zoom-adapter,
the reduction factor and consequently the area of image detail can be changed. In this
way, the size of the image can be made to t the format of the camera or video printer.
Fig. 15.16Optical path for photomicrography, with tube lens 1, intermediate image 2,
photo eyepiece 3, central shutter 4, camera lens 5 and image in the lm plane 6.
1
This can be of advantage in connection with the required standard magnications.
Such linear standard magnications are 25, 50, 75, 100, 200, 250, 400, 500, 750, 800,
and1000.
The picture taken by the camera can be shown on a monitor, printed out by a video
printer, or processedandstoredindigitalizedformona PC.
In this process, the overall magnication, M
total
, can be calculated fromthe optical
magnication, M
optical
, andthe electronic magnicationM
electronic
.
M
optical
= M
objective
M
adapter
5
where M
objective
is the magnification of the objective, and M
adapter
is the magnification of
the adapter.
M
electronic
= D
monitor
/D
sensor
6
where D
monitor
is the diagonal length of the image of the monitor and D
sensor
is the diago-
nal of the active surface of the picture sensor.
Sothe overall magnicationis
M
total
= M
optical
M
electronic
7
In addition to the conventional CCD-cameras that shoot from 2530 images per
minute, Slow-Scan CCD-cameras are also being used inevengreater numbers. These
cameras take fewer images per secondbut withhigher resolutionandwithless noise.
In combination with a PC, digitalized images can be processed and archived.
Thanks to the many highly efcient software programs, they can also be qualitatively
improved, marked, and labeled. Program modules that analyze structure make pos-
sible the quantitative measurement of the structural parameters and a description of
the measurement results in the appropriate form, the numerical values in the form of
tables or clarifying diagrams see Part IVof this book.
15.10 The Confocal Laser Scan Microscope
Depth of focal eld is a fundamental problem in light microscopy. It is also the reason
why we produce surfaces that are as plane possible when preparing metallographic/
materialographic specimens and why we arrange them perpendicularly to the micro-
scopes light ray. This is the only way toachieve a sharpimage over a larger area.
The greater a microscopes magnication, the smaller the eld of view, and the
shallower the depthof focal eld.
This system-determined limitation on the light microscope can be circumvented,
and the possibilities for its use signicantly broadened with the help of modern laser
and computer technologies. The specimen surface can be scanned in a line-by-line
manner with a focused laser ray. Confocal reproduction conditions, the recording,
storage, and processing of the signals in a PC, make a three-dimensional representa-
tion of the specimen surface possible. The laser scan microscope LSM thus combines
the advantages of the light microscope with those of the scanning microscope and the
prolometer.
15.10.1 Function of Confocal Laser Scan Microscope
Figure 15.17 shows the path of light rays and the operational mechanism for the de-
vice. The laser ray is focused onto the specimen through the objective lens. Light that is
reected there is focused onto a variable pinhole aperture by an additional lens. Only
light coming from the objectives focal plane can reach the detector unimpeded. Light
coming from other optical planes is suppressed by the confocal spatial lter that con-
sists of lens andaperture. The specimensurface, withthe light ray falling ontoit, canbe
scanned point-by-point, line by line, by means of the dichroic mirror. The light signals
receivedby the detector are convertedintoelectronic impulses anddigitally processed.
We, therefore, obtain a reproduction of the level specimen surface on a monitor.
Because of the lowdepthof focal eld, we obtainanoptical section inx, y coordinates
whenthe surface is irregular.
By successively changing the arrangement of the object along a series of dened
steps in direction z, we can record several sections and compile these images into a
three-dimensional stacked image, process them digitally and draw qualitative as well
as quantitative conclusions about the topography of the specimensurface.
Lasers with varying excitation wavelengths in the ultraviolet through infrared
spectral range are used. As lasers of wavelengths 488 and 514 nm 25 mW and HeNe
lasers of wavelengths 543 nm 1 mW and 633 nm 5 mW are usually used in
metallography/materialography.
At 0.2, the laser scan microscopes lateral resolution capability is somewhat better
thanthat of the conventional light microscope.
Depth resolution depends on the wavelength of the laser light, the numerical aper-
ture NA of the objective and the diameter of the aperture, which is a determining fac-
tor for the quality of the confocal spatial lter.
Assuming that the apertures diameter infront of the detector approaches zero, the
following holds true for reective surfaces:
Fig. 15.17Path of light rays and the operational mechanism for a confocal laser scan
microscope.
1
d
z
= n 0.89 /NA
2
8
where d
z
is the axial half-width of an intensity curve of light reflected by the object, deter-
mined by the height of the object stage; is the laser's wavelength and n is the refraction
index.
In practice, values between 20 and 50 nmturn out to correlate with a useful depth
of focal eld, depending onobjective type andthe mediumthat is betweenthe objective
andthe object.
15.10.2 Applications of Confocal Laser Scan Microscope
Possible types of lighting for LSM are bright-eld, differential interference contrast,
and uorescence. If lasers that emit polarized light are used, polarization microscopy
can also be used. Figure 15.18 shows a confocal laser scan research microscope set up
witha motorizedne focusing stage andmonitor.
In the area of material research and testing, confocal light microscopy is suitable
for the investigation of the surfaces of metallic materials, ceramics, plastics, and repli-
cas as well as of semitransparent and transparent layers such as glass, polymer foils,
coatings, or varnishes.
In addition to the representation of compounds, surface proles can be recorded
and the microroughness of very small areas suchas tears, pores, and hollowspaces can
Fig. 15.18Confocal laser scan microscope.
1
be three-dimensionally ascertained. The arrangement and thickness of single and mul-
tiple layers canalsobe representedandquantitatively analyzed.
Figure 15.19 shows a fractured steel plate, the single grains can be seen three-
dimensionally.
15.11 Stereo Microscopy
For the purpose of a three-dimensional evaluation of fractured surfaces, the size and
shape of those fractures, as well as the three-dimensional shape and conguration of
constituent elements, it is advantageous to use a stereomicroscope. With a stereomi-
croscope the same spot on a specimen can be viewed from two places at a short dis-
tance fromone another, similar tothe distance betweenthe twoeyes of a humanbeing.
Modern stereomicroscopes may use two different principles for the light ray
paths.
Following the Greenough principle, two light ray systems are directed onto the
specimen through two identical objectives that are tilted toward one another at the ste-
reo angle. This yields two images that produce a single three-dimensional image when
observedthroughthe twoeyepieces.
Following the telescope principle, two parallel but not axially aligned light beams
are directed through an objective. The beams are deected by the objective and strike
the specimen at the stereo angle. With this method of operation, an expansion of the
operational possibilities becomes relatively easy because supplementary optical mod-
ules canbe installedeither above or belowthe body of the microscope.
For stereomicroscopes, a number of exchangeable objectives are obtained with
the magnications from5to100andeyepieces from5to20.
Fig. 15.19Confocal image of a fractured steel plate.
4
Apochromatic objectives are well suited for three-dimensional observations. For
at objects like prepared specimens, wafers and foils, planachromats are better suited.
For the nest structures with very lowcontrast, the apochromats can be used with ad-
vantage.
The magnication can be changed by zoom when a special system of lenses is
used. According to design and manufacturer the variation in magnication may be be-
tween3:1or 12:1.
The observation of details depends to a high degree on the illumination that shall
be adapted to the object and the purpose of examination. Therefore, different illumina-
tion systems can be obtained like halogen-incandescent lamp for incident light or co-
axial illumination, optical ber for vertical illumination, and other light sources
for highest light intensity and for homogeneous illumination. Metallographic/
materialographic specimens or other at, strongly reecting objects like LCDs, wafers,
and integrated circuits may be examined most effectively with coaxial illumination.
Three-dimensional objects may be illuminated from two sides or with ring-
illumination. Using illumination under an angle will give an improved observation of
Fig. 15.20Stereo microscope with digital camera.
3
high differences in the surface. Vertical illumination is best suited for exposing of cavi-
tations and open pores. Fluorescence modules make examination of uorescence sub-
stances possible.
The advantages of stereomicroscope systems are: Ample working distances, large
object elds, andthe three-dimensional viewing of nonreversal images.
Stereomicroscopes can produce meaningful overall magnications of up to about
250times the original.
Figure 15.20shows a modernstereomicroscope.
16
Electron MicroscopyScanning
Probe Microscopy
AN IN-DEPTH DESCRIPTION OF ELECTRON MICROSCOPY AND SCANNING
probe microscopy falls outside the scope of this book, but in this chapter a short intro-
duction is given to the transmission electron microscope TEM, the scanning electron
microscope SEM, the focused ion beamtechniques FIB, and a number of scanning
probe microscopes SPM.
16.1 The Transmission Electron Microscope TEM
Electron beams penetrate thin layers and, in doing so, are diffracted at the crystal lat-
tice and interferences arise. One can make these visible, after amplication with elec-
tromagnetic lenses and electronic processing, as bright-dark effects. With an accelera-
tion voltage of up to 1 million volts, magnications of up to 10
6
with a resolution below
1 nm can be attained. Disruptions in the crystal lattice, such as dislocations, elimina-
tions, grain boundaries, and other lattice defects, are detectable; they appear mostly
dark.
Specimens for the TEM examinations must be thin enough for the electrons to
pass through and thick enough for their structural features to remain veriable. Vari-
ous methods canbe usedfor the preparation.
With metallic materials and ceramic basic materials, thinning procedures are pre-
ferred. Using this method, the specimen diameter 3 mm is made sufciently thin,
through either ion bombardment see Section 16.3 or electrolytically, that a hole is
produced in the middle. Areas next to the hole are sufciently thin to be suitable for
TEMexaminationsee Section8.5.
For purposes of imaging the surfaces, carbon or lacquer is used to take a replica of
the specimen. The peeled-off layer of lacquer is then vapor-coated in a vacuum cham-
ber withcarbonor metal Au, Pt to bring out the contrast. After the layer of lacquer has
beenremoved, the metal foil or carbonfoil canbe transluminated.
Fine powder, dust, or smoke particles are applied directly to a backing lm car-
bon, lacquer. With extraction replicas, individual particles of a specimen, their size,
anddistributioncanbe identied.
With the use of ultramicrotomes one can produce thin sections from embedded
powders or synthetics. Synthetic materials that tendto smudge must be workedwithat
lowtemperatures cryomicrotomy.
16.1.1 The Scanning Transmission Electron Microscope STEM
This microscope is a combinationof a TEManda SEMsee below andgives the advan-
tages of both microscope types. A STEM is a very high cost investment and primarily
usedfor research.
16.2 The Scanning Electron Microscope SEM
In the scanning electron microscope, the surface of the specimen is linearly scanned
withthe electronbeamca. 0.01 m. Secondary electrons are emittedandcapturedby
558
an electron detector. The spatial distribution of these secondary electrons can be made
visible, after electronic amplication, on a monitor. Depending on the acceleration
voltage of the primary electrons, magnications of up to 200 000 are possible. With
magnication of 1000 the depth of eld is about 35 m; the resolution power
amounts up to 0.01 m. Differences in levels on the surface of the specimen result in
differences in contrast. Moreover, shadow formations can arise as a result of the slant
with which the electron beams fall on the specimen. As a result, an image of high reso-
lutionandgreat depthof eldis obtained.
The SEM is used preferably for the examination of rough surfaces and investiga-
tions of damage or loss, e.g., fracturedsurfaces.
Preparation of the specimen for SEM examinations is simple: the specimen must
be free of volatile elements like water, oil, or grease. Loose particles must also be re-
moved. If the specimen does not consist of electricity-conducting material, the surface
must be coated with a layer of electro-conductive material C, Pt, Au to prevent charg-
ing.
In case of mounting, care should be taken that metal powder, like copper, con-
tainedinthe mounting material, is not contaminating the specimen.
16.2.1 Energy Dispersive Spectroscopy EDS
AnSEMcanbe equippedwithadditional equipment like EDSandEBSDsee below.
Besides the electrons emitted fromthe specimenmentioned above, also X-rays are
emitted. As high-energy electrons produced with an SEM interact with the atoms
within the top few micrometres of a specimen surface, X-rays are generated with an
energy characteristic of the atom that produced them. The intensity of these X-rays is
proportional to the mass fraction of that element in the specimen. In EDS, X-rays from
the specimenare detected by a solid-state spectrometer that converts themto electrical
pulses proportional to the characteristic X-ray-energies. If the X-ray intensity of each
element is compared to that of a standard of known composition and suitably cor-
rected for the effects of other elements present, then the mass fraction of each element
canbe calculated.
16.2.2 Electron Backscatter Diffraction EBSD
Electron Backscatter Diffraction EBSD has become popular among materials scien-
tists since the rst commercial automatic systems were available in 1994. The main
advantage of this method is the possibility to link morphology grain size and shape
with crystallographic features phase, orientation, disorientation on the microscopic
scale, but still ina representative specimenarea. During the examination, anelectronic
backscatter pattern EBSP is produced, an image consisting of relatively intense
bands Kikuchi bands intersecting one another and overlying the normal distribution
of backscattered electrons, as a result of Bragg diffraction of electrons by atomic
planes in the crystal lattice. The results can be compared to TEM, but the specimen
preparation is much simpler than the preparation of thin foils. The specimens, how-
ever, are considerably more difcult to prepare than for normal imaging in SEM, be-
cause of the very low information depth of the EBSD signal based on channeling ef-
fects. This means that the very thin deformed layer, often left on the specimen after
mechanical preparation, cannot be tolerated to obtain a good pattern quality, and
therefore the specimenpreparationshall be improved. Ingeneral, classic etching is not
needed for EBSD because the contrast is dened through the orientation differences.
Etching shouldevenbe avoided, as the inducedsurface roughening is disturbing due to
Chapter 16 Electron Microscopy 559
the highspecimentilt 70 during the examinationprocess. The specimenpreparation
for EBSDis discussedinSection7.10.4.
16.2.3 The Electron Probe Microanalyzer EPMA
This instrument, also called the microprobe is closely related to the SEM, only the
X-ray detectors are not analyzing only the energy as in EDS mentioned above, but the
wavelength of the X-rays generated from the interaction of the primary and backscat-
tered electrons and the specimen. This is called wavelength dispersive spectroscopy
WDS andcomparedto EDS, WDSgives muchmore accurate quantitative data for the
single components inthe specimensurface.
16.3 Focused Ion Beam FIB
A focused ion beamsystemFIB is in principle built like an SEM. In the SEMan elec-
tron beam is used for scanning, but in the FIB a beam from a liquid metal ion source
mostly gallium, Ga+ is used. This beam is focused so that it can be scanned like an
electron beam. This allows for sputtering material from the sample or for depositing
material on the sample if gases are used see Section 9.6.5. Also, imaging is possible by
ion-induced secondary electrons, as it is known fromthe SEM. As the FIB can remove
material with a very high precision, it is used for preparation of samples for TEM. This
covers bothsamples of electronic devices andsamples for material research.
The TEMsamples can be made either by using a pre-prepared sample in the form
of a thin strip of material, which then is further thinned by the FIB, or by the newer
lift-out technique. With this technique no mechanical preparation is needed, the ion
beamcuts into the base material and the sample is lifted out using a special manipula-
tor.
The great advantage of using FIBfor preparationof samples for TEMis the shorter
times compared to conventional methods see Section 8.6, and the very high rate of
success.
16.4 Scanning Probe Microscopes SPM
In addition to the methods of optical metallography/materialography already men-
tioned LM, TEM, SEM, we will briey discuss scanning probe microscopy. Inthe past
few years it has gained increasingly greater signicance in the area of metallography/
materialography.
All scanning probe microscopes work according to the following principle: the sur-
face of the specimen is scanned with the sharp tip of a needle that is mounted on a
exible cantilever. The interactive force that is present between the tip and the surface
serves as a measurement signal and can be evaluated. Through the use of piezoelectri-
cal actuators, movements of the measuring tip in the magnitude of atomic diameters
can be initiated, with a resolution of less than 1 nm. Scanning probe microscopes are
usedinbiology, physics, andmaterials science tocharacterize surfaces.
The rst device of this kind, the Scanning Tunneling Microscope STM, was devel-
oped by Binnig and Rohrer and used for the rst time in 1981. It makes use of the
quantum-mechanical tunneling effect for measurement of distance. For this purpose,
voltage is applied between the tip and the specimen. If one brings the tip closer to the
surface without actually touching it noncontact mode, a current begins to ow. Inas-
much as the amplitude of this current depends exponentially on the distance it can be
used to regulate the distance. With STM the surface topographies of conductive
samples andimages inthe atomic range canbe shown.
With the Atomic Force Microscope AFM, the tip is positioned at the free end of a
cantilever. The interaction between tip and surface, e.g., a repulsive force, is registered
throughthe vibrationof the cantilever. Its detectionoccurs inaccordance withthe light
conducting principle: a laser beamfocused on the backside of the exible cantilever is
reected and registered by a photo diode. The measured values in the nanometre range
can be used to guide piezoelectric actuators in the x-, y-, z-direction of the tip. In this
manner one canobtaina three-dimensional image of the surface onthe computer.
AFMis suited for electrical-conductive and nonconductive materials such as met-
als, ceramics, glasses, and synthetics. Samples, either unprocessed or processed, can
be examinedinair, ina gaseous environment, or inliquids.
The eld to which ATMis applied is constantly growing and nowthis technique is
also used for measuring of nano hardness and elastic modulus Youngs modulus see
Section21.6.1.
If the specimen is to be prepared metallographically/materialographically, one
must take care that it has been polished with as little resulting deformation as possible
electrolytic polishing may be an advantage, and that through chemical etching only a
minimal level contrast in the nanometre range arises between the individual phases.
Very small structural elements, e.g., the very nest precipitates, can then be identied
that can no longer be seen with a light microscope because of its limited resolution
power. Nevertheless, other local interactive forces canbe detected withthe AFMproce-
dure.
With magnetic force microscopy MFM, the surface of the sample is scanned with
a nickel or iron tip in noncontact mode. One obtains an image of the local magnetic
characteristics witha resolutioninthe nanometre range.
Adhesionforce microscopy conveys perceptions withregard to the local structure-
specic adhesive force betweenmeasuring tipandspecimensurface.
With friction force microscopy, the local frictional forces can be measured and im-
aged. This is performed in contact mode by letting the tip move across the surface of
the specimen and measuring the deection of the cantilever. Good contrasts can be ob-
tainedespecially withsynthetics.
References Part III
1 Courtesy of Carl Zeiss, Germany.
2 Courtesy of Olympus, Germany.
3 Courtesy of Leica Microsystems, Germany.
4 Courtesy of E. Bischoff, Max-Planck-Institut fr Metallforschung, Stuttgart, Germany.
Chapter 16 Electron Microscopy 561
Part IV: Quantitative
Metallography/Materialography
Automatic Image Analysis
17
Quantitative Metallography/
MaterialographyAn Introduction
WHEN MAKING A QUALITATIVE EXAMINATION OF A MICROSTRUCTURE,
the interpretation of the structure is to a high degree based on the knowledge and expe-
rience of the observer. Inquantitative metallography/materialography the constituents
in the microstructure are measured to provide more reliable data for materials engi-
neering and quality control purposes. Typical microstructural measurements include
the length, width, and area of features or the relative amount of a structure or phase.
The application of stereological principles enables two-dimensional measurement
data extracted from metallographic/materialographic specimens to provide accurate
information about three-dimensional structures increasing the usefulness and impor-
tance of quantitative microstructural analysis. It can be tedious to implement quanti-
tative methods. Digital image analysis equipment and software have beendeveloped as
tools toautomate the collectionandreporting of quantitative data.
In this chapter, the most important uses of quantitative metallography/material-
ography and corresponding ASTM standards are discussed briey. Automatic image
analysis is described in Chapter 18. Both chapters should be considered as introduc-
tions to quantitative metallography/materialography and image analysis see the Ref-
erences andLiterature List for further study of these subjects.
17.1 Quantitative Metallography/Materialography
In short, quantitative metallography/materialography can be dened as the measure-
ment of microstructural parameters. This may be linear measurements when examin-
ing layer thickness, case depth, etc., or measurements of area, when analysis of volume
fractionor grainsize is required.
Both manual quantitative methods, including measurements using point count-
ing screens or templates, and automatic image analysis are dened in a number of
standards.
17.1.1 StereologyTable 17.1
Stereological methods are procedures used to characterize three-dimensional micro-
structural features based on measurements made on two-dimensional sectioning
planes.
1
For the stereological calculations, the International Society for Stereology recom-
mends a number of symbols and notations. The most important are stated in Table
17.1.
1,2
Basic Measurements
Anumber of the above-mentioned parameters are simple counting measurements that
are relatively easy tomeasure andare usedina number of equations see below.
565
P
P
is the ratio P
/ P
T
, where P
is the number of points that fall in the -phase and

P
T
is the total number of test points see alsobelow.
P
L
is the number of points of intersections generated per unit lengthof test line. An
intersection count is the number of boundaries between the matrix phase and the
phase or constituent of interest that are crossed by the lines of a test grid. For isolated
particles in a matrix, the number of feature intersections will equal twice the number
of feature interceptions. The total length of the test line is determined in advance to
facilitate calculations.
N
L
is the number of interceptions of features divided by total test line length. The
part of the test line superimposed on the feature constitutes the intercept. The number
of interceptions equals the number of particles or clusters of particles of a phase or
TABLE 17.1Principal Symbol and Combined Notations for Quantitative Metallography/Materialography.
Symbol Units Description Common Name
P Number of point elements or test points
P
P
Point fraction (number of point elements per total number
of test points).
Point Count
L mm Length of linear elements or test line length
P
L
mm
1
Number of point intersections per unit length of test line
L
L
mm/mm Sum of linear intercept lengths divided by total test line
length
Lineal fraction
A mm
2
Planar area of intercepted features or test area
S mm
2
Surface area or interface area, generally reserved for
curved surfaces
V mm
3
Volume of three-dimensional structure elements or test
volume
A
A
mm
2
/
mm
2
Sum of areas of intercepted features divided by total test
area
Area fraction
S
V
mm
2
/
mm
3
Surface or interface area divided by total test volume
(surface-to-volume ratio)
V
V
mm
3
/
mm
3
Sum of volumes of structural features divided by total test
volume
Volume fraction
N Number of features
N
L
mm
1
Number of interceptions of features divided by total test
line length
Lineal density
P
A
mm
2
Number of point features divided by total test area
L
A
mm/
mm
2
Sum of lengths of linear features divided by total test area Perimeter (total)
N
A
mm
2
Number of interceptions of features divided by total test
area
Area density
P
V
mm
3
Number of points per test volume
L
V
mm/
mm
3
Length of feature per test volume
N
V
mm
3
Number of features per test volume Volumetric
density
L mm Mean linear interception distance, LL/NL
A mm
2
Mean area intercept, AA/NA
S mm
2
Mean particle surface area, SV/NV
V mm
3
Mean particle volume, VV/NV
constituent of interest that are crossedby the lines of a test grid. For all microstructures
withmore thana single phase, P
L
=2 N
L
andfor a single phase, P
L
=N
L
.
P
A
is the number of point features, suchas grainboundary junctions, inside a given
area, dividedby this area.
N
A
is the number of interceptions of features, such as grains or graphite nodules,
inside a givenarea, dividedby this area.
See also ASTM Standard Terminology Relating to Metallography E 7 for stan-
dardstereological terminology denitions.
To obtain a true measurement, the instrument used must be calibrated see Sec-
tion17.1.3.
Basic Equations
Based on the measurements mentioned above, a number of equations are developed
for covering the calculation of points, lines, areas, and volumes used for metall-
ographic/materialographic analysis. The most important measurements such as vol-
ume fraction, inclusionrating, etc., withthe covering ASTMstandards are describedin
short below, andthe relevant equations will be statedthere.
Use of Comparison Charts and Grids
Comparison charts were developed for the evaluation of a given microstructure. An
example is the so-called JKcharts developed by the Swedish Jernkontoret depicting a
series of typical inclusion congurations size, type, and number to be used for direct
comparison with the microscopical eld in view. Comparison charts can be used also
for determination of volume fraction and grain sizes, but a grid is used normally see
the relevant standards below.
17.1.2 Specimen Preparation
Selection of Specimens
The selection of specimens, sampling, for quantitative analysis is very important be-
cause if the measured results are to be of value, the specimens must be representative
of the material that is being analyzed.
The number of specimens and the selection depends on the type of examination to
be performed. As described in ASTMStandard Practice for Calculating Sample Size to
Estimate, with a Specied Tolerable Error, the Average for Characteristic of a Lot or
Process E122 see Section12.4, randomsampling shouldbe performed.
As an example, the sampling procedure for the ASTM Test Method for Determin-
ing the Inclusion Content of Steel E45, should be described in short: To obtain a rea-
sonable estimate of inclusion variations within a lot, at least six locations, chosen to be
as representative of the lot as possible, should be examined. For cases in which a de-
nite location within a heat, ingot, or other unit lot is unknown, statistical randomsam-
pling witha greater number of specimens shouldbe employed. Very oftenthe geometry
of the work piece plays a role; in examination of inclusions, the polished surface must
be parallel to the longitudinal axis of the product. In case of rolled or other hot worked
material, the microstructure to be measured will vary strongly according to the plane
of the preparedsurface see alsoSection2.1.
Chapter 17 Quantitative 567
Reproducibility
It is very important that the specimen surfaces examined in quantitative metallo-
graphy/materialography are prepared with the highest degree of reproducibility; only
then can the measured results be compared. In case of manual image analysis, the op-
erator might be able to compensate for minor artifacts in the prepared microstructure,
but when using digital imaging equipment to delineate structures with image segmen-
tation, artifacts may be included in the measurements producing inaccurate results
see below.
Preparation of the Specimen Surface
As a general rule the goal of specimen preparation is to consistently show the True
Structure, free of all artifacts. Aspecimenfor automatic image analysis should also be
plane, without relief and edge rounding. All phases should be visible without smearing
or other artifacts; in inclusion rating even small scratches can disturb the measuring
see Section13.6.
Preparation of specimens suitable for quantitative analysis is described in Section
13.2.3 and in every quantitative standard under the jurisdiction of the ASTMCommit-
tee E-4 see Section12.4.
Etching
For a number of quantitative examinations, such as inclusion rating, etching should
not be used; the contrast developedobscures the features tobe measured.
In other cases, etching has to be performed to obtain the contrast necessary to
showthe structures of interest suchas insteel grainsize andbanding measurements.
Reproducibility of the etching is very important in automatic image analysis so
that a uniform contrast can be developed. Variable and inconsistent etching will pro-
duce contrast irregularities whichinuence the measurements.
17.1.3 Calibration
Before making any measurement, it is essential to create calibrations for each instru-
ment microscope, video system, etc. used to deliver an image. Calibration is the pro-
cess of establishing the graphical or mathematical relationship relating the desired
property expressed in a standard unit of measure such as m to the instrument out-
put instrument units suchas lar divisions or pixels.
Although the operational requirements for equipment calibration differ widely,
the ASTM Standard Guide for Calibrating Reticles and Light Microscope Magnica-
tions E1951 provides anoverviewof calibrationconcepts andgeneralizedcalibration
procedures.
17.1.4 Field SelectionBias
Quantitative measurement of a specimen surface will take place in microscopic elds
only representing a small part of the surface. To obtain a specic measurement accu-
racy, a number of elds must be examined. This number depends on the homogeneity
of the microstructure and the magnication. The higher the magnication observed
and the lower the homogeneity of the specimen, the higher the number of elds that
will be needed to accurately evaluate the microstructure, because at higher magnica-
tion the area covered by the eld is smaller and with a heterogeneous microstructure
the variations of the surface are higher. The number of elds is stated very often in the
specic standards. If not, the number should be calculated to obtain a reasonable rela-
tive accuracy.
As a rule, the elds should be placed randomly on the specimen surface. This can
be performed easily on an upright microscope, the specimen surface being visible see
Section 15.6. It is important that the operator does not look at the image when the
placement of the elds is decidedon. This is the only way bias canbe avoided.
17.2 Volume FractionPoint Count
The volume fractionof a givenphase or constituent inanalloy is one of the most impor-
tant and most common measurements in quantitative metallography/materialo-
graphy. This is because the amount of a second phase can have a strong inuence on
the properties of the material.
The amount of a specic constituent second phase is quantied by the volume
fraction. The volume fraction of a component is designated by V
V
, and is the ratio of
the volume of this component V
referred to the test volume V

T
total volume of the
specimen. This canbe expressed:
V
V
= V
/V
T
1
V
V
corresponds to the area fraction of the structural component that is visible
in the polished specimen surface and can be determined by planimetry. Because of
the valid relationship in the range of statistical scatter, A
A
area fraction =L
L
lineal fraction =P
P
point count, the volume fractioncanalsobe determinedfromL
L
.
This is done by measurement of the fraction L
of a straight line L
T
that falls within the
component, or fromthe point fraction P
P
by counting the points P
of a point grid with

the point count P
T
that fall onthe component. This canbe expressed:
V
V
= V
/V
T
= A
/A
T
= L
/L
T
= P
/P
T
2
In ASTM Test Method for Determining Volume Fraction by Systematic Manual
Point Count E562 see below, an efcient way for statistically estimating the volume
fraction of an identiable constituent or phase from sections through the microstruc-
ture by means of a point grid, is described.
17.2.1 ASTM Test Method for Determining Volume Fraction by Systematic
Manual Point Count E 562
The test method may be used for all opaque materials see Section 12.4.3. The test
method is based on the stereological principle that a clear plastic test grid with a num-
ber of regularly arrayed points, when systematically placed over an image of a two-
dimensional section through the microstructure, can provide, after a representative
number of placements on different elds, an unbiased statistical estimation of the vol-
ume fraction of an identiable component or phase. A grid of lines or curves is super-
imposed on a magnied image of a metallographic/materialographic specimen, and
the number of points falling within the microstructural component of interest is
counted and averaged for a selected number of elds. These points divided by the total
points in the grid is the point fraction P
P
see above. Based on P
P
the volume fraction
V
V
canbe calculated.
17.3 Inclusion Rating
Inclusions can signicantly inuence the properties of a material. For this reason in-
clusionrating, especially of steel, is a very important quantitative method.
Inclusions can be exogenous like slag particles or indigenous, oxides, suldes, sili-
cates, etc., developed in the material during the manufacturing process. Normally only
the indigenous inclusions, suldes and oxides, are measured, quantifying the amount,
size, shape, and distribution. In a number of standards, ASTM E 45 see below, SAE
J422a, and the German standard SEP1570 DIN50602, the inclusions are determined
by using manual comparison chart methods based on volume fraction and point
counting. Since this involves a vast amount of counting time, image analyzers are often
usedfor inclusionrating see below.
17.3.1 ASTM Standard Test Method For Determining the Inclusion Content
of Steel E 45
ASTM E 45 covers a number of recognized methods for determining the nonmetallic
inclusioncontent of wrought steel.
The methods are both macroscopical and microscopical; only the latter shall be
shortly describedhere.
Comparison charts, mostly based on JKcharts, as described above in this chapter,
are used. The inclusions are separated into four categories, A, B, C, and D and are
graded by calculating a severity level based on width and length for Dtypes the count
of inclusions in 0.50 mm
2
elds within a 160 mm
2
specimen surface area. In Method A
Worst Field the inclusions are assessed qualitatively, seeking out and reporting only
the eld withthe highest severity rating. InMethod Dthe lengthor count and the width
of inclusions are examined and the severity level of each inclusion type for each eld of
viewis determined and reported for a 160 mm
2
specimen surface area. The Methods B
and C require that a specimen area be surveyed and inclusions greater than a certain
lengthandthose of the maximumlengthbe reported.
Manual performance of E 45 especially Method D involves much work to obtain
an acceptable measurement accuracy; therefore, the use of digital image analysis
equipment has become more commonsee Section18.5.2.
17.3.2 ASTM Practice for Obtaining JK Inclusion Ratings Using Automatic
Image Analysis E 1122 withdrawn 2006, replaced by E 45
This practice covers procedures to performJK-type inclusion ratings using automatic
image analysis inaccordance withmicroscopical methods AandDof E45.
E1122is further describedinSection18.5.2.
17.3.3 ASTM Practice for Determining the Inclusion or Second-Phase
Constituent Content of Metals by Automatic Image Analysis E 1245
The practice describes a procedure for obtaining stereological measurements that
quantify basic characteristics of the morphology of indigenous inclusions in steels and
other metals using image analysis. The practice can be applied to provide such data for
any discrete second-phase constituent inany material.
ASTME1245is further describedinSection18.5.2.
17.4 Grain Size
A very high number of metallographic/materialographic examinations are performed
to determine the grain size of the material; this parameter to a high degree inuences
the material properties.
Three procedures for determining grain size are described in ASTME112 see be-
low, the comparison procedure does not require counting of either grains, intercepts,
or intersections but only involves comparison of the grain structure to a series of
graded images. The planimetric procedure involves an actual point count of the num-
ber of grains within a known area, N
A
. N
A
is used to determine the ASTM grain size
number, Gsee below. The intercept procedure involves anactual count of the number
of grains interceptedby a test line or the number of grainboundary intersections witha
test line, per unit length of line, used to calculate the mean lineal intercept length, l. l is
usedtodetermine the ASTMgrainsize number, Gsee below.
17.4.1 ASTM Test Methods for Determining Average Grain Size E 112
ASTM E 112 includes the comparison procedure, the planimetric procedure, and the
intercept procedures. The methods apply chiey to single-phase grain structures in
metallic materials, but they can be applied to determine the average grain, crystal, or
cell size innonmetallic materials like ceramics.
ASTME112 is a very comprehensive standard covering the earlier mentioned pro-
cedures, a description of the ASTM Grain Size Number, and a number of annexes de-
scribing howtoestablishthe grainsize for a number of materials.
ASTM Grain Size Number
This number, the Gnumber, is denedas:
N
AE
= 2
G1
3
where N
AE
is the number of grains per square inch at 100magnification. To obtain the
number per square mmat 1, N
A
, N
AE
is multiplied by 15.50. The International Standard
Organization (ISO) and in several national standards, the metric grain size number, G
M
, is
basedonthe number of grains per mm
2
, at 1, andthis gives the equation:
N
A
= 82
G
M
4
The metric grain size number, G
M
, is a little lower than the ASTMgrain size num-
ber, G, for the same microstructure:
G= G
M
+ 0.046 5
Comparison Procedure
The comparison procedure, as mentioned above, does not require counting of grains,
intercepts, or intersections, but involves comparisonof the grainstructure toa series of
graded images, either in the form of a wall chart, clear plastic overlays, or an eyepiece
reticle. Experience has shown that unless the standard image reasonably well ap-
proaches that of the specimen, errors may occur. To minimize such errors, the com-
parison charts are presented in four categories: Plate IUntwinned grains at etch
includes grain size numbers 00, 0,
1
2
, 1, 1
1
2
, 2, 2
1
2
, 3, 3
1
2
, 4, 4
1
2
, 5, 5
1
2
, 6, 6
1
2
, 7, 7
1
2
, 8, 8
1
2
, 9,
9
1
2
, 10, at 100. Plate IITwinned grains at etch includes grain size numbers 1, 2, 3,
4, 5, 6, 7, 8, at 100. Plate IIITwinned grains contrast etch includes nominal grain
diameters of 0.200, 0.150, 0.120, 0.090, 0.070, 0.060, 0.050, 0.045, 0.035, 0.025, 0.020,
0.015, 0.010, 0.005 mm at 75. Plate IVAustenite grains in steel McQuaid-Ehn in-
cludes grains size numbers 1, 2, 3, 4, 5, 6, 7, 8, at 100. As an example, Plate III is used
for twinnedcopper andbrass witha contrast etch.
Repeatability and reproducibility of comparison chart ratings are generally 1
grainsize number.
Planimetric Procedure
As mentioned above, the planimetric procedure, also called Jeffries procedure, in-
volves an actual count of the number of grains within a known area circle or rect-
angle. The number of grains per unit area, N
A
, is used to determine the ASTM grain
size number, G. The precision of the method is a function of the number of grains
counted, and a magnication shall be selected which gives at least 50 grains in the eld
to be counteda minimumof three elds. Whenthe counting is done, the gure is mul-
tiplied by Jeffries multiplier, f, that is a factor relating to the magnication used, M.
The number of grains per square mmat 1, N
A
is calculatedfrom:
N
A
= fN
Inside
+ N
Intercepted
/2 6
where f is the Jeffries' multiplier taken froma table in the standard, N
Inside
is the number
of grains completely inside the test circle and N
Intercepted
is the number of grains that inter-
cept the test circle.
A precision of 0.25-grain size units can be attained with a reasonable amount of
effort. Results are free of bias and repeatability and reproducibility are less than
0.5-grain size units. An accurate count does require marking off the grains as they are
counted.
Intercept Procedure
The intercept procedure, also called Heyns procedure, is more convenient to use than
the planimetric procedure. Withthe intercept methodanaccurate estimate of the grain
size can be obtained in a fraction of the time used with the planimetric method. As
mentioned above, the intercept method involves an actual count at least 50 intercepts
of the number of grains intercepted by a test line or the number of grain boundary in-
tersections with a test line, per unit length of test line, used to calculate the mean lineal
intercept length, l
. l
is usedtodetermine the ASTMgrainsize number, G.

The precision of the method is a function of the number of intercepts and intersec-
tions counted. An intercept is a segment of test line overlaying one grain. An intersec-
tionis a point where a test line is cut by a grainboundary. Experiments have shownthat
a test pattern consisting of three concentric and equally spaced circles having a total
circumference of 500 mm gives satisfactory results. Based on the calculation of the
number of intercepts, N
L
andthe number of intersections, P
L
, the meanlineal intercept
value for eacheld, l canbe calculated:
l = l/N
L
= 1/P
L
7
A precision of better than 0.25-grain size units can be attained with a reasonable
amount of effort. Results are free of bias; repeatability andreproducibility are less than
0.5-grain size units. Because an accurate count can be made without the need of
marking off intercepts and intersections, the intercept method is, as mentioned, faster
thanthe planimetric methodfor the same level of precision.
ASTM E 1382 describes determining average grain size using semiautomatic and
automatic image analysis see below.
17.4.2 ASTM Test Methods for Estimating the Largest Grain Observed in a
Metallographic Section ALA Grain Size E 930
Commercial material specications sometimes include, in size limits for grain struc-
tures, the need for identication of the largest grain observed in a sample, often ex-
pressed in ALA as large as grain size. ASTM E 930 is used when the number of large
grains is toofewfor measurement withASTME112.
The test methods are simple manual procedures, using comparison and measur-
ing. The measuring procedure is recommendedfor greater accuracy.
17.4.3 ASTM Test Methods for Characterizing Duplex Grain Sizes E 1181
The above-mentioned test methods for determination of average grain size covers ma-
terials assumedtocontaina single log-normal distributionof grainsizes. ASTME1181
is set forth to characterize grain size in products with any other distributions of grain
size. The termduplex grain size is chosen to describe any of these other distributions
of grain size, because of its common usage and familiarity. However, the use of that
termdoes not imply that only two-grainsize distributions exist.
Duplex grain size may occur in some metals and alloys as a result of their thermo-
mechanical processing history, and these methods are made for these materials, but
they can also be used for other materials with a similar microstructure. Duplex grain
structures for example, multiphase alloys are not necessarily duplex ingrainsize, and
as suchnot coveredby these methods.
The test methods use a comparison procedure, a point count procedure based on
ASTM E 562 see above, a planimetric procedure, and a direct measurement pro-
cedure.
17.4.4 ASTM Test Methods for Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis E 1382
These test methods may be usedtodetermine the meangrainsize, or the distributionof
grain intercept lengths, or areas in metallic and nonmetallic polycrystalline materials.
The methods may be applied to specimens with equiaxed or elongated grain structures
with either uniform or duplex grain distribution. Either semiautomatic or automatic
image analysis devices may be utilizedtoperformthe measurements.
The semiautomatic procedure is based on a digitizing tablet with a measurement
resolution of at least 0.1 mm. Avariety of approaches can be employed: The simplest is
to x a photograph to the tablet surface and place a suitable grid over the photograph,
tape down the corners of the grid, and use the cursor, tted, with ne cross hairs, to
measure the appropriate features. Alternatively, the grid can be placed on an eyepiece
reticle. The cursor is moved over the table surface and the microscopist can see the
illuminated cross hairs in the cursor through the eyepieces over the eld of view and
grid pattern. A third approach is to transfer the microstructural image, the test grid
image, and cursor image to a television monitor. The microscopist moves the cursor
across the tablet surface while watching the monitor to make the appropriate measure-
ments.
The automatic procedure is describedinSection18.5.3.
17.5 Banding
A banded microstructure is caused by segregation that occurs during the dendritic so-
lidication of metals and alloys and is aligned by subsequent deformation. Solid-state
transformations may be inuenced by the resulting microsegregation pattern leading
to development of a layered or banded microstructure. The most common example of
banding is the layeredferrite-pearlite structure of wrought low-carbonandlow-carbon
alloy steels. Other examples of banding include carbide banding in hypereutectoid tool
steels andmartensite banding inheat-treatedalloy steels.
Microstructural banding inuences the uniformity of mechanical properties of
the material, andASTME1268 describes a number of procedures for testing of banded
microstructures.
17.5.1 ASTM Practice for Assessing the Degree of Banding or Orientation
of Microstructures E 1268
This practice describes a procedure to qualitatively describe the nature of banded mi-
crostructures andstereological procedures for quantitative measurement of the degree
of microstructural banding or orientation. The practice also includes a procedure us-
ing microindentation hardness testing. Only the stereological procedure will be dis-
cussedhere.
The stereological measurements are made on an etched specimen by superimpos-
ing a test grid consisting of closely spaced parallel lines of known length on the pro-
jected image of the microstructure or on a photomicrograph. Measurements are made
withthe test lines parallel andperpendicular tothe deformationdirection.
The stereological measurements may be made using a semiautomatic tracing type
image analyzer. The test grid is placed over the image projected onto the digitizing tab-
let and a cursor is used for counting. For certain microstructures where the contrast
betweenthe banded or oriented constituents is adequate, anautomatic image analyzer
may be usedfor counting see Section18.5.4.
17.6 Porosity in Thermal Spray Coatings
Thermal spray coatings are susceptible to the formation of porosity due to a lack of
fusion between sprayed particles or the expansion of gases generated during the spray
process. The determination of area percent porosity is important to monitor the effect
of variable spray parameters and the suitability of a coating for its intended purpose.
Depending on application, some or none of this porosity may be tolerable. In Test
Methods for Determining Area Percentage Porosity in Thermal Sprayed Coatings E
2109, twomethods are indicatedfor the determinationof the porosity see below.
17.6.1 ASTM Test Methods for Determining Area Percentage Porosity in
Thermal Sprayed Coatings E 2109
These test methods cover the determination of the area percentage porosity of thermal
sprayed coatings. Method A is a manual, direct comparison method using seven stan-
dard images shown on gures in the standard. These gures depict typical distribu-
tions of porosity in thermal spray coatings. Method B is an automated technique re-
quiring the use of a computerized image analyzer see Section 18.5.1. The methods
quantify area percentage porosity only on the basis of light reectivity froma metallo-
graphically polished cross section. In ASTMGuide E1920 see Section 12.4.3, a num-
ber of preparation procedures are recommended see also Material/Preparation Tables
1215.
17.7 DecarburizationCase DepthCoatings
The measurement of thickness depth of surface phenomena like decarburization,
carburizing, nitriding, and coatings surface layers is a common metallographic/
materialographic procedure. Normally a specimen is prepared and examined in an op-
tical microscope using an ocular micrometre reticle or other measuring instrument
see below. The automatic image systems are also able to measure these surface phe-
nomena see Section18.5.5.
For all measurements on layers, etc., mentioned above, the quality of the prepared
specimen is of utmost importance. The plane of the cross section must be perpendicu-
lar to the plane of the surface phenomenon to secure measurement of the true thick-
ness. The preparation must be performed so that the specimen surface is at without
edge rounding and the surface shall be without artifacts such as smearing of a softer
coating. For correct preparationsee Table 11.1andSection13.5/6.
17.7.2 ASTM Test Methods for Estimating the Depth of Decarburization of
Steel Specimens E 1077
These test methods cover procedures for estimating the depth of decarburization of
steels irrespective of the composition, matrix microstructure, or sectionshape. The fol-
lowing basic procedures may be used: Screening methods, microscopical methods, mi-
croindentation hardness methods, and chemical analysis methods. Only the micro-
scopical methods will be discussedhere.
Microscopical methods are most suitable for measuring the depth of decarburiza-
tion of as-hot rolled, as-forged, annealed, or normalized specimens. These methods
can also be applied to heat-treated specimens, although with less certainty in deter-
mining the maximum affected depth. Spheroidized-annealed or cold-worked speci-
mens can also be evaluated, but detection of structural variations due to decarburiza-
tion is more difcult than with hot-worked or fully annealed structures. Measurement
is done on an etched specimen and based on evaluation of the variation in the micro-
structure at the surface due tochange incarboncontent.
Measurements are made on a microscope using an ocular reticle, a screw Filar
micrometre ocular, or witha scale placedagainst a groundglass projectionscreen.
For use of automatic image analysis see Section18.5.5.
17.7.3 Case Depth
The measurement of the often very thin zone developed by carburizing, nitriding, etc.,
is done in much the same way as decarburization and coatings see below. The speci-
men preparation can be difcult because the often very hard zone will create problems
with the planeness of the specimen see above. For very low depths, taper sectioning
may be usedsee Section3.11.1.
For the use of automatic image analysis see Section18.5.5.
17.7.4 ASTM Test Method for Measurement of Metal and Oxide Coating
Thickness by Microscopical Examination of a Cross Section B 487
This test method covers measurement of the local thickness of metal and oxide coat-
ings by the microscopical examination of cross sections using an optical microscope.
Under good conditions, when using an optical microscope, the method is capable of
giving anabsolute measuring accuracy of 0.8 m.
A carefully prepared specimen cross section is used see above. A special prob-
lem when preparing specimens with soft coatings is embedded abrasives see Section
13.5/6.
The measuring device may be a screw Filar micrometre ocular or a micrometre
eyepiece. An image splitting eyepiece is advantageous for thin coatings on rough sub-
strate layers. The measuring device shall be calibrated at least once before and once
after the measurement using a stage micrometre. The magnication should be chosen
sothat the eldof viewis between1.5and3the coating thickness.
17.7.5 ASTM Test Methods for Thickness of Diffusion Coating C 664
These test methods cover two procedures for measuring the thickness of diffusion
coatings.
Method A is the determination of the difference in the thickness of the part before
andafter coating.
Method B is the determination of total coating thickness, dened as the distance
between the observably unaffected substrate and the exterior surface of the coating.
The total coating thickness is determined by cross-sectioning the coating, preparing a
metallographic/materialographic specimen, and microscopically measuring the coat-
ing thickness.
17.8 Other ASTM Standards for Quantitative Materialography
Belowfollows the designations of a number of ASTMstandards relating toquantitative
metallography/materialography. For further information see the Document Summa-
ries inSection12.4 the CD-ROMincludedwiththis manual.
For other standards ISO, DIN, BSI, etc. see Appendix I.
ASTMPractice for Petrographic Examinationof HardenedConcrete C856
ASTMTest Methodfor Quantitative Analysis of Textiles D629
ASTMTest Methodfor Fiber Analysis of Paper andPaperboardD1030
ASTM Test Method for Microscopical Determination of the Reectance of Vitrin-
ite ina PolishedSpecimenof Coal D2798
ASTMPractice for Calculating Sample Size to Estimate, witha SpeciedTolerable
Error, the Average for Characteristic of a Lot or Process E122
18
Automatic Image Analysis
18.1 Introduction
THE NEED TO CONSIDER DIGITAL IMAGING SYSTEMS IS PREDICATED ON
recognition of stereological principles and quantitative metallography/materialo-
graphy as essential concepts in materials science. The application of quantitative
metallography/materialography in materials science requires the measurement of mi-
crostructures. It may be argued that the study of materials cannot be termed a sci-
ence if it does not use quantitative methods.
Equipment using digital imaging technology is not essential to the implementa-
tion of quantitative metallographic/materialographic methods. Quantitative metallo-
graphy/materialography canbe practicedusing nondigital methods see Chapter 17.
Digital imaging technology is applied to materials science to expeditiously pro-
duce the structural measurements required by quantitative metallographic/materialo-
graphic standards. Performing image analysis is not a goal; rather it is a means of
achieving a goal. To hear a laboratory technician or manager discuss the need to do
image analysis is disturbing. What actually needs to be performed in a materials sci-
ence laboratory is the measurement of microstructures, i.e., quantitative metallo-
graphy/materialography. The required products of quantitative metallography/
materialography are the measured dimensions of microstructural features, numerical
values that describe the physical extent of the structures. The goals of quantitative
metallography/materialography can be more easily achieved through the use of digital
image measurement technologies to simplify and maximize control of the measure-
ment process. In the most basic sense an image analysis systemis nothing more than a
gage; principally no different than a micrometre, scale, or other device used to extract
physical dimensions fromany object. An image analysis systemis nothing more than a
tool designed to deliver digital images, extract the structural measurement data re-
quired by quantitative metallography/materialography and, as a bonus, process and
manage the data. Primarily, sucha systemoffers the possibility of making accurate and
reproducible measurements of microstructural features. The availability of relatively
inexpensive digital imaging equipment greatly facilitates the extraction of data from
microstructural images as well as producing data that are immediately ready to be
storedandanalyzedusing a wide variety of commoninformationmanagement tools.
18.2 Qualitative and Quantitative Metallography/
Materialography
18.2.1 The Transition to Quantitative Standards
The barriers to implementing quantitative methods are primarily the continued exis-
tence of qualitative standards; lack of cost effective and efcient instrumentation; and
perhaps most signicantly, the existence of procedural obstacles. Bringing rigorous
quantitative methods to metallography/materialography necessitates the existence of
specications and standards requiring these methods, the equipment and operational
577
procedures to produce the results specied in the standards, and, nally, the organiza-
tional desire toinstitute these methods.
Nearly all of the more recent standard test methods produced by ASTM Interna-
tional, as well as other standards organizations andprivate industry, are quantitative in
nature and require the actual measurement of structural features rather thanthe tradi-
tional chart comparison or other subjective methods. Newstandards generally tend to
eliminate the use of chart comparison and rating or indexing schemes. Instead they
report the actual measured values for length, width, area, etc., as well as appropriate
statistical values. In many cases, the quantitative standard actually simplies the test
method.
The equipment necessary to perform the operations required by quantitative
methods is readily available. In addition to a microscope, the components needed to
assemble an image analysis systemgenerally include: computer with monitor, camera,
and printer. Early implementations of image analysis systems required specialized and
relatively expensive hardware components. Fortunately, the exponential rise in con-
sumer use of computers and digital cameras has beneted the use of image analysis in
materials science. Many of the technologies used in consumer imaging products are
directly transferable to microstructural image analysis systems. For example, the
availability of mass-produced personal computer components and image sensor chips
have resultedindramatically lower systemhardware costs.
Acertainsymbiosis exists betweenthe advancement of digital imaging component
technology and the propagation of quantitative standards. Technological develop-
ments and component cost reductions have facilitated the adoption of more quantita-
tive standards by virtue of easing the efforts and costs of implementing the standards.
Conversely, the increased number of quantitative standards has expanded industry de-
mandfor more efcient andcost-effective systems toperformthe measurements incor-
poratedinthese standards.
Perhaps the most signicant remaining barrier to the use of quantitative methods
is organizational procedural in nature. While the imprecision and the shortcomings
of nonquantitative methods are widely recognized, there remains in many metallo-
graphic/materialographic laboratories a strong inertia slowing the adoption of new
standards. The advancement of quantitative materials science oftensuffers froma bur-
densome process of newstandards approval. Inmany organizations the effort required
to secure organizational approval of newstandards is difcult, tedious, and presents a
formidable barrier to what is technically and logically obvious. None the less, quantita-
tive methods and standards are gradually replacing qualitative procedures, driven by
the issuance by industry leaders, bothpublic andprivate, of quantitative standards and
the constantly improving price/performance ratio of the equipment necessary to con-
veniently implement the standards.
18.2.2 Structure, Stereology, and Statistics
What structural parameters shouldbe quantied? Physical metallurgy andthe study of
microstructure property relationships provide the answers. Anobvious problemis that
the preparation of materials for microscopic observation and quantication yields a
planar, two-dimensional surface onwhichthree-dimensional phase and structural fea-
tures are displayed in some cross-sectional views. The solution lies in the body of ste-
reological principles that provide a scientic basis extrapolating planar measurement
data to yield valid volumetric material structure information.
1
The physical extent of
microstructures as shown by metallographic preparation including feature number,
length, width, and area, are the primary structural dimensions of importance. Nearly
all standards for the measurement of materials microstructures call for the determina-
tion of some or all of these parameters. Several other measurements are sometimes
required including perimeter as well as calculated data such as percent area, density,
distance froma surface, aspect ratio, andshape factor. For most quantitative standards
the data extraction requirements are very basic. Commonly, in the implementation of
quantitative standards using image analysis software, far more effort is required in the
processing of the measurement data to provide reporting in the format required by the
standard. This situationis particularly encounteredwhentranslating the older qualita-
tive standards for example, ASTM Standard Test Method for Determining the Inclu-
sion Content of Steel E 45 that rely on rating or other manipulations to produce re-
sults expressedas anindex or relative value rather thanas stereological data.
An extremely important aspect of quantitative standards is the role of statistical
concepts. Not only is the validity of stereological principles predicated on meeting cer-
tainstatistical conditions, but the results tobe calculatedalsoconsist almost entirely of
statistical parameters, such as mean standard deviation and condence interval. It is
vital that the laboratory personnel who are engaged in the performance and use of
quantitative methods have a basic understanding of statistical concepts in order to ob-
tainaccurate results.
This chapter will cover the basic elements of image analysis systems and their
practical application to several of the most common quantitative standards. The sec-
tions below present an overview of image analysis functions that are frequently found
to be useful in quantitative metallography/materialography. This overview is not de-
signedto be a detailedexaminationof the vast array of image processing functions. For
a thorough discussion of many of these processing functions see the work of John C.
Russ.
3
18.3 Principles of Digital Imaging
18.3.1 What is Digital Image Analysis?
Because the terminology used in describing digital imaging equipment and systems is
confusing, often ambiguous, and because of rapid changes in technology, prone to
short-term obsolescence the discussion that follows minimizes reference to specic
components.
Howis digital image analysis applied to materials science? Image analysis is a set
of software functions that can be used to extract quantitative data from microstruc-
tural images. Digital imaging technology integrated into a system is used as a tool to
provide the measurement of microstructures as required by quantitative methods.
Employing the power of digital imaging technology, the extraction of data is accom-
plishedina more timely andefcient manner.
18.3.2 Image Acquisition
Generally an image of materials microstructure consists of a rectangular or square
area showing physical structure voids or grainboundaries or material phases embed-
ded in a matrix. In most cases the objective of quantitative analysis is to measure the
physical extent of the structure or phase, most commonly length, width, or area. In
doing so it is necessary to remove the matrix portion of the image fromconsideration.
For this reasonall of image processing is essentially a data reductionproblem. Evenfor
Chapter 18 Automatic Image Analysis 579
a standard NTSC format camera the number of pixels in an image is 307 200. Every
step in the image acquisition and processing is performed with the objective of remov-
ing pixels representing matrix material information from consideration. Ironically
the large format digital cameras capable of delivering images having more than
1 000 000 pixels one mega pixel provide an even greater amount of data that must be
eliminated to produce the quantitative information required. The argument can be
made that more pixels are not always a benet in the extraction of measurements from
materials microstructure. Very little work has been done on identifying the level on
imaging digitization that is optimal for the data extraction job at hand. The assump-
tion that more pixels are better is not a universal truth, i.e., it should not be applied to
all analysis situations. Rather, the minimum number of pixels needed to quantify the
structure, based on the requirements of the standard should be taken into account
when selecting a camera. The more image data captured beyond that required to pro-
vide the measurement tolerances required by the standard, the more elaborate and,
therefore, more exposedtoerror the image processing data reduction will be.
18.3.3 Image DigitizationGray Scale
Digitization is the process of converting a continuous scene microscopic eld of view
into a block of numerical values a number of horizontal rows and a number of vertical
columns. Individual units in the rows and columns are picture elements pixels. Pix-
els are the basic unit of digital images. Pixels have a location within the image. Xis the
horizontal position and Yis the vertical position. Each pixel also has a brightness, illu-
mination intensity, or color value. These numerical values associated with each pixel
constitute a digital image. After a structural eld of view has been digitized, all image
processing and measurement is based on the quantitative values of each pixel. A dis-
cussion of the details of image digitization can easily ll a volume, but an in-depth
knowledge of the technology is not necessary. See the excellent work of Inoue and
Spring for a detaileddiscussionof image digitization.
4
The X, Y positional information associated with a pixel is straightforward. The
pixels into which the image is divided form an array or grid. The relative position of
each pixel within the overall grid image can be expressed as a coordinate location.
Once a calibration has been established the position of each pixel can be expressed as a
real distance from the coordinate system origin or from any other point pixel in the
array. The least common denominator for an image pixel array as produced from an
NTSCstandard video camera has dimensions of 640 pixels in each horizontal rowand
480 pixels in each vertical column. A so-called mega pixel image has upwards of 1000
horizontal by 1000vertical pixels.
The third value possessed by every pixel is a measure of its illumination level. This
value is a quantication of the relative amount of light found at that location of the
image. The range of values possibly varies and is dependent on technical specications
of the camera and digitizing components used to perform digitizing. In digitizing the
total range of illumination fromno light pure black to the maximumamount of light
pure white is divided into an equal number of levels. Commonly, an image from a
monochrome camera is digitized into 256 distinct levels, beginning with 0 for no light
uptoa maximumof 255 for the maximumamount of light. Inthis scheme every level of
illumination has a value from0255. This range of digital illumination values is called
the gray scale. A gray scale having a range of from 0255 is an 8-bit gray scale, since a
digital computer represents numbers as bits and to count to 255 requires 8 bits. Im-
age illumination may be digitized into ranges other than 0255. The wider the range of
digital illumination levels, the more bits are required to count them. The number of
bits used in digitizing illumination is called the bit depth. To digitize a true color image
requires at least 24 bits and produces a total of 16.7 million possible illumination or
color levels.
18.3.4 The Histogram
Digitization of the illumination levels within a microstructural eld of viewis in fact a
measurement of the illumination. Taken together, the pixel illumination measure-
ments show a pattern of variation representing the various phases and structures
withinthe image. By counting the number of pixels at eachilluminationvalue ina digi-
tized image, anilluminationfrequency distributioncanbe produced. The frequency or
quantitative distribution is a basic statistical method for summarizing data. Once a
microstructural eld of view has been digitized its distribution of illumination values
can be viewed graphically by constructing a histogram.
5
The typical image illumina-
tion histogramuses the gray scale range as the horizontal, Xaxis, and the count of pix-
els falling into each of the gray scale levels as the vertical, Y axis. In fact, the frequency
distributionof illuminationpresents the rawimage data uponwhichall image process-
ing is based and fromwhich all materials structure measurements are extracted. If the
structural features to be measured are not represented in the initial raw data of the
illumination quantitative distribution, then measurement of those features will not be
possible. The shape and position of the illumination histogramprovides important in-
formationabout the brightness, contrast, andmeasurability of the image.
18.3.5 The Effects of Brightness and Contrast on Illumination Distribution
The effects of different illuminationbrightness levels onquantitative distributioncan
be seen as measurability by considering the example of an image of a thermally
sprayed coating structure digitized to a depth of 8 bits, having a possible range of mea-
suredilluminationvalues of 0255 displayedinFig. 18.1a.
Ahistogramof the pixel brightness distribution of this eld of viewis shown at the
right in Fig. 18.1b. Digitized pixel brightness values are shown on the horizontal X
axis beginning with a value of 0 at the left end of the axis. The vertical Y axis shows the
number of pixels at each gray scale value. An inspection of the distribution reveals sev-
eral things. First, notice that this distributionis approximately normal; it has the shape
of the classic bell curve of a normal distribution. There is also a small but prominent
Fig. 18.1aBase line image.
spike or relatively high number of pixels at the 0 or black gray scale level. Addition-
ally, the majority of the brightness measurements are clustered somewhat to the right,
or bright endof the distribution, at aroundthe 180 level. Toshowthe effects of a change
in illumination levels on the resultant distribution, the brightness level was decreased
by 15 %for the same eld of view. The image and its associated histogramare shown in
Fig. 18.2.
Notice that the distribution is basically the same shape but it has shifted to the left
or darker endof the scale andthat the most frequent illuminationvalue is nowapproxi-
mately 140. Also, the number of pixels at the 0 illumination level has increased nearly
three times.
Next the image brightness level was increased by 15 %. The average brightness
level of the resultant image is approximately 213 and the brightest areas within the im-
age have been set to 255, the highest possible level saturation. Note in Fig. 18.3 that
the distribution is shifted so far to right end of scale that a portion of the distribution
has been clipped. This means that at the higher illumination levels some data repre-
senting the brightest structural features have been lost. In most cases the loss of raw
image illumination data due to excessive or insufcient image brightness should be
avoided.
Fig. 18.1bBase image illumination.
Fig. 18.2aBrightness decreased.
Now let us examine the effects on the image illumination distribution of changes
to the eld of view contrast. Contrast is a measure of the range of illumination values
Fig. 18.2bHistogram shifted left.
Fig. 18.3aBrightness increased.
Fig. 18.3bHistogram shifted right.
between the darkest and lightest areas within the eld of view. Again, referring to the
distribution shown in Fig. 18.1a, the range of brightness values extends across the
entire 0255 gray scale range. The result of decreasing the contrast by 10 %is displayed
inFig. 18.4a.
Notice in Fig. 18.4b that the range of illumination values has been reduced and
the distribution no longer lls the gray scale with the lowest value somewhat above 0
and the highest values somewhat below the 255 maximum. A decrease in contrast has
the effect of compressing the illuminationdistribution. Increasing the contrast by 10 %
produces the image anddistributiondisplayedinFig. 18.5.
In this case, the distribution range has been expanded or stretched. Note the gaps
in the bars plotted in Fig. 18.5a, indicating that after increasing contrast some illumi-
nation levels are not present in the image. See more on stretching in the Image Pro-
cessing sectionof this chapter. Based onthese examples, several generalizations canbe
made about the optimal illumination conditions for extracting measurement data
from digital images. First, the illumination brightness level selected for the image
should provide the broadest possible range of values in the distribution histogram
while avoiding clipping at either end of the gray scale. Also the contrast level should be
selectedtomaximize the range of illuminationvalues present inthe gray scale distribu-
Fig. 18.4aContrast decreased.
Fig. 18.4bDistribution decreased.
tion. The reason for seeking these conditions is simply to create an image that provides
the maximumamount of rawdata tobe usedtodene andmeasure the material micro-
structure.
Controlling illumination is essential. And while image processing software in-
cludes many powerful methods for altering digital image brightness and contrast,
these mathematical techniques must be considered as secondary tools. The primary
and most powerful control for controlling microstructure illumination is the micro-
scope or metallograph used to obtain the images. No software alteration of image illu-
mination characteristics should be undertaken prior to a thoughtful use of microscope
illumination controls including illumination level, aperture, ltering, etc., to produce
an image possessing the illumination conditions optimal for the intended use of the
image. During the process of setting illumination conditions with the microscope the
operator may quickly digitize candidate images and use the imaging software to dis-
play a distribution histogram. A series of microscope illumination adjustments should
be made and checked by viewing the histogram until the illumination distribution is
optimized. Only after such a process should additional software illumination adjust-
ment be undertakenif necessary.
The state of the image illumination distribution along with the intended uses of
Fig. 18.5aContrast increased.
Fig. 18.5bDistribution stretched.
the digitized image determines what, if any, image processing can or should be
performed.
18.3.6 Image Processing and True Microstructure
The phrase image processing describes a wide range of operations, implemented by
software programs and designed to transform a digital image into another image by
performing one or more mathematical calculations uponthe image pixel data. There is
only one goal in applying any image processing function and that is to produce an im-
age that more clearly represents the microstructure of interest. To achieve this single
result, image processing functions are commonly used in microstructural images for
the removal of artifacts that obscure the image structures of interest and to enhance or
exaggerate image structures so as to maximize the possibility of uniquely delineating
andtherefore more accurately measuring the structures.
The goals of image processing shouldbe identical tothose of materialography, that
is, to produce a visible microstructure withno artifacts that is the truest possible depic-
tionof the material structure for the intendedpurpose. The applicationof moderncon-
trolled metallographic/materialographic processes results in observable microstruc-
tures that optimally reveal the material structural or phase constituents, or both.
Consequently, materialography or metallography is actually the most powerful image
processing tool available, in that the mechanical or chemical processes employed are
designed to physically produce true microstructure, whereas software-based image
processing relies on mathematical calculations performed upon an image to produce a
newimage displaying a structure whichinfact does not exist physically.
All applications of image processing will alter the image illumination distribution.
Therefore, any image that exists as the result of image processing is not true micro-
structure. Such an image is not necessarily bad. But recognizing this simple truth
leads to the inescapable conclusionthat inall cases electronic image processing should
be strictly limited to only those operations without which the original image would
remain unmeasureable or for purposes of human visualization to enhance the struc-
ture visibility. In regard to quantitative materials science, image processing operations
should be applied only in so far as they render the image more measurable or more
viewable. So the application of image processing processes is determined by the state
of the real world image and the use to which the digital image is to be put. In furthering
the purpose of materialography or metallography, that is to reveal microstructure for
subsequent measurement or examination, digital image manipulationis nothing more
than another process for materials specimen preparation. Digital image preparation
shouldbe usedas a secondary class of techniques to be appliedonly if the primary class
physical metallographic/materialographic methods has failedtoprovide the required
structural visibility.
There are a very large number of image processing functions available in most im-
age analysis software products. Of the many possible image processing operations a
relatively fewprovide useful results inpreparationof materials microstructure images.
Presented here is a short list of several image processing functions that are frequently
applied to improving microstructural images. For an extensive discussion of many
more image processing techniques see Russ.
3
Background Correction
A common artifact resulting from poor microscope illumination alignment is observ-
able as bright or dark areas within the image. Background correction is an image pro-
cessing programthat is usedtoreduce unevenimage illuminationdue tomisalignment
of microscope lighting. Microscope illumination alignment must always be centered.
All possible physical positioning and optical path alignment adjustments must be
made to the microscope or metallograph prior to performing software-based back-
ground correction. A common method of software background correction performs a
subtraction of a poorly illuminated image with a second copy of the same image show-
ing only the background. The background-only image canbe produced by digitizing an
image of a uniform white surface or by defocusing the optics to obliterate all image
features. Abackgroundcorrectionoperationyields a resultant image that has beencor-
rected. The images inFig. 18.6illustrate this process.
Figure 18.6c clearly shows that the dark edge seen in Fig. 18.6a has been re-
moved by the background correction. Also note that several dust particles present
within the lenses of the microscope or camera used to capture the image are visible in
both Fig. 18.6a and 18.6b and have been removed by the correction software. A side
effect or artifact of the background correction process is that the right edge of the im-
age is now slightly brighter than the balance of the image. It is a near universal truth
that the application of image processing functions seldom provides results that are
wholly without artifacts. The existence of some degree of nonuniformimage illumina-
Fig. 18.6aUnevenly illuminated image.
Fig. 18.6bBackground only copy of Fig. ???
tion may be acceptable provided it does not interfere with the measurement of the
structures of interest.
Contrast Stretching
Once digitized the image brightness and contrast may be altered using image process-
ing software. Again, it is important to use the illumination controls found on the imag-
ing system microscope being able to optimize image brightness and contrast before
resorting to software processing functions. Adjustments to brightness and contrast
should always be performed to increase the amount of illumination data available. See
Section 18.3 for examples of brightness and contrast changes to the amount and range
of data inthe digitizedimage.
Stretching techniques increase image contrast by expanding the brightness values
found in the original image into a wider range of values. Stretching is generally applied
to images that display a narrow range of illumination levels in their initial digitized
state. One approach to stretching determines the minimum and maximum illumina-
tion levels within the image and mathematically extrapolates these values to cover the
maximumpossible range, 256values inan8-bit gray scale image, as seeninFig. 18.7.
Notice that there are no 0 or 255 brightness level pixels within the image extreme
left and right ends of the distribution in Fig. 18.7a. Figure 18.7b displays the same
image after applying a contrast-stretching program to radically expand the illumina-
tion range contrast. In addition to increasing contrast across the entire image illumi-
nationrange, it is possible toincrease the contrast withina specic part of the illumina-
tion range. Stretching of this type may be helpful if several material phases have nearly
contiguous or slightly overlapping illumination ranges. This enhancement is per-
formed by dividing the histogram into three sections: brightness values that have a
value belowa dark-end threshold some value greater than the minimumillumination
values in the image; brightness values above a bright-end threshold some illumina-
tion level less than the maximum; and brightness values lying between the dark and
bright thresholds. brightness values that lie below the dark threshold are assigned a
newvalue of 0. Similarly, values that lie above the bright threshold are assigned a value
of 255. The remaining values between the dark and bright threshold are assigned new
brightness levels between 0 and 255, according to a linear mathematical extrapolation
and are thereby stretched slightly to provide a calculated set of structural brightness
levels. The histograms inFig. 18.8display the effects of this type of stretching.
Fig. 18.6cResultant image after applying background correction.
This formof histogramstretching eliminates lowand high pixel brightness values
that do not represent the structures of interest by setting them to 0 or 255. Notice the
highpixel counts at the extreme ends of the distribution.
Fig. 18.7aNarrow illumination range.
Fig. 18.7bEntire range stretched.
Fig. 18.8aOriginal image.
Watershed Filter
The watershed lter is a mathematical function that transforms an image containing
individual particles that are touching or fused together into a new image wherein the
touching or fusedobjects have beenseparated. This is a very useful tool because several
quantitative metallography/materialography standards require the measurement of
individual objects. In material microstructure analysis the watershed lter can be ap-
plied to grain size measurement as well as to other structures where it is desirable to
measure individual particles within the unprocessed image that are touching. ASTM
Standard Test Methods for Determining Average Grain Size Using Semiautomatic and
Automatic Image Analysis E 1382 for grain size measurement by image analysis de-
scribe procedures incorporating individual grain area measurement. To achieve maxi-
mumaccuracy eachgrainmust be separated.
Figure 18.9a shows a steel grain boundary structure. Notice that the dark linear
grain boundaries are broken and do not completely delineate the individual grains.
Frequently the condition of uneven and incomplete grain boundary denition is pro-
Fig. 18.8bMiddle values expanded.
Fig. 18.9aGray scale image showing incomplete grain boundaries.
duced when revealing grain boundaries by chemical etching. The watershed lter can
be applied to such images and ideally will produce an image such as seen in Fig.
18.9b, which shows all the grain boundaries completed. Such an image can be easily
measured using automated methods see Section 18.5.3 for additional discussion of
grainsize measurement.
Another example will illustrate risks of applying image processing functions as
well as demonstrate another function that occasionally is useful in materials measure-
ment. In Fig. 18.10a below, a materials image showing darker second phase particles
within a light gray matrix has been digitized. To accurately count or measure the indi-
vidual particles a watershed separation processes has been performed. The resultant
binary image with particles assigned to white and the matrix to black is shown in Fig.
18.10b.
The separation function has been fairly successful, having split many of the previ-
ously touching particles by constructing a black line between them. Note that the con-
Fig. 18.9bBinary version of Fig. ??? after watershed separation operation to ll in missing
boundaries.
Fig. 18.10aTouching particles.
structed separations tend to give angular and geometric rather than smoothly curving
edges to the particles. This type of mathematical artifact is typical of many image pro-
cessing operations and while the results are less than perfect, the slight distortion in
particle boundaries is more than offset by the overall improvement in particle measur-
ability. However, the separation has produced two relatively serious errors. In one in-
stance, near the upper center part of the image, a small triangular particle has been
created in the separation process that clearly does not exist in reality. Also, near the
lower right corner of the image a small particle has been incorrectly cracked in half.
Close examination of the Fig. 18.10a image reveals that small bright dots are found
within the particles at the site of the incorrect separations. In fact, just as in materials
where small voids or impurities can produce structural weaknesses that act as origin
sites for failures, these bright spots within the image have served as nuclei for the fail-
ure of the separation process. Caution should be used in the application of the separa-
tion function since the manufactured boundaries may result in the separated particles
having slightly altered dimensions. As discussed below, applying additional image pro-
cessing operations prior to running the separation program can minimize the occur-
rence of these errors.
Smoothing
There are a large number of processing operations designed to alter individual pixel
brightness values based upon the values of surrounding pixels. Such spatial ltering
operations exist for increasing or decreasing illumination changes within pixel neigh-
borhoods. When separating touching particles, a prior ltering operation that reduces
or smoothes illumination variability can eliminate bright spots that may lead to errors.
Applying sucha lter results inthe image showninFig. 18.10c. Compare Fig. 18.10c
withFig. 18.10a, nothing that the smoothing lter has remove the bright spots. Apply-
ing the watershed separation operation to the image in Fig. 18.10c yields the image
showninFig. 18.10d.
Figure 18.10d displays a very good separation of the particles with no grossly in-
accurate particle shapes. This example has demonstrated the ability of image process-
ing programs to both reduce as well as increase artifacts present within an image as
Fig. 18.10bAfter separation.
well as the potential benets of performing a series of image processing operations to
achieve an optimal result. Developing a multi-stage image processing procedure is
muchlike developing a metallographic/materialographic specimenpreparationproce-
dure. It is extremely important to note, however, that since the outcome of any given
image processing operation is directly dependent upon the level of illumination in the
original image, any change to the illumination level may result in an entirely different
result.
Sharpening
Sharpening is an image processing operation that is designed to accentuate the edges
of objects withinthe image. It canbe thought of as a way to bring anobject into sharper
focus. The gures below illustrate the visual as well as quantitative effects of sharpen-
ing. Figure 18.11a shows a portion of a micron scale. Figure 18.11b is a plot of the
pixel brightness levels measured along the horizontal section line drawn in Fig.
18.11a. Note that the brighter scale lines result in spikes on the illumination value
plot.
Fig. 18.10cSmoothed image.
Fig. 18.10dMore accurate separation.
A typical sharpening function has been applied to the same image and the results
are displayedinFigs. 18.11and18.11c and18.11d.
Visually the scale lines in Fig. 18.11c are more prominent and show more con-
trast between the lines and the gray matrix areas. The plot in Fig. 18.11d shows a dis-
tinct dip at the base of the spikes indicating a greater illumination difference in the
pixels at the boundary where the scale lines and the matrix meet. These visual and
quantitative changes are characteristic of the image sharpening process. By blowing
upa sectionof the image the effects of sharpening canbe seenindetail.
Note the exaggerated black to white illumination transition along the edges of the
sharpened image scale line in Fig. 18.11f. Also notice the visible pixel brightness arti-
facts created in the matrix area immediately above the scale line in the sharpened im-
age. Exaggerating minor image brightness variations may cause difculties depending
on the ultimate goals of the analysis. Sharpening lters can be valuable in enhancing
images for human viewing and can be helpful in reducing the so-called halo effect
when performing automatic detection of objects for measurement see ASTM Stan-
dard Practice for Obtaining JK Inclusion Ratings Using Automatic Image Analysis E
1122.
Fig. 18.11aScale with section line.
Fig. 18.11bPlot of illumination along section line.
Many other image processing functions including lters and morphological op-
erations exist and are commonly found in commercially available image processing
software. For a thorough discussion of many of these processing functions see the
workof JohnC. Russ.
2
18.3.7 Image Calibration
To measure the physical extent of structural features within a digital image, it is neces-
sary to create a spatial calibration. The process of calibration is the method by which
actual measurements may be extracted from any object displayed within an image. A
calibration is a numerical ratio that denes the relationship between a pixel and a real
world measurement unit such as a millimetre. Recall that a pixel is the unit building
block from which the entire digital image is formed. Spatial calibration provides a
height and width dimension for the image pixel. Within any digital image, all pixels are
identical in horizontal and vertical dimension. By assigning horizontal and vertical
pixel dimensions, structural features can be measured by counting the number of pix-
els within the feature and multiplying by the appropriate spatial calibration factors.
Pixel calibration factors are generally created for each of the magnication options
Fig. 18.11cSharpened image.
Fig. 18.11dExaggerated illumination at edges.
available through the microscope or other device that is used to acquire images for
analysis. A calibration must be associated with an image prior to performing any mea-
surements within the image. A notable exception to this requirement is the case of per-
cent area or other relative measurements wherein the desired data are expressed as a
ratioandcanbe calculatedby pixel counting.
The general process of creating a calibration involves the digitization of an image
of a scale or other object for whicha dimensional distance is known. Inmicroscopy this
is usually a slide micrometre having an etched scale in inches, millimetres, or microns,
or a geometric shape such as a circle or square with a known dimension. Figures
18.12a, 18.12b, 18.12c, and 18.12d illustrate the calibration process. First a slide
micrometre is placedonthe microscope stage, aligned, andthe image is digitized.
After the scale image is digitized the operator initiates a series of steps that include
Fig. 18.11eUnsharpened blowup.
Fig. 18.11fSharpened blowup.
drawing a calibration line on the image across some distinct distance on the scale as
seeninFig. 18.12b.
Next the software prompts the operator toenter the lengthof the calibrationline in
real worldunits, suchas millimetres, as showninFig. 18.12c.
The image analysis systemsoftware uses this information to calculate the calibra-
tion factor. Figure 18.12d shows a typical software control where the resultant cali-
brationfactor is displayedas a ratioof pixels per unit measurement.
Note that in the example a calibration factor is shown for both the X horizontal
and Y vertical pixel dimensions. If the image pixels are square and have an aspect
height to width ratio of 1 then the Xand Y calibration factors are the same. The pixel
aspect ratio is a function of the camera and digitizing hardware. It is very important to
Fig. 18.12aImage of portion of slide micrometre scale.
Fig. 18.12bScale with calibration line overlay.
Fig. 18.12cOperator input of calibration line distance.
determine the pixel aspect ratio and if it is not 1 then the X and Y calibration factors
must be calculated independently. Another feature on the calibration display panel of
importance is the name of the calibration. This name could include information about
how the calibration is congured, including optics, measurement units, etc. An addi-
tional essential item of information displayed and adjustable from this control is the
originof the XYcoordinate gridof pixels intowhichthe image is divided.
Althoughnot specically writtenfor use withdigital imaging systems, ASTMStan-
dard Guide for Calibrating Reticles and Light Microscope Magnications E 1951,
provides relevant informationonthe calibrationprocess see Section12.4.
18.4 Image Measurement
Once calibration has been established it becomes possible to extract data from an im-
age. It is at this point that digital image analysis becomes a tool to implement quantita-
tive metallography/materialography. Assuming that the metallographic/materialo-
graphic specimen preparation and digitization processes have yielded an image that
displays the microstructure clearly, the next task to be performed is the delineation of
the features to be measured. Atypical materials image is composed of a relatively large
area of matrix or background material within which one or more structural features
having one or more individual occurrences are distributed. To extract measurements it
is necessary to separate the pixels that represent the features of interest fromthe pixels
that represent the matrix or background material. This is a data reduction operation to
separate pixel data that are associated with the microstructure of interest from all
other pixel data.
It is interesting to note that from this point forward what is taking place is data
processingnot image processing.
There are two basic approaches to dening and separating the features within the
Fig. 18.12dTypical operator for control for creating spatial calibration.
image to be measured. In the more basic method the equipment operator interactively
delineates the points, lines, or areas tobe measured.
18.4.1 Manual Measurements Operator Denes Points, Lines, or Areas
Manually indicating what is to be measured by operator interaction is a simple yet use-
ful method of extracting measurements frommicrostructural images. In general there
are three possible forms to be delineated by direct operator interaction, points, lines,
and areas. Figure 18.13a shows an image of a grain boundary structure. Exercising
the line feature creation tool available with nearly all image measurement software the
operator can use the computer systemmouse to position the cursor on a grain bound-
ary, then click the mouse button and drag the cursor to another point on the grain
boundary. Another mouse click and the image measurement software immediately
counts the number of pixels in the line, calculates the length of the line, and notes the
distance onthe image.
A slightly different implementation of the same techniques allows the operator to
trace an outline of a complete grain boundary and the measurement software can im-
mediately calculate the grainarea as showninFig. 18.13b.
While manual measurement techniques are basic and require operator input, they
should not be overlooked as a viable means for accurately extracting measurement
data frommaterials structure.
Fig. 18.13aGrain diameters measured.
Fig. 18.13bGrain boundaries traced and grain areas measured.
18.4.2 Automatic Measurements Objects Dened by Image
Segmentation
Of all the many advantages of digital image analysis, possibly the single most powerful
is the process of delineating and measuring structural features over multiple elds of
viewwithout the necessity of operator interaction. The ability to measure dozens, hun-
dreds, and even thousands of individual occurrences of structural features without
constant operator involvement is a strong incentive for the implementation of image
analysis for quantitative metallography/materialography. Such automation of extract-
ing data from materials images based upon the concept of image segmentation. Seg-
mentation provides a means whereby, after initial operator setup, features can be de-
lineated and thus measured without additional operator input. In segmentation the
image is divided into the structural features of interest and the matrix or image back-
ground based upon the pixel illumination values. The division is based on the histo-
gram showing the distribution of image pixel illumination values. The process of seg-
mentation produces a range of values having a lower limit and an upper limit within
the overall image illumination distribution. The segmentation range is set to match as
closely as possible the pixel illumination values of the structure to be measured. The
success of this process is directly dependent upon the degree to which the structures to
be measured are represented by an exclusive set of pixel brightness values. Ideally the
structure tobe measuredis representedwithinthe image by a distinct range of the pixel
illuminationvalues different fromthe pixel illuminationvalues of the matrix. All image
analysis software provides a control mechanism to allow the operator to interactively
adjust the segmentation levels to detect the features of interest. Commonly, the control
will display a histogram showing the image illumination distribution with the upper
and lower segmentation range limits superimposed as a pair of vertical lines. The im-
age itself may also be shown with a color overlay corresponding to the current segmen-
tation range settings. In effect, the color will show exactly what part of the image is
being detected. Figure 18.14a shows a portionof a typical segmentationcontrol panel
providedwithimage analysis software.
In this example the histogram of an image digitized to 8 bits 0=black to 255
=white is displayed. Notice also the bar along the top of the control; the size and posi-
tion of this bar relative to the distribution histogramis a visual indicator of the current
segmentation range setting. The 0255 setting shown is actually detecting the entire
image and is simply the starting point for segmentation adjustment. The operator, us-
ing a combination of cursor positioning and mouse clicks, must move either or both of
the segmentation limits set to achieve detection of the features of interest. Figure 18.14
b shows the image under analysis.
The darker gray objects are to be detected for measurement. Since the objects are
Fig. 18.14aSegmentation control showing distribution of image illumination.
relatively darker than the surrounding matrix material, the upper segmentation limit
must be adjusted to a lower level to exclude the brighter pixels representing the matrix.
Using the software control the upper segmentation limit can be reduced. As the limit is
moved lower, the pixels falling within the range are indicated by the bar and with a
color overlay on the actual image. This color-coding method allows the operator to
clearly see the results of segmentation at each possible level. The segmentation limit
must be lowered until the best possible delineation of the objects is achieved. Figures
18.14c and 18.14d show the nal segmentation setting on the distribution plot and
the image withthe redoverlay indicating objects detectedfor measurement.
It is important tonote twoitems regarding the setting of segmentationlevels. First,
while automatic software-controlled segmentation can be performed by virtually all
image analysis software, the accuracy of the segmentation operation and therefore all
subsequent measurements, are primarily the responsibility of the operator andinmost
cases are based upon a subjective judgment concerning the optimal limit settings. Sec-
ondly, if a relatively clear distinction between object feature illumination levels and
matrix illumination levels does not exist, the process of segmentation may be difcult
andinsome cases it may be impossible toset withadequate accuracy toproduce mean-
ingful measurement results. If the structures to be measured cannot be cleanly delin-
eated by segmentation further metallographic/materialographic specimen prepara-
tion or additional image processing must be considered. It is possible that micro-
structures of certain materials, regardless of preparation and processing, do not lend
themselves to the use of segmentation to delineate features for measurement. In such
Fig. 18.14bSegmentation control showing the image under analysis.
Fig. 18.14cIllumination distribution with segmentation range set.
cases extractionof measurements must be accomplishedinteractively.
Once structural objects have been dened by segmentation, the extraction of mea-
surement data are almost trivial. All image analysis software includes a variety of mea-
surements that may be extractedfromdenedobjects. Inmost cases the variety of mea-
surements possible greatly exceeds the requirements of common quantitative metallo-
graphic/materialographic standards. Structure area, diameter, length, width, perim-
eter, and many other measurement types can be made. In the next section the applica-
tionof these measurement methods toseveral of the most commonly employedquanti-
tative standards will be discussed.
18.5 Digital Imaging Applied to Quantitative Materialography
This section is composed of a series of detailed discussions of several of the most com-
monly practiced quantitative materials standards. The Annual Book of ASTM Stan-
dards, Volume 03.01Standards Relating to Metals-Mechanical Testing; Elevated and
Low-Temperature Tests; Metallography see Part II, Section 12.4 contains the major-
ity of standards written by this body that are applied to quantitative materials micro-
structural analysis. Other standards not found in this volume but applicable to micro-
structural measurements include: ASTM Standard Test Method for Evaluating the
Microstructure of Graphite in Iron Castings A 247 and ASTMStandard Specication
for Compacted Graphite Iron Castings A 842. One or two other quantitative methods
for whichspecic standards donot exist are includedbasedupontheir widespreaduse.
18.5.1 Percent Area Volume Fraction
One of the simplest and most widely used forms of quantitative metallography/
materialography is area, or volume fraction. To perform percent area measurements
requires image digitization but does not require calibration, since the required out-
come is a ratio. The manual standard for implementing this quantitative method is
ASTMStandard Test Method for Determining Volume Fraction by Systematic Manual
Point Count E 562. This standard relies upon the use of a grid consisting of equally
spaced points formed by the intersection of ne lines. This, of course, is a method of
Fig. 18.14dImage showing detected objects with red overlay.
digitizing the microstructure. Interestingly, ASTME562 references ASTMPractice for
Inclusion or Second-Phase Constituent Content of Metals by Automatic Image Analy-
sis E1245 for the use of automatic image analysis to determine the volume fraction.
Another standard, ASTM Test Methods for Determining Area Percentage Porosity in
Thermally Sprayed Coatings E 2109, describes the use of digital imaging to measure
percent area of a specic structural feature. Performed either manually or by com-
puter, the point counting technique is the essence of percent area or volume fraction
measurement. By denition a digitized image is composed of a number of pixels that
are, in fact, a grid of equally spaced points. All that is necessary is to count the pixels
grid points that fall within the structure of interest and divide that value by the total
number of pixels in the entire eld of view. In order for the software to calculate the
percentages, the operator must use the system segmentation control to detect the
phase or phases to be measured. The detection operation is the key step in the proce-
dure and all concerns relative to segmentation discussed in Section 18.3.6 apply. Inevi-
tably, microstructures will be encountered inwhichthe pixel illuminationvalues of the
structure to be measured and the matrix have some overlap with no distinct boundary.
In these cases setting the segmentation range necessarily requires a subjective judg-
ment on the part of the operator. The reliability of the calculated volume fraction may
be improved by employing a technique of setting several segmentation ranges to detect
the same structure. Since most imaging systems have the capability of measuring more
than one segmented range simultaneously, it is a simple matter to set several ranges for
the same structure and take the statistical average for the reported result. This ap-
proach of taking a larger sample of data is consistent with statistical thinking and the
additional measurements and calculations necessary are easily performed by analysis
software. There are other advantages to using digital image measurement software for
percent area volume fraction as well as other measurements. The possibility of apply-
ing a color overlay to the image to highlight the measured phases provides an excellent
visual aid to the operator and yields highly informative images for inclusion in the re-
sults report.
Another advantage is the capability of the image measurement software to pro-
duce data that may be exported directly to external analysis and reporting software
suchas database, statistical process control, andspreadsheet programs.
18.5.2 Inclusion Rating
Inclusions are occurrences of precipitates or other products of indigenous processes
that result in random distributions of observable particles in the matrix material. Be-
cause of the signicance of inclusions in inuencing material properties, methods of
classifying and determining the level of inclusions present in materials have been de-
velopedandwidely used, primarily insteel, as a major determining factor of quality.
A number of published standards employing manual comparison as well as quan-
titative methods for determining the content of inclusions exist. ASTM Volume 03.01
includes three standards, ASTMStandard Test Methods for Determining the Inclusion
Content of Steel E 45, ASTM Standard Practice for Obtaining JK Inclusion Rating
Using Automatic Image Analysis E 1122 withdrawn 2006, replaced by E 45 and
ASTM Standard Practice for Determining the Inclusion or Second Phase Constituent
Content of Metals by Automatic Image Analysis E 1245 for determining inclusion
content.
ASTM E 45 is the original manual comparison method. Of the several methods
found in this standard by more widely practiced microscopic methods are Method A
and Method D. The heart of these methods involves classifying inclusions into four
types A, B, C, and D based upon inclusion morphology, separating each type into a
thin and heavy series based upon inclusion width and assigning each type a Severity
Level 1/ 2 to 5 based upon the total length or number of inclusions in a eld of view.
The MethodArequires the reporting of the inclusionrating for the eldof viewwiththe
most severe rating for each inclusion type. The compilation of these four ratings is the
worst eld. In Method Da specimen surface area of 160 mm
2
must be covered using
individual elds of viewof 0.05 mm
2
. This results inthe requirement to cover 320 elds
of view, eachto be rated for the severity level of all types. ASTME45 includes a series of
drawings showing the amount of inclusions at each severity level for each inclusion
type and requires that the operator judge the best comparison and record the observa-
tions.
Obviously this manual approach is quite labor intensive and has the potential to
generate subjective results particularly inthe Method Drating of 320 elds. ASTME45
is one of the best examples of a standard that has been signicantly improved by con-
verting to more quantitative and automatable methods. While incorporating the meth-
ods of E45, ASTME1122 denes inclusion typing and rating in a sufciently quantita-
tive way so as to enable these classications to be performed by image analysis
software. Although eliminating the reliance on chart comparison, ASTM E 1122 pre-
serves the traditional severity level-rating scheme rather thanrequiring a more statisti-
cally robust results report. In recognition of this short-coming ASTME 1245 has been
published and provides a thoroughly quantitative method withstatistically relevant re-
porting of results.
Following the ASTM E 45/E 1122 standard to perform the severity level rating of
inclusions using digital imaging software requires rst the separation of the inclusions
fromthe matrix by the process of segmentation. The matrix of the steel microstructure
after specimen preparation has a very high illumination level nearly white. The type A
sulde inclusions are generally quite high in illumination levels and appear in a gray
scale digital image as light gray. A-type inclusions may be close to the matrix in illumi-
nation level and therefore the requirements for specimen preparation and lighting op-
timization are critical. Background correction may be required to ensure that the A
types can be successfully segmented without detection of bits of the matrix. Inclusion
types B, C, and D are the oxide types and generally appear as black objects in the ma-
trix. The B types are sometimes described as broken stringers and occur as a series of
three or more particles strung out in a line; C types are single particles called stringers
having an elongated form with an aspect ratio of greater than designated in the stan-
dard. The D types are globular oxides and are circular with aspect length to width
ratios of less than designated in the standard. The B, C, and D oxide type inclusions
must also be separated from the matrix by segmentation. Normally segmentation to
separate the B, C, and D types is not difcult due to their high contrast with the bright
matrix.
Separation of the sulde A type inclusions fromthe B, C, and Doxide types is gen-
erally straightforward since the A types appear as brighter objects than the darker ox-
ide types. Once segmentationis established the measurement of lengthand widthof all
inclusion types and counting of the D types must be performed. These data are then
used to calculate the severity levels for each inclusion type. For many image analysis
systems, the specimens must be oriented on the microscope stage such that the elon-
gated inclusions are aligned horizontally or parallel to the X axis of stage movement.
Several difculties can be encountered when implementing this standard. To begin
with, inclusion ratings must be made for a specic eld area 0.05 mm
2
. If this area
cannot be displayed ina single digitized image, it is necessary to digitize and measure a
sequence of images until the 0.50 mm
2
area has been achieved before a rating can be
calculated. The need to measure and accumulate data over multiple images requires
more complex software and will be more time consuming. To improve efciency an
attempt should be made to choose a combination of camera lens and microscope ob-
jective magnication to yield a digitized image area of 0.50 mm
2
. Another difculty
may be encountered because of the standard requirement that inclusions as thin as
2 m be measured. Such small objects can be difcult to distinguish from commonly
occurring artifacts that possess illumination levels similar to the inclusion types. Any
scratches visible on the specimen surface after materialographic preparation may be
detected as an elongated A or C type inclusion, although generally imaging software is
designed to eliminate such artifacts due to their orientation. Amore common problem
is the misdetection of small circular artifacts as D type inclusions. It is nearly impos-
sible to separate with software ltering legitimate D types from artifacts of this class
and therefore it is absolutely essential to perform inclusion measurement only on
specimens that are freshly prepared in order to minimize the occurrence of corrosion,
oxidation, or staining. Another issue arises from the requirement to measure a rela-
tively large specimenarea, 160 mm
2
.
As mentioned earlier 320 images are needed to cover this area at 0.50 mm
2
per
image. Obtaining such a large number of images can obviously take a signicant
amount of time and has naturally led to the use of motorized microscope stages that
can be programmed to move the necessary number of elds without the need for
manual operator interaction. While without question an improvement, the use of mo-
torized stage movement along with motorized focusing procedures to eliminate opera-
tor interaction during the inclusion measurement process can also lead to problems. It
is inevitable that an unattended, fully motorized, and automatic inclusion rating pro-
cess will produce some eld ratings that are incorrect. Two types of errors are com-
monly encountered. Excessively high severity levels can be calculated because image
artifacts scratches, dust, oxidation spots, stains, etc. have been measured as inclu-
sions. Alsoslightly out-of-focus images canbe digitizedtodisplay inclusions withexag-
gerated dimensions that produce results higher thanactual severity levels. More rarely,
the focus is so far off so as to cause complete failure to detect any inclusions present in
the image. Falsely high eld measurements can be agged and the images stored sepa-
rately so at the conclusionof specimenmeasurement the operator may check the list of
suspect rating data and review the associated images. Any images displaying obvious
artifacts may then be removed from the rating database. Incorrectly under rated im-
ages are impossible to discover, short of an operator examination of every image rated.
This of course is impractical and completely defeats the desire to eliminate direct op-
erator involvement in the measurement process. Several additional error sources can
be identied including misclassication of inclusion type by the software. In contrast
to ASTME45 and ASTME1122 the ASTME1245 provides another approach to inclu-
sionrating.
ASTM E 1245 is a primary example of a stereologically and statistically robust
quantitative microstructural quality standard. The Procedures Section of E 1245 lists
the Measurement of Stereological Parameters including volume fraction of the inclu-
sions, the number of inclusions per eld, and the number of interceptions of the inclu-
sions per unit lengthof test line. Additional individual inclusionfeature measurements
may be made. From these basic measurements, statistical parameters such as aver-
ages, standard deviations, 95 % condence interval, and percent relative accuracy are
to be calculated for each type of inclusion detected. An important aspect of this stan-
dardthat is signicantly different fromits predecessors is the eliminationof separating
inclusiontypes intothinandheavy andcalculationof severity levels.
The stereological and statistical procedures embodied in the ASTM E 1245 stan-
dardmake it animportant additiontothe traditional severity rating level methods.
18.5.3 Grain Size
Grain size is a key determiner of materials properties. Several standards, both qualita-
tive and quantitative exist that describe methods for determining grain sizes see Sec-
tion 17.3. ASTM Standard Test Methods for Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis E1382 is a quantitative standard writ-
ten for implementation via digital image analysis that is based on many of the same
measurement parameters described in the quantitative methods of the ASTM Stan-
dard Test Methods for Determining Average Grain Size E 112. The several variations
in methods described in both of these standards are derived from measurement of ei-
ther grain interior areas, grain boundary lengths, or the interceptions of these features
with some pattern of test lines. The chief difculty in applying digital image analysis to
grain size determination arises from the problem of grain boundary delineation. To
showthe grain boundaries in most materials requires some formof chemical etching.
Acidic etch compounds may erode the material at the structurally weaker boundary
between grains producing a slight groove that has a lower illumination level when
viewedwitha microscope see Part II, Chapter 13. Some acidic etchants, suchas Nital,
whenappliedtosteel, chemically dissolve grains at different rates basedoneachgrains
crystal orientation. This difference in attack creates differences in elevations at the
boundaries betweenadjacent grains resulting inwhat appears to be, inbright-eldillu-
mination, black lines at the boundaries betweengrains. Inpractice the precise and uni-
form application of etchants is difcult to achieve and along with naturally occurring
variations in material etching rates, results in grain boundary visibility and appear-
ance that is highly variable. Evenwithina single microscopic eld of viewit is common
to observe strongly etched boundaries immediately adjacent to areas that display
faintly or incomplete boundary delineation. In fact, the preparation of microstructural
specimens with 100 %grain boundary delineation is uncommon. The boundary delin-
eation issue is so signicant that the ASTM E 1382 standard prefaces all discussion of
digital image measurement methods with the statement The precision of grain size
measurements using automatic image analysis is highly dependent on the quality of
the etch delineation of the grain boundaries. The grain boundaries should be fully and
uniformly delineated. If the boundary between adjacent grains is incomplete when
using a grain area method, the separate grain areas will be measured as one, resulting
in erroneously high grain area data. Similarly, missing boundaries will produce an in-
accurately low measurement when employing a grain boundary length method of
grainsize determination.
In nearly every case the application of a watershed type digital image lter must be
applied to improve grain boundary delineation before measuring grain features with
digital imaging systems. This process is commonly referred to as grain boundary re-
construction; see Section 18.3.6 for a discussion of the watershed lter. It is important
to note that the watershed lter can be too aggressive in dening boundaries; the lter
typically connects truncated grain boundaries but also tends to connect any dots ap-
pearing in the grain interiors to form boundary networks. This action can result in a
virtual fracturing of grains intosmall pieces.
Minimization of this effect can be achieved by careful operator adjustment of the
segmentation levels. Most implementations of this lter require that the operator set
the segmentation levels to select the grain interiors. In practice it may be advantageous
to set the segmentation range to over detect the grains, i.e., include some of the lighter
boundaries and grain interior artifacts along with the grain interiors. Observing the
results of boundary reconstruction at several different segmentation levels and select-
ing the most accurate level should be a part of the standard analysis procedure. It may
also be necessary to run one or more digital image processing functions designed to
eliminate grain interior artifacts that can serve as sites for nonexistent boundary con-
struction. Ultimately, it may be necessary for the operator to manually insert, via a soft-
ware drawing function, missing boundary sections. This operationobviously lacks ef-
ciency and should be avoided. In reality, boundaries have no dimensions, but in any
graphical representation they will have some width. Depending on the magnication,
the grain size and the width of the boundaries, an area reduction introduced by the
boundary delineation could be signicant, thus the boundary thickness should be kept
toa minimum.
After performing the appropriate image processing steps to reveal the complete
grain boundary network in a specic image, the image processing software can pro-
duce a binary, or black and white image with only the boundaries shown. An image
composed of only test lines in any orientation and density, linear or circular or virtu-
ally any other conguration can be constructed by software. This test line image can
be mathematically combined with the grain boundary image using a class of image
processing functions commonly termed image arithmetic. The imaging software can
produce a resultant image showing just the points where the test lines intercept the
boundaries. This is accomplished by checking pixels at exactly the same coordinate
location in both images and if the location is occupied by a boundary and by a test line
it is counted. Alternatively other image arithmetic functions may be performed to yield
animage showing just the lengths of the test lines falling withinthe graininteriors. The
grain intercept lengths displayed in these images can be measured to provide the mean
lineal intercept length, a method of grain measurement described in ASTM E 1382 as
well as in ASTM Standard Test Methods for Characterizing Duplex Grain Sizes
E1181.
In reality, perfect grain boundary delineation is not necessary. It is perfectly ac-
ceptable that over any given number of elds measured there will be some over and
some under-measured grain areas or boundary lengths. Since the statistical reporting
requirements of the quantitative standards provide methods for determining measure-
ment accuracy based on statistical parameters such as condence interval and percent
relative accuracy, if, after measuring a specimen area, appropriate statistical signi-
cance levels are not produced, then it is necessary to measure more grains in more im-
ages. Typically, imaging systemsoftware accumulates the grainfeature measurements,
as they are collected over multiple images. Based on these raw measurements the re-
quired statistical parameters are calculated. One advantage in delineating and collect-
ing individual grain areas for average grain size determination is that in the same
dataset the largest grainarea and clusters of grains canbe found. The largest grainarea
canbe usedtosatisfy the requirements of ASTMStandardTest Methods for Estimating
the Largest GrainObservedina Metallographic SectionALAGrainSize E930. Even
Table 1 of ASTM E 930 listing the relationship of the ALA grain area to the grain size
number can be created easily in software such that the grain size number can be auto-
matically reported, further streamlining the performance of ALA grain size analysis.
Grain area cluster data can be useful in characterizing duplex grain sizes as described
inASTME1181.
18.5.4 Degree of Banding
The nature and importance of quantifying banding in microstructures is discussed in
Section 17.5. ASTMStandard Practice for Assessing the Degree of Banding or Orienta-
tion of Microstructures E 1268 provides quantitative as well as qualitative methods
for assessing the degree of banding. The standard requires the measurements of vol-
ume fraction and count of feature interior interceptions or feature boundary intersec-
tions with superimposed test grid lines. Both of these operations have been discussed
see Sections 18.5.1 and 18.5.3; they can be performed using digital imaging tech-
niques providing the banded structures exhibit a sufciently high degree of illumina-
tioncontrast toenable successful segmentation. Applicationexibility is increasedand
segmentation requirements relaxed if the imaging software provides the option for di-
rect operator insertion or deletion of the test line-feature interceptions or intersec-
tions. The only other condition to be satised for banding measurements is to orient
the image so that the deformation axis seen in the structure is aligned horizontally or
vertically in the digitized image. While image rotation can be performed by software to
avoidintroductionof image processing artifacts, it is preferable toachieve the required
structure alignment by physically rotating the material specimen on the microscope
stage.
18.5.5 Depth or Thickness Measurements
Several standards exist that address the linear measurement of depth or thickness of
structures, zones, and layers. These include ASTMStandard Test Methods for Estimat-
ing the Depthof Decarburizationof Steel Specimens E1077 andASTMStandardTest
Method for Measurement of Metal or Oxide Coating Thickness by Microscopical Ex-
amination of a Cross Section B487. These standards rely primarily on the use of eye-
piece reticles or lar micrometres to performthe necessary measurements. Digital im-
aging offers several approaches to emulate the nondigital quantitative procedures.
When measuring the depth or thickness of structures that exhibit a strong contrast
with surrounding or adjacent material the segment and combine techniques de-
scribed in Section 18.5.3 may be used. Briey, an image of the segmented layer to be
measured is mathematically combined with an image of a set of section lines. A result-
ant image is produced that displays only that portion of each section line that lies on
the segmented layer and these lines are measured. While section lines may be discon-
tinuous, the image analysis software calculates the overall length of each horizontal
rowof line segments no matter howmany segments into which the line is broken. The
actual thickness measurement is made starting fromthe left end point of the left-most
segment ineachrowand nishes at the right end point of the right-most segment inthe
row. Figures 18.15ae depict this process.
For structures lacking the contrast touse the segmentationapproachthe measure-
ments can be made using operator interactive methods to construct point-to-point dis-
tances or parallel lines that are measured by the software. These methods are the digi-
tal equivalents of positioning lars for thickness measurement, withthe operator using
the computer mouse to position lar lines on the digital image as displayed in Figs.
18.16a and18.16b.
Fig. 18.15bBinary segmented
Fig. 18.15aImage of coating.
Fig. 18.15cBinary section line image.
One of the additional advantages in using digital imaging systems for thickness-
type measurements is that annotations showing measurement lines as well as the mea-
sureddistances canbe addedtothe image automatically by the software.
18.5.6 Graphite in Iron Castings
ASTM Standard Test Method for Evaluating the Microstructure of Graphite in Iron
Castings A 247 is essentially a qualitative chart comparison standard, applied to duc-
tile, gray and malleable irons. For nodular ductile and ake gray iron particles a size
maximumdiameter or length classication chart is given. Much could be done to im-
prove this standardby introducing additional quantitative procedures. The highly con-
trasted nature of microscopically observed graphite in prepared cast iron specimens
make the use of segmentation-based digital image measurement of these structures
quite straightforward. Well prepared specimens that do not exhibit graphite smearing
seldom require extensive image processing since the dark nearly black graphite
shapes are strongly contrastedwiththe bright white of the cast ironferrite matrix.
One problem that may hinder automatic measurement is the possibility, particu-
larly in gray iron, of touching graphite particles. The application of a separation lter
Fig. 18.15dCombined 18.15b and c.
Fig. 18.15eSection lines over coating.
may reduce these occurrences and as a nal solution manual editing of the image may
be undertakentoseparate massively touching particles.
Ductile Cast Iron
Although not incorporated into any ASTMstandard, an important factor in determin-
ing ductile or nodular iron product acceptability is the percentage of graphite particles
that are nodular. Digital imaging systems provide outstanding capabilities for calculat-
ing the percent nodularity. The classic function used to calculate particle roundness
nodularity is the shape factor. While several equations exist for calculating shape fac-
tor the most commonly usedis:
Shape Factor = 4
*
Pi
*
Particle Area/Particle Perimeter
2
To calculate nodule shape factor the area andperimeter of eachgraphite particle is
Fig. 18.16aVertical lar.
Fig. 18.16bHorizontal point-to-point.
measured. These values are entered into the equation and the shape factor number is
produced. Possible shape factor values range from 1.0 for a perfectly circular particle
downward towards 0 for increasingly uncircular shapes. Some shape factor level
must be chosen as a lower limit to dene the most uncircular shape to be considered
nodular. This value is often set to 0.6, so that graphite particles have a shape factor
equal to 0.6 or greater are nodules, and those with shape factors less than 0.6 are not.
Percent nodularity can then be easily calculated by dividing the total count of nodules
by a count of all graphite particles. The precision with which the imaging software de-
nes the particle perimeter lengthhas a signicant effect onthe outcome of the calcula-
tions. In particular, the measuring of small undulations in perimeter can signicantly
alter the percent nodularity since the perimeter is squared in the calculation of shape
factor. Figure 18.17a shows a nodule in an enlarged portion of a digital image. In this
view the imaging software was adjusted to measure the graphite perimeter using just
eight line segments seenas darklines aroundthe perimeter.
In Fig. 18.17b the software was readjusted to use 128 line segments to dene the
object perimeter. The 8-line delineation yields a perimeter of 0.47953 mm while the
Fig. 18.17a8-line perimeter.
Fig. 18.17b128-line perimeter.
128-line perimeter is 0.51311 mm in length. The shape factor of Fig. 18.17a is 0.929
while the shape factor of Fig. 18.17b is 0.869, a signicant difference. This example
illustrates the importance of the software algorithms used to dene objects and extract
measurements. The algorithms are in fact critical functions in the process of data pro-
duction. As such their contribution to the end result must be understood and con-
trolled if reproducible structure measurements are to be achieved. Attention to such
internal software methods is especially important when results produced by several
separate digital imaging systems are tobe compared.
Gray Cast Iron
The length of graphite akes in gray iron can normally be readily measured fromdigi-
tal images. The lengths can be input to calculations of the percentage of the akes fall-
ing ineachof the size classes listed inASTMA247. However, the task of digitally classi-
fying the Graphite Distribution Patterns as types of graphite akes described in the
standardis beyondthe capability of commonimage analysis techniques.
Compacted Graphite
Compacted graphite cast iron contains graphite particles in shapes that are intermedi-
ate between ake and spheroid shapes. This type is dened by the ASTM Standard
Specication for Compacted Graphite Iron Castings A 842 as The acceptable graph-
ite formation in the microstructure shall contain 80 % minimum Type IV graphite as
depicted in ASTM A 247 which may be arrived at by usingautomatic image analysis
methods. Also, this type is described as cast iron with the graphite in compacted ver-
miform shapes and essentially free of ake graphite. Based uponthese guidelines it is
possible to produce imaging software to calculate the percentage of graphite that is not
spheroid calculate shape factor as in ductile cast iron except the percent particles that
are not spherical is found. Also, to ensure that there is no ake graphite present, the
aspect length to width ratio may be calculated. In this case since the standard does
not provide a quantitative value to separate compacted from ake graphite, a reason-
able value must be assumed and used in the software to calculate the presence of any
ake graphite.
18.6 Digital Imaging Technology
18.6.1 Hardware
Several distinct hardware components are requiredtoperformimage digitization, pro-
cessing, and analysis. Microscopes and other optical devices are not discussed here.
The basic imaging system hardware components are: computer, camera, and printer.
Recently all hardware components needed for image digitization have become avail-
able as off-the-shelf items and the need for specialized hardware components for all
common materials structure measurements is nonexistent. A general philosophy con-
cerning selection of digital imaging systems should be based upon using the most stan-
dard components available. It is no longer necessary or even desirable to purchase pro-
prietary, single purpose, single source, and fully integrated systems. Such systems
inevitably have limited shelf life, provide functionality that is behind the curve of hard-
ware capabilities available on the open market, and provide very limited and expen-
sive upgrade possibilities. With the possible exception of image measurement soft-
ware there is no component necessary for assembling a state-of-the-art digital imaging
systemthat is not widely available commercially.
Because the same technologies developed and priced for mass-marketed con-
sumer cameras, computers, and printers are used in industrial grade digital imaging
systems, the cost of the hardware components neededtoprovide image digitizing func-
tions continues to decline while the capabilities of the components continue to
improve.
Computer
Today, computers designed for normal business or even home use have more than
adequate power and information processing capabilities to run even the most sophisti-
cated materials analysis software. It is not necessary or even desirable to procure cus-
tom designed or nonstandard computers to power digital imaging systems. All of the
computer peripherals present ina typical home computer systemdesignedfor Internet
access and game playing should in most cases be present on a system for image mea-
surement. Several specic components can be briey commented upon. For viewing
images especially those delivered by large format digital cameras, relatively large
monitors are helpful. Monitors of 19 in. or larger display size and to save laboratory
bench space albeit at a premium price at, active matrix LCD monitors should be
considered. Efcient management of digital images does require relatively large capac-
ity computer memory, high processing speed, and extensive le storage space. Fortu-
nately, computer processors, memory chips, and disk drive components are among the
most cost effective of all equipment needed for digital imaging. Rapid technological
development and a long history of downward trending prices in these devices are pri-
mary reasons to avoid imaging systems based upon private label and customdesigned
hardware that cannot be readily upgradedor enhancedwithstandardcomponents.
Cameras
No other single component required to perform digital imaging is more widely avail-
able than the camera. There are literally hundreds of camera models available. Of this
vast array there are two basic types: analog and digital. The analog camera outputs an
analog electronic signal that is essentially a television signal; it is not in digital form
and requires that image digitization be performed by a video digitizing or frame grab-
ber circuit board installed in the computer.
4
Digital cameras are designed to digitize
the image signal internally and output a digital format data stream to the computer.
The key element incameras is the sensor that converts light into anelectronic signal. At
this time the predominant sensor technology is the charged coupled device or CCDsili-
con chip. Another type of image sensor becoming increasingly available is the Comple-
mentary Metal Oxide Semiconductor or CMOS. Among the specications that differ-
entiate cameras, the physical size of the chip is one of the more signicant. Chip sizes
generally range from
1
4
,
1
3
,
1
2
,
2
3
, up to 1 in. or more. Chip size is important because all
other components remaining equal, the size of the chip is directly proportional to the
size of the digital image eld of view. Asystemequipped with a camera featuring one of
the smaller chip sizes
1
4
or
1
3
in. may not be capable of delivering the required eld of
viewarea.
Obviously the quality of the image produced by the camera is important. But other
factors such as image size, ease of operation, cost, and most importantly, how the im-
ages are tobe usedshouldbe considered.
Analog Cameras
Analog cameras output a video signal that can be displayed in real time, that is, the
image signal is output fast enough to refresh the monitor display at approximately 30
times a second. For viewing images on a monitor at a display rate that produces no
noticeable delay or jerky movement when the eld of viewis moved or the image focus
is adjusted, in general an analog camera performs better than a digital camera. Since
analog cameras contain a minimal amount of circuitry the physical size of the camera
can be relatively small. In general, the more digitizing and signal processing that is
done withinthe camera, the larger the camera body.
To digitize an image the analog camera must be connected to a digitizing circuit
board mounted inside the computer. Digitizing boards can display a live signal from
the camera along with digitizing the image for storage, processing, and measurement
see Inoue and Spring for a detailed discussion of digitizing boards
4
. There are a wide
variety of digitizing boards available. When selecting a digitizing board it is important
to match the board input and digitizing capabilities with the signal output of the ana-
log camera. Many digitizing boards are available with the capability of being con-
nected to multiple cameras. This feature is useful in laboratories requiring cameras to
be mountedona microscope, a stereoscope, a microhardness tester, andmore.
Digitizing boards are suppliedwithsoftware for adjusting the boardto accept vari-
ous camera signal formats, for capturing images, and perhaps for image le manage-
ment. Digitizing board products may also include software programs called drivers
that are designed to enable the board to work directly withspecic digital imaging soft-
ware. There is anindustry standarddigitizer-to-imaging software driver calledTWAIN.
Digitizing boards and imaging software products providing the TWAIN interface can
work together and do not require any additional special software drivers. Analog
camera/digitizing board combinations provide a fast and efcient means for digitizing
images. For most material microstructure digitizing applications high-resolution ana-
log camera/digitizing boardcombinations are the best all aroundchoice.
Digital Cameras
Digital cameras digitize the image signal output from the image sensor chip before it
enters the computer. Digital cameras connect to the computer using a variety of com-
puter ports or circuit boards, some standard and some custom designed. Digital cam-
eras are available with large format image sensor chips and can digitize images into a
very large number of pixels. With their high pixel counts digital cameras can provide
excellent quality images and are generally capable of displaying ne structural details
more sharply than an analog camera/board combination. As with digitizing boards,
digital cameras will be supplied with software for image acquisition and the availabil-
ity of TWAIN software is equally important. While providing high quality images, it
should be noted that many digital cameras are slower to capture images than analog
cameras.
The real time image display rate is 30 times a second for analog output while digi-
tal cameras may require up to several seconds to display a full image. In general, the
greater the number of pixels the digital camera offers, the longer the image capture
time. Delays in refreshing the computer image display are particularly noticeable dur-
ing focusing of the image. Additionally, digital cameras may be more complex to oper-
ate than analog systems. Digital cameras should be considered when the primary use
for the digitized images is viewing, particularly when the images are to be printed. Of
course, the quality of printed images is also a function of the printer used and printers
are briey discussedinthis section.
Black and White or Color
For extracting structural measurements frommost materials a gray scale 8 bit or 256
levels of pixel illumination is adequate. In a fewmaterials segmentation to separate a
structure for automatic delineation may require the use of a 24 bit 16.7 million levels
true color image. Due to the increased difculty in setting color segmentation levels
and inefciencies attendant to managing color images, the use of color images for ex-
tracting measurements is only recommended if the measurements are not possible
with gray scale images. Color images are recommended when the primary use of the
image is for publicationandhumanviewing.
Printers
As with cameras, a very large number of computer printers are available for use with
digital imaging systems. The growth in consumer digital photography has impacted
the quality of prints and the price of image printers very positively. Inkjet type printers
that can produce photographic quality images continue to become less expensive.
The primary printer specication used to judge the potential quality of printed images
is the number of ink dots per inchthe printer is capable of putting onthe paper. Acount
of 2400 by 1200 dots per inch is dense enough to produce high quality prints. For the
highest quality images coated photographic type paper must be used. Another type of
printer technology known as thermal dye diffusion can produce a continuous-tone
print with resolution of 300 pixels-per-inch. The quality of these prints is termed pro-
fessional grade and these printers have prices in the range of one order of magnitude
higher than ink jet printers. Specications and pricing level aside, it is recommended
that actual prints of material microstructures be viewed prior to making a decision on
printer acquisition.
18.6.2 Software
There is an enormous variety of digital imaging software available. A recent search of
the Internet yieldedthe following results:
SearchPhrase: digital imaging software WebPage Matches over 50 000
SearchPhrase: image acquisitionsoftware WebPage Matches over 2400
SearchPhrase: imaging editing software WebPage Matches over 400
SearchPhrase: image archiving software WebPage Matches over 400
SearchPhrase: image measurement software WebPage Matches over 300
Although not designed specically for materialographic structure imaging, the
number of image software product sources is signicant. Many of the products, con-
cepts, techniques, and software modules developed for other digital imaging applica-
tions canbe usedinmetallographic/materialographic systems. This results inthe avail-
ability of constantly improving software functionality at competitive prices. Of course,
several software systems have beendesignedparticularly for materials science applica-
tions. These should provide minimumbasic image processing functions as well as the
modules to performone or more of the metallographic/materialographic test methods
described in Section 18.5, depending on the requirements of the individual laboratory.
It is a near certainty that most imaging software packages will provide far more pro-
cessing and measurement capabilities than are normally needed in all but the most
diverse research and development environments. One of the challenges in selecting
software for materials analysis uses is in identifying products that provide the func-
tions needed to perform structural imaging tasks without the presence of extraneous
software capabilities that may complicate operation and inate costs. A few general
guidelines canbe suggested.
Obviously the most important consideration is that the software is capable of per-
forming the required tasks. What may not be so apparent is what those tasks are see
Section 18.7 for additional comments concerning software selection. The same gen-
eral criteria used in selecting any type of software are applicable. Avoid software that
can only be used with a specic computer or other hardware components. The soft-
ware should provide an open architecture that permits exchange of data and interac-
tion with other software products such as database, spreadsheet, and statistical pro-
cess control programs. The software must also follow industry standards for data and
image le formats, user interface control designs, and device connectivity. In most
cases it is advisable to avoid proprietary designs that create a sole source supplier
dependency.
Open Source/Public Domain Software
It is possible to obtain open source/public domain software like NIH Image from Na-
tional Institutes of Health for image processing/analysis. However, it should be noted
that the basic philosophy of open source software requires a strong commitment to
maintain and support the software on the part of the user. Often the typical
metallographic/materialographic laboratory is not able or willing to perform such
tasks.
18.7 Digital Imaging System Implementation
The selection of software should always be based on a thorough and realistic study of
current organizational tasks, established laboratory procedures and a realistic ap-
praisal of future requirements. A digital imaging system is not a stand-alone device; it
is a tool to facilitate the operationof a quantitative microstructural quality control pro-
gram. The same care and attention to detail should be accorded the selection of a digi-
tal imaging systemas to other organizational information management or quality con-
trol systems. Animaging systemis part of a bigger organizational structure.
In a well designed system implementation project three distinct phases can be
identied. The purpose of Phase 1 is to produce a master plan based on an analysis of
existing metallographic/materialographic operations and a denition of objectives.
Part of this phase is actually a traditional systems analysis study, undertaken to dene
in some detailed and formal manner the procedures and work ow of the existing
metallographic/materialographic operations. This information can serve as a base line
for integration of new equipment. A clear understanding of the standards to be fol-
lowed, the type of measurements necessary, and the volume of current as well as pro-
jectedwork are among the many questions tobe answered. It is alsoessential toconsult
with engineers, information technology personnel, and others within the organization
who will be in any way impacted by the new system. A very important factor in the
successful implementation of a digital imaging systemis the skill level required by the
systemoperator. Efcient operation of the imaging systemmay require a more techni-
cal backgroundthangeneral labwork; inparticular a rmunderstanding of basic com-
puter operation techniques is essential. Since quantitative metallography/materialo-
graphy is based on stereological and statistical principles the system operators must
also possess an understanding of these subjects. If an evaluation of potential system
operators reveals a deciency in these areas, suitable training programs should be re-
quired. The systemsuppliers should provide training in the operation of specic imag-
ing systems and software. However, general computer and quantitative methods
knowledge are a prerequisite and remedial instruction in these topics, if necessary, is
not the responsibility of equipment vendors. One important result of the initial phase
should be the generation of a set of expectations or specications that dene the func-
tions requiredof the imaging system.
The purpose of Phase 2 is to use the requirements, priorities, and specications
generated in Phase 1 to determine which of the many commercially available systems
will best meet the current and future requirements of the company. This phase may
include identication of potential suppliers, compilation of a list of products available,
demonstrations, circulation of a Request for Quotation, and of course, nal systemse-
lection.
Phase 3, the last step of the process, is actually placing the system into operation.
The process of converting to digital imaging from qualitative or manual quantitative
methods should have been dened in Phase 1. Implementation of newtechnology will
almost certainly necessitate changes inthe procedures used to employ that technology.
Commonprocedural points that may needchanging include:
1. Specic orientation and positioning of specimen may be required by standards or
by equipment.
2. Selection of microscope objective magnication may be signicant, i.e., eld of
viewarea requiredby standard.
3. Upgrading of preparation standards to eliminate artifacts that defeat automatic
imaging.
Often results obtained from image analysis equipment will not match historical
results based on qualitative estimates or chart comparison methods. In these cases it
may become necessary to devise a strategy to correlate pre-and post-digital imaging
results. Ideally, major issues arising during implementation will have been identied,
and the newsystemwill be placed into operation in an efcient and cost-effective man-
ner. Even with awless planning it is to be expected that the full use of the system at
maximumefciency will require a learning period.
ASTMStandard Guide for Laboratory Information Management Systems LIMS
E 1578, offers many insightful guides for the selection of a Laboratory Information
Management System. Many of these concepts may be adapted for use in selecting a
systemfor digital imaging and anexaminationof ASTME1578 is suggested. Aparticu-
larly useful idea found in ASTM E 1578 is the need to focus on functions, not technol-
ogy. Additionally, see ASTM E 2066-00 Standard Guide for Validation of Laboratory
InformationManagement Systems.
In conclusion, the objective of this chapter was to highlight some of the digital im-
aging functions that are commonly applied to materials structure images and to pro-
vide an overview of the use of image measurement techniques to implement selected
standard test methods. It is also hoped that these comments have initiated an aware-
ness of the necessity of quantitative metallography/materialography and also that digi-
tal imaging systems are but a part of an overall programfor the improvement of prod-
uct quality.
19
Digital Image Management
Archiving
A DIGITAL IMAGE ARCHIVING SYSTEM MAY INCLUDE ALL OF THE FEA-
tures and components of a full image measurement system, the difference being that
the primary purpose of archiving is to provide efcient and convenient yet powerful
methods for capturing, identifying, storing, and retrieving digital images and associ-
ated information rather than to extract structure measurement data. Such a system
may include sophisticated database software or simple ling schemes for identifying
images by a range of user denable classications and keyword associations. As with
digital image measurement systems the selection of archiving must be based upon an
evaluationof existing andprojectedneeds.
A broader view of laboratory digital imaging possibilities must include consider-
ation of the ASTMStandard Guide for Laboratory Information Management Systems
LIMS E1578 see Sections 12.4.2/3. ASTME1578 provides a detailed discussion of
LIMS concepts. Laboratory information management systems are designed to provide
total data management from initial material sample receipt through logging of all
specimen preparation procedures, recording of image acquisition parameters such as
microscope magnication brightness, contrast, segmentation levels, calibration, and
any image processing functions performed along with the original, intermediate, and
nal images as well as nal structural measurements data and many others. In short,
these systems aspire to compile a complete recordof all possible informationrelatedto
the processing of the specimen within the laboratory along with the ability to search,
retrieve, and report selected views or dynamic combinations of the information from
these records. These systems represent the most ambitious and sophisticated level of
digital system possible in the laboratory. The demands of design and implementation
of digital systems are increased by levels of magnitude when considering a LIMS. At
the most advanced implementation level, the LIMS must provide electronic integra-
tionof the technologies of many diverse instruments, requires the use of local as well as
wide area networking, and employs sophisticated database technologies. And because
they provide the several functional LIMS components as dened in ASTME1578 such
as data/information capture, data analysis, and reporting, systems for digital image ar-
chiving and structural measurement may be considered components or subsystems of
a LIMS.
References Part IV
1 Underwood, E. E., Quantitative Stereology, Addison-Wesley Publishing Company, Reading,
MA, USA, 1970.
2 Friel, J. J., et al., Practical Guide to Image Analysis, ASM International, Materials Park, OH,
USA, 2000.
3 Russ, J. C., The Image Processing Handbook, 3rded., CRCPress, Boca Raton, FL, USA, 1998.
4 Inoue, S. andSpring, K. R., VideoMicroscopy, PlenumPress, NewYork, NY, USA, 1997.
5 Freund, J. E., Statistics: A First Course, 2nd ed., Prentice Hall Inc., Englewood Cliffs, New
Jersey, USA, 1970.
619
Part V: Hardness Testing
20
Introduction
HARDNESS IS AN IMPORTANT PROPERTY WHEN JUDGING THE QUALITY
and possible applications of a material. It can also give indications concerning the ten-
sile strength, ductility, or wearing quality of the material.
Beginning in approximately 1822, quantitative evaluation of hardness was carried
out based on the hardness scale developed by F. Mohs. He ordered known minerals so
that the harder mineral scratchedthe one preceding it.
It must be noted that the differences in hardness between the individual steps of
the scale are not equal. For example, the difference between steps 9 and 10 is substan-
tially greater thanthat between1and9.
Around1900, further testing procedures were developedfor technical purposes. In
these procedures, hardness is not determined by scratching, but rather by indenting
the material to be tested with very hard objects of a specied size and shape. The
Brinell, Rockwell, Vickers, and Knoop hardness testing procedures are the best known
of these techniques.
Already in1900, Martens suggestedthe following denitionof hardness for techni-
cal purposes:
Hardness is the resistance of a material to penetration by another harder mate-
rial.
This simple conceptualizationremains the basis of our understanding of hardness
eventoday.
20.1 Indentation Hardness
Figure 20.1 schematically shows the signicant elements of indentation hardness test-
ing. A particular indenter 1, attached to the lower end of a press, is pressed into the
TABLE 20.1Mohs Hardness Scale.
Mohs Scale
Mohs Standard
Mineral
Equivalent Knoop
Hardness Number
1 Talc 2
2 Gypsum 32
3 Calcite 120
4 Fluorite 150
5 Apatite 400
6 Feldspar 560
7 Quartz 700
8 Topaz 1300
9 Corundum 1800
10 Diamond 6000
623
specimen surface 2 with a particular test force in Nor kgf and then pulled back. The
indentationthat is createdcanthenbe measured.
The shape and size of the indenter are decisive for indentation resistance. With
ball-shaped indenters, the specimen material is pushed away sideways and down-
wards through plastic and elastic deformation. Angular or needle-shaped indenters
can, in addition to the deformation, cause separation processes like cracks, especially
inbrittle materials ceramics.
Depending on the characteristics of the material being tested, various mostly non-
homogeneous deformation processes with multiple axes and varying degrees of elas-
ticity andplasticity occur withpenetration.
The speed of penetration also inuences the behavior of the material being tested.
For these reasons, the guidelines for the hardness testing procedures, including equip-
ment construction, indenter, penetration speed, optical system, and evaluation are of
particular importance.
Hardness is a distinguishing feature of a material. It is usually measured quantita-
tively according tothe following general relationship:
Hardness value = Test force/indentation size 1
Beginning in 1940, hardness testing procedures in which the penetration depth is
measured during application of a test force and then used to determine hardness were
developed. These procedures quickly gainedinimportance.
We differentiate among:
Hardness testing procedures withstatic loadaction.
Hardness testing procedures withdynamic loadaction.
Special hardness testing procedures.
Fig. 20.1Schematic drawing of hardness tester indicating force, indenter 1 specimen 2 and
support 3.
The most important of these will be shortly describedbelow.
20.2 ASTM Standards
To be able to compare hardness values, the equipment, testing procedures, testing
method, and evaluationmust correspond to particular standards. The following ASTM
standards describe the various hardness testing procedures. See Section 12.4.2 for
more standards onhardness.
StandardPractices for Force Vericationof Testing Machines E4
StandardTest Methodfor Brinell Hardness of Metallic Materials E10
StandardTest Methods for Rockwell Hardness andRockwell Supercial Hardness
of Metallic Materials E18
Standard Test Method for Rapid Indentation Hardness Testing of Metallic Materi-
als E103
Standard Test Method for Indentation Hardness of Metallic Materials by Portable
Hardness Testers E110
Hardness Conversion Tables for Metals Relationship Between Brinell Hardness,
Vickers Hardness, Rockwell Hardness, Rockwell Supercial Hardness, Knoop Hard-
ness andScleroscope Hardness E140
StandardPractice for Scleroscope Hardness Testing of Metallic Materials E448
StandardTest Methodfor MicroindentationHardness of Materials E384
StandardTest Methodfor Vickers Hardness of Metallic Materials E92
21
Static Hardness Testing Procedures
21.1 Brinell Hardness Testing
THE FIRST STATIC HARDNESS TESTING METHOD WAS INTRODUCED BY J.
A. Brinell, a Swedish researcher, at the 1900 Paris World Exposition. A hardened steel
ball or tungsten carbide ball with a diameter D of 1, 2, 2.5, 5, or 10 mm was used as
indenter. This was pressed into the smooth, clean specimen surface with a test force
F. Figure 21.1 shows the principle of test with test force F N, D the diameter of the
ball mm, d the mean diameter of the indentation mm, and h the depth of the inden-
tation mm. It is important that the specimen rests on a rigid support, and that the
indenter contacts the specimen without being shaken or jolted. The test force is then
increased to the predetermined maximumvalue within 210 s and held for 1015 s. If
the duration of load application falls outside of this range, this must be indicated. For
example, for nonferrous materials, the durationmay be as long as 180 s.
Depending on the elastic-plastic behavior of the material, the indentation may
vary. Figure 21.2 shows an ideal indentation, a, an indentation with sink-in due to a
high degree of elasticity b and an indentation with pile-up due to a high degree of
plasticity c.
21.1.1 Calculations and Procedures
The spherically shaped indentation that is created is measured. The Brinell hardness is
calculatedfromthe meanindentationdiameter according tothe following equation:
HBS or HBW= 0.102
F
A
= 0.102
2F
DD
D
2
d
2
1
where
HBS=Brinell hardness withsteel ball as indenter
HBW=Brinell hardness withtungstencarbide ball as indenter
F=test force inN
A=indentationsurface inmm
2
Fig. 21.1Brinell hardness testing, test principle. Force, kgf F, diameter of ball, mm D, mean
diameter of indentation, mm d, depth of indentation, mm h ASTM Standard E 10.
626
D=ball diameter inmm
d=arithmetical meanvalue of twomeasuredindentationdiameters inmm
The test force F is multiplied by 0.102 1/ 9.80665=1/ g to get the calculated
hardness as a unitless numerical value.
Specimen thickness should be at least ten times the expected indentation depth. If
the expected hardness of a material can be estimated, then the minimum specimen
thickness canalsobe estimated.
For the indentationdepth, it canbe assumedthat
A = Dh 2
The minimumthickness S of the specimenis then
S = 80.102F/DHB. . . 3
Steel balls can be recommended as indenters for Brinell hardness values of up to
350. They are permitted up to HBS=450. When testing harder materials, elastic defor-
mations of the ball must be expected. These lead to increased indentation diameters
and thus to erroneously elevated measured values. Tungsten carbide balls may be used
uptoHBW650.
Test results are givenas follows:
Durationof test loadapplication25
Test force identifying value 0.102 F 3000
Ball diameter inmm10
Identifying marking of indenter in this case tungsten carbide
W
Abbreviationfor Brinell hardness HB
DeterminedBrinell hardness value 410
The relatively large indentations are an advantage of the Brinell hardness testing
method. They ensure representative hardness values evenwhenheterogeneous materi-
als are tested.
Fig. 21.2Ball-shaped indentation shapes. Ideal indentation a, indentation with sink-in b
and indentation with pile-up c.
Chapter 21 Static Hardness Testing 627
It is important that the ball creates an easily measurable indentation. For that rea-
son, it is stipulated that the indentation diameter lies between 0.24 D and 0.6 D. If dif-
ferent ball diameters are used on the same material, the measured values can only be
compared when the indentations are geometrically similar. Accordingly, the test force
F must be appropriate for the ball diameter D. For comparison of hardness values, the
optimumstress level 0.102F/ D must therefore be closely adhered to. Table 21.1 shows
the relationship between stress level and measured hardness range for various mate-
rial categories.
If the material to be tested, and therefore the load ratio and the diameter D of the
test ball selected 10, 5, 2.5, or 1.25 mm, are known, then the test force F can be set on
the testing apparatus.
The minimumdistance fromthe middle of an indentation to the edge of the speci-
men should be at least 2.5 d for steel, gray cast iron, copper, and copper alloys. The
distance betweenadjacent indentations must be 4 d.
For light alloys, Pb, Zn, and their alloys, the respective distances should be 3 d
specimenedge and6 d adjacent indentations.
21.1.2 Brinell Hardness Testers
Figure 21.3 schematically shows the construction of a Brinell hardness testing ma-
chine with hand wheel 1, support 2, specimen 3, objective 4, indenter 5, loading
system7, andscreenfor measuring the projectedBrinell indentation6.
Figure 21.4 shows a modern Universal Hardness Tester for Vickers, Knoop,
Brinell, and Rockwell. It has unattended testing and analysis cycle via fully automated
image analysis for Brinell/Vickers and automatic focusing. The test load ranges are
9.81Nto2450 Nor 49Nto7350 N.
Testing procedure details can be found in the directions for use of the equipment
and in the procedural and material-specic norms, for example, the ASTM Test
Method for Brinell Hardness of Metallic Materials E 10. Internal company proce-
dural guidelines shouldalsobe observed.
21.2 Vickers Hardness
Smith and Sandland developed the Vickers method named for the English company
Vickers in 1925. The reason for this development was the fact that Brinell hardness
only provided usable results up to HBS=450, because higher test forces cause defor-
mationof the steel ball tobegintooccur.
In Vickers Hardness Testing, the indenter is a regular four-sided diamond pyramid
TABLE 21.1Stress Level and Recorded Hardness Range for Various Materials.
Stress Level Hardness Range, HB Material
30 70600 Steel, Iron 140 HB
10 22315 Ti, Ni-, Co, Cu-Alloys 200 HB
5 11158 Nonferrous metals and their
alloys
2.5 678 Bearing metals
1.25 339 Lead, tin
with an interfacial angle, , of 136. The geometry of this Vickers pyramid produces a
good correlation between the Vickers values HV and the Brinell hardness values HBS
between350and400.
The Vickers pyramid is pressed vertically into the specimenwitha test force P kgf
2 shownschematically inFig. 21.5. 1 is the face angle of the diamond136, d
1
and
d
2
3 are the diagonals of the impression mm. The mean diagonal diameter d of the
indentationis usedtocalculate the Vickers hardness.
HV= 0.9272
P
A
=
2P sin136 /2
d
2
1.8544
P
d
2
4
where
HV=Vickers hardness
P=test force inkgf
Fig. 21.3Schematic drawing of Brinell hardness testing machine with hand wheel 1, support
2, specimen 3, objective 4, disengaged indenter 5, screen for projection of the
indentation 6, and loading system 7.
1
A=indentationsurface inmm
2
d=arithmetical meanvalue of the measuredindentationdiagonals inmm
For Vickers Hardness, giveninGPa units, we ndthat
HV= 0.0018544 P
2
/d
2
2
5
withforce P
2
inNandthe meanlengthof indentationdiagonals inmm.
Because of the pyramidal geometry, the relationship between the indentation
depthandthe indentationdiagonals is h=d/ 7.0006.
For Vickers macrohardness testing, the test load must normally also be selected
such that the indentation diagonals are relatively large in comparison to the phase
components. The diagonal d should be a maximum of 2/ 3 of the specimen thickness,
and the penetration depth thus 1/ 10 of the specimen thickness, to exclude inuence
from the specimen support. This is important when testing thin sheets or layers see
below.
Fig. 21.4Universal hardness tester for all standard testing processes such as Vickers, Knoop,
Brinell, and Rockwell. Unattended testing and analysis cycle via fully automated image analysis
for Brinell and Vickers. Automatic focusing. Test load ranges: 9.81 N to 2450 N or 49 N to
7350 N.
2
Durationof test loadapplicationins 25
Test loadidentifying value 100
Abbreviationfor Vickers hardness HV
MeasuredVickers hardness value 780
Figure 21.6 shows the ideal indentation a and possible undesirable indentations
withsink-inb, pile-upc formationandkite shape d.
For high-test forces, determination of Vickers hardness is independent of the test
force. However, for test forces P5N the calculated Vickers hardness becomes test
force dependent. This phenomenonis knownas IndentationSize Effect ISE. Its inu-
ence is particularly disruptive in microhardness testing, where HV values that have
been measured for the same specimen with differing test forces are no longer compa-
rable. The cause can be tension induced when the Vickers pyramid is imposed or sur-
faces that have stabilized dissimilarly during metallographic/materialographic prepa-
ration.
For this reason, hardness value classicationis dividedintotest ranges.
Following the ASTMStandardTest Methodfor Vickers Hardness of Metallic Mate-
rials E92, Vickers Hardness Tests are performedwithtest forces of from1 to 120 kgf.
The ASTM Standard Test Method for Microindentation Hardness of Materials E
384 species a test force range of 11000 gf for microindentationhardness testing with
Vickers indenters see Section21.5.
At Vickers hardness testing E 92 the distance between the center of the indenta-
tion and the specimen edge and between the center of two indentations should be
2.5d. When laminated material is tested, a bond surface shall be considered as an
edge for spacing of indentationcalculations.
Inhardness testing of small parts, thinsheets, layers or foils, low-test forces should
be usedto avoidthe so-calledanvil effect. The anvil effect is causedby use of a test force
Fig. 21.5Vickers hardness testing, test principle ASTM Standard E 92.
that is too high when testing a thin specimen, resulting in a bulge or shiny spot on the
underside of the specimen. Also a force that is too highmay cause edge effects, a plastic
deformation in the direction towards the edge. For this reason an indentation shall be
in a certain distance to the edge as mentioned above. The use of low-test forces also
applies tothe determinationof hardness of individual structural constituents.
As the test force or indentation size, or both, decrease, the inuence of the speci-
men surface increases. A carefully smoothed and cleaned surface is sufcient when
macro testing, but when micro testing, the specimen must be metallographically/
materialographically prepared to remove any disruptive roughness or solidied sur-
face layers. If smoothing and polishing are insufcient, the surface can be electrolyti-
cally or chemically treated to have access to mechanically undisrupted areas. If
individual structural constituents are to be tested, additional phase contrasting, for ex-
ample by means of etching, is necessary.
21.2.2 Vickers Hardness Tester
The hardness tester showninFig. 21.4 caneasily be convertedfor use inVickers macro-
hardness measurements. The indenter is exchanged and the appropriate test force in-
crements selected. Measurement takes place onthe screenor automatically.
Depending on the producer, the machines differ in various ways. For example, the
test force may be produced mechanically or hydraulically in different increments, the
test method may be more or less automated and special testing needs may be met by
means of additional equipment.
Fig. 21.6Vickers indentation shapes. Ideal indentation a, indentation with sink-in b,
indentation with pile-up c, and kite-shaped indentation d.
21.3 Knoop Hardness Testing
Special machines were developed for lowload, microindentation hardness, and ultra-
microindentation hardness testing in order to further decrease potentially disruptive
device-relatedinuences andbetter measure very small indentations. Essentially, how-
ever, the testing procedure corresponds tothat of macrohardness testing.
In 1932, Knoop, Emerson, and Peters introduced a method developed specically
for low load and microindentation hardness testing. In Knoop hardness testing, a
rhombic-based pyramidal-shaped diamond indenter with edge angles of 172 30 A
and 130 B is used. In Fig. 21.7, the pyramidal-shaped diamond is shown with the
two angles and the long diagonal, d m. As in the Vickers method, this pyramid is
pressed vertically into the specimen surface. Knoop hardness in kgf/ mm
2
is calculated
by means of the long indentation diagonal d in m, which is 7.114 times longer than
the short diagonal of the Knoopindentation.
The following equationapplies:
HK= 14.229P
1
/d
1
2
6
where
HK=Knoophardness inkgf/ mm
2
P
1
=test force inkgf
d
1
=long indentationdiagonal inmm
Knoophardness inGPa units is determinedas follows:
HK= 0.014229 P
2
/d
2
2
7
where
P
2
=test force inN
d
2
=long indentationdiagonal inmm
650HK0.5/ 30
Fig. 21.7Knoop diamond pyramid and indentation ASTM Standard E 384.
Duration of test force application in seconds; not recorded if
between10and15 s 30
Test force identifying value: 0.102F F inN 0,5
Abbreviationfor Knoophardness HK
MeasuredKnoophardness value 650
Knoop hardness measurements are primarily taken using hardness testers devel-
oped for low load and microindentation hardness testing. In such machines, the load
system is changed accordingly and adjusted for small test forces. The screen onto
whichthe indentationis projectedis exchangedfor a measuring ocular.
Due to the measurement length that is greater than that of a comparable Vickers
indentation, measurement error is smaller in the Knoop method. Therefore, even very
thin layers or foils can be tested better. The Knoop method is also advantageous with
brittle materials, as cracks formmore easily arounda Vickers indentation.
The Knoop indenter does not produce a geometrically similar indentation as a
functionof test force. Consequently, the Knoophardness will vary withtest force.
Due to the elongated shape of the Knoop diamond, any anisotropy that may exist
inindividual structural constituents canbe ascertained. Whenthis is the case, different
measurements of the crystallite are taken and the specimen is appropriately rotated
before every newmeasurement.
Knoop hardness testing is described in ASTM Standard Test Method E 384 see
Section21.5.
21.4 Rockwell Hardness Testing
Due to a number of disadvantages of the Brinell hardness test and the limitations re-
garding testing of steels with high hardness, Stanley P. Rockwell developed a hardness
testing method in 1919. In this method, the hardness of a material is determined by
means of measured indentation depth. A diamond indenter is used for Rockwell Csee
Fig. 21.8 or a tungsten carbide/steel ball is used for Rockwell B. In Fig. 21.8 the follow-
ing symbols anddesignations are used:
1: Angle of the top of the diamond indenter 120; 2: Radius of the curvature at the
tip of the cone 0.200 mm; 3: P
0
, Preliminary test force; 4: P
1
, Additional force; 5: P,
Total test force P
0
+P
1
; 6: Depth of penetration under preliminary test force; 7: In-
crease indepthunder additional force; 8: e, Permanent increase indepthof penetration
under preliminary test force after removal of additional force, the increase being ex-
pressedinunits of 0.002 mm; 9: xxHRC, Rockwell Chardness=100e.
It can be seen that the indenter is rst pressed a small distance into the material; in
this way the inuence of the specimensurface canbe excluded.
Rockwell hardness value is calculated by means of a process internal to the ma-
chine withthe helpof a scale divisionfactor S anda numerical value N.
The simple equationfor determining Rockwell hardness is:
HR= N e/S 8
where
HR=Rockwell hardness
N=Numerical value tiedtoS
e=Remaining indentationdepthinmm
S=Scale divisioninmm
The standard indenters are a diamond cone with 120 apical angles and tungsten
carbide balls withdiameters of 1.588, 3.175, 6.350, and12.70 mm.
The preliminary test force for the Rockwell Standard Method is 98 N 10 kgf; the
possible total force is 589 N60 kgf, 981 N100 kgf, 1471N150 kgf.
For the Rockwell Supercial Hardness test, the preliminary force is 29 N 3 kgf
andthe possible total force is 147 N15 kgf, 294 N30 kgf and441N45 kgf.
Corresponding scales are available for different applicationpurposes andmaterial
groups see Table 21.2.
Lower test forces are used in Rockwell Supercial Hardness Testing. The prelimi-
nary test force is 29 Nandthe total test force canbe 147 N, 294 N, and441 N.
Rockwell scales Bfor the steel ball of 1.588 mmdiameter and Cfor the diamond
cone are the most frequently used. As in Brinell hardness testing, however, it must be
noted that deformation of the ball can occur in very hard materials with HRB. There-
fore, use of the Bsteel ball for materials harder than100HRBis not recommended.
The test object should lie solidly on the support table anvil so that it cannot slip
during the test method. Care must be taken to select the correct indenter and force
when working with thin specimens so that the hardness value of the specimen is not
falsied due to the inuence of the support table, the so-called anvil effect. Specimen
thickness should be 15 times the depth of indentation when using a ball indenter and
10 times the depth of indentation with a diamond cone. As a rule, no deformation
shouldbe visible onthe backof the workpiece after the test.
Indentations should be made at a distance of at least 2.5 times the indentation di-
ameter fromthe specimenedge. The distance betweenadjacent indentations shouldbe
three times the indentationdiameter.
The preliminary test force F should be produced within 3 s. The usual duration of
stress by the additional force is 18 s.
Further information about the method can be found in ASTM Standard Test
MethodE18.
Fig. 21.8Rockwell C hardness test with diamond indenter, test principle, see text ASTM
Standard E 18.
Designation of Rockwell hardness is made by supplying the hardness value fol-
lowed by the abbreviation HRfor Rockwell hardness and the scale symbol. This gives
information about the indenter and the force. For example, 80 HRC means a Rockwell
hardness value of 80onthe Cscale using the diamondcone as indenter.
21.4.2 Rockwell Hardness Testers
Figure 21.9 shows a basic Rockwell hardness testing machine. The testing procedure
differs in two signicant ways from the Brinell and Vickers methods described previ-
ously. First, with the help of a hand wheel, the specimen is pressed against the indenter
until the meter indicates the desired preliminary force F
0
. Then, the additional force F
1
is applied for the specied length of time. A further difference lies in the fact that the
Rockwell hardness value HR can be read fromthe meter immediately after withdraw-
ing the major force.
The signicant advantages of Rockwell hardness testing compared to the Vickers
andBrinell procedures include the simpler machine constructionwithout optical mea-
suring equipment, the direct readability of the hardness values, and the less stringent
quality requirements for the specimensurface.
For these reasons, the Rockwell methodwas quickly adoptedandis usedprimarily
for simple andfast quality control inproduction.
21.5 Microindentation Hardness
21.5.1 Methods
Measuring methods andmachines must be appropriately adaptedtoperformhardness
measurements on very small objects, thin layers, surface-treated materials, or indi-
vidual structural constituents.
TABLE 21.2Rockwell Scales and Test Conditions for Various Groups of Materials.
Scale Symbol Indenter (Diam.) Total Test Force kgf Application Example
B Steel 1.588 mm 100 Moderately hard, soft steels; brass, bronze, Al
alloys
C Diamond 150 Hardened, tempered steel; hard casting,
materials harder than HRB 100
A Diamond 60 Sintered carbides as well as HRC with low
specimen thickness
D Diamond 100 Thin steel sheets, case-hardened layers
E Steel 3.175 mm 100 Cast iron, Al and Mg alloys, bearing metals
F Steel 1.588 mm 60 Thin, soft steel sheets, annealed copper alloys
G Steel 1.588 mm 150 Copper-nickel-zinc, hard bronzes
H Steel 3.175 mm 60 Aluminum, zinc, lead
K Steel 3.175 mm 150
L Steel 6.350 mm 60
M Steel 6.350 mm 100 Soft bearing metals and thin specimens, very
small balls and heaviest load that does not
give an anvil effect
P Steel 6.350 mm 150
R Steel 12.70 mm 60
S Steel 12.70 mm 100
V Steel 12.70 mm 150
Microindentation hardness, also often called microhardness, means the determi-
nation of hardness values with lowtest forces. Compared to the macrohardness testing
methods described previously, the test force range in microhardness testing is very
small. Following the ASTM Standard Test Method for Microindentation Hardness of
Materials E 384 the range is between 1 and 1000 gf 9.810
3
and 9.8 N, and the
indentations are correspondingly small.
Inpractice, the geometric forms of the Vickers andKnoopdiamondindenters have
proved successful. In addition, the Berkovich diamond indenter must be mentioned.
This is a regular three-sidedpyramidwithanangle of 142 betweenthe lateral edge and
the opposite lateral face. The indentation surface is an equilateral triangle; the lengths
of its sides are measured.
The hardness value that has already been described, is in any case ascertained by
dividing the test force by the remaining indentationsurface.
It is especially important to monitor the loading system regularly, since the hard-
ness error percentage is directly proportional to force error. The total force should be
applied within 10 s, while the duration of the force can range from 10 to 15 s. For
steels, 10 s are sufcient. If longer load times are necessary for softer materials, this
must be indicatedinthe test protocol.
Vibrations andshaking of the machine must be avoidedduring measurement.
To achieve precise measurement values, the polished and cleaned specimen surface
should be set up perpendicularly to the direction of indentation. This is the only way to
achieve clearly dened indentations that can be evaluated to a microscopically exact
degree. The smaller the test force and the indentation, the greater the inuence of
specimenpreparation. For example, excessive polishing cancause coldwork of the sur-
face material see Part II, Section 13.16. Whenever possible, the surface should not be
Fig. 21.9Rockwell hardness tester.
2
etched since the indentation otherwise becomes uneven due to the attacked surface
andmay be difcult tomeasure.
See Part II, Table 11.1 andChapter 13.2.3 for informationregarding suitable speci-
men preparation. Small unevenly shaped specimens must be mounted or fastened into
specimen holders. It is important to ensure that the specimen cannot move under the
effects of the force.
21.5.3 Taking the Measurements
The microindentation hardness measurement method takes place in the following
way:
Turnonlighting systemandthe calibratedhardness tester
Select, carefully cleanandapply anindenter
Set or fastenspecimenmaterial ontable surface
Focus a low-enlargement lens onthe specimensurface
Select indentationarea, adjust contrast andresolutiontooptimal values
Remove lens fromandmove indenter intothe operating position
Select force
Activate test, adhere tospeciedforce times
After withdrawing the force, disengage indenter and move lens into measuring
mode
Checkindentationfor desiredpositionandsymmetry
Evaluate
Nonsymmetrical indentations canbe causedby the following:
Indenter does not penetrate specimensurface perpendicularly
Specimensurface is not level
Material is textured
Anisotropy of structural constituents
Because microindentation hardness values are strongly inuenced by different
components and their size and distribution in the material, it is advisable, depending
onthe task at hand, to make several indentations under otherwise identical conditions.
The distance between two Knoop indentations shall lengthwise be 1.5 d length of
Knoop diagonal, side by side be 4 w width of Knoop diagonal and the distance to
the edge of the specimen shall be 3w. The distance between the center of two Vickers
indentations shall be 4 d length of Vickers diagonal, and the distance to the edge of
the specimenshall be 2d.
In ceramics or other brittle substances, the indentation can cause cracks. The
ASTM Test Method for Knoop Hardness for Advanced Ceramics C 1326 and the
ASTM Test Method for Vickers Hardness for Advanced Ceramics C 1327 address
more closely the considerationof suchspecial circumstances.
When test forces and indentations are so small, high demands are placed on the
indenter in terms of precision, particularly where the four faces meet. For the Knoop
indenter the line of junction between opposite faces offset shall be not more than
1 m in length for indentations greater than 20 m in length, as shown in Fig. 21.7.
For Vickers indenters the offset shall be not more than 0.5 m. Formation of an offset
betweenthe faces cannot occur withthe Berkovichindenter, as it has only three faces.
Indenters should be examined periodically and replaced if they become worn,
dulled, chipped, cracked, or separatedfromthe mounting material.
21.5.4 Microindentation Hardness Testers
Figure 21.10 shows a modern microhardness tester. With this machine, Vickers,
Knoop, Berkovich, and Brinell testing procedures canbe carried out withadherence to
the most recent ISO and ASTM standards. Machines of this kind operate completely
automatically withmotorized lens carousel and autofocus motorized z-axis. The load
production and the load changes among nine increments from98.07 mN to 19.61 N
take place automatically when the duration of load application is between 5 and 999 s.
With the help of a video camera and appropriate measuring and controlling software,
the image of the indentation surface can be transferred to a PC and evaluated there.
Serial measurements are possible in addition to individual tests. Measurement values
can be statistically evaluated maximum, minimum, mean values, standard deviation,
histogram. Conversionof hardness values HR, HB, MPa, etc. occurs automatically.
21.5.5 Examples of Indentations
Figure 21.11 gives four examples of indentations. In Fig. 21.11 a shows three indenta-
tions indifferential interference contrast DIC; b shows Vickers indentations insteel,
indicating the softer ferrite and the harder pearlite; c shows the hardness progression
in case hardened steel; and d the indentation is in a ceramic material, Si
3
N
4
. The
brittle material causes cracks at the corners of the indentation.
21.6 Universal HardnessMartens HardnessInstrumented
Indentation TestingNano Indentation
The extent of elastic and plastic deformation varies greatly among technical materials.
In rubber, for example, elasticity predominates, and the indentation regresses almost
completely when the load is removed, whereas in materials like lead the hardness in-
dentation is retained. The hardness values of the two materials can therefore not be
comparedtoeachother.
Comparison is possible when the Universal hardness, HU, is calculated. In this
procedure that has been known since 1940, the Vickers hardness is measured under
force. The Universal hardness is calculated from the maximal test force P
max
and the
indentation depth h
max
. Universal hardness is now known as Martens hardness, HM
see below.
Fig. 21.10Microhardness testing machine.
3
By means of this procedure, hardness values from all material types can be com-
pared on one scale, which is a great advantage, particularly for industrial purposes.
The Vickers procedures visual evaluation of the indentation, along with its possibility
of error, is hereby eliminated. The indentation depth is recorded by measuring tech-
niques that make possible the automationof the procedure.
Additional valuable quantitative information about a materials elastic and plastic
behavior can be extracted from load-indentation depth curves, Fig. 21.12, that are a
schematic representation of the test force indentation-load, F, versus depth of inden-
tation displacement, h. The diagram shows that the depth of indentation displace-
ment increases with increasing load. At unloading only the elastic portion of the dis-
placement is recovered, which allows for separation of the elastic properties of the
material fromthe plastic properties. Based on the maximumdepth, h
max
and the maxi-
mumload, F
max
, the Martens hardness, HM, previously Universal hardness, can be de-
ned see below. It is also possible from Fig. 21.12 to calculate the elastic modulus
Youngs modulus basedonthe slope of the unloading curve.
Fig. 21.11Examples of Vickers and Knoop indentations. Three Vickers indentations in DIC,
220X a, indentations in steel indicating ferrite and pearlite, BF 500X b, progression of
hardness in a case hardened steel, BF, 100X c, and a Vickers indentation in silicon nitride with
cracks at the corners, DIC, 200X d.
21.6.1 Instrumented Indentation TestingNano Indentation
In classical light-optical microhardness testing, even when using automatic machines
with high-grade optical measurement systems, a Vickers or Knoop diagonal length is
recordable to at most 23 m. This is due to the limited resolution capability. When
working with microcrystalline materials and extremely thin layers, however, hardness
indentations of substantially smaller indentation size are required. This is achieved by
using the testing principle, Instrumented Indentation Testing IIT, also called nano
indentation. IITis usedfor determinationof Martens hardness, HM, Indentationhard-
ness, H
IT
, and Indentation modulus, E
IT
. The indentation depth h is measured and
used to calculate the hardness value. In this way, indentation depths to 0.1 nm can be
recordedandevaluatedinadherence tointernational standards see below.
Martens Hardness Scale: The Martens hardness value is calculated by dividing the
test force F by the surface area of the indenter penetrating beyond the original surface
of the test piece A
s
h.
For Vickers indenter:
HM= F/A
s
h = F/26.43h
2
9
For Berkovichindenter:
HM= F/A
s
h = F/26.44h
2
10
Indentation Hardness Scale: The indentation hardness H
IT
is calculated from the
test force, F, divided by the projected area of the indenter in contact with the test piece
at maximumload:
H
IT
= F/Ah
c
11
where the projected contact area Ah
c
is calculated from knowledge of the geometry of
the indenter andthe stiffness of the contact.
During the indentation the force-trajectory progression can be recorded that gives
signicantly more information about elastic-plastic behavior than does a classical in-
dentation for which the size is evaluated. In this way, hardness, elasticity, or viscoelas-
Fig. 21.12Schematic representation of indentation forcedepth of indentation displace-
ment data during one complete cycle of loading and unloading.
tic properties of paint, varnish, or synthetic layers, galvanized layers, carbide layers of
TiN or TiC, diamond and anodized layers as well as bers and foils can be determined
andcompared. Also, the hardness andelastic modulus of a single grainina microstruc-
ture can be measured. Fully automated measurement and evaluation ensure high re-
producibility andprevent subjective error.
Instruments for IIT work with test forces down to 1 nN and indentation depths
displacement down to 0.1 nm. HM can be measured with Vickers and Berkovich in-
denters. For measurements in the nano range the Berkovich indenter, having only
three faces see Section 21.5.3 is preferred, but other geometries like sphero-conical
indenters are alsoused.
Instrumented Indentation Testing is described in ASTM Work Item, Practice for
InstrumentedIndentationTesting WK382 andinthe StandardISO14577.
21.7 Precision of Hardness Values
The hardness testing procedure takes place in two steps: The production of the hard-
ness indentation and its measurement. The measurement value that is obtained in the
presence of known standard testing machine and specimen conditions is inuenced by
the geometric precision of the indentation specimen and by penetration direction, test
force, test time, penetration speed, and temperature. This can lead to constant or vari-
able errors.
For this reason the testing machine shall be veried. The direct verication of the
hardness tester includes the inspection of the force application, the indenters, and the
measuring device at regular intervals. If the test force or the indenter is changed, a new
vericationmust be performed.
Indirect verication takes place by making a series of at least ve test impressions
on a standardized hardness test block. The closer the mean values of the test impres-
sions are to the hardness of the test block, the more exact the hardness tester functions.
The difference in hardness values around a mean value may be an indication of the
precisionof the hardness tester: The less difference the higher precision.
A verication report often should be worked out after the verication. The test re-
port should contain the following information: Reference to the ASTM test method.
Method of verication. Identication of the hardness testing machine. Means of veri-
cation. Type of indenter and test force. The result obtained. Date of verication and
reference to the calibration institution. Identity of the person performing the verica-
tion.
For specication regarding the single hardness testing method, see the relevant
ASTMstandardstatedinSection20.2.
21.8 Conversion of Hardness Values
The conversion back and forth among Brinell, Vickers, or Rockwell hardness values is
possible withthe helpof conversiontables see below. The conversionvalues are solely
empirical innature.
Incertaincases the following equations canbe used; these shouldbe consideredas
rules of thumb, not as exact as the equations stated in the conversion tables mentioned
below.
Simple Hardness ConversionEquations:
FromHBtoHV: HB0.95HV
FromHRBtoHB: HRB1761165/
HB
FromHRCtoHV: HRC1161500/
HV
FromHVtoHK: HVHKinlowloadrange
Procedural informationcanbe foundinthe ASTMStandardHardness Conversion
Tables for Metals RelationshipbetweenBrinell Hardness, Vickers Hardness, Rockwell
Hardness, Rockwell Supercial Hardness, Knoop Hardness, and Scleroscope Hard-
ness E140. Please refer toASTME140inthe CD-ROMincludedwiththis manual.
Values that have been estimated using the equations given above or taken fromthe
conversiontables shouldbe indicated, stating the original hardness value.
22
Dynamic Hardness Testing
Procedures
IN DYNAMIC HARDNESS TESTING PROCEDURES, THE INDENTER HITS
the specimen surface with impact. The specimen material can thereby be elastically
and unelastically deformed. Deformation that arises due to the kinetic energy of the
indenter and remains can be measured. In such dynamic-plastic procedures, the hard-
ness value is the quotient of the test force and the indentation size. We distinguish be-
tweenfall hardness testing andimpact hardness testing see Fig. 22.1.
In the fall hardness testing method a, an object of dened mass falls freely onto
the specimen along with the indenter ball and creates an indentation. In the impact
hardness testing method b, the ball rests on the specimen surface. Triggered by a
hammer blow or by spring force, an object of known mass is thrust onto the indenter,
whichthenpenetrates the specimen.
One such instrument is the Poldi impact hardness tester, Poldi hammer for short.
The indenter is pressed, by means of a hammer blow, simultaneously intothe specimen
and into a comparison rod of known Brinell hardness. The HBP hardness can then be
determinedby comparison.
With the Baumann hammer, the indenter is driven into the specimen surface by
means of spring force. The indentation is measured and assigned a corresponding
Brinell hardness value.
Fig. 22.1Principles of dynamic hardness testing procedures, schematic. Rebound with drop
a, and rebound with spring loaded hammer and ball placed on the work piece b.
644
In dynamic-elastic hardness test procedures, the rebound height, or rebound
angle is measured see Fig. 22.2. In materials with lowdeformation potential, such as
tungsten carbide or rubber, the indenter, which hits the specimen surface at a dened
velocity, springs back. We can infer a hardness value from the rebound height that is
proportional to the rebound energy. Such dynamic-elastic procedures also include the
Shore hardness testing methodandthe Equotipmethod.
The Scleroscope functions according to the drop hammer principle. The indenter
is either a roundeddiamondpoint of a particular size andshape or a steel ball that rests
on a drop hammer. This falls through a pipe vertically onto the specimen and rebounds
again up to a particular height Fig. 22.2a. This rebound height is a measure of hard-
ness that is given in Shore hardness values. In the Model C Scleroscope, a high-
precision, low-friction glass pipe is used. The rebound height can be recorded on a
scale of 0140, and the hardness can be read in HSc. In the Model D Scleroscope, the
hammer is automatically detained after reaching the rebound height, and height and
hardness are then recorded using technical measuring instruments. Since the hammer
is larger and heavier compared to the one used for the Model C, the fall height can be
reduced without changing the impact energy. The hardness values are given in HSd.
Depending on the machine model, application, and test material, various indenters
and scales are used. More exact guidelines are found in the ASTMStandard Practice E
448.
The Equotip tester functions according to the drop hammer principle. A carbide
ball 3 mm in diameter is used as indenter. After the release of a preloaded spring, the
indenter is thrust against the test specimen. Impact andreboundvelocity of the ball are
electronically measured at a distance of 1 mm above the test surface. From the rela-
tionship between these two velocities we can ascertain an L hardness value named
after D. Leeb, the machines inventor. Hardness measurements of upto approximately
1200 HVcanbe calculatedwiththis method.
The advantages of the portable machines described above include their suitability
for use onslantedsurfaces andthe short durationonly a fewseconds of the test proce-
dure. The disadvantage is that these methods do not supply the hardness values with
the same highprecisionas the static hardness testers.
Fig. 22.2Types of rebound hardness testers, schematic. Hardness value based on height of
rebound a, and hardness value based on rebound angle b.
Chapter 22 Dynamic Hardness 645
23
Special Methods for Hardness
Testing
SPECIAL HARDNESS TESTING PROCEDURES INCLUDE THE MARTENS
scratch hardness determination as well as the Mohs scratch hardness. In the Martens
procedure, a specimen surface under a specied test force is scratched by a diamond
cone witha 90-deg apical angle. The test force Fis varieduntil a scratchwidthof 10 m
is microscopically measured. In this way, a particular scratch hardness value can be
attributedtothe specimen.
There are continuous test procedures that allowus to record hardness progression
curves for case-hardened or nitrided steels. In these, the width of the scratch that ap-
pears is evaluated, at a constant test force, in light of the scratch length. Or, the force
trajectory-dependent indentation process may be recorded by means of technical mea-
surement instruments, much as is done in instrumented indentation testing see Sec-
tion21.6.1.
References Part V
1 Courtesy of Deutscher Verlag fr Grundstofndustrie.
2 Courtesy of Emco-Test PrfmaschinenGmbH.
3 Courtesy of Struers A/S.
646
Part VI:
The Metallographic/Materialographic
Laboratory
24
Introduction
24.1 Establishing a Metallographic/Materialographic Laboratory
WHEN ESTABLISHING A METALLOGRAPHIC/MATERIALOGRAPHIC LABO-
ratory, many conditions have to be taken into consideration. The two main conditions
are: 1What is the purpose of the metallographic/materialographic examination? Is it
quality control, research, education, etc.?; 2 What is the specimen volume; few or
many specimens per day?
Another important condition is the degree of automation of the preparation pro-
cess. This really depends on the volume of specimens to be prepared and the size of the
specimens, as well as the specimen quality reproducibility. The occupational situa-
tion for the persons performing the preparation should also be taken into consider-
ation.
Chapter 25 discusses the above-mentioned conditions and other important mat-
ters connected to planning for and establishing a metallographic/materialographic
lab, and suggestions for a number of laboratories suited for different purposes and ca-
pacities will be given.
24.2 Running a Metallographic/Materialographic Laboratory
The metallographic/materialographic laboratory should be considered a production
unit, producing specimens of the desired quality at the lowest price. This means that
correct planning must be made, covering boththe day-to-day operationand preventive
maintenance.
24.3 Occupational Safety and Health
The work in the laboratory involving machines, chemicals, etc., makes it imperative
that all relevant rules and regulations covering occupational safety are followed. This
subject is describedinChapter 26.
649
25
How to Build a Metallographic/
A LABORATORY IS SELDOMBUILT FROMSCRATCH. ANEXISTINGLABORA-
tory should usually be changed, possibly moved to other locations, etc. In all these
cases it is very useful to analyze a number of factors regarding the laboratory so that
the right changes, gradually, canbe made.
25.1 Purpose
The purpose of the laboratory as part of a larger organization should be considered.
The purpose may be quality inspection of parts from a running production, meaning
that the preparation with examination result should be nished in a short time, or a
research lab with large test series that can be prepared at a steady speed with ample
time available.
Three purposes together with the capacity, number of specimens to prepare per
week, shouldbe discussedhere.
25.1.1 Quality Control QC
The laboratory performing quality inspection ranges from the relatively small sub-
supplier, who prepares a fewspecimens per week, to the large lab with several hundred
specimens per week.
In both cases, the specimen size and the materials to be prepared are known and
often of a limited number. This means that xed documented procedures can be estab-
lished. This ensures the reproducibility that is very important if the analysis over a pe-
riodof time shall provide a true picture of the product quality.
Although a smaller lab with fewspecimens per week could prepare the specimens
by handandstill be rational, the preparationshouldbe performedwitha small semiau-
tomatic grinder/polisher to secure the reproducibility. This also makes it possible to
use a rather untrainedpersonfor the preparation, whichcanbe of advantage, whenthe
specimenvolume is low, andit is not possible tohave a full-time persononthe job.
A lab with higher volume will use semiautomatic or fully automatic equipment to
have rational specimen production, at the same time securing reproducibility and a
programmedprocess.
The cost per specimen is important see Section25.2.2.
If preparation time is important, electrolytic polishing should be considered if the
materials are suitedfor this see Chapter 8.
AQClab often will have the advantage of digital imaging connected to a systemfor
registration, connecting the metallographic/materialographic analysis with other tests
like hardness, etc. see Chapter 19.
If a QC lab also makes failure analysis, this might indicate other types of equip-
ment see below.
650
25.1.2 Research and Education
Research
Like the QC lab, the research lab needs a high reproducibility to secure correct inter-
pretation of the materials being developed. For this reason, semiautomatic equipment
should be used. This equipment should have a reasonable capacity, but the production
of specimens can usually be planned for and high-production equipment is not
needed.
For research, typically a wide spectrum of materials should be prepared and the
equipment should preferably be for mechanical preparation. Electrolytic polishing
and thinning TEM could be interesting also, electrolytic polishing resulting in
deformation-free specimens see Chapter 8.
Education
As part of education in physical metallurgy, the students often have to prepare one or
more materials, both to experience the metallographic/materialographic process and
tobe able tosee a preparedmicrostructure ina microscope withtheir owneyes.
A group of students usually works with specimen preparation at the same time,
and this can be done on a number of small grinder/polishers, either by hand or with a
simple semiautomatic specimenmover.
Education is often connected to a research lab, but equipment used for research
shouldnot be usedby the students for educational purposes.
25.1.3 Testing and Inspection LaboratoriesFailure Analysis
Laboratories established for preparation of specimens for customers should be able to
prepare all materials for a wide number of examinations. The job may be just one
specimen representing a failure, a special case archaeology, forensic, or a series of
specimens. For this reason, equipment for both mechanical preparation and electro-
lytic polishing should be available, high productivity playing a minor role, with the
possibility of preparing all difcult materials playing a major role. Preparation of
specimens for failure analysis is often difcult because the specimen is not regular,
but has to be taken froma work piece at a special location, and the area to be prepared
is oftendifcult to establish. Incertaincases handpreparationis preferred, but inmost
cases the specimen can be mounted so that a semiautomatic grinder/polisher can be
used. Therefore, even large laboratories with advanced automatic equipment, some-
times engaged in failure analysis, need a small semiautomatic machine for single
specimens.
25.2 Rationalization and Automation
The demand for more cost-efcient processes and procedures has been increasing in
all parts of the society for a long time. In the metallographic/materialographic lab, the
focus is oncost per specimen, including all the costs covering manpower, equipment,
consumables, locations, administration, energy consumption, etc.
Examples are changes in the production, the organization, or the requirements to
documentation. As a result, the lab has to produce more specimens without increasing
the personnel, or the quality of the specimens should be improved because an auto-
Chapter 25 How to Build 651
matic image analyzer has beeninstalled. Improvements inquality have tobe made very
oftenwithout a similar increase tothe budget.
The demand for a higher specimen quality and a better reproducibility is also in-
creasing because of quality standards like ISO9000andIS9000.
Rationalizationcanoftenbe made inall steps fromthe work piece/specimenarriv-
ing in the lab to the nished report leaving the lab. This can be in specimen handling,
choice of equipment, preparation procedures, and administrative routines, including
writing of reports and ling the micrographs. At the same time the occupational safety
canvery oftenbe improved.
Automation according to the state-of-the-art is limited to the preparation pro-
cess fromplane grinding to the nished specimen and to the automatic printing of mi-
crophotographs through digital systems see below. In case of image analysis, this can
alsobe automatic see Part IV.
25.2.1 ReproducibilityStandardsOccupational Safety
Basically the only assurance that a microstructure is true depends on the evaluation
done by the person who is interpreting the structure. In most technical matters, the
result can be measured and the correctness be veried, but this is not possible with a
microstructure. A high element of subjectivity is present when it should be decided
whether a microstructure is true. It is very possible, of course, to measure the struc-
ture using image analysis, but whether the microstructure being measured is the true
structure representing the work piece material, or not, is based on the evaluation of an
experiencedperson.
For this reason, it is very important that methods are developed, documented, and
followed when making a preparation. A proven method guaranteeing the true struc-
ture, executed on a machine with constant parameters and uniform consumables,
makes it possible with a high certainty to say that a running production of specimens
is correct. As soon as human treatment is involved, the risk of an incorrect result will
increase.
In modern quality control QC, according to standards like ISO9000 and IS 9000,
the correct measurement of all results is very important. Therefore, in the case of
metallography/materialography, the microscope should be calibrated regularly to en-
sure that the analysis is correct. It is very difcult, however, to give correct measuring
data for the preparation process, securing a correct preparation, as mentioned above.
Therefore, the responsibility of the correct structure is transferred to the skilled person
evaluating the microstructure, and to support this, a documented procedure using
semiautomatic or automatic preparationequipment shouldbe workedout.
In a number of ASTMstandards, such as Standard Test Methods for Determining
Average Grain Size Using Semiautomatic and Automatic Image Analysis E 1382, the
preparation is part of the standard, spelling out that the true structure must be avail-
able at a high reproducibility. In most cases, however, the methods for a given material
must be workedout inthe laboratory see Section13.2.3.
Occupational safety and health play an increasing role, both regarding the physi-
cal work done by the operator and the total laboratory environment see Chapter 26.
Using semiautomatic or fully automatic equipment for cutting-off, mounting, and
preparation will reduce the amount of physical power needed and, when possible, the
equipment canbe connectedtoanexhaust systemtoavoidcontaminating the air.
25.2.2 ProductivityCost Per Specimen
Essentially the preparation of a specimen can be seen as a production as any other
item made in a production facility. This means that preparation should be constantly
analyzedaccording tothe following demands:
Increasedproductivity
Improvedquality
Cost reduction
The increase in productivity can be obtained by analyzing the whole preparation
process andcalculating the cost per specimensee below.
Improved quality can often be achieved by using semiautomatic or automatic
equipment. This also usually provides increased productivity. Cost reduction can often
be obtained by reducing the cost per specimen, but other factors should also be ana-
lyzed to give the most cost-efcient function of the total metallographic/material-
ographic lab.
The following shouldbe takenintoconsideration:
Development of the correct application for each material: It is very important that
the optimumprocess is found for a given material. One or more preparation steps can
oftenbe omittedor times canbe reduced.
Training of Personnel: The persons responsible for the preparation should be
trainedtooptimize the use of equipment andconsumables.
Service: The equipment should be serviced regularly preventive servicing to
avoid breakdowns. If breakdowns happen, a service support should be available from
the supplier, keeping the downtime short.
Cost per Specimen
A cost-savings analysis must be made to decide on the present cost per specimen and a
possible lower cost per specimen.
The analysis is supposedtoshowall costs involvedinmaking a specimen.
Operator costs
Consumable costs
Depreciationof equipment
The rst stepinthe analysis is todecide onthe actual costs.
Operator costs are calculated for the total operator time used per specimen from
receiving the work piece specimen through to a prepared specimen that is ready for
the microscope. Consumable costs are calculated by listing all consumables used for
eachpreparationstepandcalculating the amount usedper step.
For the equipment, the service costs and depreciation costs are calculated, the lat-
ter based on the total investment in equipment, time of depreciation, and the interest
rate.
The cost per specimen will usually be lower when using more automatic prepara-
tion equipment, and often depends on the number of specimens made per day. In Fig.
25.1, two curves are shown indicating the cost per specimen for a highly automated
machine Equipment 1 and a relatively simple piece of equipment Equipment 2. It
canbe seenthat around55 specimens per day, the price per specimenis lower using the
expensive machinery.
The Payback Time is interesting too. This indicates the time for howlong the new
equipment should operate before the savings are so high that the investment is paid
back. Figure 25.2 shows an example of Equipment 1 mentioned earlier. The Payback
Time shows that the expensive automatic equipment Equipment 1 is paid back in
one year whenapproximately 38specimens are preparedper day.
Additionally, the advantage of having a higher certainty for correctly prepared
specimens should be taken into consideration also, supporting the procurement of au-
tomatic equipment.
25.3 Planning the Metallographic/Materialographic Laboratory
25.3.1 Basic Planning
The metallographic/materialographic lab, like all other investments, should be subject
to a total cost-benet analysis. It is, however, not as easy to calculate as the more
straightforward processes like a production facility. The lab is a mixture of production
specimen preparation, analysis, reporting, and other administrative work, often with
a highvariationinthe workload.
The metallographic/materialographic lab is established like any other lab, but a
number of specic features shouldbe evaluated.
The lab should be split into several rooms, the basic parts including a room for
cutting, a roomfor preparation, anda microscope room.
Fig. 25.1Cost per specimen. Comparison between preparation with a highly automated
machine Equipment 1 and a relatively simple piece of equipment Equipment 2.
Fig. 25.2Payback time. Payback time in years in relation to number of specimens per day for
Equipment 1 in Fig. 25.1.
A good workowshould be secured. Considering the number of apparatus, the in-
stallation of electric power both 1-phase and 3-phase, compressed air, water drains,
and ventilationshould be made exible and easy to maintainThe oor load should also
be takenintoconsideration.
Because of the relatively large machines usedinmaterialographic preparation, the
passages and doors need to be wide enough so that machines up to 1.3 m 4.3 ft can
pass through.
A persons workplace in the lab should have the best possible lighting daylight,
lownoise level, andcorrectly placedfume hoods.
A 2025 % spare area should be designed, if possible, to make room for future ex-
pansion.
It is important to consider all demands regarding safety cupboard for rst aid,
etc. see Chapter 26.
With both basic and detailed planning it is important that the personnel already
using the lab, or intending to work in the new lab, participate in the planning work.
This ensures that a lot of problems are solved in the planning stage and the most ef-
cient functionis obtained.
25.3.2 Detailed Planning
Factors like type of specimenmaterial, number of specimens to prepare, etc., will inu-
ence the details inthe lab.
Specimen Material
The specimen material inuences the type of equipment used. If only one type of mate-
rial is to be prepared, relatively simple machinery may be used. In the case of a vast
spectrumof materials, more machinery may be needed because of the different prepa-
rationmethods needed.
Number of Specimens
The average number of specimens per day will vary very muchfromlab to lab. AQClab
might have a hundredor more specimens per day, maybe inworking shifts. Inthis case,
a very rational preparation can take place see Section 25.2. In a research lab perhaps
only ten specimens per day are made on average, but the materials span widely so that
several types of preparationprocesses are available.
In some cases with very fewspecimens, the preparation might be performed in the
Chemical Lab or Materials Testing Lab.
The Specimen Size and Shape
In some cases the lab receives the specimens cut to the right size. In other cases large
work pieces, machine parts, or stock material are received and the lab should take care
of cutting out the specimen. This may require a special room for cutting, often with
large machines.
The mounting of the specimen will vary. In mounting a large number of speci-
mens, a special room for hot mounting presses should be considered. In the case of
coldmounting, fume hoods must be available.
Type of Examination
For labs working with QC or other types of inspection, the lab might be under time
pressure, being required to deliver an analysis result in a given period of time. This
inuences howthe lab is organized, securing fast results and reporting, effective com-
munication, etc. In some cases, the metallographic/materialographic analysis is com-
bined with other examinations, like hardness testing, and care should be taken that
these other instruments are integrated inthe best possible way inthe lab. Insome labo-
ratories, the specimens, before or after preparation, have to be treated in other labora-
tories and a rational cooperation must be secured. Using a digital camera, the images
often necessary for reporting can easily be communicated, avoiding the more tedious
photographic work.
Personnel
Persons with different educational background and training are needed in the
metallographic/materialographic lab. Cutting, mounting, and preparation work can
be done by persons with little or no metallographic/materialographic background. For
persons without knowledge of metallography/materialography, they should be trained
thoroughly before starting the work because lack of knowledge may jeopardize the
preparationresult.
Interpreting the microstructure, working out reports, etc., shouldbe performedby
persons with the necessary education in metallography/materialography. In spite of
the increasing use of semiautomatic equipment, it should be emphasized that the per-
sonnel should be well trained and be allowed to develop experience over a long period
of time.
25.4 Equipment and Laboratory Layout
A large selection of equipment for preparation, examination, and reporting IT is
available in the market. The tendency goes towards automation both regarding prepa-
ration and analyzing, where the result will now be electronically communicated in IT
networks.
It is important to select the right equipment, both to secure a high quality, cost-
efcient production of specimens and to secure a certain exibility increase in the
number of specimens to be prepared and analyzed. Table 25.1 gives an overviewof the
equipment neededfor a metallographic/materialographic lab, andinthe following sec-
tions examples for different labs are given.
The layout of the lab with several rooms and the correct installations, etc., also
plays an important role to ensure an efcient specimen production. This will be dis-
cussedbelow.
25.4.1 EquipmentTable 25.1
The basic equipment is stated in Table 25.1, but in each category several models are
available, e.g., a grinder/polisher canbe hand-operatedor automatic see Chapter 7.
In the following sections some examples are given for different sizes of labs, indi-
cating the types of machines.
Small Laboratory
A laboratory with only one to ten specimens per day can be dened as a small lab. This
type of lab can be at a sub-supplier to a large company, where a metallographic/
materialographic examinationis part of the specications for the suppliedproduct.
The following equipment shouldbe available:
TABLE 25.1Equipment, Accessories, and Consumables for a Metallographic/Materialographic Laboratory.
Preparation Stage Process Equipment
Accessory/
Consumable
Sectioning Wet abrasive cutting
Precision cutting
Cut-off machine
Precision cutter
Cut-off wheels,
additive for cooling
uid
Shearing Shear
Sawing Hacksaw Saw blades
Bandsaw Saw bands, cutting uid
Wire cutting Wire cutter Wire
Mounting Hot compression Hot mounting press Hot mounting resins
mounting
Cold (castable) Mounting molds Cold mounting resins
mounting
Heating of epoxy Small oven Cold mounting epoxy
Clamping (sheets) Clamp
Impregnation Vacuum impregnation
apparatus
Resins with low viscosity
Vacuum pump Dye
Marking Engraving Engraver Engraving needless
Surface preparation
mechanical
Grinding Plane grinder with
grinding stone
Grinding stones,
additive for cooling uid
Grinder/Polisher/
sample mover
Disks (platens),
rigid composite disks
(RCD),
wet grinding papers,
diamond disks
Belt grinder Grinding belts
Mechanical polishing Grinder/polisher/sample
mover
Disks (platens),
polishing cloths,
Vibratory polisher diamond consumables,
lubricants,
oxide consumable
(Al
2
O
3
, SiO
2
)
Dispensing of diamond
suspension
Dosing unit Diamond suspension
Surface preparation
electrolytic
Electrolytic polishing Electropolisher Electrolytes
Electrolyte containers
Thinning for TEM Electrolytic polishing Jet-thinning apparatus Electrolytes
Cleaning Ultrasonic cleaning Ultrasonic apparatus Cleaning liquids
Ethanol, cotton
Drying Drying apparatus
(hair dryer)
Conservation Desiccator Desiccants
Special cupboard Protective media
Etching Chemical etching Plastic container, pair of
tongs
Etchants
Electrolytic etching DC-power supply with
pair of tongs
Etchants
Sectioning: Cut-off machine, table top, hand operated, cut-off wheel diameter
200250 mm810 in. For an examination of sheet products, a hand shear should be
available. Avertical bandsawmight be useful also.
Mounting: Cold mounting materials with mounting cups or a hot mounting press,
or both, if the investment is justied. In the case of sheet specimens, a clamp can be
usedfor manual preparation.
Plane grinding/Fine grinding/Polishing: Rotating grinder/polisher 2 speeds, 200
or 250 mm 8 or 10 in disk diameter. This is sufcient for manual preparation, but to
ensure highest reproducibility and avoid tedious work, a small specimen mover for
three or six specimens should be mounted on the grinder/polisher. This also ensures a
relatively high quality of the specimens, even with a relatively unskilled operator. A
dosing unit, adding diamond suspension and lubricant in an optimal way, will also im-
prove quality andeconomy.
Microscope/Documentation: A small or medium-sized light microscope with
bright eld/dark eld and differential interference contrast DIC is recommended see
TABLE 25.1(Continued.)
Preparation Stage Process Equipment
Accessory/
Consumable
Potentiostatic etching Potentiostat
Thermal etching Oven
Vapor deposition
Sputtering
Vacuum chamber
Ion etching
Examination Optical microscopy Magnifying glass,
Light microscope, small,
medium, large
Stereomicroscope
Image analysis system
Objectives
Eyepieces
Electron microscopy SEM Sample mounts
EPMA
TEM
STEM Sample mounts
Documentation Microscopy Macro camera Films, paper
Micro camera
Polaroid camera
Digital camera
PC with monitor
Video equipment
Printer
Cutter
Refrigerator
Indentation hardness
testing
Vickers/Knoop
microindentation
hardness
Microhardness tester Indenters
Brinell/Vickers hardness Universal hardness tester Indenters
Rockwell hardness Rockwell hardness
tester
Indenters
Part III. For making images for reporting, a Polaroid 4 in5 in or digital camera
shouldbe used, the latter inconnectiontoa PCanda printer.
Medium-Sized Laboratory
Amedium-sized lab will prepare three to fty specimens a day, mounted or unmounted
see Table 25.1.
The following equipment canbe recommended:
Sectioning: Cut-off machine, table top or oor model, automatic feed, cut-off
wheel diameter 250350 mm1014 in. For large work pieces, larger automatic ma-
chines with a wheel diameter up to 600 mm24 in are needed see Section 2.5. If pre-
cision cutting or cutting with lowest possible deformation of the cut surface is needed,
a precision cutter should be available. A bandsawcan also be useful, and a hand shear
canbe usedfor sheet products.
Mounting: One or two hot mounting presses and consumables for cold mounting.
A vacuum impregnation apparatus and a small oven for accelerating the curing of ep-
oxy coldmounting resins might be included.
Plane grinding: With large specimens and a relatively high production with the
specimens xed in holders, a special plane grinding machine is recommended using a
grinding stone. In most cases, however, the plane grinding can take place on the same
machine as for ne grinding/polishing.
Fine grinding/polishing: This is preferably done on a table model, semiautomatic
system, consisting of a grinder/polisher with a 250 or 300 mm 10 or 12 in disk and
specimen mover with specimen holders for xed or single specimens, or both, which
canprepare up to six to eight specimens at a time. To obtainthe highest reproducibility
a semiautomatic, programmable systemwith a dosing unit included is recommended.
In case of a relatively high production of larger specimens, a oor-based, program-
mable grinder/polisher, using specimens xedina holder is recommended.
To save manpower and increase the reproducibility, a fully automatic preparation
system could be used. A fully automatic system might show a favorable cost/benet
see Section25.2, especially for difcult toprepare materials.
An electropolisher could be of advantage as a supplement to the mechanical
preparation equipment, depending on the type of material to be prepared see Chapter
8.
Etching: Chemical etching is typically used and needs only a very low investment
see Table 25.1. If other contrasting methods should be used, like thermal etching or
interference layers, special equipment must be procured see Table 25.1 and Chapter
9.
Microscopy/Documentation: A good quality light microscope with good optics
should be available. This shall have bright eld/dark eld, polarized light, differential
interference contrast DIC, anduorescence.
For documentationone or more of the following cameras shouldbe available:
A normal, single lens reex camera 35 mm, a Polaroid camera 4 in5 in, or a
digital camera. For all types, an automatic control unit should be connected to the mi-
croscope. For a digital camera, a PCwithmonitor shouldbe available anda printer.
For macro work, a stereomicroscope with camera connection should be available.
Acamera for macrophotography shouldbe available also.
Large-Sized Laboratory
The large laboratory has from10100/ 200 specimens per day, and the specimens pro-
duced are very often for quality control relating to a production. Therefore, the main
concernis tohave a fast, efcient owof preparedspecimens.
The following equipment canbe recommended:
Sectioning: The conditions are the same as mentioned above under the Medium-
SizedLaboratory.
Mounting: The conditions here are also close to the medium-sized lab, only a
larger number of mounting presses may be needed.
Plane grinding: With a large number of specimens and using specimen holders
with xed specimens, plane grinding can be a bottleneck; therefore, a special plane
grinding machine is recommended, using a grinding stone. In some cases, the plane
grinding will be part of a fully automatic systemsee below.
Fine Grinding/Polishing: With a large number of specimens, handling, manual
cleaning, etc., should be avoided to save time. Therefore, fully automatic systems with
a high number of preparation programs and built-in dosing and cleaning are recom-
mended. These systems can be used for both normal specimen sizes and for large,
unmounted specimens. The only manual handling is placing the specimens in a holder
andremoving the nishedspecimenready for etching/microscopy fromthe holder.
An alternative is one or more of the systems described above under Medium-Sized
Labs. Electropolishing may be useful also, as mentionedabove.
Etching/Microscopy/Documentation: This is the same as mentioned under
Medium-SizedLabs.
25.4.2 LayoutFurnitureInstallations
The layout of a metallographic/materialographic lab should include several rooms,
making it possible to keep the different activities separated. The furniture should be
appropriate and the installations specically made to ensure an effective working pro-
cedure.
The space between tables and machines should be so that several persons can
work and move around in the lab without disturbing each other. During planning,
space should also be reserved for extension considering a period of three to ve years,
often, a relatively newlabgets crammedafter a fewyears.
Rooms
A metallographic/materialographic lab should have at least three rooms, each con-
nected with a door for easy passage from room to room. A lab for quality control pur-
poses could have three rooms, and a research lab, covering a wide material eld and
many different processes might have four rooms.
Room 1: This is the room for dirty processes, sectioning, and mounting. If cold
mounting is performed in this room, a fume hood should be installed. Plane grinding
also may be done in this room if a special machine is available for plane grinding. A
sink should be installed in this room, and the idea is that a specimen, leaving the room,
is cleanandready for the proper preparationinRoom2.
Room2: This is the main area of the lab, containing a preparation area and possi-
bly an area for the personnel for working out preparation reports, etc. see below. Ma-
chines for preparation should be placed so that persons passing by do not disturb the
operator. Table space around a machine should be 80100 cm 34 ft to ensure an
efcient working order andmake roomfor possible service workonthe machine.
At least one or two sinks shouldbe placedvery close to the grinder/polisher. It must
be understoodthat cleaning is a very important part of the preparationprocess, andthe
operator shouldbe able tocleanthe specimens whenonly moving a fewsteps.
Another sink is placed under a fume hood to be used for chemical etching. The
same hood, if large enough, can be used for electrolytic polishing, with the polishing
table being placedunder the hood.
Asmall, lowcost, upright or inverted microscope, placed near the preparationma-
chines, is also useful to examine the specimens between the preparation steps. Other
instruments like hardness testers are also placed in this room. Space should be avail-
able for desks with PCs for the personnel, preferably separated fromthe machine area,
if these are not placedinconnectionwithRoom3together withthe microscopes.
Room 3: This is the microscope room with a large microscope and possibly a
stereomicroscope and other examining instruments. The working places for the per-
sonnel canbe placed inthis roomalso, separated fromthe microscopes, preferably as a
separate ofce. In the ideal microscope room, an air conditioning system keeps a
constant temperature. Specimens can also be stored in this room in a desiccator one
for eachmetallographer or a special cupboard.
Room4: Incertaincases, a fourthroommay be recommended. This roomwill take
over the etching functions of Room2. The roomwill have one or two fume hoods for
etching, electropolishing, andother processes that must be kept under strict control.
Darkroom: For photographic work, one or two darkrooms will be necessary, but
this wont be necessary if only digital photography is used.
Furniture
Laboratory furniture is available frommany suppliers, but it should be taken into con-
sideration that this furniture is made typically for chemical labs, not metallographic/
materialographic labs. The most important points to observe are the following: The
metallographic/materialographic machine has a certain height, and the working area
of the machine is often too high for convenient work if the table is a normal lab table.
The surfaces of tables, etc., should be resistant to acids, alcohol, etc. Drawers for the
grinding/polishing disks should be available, preferably placed under the tabletops
very close to the machines. Shelves for consumables like cut-off wheels, grinding pa-
per, etc., and storing space for other consumables, specimen holders, etc., should be
close to the machines, and correctly made storage space for chemicals, glass articles,
etc., should be close to fume hoods. Channels for taking pipes, tubes, and cables to the
machines shouldbe made inthe tables.
Other furniture is solid tables for microscopes, special cupboards for storing of
specimens, cupboards for archiving, etc., shelves for a small library, and a refrigerator
for storing of polaroidlms, etc.
Installations
The metallographic/materialographic labshouldhave the following installations:
Hot/cold water at all sinks and compressed air preferably at all sinks and at all
tables and places to be used for equipment. The compressed air should be clean, pass-
ing a water/oil separator and a particle lter. Adequate three-phase and one-phase elec-
tricity should be taken to all tables and places to be used for equipment, especially cut-
off machines require a highamperage.
Drainage should be installed in all tables and places to be used for equipment. The
drainage should be made according to the regulations of the local authorities, taking
into consideration that acid and other chemicals together with debris from the prepa-
rationprocess will owinthe drainage system.
For installations regarding protectionof personnel see Chapter 26.
25.5 Maintenance
The most obvious reason for maintaining the laboratory in good working order is
economy. A badly organized laboratory that cannot carry out its work properly and
timely cancause unnecessary additional lab expenses and costs due to delayed produc-
tion.
Another important reason to focus on quality inspection and competitiveness is
that the laboratory is a showcase for the company. Any manufacturing company that
wants to attract customers and convince them of the quality of its goods needs a well
equipped and presentable laboratory. A well run metallographic/materialographic
laboratory with a good working atmosphere will reect positively on the companys
image.
The maintenance canbe split intoorganizing, cleaning, andservicing.
25.5.1 Organizing
Accessories and consumables for machines should be in easy reach of the operators.
Special lab furniture or wall shelves help to keep grinding paper, cut-off wheels, polish-
ing cloths, and disks out of the way but still accessible. In a metallographic/materialo-
graphic lab a large variety of small items are needed in everyday operation. Small tool
or tackle boxes help to keep screws, tweezers, springs, rings, dummy samples in or-
der. Wire racks over the sinkare essential for storing wet glassware.
It is always important to have enoughconsumables available to guarantee uninter-
ruptedwork.
Large quantities of consumables shouldnot be stockedinthe laboratory, but inthe
mainstoreroombecause they take uptoomuchof the valuable space inthe lab.
25.5.2 Cleaning
Keeping the machines and work area clean is one of the most important matters in a
metallographic/materialographic laboratory. Every machine should be wiped clean
witha wet clothbefore the staff leaves inthe afternoon. This shouldalso be done before
shift change, sothat the incoming operators start withcleanmachines. If this routine is
not possible, a specic day or time should be set aside each week for cleaning the ma-
chines.
Recirculation cooling units have to be cleaned and relled at regular intervals, at
least once a month depending on the workload. The spray nozzles of certain automatic
diamond dispensing systems must be cleaned occasionally to avoid drying of the dia-
mondsuspensions inside the nozzles.
As a rule, rigid composite disks RCDs and polishing cloths should not be cleaned
regularly. However, they can be cleaned with water/soap or ethanol, or both, if too
much debris has built up on the surface and stops themfromgrinding/polishing prop-
erly, or if they are contaminated.
25.5.3 Servicing
Regular service checks ensure that the equipment is always in a correct working condi-
tion. This is crucial because correct maintenance is the basis of reliability, avoiding
irritating stops, and reproducibility, and securing the correct preparation result, even
over a long periodof time.
26
Occupational Safety and Health in
the Metallographic/
OCCUPATIONAL SAFETY AND HEALTH ARE IMPORTANT IN A METALLO-
graphic/materialographic labs considering the use of machines, chemicals, plastics,
etc.
The dangers in the metallographic/materialographic laboratory will be discussed,
and a special section will describe dangerous and hazardous materials. In Section
26.1.8 the ASTM Guide for Metallographic Laboratory Safety E 2014 will be shortly
described, the only standard specically covering the safety in the metallographic/
materialographic lab. The standard is stated in full in the CD-ROM included in this
manual.
At the end of this chapter, the most important rules and regulations for safety and
healthcovering the metallographic/materialographic labwill be stated.
26.1 Dangers in the Metallographic/Materialographic
Laboratory
The laboratory having functions like cut-off, specimen preparation, and etching in-
volves a number of potential dangers. In the following the most important precautions
regarding safety and health are mentioned, not claiming that all potential dangers and
necessary safety andhealthmeasures are mentioned.
26.1.1 Sectioning
Eye protection and gloves should be used when working with machines and tools for
sectioning. Abrasive cut-off machines will have a hood shield protecting the operator
against cooling uid, pieces froma broken cutting wheel, etc. According to safety regu-
lations, the machine can only be started when the hood is closed. When cutting with
bakelite or rubber wheels, fumes develop, and at larger machines the cutting chamber
shouldbe connectedtoanexhaust system.
For bandsaws, the operator will guide the work piece into the band, and it is very
important that this is done indirectly using a distance piece or a special holder for the
workpiece.
A Standard Operating Procedure SOP, including a Job Safety Analysis JSA see
Section 26.2.3/4 should be completed for each piece of equipment being used for
sectioning.
26.1.2 Mounting
With hot compression mounting, the main danger is the high temperatures used in the
mounting presses. Gloves should be used for handling of the hot mounts, and when
664
lling mounting material such as bakelite powder into the press, inhalation of dust
shouldbe avoided.
ASOP, including a JSA, shouldbe completedfor eachpiece of equipment.
At cold castable mounting there are several potential dangers. The cold mount-
ing resins are potentially dangerous to health see Section 26.1.7, and therefore all
handling shouldbe done withrubber latex gloves toavoidskincontact andthe mixing
and hardening shall take place under a fume hood. When using an oven for accelerat-
ing the hardening of epoxy, gloves shouldbe used.
MSDS information should be available for all mounting resins see Section
26.2.2.
The semiautomatic preparation machines are basically safe to use. If a specimen is
slung away from the specimen holder during rotation, the specimen will usually be
kept inside the machine, and the speeds of the disks and holders are relatively low. To
avoid dirty hands, especially when using rigid composite disks that create a very ne
sludge that is difcult to remove fromthe skin, rubber or plastic gloves should be used.
For large machines using a ammable alcohol-based lubricant, the alcohol fumes can
be rather strong, and the machine should be placed in connection to a fume exhaust
system. Abetter solutionmight be tochange the lubricant toa water-basedtype.
When working with semiautomatic machines, a laboratory coat should be used to
avoid that ties or other pieces of clothing get into contact with the rotating specimen
holder.
Fully automatic systems are totally enclosed and will not operate if the protective
shields are not closed.
At manual grinding/polishing, care should be taken that a specimen released by
the operator andying fromthe grinding/polishing diskwill not injure other persons.
A SOP, including a JSA, should be completed for all mechanical and polishing
equipment.
26.1.4 Electrolytic Polishing/Etching
The most serious potential danger at electrolytic polishing and etching is the mixing,
handling, use, andstoring of electrolytes see Section26.1.5. During the polishing pro-
cess, care should be taken to avoid heating of the electrolyte that may cause a re or
even an explosion. It is important to keep a correct level of electrolyte in the electrolyte
container because too little electrolyte might give air pockets in the polishing chamber
causing a spark betweenanode and cathode, whichmight ignite the alcohol inthe elec-
trolyte.
ASOP, including a JSA, shouldbe completedfor eachelectropolisher.
26.1.5 EtchingEtchantsElectrolytes
The etching procedure should be performed using gloves and eye protection under a
fume hood. The most serious potential dangers are connected to the mixing, handling,
and storing of the chemicals used for etchants, and the same is the case for electrolytes.
The user should have sufcient information on all the chemicals used from training
and MSDSs, which should be available in the laboratory see Section 26.2. Etchants/
electrolytes are mostly solutionmixtures of different materials mixedinthe laboratory.
During the mixing, very dangerous reactions canbe establishedlike re, explosion, and
dissolution, creating dangerous substances. The etchants are generally more danger-
Chapter 26 Occupational Safety and Health 665
ous thanthe electrolytes because they containvery oxidizing substances.
As a rule, the mixing should always start with the water alcohol and then mix the
other ingredients into this. A special procedure, however, should often be followed to
obtain the necessary safety, and certain combinations of chemicals are known to be
dangerous. Information on this must be available in the laboratory. A number of the
most hazardous materials are mentioned below, and further information can be ob-
tained in the Standard Guide on Metallographic Laboratory Safety E2014 in Section
26.1.8of this book.
Acetic Acid: Extreme care should be taken when mixing with other acids like per-
chloric acid and nitric acid. Mixtures of acetic acid and perchloric acid should be
avoided.
Chromic Acid: Very strong oxidation substance, very strong reaction with organic
or easy to oxidize material and it cannot be safely mixed with acetic acid and most or-
ganic liquids, suchas alcohols or glycerol. Poisonous.
Nitric Acid: Strong oxidizing acid, creating gases withmany organic materials and
metals. Donot store solutions of more than3%nitric acidinethanol.
Perchloric Acid: Very aggressive acid that can cause serious explosions at higher
concentrations. Very dangerous at contact with metals that oxidize easily, such as bis-
muth. Contact to organic material should also be avoided; if absorbed in organic mate-
rial the material must be placed in water. Organic material should never be used to
wipe upperchloric acid.
Picric Acid: Aggressive oxidizer and should always be stored in wet condition. In
dry conditionthe riskof explosionis high. Storage shouldbe cool andre safe.
Toxic Substances
Toxic materials are substances that, when inhaled or taken in by the mouth or by the
skin, can lead to death or serious damage to the health. These substances are listed by
ofcial organizations like the National Institute for Occupational Safety and Health
NIOSH see Section 26.5, and rules are dened for their use, storing, handling and
disposal. Also, for many substances the permissible exposure through air and skin is
statedsee Section26.5.
A number of toxic substances with CAS Nos. see Section 26.5.1 often used in a
metallographic/materialographic laboratory are mentionedbelow.
Chemicals based on the metals Be, Pb, Cr, Cu, Ag, U, Sn, Zn not ZnO
2
: Poisonous
as liquids or as vapor.
ChlorinatedCarbohydrates: These solvents are very dangerous toinhale.
Cyanides CAS No. 460-19-5: These react strongly with acids, even the CO
2
con-
tent inhumidatmospheric air gives a reaction. Very poisonous.
Hydrouoric Acid, Anhydrous CAS No. 7647-01-0: In concentration higher than
0.5 %the acid is very dangerous, making very serious damage to tissue. Attacks almost
all metals andglass. Very dangerous.
Mercury CASNo. 7439-97-6: Chemicals bond on mercury and mercury vapor are
poisonous.
Methanol CASNo. 67-56-1: Poisonous.
Oxalic Acid CAS No. 144-62-7 Anhydrous CAS No. 6153-56-6 Dihydrate: In
concentrations higher than5%oxalic acidis poisonous.
Phosgen Carbonyl Chloride CASNo. 75-44-5: Very dangerous to the respiratory
system.
Flammable Liquids
Flammable liquids are used in metallographic/materialographic preparation for elec-
trolytic polishing, lubrication, etching, andcleaning.
OSHA see Section 26.5 denes ammable liquids. Class I liquids as any liquid
having a ashpoint below 100F 37.8C, except any mixture having components
with ashpoints of 100F 37.8C or higher, the total of which make up 99 %or more
of the total volume of the mixture.
Liquids, which are somewhat harder to ignite, with a ash point above 100F
37.8C are called combustible liquids, Class II liquids. These are dened by OSHA
as liquids with ashpoints at or above 100F 37.8C and below140F 60C, except
any mixture having components with ashpoints of 200F 93.3C or higher, the vol-
ume of whichmake up99%or more of the total volume of the mixture.
Class III liquids are evenharder toignite andare denedby OSHAas liquids.
Class IIIA liquids include those with ashpoints 140F 60C or above and below
200F 93.3C, except any mixture having components with ashpoints of 200F
93.3C, or higher, the total volume of whichmake up99 %or more of the total volume
of the mixture.
Class IIIBliquids include those withashpoints at or above 200F93.3C.
When a combustible liquid is heated for use to within 30F 16.7C of its ash-
point, it should be handled in accordance with the requirements for the next lower
class of liquids.
All containers withammable liquids shouldbe markedsee Section26.5.3.
The number of ammable liquids stored in the lab should be kept at a minimum
andcarefully protectedagainst heat andagainst possible ignition.
All rules and regulations should be followed carefully when handling ammable
liquids. Heating in open containers should be done with special care, using a fume
hoodandspecial electric heating plates.
The ammable liquids are also very often dangerous to health and precautions
shouldbe takenaccording tothe MSDSfor the liquidsee Section26.2.2.
Disposal can be a problem and should be done according to rules and regulations
by local authorities.
26.1.6 Dust
Dust can be developed fromspecimen material, abrasives, or powders used for mount-
ing. This should be suppressed as much as possible, because even if not toxic, the dust
cangive respiratory problems. Dust frommetals canbe toxic andshouldbe avoided.
26.1.7 Cold Castable Mounting Resins
All the cold castable mounting resins described in Section 3.8 are potentially danger-
ous tohealth.
Epoxy
This material, both resin and hardener, can damage the skin, causing allergic reac-
tions. The material should never come in contact with skin and the vapors should not
be inhaled. All work with epoxy should take place under a fume hood using personal
protective equipment PPE specied in the MSDS. It is recommended that containers
andstirring pins are disposedof after mixing.
The epoxy is not dangerous whenit has fully hardened.
Acrylics and Polyesters
Mixing should always take place under a fume hood and gloves should be used when
handling these materials toavoidinhalationandskincontact.
26.1.8 Standard Guide on Metallographic Laboratory Safety E 2014
This ASTM guide covers the outline of the basic safety guidelines to be used in a
metallographic/materialographic laboratory. Safe working habits are discussed for
various tasks performed in the laboratory and the guide goes into more details of the
work than stated above in this chapter. Please refer to ASTM E 2014 in the CD-ROM
includedwiththis book.
26.2 Safety Information
It is very important that the user of a chemical substance is informed on all important
facts regarding the substance. According to the OSHAStandard 29 CFR1910.1200 see
Section 26.5.3, any chemical should be labeled for safe identication and a Material
Safety Data Sheet MSDS shouldbe available onthe working place for any chemical.
26.2.1 Identication
It is important that the dangerous materials can be identied. Materials that are in one
way or another hazardous should be marked with a label according to a system, as
stated in the standards see Section 26.5. This label must express a number of facts
regarding the substance so that the user is able to evaluate the possible hazard. The
container with the substance is usually labeled by the supplier, but in cases where
chemicals are taken into smaller containers in the lab and in other cases where the
original container is not used, a newlabel must be used.
Below two ofcial identication systems, NFPA and EU EC, used by suppliers
of chemicals andone system, HMIS, developedfor use inthe laboratory, are described.
NFPA 704 Hazard Identication Ratings System
This identication system, developed by the National Fire Protection Association
NFPA uses the Hazard Diamond see Fig. 26.1 for identication of health, amma-
Fig. 26.1The NFPA diamond symbol: 1 Indication of color and type of hazard of the four
small diamonds. 2 Example of number ratings and symbol.
bility and instability reactivity see also Section 26.5.11. The diamond is broken into
four smaller diamonds one each blue, red, yellow, and white. The numbers in the three
colored diamonds range from 0 least severe hazard to 4 most severe hazard. The
fourth white diamond is left blank and is used only to devote special re ghting
measures/hazards, indicatedwithspecial symbols.
Meaning of ColorsRatings of Numbers
Red: FLAMMABILITYInstability is the degree of susceptibility toburning.
0 Will not burn.
1 Must be preheated to burn. Flash point above 200F 93.5C.
2 WARNING: Ignites with moderate heat. Flash point 100F200F 3893.5C.
3 HAZARDOUS: Ignites at room temperature. Flash point 73F99F 2337C.
4 EXTREMELY DANGEROUS: Highly ammable liquids and explosive gases. Flash
point below 73F 23C.
Yellow: REACTIVITYInstability is the degree of susceptibility of materials to re-
lease energy.
0 Normally stable at all temperatures. Not reactive with water.
1 CAUTION: May become unstable when heated or mixed with water.
2 HAZARDOUS: Normally unstable or may have violent chemical change when mixed
with water.
3 DANGEROUS: Explodes with exposure to conned heat, shock, or when mixed with
water.
4 EXTREMELY DANGEROUS: Explodes at room temperature.
Blue: HEALTHHAZARDis the degree of injury fromburning materials.
0 Creates no unusual hazard.
1 CAUTION: Causes irritation or minor injury.
2 HAZARDOUS: Intense exposure may be harmful.
3 EXTREMELY DANGEROUS: Avoid skin contact and inhalation.
4 FATAL: Too dangerous to enter without specialized protective equipment.
White: OTHERindicates special warnings.
ACID acid
ALK alkali
COR corrosive
OXY oxidizing chemicals
radiation
P subject to polymerization when mixed with water
W do not use water
EU EC Identication System
The European Union EU has issued a directive, Council Directive 67/548/EEC of 27
June 1967, covering classication, packaging, andlabeling of dangerous substances.
According to this directive, all dangerous substances sold in the EU, the European
Economic Area and selected other countries, should be marked with a labeling symbol
andone or more RiskPhrases andSafety Phrases.
Labeling Symbols
The symbols indicate the basic serious dangers, expressed in a gure, and a short text
expressing the Category of Danger, Symbol Letter, and Indication of Danger see Fig.
26.2.
Risk PhrasesSafety Phrases
To give further information to the user of the substance, one or more Risk Phrases R
Phrases and Safety Phrases S Phrases should be indicated. The phrases are often
combined see below. A high number of R and S phrases are available and a few ex-
amples are givenbelow, indicating the number of the phrase.
Examples of RPhrases:
R1 Explosive when dry
R10 Flammable
R20 Harmful by inhalation
R21 Harmful in contact with skin
R20/21 Harmful by inhalation and in contact with skin
R24 Toxic in contact with skin
R25 Toxic if swallowed
R24/25 Toxic in contact with skin and if swallowed
Examples of SPhrases:
S1 Keep locked up
S15 Keep away from heat
S20 Do not eat or drink when using
S24 Avoid contact with the skin
S25 Avoid contact with eyes
S24/25 Avoid contact with skin and eyes
S36 Wear suitable protective clothing
S37 Wear suitable gloves
HMIS: Hazardous Materials Identication System
Incase the user makes the labeling, this canbe supported by systems developed for this
purpose.
HMIS is a complete program that helps employers comply with OSHAs Hazard
CommunicationStandardHCS. The programuses a numerical hazardrating system,
labels with colored bars giving information on health, ammability, and reactivity haz-
ards. Training material is provided to informworkers of chemical hazards in the work-
place see Section26.5.12.
26.2.2 Material Safety Data Sheet MSDS
A Material Safety Data Sheet MSDS is designed to provide both laboratory personnel
and emergency personnel with the proper procedures for handling or working with a
particular substance. MSDSs include informationsuchas physical data, healtheffects,
rst aid, reactivity, storage, disposal, protective equipment, and spill/leak procedures.
These are of particular use if a spill or other accidents occur.
MSDSs are made according to the OSHA Standard on Hazard Communication
HCS or the ECDirective onSafety Data Sheets see Section26.5.
MSDSs are meant for:
Fig. 26.2EU labeling system. Symbols pictograms with words and letters indicating
categories of danger.
Employees whomay be occupationally exposedtoa hazards at work.
Employers whoneedtoknowthe proper methods for storage, etc.
Emergency responders such as re ghters, hazardous material crews, emergency
medical technicians, andemergency roompersonnel.
MSDSs are not meant for consumers. An MSDS reects the hazards of working
with the material in an occupational fashion. For example, an MSDS for a given paint
is not highly pertinent to someone who uses a can of paint once a year, but is extremely
important tosomeone whodoes this ina connedspace for 40 hours a week.
The MSDS Format
The formats of MSDSs tend to vary, but they usually convey the same basic kinds of
information.
Supply of MSDS
MSDSs should be kept at the workplace. They are usually delivered by the supplier of a
given product. If it is not delivered, ask the supplier for immediate delivery. For com-
monly known substances, MSDSs can be obtained from an OSHA ofce or science li-
brary. Many organizations and chemical suppliers, like Cornell University and Sigma-
Aldrichhave databases withMSDSonthe Internet.
26.2.3 Standard Operating Procedure SOP
Standard Operating Procedures SOPs can be made for chemicals or processes and
shall contain the operating procedure in relative detail so that an operator can perform
the procedure ina satisfactory way without risk. Oftenat procedures involving hazard-
ous materials or other potential risks a Job Safety Analysis JSA is included in the SOP
see below.
26.2.4 Job Safety Analysis JSA
The Job Safety Analysis JSA is a very effective means of helping reduce accidents and
injuries in the workplace. Any job that has hazards or potential hazards is a candidate
for a JSA. Based on the operating procedure SOP, the potential hazards for each step
in the working process are identied. It is very important to look at the entire environ-
ment to determine every hazard that might exist. Based on the steps in the working
process and potential hazards, it is decided what actions are necessary to eliminate,
control, or minimize hazards that could lead to accidents, injuries, damage to the envi-
ronment, or possible occupational illness.
26.3 Disposal of Chemicals
Disposal of chemicals should follow the local rules and regulations. These can vary
very much from place to place and therefore it is very important to obtain the rules
fromthe local authorities.
As a common rule, the chemicals should be kept separated. Strongly oxidizing
chemicals especially should not be mixed with other chemicals. The chemicals for dis-
posal should be carefully categorized so that no mistake can take place when the waste
is transportedandtreatedfurther.
Typical categories couldbe:
1 Chlorinatedhydrocarbons like trichloroethylene
2 Hydrocarbons containing aromatic solvents like xylene, terpentine, kerosene
3 Hydrocarbons not containing aromatic solvents like acetone, ketones, alcohols
4 Acidic, aqueous solutions containing chromiumcompounds
5 Acidic, aqueous solutions containing nitric acid, but not hydrouoric acid
6 Acidic, aqueous solutions containing hydrouoric acidor HFsalts
7 Acidic, aqueous solutions containing hydrochloric acid, sulfuric acid or phos-
phoric acid
8 Basic aqueous solutions containing metal compounds but not cyanide
9 Metal sludge containing chromium, copper, nickel, zinc, lead, cadmiumandsilver
26.4 Occupational Safety in General
26.4.1 Standards
Inthe sections above, the hazards of chemicals andmachines have beendiscussed.
As a rule, the machines and apparatus are designed and manufactured according
to relevant standards. These are the technical standards, safety standards, and oc-
cupational standards. The occupational standards, describing the conditions, when
working in the laboratory concerning machines and chemicals, can be the OSHA stan-
dards No. 29 CFR 1910.212, General Requirements for All Machines, No. 29 CFR
1910.215, Abrasive Wheel Machinery, No. 29 CFR 1910.95, Occupational Noise Expo-
sure, No. 29 CFR1910.120, General DescriptionandDiscussionof the Levels of Protec-
tion and Protective Gear, and the important Hazard Communication standard, No. 29
CFR1910.1200see Section26.5.
26.4.2 Training
It is very important that the personnel be trained, bothinusing the machines and other
equipment, and in health and safety precautions. Not only the training in the practical
use, but aneducationinthe correct attitudes is alsoimportant.
26.4.3 Maintenance and Service
It is important that all equipment, building parts, and installations are kept in good
working order andrepair is made immediately incase of failure.
Unauthorizedpersonnel shouldnot performrepair work.
26.5 Standards and RegulationsOrganizations
A number of American and International organizations are responsible for issuing
standards and regulations connected to occupational safety and health in the
metallographic/materialographic laboratory.
The rst section below states a number of abbreviations used in connection with
safety andhealth.
26.5.1 Designations and Abbreviations Used to Describe a Chemical
Substance
Ca: Asubstance NIOSHsee below considers a potential occupational carcinogen
CAS Number: Chemical Abstract Service Registry Number. This number identies
each chemical. The Chemical Abstracts Service is a division of the American Chemical
Society
IDLH: Immediately Dangerous toLife or HealthConcentrations
PEL: Permissible Exposure Limit
PPE: Personal Protective Equipment
REL: RecommendedExposure Limit
RTECS: Registry of Toxic Effects of Chemical Substances see Section26.5.4
STEL: Short-TermExposure Limit as designatedby ST preceding the value
TLV: ThresholdLimit Value, issuedby ACGIHsee Section26.5.8
TWA: Time-WeightedAverage usedinREL
UNNumber: Four digit number toidentify hazardous chemicals transport.
26.5.2 ASTM Standard
The only standard that directly describes the safety in the metallographic/material-
ographic laboratory is issuedby ASTM.
Standard Guide on Metallographic Laboratory Safety E 2014 covers the outline
of the basic safety guidelines to be used in a metallographic/materialographic labora-
tory. This standard is stated with its full text in the CD-ROM included with this book
see Section26.1.8.
All other standards see below are directed towards the problems in general and
specic matters inside and outside the metallographic/materialographic lab. E 2014,
being specic regarding metallographic/materialographic labs, makes it an important
document that should be followed by all metallographic/materialographic labora-
tories.
26.5.3 OSHAOSHA Standards
In 1970, the Occupational Safety and Health Act was passed by the U.S. Congress, es-
tablishing NIOSHsee below andOSHA.
Occupational Safety andHealthAdministrationOSHA inthe U.S. Department of
Labor has issueda number of regulations standards covering occupational safety and
health in laboratories in general, these also covering the metallographic/material-
ographic laboratory.
In the following, the most important standards are described in short form, with
the important HazardCommunicationStandardinrelative detail.
Standard Title: Hazard Communication Standard
StandardNumber: 29CFR1910.1200
The Hazard Communication Standard HCS, sometimes called the Right to
Knowlawor HazCom, is a set of regulations rst promulgated in 1988 by the Ofce of
Occupational Safety and Health Administration OSHA. HCSs purpose is to ensure
that the hazards of workplace chemicals are evaluated, and that information on the
hazards is provided to employers and employees. Details of the standard are provided
in parts 1910.1200 of the Code of Federal Regulations CFR of Chapter XVII of Title 29
under the Department of Labor. HCS covers nearly all employers and is applicable to
most workoperations where hazardous materials are present.
Contents:
In short, the standard requires that every affected employer must establish a pro-
gram to inform the employees of the hazards associated with the materials in their
workplace. The programmust have ve maincomponents as follows:
WrittenHazardCommunicationProgramdocumentation
Identifying andkeeping aninventory of hazardous chemicals
Obtaining and keeping material safety data sheets MSDS on the identied haz-
ards
Ensuring that the hazardous materials are labeledwithname andhazard
Training employees on the standard, safety information, labeling, and protective
measures
Hazardous Chemicals/Materials
The HCS covers chemicals in all physical formsliquids, solids, gases, vapors, fumes,
and mistswhether they are contained or not. The hazardous nature of the chemical
and potential for exposure are the factors that determine whether a chemical is cov-
ered. If it is hazardous andthere is potential for exposure, the rule applies.
Written Program
Under the standard eachlaboratory employer must complete and keep a writtenHaz-
ard Communication Program. The written program describes how the requirements
for labels and other forms of warning, material safety data sheets MSDSs, and em-
ployee information and training are implemented in the workplace. It indicates who is
responsible for MSDSs, labels, warning signs, and training, as well as the location of
the inventory. MSDSs and other information and resources pertaining to hazardous
chemicals and safety measures. An inventory list of hazardous chemicals is required to
be maintainedas part of the writtenprogram.
Chemical Inventory
The person working in the laboratory needs to know about the hazards to be able to
protect oneself. The leader of the laboratory is responsible for establishing an inven-
tory of hazardous chemicals.
All potentially hazardous chemicals in containers should be registered and chemi-
cals possibly generated inwork operations should be included, including vapor, fumes,
dust, etc. In the inventory, information based on the labels and the MSDSs made avail-
able by the supplier of the chemical is stated.
MSDS
The role of the MSDS is to provide detailed information on each hazardous chemical,
including its potential hazardous effects, its physical andchemical characteristics, and
recommendations for appropriate protective measures. This information is useful for
designing protective programs, as well as informing the chemical user of the hazards.
MSDSs must be readily accessible to users when they are in their work areas. Some
laboratories keep the MSDSs in a binder in the individual work area or in a central
locationinthe department.
An MSDS should be available for each hazardous chemical used in the lab. The
MSDSmust be inEnglish. The MSDSshould be delivered by the supplier, and it should
include all of the information required under the rule. If an MSDSis not supplied auto-
matically it should be requested for. If an MSDS is obviously inadequate an appropri-
ately complete one shouldbe requested.
Employees shouldnot use or be exposedtoany chemicals for whichthe safety data
have not beenreviewedandappropriate safety measures implemented.
Labels
Containers of hazardous chemicals must be labeled, tagged, or marked with the iden-
tity of the material and appropriate hazard warnings. The original label must include
the identity of the material, appropriate hazard warnings, and the manufacturer name
and address. The identity used by the supplier may be a common or trade name, or a
chemical name. The hazard warning is a brief statement of the hazardous effects of the
chemical ammable, causes lung damage. Labels frequently contain other infor-
mation, such as precautionary measures do not use near open ame. Labels must
be legible andprominent.
Secondary Containers Label and Signs
If materials are transferred from the original container into other containers, these
must be labeledas well. Depending onthe employers writtenplan, the secondary labels
may be warning symbols, text, or use a numerical hazard rating system, such as HMIS
andNFPAsee Section26.2.
Large containers or storage units containing hazardous chemicals or mixtures
must also be labeled or have warning signs. It is strongly recommended that other
warning or caution signs be placed in the work areas to remind individuals of the haz-
ards andof the protective equipment that may be necessary inthe area.
Employee Information and Training
An employee working with hazardous chemicals must receive both information and
training onthe hazardcommunication.
Information and training may be done either by individual chemical, or by catego-
ries of hazards such as ammability or carcinogenicity. If there are only a fewchemi-
cals in the laboratory, each chemical may be discussed individually. Where there are
large numbers of chemicals, or the chemicals change frequently, training may be based
on the hazard categories e.g., ammable liquids, corrosive materials, carcinogens.
Employees must have access to the substance-specic information on the labels and
MSDSs.
The underlying purpose of the HCS is to reduce the incidence of chemical source
illnesses and injuries. In general, the most important aspects of training are to ensure
employees are aware that they are exposed to hazardous chemicals, that they know
howto read and use labels and material safety data sheets, and that, as a consequence
of learning this information, they are following the appropriate protective measures
e.g., personal protective equipment, safe procedures, engineering controls.
Frequently Asked Questions on HCS HAZCOM
HCS being an important standard, the answers to a number of questions can be of
interest.
What are the containers labeling requirements under HCS?
Under HCS, the manufacturer, importer, or distributor is required to label each con-
tainer of hazardous chemicals. If the hazardous chemicals are transferred into un-
marked containers, these containers must be labeled with the required information,
unless the container into which the chemical is transferred is intended for the immedi-
ate use of the employee whoperformedthe transfer.
Can MSDSs be stored in a computer to meet the accessibility requirements
of HCS?
If the employees work area includes the area where the MSDSs can be obtained, then
maintaining MSDSs on a computer would be in compliance. If the MSDSs can only be
accessed out of the employees work areas, then the employer would not be in compli-
ance withHCS.
When is the supplier required to distribute MSDSs?
Hazard information must be transmitted on Material Safety Data Sheets MSDSs that
must be distributed to the customer at the time of rst shipment of the product. The
Hazard Communication Standard also requires that MSDSs be updated by the chemi-
cal manufacturer or importer within three months of learning of new or signicant
information, regarding the chemicals hazardpotential.
What is considered proper training under HCS?
Employees are to be trained at the time they are assigned to work with a hazardous
chemical. The intent of this provision is to have information prior to exposure to pre-
vent the occurrence of adverse health effects. This purpose cannot be met if training is
delayeduntil a later date.
The training provisions of the HCS are not satised solely by giving the employee
the data sheets to read. An employers training programis to be a forumfor explaining
to employees not only the hazards of the chemicals in their work area, but also howto
use the information generated in the hazard communication program. This can be ac-
complished in many ways audiovisuals, classroominstruction, interactive video, and
should include an opportunity for employees to ask questions to ensure that they un-
derstandthe informationpresentedtothem.
Training need not be conducted on each specic chemical found in the workplace,
but may be conducted by categories of hazard e.g., carcinogens, acutely toxic agents
that are or may be encounteredby anemployee during the course of his duties.
Furthermore, the training must be comprehensible. If the employees receive job
instructions in a language other than English, then the training and information to be
conveyedunder the HCSwill alsoneedtobe conductedina foreignlanguage.
What are the requirements for refresher training or retraining a new hire?
Additional training is to be done whenever a new physical or health hazard is intro-
duced into the work area, not a newchemical. For example, if a newsolvent is brought
into the workplace, and it has hazards similar to existing chemicals for which training
has already been conducted, then no new training is required. As with initial training,
and in keeping with the intent of the standard, the employer must make employees
specically aware which hazard category i.e., corrosive, irritant, etc. the solvent falls
within. The substance-specic data sheet must still be available, and the product must
be properly labeled. If the newly introduced solvent is a suspect carcinogen, and there
has never been a carcinogenic hazard in the workplace before, then new training for
carcinogenic hazards must be conducted for employees in those work areas where em-
ployees will be exposed.
It is not necessary for the employer to retrain each new hire if that employee has
receivedprior training by a past employer, anemployee union, or any other entity. Gen-
eral information, such as the rudiments of the HCS could be expected to remain with
an employee from one position to another. The employer, however, maintains the re-
sponsibility to ensure that their employees are adequately trained and are equipped
with the knowledge and information necessary to conduct their jobs safely. It is likely
that additional training will be neededsince employees must knowthe specics of their
newemployers programs such as where the MSDSs are located, details of the employ-
ers in-plant labeling system, and the hazards of new chemicals to which they will be
exposed.
Do you need to keep MSDSs for commercial products such as Windex
and White-out?
OSHAdoes not require that MSDSs be provided to purchasers of household consumer
products when the products are used in the workplace in the same manner that a con-
sumer would use them, i.e., where the duration and frequency of use and therefore
exposure is not greater than what the typical consumer would experience. This ex-
emption in OSHAs regulation is based, not on the chemical manufacturers intended
use of his product, however, but on howit actually is used in the workplace. Employees
who are required to work with hazardous chemicals in a manner that results in a dura-
tion and frequency of exposure greater than what a normal consumer would experi-
ence have a right toknowabout the properties of those hazardous chemicals.
What are the requirements and limits to use generic MSDSs?
The requirements for MSDSs are found in paragraph g of the standard. MSDSs must
be developed for hazardous chemicals used in the workplace, and must list the hazard-
ous chemicals that are found in a product in quantities of 1 % or greater, or 0.1 % or
greater if the chemical is a carcinogen. The MSDS does not have to list the amount that
the hazardous chemical occurs inthe product.
Therefore, a single MSDScanbe developedfor the various combinations of chemi-
cals, as long as the hazards of the various mixtures are the same. This generic MSDS
must meet all of the minimum requirements found in HCS, including the name, ad-
dress, and telephone number of the responsible party preparing or distributing the
MSDSwhocanprovide additional information.
What is the application of HCS to an ofce environment?
Ofce workers who encounter hazardous chemicals only in isolated instances are not
covered by the rule. OSHAconsiders most ofce products such as pens, pencils, adhe-
sive tape to be exempt under the provisions of the rule, either as articles or as con-
sumer products. OSHA has previously stated that intermittent or occasional use of a
copying machine does not result in coverage under the rule. However, if an employee
handles the chemicals to service the machine, or operates it for long periods of time,
thenthe programwouldhave tobe applied.
Is an MSDS required for a nonhazardous chemical?
MSDSs that represent nonhazardous chemicals are not covered by the HCS. Para-
graph 29 CFR1910.1200 g 8 of the standard requires that the employer shall main-
tain in the workplace copies of the required MSDSs for each hazardous chemical, and
shall ensure that they are readily accessible during each work shift to employees when
they are in their work areas. OSHA does not require nor encourage employers to
maintain MSDSs for nonhazardous chemicals. Consequently, an employer is free to
discardMSDSs for nonhazardous chemicals.
Standard Title: Occupational Exposure to Hazardous Chemicals in
Laboratories
StandardNumber: 29CFR1910.1450
Scope and Application
The standardcovers all laboratories engagedinthe laboratory use of chemicals dened
as hazardous by this standard, generally, superseding provisions of all other health
standards except in specic instances. The obligation to maintain employee exposures
at or below the permissible exposure limits PELs specied in the air contaminants
standardandinsubstance specic standards is retained.
It does not apply to users of hazardous chemicals, whichdo not meet the denition
of laboratory use, and in such cases, the employer must comply with the relevant stan-
dardeventhoughuse occurs ina laboratory.
The standard does not apply for laboratory use of hazardous chemicals that pro-
vide no potential for employee exposure such as procedures using chemically impreg-
natedtest media andcommercially preparedtest kits.
Employee Exposure Determination
The employer must measure the employees exposure periodically to any substance
regulated by a standard which requires monitoring if there is reason to believe that
exposure levels for that substance routinely exceed the actionlevel or inthe absence of
an action level, the PEL. The employer must notify the employee of the results within
15working days after receipt of the monitoring results.
Chemical Hygiene Plan
Where hazardous chemicals are used a laboratory covered by this standard the em-
ployer must develop and carry out the provisions of a written Chemical Hygiene Plan
CHP. The CHP must include the necessary work practices, procedures, and policies
to ensure that employees are protected fromall potentially hazardous chemicals in use
in their work area. The plan must be available to employees, to employee representa-
tives, andtothe Assistant Secretary for Occupational Safety andHealth.
Employee Training and Information
The employer must provide employees with information and training to ensure that
they are aware of the hazards of the chemicals present intheir work area. This informa-
tion must be provided at the time of an employees initial assignment to a work area
where hazardous chemicals are present and prior to assignments involving new expo-
sure situations.
Employees must be informedof:
The contents of this standardandits appendices must be made available tothem
The locationandavailability of the employers Chemical Hygiene Plan
The permissible exposure limits for OSHA
Signs and symptoms associated with exposures to hazardous chemicals used in
the laboratory
The locationand availability of knownreference material onthe hazards, safe han-
dling, storage, anddisposal of hazardous chemicals foundinthe laboratory includ-
ing, but not limited to Material Safety Data Sheets MSDS received fromchemical
suppliers
Medical Consultation and Examinations
All employees who work with hazardous chemicals must be given the opportunity to
receive medical attention, including any follow-upexaminations, whichthe examining
licensed physician determines to be necessary under certain circumstances. Medical
examinations and consultants must be provided without cost to the employee, without
loss of pay, andat a reasonable time andplace.
The employer must provide certain information to the physician, including the
identity of the hazardous chemicals, a description of the conditions under which the
exposure occurred, and a description of the signs and symptoms of exposure that the
employee is experiencing.
Hazard Identication
Labels on incoming containers of hazardous chemicals must not be removed or de-
faced. MSDSs on incoming hazardous chemicals must be retained and made available
tolabemployees.
Respirator Use
Where the use of respirators is necessary to maintain exposure below permissible ex-
posure limits, the employer must provide, at no cost to the employee, the proper respi-
rator equipment.
Record Keeping
The employer must establish and maintain for each employee an accurate record of
any measurements taken to monitor employee exposure and any medical consultation
andexaminationincluding tests or writtenopinions.
Standard Title: List of Highly Hazardous Chemicals, Toxics and Reactives
StandardNumber: 29CFR1910.119AppA
The standard contains a listing of toxic and reactive highly hazardous chemicals
that present a potential for a catastrophic event at or above the treshold of quantity.
Chemical name, CAS number Chemical Abstract Service Number and Treshold
Quantity inPounds are statedinthe list.
Standard Title: Flammable and Combustible Liquids
StandardNumber: 29CFR1910.106.
The standard denes ammable and conbustible see Section 26.1.5 and
states the rules and regulations regarding safety and health, using ammable liquids in
general.
Standard Title: General Description and Discussion of the Levels of
Protection and Protective Gear
StandardNumber: 29CFR1910.120AppB
Scope and Application
The standard gives information about personal protective equipment PPE protection
levels, whichmay be usedtoassist employers incomplying withthe PPErequirements.
As required by the standard, PPE must be selected, which will protect employees
fromthe specic hazards, whichthey are likely toencounter during their workon-site.
Selectionof the appropriate PPEis a complex process, whichshouldtake into con-
sideration a variety of factors. Key factors involved in this process are identication of
the hazards, or suspected hazards; their routes of potential hazard to employees inha-
lation, skin absorption, ingestion, and eye or skin contact; and the performance of the
PPEmaterials and seams in providing a barrier to these hazards. The amount of pro-
tection provided by PPE will protect well against some hazardous substances and
poorly, or not at all, against others.
Standard Title: Availability of NIOSH Registry of Toxic Effects of Chemical
Substances RTECS non-mandatory.
StandardNumber: 29CFR1910.1020App. B
The standard applies to all employee exposure and medical records, and analyses
thereof, of employees exposed to toxic substances or harmful physical agents para-
graph b 2. The termtoxic substance or harmful physical agent is dened by para-
graph c 13 to encompass chemical substances, biological agents, and physical
stresses for which there is evidence of harmful health effects. The regulation uses the
latest printed edition of the National Institute for Occupational Safety and Health
NIOSH see below, Registry of Toxic Effects of Chemical Substances RTECS as one
of the chief sources of information as to whether evidence of harmful health effects
exists. If a substance is listed in the latest printed RTECS, the regulation applies to ex-
posure and medical records and analyses of these records relevant to employees ex-
posedtothe substance.
It is appropriate to note that the nal regulation does not require that employers
purchase a copy of RTECS, and many employers need not consult RTECS to ascertain
whether their employee exposure or medical records are subject to the rule. Employers
who do not currently have the latest printed edition of the NIOSH RTECS, however,
may desire to obtain a copy. The RTECS is issued in an annual printed edition as man-
dated by section 20 a 6 of the Occupational Safety and Health Act 29 U.S.C. 669 a
6.
26.5.4 National Institute for Occupational Safety and Health NIOSH
National Institute for Occupational Safety and Health NIOSH is, like OSHA estab-
lished according to the Occupational Safety and HealthAct of 1970. They are, however,
two distinct agencies with separate responsibilities, NIOSH is in the U.S. Department
of HealthandHumanServices.
NIOSHis the Federal agency responsible for conducting researchand making rec-
ommendations for the preventionof work-relateddisease andinjury.
NIOSH works with the Health Hazard Evaluation Program, investigating poten-
tially hazardous working conditions and with the NIOSH Publications Ofce supply-
ing informationonhazardous materials. NIOSHhas a number of other activities.
NIOSH Pocket Guide
NIOSH Pocket Guide to Chemical Hazards is a useful book that can be obtained from
NIOSH. It includes the following:
Chemical Names, synonyms, trade names, conversion factors, CAS, RTECS, and
DOTNumbers
NIOSHRecommendedExposure Limits NIOSH, RELS
Permissible Exposure Limits PELs
NIOSHImmediate Dangerous toLife andHealthvalues NIOSHIDLHs.
Aphysical descriptionof the agent withchemical andphysical properties
Measurement methods
Personal ProtectionandSanitationRecommendations
Respirator Recommendations
Information on Health Hazards including route, symptoms, rst aid, and target
organinformation.
RTECS Database
The Registry of Toxic Effects of Chemical Substances RTECS is a database of toxi-
cological information compiled, maintained, and updated by the NIOSH. RTECS
contains over 133 000 chemicals as NIOSH strives to fulll the mandate to list all
known toxic substances and the concentrations at which toxicity is known to oc-
cur.
RTECS is a compendium of data extracted from the open scientic literature.
The data are recorded in the format developed by the RTECS staff and arranged in
alphabetical order by prime chemical name. No attempt has been made to evaluate the
studies citedinRTECS. The user has the responsibility of making suchassessments.
26.5.5 International Chemical Safety Cards ICSCS
The International Chemical Safety Cards are worked out by an international group of
experts under The International Programme on Chemical Safety under the World
HealthOrganizationWHO.
The ICSCs are based on standard phrases, the criteria for which are given in the
Compilers Guide. A certain number of Cards are available in 22 languages and their
translationintoa further eight languages is on-going.
The rst edition of the Compilers Guide and ten series, representing over 900
Cards, have been published as hard copies in English, Spanish, Japanese, Chinese, and
Polish, and about 1300 Cards are available in electronic form. Cards in English are
available on the ILO Web site: www.ilo.org/public/english/protection/safework/cis/
products/icsc
An ICSC summarizes essential health and safety information on chemicals for
their use at the shop oor level by workers and employees in factories, agriculture,
construction, andother workplaces.
ICSCs are not legally binding documents, but consist of a series of standard
phrases, mainly summarizing health and safety information collected, veried, and
peer reviewed by internationally recognized experts, taking into account advice from
manufacturers andPoisonControl Centers.
The identication of the chemicals on the Cards is based on the UN numbers, the
Chemical Abstracts Service CAS number, and the Registry of Toxic Effects of Chemi-
cal Substances RTECS/NIOSH numbers. It is thought that the use of those three sys-
tems assures the most unambiguous method of identifying the chemical substances
concerned, referring as it does to numbering systems that consider transportation
matters, chemistry, andoccupational health.
ICSCs and Material Safety Data Sheets
Great similarities exist between the various headings of the ICSC and the manufactur-
ers Safety Data Sheet SDS or Material Safety Data Sheet MSDS of the International
Council of Chemical Associations. However, MSDSs and the ICSCs are not the same.
The MSDS, in many instances, may be very complex technically and too expensive for
shop oor use, and secondly it is a management document. The ICSCs, on the other
hand, set out peer-reviewed information about substances in a more concise and
simple manner. Although not a legal document, the ICSCis an authoritative document
emanating from WHO/ILO/UNEP. This is not to say that the ICSC should be a substi-
tute for an MSDS, nothing can replace managements responsibility to communicate
with workers on the exact chemicals, the nature of those chemicals used on the shop
oor and the risk posed in any given work place. Indeed, the ICSC and the MSDS can
even be thought of as complementary. If the two methods for hazard communication
can be combined, then the amount of knowledge available to the safety representative
or shopoor workers will be more thandoubled.
26.5.6 Environmental Protection Agency EPA
The U.S. Environmental Protection Agency is to protect human health and to safe-
guardthe natural environmentair, water, andlandwhichlife depends on.
EPA administrates important laws like Occupational Safety and Health Act and
Toxic Substances Control Act, both important in relation to metallographic/material-
ographic laboratories.
26.5.7 National Technical Information Service NTIS
The National Technical Information Service NTIS is the largest, central resource for
government-funded scientic, technical, engineering, and business information avail-
able inUnitedStates.
Toxic Substances Control Act TSCA Chemical Substances InventoryRevised
Inventory Synonym and Preferred Name File: This inventory list covers more than
65 000chemicals as denedunder TSCA.
26.5.8 American Conference of Government Industrial Hygienists ACGIH
The American Conference of Governmental Industrial Hygienists, Inc. ACGIH, is an
organization open to all practitioners in industrial hygiene, occupational health, envi-
ronmental health, or safety.
ACGIH publishes over 400 titles in occupational and environmental health and
safety. They are best known for their Treshold Limit Values publication that lists the
TLVs for over 700 chemical substances and physical agents, as well as 50 Biological
Exposure Indices for selectedchemicals.
26.5.9 National Toxicology Program NTP
The National Toxicology Programis an organization under U.S. Department of Health
andHumanServices DHHS tocoordinate toxicological testing programs.
NTPhas collectedhealthandsafety data onover 2000chemicals.
26.5.10 Agency for Toxic Substance and Disease Registry ATSDR
The Agency for Toxic Substances and Disease Registry ATSDR is an agency under
U.S. Department of HealthandHumanServices.
The mission is to prevent exposure and advise human health effects associated
withexposure tohazardous substances.
ATSDRTOXFAQs is a series of summaries about hazardous substances. Eachfact
sheet serves as a quickandeasy tounderstandguide, www.atsdr.cdc.gov/toxfaq.html.
26.5.11 National Fire Protection Association NFPA
The National Fire Protection Association NFPA is a nonprot organization that is re-
sponsible for over 300codes covering basic re safety, electricity, andother topics.
The NFPA704HazardIdenticationRatings Systemis describedinSection26.2.
26.5.12 National Paint and Coatings Association NPCAHMIS
The National Paint and Coatings Association NPCA has established a complete pro-
gram, HMIS, Hazardous Materials Identication System that helps employers com-
ply withOSHAs HazardCommunicationStandardHCS see Section26.2.
26.5.13 BSIISO
British Standards Institution is the independent national body responsible for prepar-
ing British Standards. BSI cooperates with ISOInternational Standard Organization
andEUEuropeanUnion.
The British Standard BS 7750 on Environmental Management has been used as
the basis for the standard, BS EN ISO 14001: 1996, Environmental Management Sys-
tems. This standard covers all sides of environmental management and connects to the
quality standardBSENISO9000: 2000.
The standard BS 8800: 1996, Guide to Occupational Health and Safety Manage-
ment Systems, puts emphasis on OHS management. Two standards are established
basedonthis standard:
OHSAS 18001: 1999, Occupational Health and Safety Management Systems
Specications.
OHSAS 18002: 2000, Occupational Health and Safety Management Systems.
Guidelines for the implementationof OHSAS18001.
An important factor in OHSAS 18001: 1999 is Risk Assessment dened as The
overall process of estimating the magnitude of risk anddeciding whether or not the risk
is tolerable or acceptable. Risk assessment involves three basic steps: 1 identify haz-
ards; 2 estimate the risk from each hazardthe likelihood and severity of harm; 3
decide if the riskis tolerable.
26.5.14 EU
The European Union EU European Community EC has established a number of
directives, covering occupational safety.
The directive 67/548/EECon dangerous substances is described further in Section
26.2.
26.6 Literature on Laboratory Safety
Literature can be seen in References of the Standard Guide on Metallographic Labora-
tory Safety E 2014 in the CD-ROMincluded with this manual see Section 26.1.8. In
addition the books by Petzow and Vander Voort Refs 2 and 9, Part I can be recom-
mended.
27
Literature
27.1 Books
THE BOOKS LISTED BELOW COVER THE FIELD OF METALLOGRAPHIC/
materialographic preparation and examination. They are intended as a supplement to
this bookandshouldnot be consideredas a complete list of books onthese subjects.
Amelinckx, S., Van Dyck, D., Van Landuyt, J., and Van Tendeloo, G., Handbook of Microscopy: Applications in
Materials Science, Solid-State Physics, andChemistry. Wiley-VCH, NewYork, N.Y., USA, 1997.
Beraha, E. andShipgler, B., Color Metallography, ASMMaterials Park, Ohio, USA, 1977.
Bjerregaard, L., Geels, K., Ottesen, B., and Rckert, M., Metalog Guide, Struers A/S, Copenhagen, Denmark,
2000.
Bouseld, B., Surface PreparationandMicroscopy of Materials, JohnWiley &Sons, Chichester, UK, 1992.
Bramtt, B. L. and Benscoter, A. O., Metallographers GuidePractices and Procedures for Iron and Steels, ASM
International, Metals Park, Ohio, USA, 2001.
Burgess, D. and Blanchard, R. A., Wafer Failure Analysis for Yield Enhancement, Accelerated Analysis, Half
MoonBay, California, USA, 2001.
Bhler, H. E. and Hougardy, H. P., Atlas of Interference Layer Metallography, Deutsche Gesellschaft fr Met-
allkunde, Oberursel, Germany, 1980.
Durand-Charre, M., Microstructure of Steels and Cast Irons, Springer-Verlag NewYork, Inc., NewYork, NY, USA,
2004.
Durand-Charre, M. and Durand-Charre, M., Microstructure of Superalloys, Taylor &Francis, Inc., Philadelphia,
PA, USA, 1998.
Elssner, G., Hoven, H., Kiessler, G., andWellner, P., Ceramics andCeramic Composites: Materialographic Prepara-
tion, Elsevier Science, Inc., NewYork, NY, USA, 1999.
Freund, J. E., Statistics: a First Course, 2nded., Prentice Hall, EnglewoodCliffs, NewJersey, USA, 1970.
Friel, J. J., et al., Practical Guide toImage Analysis, ASMInternational, Materials Park, Ohio, USA, 2000.
Handbook of Thermal Spray Technology, ASMInternational, Materials Park, Ohio, USA, 2004.
Higginson, R. L. and Sellars, C. M., Worked Examples in Quantitative Metallography, Maney Publishing, Cam-
bridge MA, USA, 2003.
Inoue, S. andSpring, K. R., VideoMicroscopy, PlenumPress, NewYork, NY, USA, 1997.
Kapitza, H. G., Microscopy fromthe Very Beginning, Carl Zeiss, Jena, Germany, 1994.
Metals Handbook, Metallography and Microstructures, Vol. 9, ASM International, Materials Park, Ohio, USA,
2004.
Petzow, G., Metallographic Etching, ASMInternational, Materials Park, Ohio, USA, 1999.
Ross, Boit, and Staab, edit., Microelectronics Failure Analysis, ASMInternational, Materials Park, Ohio, USA,
1999.
Rostoker, W. and Dvorak, J. R., Interpretation of Metallographic Structures, Elsevier Science, Inc., NewYork, NY,
USA, 1990.
Russ, J. C., The Image Processing Handbook, 3rded., CRCPress, Boca Raton, FL, USA, 1998.
Samuels, L. E., Metallographic Polishing by Mechanical Methods, ASMInternational, Materials Park, Ohio, USA,
2003.
Schumann, H. andOettel, H., Metallograe, Wiley-VCHVerlag, Weinheim, Germany, 2004 InGerman.
Tegart, Mc.G., The Electrolytic and Chemical Polishing of Metals in Research and Industry, Pergamon Press, Lon-
don, UK, 1959.
Tomer, A., Structure of Metals throughOptical Microscopy, ASMInternational, Materials Park, Ohio, USA, 1990.
Underwood, E. E., Quantitative Stereology, Addison-Wesley Publishing Company, Reading, MA, USA, 1970.
685
Vander Voort, G. V., Metallography Principles andPractice, ASMInternational, Materials Park, Ohio, USA, 1999.
Waschull, H., Prparative Metallographie, Wiley-VCHVerlag, Weinheim, Germany, 1993 InGerman.
Weck, E. and Leistner, E., Metallographic Instructions for Colour Etching by Immersion, Part I 1982, II 1983,
III 1986, Deutscher Verlag fr SchweisstechnikGmbH, Dsseldorf, Germany.
27.2 Periodicals
THE PERIODICALS STATED IN THIS LIST COVER THE FIELD OF METALLO-
graphic/materialographic preparation and interpretation, but it should not be consid-
ereda complete list of all periodicals covering these subjects.
Advanced Functional Materials, English/18 issues yearly, Wiley-VCH, P.O. Box 191161, D-69451, Weinheim, Germany.
Advanced Materials, English/24 issues yearly, Wiley-VCH, P.O. Box 191161, D-69451, Weinheim, Germany.
Advanced Materials and Processes, English/monthly, ASMInternational, Materials Park, OH44073, USA.
Advanced Engineering Materials, English/monthly, Wiley-VCH, P.O. Box 191161, D-69451, Weinheim, Germany.
Alloy Digest, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
Electronic Device Failure Analysis, English/quarterly, ASMInternational, Materials Park, OH44073, USA.
International Materials Reviews, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
JOM, English/monthly, TMS The Minerals, Metals and Materials Society, 184Thorn Hill Road, Warrendale, PA15086, USA.
Journal of Electronic Materials, English/monthly, TMS The Minerals, Metals and Materials Society, 184 Thorn Hill Road,
Warrendale, PA15086, USA.
Journal of Failure Analysis and Prevention, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
Journal of Materials Engineering and Performance, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
Journal of Phase Equilibria and Diffusion, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
Journal of the American Ceramic Society, English/monthly, American Ceramic Society, P.O. Box 6136, Westerville, OH43086-
6136, USA.
Journal of Thermal Spray Technology, English/quarterly, ASMInternational, Materials Park, OH44073, USA.
Materials Characterization, English/10 issues yearly, Elsevier Science Publishing Co. Inc., 655 Avenue of the Americas, New
York, NY10010, USA.
Metallurgical and Materials Transactions A, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
Metallurgical and Materials Transactions B, English/bimonthly, ASMInternational, Materials Park, OH44073, USA.
Praktische Metallographie/Practical Metallography, bilingual, German/English/monthly, Carl Hanser Verlag, Kolbergstrasse
22, 81679 Mnchen, Germany.
SlipLines, newsletter, English/quarterly, IMS International Metallographic Society, ASM International, Materials Park, OH
44073, USA.
Structure, English/German/French editions, twice a year, StruersA/S, Pederstrupvej 84, 2750 Ballerup, Denmark.
Welding Journal, English/monthly, AWSAmericanWelding Society, 550 N.W. LeJeunne Road, Miami, FL33126, USA.
Appendixes
Appendix I: Other Standards on Metallography/
Materialography
A NUMBER OF STANDARDS, OTHER THAN ASTM, COVERING METALLO-
graphy/materialography from ISO International Standard Organization and a num-
ber of important industrial countries are listedbelow. The list is not complete.
ISO standards/National standards: The national standards, which are local ver-
sions of ISOstandards, are not indicatedbelow.
CEN European Committee for Standardization is involved in European Stan-
dards EN, Technical Specications CEN TS, Technical Reports CEV TR and CEN
WorkAgreements CWA. All documents are suppliedby the national members of CEN.
ISO INTERNATIONAL STANDARD ORGANIZATION
ISO 643 SteelsMicrographic determination of the ferritic or
austenitic grain size
ISO 945 Cast ironDesignation of microstructure of graphite
ISO 1083 Spheroidal graphite cast ironsClassication
ISO 1463 Metallic and oxide coatingsMeasurements of thickness
Microscopical method
ISO 2064 Metallic and other inorganic coatingsDenitions and
conventions concerning the measurement of thickness
ISO 2624 Copper and copper alloysEstimation of average grain size
ISO 2639 SteelDetermination and verication of the effective depth
of carburized and hardened cases
ISO 3057 Nondestructive testingMetallographic replica techniques
of surface examination
ISO 3082 Iron oresSampling and sample preparation procedures
ISO 3085 Iron oresExperimental methods for checking the
precision of sampling, sample preparation and
measurement
ISO 3754 SteelDetermination of effective depth of hardening after
ame or induction hardening
ISO 3763 Wrought steelsMacroscopic methods for assessing the
content of nonmetallic inclusions
ISO 3887 SteelsDetermination of depth of decarburization
ISO 4499 Hard metalsMetallographic determination of
microstructure
ISO 4505 Hard metalsMetallographic determination of porosity and
uncombined carbon
ISO 4524-1 Metallic coatingsTest methods for electrodeposited gold
and gold alloy coatingsPart 1 Determination of coating
thickness
ISO 4967 SteelDetermination of content of nonmetallic inclusions
Micrographic method using standard diagrams
ISO 4968 SteelMicrographic examination by sulfur prints
Baumann method
ISO 4969 SteelMacroscopic examination by etching with strong
mineral acids
ISO 4970 SteelDetermination of total or effective thickness of thin
surface-treated layers
ISO 5949 Tool steels and bearing steelsMicrographic method for
assessing the distribution of carbides using reference
photomicrographs
ISO 6196 MicrographicsVocabularyPart 1: General terms
Chapter 27 Books 687
ISO 8036 Optics and photonicsMicroscopesImmersion liquids for
light microscopy
ISO 9042 SteelsManual point counting method for statically
estimating the volume fraction of a constituent with a point
grid
ISO 9220 Metallic coatingsMeasurement of coating thickness
Scanning electron microscope method
ISO 11567 Carbon breDetermination of lament diameter and
cross-sectional area
ISO 13520 Determination of ferrite content in austenitic stainless steel
castings
ISO 14250 SteelMetallographic characterization of duplex grain size
and distribution
ISO/TR 14321 Sintered metal materials, excluding hardmetals
Metallographic preparation and examination
ISO 14703 Fine ceramics advanced ceramics, advanced technical
ceramicsSample preparation for the determination of
particle size distribution of ceramic powders
ISO 14923 Thermal SprayingCharacterization and testing of
thermally sprayed coatings
ISO 16793 Nuclear fuel technologyGuide for ceramographic
preparation of UO
2
sintered pellets for microstructure
examination
ISO 17642-2 Destructive tests on welds in metallic materialsCold
cracking tests for weldmentsArc welding processesPart
2: Self-restraint tests
ISO 20160 Implants for surgeryMetallic materialsClassication of
microstructures for alphabeta titanium alloy bars
ISO 21227 Paints and varnishesEvaluation of defects on coated
surfaces using optical imagingPart 1: General guidance
FRANCE
NF A04-105 Iron and steel. Methods of determination of the
nonmetallic inclusion content of wrought steels. Part 1:
Macroscopic methods.
NF A04-106 Iron and steel. Methods of determination of content of
nonmetallic inclusions in wrought steel. Part II:
Micrographic method using standards diagrams.
NF A04-107 Iron and steel. Micrographic method of dtermination of the
nonmetallic inclusion content of unalloyed wire rod.
NF A04-108 Iron and steel. Characterization of sulde shapes in
structural steels with improved machinability using
standard diagrams. Micrographic method.
NF A04-110 Iron and steel. Wire rods of non-alloy general purpose steel
for wire drawing. Surface examination.
NF A04-111 Iron and steel. Micrographic determination of the extent of
decarburization of non-alloy high carbon steel wire rod.
NF A04-112 Iron and steel. Macrographic method of showing and
describing the chemical heterogeneity of effervescent steel
wire rod.
NF A04-113 Iron and steel. High carbon steel wire rod derived from
ingots. Macrographic method of showing and describing
the chemical heterogeneity.
NF A04-114 Iron and steel. High carbon continuous cast steel wire rod.
Macrographic method of showing and describing the
chemical heterogeneity.
A04-115 Iron and steel. Characterization of sulde shapes in
free-cutting steels using standards diagrams. Micrographic
method.
NF A04-203 Steel products. Determination of the effective hardening
after ame or induction hardening.
NF A04-204 Steel products. Determination of the total or conventional
thickness of surface hardened thin layers.
NF A04-503 Semi-products made from aluminum, copper, nickel and
their alloys. Determination of grain size. Aluminium and
aluminium alloys.
NF A05-150 Steel products. Techniques of micrographic examination.
NF A05-151 Steel products. Macrographic examination by sulfur print
Baumann method.
NF A05-152 Steel products. Macroscopic examination by etching with
strong mineral acids.
NF A05-153 Iron and steel. Macroscopic examination by means of
copper salt etching.
NF A05-154 Steel products. Metallographic replica techniques optical
examination.
NF A05-156 Iron and steel. Macrographic examination by sodium sulfur
print so-called lead print method.
A05-165 Steel products. Manual point counting method for
statistically estimating the volume fraction of a constituent
with a point grid.
NF A95-342 Powder metallurgy. Sintered materials including
hardmetals. Micrographic examination techniques.
NF EN 1321 Destructive tests on welds in metallic materials.
Macroscopic and microscopic examination of welds.
NF EN 12797 BrazingDestructive tests of brazed joints.
NF EN 24499 Hard metals. Metallographic determination of
microstructure.
NF EN 24505 Hard metals. Metallographic determination of porosity and
uncombined carbon.
XP ENV 10247 Micrographic examination of the nonmetallic inclusion
content of steels using standard pictures.
GERMANY
DIN V ENV
1071-5
Pre-standard Advanced technical ceramicsMethods of
test for ceramic coatingsPart 5: determination of porosity
DIN CEN/TS
1071-10
Advanced technical ceramicsMethods of test for ceramic
coatingsPart 10: determination of coating thickness by
cross sectioning
DIN EN 1321 Destructive tests of welds in metallic materials
macroscopic and microscopic examination of welds
DIN EN
2004-10
Aerospace seriesTest methods for aluminium and
aluminium alloy products; Part 10: preparation of
micrographic specimens for aluminium alloys
DIN EN 2007 Aerospace seriesTest methods for aluminium and
aluminium alloy productsmetallographic determination
of cladding thickness and copper diffusion in the cladding
for rolled products
DIN EN 3684 Aerospace seriesTest methodstitanium alloy wrought
productsdetermination of beta transus temperature;
metallographic method
DIN EN 10247 Micrographic examination of the nonmetallic inclusion
content of steels using standard pictures
DIN 50192 Determination of the depth of decarburization
DIN 50600 Testing of metallic materials; metallographic micrographs;
picture scales and formats
DIN 50601 Metallographic examination; determination of the ferritic
or austenitic grain size
DIN 50602 Metallographic examination; microscopic examination of
special steels using standard diagrams to assess the content
of non-metallic inclusions
DIN 54150 Nondestructive Testing Impression Methods for Surface
Examination
JAPAN
JIS H 0501 Methods for estimating average grain size of wrought
copper and copper alloys
JIS G 0551 SteelsMicrographic determination of the apparent grain
size
JIS G 0552 Method of ferrite grain size test for steel
JIS G 0553 Macrostructure detecting method for steel, Edition 1
JIS G 0555 Microscopic testing method for the non-metallic inclusions
in steel
JIS Z 6014 MicrographicsTest charts for digitizing image
Description and use in electronic imagery
UNITED KINGDOM
BS M 37 Method for the etch inspection of metallic materials and
components
BS EN 1321 Destructive test on welds in metallic materials.
Macroscopic and microscopic examination of welds
BS 4490 Methods for micrographic determination of the grain size
of steel
BS 5710 Macroscopic assessment of the nonmetallic inclusion
content of wrought steels
BS 6285 Macroscopic assessment of steel by sulfur print
BS 6286 Measurement of total or effective thickness of thin
surface-hardness layers in steel
BS 6479 Determination and verication of effective depth of
carburized and hardened cases of steel
BS 6481 Determination of effective depth of hardening of steel after
ame or induction hardening
BS 6533 Guide to microscopic examination of steel by etching with
strong acids
BS 6617 Determination of decarburization in steel. Methods for
determining decarburization by microscopic and
microhardness techniques
BS 7590 Method for statistically estimating the volume fraction of
phases and constituents by systematic manual point
counting with a grid
BS 7590 A Worksheet for the determination of volume fraction by
systematic manual point count
BS 10247 Micrographic examination of the nonmetallic inclusion
content of steels using standard pictures
BS EN 10328 Iron and steeldetermination of the conventional depth of
hardening after surface heating
93/7105316 DC Aerospace series. Test methods for aluminium and
aluminium alloy products. Metallographic determination of
cladding thickness and copper diffusion in the cladding for
rolled products prEN 2007
94/710839 DC Aerospace series. Test methods. Titanium alloy wrought
products. Determination of primary content. The point
count method and line intercept method prEN 3683
94/710840 DC Aerospace series. Test methods. Titanium alloy wrought
products. Determination of transus temperature.
Metallographic method prEN 3684
Appendix II: Other Standards on Hardness Testing
A number of standards, other than ASTM, covering hardness testing from ISO Inter-
national Standard Organization and a number of important industrial countries are
listedbelow. The list is not complete.
ISO standards/National standards: The national standards, which are local ver-
sions of ISOstandards, are not indicatedbelow.
CEN European Committee for Standardization is involved in European Stan-
dards EN, Technical Specications CEN TS, Technical Reports CEV TR and CEN
WorkAgreements CWA. All documents are suppliedby the national members of CEN.
ISO International Standard Organization
A number of standards covering hardness testing fromISOare listed below. The list is
not complete.
ISO INTERNATIONAL STANDARD ORGANIZATION
ISO 48 Rubber, vulcanized or thermoplasticDetermination of
hardness hardness between 10 IRHD and 100 IRHD
ISO 3738-1 Hard metalsRockwell hardness test scale APart 1:
Test method
ISO 3738-2 Hard metalsRockwell hardness test scale APart 2:
Preparation and calibration of standard test blocks
ISO 3878 Hard metalsVickers hardness test
ISO 4384-1 Plain bearingsHardness testing of bearing metalsPart
1: Compound materials
ISO 4384-2 Plain bearingsHardness testing of bearing metalsPart
2: Solid materials
ISO 4498 Sintered metal materials, excluding hardmetals
Determination of apparent hardness and microhardness
ISO 4498-1 Sintered metal materials, excluding hardmetals
Determination of apparent hardnessPart 1: Materials of
essentially uniform section hardness
ISO 4498-2 Sintered metal materials, excluding hardmetals
Determination of apparent hardnessPart 2:
Case-hardened ferrous materials, surface enriched by
carbon or carbon and nitrogen
ISO 4507 Sintered ferrous materials, carburized or carbonitrided
Determination and verication of hardening depth by a
microhardness test
ISO 4516 Metallic and other inorganic coatingsVickers and Knoop
microhardness tests
ISO 4545 Metallic materialsHardness testKnoop test
ISO 4546 Metallic materialsHardness testVerication of Knoop
hardness testing machines
ISO 4547 Metallic materialsHardness testCalibration of
standardized blocks to be used for Knoop hardness testing
machines
ISO 6506-1 Metallic materialsBrinell hardness testPart 1: Test
method
ISO 6506-2 Metallic materialsBrinell hardness testPart 2:
Verication and calibration of testing machines
ISO 6506-3 Metallic materialsBrinell hardness testPart 3:
Calibration of reference blocks
ISO 6507-1 Metallic materialsVickers hardness testPart 1: Test
method
ISO 6507-2 Metallic materialsVickers hardness testPart 2:
Verication of testing machines
ISO 6507-3 Metallic materialsVickers hardness testPart 3:
Calibration of reference blocks
ISO 6508-1 Metallic materialsRockwell hardness testPart 1: Test
method scales A, B, C, D, E, F, G, H, K, N, T
ISO 6508-2 Metallic materialsRockwell hardness testPart 2:
Verication and calibration of testing machines scales A,
B, C, D, E, F, G, H, K, N, T
ISO 6508-3 Metallic materialsRockwell hardness testPart 3:
Calibration of reference blocks scales A, B, C, D, E, F, G,
H, K, N, T
ISO 9015-1 Destructive test on welds in metallic materialsHardness
testingPart 1: Hardness test on arc welded joints
ISO 9015-2 Destructive tests on welds in metallic materialsHardness
testingPart 2: Microhardness testing of welded joints
ISO 9385 Glass and glass-ceramicsKnoop hardness test
ISO 14271 Vickers hardness testing of resistance spot, projection and
seam welds low load and microhardness
ISO 14577-1 Metallic materialsInstrumented indentation test for
hardness and materials parametersPart 1: Test method
hardness and materials parametersPart 2: Verication
and calibration of testing machines
hardness and materials parametersPart 3: Calibration of
reference blocks
ISO 18571 Rubber, vulcanized or thermoplasticHardness testing
Introduction and guide
France
NF A95-329 Powder metallurgy. Sintered metal materials excluding
hardmetals. Measurement of Vickers microhardness
NF A95-348 Powder metallurgy. Sintered ferrous materials, carburized
or carbonitried. Determination of effective case depth by
the Vickers microhardness testing method.
Germany
DIN EN 1043-2 Destructive test on welds in metallic materialsHardness
testPart 2: Micro hardness testing on welded joints
DIN CEN/TS
1071-7
test for ceramic coatingsPart 7: Determination of
hardness and Youngs modulus by instrumented
indentation testing
DIN CEN/TS
1071-8
test for ceramic coatingsPart 8: Rockwell indentation
test for evaluation of adhesion
Japan
JIS Z 2255 Method for ultra-low loaded hardness test
JIS Z 2255 Method for ultra-low loaded hardness test
JIS R 1623:1995 Testing method for Vickers hardness of ne ceramics at
elevated temperatures
JIS B 7724:1999 Brinell hardness testVerication of testing machines
JIS B 7726 Rockwell hardness testVerication of testing machines
JIS B
7727:2000
Shore hardness testVerication of testing machines
JIS B 7730 Rockwell hardness testCalibration of reference blocks
United Kingdom
BS DD ENV
843-4
Advanced technical ceramicsmonolithic ceramics
mechanical properties at room temperaturePart 4.
Vickers, Knoop and Rockwell supercial hardness tests
BS 1881 P 202 Recommendations for surface hardness testing by rebound
hammer
BS 2782 P3
METH 3665 C
Determination of Rockwell hardness
BS 3900-E12.1 Methods of test for paintsdetermination of Knoop
hardness by measurement of the indentation length using
a microscope
BS 4443 P2 Method 7, indentation hardness tests
BS 5411 P6 Vickers and Knoop microhardness tests
BS 5600 P4 S4.5 Powder metallurgical materials and productsmethods of
testing and chemical analysis of hardmetalsRockwell
hardness test scale A
BS 6431 P13 Method for determination of scratch hardness of surface
according to Mohs
BS 6617 Determination of decarburization in steel. Method for
determining decarburization by microscopic and
micro-hardness techniques
BS 7442 P3 S3.2 Determination of Shore hardness
BS EN 23878 HardmetalsVickers hardness test
BS EN 24428-1 Sintered metal materials, excluding hardmetals
determination of apparent hardnessPart 1. Materials of
essentially uniform section hardness
Appendix III: Hardness Conversion Tables for Metals E 140
IncludedonCD-Rominbackof this book.
Appendix IV: SI Quick Reference Guide: International System of
Units SI
IncludedonCD-Rominbackof this book.
Glossary
Abrasion The process of rubbing, grinding, or wearing away by the
use of abrasives; a roughening or scratching of a surface due
to abrasive wear [1].
Abrasive A substance capable of removing material from another
substance in machining, abrasion, or polishing that usually
takes the form of several small, irregular shaped particles of
hard material [1].
Abrasive disk (1) Grinding wheel mounted on a steel plate, with the
exposed flat side being used for grinding. (2) Grinding disk
with a layer of abrasive product [1].
Abrasive paper See Grinding paper.
Abrasive wet cutting Cutting method for almost all solid materials using
mechanical friction and wear with abrasives bonded in a
cut-off wheel (similar to grinding) [3].
Achromatic Literally, color-free. A lens or prism is said to be achromatic
when corrected for two colors. The remaining color seen in
an image formed by such a lens is said to be secondary
chromatic aberration [2]. See Achromatic objective.
Achromatic objective An objective that is corrected chromatically for two colors,
and spherically for one, usually in the yellow-green part of
the spectrum [2].
Acid A chemical substance that yields hydrogen ions H
+
when
dissolved in water gives a pH of less than 7 [1]. See also
Base.
Age hardening Hardening through aging, usually after rapid cooling or cold
working [1]. See also Precipitation hardening.
Aging A change in the property of certain metals and alloys that
occurs at room temperature or slightly elevated
temperatures, after hot working or heat treatment, or after
cold working. The aging is usually due to phase changes
(precipitation) [1]. See also Precipitation hardening.
Air-hardening steel A steel containing sufficient carbon and other alloying
elements to harden fully during cooling in air or other
gaseous media from a temperature above its transformation
range. Same as self-hardening steel [1].
Alloy A substance having metallic properties and being composed
of two or more chemical elements of which at least one is an
elemental metal [1].
Alloying element An element added to a metal (and which remains within the
metal) to effect changes of properties [1].
Alloy steel Steel containing significant quantities of alloying elements
(other than carbon and the commonly accepted amounts of
manganese, copper, silicon, sulfur, and phosphorus) to
improve the mechanical properties [1].
Alpha brass Solid solution phase of one or more alloying elements in
copper and having the same crystal lattice as copper [2].
Alpha iron Fe Solid phase of pure iron [2].
Amalgam Alloy with mercury and one or more other metals [3].
Amorphous Not having a crystal structure; noncrystalline [1].
695
Anisotropy Characterized by having different values of a property in
different crystallographic directions [1].
Annealing Heating to and holding metals and alloys at a suitable
temperature followed by cooling at a suitable rate, used
primarily to soften metals, but also to simultaneously
produce desired changes in properties or in microstructure
[3].
Anode Electrode where electrons leave (current enters) an
operating system (battery, X-ray tube, electrolytic cell) [3].
See also Cathode.
Anode corrosion The dissolution of a metal acting as an anode [3].
Anodic etching See Electrolytic etching.
Anvil effect The effect caused by use of too high a load, or when testing
the hardness of too thin a specimen, resulting in a bulge or
shiny spot on the underside of the specimen [2].
Aperture, optical The working diameter of a lens or a mirror [2].
Apochromatic
objective
An objective with longitudinal chromatic correction for red,
green, and blue, and spherical chromatic correction for
green and blue. This is the best choice for high resolution or
color photomicrography [2].
Arc cutting A group of cutting processes that melts the metals to be cut
with the heat of an arc between an electrode and the base
material [1].
Artifact A false microstructural feature that is not an actual
characteristic of the specimen; it may be present as a result
of improper or inadequate preparation, handling methods,
or optical conditions for viewing [2].
Attack polishing Simultaneous etching and mechanical polishing by adding a
weak etching solution to the polishing compound [1]. See
also Chemical mechanical polishing.
Austenite A face-centered cubic solid solution of carbon or other
elements in gamma iron [2].
Austenitic steel An alloy steel whose structure is austenitic at room
temperature [1].
Automatic image
analysis
A device which can be programmed to detect and measure
features of interest in an image. It may include accessories
such as automatic focus and an automatic traversing stage to
permit unattended operation [2].
Bainiteupper,
lower, intermediate
Metastable microstructure or microstructures resulting from
the transformation of austenite at temperatures between
those which produce pearlite and martensite. These
structures may be formed on continuous (slow) cooling if
the transformation rate of austenite to pearlite is much
slower than that of austenite to bainite. Ordinarily, these
structures may be formed isothermally at temperatures
within the above range by quenching austenite to a desired
temperature and holding for a period of time necessary for
transformation to occur. If the transformation temperature
is just below that at which the finest pearlite is formed, the
bainite (upper bainite) has a feathery appearance. If the
transformation temperature is just above that at which
martensite is produced, the bainite (lower bainite) is
acicular, resembling slightly tempered martensite. At the
higher resolution of the electron microscope, upper bainite
is observed to consist of plates of cementite in a matrix of
ferrite. These discontinuous carbide plates tend to have
parallel orientation in the direction of the longer dimension
of the bainite areas. Lower bainite consists of ferrite needles
containing carbide platelets in parallel array cross-striating
each needle axis at an angle of about 60. Intermediate
bainite resembles upper bainite; however, the carbides are
smaller and more randomly oriented [2].
Banded structure
banding
Alternate bands parallel with the direction of working
resulting from the elongation of segregated areas [2].
Band saw Mechanical cutting method using an endless steel saw blade.
Base A chemical substance that yields hydroxyl ions OH
, when
dissolved in water gives a pH of more than 7 [1].
Base metal (1) After welding, that part of the metal which was not
melted. (2) A metal that readily oxidizes, or that dissolves to
form ions [1]. See also Noble metal.
Beilby layer A layer of amorphous or amorphous-like character
developed on the surface of a specimen during mechanical
polishing. Theory by G. Beilby, but later research has shown
that the layer does not exist.
Beta structure Structurally analogous body-centered cubic phases (similar
to beta brass), or electron compounds, that have ratios of 3
valence electrons to 2 atoms [2].
Binder Cementing medium holding together mixtures of particles
or powder [3].
Blow torch Method for cutting metal using an acetylen burner, with the
possibility of adding an extra flow of oxygen, melting, and
blowing away the material. Also called oxyacetylen torching.
Bond The material that binds the abrasive in a cut-off wheel and in
other abrasive products.
Glossary 697
Brass Alloy consisting of copper (over 50 %) and zinc, to which
small amounts of other elements may be added [3].
Brighteld
illumination
For reflected light, the illumination which causes specularly
reflected surfaces normal to the axis of a microscope to
appear bright. For transmission electron microscopy, the
illumination of an object so that it appears on a bright
background [2].
Brinell hardness
testing
Hardness test performed by forcing a hard steel or tungsten
carbide ball of specified diameter into a material [3].
Brittleness The tendency of a material to fracture without first
undergoing significant plastic deformation [1]. See also
Ductility.
Bronze Copper-tin alloy with or without small amounts of other
alloying elements such as phosphorus and zinc [3].
Burning
metallography/
materialography
Can occur in cutting and grinding, when sufficient heat is
generated on the surface of the work piece to cause
discoloration or a change of the microstructure by
tempering or hardening [1].
Calibration (1) The act or process of determining the relationship
between a set of standard units of measure and the output
of an instrument or test procedure. (2) The graphical or
mathematical relationship relating the desired property
(expressed in a standard unit of measure such as
micrometres or Kg/ mm
2
) to the instrument output
(instrument units such as filar divisions or pixels) [2].
Carbide A compound of carbon with one or more elements, which,
in customary formulation, are considered as being more
positive than carbon [2].
Carbide tools Cutting or forming tools, usually made of tungsten, titanium,
tantalum, or niobium carbides or a combination of them in
a matrix of cobalt, nickel, or other metals. Carbide tools are
characterized by high hardness and compressive strength
and may be coated to improve wear resistance [1].
Carbon steel Steel containing carbon up to 2 % [3].
Carbonitriding A case-hardening process by which a suitable ferrous metal
is heated in a gaseous atmosphere. Through the gas, the
metal surface will absorb carbon and nitrogen by diffusion
and form a very hard compound layer [1].
Carburizing Absorption and diffusion of carbon into solid ferrous alloys
by heating to a temperature usually above Ac
3
, in contact
with a suitable carbonaceous material. A form of case
hardening [1]. See also Case hardening.
Case In a ferrous alloy, the outer portion that has been made
harder than the inner portion as a result of altered
composition, or structure, or both, from treatments such as
carburizing, nitriding, and induction hardening [2]. See also
Core.
Case hardening A generic term covering several processes applicable to steel
that change the chemical composition of the surface layer
by absorption of carbon, nitrogen, or a mixture of the two
by diffusion. It is also called carburizing, nitriding,
carbonitriding, cyaniding, nitrocarburizing, and quench
hardening [1].
Cast iron Generic term of a large family of cast ferrous alloys
containing 2.54 % carbon and about 13 % silicon. The
carbon content exceeds the solubility of carbon in austenite
that exists at the eutectic temperature, which is usually more
than 2 % [3].
Cast structure The structure, on a macroscopic or microscopic scale, of a
casting [2]. See also Dendrites.
Cathode Electrode where the electrons enter (current leaves) an
operating system [3]. See also Anode.
Cemented carbides
sintered carbides
Material made by pressing and sintering a powder of one or
more metallic carbides with a small amount of metal
(cobalt) serving as a binder [1].
Cementite A very hard and brittle compound of iron and carbon
corresponding to the empirical formula Fe
3
C. It is
commonly known as iron carbide and possesses an
orthorhombic lattice. In plain-carbon steels some of the
iron atoms in the cementite lattice are replaced by
manganese, and in alloy steels by other elements such as
chromium or tungsten. Cementite will often appear as
distinct lamellae or as spheroids or globules of varying size
in hypo-eutectoid steels. Cementite is in metastable
equilibrium and has a tendency to decompose into iron and
graphite, although the reaction rate is very slow [2].
Ceramic Inorganic, nonmetallic material with crystalline and
noncrystalline structures (for instance: metal carbides,
oxides, nitrides, and borides are ceramics) [3].
Cermets Powder metallurgy product consisting of ceramic particles
bonded with metal [1].
CG iron Same as compacted graphite cast iron [1]. See also
Compacted cast iron.
Chemical deposition Precipitation of a metal from solutions of its salts through
the introduction of another metal or reagent to the solution
[1].
Chemical etching Develops the microstructure by using an electrochemical
process, which takes advantage of the differences in the
electrochemical potentials of the various constituents in the
structure [3].
Chemical polishing Improving the surface luster of a metal by chemical
treatment [1]. See also Chemical mechanical polishing.
Glossary 699
Chemical
mechanical
polishing
Using a combination of a chemical solution (usually an
etchant) with an oxide suspension on a polishing cloth,
resulting in a scratch free surface. Mainly used for very soft
or ductile metals [3]. See also Oxide polishing.
Chips Pieces of material removed from a work piece by cutting
tools or by an abrasive medium [3].
Clad metal A composite metal containing two or three layers that have
been bonded together. The bonding may have been
accomplished by co-rolling, welding, casting, heavy chemical
deposition, or heavy electroplating [1].
Clay Earthy or stony mineral aggregate, which is plastic when
sufficiently pulverized and wetted, rigid and dry, and
vitreous when fired at a sufficiently high temperature [3].
Cold etching Reveals the microstructure at room temperature and below
[4].
Cold rolled sheet Sheets of metal made by feeding metal through mill rolls at
room temperature [3].
Cold worked
structure
A microstructure resulting from plastic deformation of a
metal or alloy below its recrystallization temperature [1].
Combined carbon That part of the total carbon in steel or cast iron that is
present as other than free carbon [1]. See also Free carbon.
Comet tails Artifact in the form of unidirectional scratches developed by
mechanical polishing of a metallographic/materialographic
surface.
Compacted graphite
cast iron
Cast iron having a graphite shape intermediate between the
flake form typical of gray cast iron and the spherical form of
fully spherulitic cast iron. Also known as CG iron [1].
Component One of the independently variable substances by means of
which the composition of each phase of a system of
heterogeneous equilibrium may be described completely;
usually an element, or a compound that remains
undissociated throughout the range of temperature and
pressure concerned [2].
Composite material A heterogeneous, solid structural material consisting of two
or more distinct components that are mechanically or
metallurgically bonded together (such as a cermet, or boron
wire embedded in a matrix of epoxy resin) [1]. See also
Cermet.
Condenser A term applied to lenses or mirrors designed to collect,
control, and concentrate radiation in an illumination system
[2].
Constant feed speed In cutting: Cutting principle where the movement of the
specimen or the cut-off wheel is kept constant throughout
the cutting process. This cutting principle is preferred to the
principle of Constant force as it will produce the least
deformation possible while still achieving the shortest
cutting times [3]. See also Constant force.
Constant force In cutting: Cutting principle where the force applied is kept
constant throughout the cutting process. Constant force can
produce damage to the sample especially at sample entry
and exit [3].
Constituent A phase, or combination of phases, which occurs in a
characteristic configuration in an alloy microstructure [2].
Contamination
metallography/
materialography
(1) Debris from grinding or dust from the lab environment
contaminating a polishing cloth resulting in scratches of the
specimen surface. (2) Material from a source other than the
specimen itself, which is deposited on the specimen surface
during preparation [3].
Continuous phase The phase forming the matrix or background in which other
phases may be dispersed as isolated units [2].
Controlled etching Electrolytic etching with selection of suitable etchant and
voltage, resulting in a balance between current and dissolved
ions [4].
Conversion,
hardness
The exchange of a hardness number determined by one
method for an equivalent hardness number of a different
scale [2].
Coolant See Cutting uid.
Core (1) Case hardeninginterior portion of unaltered
composition, or microstructure, or both, of a case-hardened
steel article. (2) Clad productsthe central portion of a
multilayer composite metallic material [2].
Corrosion Deterioration of a metal by chemical or electrochemical
reaction with its environment [1].
Corrosion
embrittlement
The chemical or electrochemical reaction between a
material, usually a metal, and its environment that produces
a deterioration of the material and its properties [1].
Corrosion fatigue Cracking produced by the combined action of repeating and
fluctuating stress and a corrosive environment [1].
Coupon A piece of material especially made for testing. Known from
printed circuit boards, where a coupon is made together
with the board.
Creep Time-dependent strain occurring under stress [1].
Crystal A solid composed of atoms, ions, or molecules arranged in a
pattern which is periodic in three dimensions [2].
Crystallite A crystalline grain not bounded by habit planes [2].
Cut-off wheel Abrasive wheel consisting of an abrasive in a bond for
cutting any material or part [3].
Cutting
metallography/
materialography
Sectioning of a piece of material to obtain a specimen [3].
See also Cut-off wheel.
Cutting uid Fluid used to cool a work piece, wash chips away, and
improve surface finish and cut-off wheel lifetime [3].
Glossary 701
Cutting speed The linear or peripheral speed of relative motion between
the tool and work piece in the principal direction of cutting
[1].
Darkeld
illumination
The illumination of an object such that it appears
illuminated with the surrounding field dark. This results
from illuminating the object with rays of sufficient obliquity
so that none can enter the objective directly. As applied to
electron microscopy, the image is formed using only
electrons scattered by the object [2].
Decarburization Loss of carbon from the surface of a carbon-containing alloy
due to a reaction with one or more chemical substances in a
medium that contacts the surface. Decarburization may be
either (1) partial. That is, where carbon content is less than
the unaffected interior but greater than the room
temperature solubility limit of carbon in ferrite or (2)
complete. That is, where carbon content is less than the
solubility limit of carbon in ferrite so that only ferrite is
present [2].
Deep drawing Forming of deeply recessed parts by means of plastic flow of
the material [1].
Deep etching Macroetching; etching preliminary to macro-examination,
intended to develop gross features such as segregation, grain
flow, cracks, or porosity [2]. See also Macroetching.
Deformation
metallography/
materialography
Plastic deformation, which may also be referred to as cold
work, can result in subsurface defects after grinding,
lapping, or polishing. Remaining plastic deformation can
first be seen after etching. Plastic deformation (deformed
layer) is an artifact that has to be removed during sample
preparation [3].
Deformation bands Bands produced within individual grains during cold
working which differ variably in orientation from the matrix
[2].
Dendrites Crystals, usually formed during solidification or sublimation,
which are characterized by a tree-like pattern composed of
many branches; pine-tree or fir-tree crystals [2].
Depth of eld The depth or thickness of the object space that is
simultaneously in acceptable focus [2].
Diamond polishing Polishing using diamond as abrasive. Removes scratches
introduced during fine grinding. Makes the specimen
suitable for microscopic observation [3]. See also Final
polishing, Polishing.
Diamond wheel A grinding wheel in which crushed and sized industrial
diamonds are held in a resinoid, metal, or vitrified bond [1].
Diaphragm A fixed or adjustable aperture in an optical system.
Diaphragms are used to intercept scattered light, to limit
field angles, or to limit image-forming bundles or rays [1].
Differential
interference contrast
illumination DIC
A microscopical technique employing a beam-splitting
double-quartz prism; that is a modified Wollaston prism
placed ahead of the objective with a polarizer and analyzer
in the 90 crossed positions. The two light beams are made
to coincide at the focal plane of the objective, thus rendering
height differences visible as variations in color. The prism
can be moved, shifting the interference image through the
range of Newtonian colors [2].
Diffraction (1) A modification which radiation undergoes, as in passing
by the edge of opaque bodies or through narrow slits, in
which the rays appear to be deflected. (2) Coherent
scattering of X-radiation by the atoms of a crystal which
necessarily results in beams in characteristic directions.
Sometimes called reflection. (3) The scattering of electrons,
by any crystalline material, through discrete angles
depending only on the lattice spacings of the material and
the velocity of the electrons [2].
Diffusion The spontaneous movement of atoms or molecules to new
sites within a material [1].
Direct cut
metallography/
materialography
Cutting mode in which the cut-off wheel cuts directly
through the work piece; also called chop cutting [3].
Dislocation A linear imperfection in a crystalline array of atoms [1].
Dislocation etching Reveals exit point of dislocations on the specimen surface
[4].
Dissolution etching Reveals the microstructure by surface removal [4].
Double etching Two etchants are used sequentially; the second one will
accentuate a particular microstructural feature [4].
Drawing Forming recessed parts of metal by pressing them in or
through a die. Reducing cross section of a wire or tube by
pulling it through a die [1].
Drop etching Placing a drop of an etchant on a selected area of the
specimen surface to develop the microconstituents [4].
Dry etching Develops the microstructure by gaseous exposure [4].
Ductile cast iron A cast iron that has been treated while molten with an
element such as magnesium or cerium to induce the
formation of free graphite as nodules or spherulites, which
imparts a measurable degree of ductility to the cast metal.
Also known as nodular cast iron, cast iron with spheroidal
graphite and SG iron [1].
Ductility Ability of a material to deform plastically without fracturing,
measured by elongation or reduction of area in a tensile test
[1]. See also Brittleness.
Duplex
microstructure
A two-phase structure [2].
Dye penetrant Color spray used in nondestructive testing to find cracks in
surface of parts [3].
Glossary 703
Elastic deformation Change of dimensions of a piece of material under stress.
Upon release of stress original dimensions are restored
again (example: elastic band which takes its original shape
after it has been stretched) [3].
Elasticity Ability of a solid to deform in direct proportion to and in
phase with increases or decreases in applied force [3].
Electrical discharge
machining EDM
Removal of stock from an electrically conductive material by
rapid, repetitive spark discharge through a dielectric fluid
flowing between the work piece and a shaped electrode [1].
Electrolyte Liquid, most often a solution, that will conduct an electric
current [1].
Electrolytic cell An assembly consisting of a vessel, electrodes (anode and
cathode) and an electrolyte in which electrolysis can be
carried out [1].
Electrolytic etching Development of microstructure by selective dissolution of
the polished surface under application of a direct current
[1]. Also called anodic etching.
Electrolytic
polishing
A metallographic preparation procedure where metal is
preferentially dissolved from high points on an anodic
surface by passage of an electric current through a
conductive bath, to produce a specular reflecting surface.
Used as an alternative to mechanical polishing [2].
Electron microscopy The study of materials by means of the electron microscope
[2]. See also SEM and TEM.
Embedded abrasives Loose abrasive particles pressed into the surface of a
specimen. This happens mainly with soft or ductile
materials, or both. Abrasives can be embedded when using a
small abrasive particle size, the grinding or polishing cloth
used has a low resilience or a lubricant with a low viscosity
is used or a combination of these conditions takes place [3].
Equiaxed grain A polygonal crystallite, in an aggregate, whose dimensions
are approximately the same in all directions [2].
Equilibrium diagram A graphical representation of the temperature, pressure, and
composition limits of phase fields in an alloy system, as they
exist under conditions of complete equilibrium [1].
Etchant Chemical substance or mixture used for etching [1].
Etch gures Markings formed on a crystal surface by etching or chemical
solution and usually related geometrically to the crystal
structure [2].
Etching Controlled preferential attack on a metal surface for the
purpose of revealing structural details [2].
Eutectic Phase consisting of intermixed solid constituents formed by
a eutectic reaction, (pearlite=ferrite end cementite). The
number of solids being the same as the number of
components in the system [3].
Eutectic structure The structure resulting when an alloy has passed through a
eutectic equilibrium upon freezing [2].
Exogenous
inclusions
A nonmetallic constituent produced by entrapment of
foreign material in the melt [2]. See also Inclusions,
Nonmetallic inclusions.
Eyepiece The lens system used in an optical instrument for
magnification of the image formed by the objective [2].
Fatigue Process by which repeated or fluctuating stress, or both,
leads to fracture [3].
Feed speed Rate by which a tool or cut-off wheel advances along or into
the surface of a work piece [3].
Ferrite Designation commonly assigned to alpha iron containing
alloying elements in solid solution. Increasing carbon
content markedly decreases the high-temperature limit of
equilibrium [2].
FG Fine Grinding. Reduces surface roughness of a specimen to
a degree that is suitable for polishing [3].
Field The portion of the object in view [2].
Field metallography Metallographic techniques carried out in the field when the
part or component is too large to bring to a metallographic
laboratory or a specimen cannot be removed [1].
Filar An eyepiece equipped with a fiducial line in its focal plane,
which is movable by means of a calibrated micrometre
screw, in order to make accurate measurements of length
[2].
Filler Material used to increase the bulk of a product without
adding to its effectiveness in functional performance [3].
Final polishing The final step in a specimen preparation process producing
a surface suitable for microscopic examination.
Flame spraying Coating technique in which the coating material is fed as
wire or powder into a flame and sprayed in the molten state
against the surface to be coated [3].
Flow lines A fiber pattern, frequently observed in wrought metal, which
indicates the manner in which the metal flowed during
deformation [2].
Fluorescent screen A sheet of material which emits visible light when exposed to
invisible radiation [2].
Foil A thin sheet of a material, usually a metal, not exceeding
0.13 mm 0.005 in. in thickness [2].
Forging Process of plastically deforming metal, usually hot, into a
desired shape with compressive force, with or without dies
[1].
Formability
workability,
drawability
Relative ease with which a metal can be shaped through
plastic deformation [1].
Fractography Description of fractures with macrographs 25 and
micrographs at high magnification 25 from the optical
microscope and the SEM [3].
Glossary 705
Fracture test Test in which a specimen is broken and its fracture surface
examined to determine such factors as composition, grain
size, case depth, or soundness [1].
Free carbon Part of the total carbon in steel or cast iron that is present in
elemental form as graphite [1]. See also Combined carbon.
Free machining Machining capabilities of an alloy to which one or more
ingredients have been introduced to produce small broken
chips, better surface finish, and longer tool lifetime during
the machining process [1].
Galvanizing Coating the surface of iron or steel with zinc applied
electrolytically or by hot dipping [3].
Goniometer An instrument devised for measuring the angle through
which a specimen is rotated [1].
Grain An individual crystallite in metals [2].
Grain boundary An interface separating two grains, where the orientation of
the lattice changes from that of one grain to that of the
other. When the orientation change is very small the
boundary is sometimes referred to as a subboundary [2].
Grain boundary
etching
Reveals the intersections of the individual grains. Grain
boundaries have a higher dissolution potential than the
individual grains because of their high density of structural
defects. Accumulation of impurities in grain boundaries
increases this effect [4].
Grain size (1) Measure of the areas or volume of grains in a
polycrystalline material, usually expressed as an average
when the individual sizes are fairly uniform. In metals
containing two or more phases, grain size refers to that of
the matrix unless otherwise specified. Grain size is reported
in terms of number of grains per measuring unit area or
volume, average diameter, or as a grain size derived from
area measurements. See also ASTM Standard E 112. (2)
Dimension of one individual particle of an abrasive,
measured in micrometres, m [1]. See also Grit size.
Grain-contrast
etching
Etching the surface of the grains according to their crystal
orientation. They become distinct by the different reflectivity
caused by reaction layers or surface roughness [4].
Graphite The polymorph of carbon with a hexagonal crystal structure
[1]. See also CG iron, Gray cast iron, Nodular cast iron,
Spheroidal cast iron.
Graphitic carbon Free carbon in steel or cast iron [1].
Graticule A scale on glass or other transparent material placed in the
eyepiece or at an intermediate plane on the optic axis of a
light microscope for the location and measurement of
objects (a graticule is different than a reticle) [2]. See also
Reticle.
Gray cast iron or
gray iron
Cast iron that looks gray on the fractured surface due to the
presence of free graphite. Contains carbon as graphite in
form of flakes or nodules [3].
Grinding The removal of material from the surface of a specimen by
abrasion through the use of randomly oriented
hard-abrasive particles bonded to a suitable substrate, such
as paper or cloth, where the abrasive particle size is
generally in the range of 60 to 600 grit (approximately
150 to 15 m) but may be finer [2].
Grinding paper Coated abrasive product in which paper is used as a backing
material [3].
Grit size Nominal size of abrasive particles in a grinding wheel,
corresponding to the number of openings per linear inch in
a screen through which the particles can just pass.
Sometimes but inadvisably called grain size [1]. See Grain
size.
Half moon
phenomenon
Appears mainly when using wet grinding disk and coarse
SiC-paper for plane and fine grinding of specimens clamped
in a specimen holder. This phenomenon is due to the fact
that the abrasive grains of the SiC-paper are not getting
worn down at the edge of an SiC-paper as fast as in the
middle, combined with the higher speed at the periphery of
the disk [3].
Hardening Increasing hardness of a metal with a suitable treatment,
usually through heating and fast cooling [1].
Hardness
indentation
Resistance of a metal to plastic deformation, usually by
indentation. However, the term may also refer to resistance
to scratching, abrasion, or cutting. Indentation hardness may
be measured by various hardness testing methods, such as
Brinell, Rockwell, Vickers, Knoop, and Scleroscope [3].
Heat-resistant alloy Alloys used for applications for which resistance against
high temperature and corrosion, combined with high
stresses are required. They are usually high nickel alloys [1].
Heat tinting Coloration of a metal surface through a thin oxide film,
formed by heating in oxidizing atmosphere, to reveal details
of the microstructure [1].
Heat treatment Heating and cooling a solid metal or alloy in such a way that
desired properties are obtained [1].
Heterogenous Nonuniform in microstructure or composition [2].
High alloy steel Contains up to 2.5 % carbon and more than 6 % metallic
alloying elements, mainly chromium (Cr), nickel (Ni),
vanadium (V), tungsten (W), and manganese (Mn). Very hard
tool steels and ductile stainless steels are high alloy steels
[3].
Homogenizing Holding at high temperature to eliminate or decrease
chemical segregation by diffusion [1].
Glossary 707
Hot dip coating Metallic coating obtained by dipping the basic metal into a
molten metal [1].
Hot etching Development and stabilization of the microstructure at
elevated temperature in etching solutions or gases [4].
Identication
selective etching
Etching for the identification of particular microconstituents
without attacking any others [4].
Image A representation of an object produced by means of
radiation, usually with a lens or mirror system [2].
Image processing, in
image analysis
The computer modification of a digitized image on a
pixel-by-pixel basis to emphasize or de-emphasize certain
aspects of the image [2]. See also Automatic image analysis.
Immersion etching The specimen is immersed in the etchant with the polished
surface up and is agitated. This is the most common etching
method [4].
Immersion objective An objective in which a medium of high refractive index is
used in the object space to increase the numerical aperture
and hence the resolving power of the lens [2].
Impact test A test to determine the behavior of materials when subjected
to high rates of loading, usually bending, tension, and
torsion. The quantity measures the energy absorbed in
breaking the specimen by a single blow, as in Charpy and
Izod tests [1].
Impregnation
metallography/
materialography
Process of filling voids and cracks under vacuum with a
sealing medium, for instance, epoxy cold mounting resin [3].
Impression (1) Electron microscopy. The reproduction of the surface
contours of a specimen formed in a plastic material after the
application of pressure and heat, or both.
(2) Hardness. The imprint or dent made in the specimen by
the indenter of a hardness-measuring device [2].
Impurities Elements or compounds whose presence in a material is
undesired [1].
Inclusions Foreign material held mechanically, usually referring to
nonmetallic particles, such as oxides, sulfides, silicates, etc.
[2]. See also Exogenous inclusions, Nonmetallic inclusions.
Indentation
hardness
Resistance of a material to indentation. This is the usual type
of hardness test, in which a pointed or rounded indenter is
pressed into a surface under a substantially static load [3].
See also Hardness.
Indigenous
endogenous
inclusion
A nonmetallic material that precipitates from the melt [2].
See Inclusions.
Induction hardening Surface hardening in which only the surface layer of a
suitable ferrous work piece is heated by electrical induction
to hardening temperature and then quenched [3].
Ingot Casting of a simple shape suitable for hot working or
remelting [1].
Intercrystalline Between crystals, or between grains of a metal, the same as
intergranular [1].
Intercrystalline
cracks
Cracks or fractures that occur between the grains or crystals
in a polycrystalline aggregate [2].
Interdendritic
corrosion
Corrosive attack that progresses preferentially along an
interdendritic path [1].
Interface Surface that forms the boundary between phases or systems,
or both [1].
Intergranullar
corrosion
A preferential attack at the grain boundaries [2].
Intracrystalline Within or across the crystals or grains of a metal, same as
transcrystalline and transgranular [1].
Inverted microscope A microscope so arranged that the line of sight is directed
upwards through the objective to the object [2].
Ion etching Surface removal by bombardment with accelerated ions in a
vacuum 1 to 10 kV [4].
Iron Iron-based metals not falling into the steel category, such as
pure iron, gray iron, pig iron, white cast iron, etc. [3].
Isotropy The condition of having the same values of properties in all
directions [2].
Kikuchi lines Light and dark lines superimposed on the background of a
single crystal electron diffraction pattern caused by
diffraction of diffusely scattered electrons within the crystal
[2].
Koehler illumination A specular illumination system. In reflected-light
microscopy, used directly for the brightfield mode, and as a
preliminary setup for all other modes except darkfield. The
image of the field diaphragm is focused on the specimen
surface and the image of an undiffused lamp source is
focused in the plane of the aperture diaphragm [2].
Knoop hardness Microhardness determined from resistance of a metal to
indentation using a rhombic-based pyramidal diamond
indenter, which makes an impression with one long and one
short diagonal [3].
Lamellar structure A microstructure consisting of parallel plates of a second
phase [3]. See Pearlite.
Laminate (1) A composite material, usually in the form of sheet or bar,
composed of two or more materials bonded to form a solid
structure. (2) Product of two or more bonded metal layers
[3].
Lapping The abrasive removal of material using graded abrasive
particles in a loose form as in a liquid slurry on a platen [2].
Lapping tracks Indentations on the specimen surface made by abrasive
particles moving freely on a hard surface. These are not
scratches from a cutting action, but are the distinct tracks of
particles tumbling over the surface without removing
material [3].
Glossary 709
Light metal Low density metal such as aluminum, magnesium, titanium,
beryllium, or their alloys [1].
Light micoscopy See Optical microscope.
Long-term etching Etching times of a few minutes to several hours [4].
Lubricant Any substance used to reduce friction between surfaces in
contact. Liquid used for cooling and lubricating. Depending
on the type of material and the preparation stage, different
types of lubricants can be used for grinding and polishing
[3].
Machining Removing surface material in the form of chips, usually with
a mechanical tool [3].
Macroetching Controlled etching of the surface of a metallic specimen,
intended to reveal a structure which is visible at low
magnifications (not usually greater than ten times) [2]. See
also Deep etching.
Macroscopic Observation using the naked eye or magnifications up to
1030 times [3].
Macrostructure Structure of metals as revealed by macroscopic examination
of the etched surface of a polished specimen [1].
Magnetic-particle
inspection
A nondestructive method of inspection for determining the
existence and extent of possible defects in ferro-magnetic
materials. On the surface of a magnetized part fine magnetic
particles are attracted to areas where the magnetic field is
displaced or interrupted, such as cracks or pores [1].
Malleability The characteristic of metals that permits plastic deformation
in compression without rupture [1].
Malleable cast iron A cast iron made by prolonged annealing of white cast iron
in which decarburization or graphitization, or both, takes
place to eliminate some or all of the cementite [1].
Martensite Metastable phase resulting from the diffusionless athermal
decomposition of austenite below a certain temperature
known as the M
s
temperature (martensite start
temperature). It is produced during quenching when the
cooling rate of a steel, in the austenitic condition, is such
that the pearlite and bainite, or both, transformation is
suppressed. The composition of the martensite is identical
with that of the austenite from which it transformed. Hence,
martensite is a super-saturated solid solution of carbon in
alpha iron (ferrite) having a body-centered tetragonal lattice.
It is a magnetic plate-like constituent formed by a
diffusionless shear type of transformation. These plates may
appear needle-like or veriform in cross section [2].
Materialography Materialography is defined as an investigative method of
materials science. It emcompasses the optical examination
of microstructures, and its goal is a qualitative and
quantitative description of the microscopic structural
analysis of solid materials. Materialography includes
metallography, ceramography, plastography, and mineralogy
[4]. See also Metallography.
Matrix The continuous phase [2]. See Continous phase.
Mechanical
polishing
Specimen preparation process using finer and finer
abrasives, mostly diamond, to obtain a surface suited for
microscopic examination.
Mechanical
properties
The properties of a material that reveal its elastic and
inelastic behavior when force is applied, by indicating its
suitability for mechanical applications; for example,
modulus of elasticity, tensile strength, elongation, hardness,
and fatigue limit [1]. Compare with Physical properties.
Mechanical testing Determination of mechanical properties [1].
Mechanical twin A twin formed in a crystal by simple shear under external
loading [1]. See also Twin bands.
Metallograph An optical instrument for the examination of metallographic/
materialographic specimens. In principle it consists of a
light source, a microscope, and a camera.
Metallography That branch of science which relates to the constitution and
structure, and their relation to the properties, of metals and
alloys [2]. See also Materialography.
Metallurgy The science and technology of metals and alloys [1].
Metastable A state of apparent equilibrium which has a higher free
energy than has the true equilibrium state; usually applied to
a phase existing outside its temperature and pressure span
of equilibrium existence, by reason of a greatly delayed
transformation [2].
Microetching Development of microstructure for microscopic
observation.The usual magnification exceeds 25 (50 in
Europe) [1].
Micrograph A graphic reproduction of an object as seen through the
microscope or equivalent optical instrument, at
magnifications greater than ten diameters [2].
Micro indentation
hardness
microhardness
Hardness of a material determined by forcing an indenter
into the polished surface of a material under very light load
using a microhardness tester [3]. See also Micro penetration
hardness.
Micro penetration
hardness
The hardness number obtained by use of a low load tester
whose indentation is usually measured with a high power
microscope [2]. See also Micro indentation hardness.
Microscopy The science of the interpretive use and applications of
microscopes [1].
Glossary 711
Microstructure The structure of a suitably prepared specimen as revealed by
a microscope [2].
Mineralogy Scientific study of minerals [3]. See also Petrographic
examination.
Modulus of elasticity
E
The measure of rigidity or stiffness of a metal; the ratio of
stress, below the proportional limit, to the corresponding
strain. In terms of stress-strain diagram, the modulus of
elasticity is the slope of the stress-strain curve in the range of
linear proportionality of stress to strain. Also known as
Young's modulus [1].
Monochromatic
homogeneous
Of the same wavelength [2].
Monocrystalline A solid composed of a unique crystal [3].
Morphology The shape characteristics of a structure; the form and
orientation of specific phase or constituent [2].
Mounting To embed the specimen in resin to facilitate the further
handling during grinding and polishing, and to improve the
preparation result [3].
Multiple etching A specimen is etched sequentially with the specific etchants
to reveal certain constituents [4].
Nitriding Nitriding is a form of surface hardening. By exposing a
ferrous part at a certain temperature to nitrogenous
materials, nitrogen will diffuse into the surface of the part
and form hard nitrides [3].
Nitrocarburizing Any of several case-hardening processes in which both
nitrogen and carbon are absorbed into the surface layers of
a ferrous material at a certain temperature. Nitrocarburizing
improves fatigue resistance [1].
Noble metal (1) A metal whose potential is highly positive relative to the
hydrogen electrode. (2) A metal with marked resistance to
chemical reaction, particularly to oxidation and to solution
by inorganic acids. The term as often used is synonymous
with precious metal [1].
Nodular cast iron Also called ductile cast iron; trace amounts of magnesium
are added to the melt to induce formation of free graphite
in the form of nodules. See also Spheroidal cast iron.
Nonmetallic
inclusions
Particles of impurities (usually oxides, sulfides, silicates, and
such) that are held mechanically or are formed during
solidification or by subsequent reaction within the solid
metal [2]. See also Exogenous inclusions, Inclusions.
Nondestructive
testing
Inspection by methods that do not destroy the part in order
to determine its suitability for use [1]. See also Field
metallography.
Normalizing Heating a ferrous alloy to a suitable temperature above the
transformation range and then cooling it in air to a
temperature substantially below the transformation range
[1].
Numerical aperture
NA
The sine of half the angular aperture of an objective lens
multiplied by the refractive index of the medium between
the lens and the sample [2].
Objective The primary magnifying system of a microscope [1].
Ocular See Eyepiece.
Optical etching Develops the microstructure by using special illumination
techniques (dark field, interference contrast, polarized light,
phase contrast) [4].
Optical microscope Instrument containing one or more lenses which uses
artificial light to produce an enlarged image of an object
placed in the focal plane of the lens(es) [3].
Ore A natural mineral that may be mined and treated for the
extraction of any of its components, metallic or otherwise
[3].
Organic materials For example, wood, bone, tissue, teeth, paper.
Orientation The angular position of a crystal described by the angles
which certain crystallographic axes make with the frame of
reference. In hardness measurements, the relationship
between the direction of the axes of the indenter of a
hardness tester and the direction of nonhomogeneous
properties of the specimen [2].
Overheating (1) In ferrous alloys, heating to an excessively high
temperature such that the properties/structure undergo
modification. The resulting structure is very coarse-grained.
Unlike burning, it may be possible to restore the original
properties/structure by further heat treatment or mechanical
working, or a combination thereof. (2) In aluminum alloys,
overheating produces structures that show areas of
resolidified eutectic or other evidence that indicates the
metal has been heated within the melting range [2].
Oxide polishing Process used for the final polishing of a specimen with a
suspension containing fine abrasive particles of oxides
(aluminum oxide, silicon dioxide) with or without chemicals
of different pH. See also Final polishing.
Oxidation (1) A reaction in which there is an increase in valence
resulting from a loss of electrons. (2) A corrosion reaction in
which the corroded metal forms an oxide; usually applied to
reaction with a gas containing elemental oxygen, such as air
[1].
P Polishing (mechanical) taking place as the last steps (P1, P2,
P3, etc.) of metallographic/materialographic preparation to
obtain a surface suited for microscopic examination. See
also Final polishing, Oxide polishing, Polishing.
Particle size The controlling linear dimension of an individual particle,
such as of a powdered metal, as determined by analysis with
screens or other suitable instruments [1].
Glossary 713
Pearlite A metastable microstructure formed when local austenite
areas attain the eutectoid composition in alloys of iron and
carbon containing greater than 0.025 % but less than 6.67 %
carbon. The structure is an aggregate consisting of alternate
lamellae of ferrite and cementite formed on slow cooling
during the eutectoid reaction. In an alloy of given
composition, pearlite may be formed isothermally at
temperatures below the eutectoid temperature by quenching
austenite to a desired temperature (generally above 550C)
and holding for a period of time necessary for
transformation to occur. The interlamellar spacing varies
directly with the transformation temperature; that is, the
higher the temperature the greater the spacing [2].
Petrographic
examination
Methods of examining nonmetallic matter under suitable
microscopes to determine structural relationships and to
identify the phases or minerals present. With transparent
materials, the determination of the optical properties, such
as the indices of refraction and the behavior in transmitted
polarized light, serve as means of identification. With
opaque materials, the color, hardness, reflectivity, shape, and
etching behavior in polished sections serve as means of
identification. Metallographic applications include
examination of particles mechanically or chemically
separated from the metal by these methods [2].
PG Plane (planar) grinding. Removes damage introduced by
cutting, and levels specimens clamped in a holder for
automatic grinding [3]. See also Planar grinding.
pH The negative logarithm of the hydrogen-ion activity. It
denotes the degree of acidity or basicity of a solution. At
25C 77F, 7.0 is the neutral value. Lower values than 7.0
indicate acidity and higher values increasing basicity [1].
Phase A physically homogeneous and distinct portion of a material
system [1].
Phase contrast
microscopy
A special method of controlled illumination, ideally suited
for observing thin, transparent objects whose structural
details vary only slightly in thickness or refractive index. This
can also be applied to the examination of opaque materials
to determine surface elevation changes [2].
Photo micrograph See Micrograph.
Physical etching Develops the microstructure through removal of surface
atoms, lowering the grain surface potential and deposition
of interference layers [4].
Physical properties Properties, other than mechanical properties, that pertain to
the physical nature of a material; for example, density,
electrical conductivity, thermal expansion, reflectivity
magnetic susceptibility, and so on [1]. See also Mechanical
properties.
Physical testing Determination of physical properties [1].
Pig Metal casting poured from the melting furnace, used for
remelting [3].
Pitting
metallography
Forming small sharp cavities in a metal surface if
electrolytic polishing is not performed correctly.
Pixel picture
element
Smallest spatial unit of an image [2].
Planar grinding The first step in a preparation procedure used to bring all
specimens into the same plane of polish. It is unique to semi
or fully automatic preparation equipment that utilize
specimen holders [2]. See also PG.
Plane grinding See PG.
Plasma spraying Coating technique in which the coating material is fed as
powder into an ionized gas atmosphere (plasma) and
sprayed in the molten state onto the surface to be coated [3].
Plastic Any of various organic compounds produced by
polymerization, capable of being molded, extruded, cast into
various shapes and films, or drawn into filaments used as
textile fibers [3].
Plastic deformation Deformation that remains or will remain permanent after
release of the stress that caused it [1].
Plasticity The capacity of a material to deform nonelastically without
rupturing [1].
Plating Forming an adherent layer of metal on metal, usually
through a galvanic process. Any adherent layer of metal on
other material can also be called plating [3].
Plowing In tribology, the formation of grooves by plastic deformation
of the softer of two surfaces in relative motion [1].
Polarized light
illumination
A method of illumination in which the incident light is plane
polarized before it impinges on the specimen [2].
Polishing A mechanical, chemical, or electrolytic process or
combination thereof used to prepare a smooth reflective
surface suitable for microstructure examination, free of
artifacts or damage introduced during prior sectioning or
grinding [2]. See also Final polishing, Oxide polishing,
Polishing cloth.
Polishing artifact A false structure introduced during a polishing stage of a
surface preparation sequence [1]. See also Artifact.
Polishing cloth A substrate, mostly a textile or a nonwoven material, used
for polishing of specimens with selected abrasives. See also
Final polishing, Oxide polishing, Polishing.
Polishing rate The rate of which material is removed from a surface during
polishing. It is usually expressed in terms of the thickness
removed per unit of time or distance traversed [1].
Polycrystalline Characteristic of an aggregate composed of more than one,
and usually of a large number, of crystals [2].
Glossary 715
Polymers Plastics, for instance polyethylene, epoxy, polyester and
polyacryl, and polyamide (Nylon) [3].
Pores Small voids in the body of a material [1].
Porosity Holes in a solid, not necessarily connected [2].
Potentiostatic
etching
Anodic development of the microstructure at a constant
potential enables a defined etching of singular phases [4].
Powder Particles of a solid characterized by small size, nominally
within the range from 0.1 to 1000 m [3].
Powder metallurgy Production and use of metal powders, which are hot pressed
and sintered into solid materials and shaped objects [1].
Precious metals Gold, silver, and platinum-group metals [3].
Precipitation Separation of a new phase from solid, liquid, or gaseous
solutions, usually with changing conditions of temperature
or pressure, or both [2].
Precipitation etching Develops the microstructure by the formation of reaction
products at the specimen surface [4].
Precipitation
hardening
Hardening caused by precipitation of a constituent from a
supersaturated solid solution [1]. See also Age hardening,
Aging.
Primary crystals The first type of crystals that separates from a melt on
cooling [2].
Primary etching Develops the cast microstructures including coring [4]. See
also Secondary etching.
Pull-out Void existing on the plane of polish of a metallographic
specimen caused by the dislodging of a particle or
constituent during the grinding or polishing operation [2].
Quantitative
metallography
Determination of specific characteristics of a microstructure
by making quantitative measurements on micrographs or
metallographic/materialographic images. Quantities so
measured include volume concentration of phases, grain
size, particle size, and surface-area-to-volume ratios of
micro-constituents, particles, or grains [1]. See also
Automatic image analysis.
Quenching Rapid cooling, usually in water [3].
Quenching crack A crack formed as a result of thermal stresses produced by
rapid cooling from a high temperature, not to be confused
with fire crack [2].
Ram Moving part in e.g, the cylinder of a mounting press [3].
Rare earth metals One of the group of 15 chemically similar metals with
atomic numbers 57 through 71, commonly referred to as the
lanthanides [1].
RCD Rigid composite disk, hard or soft, used for fine grinding.
See also Rigid grinding disk.
Recarburize (1) Increase the carbon content of molten cast iron or steel
by adding carbonaceous material, high-carbon pig iron or a
high carbon alloy. (2) Carburize a metal part to return
surface carbon loss in processing [1].
Recrystallization The formation of a new grain structure through nucleation
and growth commonly produced by subjecting a metal, that
may be strained, to suitable conditions of time and
temperature [3].
Reected light In the metallographic/materialographic microscope the
specimen is illuminated with reflected (incident) light. For
examination of mineralogical thin sections and in biology
the transmitted light is used.
Refractory (1) Material of very high melting point with properties that
make it suitable for furnace linings and kiln construction.
(2) Quality of resisting heat [1].
Refractory alloy (1) Heat-resistant alloy. (2) Alloy having an extremely high
melting point. (3) An alloy difficult to work at elevated
temperatures [1].
Refractory metal Metal with an extremely high melting point, above the range
of iron, cobalt, and nickel (Mo, V, W, Ta, Nb) [3].
Relief Due to varying hardness or wear rate of a matrix or
individual phases, or both; material is removed at different
rates, and relief is developed [3].
Removal rate The rate at which material is removed from a surface during
grinding and polishing. See also Polishing rate.
Glossary 717
Replica A reproduction of a surface in a material, for example, a
plastic.
(1) Atomic. A thin replica devoid of structure on the
molecular level, prepared by the vacuum or hydrolytic
deposition of metals or simple compounds of low molecular
weight.
(2) Cast. A reproduction of a surface in plastic made by the
evaporation of the solvent from a solution of the plastic or
by polymerization of a monomer on the surface.
(3) Collodion. A replica of a surface cast in nitro-cellulose.
(4) Formvar. A reproduction of a surface in a plastic
Formvar film.
(5) Gelatin. A reproduction of a surface prepared in a film
composed of gelatin.
(6) Impression. A surface replica which is made by
impression. The results of making an impression.
(7) Molecular. The reproduction of a surface in a high
polymer such as collodion and other plastics.
(8) Negative. That replica which is obtained by the direct
contact of the replicating material with the specimen. In it,
the contour of the replica surface is reversed with respect to
that of the original.
(9) Oxide film. A thin film of an oxide of the specimen to be
examined. The replica is prepared by air, oxygen, chemical,
or electrochemical oxidation of the parent metal and is
subsequently freed either mechanically or chemically for
purposes of examination.
(10) Plastic. A reproduction in plastic of the surface to be
studied, prepared by evaporation of the solvent from a
solution of plastic, by polymerization of a monomer, or
solidification of a plastic on the surface.
(11) Positive. A replica, the contours of which correspond
directly to the surface being replicated; that is, elevations on
the surface are elevations on the replica.
(12) Preshadowed. A replica formed by the application of
the shadowing material to a surface to be replicated, before
the thin replica film is cast or otherwise deposited on the
surface.
(13) Pseudo. A replica which has portions of the material
being replicated embedded in it.
(14) Tape replica method (faxfilm). A method of producing a
replica by pressing the softened surface of a tape or sheet of
a plastic material on the surface to be replicated.
(15) Vapor depositeda replica formed of a metal or a salt
by the condensation of the vapors of the material onto the
surface to be replicated [2].
Reproducibility The ability to achieve the same result every time. In
specimen preparation reproducibility is crucial, as specimen
preparation is often employed in quality inspection and
failure analysis. Reproducibility can be ensured by using
consumables of high standard and uniform quality, and by
using automatic preparation equipment which controls
preparation parameters, e.g., rotational speed, force, dosing
levels, and time [3].
Resolution The fineness of detail in an object which is revealed by an
optical device. Resolution is usually specified as the
minimum distance by which two lines or points in the object
must be separated before they can be revealed as separate
lines or points in the image. The theoretical limit of
resolution is determined from the equation:
d = 0.61/n sin A.A./2
where
d = minimum distance between object points
observed as distinct points in the image;
= wavelength of the radiation employed;
n = the minimum refractive index of the media
between the object and the objective lens;
A.A. = the angular aperture 2. See also Resolving
power.
Resolving power The ability of a given lens system to reveal fine detail in
an object 2. See also Resolution.
Reticle A system of lines, circles, dots, cross hair or wires, or
some other pattern, placed in the eyepiece or an
intermediate plane on the optic axis which is used as a
measuring reference, focusing target, or to define a
camera field of view a reticle is different than a graticule
2. See also Graticule.
Rigid grinding disk A nonfabric support surface, such as a composite of
metal/ceramic or metal/polymer, charged during use with
an abrasive usually 6 to 15 micrometre diamond
particles and used for grinding operations in a
metallographic preparation 2. See also RCD.
Rockwell hardness
test
Indentation hardness test based on the depth of
penetration of a specified penetrator cone or ball into a
specimen under a specified load 3.
Roughness Relatively finely spaced surface irregularities, the heights,
width, and directions of which establish the predominant
surface pattern 1.
Glossary 719
Rough polishing A polishing process after fine grinding to remove the layer
of significant damage caused by the grinding. Rough
polishing is followed by the steps polishing and final
polishing to finish the specimen preparation. See also
Final polishing, Oxide polishing, Polishing.
Scanning
microscope
An electron microscope in which the image is formed by a
beam operating in synchronism with an electron probe
scanning the object. The intensity of the image forming
beam is proportional to the scattering or secondary
emission of the specimen where the probe strikes it 2.
See also SEM.
Scratches A groove produced in a surface by an abrasive point 1.
Secondary etching Develops the microstructures that differ from primary
structures through transformation and heat treatment in
the solid state 4. See also Primary etching.
Segregation Concentration of alloying elements in specific regions in a
metallic object 2.
Segregation coring
etching
Develops segregation coring mainly in macrostructures
and microstructures of castings 4.
SEM Scanning Electron Microscope is a type of electron
microscope capable of producing high resolution images
of a specimen surface. Due to the manner in which the
image is created, SEM images have a characteristic
three-dimensional appearance and are useful for judging
the surface structure of the specimen 3. See also
Scanning microscope.
SG iron See Ductile cast iron.
Shear 1 That type of force that causes or tends to cause two
contiguous parts of the same body to slide relative to each
other in a direction parallel to their plane of contact. 2 A
type of cutting tool with which a material in the form of
wire, sheet, plate, or rod is cut between two opposing
blades. 3 The type of cutting action produced by rake so
that the direction of chip flow is other than at right angles
to the cutting edge 1.
Short-term etching Etching time of seconds to a few minutes 4.
Shrinkage Reduction in volume of a material from beginning to end
of solidification 3.
Shrinkage cavity A void left in cast metals as a result of solidification
shrinkage 1.
Shrinkage gaps Gaps are voids between the mounting resin and sample
material caused by shrinkage of the mounting resin 3.
Single specimen Single specimens can be prepared on preparation systems
using specimen mover plates. The specimens are not
clamped and force is applied to each individual specimen
3.
Sintering Bonding of particles in a mass of metal powder by
heating, usually with prior compacting 3.
Slag Nonmetallic product resulting from the dissolution of flux
and nonmetallic impurities in smelting, refining, and
certain welding operations 1. See also Inclusions.
Slip Translation of a portion of a crystal relative to the
adjacent portion 2.
Slip lines Traces of slip planes observed at low magnifications on
the polished surface of a crystal which has been deformed
after polishing; since no differences in orientation exist,
repolishing will remove the traces. With increasing
resolving power and magnification, an individual line may
be revealed as a series of parallel lines. The line which is
visible at low magnifications is then described as a slip
band 2.
Smearing Plastic deformation of a soft matrix or soft phases.
Instead of being cut, the material is pushed, moved across
the surface. Smearing occurs when the abrasive is too
small or when using the wrong lubricant or polishing
cloth, or a combination of these conditions, which
reduces the cutting effect of the abrasive 3.
Soldering Bonding of metals using filler metals at temperatures
below 450C 3.
Specimen A test object, often of standard dimensions or
configuration, or both, which is used for destructive and
nondestructive testing. One or more specimens may be
cut from each unit of a sample 1.
Specimen holder
metallography/
materialography
A holder in which 312 specimens are clamped. During
specimen preparation force is applied to the center of the
holder 3.
Spheroidal cast iron
SG
Same as nodular cast iron or ductile cast iron. See also
Nodular cast iron.
Spheroidite A coarse aggregate of carbide and ferrite usually produced
by tempering martensite at temperatures slightly below
the eutectoid temperature. Generally, any aggregate of
ferrite and large spheroidal carbide particles no matter
how produced 2.
Spheroidizing Heating and cooling to produce a spheroidizing or
globular form of carbide in steel 1.
Stage A device for holding a specimen in the desired position in
the optical path 2.
Stage micrometre A graduated scale used on the stage of a microscope for
calibration 2.
Staining Staining is a discoloration of the specimen surface,
typically caused by water, alcohol, or etching solutions
3.
Glossary 721
Stainless steel Any of several steels containing 12 to 30 % chromium as
the principal alloying element 1.
Steel Malleable iron-base alloy, containing carbon and other
alloying elements. Carbon and low-alloy steels contain a
maximum of 2 % carbon, high-alloy steels up to 2.5 %
carbon and over 8 % metallic alloying elements 3.
Stereology The study of mathematical procedures used to derive
three-dimensional parameters describing a structure from
two-dimensional measurement 2.
Stereomicroscope A light optical microscope that permits each eye to
examine the specimen at a slightly different angle, thereby
retaining its three-dimensional relationship 2.
Strain hardening An increase in hardness and strength caused by plastic
deformation at temperatures below the recrystallization
range 1.
Stringer A single, high-aspect ratio, elongated inclusion, two or
more elongated inclusions, or a number of small
nondeformable inclusions aligned in a linear pattern due
to deformation 2. See also Inclusions.
Structure As applied to a crystal, the shape and size of the unit cell
and the location of all atoms within the unit cell. As
applied to microstructure, the size, shape, and
arrangement of phases 2. See also True structure,
Polishing.
Subgrain A portion of a crystal or grain, with an orientation slightly
different from the orientation of neighboring portions of
the same crystal or grain 1.
Substrate Substratum that which lies under 2.
Superalloy Same as heat-resistant alloy; superalloys are heat and
corrosion resistant and ductile and contain up to 20 %
chromium Cr 3. See also Heat-resistant alloy.
Swab etching Wiping the specimen surface with cotton saturated with
an etchant. This will simultaneously remove undesired
reaction products 4.
Swarf Mixture of chips, abrasive material, and lubricating
medium developing during grinding/polishing.
Technical ceramics Pressed and sintered oxides, carbides, and nitrides. They
are very dense, insulators, highly wear resistant, and
resistant against chemicals: aluminum oxide Al
2
O
3
,
silicon carbide SiC, silicon nitride Si
3
N
4
, tungsten
carbide WC, titanium carbide TiC, boron carbide
B
4
C, titanium boride TiB
2
, zirconium oxide ZrO
2
3.
TEM The Transmission Electron Microscope is an imaging
instrument whereby a beam of electrons is focused onto a
specimen causing an enlarged version to appear on a
fluorescent screen or layer of photographic film or can be
detected by a CCD camera 3. See also Thin foil,
Transmission microscope.
Tensile testing To determine the strength of a material by pulling a
sample applying equal and constant stress until it breaks.
The elongation of the sample is also measured. Also
known as tension testing 3.
Thermal Any physical process taking place due to heat 3.
Thermal etching Annealing the specimen in a vacuum or inert atmosphere.
This is a preferred technique for high-temperature
microscopy and for ceramics 4.
Thermoplastic resins Mounting resins that soften or melt at elevated
temperatures and harden during cooling 3.
Thermosetting
resins
Mounting resins that cure under heat and pressure and
cannot be melted after curing. They are also called
duroplastics 3.
Thin foil A very thin specimen prepared for transmission
microscopy. See also TEM.
Tool steel Any of a class of carbon and alloy steels commonly used
to make tools. Tool steels are characterized by high
hardness and resistance to abrasion, often accompanied
by high toughness and resistance to softening at elevated
temperature. These attributes are generally attained with
medium carbon and high-alloy contents 1.
Traditional ceramics Earthenware, brick, clay, porcelain 3.
Transmission
microscope
A microscope in which the image forming rays pass
through are transmitted by the specimen being observed
2. See also TEM.
True structure The microstructure representing the material without any
influences from the preparation of the specimen. See also
Structure, Polishing.
Twin bands Bands across a crystal grain, observed on a polished and
etched section, the crystallographic orientations of which
have a mirror image relationship to the orientation of the
matrix grain across a composition plane which usually is
parallel to the sides of the band. 1 Annealing twins
twin bands which are produced during annealing
following cold work. 2 Mechanical twinstwin bands
which are produced by cold work. 3 Neumann bands
mechanical twins in ferrite 2.
Ultrasonic cleaning Immersion cleaning aided by ultrasonic waves that cause
microagitation 1.
Glossary 723
Ultrasonic testing Nondestructive test used on sound conductive materials to
locate cavities, cracks, and structural discontinuities by
means of ultrasonic impulse 3.
Vibratory polishing Mechanical polishing process where one or several
specimens are moved around in a bowl through vibration
of the bottom of the bowl.
Vickers In a more restricted sense, the 136 diamond pyramid
indenter used in microindentation hardness tests 2. See
also Micro indentation hardness, Micro penetration
hardness, Vickers hardness test.
Vickers hardness
test
Indentation hardness test using a pyramid-shaped
diamond indenter and variable loads which enables the
use of one hardness scale for all materials from very soft
lead to tungsten carbide 3. See also Micro indentation
hardness, Micro penetration hardness, Vickers.
Weld Union between materials by welding 3. See also Welding.
Welding Joining two or more pieces of metal by applying heat or
pressure, or both, with or without a filler material, to
produce a localized union through fusion or
recrystallization across the interface 1.
Weld structure The microstructure of a weld deposit and heat-affected
base metal 2. See also Welding.
Wet etching The specimen surface has to be wetted before immersion
into the etching solution. This is important for color
etchants 4.
Whiskers Metallic or ceramic filaments, mostly microscopic, more
or less evenly distributed in a matrix 3.
White cast iron Cast iron that shows a white fracture because the carbon
is present in the form of iron carbide, Fe
3
C, which gives
it its very high hardness and also brittleness 3.
White metal A general term covering a group of white-colored metals
and their alloys of relatively low melting points lead,
antimony, tin, cadmium, bismuth, and zinc and alloys
based on these metals 1.
Wire cutting A cutting method mainly used for sectioning of small
specimens of various types of materials. A fine wire is
drawn along the work piece with a controlled force. The
abrasive is either diamond bonded to the wire, or an
abrasive slurry that is dripped continuously onto the wire
and drawn into the cut 3.
Workability See Formability.
Work hardening A change in the hardness of a material as a result of
plastic deformation 2.
Working distance The distance between the surface of the specimen being
examined and the front surface of the objective lens 2.
Wrought iron An iron produced by direct reduction or ore or by refining
molten cast iron under conditions where a pasty mass of
solid iron with included slag is produced. The iron has a
low carbon content 1.
X-ray testing Using X-ray radiation to check work pieces for cavities,
cracks, pores, and overlaps. Especially used for checking
of welds 3.
Youngs modulus A term used synonymously with modulus of elasticity. The
ratio of tensile or compressive stresses to the resulting
strain 1. See also Modulus of elasticity.
References Glossary
[1] Benscoter, A. O. and Bramfitt, B. L., Metallographers Guide, Practices and
Procedures for Irons and Steels, ASM International, Materials Park, Ohio, USA, 2002.
Reprinted with permission of ASM International. All rights reserved. www.
asminternational.org
[2] ASTM Standard, Terminology Relating to Metallography E 7, ASTM International,
West Conshohocken, Pennsylvania, USA, 2003.
[3] Terms defined by Struers in the on-line training material e-Education and e-Training
under www.struers.com.
[4] Petzow, G., Metallographic Etching, ASM International, Materials Park, Ohio, USA,
1999.
Glossary 725
Subject Index
A
Abbreviations
occupational safety and health,
labs, 673674
specimen preparation, 221
Abrasive cut-off machines, 3643
design principles of wheel-work
piece contact, 3639
machine designs, 3943
Abrasive cut-off wheels, 3236
consumable wheels, 3234
slow consumable wheels, 3436
Abrasives, 1819
aluminum oxide, 18
cubic boron nitride, 18
diamond, 1819
polishing, 129132
silicon carbide, 18
wet abrasive cutting,
sectioning, 1621
Acrylics
labs, 668
After preparation cleaning, 8284
Agency for Toxic Substance and
Disease Registry ATSDR, 683684
Alcohol-based grinding/polishing
uids, 97
Alumina wet grinding paper, 105106
Aluminum
electrolytic polishing and
etching, 464
Aluminum alloys, 356358
Aluminum oxide
abrasive types, 18
grinding abrasives, 93
American Conference of Government
Industrial Hygienists ACGIH, 683
Analog cameras, automatic image
analysis, 614615
Anodic etching, 172173
Anodized coatings, specimen
preparation, 247251
Anodizing, etching, 173
Antimony, specimen preparation,
361364
Arc of contact, metallographic/
materialographic cutting
operation, 31
Archiving, 619
Artifacts of electrolytic polishing,
selection of preparation method, 7
ASTM B 487, 576
ASTM C 664, 576
ASTM E 45, 570
ASTM E 112, 571573
ASTM E 562, 569
ASTM E 930, 573
ASTM E 1077, 575
ASTM E 1122, 570
ASTM E 1181, 573
ASTM E 1245, 570
ASTM E 1268, 574
ASTM E 1382, 573
ASTM E 1578, 619
ASTM E 2014, 668, 674
ASTM E 2109, 574575
ASTM standards
cutting uids, wet abrasive
cutting, 29
hardness, 625
metallography, 188193
Atomic force microscope AFM, 561
Automatic grinding equipment,
119, 135
Automatic image analysis, 577617
analog cameras, 614615
automatic measurements,
600602
background correction, 586588
banding degree, 608
brightness and contrast, 581586
cameras, 614615
compacted graphite, 613
computers, 614
contrast stretching, 588589
depth measurements, 608610
digital cameras, 615616
digital imaging, 579, 602613
digital imaging technology,
613616
ductile cast iron, 611613
grain size, 606608
graphite in iron castings, 610611
gray cast iron, 613
hardware, 613616
727
histogram, 581
image acquisition, 579580
image calibration, 595598
image digitization, 580581
image measurement, 598602
image processing, 586595
implementation, 617618
inclusion rating, 603606
manual measurements, 599600
open source/public domain
software, 617
percent area, 602603
printers, 616
sharpening, 593595
smoothing, 592593
software, 616617
thickness measurements, 608610
volume fraction, 602603
watershed lter, 590592
Automatic measurements, automatic
image analysis, 600602
Automatic systems, polishing, 140143
Automation labs, 651654
Availability of NIOSH Registry of Toxic
Effects of Chemical Substances, 681
B
Background correction, automatic
Bacteria and fungi, cutting uids, wet
abrasive cutting, 2829
Bakelite bond, 2021
Banding, quantitative metallography/
materialography, 574
Banding degree, automatic image
analysis, 608
Bandsawing, 4852
blades, 4951
cutting uids, 51
machines, 4951
safety, 49
tips, 5152
Barium titanate, specimen
preparation, 241
Baumann hammer, 644
Before preparation start cleaning, 82
Beryllium, specimen preparation,
365367
Bias, quantitative metallography/
Blades, bandsawing, 4951
Bond materials
cut-off wheel, 2021
wet abrasive cutting, sectioning,
1621
Bones, specimen preparation, 427430
Boron carbide
Brass, specimen preparation, 376380
Brightness and contrast, automatic
Brinell hardness testing, 626628
British Standards Institution, 684
Brittle materials, grinding, 9293
Bronze
electrolytic polishing
and etching, 467
Building labs, 649, 650663
C
Calcium oxide, specimen
preparation, 241
Calibration, quantitative
metallography/materialography, 568
Cameras, automatic image
analysis, 614615
Capacitors, specimen preparation,
298300
Carbonitrided steels, specimen
preparation, 339342
Cement clinker, specimen preparation,
346349
Cemented carbides, 187
Ceramic capacitors, specimen
preparation, 281284
Ceramic layers, specimen preparation,
268270
Ceramic resistors, specimen
preparation, 281284
Ceramics
deformation, grinding, 9293
specimen material, 182
Cerium oxide, specimen
preparation, 241
Chemical disposals, occupational safety
and health, labs, 672673
Chemical etching, 172
Chemical mechanical polishing CMP,
7, 151152
Chemical microetching, examination
purpose, 194217
Chemical polishing, 7
electrolytic polishing/etching, 168
Chips, sliding, plowing, grinding
mechanics, 22
Chromium
and etching, 464465
Chromium carbide, specimen
preparation, 232235
Chromium oxide, specimen
preparation, 238240
Circular sawing, 48
Clamping, thermal damage, wet
Classical etching, 172
Classication of materials, specimen
material, 181
Cleaning, 8284
after preparation, 8284
drying, 83
ethanol, 83
grinding disks, 84
hand, 8283
polishing cloths, 84
before preparation start, 82
rubbing effect, 83
ultrasonic, 83
ultrasonic apparatuses, 83
Cleanliness, 84
Cloths, polishing, 124129
Coatings, specimen material, 182183
Cobalt
and etching, 465466
Cobalt-based super alloys, specimen
preparation, 373376
Cold mounting resins, occupational
safety and health, labs, 667
Color etching, 172
Color ratings system, occupational
Compacted graphite, automatic image
analysis, 613
Comparison procedure, quantitative
metallography/materialography,
571572
Composites
Compressed air, cleaning, 83
Computers, automatic image
analysis, 614
Concrete, specimen preparation,
346349
Confocal laser scan microscope,
552555
Consumable abrasive cut-off wheels
storing, 3334
wheel dimensions, 33
wheel velocity, 3233
Consumables, specimen preparation,
221
Contemporary grinding, 106117
diamond lm, 109
diamond pads, 109
ne grinding cloths, 116
magnetic xation, 106107
metal-bonded diamond-coated
disks, 109
resin-bonded diamond grinding
disks, 107108
resin-bonded SiC grinding
disks, 108
rigid composite disks, 109116
Contrast stretching, automatic image
analysis, 588589
Cooling, cutting uids, 26
Cooling system, cutting uids, wet
Copper
and etching, 466
Copper-bearing alloys, specimen
preparation, 380383
Cubic boron nitride, abrasive types, 18
Subject Index 729
Cubic boron nitride CBN, grinding
abrasives, 97
Cut-off grinding process, wet abrasive
cutting, sectioning, 1516
Cut-off wheel
abrasive types, 1819
bond material, 2021
grade, 20
grain size, 1920
rpm, 30
selection, 4445
specications, 1618
structure, 20
truing and dressing, 26
wear, 2526
1621
Cutting uids, 2629
ASTM standards, 29
bacteria and fungi, 2829
bandsawing, 51
cooling system, 2728
grinding uid application, 27
grinding uid concentration, 28
grinding uid disposal, 29
health and safety aspects, 29
lubrication and cooling, 26
synthetic grinding uids-oil-
based, 2627
water quality, 28
CVD coatings, specimen preparation,
247251
D
Dangers, occupational safety and
health, labs, 664
Dark-eld illumination DF,
etching, 169
Decarburization, quantitative
575576
Deformation, 8993
brittle materials, 9293
ceramics, 9293
grinding, 86
metals, 8992
polishing, 122124
Depth measurements, automatic image
analysis, 608610
Design principles of wheel-work
piece contact
abrasive cut-off machines, 3639
direct cutting, 36
oscillating cutting, 3637
rotating work piece, 39
step cutting, 3839
Diamond products
abrasive types, 1819
lm, 109
xed grains, 95
loose grains, 9596
monocrystalline, 94
pads, 109
pastes, 96
polycrystalline, 94
sprays, 96
suspensions, 96
Differential interference contrast DIC,
etching, 169
Diffusion coatings, specimen
preparation, 251254
Digital cameras, automatic image
analysis, 615616
Digital image management, 619
Digital imaging, automatic image
analysis, 579, 602613
Digital imaging technology, automatic
Diodes, specimen preparation, 281284
Direct cutting, design principles of
wheel-work piece contact, 36
Documentation, optical reected light
microscope, 550552
Drying, cleaning, 83
Ductile cast iron, automatic image
analysis, 611613
Dust, occupational safety and health,
labs, 667
Dynamic hardness testing procedures,
644645
E
Economy, grinding, traditional, 105
Edge retention, grinding, traditional,
103105
Education, labs, 651
Electric discharge machining EDM,
sectioning by melting, 46
Electrolytes, polishing/etching, 163164
Electrolytic polishing and etching,
172173, 453475
aluminum, 464
bronze, 467
chromium, 464465
cobalt, 465466
copper, 466
gray cast iron, 459
hard metals, 474475
heat treated steels, 459460
high carbon steels, 457
high-speed steels, 462463
iron, 462
lead, 467468
low-alloyed tool steels, 463
low carbon steels, 457458
magnesium, 468469
nickel, 469
silver, 469470
stainless steels, 460461
super alloys, 461
tin, 470471
titanium, 471
tungsten, 472
vanadium, 472473
zinc, 473
zirconium, 474
Electrolytic polishing/etching, 156168
chemical polishing, 168
electrolytes, 163164
electrolytic thinning for
transmission electron microscope
TEM, 167168
electropolishing in practice,
164165
equipment, 165166
eld metallography, 166167
nondestructive electropolishing,
166167
labs, 665
process, 156163
Electrolytic polishing etching,
artifacts, 7
Electrolytic thinning for transmission
electron microscope TEM, 167168
Electrolytically deposited coatings,
251254
Electron backscatter diffraction
EBSD, 559560
polishing, 149150
Electron microscopy, 558561
atomic force microscope AFM,
561
electron backscatter diffraction
EBSD, 559560
electron probe microanalyzer
EPMA, 560
energy dispersive spectroscopy
EDS, 559
focused ion beam FIB, 560
magnetic force microscopy
MFM, 561
scanning electron microscope
SEM, 558559
scanning probe microscopes
SPM, 560561
scanning transmission electron
microscope STEM, 558
transmission electron microscope
TEM, 558
Electron probe microanalyzer EPMA,
560
Electropolishing in practice, 164165
Energy dispersive spectroscopy EDS,
559
Engraving, marking, 80
Environment, grinding, traditional, 105
Environmental Protection Agency
EPA, 683
EPDM polymers, 430436
Epoxy, occupational safety and health,
labs, 667
Equipment
electrolytic polishing/etching,
165166
labs, 656660
Equotip tester, 645
Etchant names, examination purpose,
217
Etching, 169176
anodic, 172173
anodizing, 173
chemical, 172
Subject Index 731
classical, 172
color, 172
dark-eld illumination DF, 169
differential interference contrast
DIC, 169
electrolytic, 172173
examination purpose, 194
uorescence, 170
grain boundary etching, 171
grain contrast etching, 170171
heat tinting, 172
ion, 173174
macroetching, 174175
microetching, 169
microscope techniques, 169170
labs, 665666
physical, 173174
polarized light POL, 169170
potentiostatic, 173
precipitation, 172
preparation process, 13
reactive sputtering, 174
relief polishing, 173
reproducibility, 171172
sputtering, 174
thermal, 174
vapor deposition, 174
Ethanol, cleaning, 83
European Union EU, occupational
safety and health, labs, 669670, 684
Examination purpose, 179, 188
ASTM standards, 188217
chemical microetching, 194217
etchant names, 217
etching practice, 194
Eyepieces, optical reected light
microscope, 535536
F
Failure analysis, labs, 651
Feed speed, metallographic/
materialographic cutting operation,
3031
Ferrous metals, specimen material,
183184
Field metallography
166167
polishing, 150151
Field metallography/materialography,
Field selection, quantitative
568569
Fine grinding, 86, 119
Fine grinding cloths, 116
Fixed grains, diamond products, 95
Flammable and Combustible Liquids,
680
Flammable liquids, occupational safety
Fluorescence, etching, 170
Focused ion beam FIB, 560
Force
material removal, grinding, 89
metallographic/materialographic
cutting operation, 30
Fracturing, sectioning, 45
Free cutting, 3132
automatics, 32
hand, 32
G
Galvanization, specimen preparation,
251254
General Description and Discussion of
the Levels of Protection and
Protective Gear, 680681
General studies or routine work, 14
General use, machine designs, abrasive
cut-off, 4041
Generic methods, specimen
preparation, 219
Germanium, specimen preparation,
288291
Glasses, specimen preparation,
244247
Gold, specimen preparation, 384387
Grades
cut-off wheel, 20
hard, 20
soft, 20
Grain boundary etching, 171
Grain contrast etching, 170171
Grain penetration, material removal,
grinding, 89
Grain shape, material removal,
grinding, 88
Grain size
automatic image analysis,
606608
cut-off wheel, 1920
quantitative metallography/
Graphite in iron castings, automatic
Gray cast iron
automatic image analysis, 613
electrolytic polishing and etching,
459
Grinding, 8586
chips, sliding, plowing, 22
contemporary, 106117
deformation, 86, 8993
ne, 86
material removal, 8689
plane, 85
traditional, 99106
2122
Grinding, traditional, 99106
alumina wet grinding paper,
105106
economy, 105
edge retention, 103105
environment, 105
relief, 103105
SiC wet grinding paper, 100105
stones/disks, 99100
zirconia alumina wet grinding
paper, 105106
Grinding abrasives, 9397
aluminum oxide, 93
boron carbide, 97
cubic boron nitride CBN, 97
diamond, 9496
silicon carbide, 93
Grinding disks cleaning, 84
Grinding uid
application, 27
concentration, 28
disposal, 29
Grinding/polishing equipment, 117119
automatic grinding, 119
ne grinding, 119
manual grinding, 117119
plane grinding, 117119
Grinding/polishing uids, 89, 9799
alcohol-based, 97
oil-based, 9899
water-based, 97
water-oil based, 98
Grit number, 19
H
Hacksawing, 48
Hand cleaning, 8283
Hard grade, 20
Hard metals, electrolytic polishing
and etching, 474475
Hardness, 623625
ASTM standards, 625
indentation, 623624
testing special methods, 646
Hardness values
conversion, 642643
precision, 642
Hardware, automatic image
analysis, 613616
Hazard Communication Standard
HCS, OSHA standard, 674679
Health and safety aspects, cutting
uids, 29
Heat tinting, etching, 172
Heat treated steels, electrolytic
polishing and etching, 459460
High-alloy steels, specimen
preparation, 325328
High carbon steels
457
High-speed steels
462463
Histogram, automatic image analysis,
581
HMIS, occupational safety and health,
labs, 670
Subject Index 733
Hot dip zinc coatings, specimen
preparation, 254257
Human eye, light microscopy, 526527
Hydroxyapatite HA coating, specimen
preparation, 223226
I
Identication tag marking, 80
Illumination, optical reected light
microscope, 536537
Image
acquisition, 579580
calibration, 595598
digitization, 580581
measurement, automatic image
analysis, 598602
processing, automatic image
analysis, 586595
Implementation, automatic image
analysis, 617618
Inclusion rating
603606
Indentation hardness, 623624
Instrumented indentation testing,
641642
Integrated circuits. specimen
preparation, 301305
Intercept procedure, quantitative
572573
International Chemical Safety Cards,
682683
Ion etching, 173174
Iron, electrolytic polishing and etching,
462
J
Job Safety Analysis JSA, 670672
K
Knoop hardness testing, 633634
L
Laboratory information management
systems LIMS, 619
Labs, 649
automation, 651654
building, 649, 650663
education, 651
equipment, 656660
failure analysis, 651
layout, 660662
maintenance, 662663
649, 664684
planning, 654656
purpose, 650
quality control, 650
rationalization, 651654
research, 651
running, 649
testing and inspection labs, 651
Laser torching, sectioning by
melting, 46
Layout, labs, 660662
Lead
467468
Light microscopy, 525527
human eye, 526527
magnication, 527
magnifying lens and microscope,
527
visible light, 525526
List of Highly Hazardous Chemicals,
Toxics and Reactives, OSHA
standards, 680
Literature, occupational safety and
health, labs, 684686
Loose grains, diamond products, 9596
Low-alloy steels, specimen preparation,
336339
Low-alloyed steels, electrolytic
polishing and etching, 463
Low carbon steels
457458
Lubricants, 9799
cutting uids, 26
M
Machine designs, 3943
general use, 4041
polishing, 135139
precision, 4143
Machines, bandsawing, 4951
Macroetching, 174175
Magnesium
468469
Magnesium oxide, specimen
preparation, 241
Magnetic xation, contemporary
grinding, 106107
Magnetic force microscopy MFM, 561
Magnication, light microscopy, 527
Magnifying lens and microscope, 527
Maintenance, labs, 662663, 673
Malleable cast iron, specimen
preparation, 315318
Manganese, specimen preparation,
395397
Manual grinding equipment,
117119, 135
Manual measurements, automatic
Marking, 80
engraving, 80
identication tag, 80
stamping, 80
with waterproof ink, 80
Martens scratch hardness, 646
Material exam, 179
Material removal, 8689
force on specimens, 89
grain penetration, 89
grain shape, 88
grinding, 86
grinding/polishing uids, 89
polishing, 120122
rake angle, 8788
Material Safety Data Sheet MSDS,
occupational safety and health, labs,
670672
Materialographic specimen, 79
specimen or sample, 89
Materialography, 3
Mechanical damage, wet abrasive
cutting, 2223
unplane surface, 23
waviness, 23
Mechanical polishing artifacts,
selection of preparation method, 7
Mechanical preparation, occupational
Mechanical surface preparation. see
grinding
Medium carbon steels, specimen
preparation, 307311
Metal-bonded diamond-coated disks,
contemporary grinding, 109
Metallographic/materialographic
cutting operation
arc of contact, 31
cut-off wheel rpm, 30
feed speed, 3031
force, 30
free cutting, 3132
power, 31
wet abrasive cutting,
sectioning, 2932
wheel velocity, 30
Metallographic/materialographic
preparation, 56
Metallography, 3
Metals, deformation, grinding, 8992
Microelectronic material, specimen
preparation, 291293
Microelectronic materials, polishing,
143147
Microelectronic packages
polishing, 147149
specimen preparation,
295298, 301305
Microetching, 169
Microindentation hardness, 636639
Microscopes
options, 537538
techniques, etching, 169170
Microtomy, polishing, 155
Mineralogical materials, specimen
material, 184
Minerals, ores, specimen preparation,
349352
Subject Index 735
Mohs scratch hardness, 646
Molybdenum, specimen preparation,
398401
Monocrystalline, diamond products, 94
Mounting
labs, 664665
N
National Fire Protection Association
NFPA, 684
National Paint and Coatings
Association, 684
National Technical Information Service
NTIS, 683
National Toxicology Program NTP,
683
NFPA 704 Hazard Identication
Ratings System, 668669
Nickel
469
NIOSH standards, 681682
Nodular cast iron, specimen
preparation, 319321
Nondestructive electropolishing,
166167
Nonferrous metals, specimen material,
184186
O
Occupational Exposure to Hazardous
Chemicals in Laboratories, 679680
Occupational Safety and Health
Administration OSHA standards
Availability of NIOSH Registry of
Toxic Effects of Chemical
Substances, 681
Flammable and Combustible
Liquids, 680
General Description and
Discussion of the Levels of
Protection and Protective Gear,
680681
Hazard Communication Standard
HCS, 674679
List of Highly Hazardous
Chemicals, Toxics and
Reactives, 680
Occupational Exposure to Hazardous
Chemicals in Laboratories, 679680
Occupational safety and health labs,
649, 664684
abbreviations, 673674
acrylics, 668
Agency for Toxic Substance and
Disease Registry ATSDR,
683684
American Conference of
Government Industrial
Hygienists ACGIH, 683
ASTM E 2014, 668, 674
British Standards Institution, 684
chemical disposals, 672673
cold mounting resins, 667
color ratings system, 669
dangers, 664
dust, 667
electrolytic polishing/etching, 665
Environmental Protection Agency
EPA, 683
epoxy, 667
etching, 665666
EU system, 669670
European Union EU, 684
ammable liquids, 667
HMIS, 670
International Chemical Safety
Cards, 682683
Job Safety Analysis JSA,
670672
literature, 684686
maintenance and service, 673
Material Safety Data Sheet
MSDS, 670672
mechanical preparation, 665
mounting, 664665
National Fire Protection
Association NFPA, 684
National Paint and Coatings
Association, 684
National Technical Information
Service NTIS, 683
National Toxicology Program
NTP, 683
NFPA 704 Hazard Identication
Ratings System, 668669
NIOSH standards, 681682
OSHA standards, 674681
polyesters, 668
risk phrases, 670
safety information, 668672
sectioning, 664
Standard Operating Procedure
SOP, 670672
standards, 673
toxic substances, 666
training, 673
Oil-based grinding/polishing uids,
9899
Open source/public domain software,
image analysis, 617
Optical examination methods, reected
light microscope, 540546
Optical bers, specimen preparation,
244247
Optical reected light microscope,
528555
confocal laser scan microscope,
552555
documentation, 550552
eyepieces, 535536
illumination, 536537
microscope options, 537538
optical examination methods,
540546
path of light rays, 528
practical use of microscope,
546550
reected-light microscope,
538540
stereo microscopy, 555557
Ores, specimen preparation, 349352
Organic materials, specimen material,
186187
Oscillating cutting, design principles of
wheel-work piece contact, 3637
Oxyacetylene torching, 46
P
Paint layers, specimen preparation,
257260
Palladium, specimen preparation,
406409
Parameters, specimen preparation,
220221
Pastes, diamond products, 96
Path of light rays, optical reected light
microscope, 528
PCB coupon, specimen preparation,
305307
Percent area, automatic image analysis,
602603
Phenolic bond, 2021
Physical etching, 173174
Pitting, 9
Plane grinding, 85, 117119
Planimetric procedure, quantitative
Planning, labs, 654656
Plasma spray coatings, specimen
preparation, 265267, 270273
Plasma torching, sectioning by
melting, 46
Plated coatings, specimen preparation,
251254
Point count, quantitative
Polarized light POL, etching, 169170
Poldi impact hardness tester, 644
Polishing, 120155
abrasives, 129132
automatic grinding/polishing
equipment, 135
automatic systems, 140143
chemical mechanical polishing
CMP, 151152
cloths, 84, 124129
deformation, 122124
dynamics, 139140
electron backscatter diffraction
EBSD, 149150
eld metallography, 150151
machine design, 135139
manual grinding/polishing
equipment, 135
material removal, 120122
Subject Index 737
microelectronic materials,
143147
microelectronic packages,
147149
microtomy, 155
polishing dynamics, 139140
preparation methods, 132134
printed circuit boards PCB,
143
rough, 120
semiautomatic systems, 140143
thin sections, 152154
ultramilling, 155
Polycrystalline diamond products, 94
Polyesters, occupational safety and
health, labs, 668
Polymers, specimen material, 187
Porosity in thermal spray coatings,
574575
Potentiostatic etching, 173
Powder metals
Power, metallographic/
materialographic cutting
operation, 31
Power hacksawing, 48
Practical use of microscope, 546550
Precipitation etching, 172
Precision
cut-off, slow consumable wheels,
35
machine designs, abrasive, 4143
Preparation methods
polishing, 132134
selection of preparation
method, 7
Preparation process, 913
etching, 13
mounting, 11
sectioning, 1011
surface preparation, 1113
Preservation, 81
Printed circuit boards PCB,
polishing, 143
Printers, automatic image analysis, 616
Process, electrolytic polishing/etching,
156163
Punching, shearing, 47
Purpose, labs, 650
PVD coatings, specimen preparation,
247251
Q
Quality control labs, 650
Quantitative metallography/
ASTM B 487, 576
ASTM C 664, 576
ASTM E 45, 570
ASTM E 112, 571573
ASTM E 562, 569
ASTM E 930, 573
ASTM E 1077, 575
ASTM E 1122, 570
ASTM E 1181, 573
ASTM E 1245, 570
ASTM E 1268, 574
ASTM E 1382, 573
ASTM E 2109, 574575
banding, 574
bias, 568569
calibration, 568
comparison procedure, 571572
decarburization, 575576
eld selection, 568569
grain size, 571573
inclusion rating, 570
intercept procedure, 572573
other standards, 576
planimetric procedure, 572
point count, 569
porosity in thermal spray
coatings, 574575
stereology, 565567
volume fraction, 569
R
Rake angle, material removal,
grinding, 8788
Rationalization, labs, 651654
Reactive sputtering, etching, 174
Reected-light microscope, 538540
Relief
grinding, 103105
polishing, 173
Reporting locations, 15
Reproducibility, etching, 171172
Research labs, 651
Research studies, 14
Resin-bonded diamond grinding disks,
107108
Resin-bonded SiC grinding disks, 108
Resistors, specimen preparation,
293295
Rigid composite disks, grinding,
109116
Risk phrases, occupational safety
Rockwell hardness testing, 634636
Rotating work piece, 39
Rough polishing, 120
Rubber bonds, 21
Rubbing effect, cleaning, 83
Running labs, 649
S
Safety
bandsawing, 49
labs, 668672
Sample, materialographic specimen,
89
Sawing
bandsawing, 4852
circular sawing, 48
hacksawing, 48
power hacksawing, 48
sectioning, 4752
Scanning electron microscope SEM,
558559
Scanning probe microscopes SPM,
558561, 560561
Scanning transmission electron
microscope STEM, 558
Scleroscope, 645
Section type, selection, sectioning,
1415
Sectioning, 1453, 15
abrasive cut-off machines, 3643
abrasive cut-off wheels, 3236
fracturing, 45
labs, 664
other methods, 4553
sawing, 4752
sectioning by melting, 46
selection, 1415
shearing, 4647
wet abrasive cutting, 1532
wet abrasive cutting tips, 4345
wire cutting, 5253
Sectioning by melting, 46
electric discharge machining
EDM, 46
laser torching, 46
oxyacetylene torching, 46
plasma torching, 46
Selection, sectioning, 1415
general studies or routine
work, 14
reporting locations, 15
research studies, 14
section type, 1415
study of failures, 14
Selection of preparation method, 67
artifacts of electrolytic
polishing, 7
artifacts of mechanical
polishing, 7
preparation methods, 7
Semiautomatic systems, polishing,
140143
Semiconductors, specimen
preparation, 288291
Sharpening, automatic image analysis,
593595
Shearing
punching, 47
sectioning, 4647
Si wafers, specimen preparation,
288291
SiC bers in Ti matrix, specimen
preparation, 273276
SiC wet grinding paper, 100105
Silicon, specimen preparation, 288291
Silicon carbide
abrasive types, 18
Subject Index 739
Silicon nitride, specimen preparation,
235237
Silicon oxide, specimen preparation,
241
Silver
469470
Sintered carbides
Slow consumable wheels
precision cut-off, 35
storing, 36
truing and dressing, 3435
use, 35
wheel dimensions, 35
wheel velocity, 35
Smoothing, automatic image analysis,
592593
Soft grade, 20
Software, automatic image analysis,
616617
Solder balls, specimen preparation,
295298
Sorby, Henry Clifton, 56
Special methods hardness testing, 646
Specimen material, 179, 181187
ceramics, 182
classication of materials, 181
coatings, 182183
composites, 183
ferrous metals, 183184
materialographic specimen, 89
mineralogical materials, 184
nonferrous metals, 184186
organic materials, 186187
polymers, 187
powder metals, 187
sintered carbides, 187
Specimen preparation,
179180, 218521
abbreviations, 221
acrylics, 436439
aluminum, 352356
aluminum alloys, 356358
aluminum oxide, 238240
anodized coatings, 247251
antimony, 361364
barium titanate, 241
beryllium, 365367
bones, 427430
boron carbide, 227232
brass, 376380
bronze, 376380
calcium oxide, 241
capacitors, 298300
carbonitrided steels, 339342
cement clinker, 346349
ceramic capacitors, 281284
ceramic layers, 268270
ceramic resistors, 281284
ceramics, 232235
cerium oxide, 241
chromium, 367370
chromium carbide, 232235
chromium oxide, 238240
cobalt, 370373
cobalt-based super alloys,
373376
composites, 276281
concrete, 346349
consumables, 221
copper, 376380
copper-bearing alloys, 380383
CVD coatings, 247251
diffusion coatings, 251254
diodes, 281284
453475
electrolytically deposited
coatings, 251254
EPDM polymers, 430436
eld metallography/
galvanization, 251254
generic methods, 219
germanium, 288291
glasses, 244247
gold, 384387
gray cast iron, 315318
high-alloy steels, 325328
high carbon steels, 307311
high-speed steels, 343346
hot dip zinc coatings, 254257
hydroxyapatite HA coating,
223226
integrated circuits, 301305
lead, 387391
low-alloy steels, 336339
low carbon steels, 311314
magnesium, 391394
magnesium oxide, 241
malleable cast iron, 315318
manganese, 395397
medium carbon steels, 307311
microelectronic material,
291293
microelectronic packages,
295298, 301305
minerals, ores, 349352
molybdenum, 398401
nickel, 402405
nodular cast iron, 319321
optical bers, 244247
paint layers, 257260
palladium, 406409
parameters, 220221
PCB coupon, 305307
plasma spray coatings,
265267, 270273
plated coatings, 251254
powder metals, 439443
PVD coatings, 247251
resistors, 293295
semiconductors, 288291
Si wafers, 288291
SiC bers in Ti matrix, 273276
silicon, 288291
silicon nitride, 235237
silicon oxide, 241
silver, 409412
sintered carbides, 443447
solder balls, 295298
stainless steels, 328333
steps, 219220
super alloys, 333335
teeth, 427430
thermal spray coatings, 260265
tin, 413416
tin cubic boron nitride, 232235
tissue, 427430
titanium, 416420
titanium carbide, 232235
titanium nitride, 232235
transistors, 301305
trouble shooting, 476521
tungsten carbide, 232235
uranium, 447450
white cast iron, 322324
wrought aluminum alloys,
359361
YBCO ceramic super conductors,
285288
zinc, 420423
zinc oxide, 241
zirconium, 424427
zirconium dioxide, 241
Sprays, diamond products, 96
Sputtering, etching, 174
Stainless steels
460461
Stamping, marking, 80
Standard Operating Procedure SOP,
670672
Standards, occupational safety and
health, labs, 673
Static hardness testing, 626643
Brinell hardness testing, 626628
hardness values conversion,
642643
hardness values precision, 642
instrumented indentation
testing, 641642
Knoop hardness testing, 633634
microindentation hardness,
636639
Rockwell hardness testing,
634636
universal hardness, 639642
Vickers hardness testing, 628632
Step cutting, design principles of
wheel, 3839
Steps, specimen preparation, 219220
Stereo microscopy, 555557
Stereology, 565567
Stones/disks, grinding, 99100
Storage, 81
Storing
consumable abrasive cut-off
wheels, 3334
Subject Index 741
Structure, cut-off wheel, 20
Study of failures, selection, sectioning,
14
Super alloys
461
Surface preparation, 1113
Suspensions, diamond products, 96
Synthetic grinding uids-oil-based,
2627
T
Teeth, specimen preparation, 427430
Testing and inspection labs, 651
Thermal damage, wet abrasive cutting,
2325
clamping, 2425
wet cutting, 25
Thermal etching, 174
Thermal spray coatings, specimen
preparation, 260265
Thickness measurements, automatic
Thin sections, polishing, 152154
Tin
470471
Tin cubic boron nitride, specimen
preparation, 232235
Tissue, specimen preparation, 427430
Titanium
and etching, 471
Titanium carbide, specimen
preparation, 232235
Titanium nitride, specimen
preparation, 232235
Toxic substances, occupational safety
Traditional grinding, 99106
Traditional versus contemporary
methods, specimen preparation, 218
Training, occupational safety and
health, labs, 673
Transistors, specimen preparation,
301305
Transmission electron microscope
TEM, 558
Trouble shooting, specimen
preparation, 476521
True microstructure, 56, 6
Truing and dressing
cut-off wheel wear, wet abrasive
cutting, 26
Tungsten, electrolytic polishing and
etching, 472
Tungsten carbide, specimen
preparation, 232235
U
Ultramilling, polishing, 155
Ultrasonic apparatuses cleaning, 83
Ultrasonic cleaning, 83
Universal hardness, static hardness
testing, 639642
Unplane surface, mechanical damage,
wet abrasive cutting, 23
Uranium, specimen preparation,
447450
Use, slow consumable wheels, 35
V
Vanadium, electrolytic polishing and
etching, 472473
Vapor deposition, etching, 174
Vickers hardness testing, 628632
Visible light, light microscopy, 525526
Volume fraction
602603
W
Water-based grinding/polishing uids,
97
Water-oil based grinding/polishing
uids, 98
Water quality, cutting uids, wet
Waterproof ink marking, 80
Watershed lter, automatic image
analysis, 590592
Waviness, mechanical damage, wet
Wet abrasive cutting, sectioning, 1532
abrasives and bond materials,
1621
cut-off grinding process, 1516
cut-off wheel, 1621
cut-off wheel wear, 2526
cutting uids, 2629
grinding mechanics, 2122
mechanical damage, 2223
thermal damage, 2325
tips, 4345
Wet cutting, thermal damage, 25
Wheel dimensions
wheels, 33
Wheel velocity
wheels, 3233
White cast iron, specimen preparation,
322324
Wire cutting, 5253
Wrought aluminum alloys, specimen
preparation, 359361
Y
YBCO ceramic super conductors,
Z
Zinc
473
Zinc oxide, specimen preparation, 241
Zirconia alumina wet grinding paper,
105106
Zirconium
474
Zirconium dioxide, specimen
preparation, 241
Subject Index 743

A.S.T.M.24, Metallographic and Materialographic Specimen Preparation-2006

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A.S.T.M.24, Metallographic and Materialographic Specimen Preparation-2006

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Metallographic and

is another important parameter since it determines

a given wheel should wear faster. It can be

in a given cut-off operation will increase until the grain fracture

The G-rationeeds tobe as highas possible tosecure agoodeconomy of acut.

is the number of points that fall in the -phase and

referred to the test volume V

of a point grid with

is usedtodetermine the ASTMgrainsize number, G.

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