Metallographic Etching-Gunter Petzow

Metallographic
Etching
Metallographic and Ceramographic Methods
f or Revealing Microstructure
Gnter Petzow
Max Planck InstituteJor Metals R esearch,
Institute Jor Materials Science,
Stuttgart, West Germany
Translators from the German version:
Rosemarie Koch and James A. Nelson
L11~
AMERICAN SOCIETY FOR METALS
~ Metals Park, 0hio 44073
A I" ON., ....

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OriginaUy published in 1976 as

Metallographische Atzen
'~'\\ UI)N
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HU L, Ivl
lli I __ ___,'".1./ ." ...
Copyright 1976 by
Gebrder Borntraeger, Berlin- Stuttgart
'JU
\
0 . . ..
;:.
'J,
\' ')
Enlarged English translation copyright ' 1978 - ,.--- ..: . ", .. -- . ~

by the
AMERICAN SOCIETY FOR MET ALS
AU rights reserved
No part of this book may be reproduced , stored in a

retrieval system, or transmitted, in any form or by
any means, electronic, mechanical, photocopying,
recording, or otherwise, without the prior
written permission of the publisher.
Nothing contained in this book is to be construed as a
grant of any right of manufacture, sale, or use in
connection with any method , process, apparatus , product,
or composition, whether or not covered by letters patent
or registe red trademark, nor as a defense against
liability for the infringement of letters patent or
./} \
registered trademark.
{i
~ r
fI
To Robert 1. Gray and E. Daniel A lbrecht,

two distinguished contributors to th e
development of modern metallography,
for their encouragement in preparing th e
English version of this book.
~f
./
D
y
:i
l'
I
Library of Congress Cataloging in Publication Data
Petzow, G .
Metallographic etching.
HAn improved version of the 5th edition of . . . Metallo
graphische tzen."
Contains bibliographic references .
Ineludes index o
l . Metallographic specimens, 2. Metals- Etching.
1. Title.
TN690.7P4713
1978
669' .95'028
78-8023
tIj J'.
ISBN 0-87170-002-6
(, ~
PRINTED IN TH E UNITED STATES OF AMERICA
"f ,
1 ..h.t
1}
A I" ON., ....

//'
. -, - Lt"IISI'rIf'uf\lJl
,~'-__. ,f;:._ .L ~.;.
' 1-
-l] "
tq
\JI I lli ,
....c.:......~..... _o..
OriginaUy published in 1976 as

Metallographische Atzen
'~'\\ UI)N
~I -~/
HU L, Ivl
lli I __ ___,'".1./ ." ...
Copyright 1976 by
Gebrder Borntraeger, Berlin- Stuttgart
'JU
\
0 . . ..
;:.
'J,
\' ')
Enlarged English translation copyright ' 1978 - ,.--- ..: . ", .. -- . ~

by the
AMERICAN SOCIETY FOR MET ALS
AU rights reserved
No part of this book may be reproduced , stored in a

retrieval system, or transmitted, in any form or by
any means, electronic, mechanical, photocopying,
recording, or otherwise, without the prior
written permission of the publisher.
Nothing contained in this book is to be construed as a
grant of any right of manufacture, sale, or use in
connection with any method , process, apparatus , product,
or composition, whether or not covered by letters patent
or registe red trademark, nor as a defense against
liability for the infringement of letters patent or
./} \
registered trademark.
{i
~ r
fI
To Robert 1. Gray and E. Daniel A lbrecht,

two distinguished contributors to th e
development of modern metallography,
for their encouragement in preparing th e
English version of this book.
~f
./
D
y
:i
l'
I
Library of Congress Cataloging in Publication Data
Petzow, G .
Metallographic etching.
HAn improved version of the 5th edition of . . . Metallo
graphische tzen."
Contains bibliographic references .
Ineludes index o
l . Metallographic specimens, 2. Metals- Etching.
1. Title.
TN690.7P4713
1978
669' .95'028
78-8023
tIj J'.
ISBN 0-87170-002-6
(, ~
PRINTED IN TH E UNITED STATES OF AMERICA
"f ,
1 ..h.t
1}
Preface
:~,
"Jito.
In the last few years, metallographic prepara.tion techniques have been

improved considerably. During this progress, the transition from manual
and empirical methods to reproducible and automatic techniques - although not yet complete-has become l;\ reality. Taking this into account,
the modern preparation techniques and their functional interrelationships
are first treated in the present book, then well-proven metallographic
recipes for individual materials are listed. In addition to the classical
materials, those special metals and alloys are treated which find their
application in aerospace and nuclear engineering. Sirnilarly, techniques
and recipes for metal-ceramics and special ceramics are presented,
because these materials also are investigated more and more by "metallographic" -or, better, "ceramographic" -methods.
Instructions for specimen preparation not only are numerous but also
frequently contradict each other. Therefore, mainly the author's
experience - rather ' than data in the literature ~ was .used in compiling
the preparation recipes in this book. Special attention was given to those
pro ce dures that appear particularly suitable for small or medium-size
metallographic laboratories, which normally are not equipped with expensive and sophisticated instruments. The selected recipes are simple and
well-proven in practice; complicated, seldom used procedures of poor
reproducibility have been omitted.
. The present English-language book, "Metallographic Etching," is an
improved version of the 5th edition of the booklet "Metallographisches
tzen" (in German), published in 1976. The pro ven grouping of the
various recipes into certain classes of materials has be en maintained,
because it enables the ready exchange, variation, and combination of
various procedures between and within certain groups of materials.
I wish to thank all those who assisted me in the preparation of this
edition in English, particularly Rosemarie Koch and James A. Nelson
for their translation services. For their critical reading of the manuscript
I am indebted to Winfried J. Huppmann, lan Yapp, and Alan Prince.
And, finally, I would like to acknowledge the tedious task of typing
the manuscript by Antonie Rohrbach, Gertrud Thede, and Inge Hormann.
Stuttgart, 8 July 1977
,-
GNTER PETZOW
Preface to the German Edition

Vorwort
t
',.
Seit der letzten Auflage des tzheftes im Jahre 1957 hat sich die Situation
auf dem Werkstoffgebiet weitgehend verandert. Das Aufkommen neuer und
die Optimierung bekannter Technologiel\ haben viele Werkstoffe hervorgebracht,
deren Aufbau und Eigenschaften nicht zuletzt in den metallographischen Laboratorien in Forschung und Praxis aufgeldart und berprft werden mssen. Dem
wurde auch die metallographische Praparationstechnik angepasst: Der bergang
von der handwerklichen Empirie zur reproduzierbaren, automatisierten Metho'de
wurde, wenn auch nicht vollstiindig, so doch in erheblichem Ausmass vollzogen.
Das alles musste sich natrlich auf Inhalt und Umfang dieser Auflage auswirken.
So ist letzten Endes ein neues Buch unter neuem Titel entstanden, das nur
noch teilweise mit der vorhergehenden Auflage zu vergleichen ist.
Neben einer alle modemen Methoden einschliessenden Beschreibung der
Praparationstechniken wurde eine ganze Reihe von Werkstoffgruppen neu aufgenommen; angefangen von metallischen Hochleistungswerkstoffen im Flugzeug-, Reaktor- und Raketenbau bis hin zu den metallkeramischen und keramis,ehen Sondt<rwerkstoffen, die. in Z,unehmendem Ma,ss lichtmikroskopis.ch ).mtersueht werden. Die in den frheren Auflagen bewahrte Anordnung der Rezepte
in bestimmte Materialklassen wurde beibehalten, da sie die bersicht ber
Austauseh, Variation und Kombination innerhalb ahnlicher Werkstoffe erleichtert. Fr das sehnelle und gezielte Auffinden eines Rezeptes fr eine bestimmte
Anwendung wurde zusatzlieh ein nach Werkstoffen geordnetes Stichwortverzeichnis angefgt.
Da die in der Literatur vorhandenen Angaben ber die Schliffherstellung sehr
zahlreiehund teilweise widersprchlich sind, wurde bei der Auswahl der Praparationsrezepte in erster Linie auf eigene Erfahrungen zurekgegriffen. Besonders
beaehtetwurde dabei ihre Eignung fr kleine bis mittlere metallographische
Laboratorien, in denen aufwendige Einrichtungen selten sind. Die ausgewhlten
Rezepte sind daher einfaeh und bewab,rt; komplizierte, sebr anfiillige und wenig
erprobte Angaben wurden nicht bercksichtigt.
Allen Damen und Herren, die mir bei der Fertigstellung des Atzheftes geholfen
haben, mochte ieh herzlich danken: Insbesondere den Damen Karin Kuhn, Karin
Exner und Gonde Kiessler, die mir bei der anfangliehen Durchsicht der Literatur
und beim Lesen deL Korrekturfahnen sehr behilflieh waren. Fr die kritischen
Kommentare zu vielen Rezepten bin ieh den Mitgliedem des Aussehusses fr
Metallographie der Deutschen Gesellsehaft fr Metallkunde allen voran Frau
Grete Petrich sowie Herm Dr. H. P. Hougardy und Herrn F. Spies vom
Max-Planek-Institut fr Eisenforschung sehr verbunden; ebenso Herm Dr. Lipp
vom Elektroschmelzwerk Kempten fr die Komgrossenangaben der Schleifund Poliermittel. Frau Dr. Angelica Schrader, die das tzheft im Jabre 1934
begrndete und fr alle vorhergehenden Ausgaben verantwortlich zeichnet, hat
auch an der Fertigstellung dieser Auflage aktiven Anteil genommen.
Stuttgart, im November 1975
GiNTER PETZOW
13;;,
vii
Contents
1. Technical Tips for Preparation of Metallographic
Specimens -1
Specimen Sectioning-2
Mounting-3
Identification (Marking)-7
Grinding and Polishing - 8
Mechanical Grinding and Polishing - 9
Microtome Cutting - 16
Electrolytic Grinding and Polishing - 16
Chemical Polishing - 20
Combination Polishing Methods-21
Automatic Grinding and Polishing-22
Evaluation of Polishing Methods-22
Cleaning - 23
Etching-24
Optical Etching - 25
Electrochemical (Chemical) Etching-25
Physical Etching-29
Specimen Storage-29
Reproducibility in Etching - 30
Etching N omenclature - 31
Explanation of Etching Terms-31
Nondestructive Metallographic Testing-34
2. Preparation of Metals and Alloys-37

Ag Silver-37
Al Aluminum - 39
Au Gold-43
Ir Iridium - 43
Os Osmium-43
Pd Palladium-43
Pt Platinum - 43
Rh Rhodium-43
Ru Ruthenium-43
Be Beryllium-46
ix
.<.l(:,.
Confents
Bi Bismuth --:-48
Sb Antimony-48
Cd Cadmium -50
In Indium - 50
TI Thallium - 50
Co Cobalt-51
Cr Chromiun - 54
Mo Molybdenum-54
Nb Niobium - 54
Re Rhenium - 54
Ta Tantalum-54
V Vanadium-54
W Tungsten - 54
Cu Copper - 58
Fe Iron, Steel, Cast Iron.-61
Ge Germanium -68
Se Selenium -68
Si Silicon - 68
Te Tellurium-68
AmBy and AUBYI Compounds-68
Hf Hafnium-70
Zr Zirconium - 70
Hg Mercury Allys (Amalgamates)-71
Mg Magnesium-72
Mn Manganese - 75
Ni Nickel- 75
Pb Lead-79
Pu Plutonium - 81
Th Thorium - 81
U Uranium-81
RE Lanthanum and Rare Earths (Lanthanides)-83
Ce Cerium-83
Dy Dy~prosium - 83
Er Erbium - 83
Gd Gadolinium - 83
Ho H~lmium - 83
La Lanthanum - 83
Lu Llltetium - 83
Nd N~odymium-83
Pm Promethium -83
Pr Praseodymium - 83
Sm Samarium-83
Tb Terbium-83
Tm Thulium - 83
Yb Ytterbium - 83
Sn Tin-84
Ti Titanium - 85
Zn Zinc-88
Confents
xi
3. Preparation of Special Cerarnics and Cermets

(Ceramography)-91
Oxides-92
Carbides - 94
Nitrides - 97
Borides-98
Phosphides and Sulfides - 98
Cermets-99
Iron Oxide Layers on Iron-;-100
APPENDIX A: Suggestions for Handling Hazardous

Materials-l03
APPENDIX B: Chernicals Used to Prepare Etchants in
Chapters 2 and 3-105
APPENDIX C: References-l08
Safety and Toxicology-108
General Textbooks and Reviews - 109
Metallographic Preparation - 110
Handbooks, Compilations, and Tables-ll1
Journals of Mostly Metallographic Content-112
APPENDIX D: Sorne Suppliers oC Metallographic Equipment

and Materials -113
North America-l13
South America-1l4
Central America - 116
Europe-116
Asia-121
Australia-124
New Zealand - 124
Middle East- 124
Africa-126
Index-129
.<.l(:,.
Confents
Bi Bismuth --:-48
Sb Antimony-48
Cd Cadmium -50
In Indium - 50
TI Thallium - 50
Co Cobalt-51
Cr Chromiun - 54
Mo Molybdenum-54
Nb Niobium - 54
Re Rhenium - 54
Ta Tantalum-54
V Vanadium-54
W Tungsten - 54
Cu Copper - 58
Fe Iron, Steel, Cast Iron.-61
Ge Germanium -68
Se Selenium -68
Si Silicon - 68
Te Tellurium-68
AmBy and AUBYI Compounds-68
Hf Hafnium-70
Zr Zirconium - 70
Hg Mercury Allys (Amalgamates)-71
Mg Magnesium-72
Mn Manganese - 75
Ni Nickel- 75
Pb Lead-79
Pu Plutonium - 81
Th Thorium - 81
U Uranium-81
RE Lanthanum and Rare Earths (Lanthanides)-83
Ce Cerium-83
Dy Dy~prosium - 83
Er Erbium - 83
Gd Gadolinium - 83
Ho H~lmium - 83
La Lanthanum - 83
Lu Llltetium - 83
Nd N~odymium-83
Pm Promethium -83
Pr Praseodymium - 83
Sm Samarium-83
Tb Terbium-83
Tm Thulium - 83
Yb Ytterbium - 83
Sn Tin-84
Ti Titanium - 85
Zn Zinc-88
Confents
xi
3. Preparation of Special Cerarnics and Cermets

(Ceramography)-91
Oxides-92
Carbides - 94
Nitrides - 97
Borides-98
Phosphides and Sulfides - 98
Cermets-99
Iron Oxide Layers on Iron-;-100
APPENDIX A: Suggestions for Handling Hazardous

Materials-l03
APPENDIX B: Chernicals Used to Prepare Etchants in
Chapters 2 and 3-105
APPENDIX C: References-l08
Safety and Toxicology-108
General Textbooks and Reviews - 109
Metallographic Preparation - 110
Handbooks, Compilations, and Tables-ll1
Journals of Mostly Metallographic Content-112
APPENDIX D: Sorne Suppliers oC Metallographic Equipment

and Materials -113
North America-l13
South America-1l4
Central America - 116
Europe-116
Asia-121
Australia-124
New Zealand - 124
Middle East- 124
Africa-126
Index-129
Chapter 1:
Technical Tips Cor Preparation oC

Metallographic Specimens
~.
'4'.
,'.'.
The methods of preparing metallographic sections for macroscopic

and microscopic investigations are numerous and diverse. This is due
to the variety of materials requiring investigation and the manner in
which we have inherited much of the current data. Handed-down formulas
have to be taken into consideration together with a more scientific
approach to specimen preparation, patent rights, and commercial aspects
as well as modern developments of improved preparation techniques
and equipment. Thus, a comprehensive survey of specimen preparation
is, at best, difficult. Nevertheless, some correlations are apparent and
will be systematically explained prior to the tabulation of currently
accepted metallographic etchants. There is no universal technique that
will meet all the demands of metaHographic specimen preparation.
Metallographic preparation normally requires a specific sequence of
operations which ineludes sectioning, mounting, identification, grinding,
polishing, eleaning, and etching. Each of these steps can be carried
out in different ways and may vary according to the specific material
properties. In principIe, specimen preparation requires several steps,
even though not aH have to be pursued in every application. Care must
be taken in performing each step because carelessness at any stage
may affect later steps. In extreme cases, improper preparation may
result in a false structure leading to erroneous interpretation.
A satisfactory metallographic specimen for macroscopic andj or microscopic investigation must inelude a representative plane area of the
material. To elearly distinguish the structural details, tbis area must
be free from changes caused by surface deformation, flowed material
(smears), plucking (pull-out) and scratches. In certain cases, the edges
of the specimen must be preserved. By observing simple common-sense
principIes, acceptable preparation is possible for any solid-state material,
although in many cases it would require a lot of patience. Even for
routine examinations in the least critical applications, poor specimen
preparation is unacceptable because the observations and resulting
conclusions are, at best, questionable.
1
Technical Tips for Preparation of Specimens
Specimen Sectioning (Fig. 1)
Mounting (Fig. 2)
Mounting specitnens in a holding device is necessary when preparing
irregular, small, very soft, porous, or fragile specimens and in those
cases where edge retention is required.
Embedding is indispensable when multiple specitnens are to be included
SPECIMEN SECTlONING
Mechankal
Torch
Wire
Flal
Electrode
Abrosive
Cutting
"lit
Ult rasonic _1 '

Chiseling
Airbrasive
(Sand Blasting)
Cut-Off Wheel .
.ow Speed Oiamond
Elec!rochemical
L,.
Vertical
Mmi",
Embedding(Mountingl
tAcid Sawing
Hot
Cutting
tKnife Edge
Oblique
Clamping
Acid Jet
Sawing
Wire Saw
Saw
Cleaving
MOUNTING
I
are troublesome and titne-consuming and only useful for special applications (single crystals, semiconductors and brittle materials). They are
not economical for routine work.
The most versatile and economical sectioning method is abrasive
cutting. A thin, rapidly rotating, consumable abrasive wheel produces
high-quality, low-distortion cuts in titnes ranging from 15 seconds to
several minutes, depending upon the material and the cross-sectional
area. This technique is almost universally applicable. Important parameters in abrasive cutting are wheel composition, coolant condition, and
technique. Abrasive wheels consist of abrasive grains (alumina or silicon
carbide) bonded together with either resin or rubber or a rubber-resin
combination. By means of manufacturing controls, either "soft" Oow
wear resistance) or "hard" (high wear resistance) wheels may be
produced. Diamond abrasive blades are either resin or metal bonded.
Generally, soft bonded cutoff wheels are used to cut hard materials;
hard wheels are used for soft materials. The recent deyelopment of
gravity-fed, low-speed (to 300 rpm) diamond sawing has provided a rapid
and highly satisfactory means of sectioning small and delicate samples
with minimal distortion.
The first step in specimen preparation-selection and separation of

samples from the bulk material (sampling)-is of special itnportance.
If the choice of a sample is not representative of the material, it cannot
be cQrrected latero It is also difficult to compensate for itnproper
sectioning, beca use additional, time-consuming corrective steps may be
necessary to remove the damage produced.
Sectioning should render aplane surface suitable for further preparation
without causing severe changes in the material. AIterations in the sample
structure can be produced by deformation and the creation and further
development of cracks and breakouts due to generation of heat, recrystallization, local tempering, and in extreme cases, partial melting. These
problems can be minimized by the use of generous amounts of inert
lubricants and coolants (water, oil, compressed air, etc.).
When sectioning with a torch or by normal mechanical sawing, cutting,
sand blasting, or cleaving, care must be taken to cut sufficiently far
from the area of interest to avoid hannful effects. The pre-sample must
be large enough for the final sample to remain in the original state.
This pre-sample may then be heavily ground or cut by. more sophisticated
and delicate means to produce the desired plane for further preparation.
IdealIy, onIy methods that produce surfaces suitable for itnmediate fine
grinding or even polishing should be used. Such methods include abrasive
cutting, ultrasonic chiseling, are cutting, and electrochemical machining.
Although the goal is to use such material-preserving methods for sectioning
in the first place without the detour of a pre-sample, these methods
Cold
Inorgoni
Materials
lathe
Organic
Matria,s
Metals and AUOYS1
Hand
SUlfurj
.
Automatlc
Plastics
Glass
Thermosetting
Flg. l. Methods of metallographic specimen sectioning.
Galvonic
Resins
Inorganic
MateF~nts
tputties
Thermoplastic
Fig. 2. Methods of metallographic mounting.
11
Gypsum
Specimen Sectioning (Fig. 1)
Mounting (Fig. 2)
Mounting specitnens in a holding device is necessary when preparing
irregular, small, very soft, porous, or fragile specimens and in those
cases where edge retention is required.
Embedding is indispensable when multiple specitnens are to be included
SPECIMEN SECTlONING
Mechankal
Torch
Wire
Flal
Electrode
Abrosive
Cutting
"lit
Ult rasonic _1 '

Chiseling
Airbrasive
(Sand Blasting)
Cut-Off Wheel .
.ow Speed Oiamond
Elec!rochemical
L,.
Vertical
Mmi",
Embedding(Mountingl
tAcid Sawing
Hot
Cutting
tKnife Edge
Oblique
Clamping
Acid Jet
Sawing
Wire Saw
Saw
Cleaving
MOUNTING
I
are troublesome and titne-consuming and only useful for special applications (single crystals, semiconductors and brittle materials). They are
not economical for routine work.
The most versatile and economical sectioning method is abrasive
cutting. A thin, rapidly rotating, consumable abrasive wheel produces
high-quality, low-distortion cuts in titnes ranging from 15 seconds to
several minutes, depending upon the material and the cross-sectional
area. This technique is almost universally applicable. Important parameters in abrasive cutting are wheel composition, coolant condition, and
technique. Abrasive wheels consist of abrasive grains (alumina or silicon
carbide) bonded together with either resin or rubber or a rubber-resin
combination. By means of manufacturing controls, either "soft" Oow
wear resistance) or "hard" (high wear resistance) wheels may be
produced. Diamond abrasive blades are either resin or metal bonded.
Generally, soft bonded cutoff wheels are used to cut hard materials;
hard wheels are used for soft materials. The recent deyelopment of
gravity-fed, low-speed (to 300 rpm) diamond sawing has provided a rapid
and highly satisfactory means of sectioning small and delicate samples
with minimal distortion.
The first step in specimen preparation-selection and separation of

samples from the bulk material (sampling)-is of special itnportance.
If the choice of a sample is not representative of the material, it cannot
be cQrrected latero It is also difficult to compensate for itnproper
sectioning, beca use additional, time-consuming corrective steps may be
necessary to remove the damage produced.
Sectioning should render aplane surface suitable for further preparation
without causing severe changes in the material. AIterations in the sample
structure can be produced by deformation and the creation and further
development of cracks and breakouts due to generation of heat, recrystallization, local tempering, and in extreme cases, partial melting. These
problems can be minimized by the use of generous amounts of inert
lubricants and coolants (water, oil, compressed air, etc.).
When sectioning with a torch or by normal mechanical sawing, cutting,
sand blasting, or cleaving, care must be taken to cut sufficiently far
from the area of interest to avoid hannful effects. The pre-sample must
be large enough for the final sample to remain in the original state.
This pre-sample may then be heavily ground or cut by. more sophisticated
and delicate means to produce the desired plane for further preparation.
IdealIy, onIy methods that produce surfaces suitable for itnmediate fine
grinding or even polishing should be used. Such methods include abrasive
cutting, ultrasonic chiseling, are cutting, and electrochemical machining.
Although the goal is to use such material-preserving methods for sectioning
in the first place without the detour of a pre-sample, these methods
Cold
Inorgoni
Materials
lathe
Organic
Matria,s
Metals and AUOYS1
Hand
SUlfurj
.
Automatlc
Plastics
Glass
Thermosetting
Flg. l. Methods of metallographic specimen sectioning.
Galvonic
Resins
Inorganic
MateF~nts
tputties
Thermoplastic
Fig. 2. Methods of metallographic mounting.
11
Gypsum
in a single mount or when automatic devices are to be used in further

preparation. In most cases, mounting follows sectioning, hut in the
handling of a great number of very small specimens, it may be advantageous to reverse this order.In general, the mounting procedure can
be~asily adapted to the special problem in question. The existing
multiplicity of mounting techniques may be reduced to those two basic
meihods generalIy used: clamping and embedding.
Clamping is a means of holding specimens (samples) together in a
simple fixture device (Fig. 3). The specimens and the clamp should
a
{I}
()
Surface
~
~
Sample
d
_
Spacer
('
O Fixture
{j;
'.;
[8J
Fig. 3. Examples of fixtures used

for clamping: (a) tu be seetion, (b)
sheet metal, (e) rods, (d) irregular
pieces, (e) wires.
Resin + Pressure + Heat

= Polymer
Monomer + Catalyst (Heat) = Polymer + Heat.
Hot mounting (compression molding) requires the use of a press which

exerts sufficient pressure (usually 29 MPa [4200 psi]) to a specimen
mold heated to approximately 150 oC (300 F). Under pressure and heat,
the powdered resin fuses into a solid mass. Thermosetting resins, such
as phenolics, cure and harden irreversibly with time; thermoplastics
solidify when cooled to a lower temperature under pressure, but can
be remeIted .
Cold mounting (room-temperature-curing resins) requires uniform mixing of two components, usually powder and liquid or two liquids (a
monomer and a catalyst). This mixtureis cast into a suitable permanent,
reusable mold (metal or giass ring on a giass plate) or a consumabie
mold (phenolic ring on a glass piate) which becomes part of the mount.
The two chemicai components react to form a solid mount (Fig. 4).
a.
gene rally have similar mechanical and chemical characteristics so that

neither polishing surface relief nor interference duringetching occurs.
Clamps are most commonly made of soft steels, stainless steel, aluminum
alloys, or copper 'alloys. Stainless steel is the best choice for a wide
variety of materipls.
Shock-absorbing spacers (cork, rubber, or plastic) are sometimes used
to reduce defortpation but may interfere with preparation. A common
problem ep.counfered with clamps is the tendency of etching solutions
and solvents to seep froro gaps between the specimens and produce
ugly stains.
i
.. Plastic embeddlng is the most popular method of mounting me tallographic specimens at this time. The two main families of plastic used
in metallographic mounting are the "hot" mounting and "cold" mounting
resins:
Hot:
Cold:
Side View
....
::IJm_
Insert Sample
Add Mounting
Material
Remove Sample
Fig. 4. Cold mounting of metallographie

samples using (a) flexible, (b) inflexible, plastic molds.
Room-temperature-curing piastics are also advantageous when mounting

specimens that are porous or contain fine cracks. With the aid of a
vacuum chamber, pores and cracks may be filled and bubbles eliminated .
This vacuum impregnation technique is particularly useful in the preparation of powder metal, ceramic, or porous specimens in general.
Thin layers, platings, or diffusion zones present a problem due to
the difficulty in observing and measuring the thin areas. The apparent
thickness of thin layers mayhe increased by means of a taper technique,
in which the specimen is tilted at a shallow angle in the mold, as shown
in a single mount or when automatic devices are to be used in further

preparation. In most cases, mounting follows sectioning, hut in the
handling of a great number of very small specimens, it may be advantageous to reverse this order.In general, the mounting procedure can
be~asily adapted to the special problem in question. The existing
multiplicity of mounting techniques may be reduced to those two basic
meihods generalIy used: clamping and embedding.
Clamping is a means of holding specimens (samples) together in a
simple fixture device (Fig. 3). The specimens and the clamp should
a
{I}
()
Surface
~
~
Sample
d
_
Spacer
('
O Fixture
{j;
'.;
[8J
Fig. 3. Examples of fixtures used

for clamping: (a) tu be seetion, (b)
sheet metal, (e) rods, (d) irregular
pieces, (e) wires.
Resin + Pressure + Heat

= Polymer
Monomer + Catalyst (Heat) = Polymer + Heat.
Hot mounting (compression molding) requires the use of a press which

exerts sufficient pressure (usually 29 MPa [4200 psi]) to a specimen
mold heated to approximately 150 oC (300 F). Under pressure and heat,
the powdered resin fuses into a solid mass. Thermosetting resins, such
as phenolics, cure and harden irreversibly with time; thermoplastics
solidify when cooled to a lower temperature under pressure, but can
be remeIted .
Cold mounting (room-temperature-curing resins) requires uniform mixing of two components, usually powder and liquid or two liquids (a
monomer and a catalyst). This mixtureis cast into a suitable permanent,
reusable mold (metal or giass ring on a giass plate) or a consumabie
mold (phenolic ring on a glass piate) which becomes part of the mount.
The two chemicai components react to form a solid mount (Fig. 4).
a.
gene rally have similar mechanical and chemical characteristics so that

neither polishing surface relief nor interference duringetching occurs.
Clamps are most commonly made of soft steels, stainless steel, aluminum
alloys, or copper 'alloys. Stainless steel is the best choice for a wide
variety of materipls.
Shock-absorbing spacers (cork, rubber, or plastic) are sometimes used
to reduce defortpation but may interfere with preparation. A common
problem ep.counfered with clamps is the tendency of etching solutions
and solvents to seep froro gaps between the specimens and produce
ugly stains.
i
.. Plastic embeddlng is the most popular method of mounting me tallographic specimens at this time. The two main families of plastic used
in metallographic mounting are the "hot" mounting and "cold" mounting
resins:
Hot:
Cold:
Side View
....
::IJm_
Insert Sample
Add Mounting
Material
Remove Sample
Fig. 4. Cold mounting of metallographie

samples using (a) flexible, (b) inflexible, plastic molds.
Room-temperature-curing piastics are also advantageous when mounting

specimens that are porous or contain fine cracks. With the aid of a
vacuum chamber, pores and cracks may be filled and bubbles eliminated .
This vacuum impregnation technique is particularly useful in the preparation of powder metal, ceramic, or porous specimens in general.
Thin layers, platings, or diffusion zones present a problem due to
the difficulty in observing and measuring the thin areas. The apparent
thickness of thin layers mayhe increased by means of a taper technique,
in which the specimen is tilted at a shallow angle in the mold, as shown
d= l'sina
d True Thickness 01 Laye<
1 Observed Thickness
a Tilt Angle
Mounting Material
[;z
Amount ta be
Fig. 5. Taper
sectioning
(oblique
mounting to increase width of layer).
Table 1. Increase in Width of Layer as a Function
of Tilt Angle (Compare Fig. 5)
Increase 'in
layer widtb
Tilt
angle
Increase in
layer width
25 :1
20:1
15:1
10:1
2~0'
250'
350'
540'
5:1
2:1
1.5: 1
TUt
angle
ll030'
300
4150'
in Fig. 5. The width advantage gained is dependent on the angle, as

tabulated in Table l.
Important properties of mounting materials (encapsulants) suitable for
metallographic hot and cold mounting are:
..'
Inertness to" sample material, etchant, mold, or any other reagent

used in pre,Paration
l
Moderate viscosity in the liquid state and freedom from bubbles
after .solid'Vication
"
L0'Y linear shrinkage
Good adhesion to the specimen
Hardness "and wear resistance similar to those of the specimen
~
These requirements are satisfied by many of the commercially available

thermosetting ,and thermoplastic mounting materials. While thermoplasties remain plastic in the characteristic temperature interval even after
repeated heating, thermosetting materials harden irreversibly upon applieation of heat and pressure, and j or under the influence of a catalyst.
A1though many mounting plastics possess the required characteristics,
one type usually works best for a given application. Properties of
{j(;':
encapsulants may be modified to make them suitable for special purposes.

Metallic fillers such as silver or copper may be added to produce
electroconductivity in electrolytic applications. Conductivity can also
be achieved by drilling a hole through the mount from the rear up to
the sample and inserting a conductor. Hardness or wear resistance may
be increased through the addition of an abrasive filler such as alurnina.
This is particularly helpful in preserving the critical edges of hard
specimens. Fillers are usually added to compression (hot) molding plastics
during the manufacturing process. 'In room-temperature-curing eneapsulants, the fillers are often added when mixing, prior to casting. Shrinkage
gaps sometimes occur whenthe mounting plastic recedes from the sample
surface during curing. A low-shrinkage epoxy resin or the preparation
of critical surfaces with a pre-coating of plastic or electroplated metal
may avoid or minimize this problem and allow mounting to proceed
in the usual manner.
Heating of specimens, expected in compression molding, sometimes
occurs in "cold" mounting also. Exothermic reactions in these encapsulants, particularly with acrylics, may reach as high as 150 oC (300 F)
during curing. This may also occur in epoxies and polyesters when the
catalyst or hardener ratio is too high or ifheat dissipation is poor.
Mixing ratios should always be followed closely and cast mounts should
be cured in a .well-ventilated area, even a fume hood if available. Chilled
water cooling may sometimes be required.
Materials whieh are temperature andj or pressure sensitive should be
mounted in room-temperature-curing resins. Rigid materials that are not
heat sensitive may be prepared more economically by compression
molding. If only a few specimens are to be prepared, hot mounting
is less time-consuming than cold mounting; with a larger number of
specimens, the reverse holds.
Identification (Marking) (Fig, 6)

Specimens are useful only iftheir origin is known. Therefore, specimens
should be clearly marked so that their identity is not lost at any time
in the preparation sequence. It is important that marking does not cause
any changes to the surface of the specimen. Methods such as stamping
or vibration-engraving produce local deformation. In electroengraving,
which utilizes the principIe of spark evaporation, local changes in
composition can take place through reaction with the surrounding atmosphere. Thesechanges can alter the microstrueture, through decarburization or remelting and quench cooling. Heat treated specimens are
particularly susceptible to such effects. Markings should be placed on
d= l'sina
d True Thickness 01 Laye<
1 Observed Thickness
a Tilt Angle
Mounting Material
[;z
Amount ta be
Fig. 5. Taper
sectioning
(oblique
mounting to increase width of layer).
Table 1. Increase in Width of Layer as a Function
of Tilt Angle (Compare Fig. 5)
Increase 'in
layer widtb
Tilt
angle
Increase in
layer width
25 :1
20:1
15:1
10:1
2~0'
250'
350'
540'
5:1
2:1
1.5: 1
TUt
angle
ll030'
300
4150'
in Fig. 5. The width advantage gained is dependent on the angle, as

tabulated in Table l.
Important properties of mounting materials (encapsulants) suitable for
metallographic hot and cold mounting are:
..'
Inertness to" sample material, etchant, mold, or any other reagent

used in pre,Paration
l
Moderate viscosity in the liquid state and freedom from bubbles
after .solid'Vication
"
L0'Y linear shrinkage
Good adhesion to the specimen
Hardness "and wear resistance similar to those of the specimen
~
These requirements are satisfied by many of the commercially available

thermosetting ,and thermoplastic mounting materials. While thermoplasties remain plastic in the characteristic temperature interval even after
repeated heating, thermosetting materials harden irreversibly upon applieation of heat and pressure, and j or under the influence of a catalyst.
A1though many mounting plastics possess the required characteristics,
one type usually works best for a given application. Properties of
{j(;':
encapsulants may be modified to make them suitable for special purposes.

Metallic fillers such as silver or copper may be added to produce
electroconductivity in electrolytic applications. Conductivity can also
be achieved by drilling a hole through the mount from the rear up to
the sample and inserting a conductor. Hardness or wear resistance may
be increased through the addition of an abrasive filler such as alurnina.
This is particularly helpful in preserving the critical edges of hard
specimens. Fillers are usually added to compression (hot) molding plastics
during the manufacturing process. 'In room-temperature-curing eneapsulants, the fillers are often added when mixing, prior to casting. Shrinkage
gaps sometimes occur whenthe mounting plastic recedes from the sample
surface during curing. A low-shrinkage epoxy resin or the preparation
of critical surfaces with a pre-coating of plastic or electroplated metal
may avoid or minimize this problem and allow mounting to proceed
in the usual manner.
Heating of specimens, expected in compression molding, sometimes
occurs in "cold" mounting also. Exothermic reactions in these encapsulants, particularly with acrylics, may reach as high as 150 oC (300 F)
during curing. This may also occur in epoxies and polyesters when the
catalyst or hardener ratio is too high or ifheat dissipation is poor.
Mixing ratios should always be followed closely and cast mounts should
be cured in a .well-ventilated area, even a fume hood if available. Chilled
water cooling may sometimes be required.
Materials whieh are temperature andj or pressure sensitive should be
mounted in room-temperature-curing resins. Rigid materials that are not
heat sensitive may be prepared more economically by compression
molding. If only a few specimens are to be prepared, hot mounting
is less time-consuming than cold mounting; with a larger number of
specimens, the reverse holds.
Identification (Marking) (Fig, 6)

Specimens are useful only iftheir origin is known. Therefore, specimens
should be clearly marked so that their identity is not lost at any time
in the preparation sequence. It is important that marking does not cause
any changes to the surface of the specimen. Methods such as stamping
or vibration-engraving produce local deformation. In electroengraving,
which utilizes the principIe of spark evaporation, local changes in
composition can take place through reaction with the surrounding atmosphere. Thesechanges can alter the microstrueture, through decarburization or remelting and quench cooling. Heat treated specimens are
particularly susceptible to such effects. Markings should be placed on
T
Inscribing
Simultaneous Embedding
of a Written Identifi cotian Slip (only for
Transparent Mounts)
T
Engroving
Stamping
Mechanical Grinding and Polishing
1
Vibration
Fig. 6. Methods for

graphic specimens.
Elec tro
identifying metallo-
the side opposite the critical face to avoid damage. Identification labels
should be fixed on the mounts immediately to avoid loss of identity
at this point.
1
Grinding and Polishing (Fig. 7)

Coarse and fine grinding are the initial steps in producing a satisfactory
polished specime~ . Together with polishing, grinding serves to smooth
the surface, rem6ve the altered surface material, and reveal the true
structure of the specimen. These processes are carried out in several
steps from coarse to fine so that the deformed layer may be effectively
reduced. Coarse grinding removes heavy surface damage and produces
a flat surface comparable to filing or planing, which are seldom used
in metallography. The surface roughness resulting from coarse grinding
is in the range of 10 to 100 J.l.m (1 J.l.m = 10- 3 mm = 3.9 X lO -s
in.). Grinding leaves a roughness of 1 to 10 J.l.m, and fine grinding of
about 1 J.l.m. A1though grinding produces a flat, smooth surface, it is
suitable for macroscopic examination or macroetching only.
Because there is not a sharp fine between grinding and polishing,
' -1
I
,".
Electrolyticol
Me.;honical
ElectroErosive
Highly Deformed Smear Zone
Contours 01
Equal Deformation
.J::.
POLl SHING
Cutting by
Microtome
el
Vibration
Rotation
"
,,
"
Mechanical
w
t eDryHand
]
-'"
,,',
..---.
t-1
;;:}
I
-,,/
"
't
,
\
'
,,"
I
I
,_
....
Chemical
Electrolytical
Mechanicol
Electrolytical
Be l t
/:.<,;
Mechanical grinding and polishing are most common . They are usually
accomplished by abrasive removal, using a manual technique on fixed
abrasives, vibrating platens, rotating wh.eels, or continuous belts .
During mechanical grinding and polishing, the .surface is rempved by
the abrasive in the form of shavings or chips. To a'tesser degree, removal
takes place through adhesive interaction between sample and polishing
support. Scratches, deforination, and some smearing are characteristic
consequences of mechanical grinding and polishing. The purpose of
grinding and pofishing is to produce a suitable surface by means of
a step-by-step removal of deformed material until it becomes negligible .
While deformation is predominant in coarse grinding, smearing due
to plastic flow is more prevalent during polishing. This is illustrated
schematically in Fig. 8. It is assumed that polishing produces a flat
1i.
QJ
GRINDING
there is considerable overlap between fine grinding and coarse polishing.

For this reason, grinding and polishing are described here together.
IDENTIFICATION
Fig. 7. Methods of metallographic grinding and polishing.
Undeformed Region
Fig. 8. Schematic diagram of the surface region of a microsection after grinding and
polishing. (Section at right angle to surface.)
T
Inscribing
Simultaneous Embedding
of a Written Identifi cotian Slip (only for
Transparent Mounts)
T
Engroving
Stamping
Mechanical Grinding and Polishing
1
Vibration
Fig. 6. Methods for

graphic specimens.
Elec tro
identifying metallo-
the side opposite the critical face to avoid damage. Identification labels
should be fixed on the mounts immediately to avoid loss of identity
at this point.
1
Grinding and Polishing (Fig. 7)

Coarse and fine grinding are the initial steps in producing a satisfactory
polished specime~ . Together with polishing, grinding serves to smooth
the surface, rem6ve the altered surface material, and reveal the true
structure of the specimen. These processes are carried out in several
steps from coarse to fine so that the deformed layer may be effectively
reduced. Coarse grinding removes heavy surface damage and produces
a flat surface comparable to filing or planing, which are seldom used
in metallography. The surface roughness resulting from coarse grinding
is in the range of 10 to 100 J.l.m (1 J.l.m = 10- 3 mm = 3.9 X lO -s
in.). Grinding leaves a roughness of 1 to 10 J.l.m, and fine grinding of
about 1 J.l.m. A1though grinding produces a flat, smooth surface, it is
suitable for macroscopic examination or macroetching only.
Because there is not a sharp fine between grinding and polishing,
' -1
I
,".
Electrolyticol
Me.;honical
ElectroErosive
Highly Deformed Smear Zone
Contours 01
Equal Deformation
.J::.
POLl SHING
Cutting by
Microtome
el
Vibration
Rotation
"
,,
"
Mechanical
w
t eDryHand
]
-'"
,,',
..---.
t-1
;;:}
I
-,,/
"
't
,
\
'
,,"
I
I
,_
....
Chemical
Electrolytical
Mechanicol
Electrolytical
Be l t
/:.<,;
Mechanical grinding and polishing are most common . They are usually
accomplished by abrasive removal, using a manual technique on fixed
abrasives, vibrating platens, rotating wh.eels, or continuous belts .
During mechanical grinding and polishing, the .surface is rempved by
the abrasive in the form of shavings or chips. To a'tesser degree, removal
takes place through adhesive interaction between sample and polishing
support. Scratches, deforination, and some smearing are characteristic
consequences of mechanical grinding and polishing. The purpose of
grinding and pofishing is to produce a suitable surface by means of
a step-by-step removal of deformed material until it becomes negligible .
While deformation is predominant in coarse grinding, smearing due
to plastic flow is more prevalent during polishing. This is illustrated
schematically in Fig. 8. It is assumed that polishing produces a flat
1i.
QJ
GRINDING
there is considerable overlap between fine grinding and coarse polishing.

For this reason, grinding and polishing are described here together.
IDENTIFICATION
Fig. 7. Methods of metallographic grinding and polishing.
Undeformed Region
Fig. 8. Schematic diagram of the surface region of a microsection after grinding and
polishing. (Section at right angle to surface.)
10
surface and that grinding scratches have been removed. The scratch
troughs have been filled with material previously protruding aboye the
surface. This is the result of the rolling action of loose, unsupported
abrasive particles in the cloth polishing steps. This filling effect gives
rise to the smeared black layer in Fig. 8. The black region is composed
of severely deformed material from the specimen, mixed with polishing .
compound. Adjacent to this layer is a range of deformed material with
a decreasing severity of deformation toward the interior of the specimen.
Lines of equal deformation do not run parallel to the specimen surface,
but follow the pro fiJe generated by the coarse grinding action.
Varying surface conditions produce different properties such as
electrochemical potentials. Areas having the highest degree of deformation, for example, have the greatest reaction to etching solutions and
are, therefore, dissolved at a higher rateo This is the reason for the
reappearance of scratches on polished surfaces after etching, revealing
poor preparation.
The depth of scratches (roughness) plus the depth of deformaiion
equals the total depth of disturbed material as shown in Fig. 9. This
is based on references from literature using steel as the example. The
depth of roughness is directly proportional to the particle size of the
abrasive, but the depth of deformation approaches a constant value
after the initial increase.
Depth of
Roughness
Depth of
Grinding Steps
An understanding of the relationship illustrated in Fig. 9 is necessary
ti k _. '. .. '. . . '.
201
cE
16f-''I
I
E
5.
E.12~?j!:.~
:l.
,;
~.
:::l.
. ~.
(O
~;
4"
,1 I
10
;t-:= I
-,
l'
-~jLIr-r-l''-+ .I
VJ
oep t h of Roughness
Final
Polishing
Polishing Steps
Fines!
Grinding
Fine
Polishing
Fine
Grinding
Coarse or
Pre-Polshing
Coarse or
Pre-Grinding :
(up to
I
500.m)
Pumice
Kieselquhr,Tripoli
Sn02
I>1g0
Fe, O,
Cr,O,
Emerv
Natural Corundum
Svnthetic Corundum
BeO
AI 2 0 J
SiC
B4 C
Diamond
=H
II~
I -==:::
-=----,
20
60
70
Particle Size 01 Grinding Compound in ~m
11
for the successful application of abrasive polishing. In practice, the

curves are followed from right to left or from coarser to finer abrasive
sizes. Removal of all deformation is the key to successful optical
measurements and microhardness testing.
lt is not adequate to remo ve roughness (visible scratches) from the
surface without removing the deformed layer as well. Coarse grinding
should be kept to a minimum beca use. there is a tendency to produce
severe deformation. Since depth of deformation decreases sharply after
a particle size of approximately 30 !-Lm, which corresponds to a grit
size of about 400, increased time should be spent in removing previous
damage. Care must be taken to prevent cross contamination of coarse
abrasive particles in the finer steps (careful cleaning between steps!).
A number of parameters are influential during mechanical grinding
and polishing. These will be explained subsequently.
Grinding and Polishing Compounds. Inorganic powders are used as
abrasives in metallography. They are listed in Table 2 in order of increasing
Mohs hardness from pumice (the softest) at the top to diamond (the
hardest) at the bottom. This indicates that a given material is able to
scratch the one aboye it on the scale. AIso shown is Rosiwal's hardness
scale using corundum al 1000 as a reference value.
Figure 10 illustrates the common areas of application for the more
usual grinding and polishing abrasives. In principie, any one abrasive
Depth of
Disturbed Material
+ Deformation
80
I
I
I
I
Fig. 9. Depth of roughness, deformation, and total

depth of disturbed surface layer as a function of
particle size of grinding and polishing compounds.
0.1
Depth of Roughness in 11m
10
Fig. 10. Ranges of application of metallographic grinding and

polishing compounds.
fiIiiiIl
100
10
surface and that grinding scratches have been removed. The scratch
troughs have been filled with material previously protruding aboye the
surface. This is the result of the rolling action of loose, unsupported
abrasive particles in the cloth polishing steps. This filling effect gives
rise to the smeared black layer in Fig. 8. The black region is composed
of severely deformed material from the specimen, mixed with polishing .
compound. Adjacent to this layer is a range of deformed material with
a decreasing severity of deformation toward the interior of the specimen.
Lines of equal deformation do not run parallel to the specimen surface,
but follow the pro fiJe generated by the coarse grinding action.
Varying surface conditions produce different properties such as
electrochemical potentials. Areas having the highest degree of deformation, for example, have the greatest reaction to etching solutions and
are, therefore, dissolved at a higher rateo This is the reason for the
reappearance of scratches on polished surfaces after etching, revealing
poor preparation.
The depth of scratches (roughness) plus the depth of deformaiion
equals the total depth of disturbed material as shown in Fig. 9. This
is based on references from literature using steel as the example. The
depth of roughness is directly proportional to the particle size of the
abrasive, but the depth of deformation approaches a constant value
after the initial increase.
Depth of
Roughness
Depth of
Grinding Steps
An understanding of the relationship illustrated in Fig. 9 is necessary
ti k _. '. .. '. . . '.
201
cE
16f-''I
I
E
5.
E.12~?j!:.~
:l.
,;
~.
:::l.
. ~.
(O
~;
4"
,1 I
10
;t-:= I
-,
l'
-~jLIr-r-l''-+ .I
VJ
oep t h of Roughness
Final
Polishing
Polishing Steps
Fines!
Grinding
Fine
Polishing
Fine
Grinding
Coarse or
Pre-Polshing
Coarse or
Pre-Grinding :
(up to
I
500.m)
Pumice
Kieselquhr,Tripoli
Sn02
I>1g0
Fe, O,
Cr,O,
Emerv
Natural Corundum
Svnthetic Corundum
BeO
AI 2 0 J
SiC
B4 C
Diamond
=H
II~
I -==:::
-=----,
20
60
70
Particle Size 01 Grinding Compound in ~m
11
for the successful application of abrasive polishing. In practice, the

curves are followed from right to left or from coarser to finer abrasive
sizes. Removal of all deformation is the key to successful optical
measurements and microhardness testing.
lt is not adequate to remo ve roughness (visible scratches) from the
surface without removing the deformed layer as well. Coarse grinding
should be kept to a minimum beca use. there is a tendency to produce
severe deformation. Since depth of deformation decreases sharply after
a particle size of approximately 30 !-Lm, which corresponds to a grit
size of about 400, increased time should be spent in removing previous
damage. Care must be taken to prevent cross contamination of coarse
abrasive particles in the finer steps (careful cleaning between steps!).
A number of parameters are influential during mechanical grinding
and polishing. These will be explained subsequently.
Grinding and Polishing Compounds. Inorganic powders are used as
abrasives in metallography. They are listed in Table 2 in order of increasing
Mohs hardness from pumice (the softest) at the top to diamond (the
hardest) at the bottom. This indicates that a given material is able to
scratch the one aboye it on the scale. AIso shown is Rosiwal's hardness
scale using corundum al 1000 as a reference value.
Figure 10 illustrates the common areas of application for the more
usual grinding and polishing abrasives. In principie, any one abrasive
Depth of
Disturbed Material
+ Deformation
80
I
I
I
I
Fig. 9. Depth of roughness, deformation, and total

depth of disturbed surface layer as a function of
particle size of grinding and polishing compounds.
0.1
Depth of Roughness in 11m
10
Fig. 10. Ranges of application of metallographic grinding and

polishing compounds.
fiIiiiIl
100
12
Technical Tips lor Preparaton of Specimens
Table 2. Abrasives and Polishing Compounds

Standard
minerals
of Mohs
seale
Rosiwal
grinding
hardness
Materials for
comparison
Abrasives and
polishing compounds
0.03
2 Gypsum,
rock salt
1.25
Standard
minerals
of Mohs
scale
Remarks
Materials for
.eomparison
4 Fluorspar
5 Apatite
6.5
Marble, brass,
iron, nickel
Steels,
unhardened
Window glass
6 Feldspar
Pumlce (mixtures of
Si02 and AI 20 3).
Mild abrasive.
OccasionalIy
for silver.
Kieselguhr and
tripoli (silicic
aed and alumina
mixtures).
Prepolishing
paste for brass
and preeous
metals.
Tio dioxlde (S002)'
For fme polishing

of ores.
Magoesia (MgO).
For polishing of
magnesium and
a1uminum and
their alloys.
Cerium oxide
(Ce 20 3)
Rarely used in
metallography.
Mostly for glass .
Iroo oxide (Fe 20, ;

polishing red) .
For polishing of
soft metals aod
alloys.
Quartz (Si02, sand).
Not used in
metallography.
37
"
Low-carbon
steels,
hardened
,
7 Quartz
120
.~
'.
175
0.9% C
steel,
hardened;
tungsten
Special steels
Chromium oxide
(Cr203)'
F or polishing of
hard metals and
alloys; for
example, chromium,
steels.
Emery (50-70%
AI 20,; remainder
SiO" Fe, 0, and
Fe 30 4 ) .
Seldom used
abrasive and
polishing compound.
Abrasives and
polishing compounds
Natural corundum
(90-95% AI 2 0 3),
Importaot abrasive foc steel,

cast steel,
sintered metals,
hard steels.
Berylllum oxide
(BeO).
Toxic! For poiishing of

cemented carbides.
Alumioa (A1 2 3;
modification: cubic
'Y-a1umina, hexagonal
<x-alumina).
Commonly used
polishing compound.
Univecsally suitable for metallographic purposes.
Silicoo carbide
(SiC; carborundum).
Commonly used
abrasive.
Universally suitable for metallographic purposes.
Boron carbide
(B. C),
For grinding of
cemented carbides.
Diamood.
For grinding and

polishing of most
metals, g1asses,
preeous stones.
>,
14000
Abrasive wheels
for steels,
brasses, etc.
. Synthetic coruodum
or electrocoruodum
(60-95% A1 20 3;
remaindec Si02, Ti02 ,
Fe 20 3; variatioos:
precious coruodum,
aluodum, and
corundum with
AI203 > 99%).
10 Diamond
Remarks
1000
Aluminum, zinc,
magnesium,
copper, silver,
gold
4.5
8 ropaz
9 Corundum
Rosiwal
grinding
hardness
Lead, tin
3 Calcite
13
Table 2. Abrasives and Polishing Compounds (con(inued)
Graphite
I Talcum
could be used over the en tire range of specimen preparation _ a real

possibility with diamond and alumina. Other abrasives are not as versatile,
due to economics, availability, and efficiency of application. The subdivision into several grinding and polishing steps shown in Fig. 10 is arbitrary
and not intended to be strictly observed; it is presented as a useful
guide in practice.
Uniform particle size ofknown values is essential for good me tallographic abrasives. Different size designations are in use. Figure 11 shows
the relationship between mesh or grit size, emery grade, and true particle
size in microns. Mesh is a number used to denote the size of individual
tll
il
12
Technical Tips lor Preparaton of Specimens
Table 2. Abrasives and Polishing Compounds

Standard
minerals
of Mohs
seale
Rosiwal
grinding
hardness
Materials for
comparison
Abrasives and
polishing compounds
0.03
2 Gypsum,
rock salt
1.25
Standard
minerals
of Mohs
scale
Remarks
Materials for
.eomparison
4 Fluorspar
5 Apatite
6.5
Marble, brass,
iron, nickel
Steels,
unhardened
Window glass
6 Feldspar
Pumlce (mixtures of
Si02 and AI 20 3).
Mild abrasive.
OccasionalIy
for silver.
Kieselguhr and
tripoli (silicic
aed and alumina
mixtures).
Prepolishing
paste for brass
and preeous
metals.
Tio dioxlde (S002)'
For fme polishing

of ores.
Magoesia (MgO).
For polishing of
magnesium and
a1uminum and
their alloys.
Cerium oxide
(Ce 20 3)
Rarely used in
metallography.
Mostly for glass .
Iroo oxide (Fe 20, ;

polishing red) .
For polishing of
soft metals aod
alloys.
Quartz (Si02, sand).
Not used in
metallography.
37
"
Low-carbon
steels,
hardened
,
7 Quartz
120
.~
'.
175
0.9% C
steel,
hardened;
tungsten
Special steels
Chromium oxide
(Cr203)'
F or polishing of
hard metals and
alloys; for
example, chromium,
steels.
Emery (50-70%
AI 20,; remainder
SiO" Fe, 0, and
Fe 30 4 ) .
Seldom used
abrasive and
polishing compound.
Abrasives and
polishing compounds
Natural corundum
(90-95% AI 2 0 3),
Importaot abrasive foc steel,

cast steel,
sintered metals,
hard steels.
Berylllum oxide
(BeO).
Toxic! For poiishing of

cemented carbides.
Alumioa (A1 2 3;
modification: cubic
'Y-a1umina, hexagonal
<x-alumina).
Commonly used
polishing compound.
Univecsally suitable for metallographic purposes.
Silicoo carbide
(SiC; carborundum).
Commonly used
abrasive.
Universally suitable for metallographic purposes.
Boron carbide
(B. C),
For grinding of
cemented carbides.
Diamood.
For grinding and

polishing of most
metals, g1asses,
preeous stones.
>,
14000
Abrasive wheels
for steels,
brasses, etc.
. Synthetic coruodum
or electrocoruodum
(60-95% A1 20 3;
remaindec Si02, Ti02 ,
Fe 20 3; variatioos:
precious coruodum,
aluodum, and
corundum with
AI203 > 99%).
10 Diamond
Remarks
1000
Aluminum, zinc,
magnesium,
copper, silver,
gold
4.5
8 ropaz
9 Corundum
Rosiwal
grinding
hardness
Lead, tin
3 Calcite
13
Table 2. Abrasives and Polishing Compounds (con(inued)
Graphite
I Talcum
could be used over the en tire range of specimen preparation _ a real

possibility with diamond and alumina. Other abrasives are not as versatile,
due to economics, availability, and efficiency of application. The subdivision into several grinding and polishing steps shown in Fig. 10 is arbitrary
and not intended to be strictly observed; it is presented as a useful
guide in practice.
Uniform particle size ofknown values is essential for good me tallographic abrasives. Different size designations are in use. Figure 11 shows
the relationship between mesh or grit size, emery grade, and true particle
size in microns. Mesh is a number used to denote the size of individual
tll
il
14
Fine Grinding
Technical Tps for Preparaton of Specimens

LKough
15
Control of heat at the specimen-abrasive interface.

Control of harmful dust.
ishi,.!!
Longer life for fixed abrasives because removed products are

continuously flushed away.
Pressure, Time, Velocity. Increasing the value of pressure, time, and
velocity generalIy works toward a higher material-removal rate. The
effect on deformation varies such that:
Gl
ao.
lO
Mesh
11 1 1
11111 1 1 fmey
10080 60
40
20
Gr~~~----
jllW
a
~
Porticle Size in I-'m
Fig. 11. Relationship between mesh size,

grit size, emery grade, and particle size
in microns.
abrasive grains. ,\his corresponds to the screen openings per linear inch
in the standard sieve. For example, an abrasive of 320 mesh contains
partieles that will just pass through a screen having 240 openings to
the linear inch"but will be retained by the next-finer, 320-mesh screen.
In addition to ~esh size, grit size and emery grade are also commonly
used as stand~lfds to elassify abras iv e materials.
Sharp edges" high hardness, high coating density, and good bonding
.. to the suppor(tP,aterial substantially increase the cutting rate and reduce
the depth of deformation. Diamond is superior to the other abrasives
because of the.degree to which it meets the aboye requirements.
Grinding and Polishing Fluids. A1though sorne specimen-preparation
work is done in 'ir or inert gas without liquid vehieles, this is the exception.
Normally, all metallographic preparation steps require a liquid vehiele
as a coolant and/or dispersant, causing loose abrasives to be distributed
more uniformly onto eloth surfaces. Wet polishing hasnumerous advantages, which inelude:
Excessive pressure may cause heating and flowed material, which

can cause changes in microstructure. Pressure should not be too
high, especially during polishing.
Short grinding times and long polishing times are preferable (Fig.
9). However, cloth polishing with abrasives other than diamond
should be as brief as possible, because severe relief effects may
result from the differing removal rates for individual microstructural
components.
The harder the specimen material, gene rally the lower the applied
grinding and polishing speed. However this "rule" is only of limited
validity. For sorne extremely hard materials (ceramics, intermetallic
compunds, cemented carbides), higher polishing speeds are preferred in most cases.
Because increased grinding and polishing speeds produce higher
surface temperatures, heat-sensitive materials must be polished at
lower speeds.
Specimen Motion in Grinding and POlishing. The motion of the specitnen
during grinding and polishing operations affects edge retention. For the
best results, the specimen must be held flat against the abrasive surface
at a11 times. To avoid the formation of oriented grinding and polishing
grooves, these operations are best performed by rotating the specimen
90 between each step. When using a wheel for grinding and polishing,
rotating the specimen opposite to the wheel rotation eliminates directional
effects.
Grinding and Polishing Substrates. A wide variety of substrate materials
are used in metallographic specimen preparation. Paper, eloth, metal,
wood, glass, hard rubber, and pitch have a11 been used as supports
in abrasive preparation. Coarse grinding is most commonly performed
on coated paper discs or eloth belts. Fine grinding is usua11y executed
on coated paper abrasives; rough and final polishing is almost always
done on fabrics such as wool, silk, cotton, feIt, and various synthetic
materials. The choice of eloth type is very important; certain eloths
work well in certain applications but not in others. Low-nap eloths are
14
Fine Grinding

LKough
15
Control of heat at the specimen-abrasive interface.

Control of harmful dust.
ishi,.!!
Longer life for fixed abrasives because removed products are

continuously flushed away.
Pressure, Time, Velocity. Increasing the value of pressure, time, and
velocity generalIy works toward a higher material-removal rate. The
effect on deformation varies such that:
Gl
ao.
lO
Mesh
11 1 1
11111 1 1 fmey
10080 60
40
20
Gr~~~----
jllW
a
~
Porticle Size in I-'m
Fig. 11. Relationship between mesh size,

grit size, emery grade, and particle size
in microns.
abrasive grains. ,\his corresponds to the screen openings per linear inch
in the standard sieve. For example, an abrasive of 320 mesh contains
partieles that will just pass through a screen having 240 openings to
the linear inch"but will be retained by the next-finer, 320-mesh screen.
In addition to ~esh size, grit size and emery grade are also commonly
used as stand~lfds to elassify abras iv e materials.
Sharp edges" high hardness, high coating density, and good bonding
.. to the suppor(tP,aterial substantially increase the cutting rate and reduce
the depth of deformation. Diamond is superior to the other abrasives
because of the.degree to which it meets the aboye requirements.
Grinding and Polishing Fluids. A1though sorne specimen-preparation
work is done in 'ir or inert gas without liquid vehieles, this is the exception.
Normally, all metallographic preparation steps require a liquid vehiele
as a coolant and/or dispersant, causing loose abrasives to be distributed
more uniformly onto eloth surfaces. Wet polishing hasnumerous advantages, which inelude:
Excessive pressure may cause heating and flowed material, which

can cause changes in microstructure. Pressure should not be too
high, especially during polishing.
Short grinding times and long polishing times are preferable (Fig.
9). However, cloth polishing with abrasives other than diamond
should be as brief as possible, because severe relief effects may
result from the differing removal rates for individual microstructural
components.
The harder the specimen material, gene rally the lower the applied
grinding and polishing speed. However this "rule" is only of limited
validity. For sorne extremely hard materials (ceramics, intermetallic
compunds, cemented carbides), higher polishing speeds are preferred in most cases.
Because increased grinding and polishing speeds produce higher
surface temperatures, heat-sensitive materials must be polished at
lower speeds.
Specimen Motion in Grinding and POlishing. The motion of the specitnen
during grinding and polishing operations affects edge retention. For the
best results, the specimen must be held flat against the abrasive surface
at a11 times. To avoid the formation of oriented grinding and polishing
grooves, these operations are best performed by rotating the specimen
90 between each step. When using a wheel for grinding and polishing,
rotating the specimen opposite to the wheel rotation eliminates directional
effects.
Grinding and Polishing Substrates. A wide variety of substrate materials
are used in metallographic specimen preparation. Paper, eloth, metal,
wood, glass, hard rubber, and pitch have a11 been used as supports
in abrasive preparation. Coarse grinding is most commonly performed
on coated paper discs or eloth belts. Fine grinding is usua11y executed
on coated paper abrasives; rough and final polishing is almost always
done on fabrics such as wool, silk, cotton, feIt, and various synthetic
materials. The choice of eloth type is very important; certain eloths
work well in certain applications but not in others. Low-nap eloths are

16
17
generally preferred for rough polishing and medium-nap c10ths for final
polishing. Abrasives are usually applied to c10ths in the form of paste
suspensions or slurries.
Thermo
Hard or firm support materials tend to promote deeper deformation .

More elastic support materials favor less deformation but increase
the tendency to relief and edge rounding.
Microtome Cutting
Microtome cutting employs a cemented carbide or diamond knife which
mechanically slices a layer from the bulk material. Although the action
of a microtome is similar to planing or milling, the principies of mechanical
grinding and polishing still apply. High-quality cuts, free from deformation
and flow , are possible with the micro tome only if the cutting angle
is properly adjusted . This technique is particularly useful in cutting
aggregate materials such as lamellar structures, having varying degrees
of hardness. Microtome cutting is, however, restricted to materials of
about 150 HV or less.
Similar to microtome cutting is micromilling. Whereas the knife of
a microtome removes a surface layer by cutting and acts like aplane,
the micromill has a rotating milling head which removes layers 5 to
15 J..I-m in thickness with high precision . As with the cutting knife of
the microtome, the milling tool of the milling device is made of either
diamond or cemented carbide. Micromilling combines all grinding and
polishing operations into one step and produces aplane surface of high
quality with respect to scratches and surface damage.
Electrolytic Grinding and Polishing
Although electrolytic grinding and electroerosive grinding (Fig. 7) are
seldom used, electrolytic polishing is commonly employed. Electrolytic
polishing, also called anodic polishing, occurs through anodic dissolution
of the specimen surface in an electrolytic cell .
Figure 12 is a diagram showing a simple electrolytic cell that is easily
set up in the laboratory. The orientation of the anode (sample) to the
cathode may be adapted to suit the particular application . Commercially
designed and produced instruments are available which are versatile
enough to meet most laboratory requirements .
Electrolytes suitable for metallographic purposes are usually mixtures
of acids su eh as phosphoric, sulfuric, and perchloric in ionizing solutions
such as water, acetic acid, or alcohol. Glycerol, butyl glycol, urea, etc .
are added to in crease the viscosity . Metals which form highly soluble
.---l-----ct---~
Reslst or
-J
Fig. 12. Electrolytic polishing
cell in series mode .
/
Contolner wlth Electrolyte
~ Cooling
Woter
hydroxides are prepared with alkaline solutions, while those forming

highly soluble cyanides are treated in cyanides. Most of the electrolytes
mentioned in Chapters 2 and 3 are harmless when handled according
to known common-sense precautions . Mixtures of perchloric acid,
however, are particularly prone to decompose violently and should,
therefore, be treated with extreme careo (See Appendix A.)
The tendency of perchloric acid mixtures to explode is related to
tbe concentration . This is illustrated in Fig. 13 , the ternary diagram for
perchloric acid, water, and acetic acid. Mixtures outside the irnmediate
danger zone can undergo local changes in concentration by means of
evaporation , temperature increase, contact with organic material, or
contact with bismuth or sparks . If this occurs, the solution may move
into the danger zone without the operator's awareness. To minimize
such dangers, the electrolyte should be sti rred and cooled . In any case,
and at all times, caution is advised when using perchloric acid.
Significant parameters which affect the results of electropolishing are :
Current density (A/cm )

V oltage (V)
Electrolyte composition, temperature , and flow rate
Polishing time
Initial condition of the specimen surface
Cathode size, shape, and composition .
Most formulas in Chapters 2 and 3 specify these details; they are

mitted when they are not critical or can easily be established by the
operator.

16
17
generally preferred for rough polishing and medium-nap c10ths for final
polishing. Abrasives are usually applied to c10ths in the form of paste
suspensions or slurries.
Thermo
Hard or firm support materials tend to promote deeper deformation .

More elastic support materials favor less deformation but increase
the tendency to relief and edge rounding.
Microtome Cutting
Microtome cutting employs a cemented carbide or diamond knife which
mechanically slices a layer from the bulk material. Although the action
of a microtome is similar to planing or milling, the principies of mechanical
grinding and polishing still apply. High-quality cuts, free from deformation
and flow , are possible with the micro tome only if the cutting angle
is properly adjusted . This technique is particularly useful in cutting
aggregate materials such as lamellar structures, having varying degrees
of hardness. Microtome cutting is, however, restricted to materials of
about 150 HV or less.
Similar to microtome cutting is micromilling. Whereas the knife of
a microtome removes a surface layer by cutting and acts like aplane,
the micromill has a rotating milling head which removes layers 5 to
15 J..I-m in thickness with high precision . As with the cutting knife of
the microtome, the milling tool of the milling device is made of either
diamond or cemented carbide. Micromilling combines all grinding and
polishing operations into one step and produces aplane surface of high
quality with respect to scratches and surface damage.
Electrolytic Grinding and Polishing
Although electrolytic grinding and electroerosive grinding (Fig. 7) are
seldom used, electrolytic polishing is commonly employed. Electrolytic
polishing, also called anodic polishing, occurs through anodic dissolution
of the specimen surface in an electrolytic cell .
Figure 12 is a diagram showing a simple electrolytic cell that is easily
set up in the laboratory. The orientation of the anode (sample) to the
cathode may be adapted to suit the particular application . Commercially
designed and produced instruments are available which are versatile
enough to meet most laboratory requirements .
Electrolytes suitable for metallographic purposes are usually mixtures
of acids su eh as phosphoric, sulfuric, and perchloric in ionizing solutions
such as water, acetic acid, or alcohol. Glycerol, butyl glycol, urea, etc .
are added to in crease the viscosity . Metals which form highly soluble
.---l-----ct---~
Reslst or
-J
Fig. 12. Electrolytic polishing
cell in series mode .
/
Contolner wlth Electrolyte
~ Cooling
Woter
hydroxides are prepared with alkaline solutions, while those forming

highly soluble cyanides are treated in cyanides. Most of the electrolytes
mentioned in Chapters 2 and 3 are harmless when handled according
to known common-sense precautions . Mixtures of perchloric acid,
however, are particularly prone to decompose violently and should,
therefore, be treated with extreme careo (See Appendix A.)
The tendency of perchloric acid mixtures to explode is related to
tbe concentration . This is illustrated in Fig. 13 , the ternary diagram for
perchloric acid, water, and acetic acid. Mixtures outside the irnmediate
danger zone can undergo local changes in concentration by means of
evaporation , temperature increase, contact with organic material, or
contact with bismuth or sparks . If this occurs, the solution may move
into the danger zone without the operator's awareness. To minimize
such dangers, the electrolyte should be sti rred and cooled . In any case,
and at all times, caution is advised when using perchloric acid.
Significant parameters which affect the results of electropolishing are :
Current density (A/cm )

V oltage (V)
Electrolyte composition, temperature , and flow rate
Polishing time
Initial condition of the specimen surface
Cathode size, shape, and composition .
Most formulas in Chapters 2 and 3 specify these details; they are

mitted when they are not critical or can easily be established by the
operator.
18
Tecllnical Tips for Preparation of Specimens
HCI04
Commonly Used
Eleetrolytes
-:s:-
c:'-
;\0
,,:
-\0
<;!-
...
. 'o
(CH3CO)20 in Vol.-%
Fig. 13. Explosive, combustible, and harmless compositions of perchloric

acid - acetic anhydride - water mixtures.
Anodie Oisintegration
-Oireet -l'
---Indireet
;O
S
c:
~
Me++ +
"'.........
..
.-
/.
Me +20H-- MeO+H20+2e
I MeO+2H+ _
Me+++H20
I
>{
I
~- ,Me?:Me+++2e j Me
(5
D
I 40H='02+ 2H20 +4e
Suilable
:
t+-Po/ishing Range.......- Oxygen_
I
Formallon
I
-El
iC-- Layer of Reaetion Produels
Polishing-----
....
19
A typical idealized current density versus applied voltage relationship

for many common eIectrolytes is shown in Fig. 14, with four characteristic
regions noted:
----j.,80
"
Vo/tage in V
Fig. 14. Idealized current density versus

applied voltage. See text for discussion.
A fo B. The anode material goes directly into solution. A liquid

layer forms at the surface with a higher metal-ion concentration
than is present in the rest of the solution. Electrolytic etching occurs
in this area.
2 B fo C. It is assumed that formation of a thin layer of reaction
products causes passivity.
3 e fo D. Polishing proceeds due to diffusion and electrochemical
processes.
4 D fo E. Oxygen evolutioil occurs at a low rate, initially. Gas bubbles
adhere to the surface of the anode and remain there for a relatively
long time, with pitting as a resulto With increasing voltage, the rate
of oxygen evolution increases and the bubbles remain for shorter
periods of time, until they do not adhere at all.
A1though anodic polishing begins at point B of the curve, only between

points C and O is there freedom from other negative effects (passivation,
oxygen formation). Metallographic specimen preparaton, therefore, is
concerned with area C-O of the current density versus voltage curve.
Region O-E is rarely used and then only in industrial applications. The
different regions illustrated in Fig. 14 are not always clearly observed.
Electrolytes of high specific resistance produce rather flat curves.
The initial condition of the specimen surface has a definite influence
on the polishing time. In general, the better the surface at the start
and the higher the current density, the shorter the polishing time.
Electrolytic polishing requires electrical conductivity of the sample
material; this is the case for aH metals and aHoys, as well as for sorne
nonmetals, such as carbides and graphite. In principIe, all homogeneous
metals and alloys are suitable for electrolytic preparation; heterogeneous
materials such as gray iron are not ideally suited for electropolishing
due to electrochemical potental differences between the various phases .
However, examples of electropolishing of heterogeneous alloys are
becoming increasingly common. Sorne advantages of electropolishing
are:
Freedom from deformation and flowed material
Rapidity and reproducibility. However, this is only valid if suitable
conditions are established
No (or minimal) surface heating
Capability of sequential electroetching with the same instrument
18
Tecllnical Tips for Preparation of Specimens
HCI04
Commonly Used
Eleetrolytes
-:s:-
c:'-
;\0
,,:
-\0
<;!-
...
. 'o
(CH3CO)20 in Vol.-%
Fig. 13. Explosive, combustible, and harmless compositions of perchloric

acid - acetic anhydride - water mixtures.
Anodie Oisintegration
-Oireet -l'
---Indireet
;O
S
c:
~
Me++ +
"'.........
..
.-
/.
Me +20H-- MeO+H20+2e
I MeO+2H+ _
Me+++H20
I
>{
I
~- ,Me?:Me+++2e j Me
(5
D
I 40H='02+ 2H20 +4e
Suilable
:
t+-Po/ishing Range.......- Oxygen_
I
Formallon
I
-El
iC-- Layer of Reaetion Produels
Polishing-----
....
19
A typical idealized current density versus applied voltage relationship

for many common eIectrolytes is shown in Fig. 14, with four characteristic
regions noted:
----j.,80
"
Vo/tage in V
Fig. 14. Idealized current density versus

applied voltage. See text for discussion.
A fo B. The anode material goes directly into solution. A liquid

layer forms at the surface with a higher metal-ion concentration
than is present in the rest of the solution. Electrolytic etching occurs
in this area.
2 B fo C. It is assumed that formation of a thin layer of reaction
products causes passivity.
3 e fo D. Polishing proceeds due to diffusion and electrochemical
processes.
4 D fo E. Oxygen evolutioil occurs at a low rate, initially. Gas bubbles
adhere to the surface of the anode and remain there for a relatively
long time, with pitting as a resulto With increasing voltage, the rate
of oxygen evolution increases and the bubbles remain for shorter
periods of time, until they do not adhere at all.
A1though anodic polishing begins at point B of the curve, only between

points C and O is there freedom from other negative effects (passivation,
oxygen formation). Metallographic specimen preparaton, therefore, is
concerned with area C-O of the current density versus voltage curve.
Region O-E is rarely used and then only in industrial applications. The
different regions illustrated in Fig. 14 are not always clearly observed.
Electrolytes of high specific resistance produce rather flat curves.
The initial condition of the specimen surface has a definite influence
on the polishing time. In general, the better the surface at the start
and the higher the current density, the shorter the polishing time.
Electrolytic polishing requires electrical conductivity of the sample
material; this is the case for aH metals and aHoys, as well as for sorne
nonmetals, such as carbides and graphite. In principIe, all homogeneous
metals and alloys are suitable for electrolytic preparation; heterogeneous
materials such as gray iron are not ideally suited for electropolishing
due to electrochemical potental differences between the various phases .
However, examples of electropolishing of heterogeneous alloys are
becoming increasingly common. Sorne advantages of electropolishing
are:
Freedom from deformation and flowed material
Rapidity and reproducibility. However, this is only valid if suitable
conditions are established
No (or minimal) surface heating
Capability of sequential electroetching with the same instrument
20
Possible removal of mechanical damage caused by mechanical

grinding and polishing.
In spite of many advantages, chemical polishing is seldom used for

metallographic preparation. This may be due to a lack of awareness
by practicing metallographers, and by the limited number of published
formulas .
Edges are selectively attacked, producing a radius and resulting

in poor edge preservtion.
Macroscopic out-of-flatness cannot be remedied.
Residues may be deposited on the surface during polishing.
Oxidarion of sorne specimens may interrupt the process.
If the mounting material is nonconductive, special mounting procedures are necessary to produce electroconductivity.
Coarse-grain materials are less suited for electropolishing.
Depressions may occur around inclusions because of the higher
solution rates of the metallic material in that zone.
Combination Polishing Methods

When a single method of specimen preparation fails to produce the
desired results, a combination of methods may work very well. Sorne
examples are described below.
Etch-Polishing Sequence. Flowed metal layers may be effectively removed by lightly etching and mechanical repolishing one or more times
at the conclusion of final mechanical polishing.
Attack-PoJishing. This consists of the simultaneous application of a
chemical etchant during the final polishing sequence; it is especially
use fuI in avoiding flow layers on soft metal s and alloys as well as refractory
metals.
Multiple'PoJishing. When electrolytic polishing is used with heterogeneous aIloys, sorne undesirable surface effects like relief formation or ,
surface layers may be produced. A brief intermediate mechanical polishing
step may remo ve this condition and produce a satisfactory finish.
Electrolytic Lapping. This is the simultaneous electrolytic and mechanical removal of material. In this technique, the specimen (anode)
is held against a cloth saturated with electrolyte and mounted on a
support or wheel which serves as the cathode . This method, illustrated
in Fig. 15, is considered semiautomatic. Although direct current is most
frequently used in electrolytic lapping, low-frequency alternating current
produces superior results with sorne metals, such as molybdenum,
Chemical Polishing
:;,
Simplicit" and economy

Lile pre-preparation required; 320-grit finish is adequate; specimens
cut with 'an abrasive cutoff wheel may be polished without further
preparatin
Simple treatment after polishing; in most cases, rinsing in water
'is adequate
No deformation or flow lines produced
Specimen and/or mount need not be electrical conductors.
Polish ing Disc (Colhode)
Disadvantages of chemical polishing are:

Higher rate of attack at edges
21
Orange-peel effect with coarse-grain materials

Only small-scale roughness may be smoothed out
Formation of a surface film composed of reaction products.
Restrictions on the use of electropolishing are imposed by the lack

of etchants for many heterogeneous alloys as well as by the following
disadvantages:
Chemical polishing is a process by which simple immersion of a

specimen in a suitable polishing solution (electrolyte) produces a polished
surface without the use of externally applied current. When the specimen
is agitated in the polishing bath (seconds to minutes), surface roughness
is removed and a deformation-free polished surface is produced.
The polishing solutions almost always contain oxidizing agents such
as nitrie, sulfuric, and chromic acids or hydrogen peroxide. Viscous
agents are also added to control diffusion and convection rates, producing
a more uniform process. Phosphoric acid, for example, forms a liquid
film of high viscosity when reacting with metal ions. Most chemical
polishing solu~ions are quite insensitive to concentration changes.
The advan\ages of ehemical polishing are:
Fig. 15. Electrolytic lapping.
..
,i'rj
;",~b l
20
Possible removal of mechanical damage caused by mechanical

grinding and polishing.
In spite of many advantages, chemical polishing is seldom used for

metallographic preparation. This may be due to a lack of awareness
by practicing metallographers, and by the limited number of published
formulas .
Edges are selectively attacked, producing a radius and resulting

in poor edge preservtion.
Macroscopic out-of-flatness cannot be remedied.
Residues may be deposited on the surface during polishing.
Oxidarion of sorne specimens may interrupt the process.
If the mounting material is nonconductive, special mounting procedures are necessary to produce electroconductivity.
Coarse-grain materials are less suited for electropolishing.
Depressions may occur around inclusions because of the higher
solution rates of the metallic material in that zone.
Combination Polishing Methods

When a single method of specimen preparation fails to produce the
desired results, a combination of methods may work very well. Sorne
examples are described below.
Etch-Polishing Sequence. Flowed metal layers may be effectively removed by lightly etching and mechanical repolishing one or more times
at the conclusion of final mechanical polishing.
Attack-PoJishing. This consists of the simultaneous application of a
chemical etchant during the final polishing sequence; it is especially
use fuI in avoiding flow layers on soft metal s and alloys as well as refractory
metals.
Multiple'PoJishing. When electrolytic polishing is used with heterogeneous aIloys, sorne undesirable surface effects like relief formation or ,
surface layers may be produced. A brief intermediate mechanical polishing
step may remo ve this condition and produce a satisfactory finish.
Electrolytic Lapping. This is the simultaneous electrolytic and mechanical removal of material. In this technique, the specimen (anode)
is held against a cloth saturated with electrolyte and mounted on a
support or wheel which serves as the cathode . This method, illustrated
in Fig. 15, is considered semiautomatic. Although direct current is most
frequently used in electrolytic lapping, low-frequency alternating current
produces superior results with sorne metals, such as molybdenum,
Chemical Polishing
:;,
Simplicit" and economy

Lile pre-preparation required; 320-grit finish is adequate; specimens
cut with 'an abrasive cutoff wheel may be polished without further
preparatin
Simple treatment after polishing; in most cases, rinsing in water
'is adequate
No deformation or flow lines produced
Specimen and/or mount need not be electrical conductors.
Polish ing Disc (Colhode)
Disadvantages of chemical polishing are:

Higher rate of attack at edges
21
Orange-peel effect with coarse-grain materials

Only small-scale roughness may be smoothed out
Formation of a surface film composed of reaction products.
Restrictions on the use of electropolishing are imposed by the lack

of etchants for many heterogeneous alloys as well as by the following
disadvantages:
Chemical polishing is a process by which simple immersion of a

specimen in a suitable polishing solution (electrolyte) produces a polished
surface without the use of externally applied current. When the specimen
is agitated in the polishing bath (seconds to minutes), surface roughness
is removed and a deformation-free polished surface is produced.
The polishing solutions almost always contain oxidizing agents such
as nitrie, sulfuric, and chromic acids or hydrogen peroxide. Viscous
agents are also added to control diffusion and convection rates, producing
a more uniform process. Phosphoric acid, for example, forms a liquid
film of high viscosity when reacting with metal ions. Most chemical
polishing solu~ions are quite insensitive to concentration changes.
The advan\ages of ehemical polishing are:
Fig. 15. Electrolytic lapping.
..
,i'rj
;",~b l
22

tungsten, and rhenium. Dilute solutions of sodium thiosulfate, nitnc

acid, oxalic acid, piric acid, and hydrogen peroxide are suitable for
both electrolytic lapping and etching. The addition of abrasives such
as alumina has no effect in most applications.
Electrolytic lapping combines the advantages and disadvantages of
electrochemical and mechanical polishing. It can be used for heterogeneous as well as homogeneous metals and alloys, and has pro ven
successful as an addition to other methods; in sorne cases, it succeeds
when electrolytic or mechanical polishing alone fails.
Automatic Grinding and Polishing

Manual specimen preparation tends to be routine, monotonous, and
even tedious. This is espeeially .true of mechanical polishing. When
operators beeome tired and disinterested, the work they produce may
decrease in quality and volume. Preparation errors are more likely to
oecur, whieh can ultimately result in erroneous interpretations. Thus,
it is understandable that again and again attempts have been made to
automate the mechanieal fine grinding and polishing steps.
Prior to 1950, manual preparation was the only means eonsidered
. satisfactory for the sensitive grinding and polishing steps. Since then,
there has be en a considerable upswing in the development of preeision
instruments for automation of metallographie preparation. For the most
part, these have been confined to individual steps; and, to this date,
no satisfactory fully automatie system has been deve1oped. Speeimens
must still be handled between steps, but the ideal system would be
to insert samples at one end and remove completely polished specimens
at the other end. This would be particularly helpful in preparing matefals
requiring numerous lengthy steps. Nevertheless, the automation of the
single steps inereases quality, volume, and uniformity by removing most
of the physieal ef(ort from specimen preparation.
Evaluation of Po/~hing Methods

Reflectivity of the finish-polished surfaee is one sensllve eriterion
for judging quality. Deviations from the reflectivity of ideal surfaces
with an atomie Toughness give an indication of the effeet of different
polishing methods; for example, cleavage surfaces of crystals or surfaces
of single crystals ' grown under an ultrahigh vaeuum are good referenee
standards. Therefore, reflectivity is suitable in evaluating the effectiveness of in.dividual polishing methods.
Figure 16 shows the mean deviation, in percentage of refleetivity,
of polished surfaces from ideal surfaces of various materials. The base
line represents refleetivity values for freshly cleaved surfaces-the ideal
Ir
<l
t?2Z:zI
23
Fblished with Alumina
---.. Electralytically Lapped

+ - - + Diamond Polished
I:r----. Cut by Microtome

10
5.
0--0
Electrolytically Fblished
WiiJ
+--+
~
~I:::.
0-0
O'
Cu
z:::=g
Au
<==
+--+
tr--I:::.
Ag
&--1:::.
0--0
Bi
Ni
Sb 2 S3
Fig. 16. Mean deviations ilR, in percentage of reflectivity,

of a polished surface from an ideal surface.
values of surfacequality obtainable. Meandeviations fordifferent

polishing methods are plotted for different materials.
Obviously, any polishing treatment will produce a lower quality than
the ideal cleaved surface. Of the popular polishing techniques, alumina
polishing produces the poorest values while electrolytic and diamond-knife
microtoming will produce results approaehing the ideal values.
It is also obvious from Fig. 16 that the effectiveness of different
polishing methods varies from material to material. Antimony trioxide
(Sb2 0 3 ), for example, shows the same deviation when prepared with
alu mina slurries as gold and copper do after eleetrolytic polishing.
Properties other than refleetivity are also affected by the polishing
teehnique. Severe grinding and polishing stresses ha ve a notieeable affect
on microhardness. When reporting surfaee condition, information coneerning the grinding and polishing techniques should be included. Differenees in actual results compared with expeeted results may stem
from differences in the manner of preparation. For routine preparation
and examination of mieroseetions, these eonsiderations are of secondary
importance. AlUIll,ina and other oxides are widely used beeause they
produce acceptable results at a reasonable cost.
Cleaning (Fig. 17)

Cleanliness is an important requirement for sueeessful metallography.
Speeimens must be cleaned after each step; alI grains from one grinding
.111 ,
22

tungsten, and rhenium. Dilute solutions of sodium thiosulfate, nitnc

acid, oxalic acid, piric acid, and hydrogen peroxide are suitable for
both electrolytic lapping and etching. The addition of abrasives such
as alumina has no effect in most applications.
Electrolytic lapping combines the advantages and disadvantages of
electrochemical and mechanical polishing. It can be used for heterogeneous as well as homogeneous metals and alloys, and has pro ven
successful as an addition to other methods; in sorne cases, it succeeds
when electrolytic or mechanical polishing alone fails.
Automatic Grinding and Polishing

Manual specimen preparation tends to be routine, monotonous, and
even tedious. This is espeeially .true of mechanical polishing. When
operators beeome tired and disinterested, the work they produce may
decrease in quality and volume. Preparation errors are more likely to
oecur, whieh can ultimately result in erroneous interpretations. Thus,
it is understandable that again and again attempts have been made to
automate the mechanieal fine grinding and polishing steps.
Prior to 1950, manual preparation was the only means eonsidered
. satisfactory for the sensitive grinding and polishing steps. Since then,
there has be en a considerable upswing in the development of preeision
instruments for automation of metallographie preparation. For the most
part, these have been confined to individual steps; and, to this date,
no satisfactory fully automatie system has been deve1oped. Speeimens
must still be handled between steps, but the ideal system would be
to insert samples at one end and remove completely polished specimens
at the other end. This would be particularly helpful in preparing matefals
requiring numerous lengthy steps. Nevertheless, the automation of the
single steps inereases quality, volume, and uniformity by removing most
of the physieal ef(ort from specimen preparation.
Evaluation of Po/~hing Methods

Reflectivity of the finish-polished surfaee is one sensllve eriterion
for judging quality. Deviations from the reflectivity of ideal surfaces
with an atomie Toughness give an indication of the effeet of different
polishing methods; for example, cleavage surfaces of crystals or surfaces
of single crystals ' grown under an ultrahigh vaeuum are good referenee
standards. Therefore, reflectivity is suitable in evaluating the effectiveness of in.dividual polishing methods.
Figure 16 shows the mean deviation, in percentage of refleetivity,
of polished surfaces from ideal surfaces of various materials. The base
line represents refleetivity values for freshly cleaved surfaces-the ideal
Ir
<l
t?2Z:zI
23
Fblished with Alumina
---.. Electralytically Lapped

+ - - + Diamond Polished
I:r----. Cut by Microtome

10
5.
0--0
Electrolytically Fblished
WiiJ
+--+
~
~I:::.
0-0
O'
Cu
z:::=g
Au
<==
+--+
tr--I:::.
Ag
&--1:::.
0--0
Bi
Ni
Sb 2 S3
Fig. 16. Mean deviations ilR, in percentage of reflectivity,

of a polished surface from an ideal surface.
values of surfacequality obtainable. Meandeviations fordifferent

polishing methods are plotted for different materials.
Obviously, any polishing treatment will produce a lower quality than
the ideal cleaved surface. Of the popular polishing techniques, alumina
polishing produces the poorest values while electrolytic and diamond-knife
microtoming will produce results approaehing the ideal values.
It is also obvious from Fig. 16 that the effectiveness of different
polishing methods varies from material to material. Antimony trioxide
(Sb2 0 3 ), for example, shows the same deviation when prepared with
alu mina slurries as gold and copper do after eleetrolytic polishing.
Properties other than refleetivity are also affected by the polishing
teehnique. Severe grinding and polishing stresses ha ve a notieeable affect
on microhardness. When reporting surfaee condition, information coneerning the grinding and polishing techniques should be included. Differenees in actual results compared with expeeted results may stem
from differences in the manner of preparation. For routine preparation
and examination of mieroseetions, these eonsiderations are of secondary
importance. AlUIll,ina and other oxides are widely used beeause they
produce acceptable results at a reasonable cost.
Cleaning (Fig. 17)

Cleanliness is an important requirement for sueeessful metallography.
Speeimens must be cleaned after each step; alI grains from one grinding
.111 ,
24
CLEANING
I
Blow-Off
Wipe-Off
Dissolving
Electrolytie
ETCHING
Ultrasonic
Drying
Without
Changing
Optical
Etehing
Emulsifying
Fig. 17. Methods of cleaning metallographic specimens.
and polishing step must be completely removed from the specimen to

avoid contamination, which would reduce the efficiency of the next
preparation step. Thorough cleaning is particularly critical after rme
grinding and before rough polishing and all subsequent steps.
CIean, grease-free surfaces are essentiaI for subsequent chemical or
electrolytic treatment. Residues, fingerprints, and inconspicuous ftlms
may interfere with etching, causing various areas to be attacked at
different rates. Every single microsection-preparation procedure must
be followed by thorough cleaning, which can be performed in different
ways.
Rnsing is inost frequent1y used and consists of holding the specimen
under a stream of running water and wiping the surface wth a soft
brush or cotton swab.
Ultrasonic cleaning is the most effective and thorough method of
cleaning. Not only are surface contaminants removed, but particulate
matter held in crevices, cracks, or pores is removed by the action of
cavitation. UsualIy this ultrasonic cleaning needs only 10 to 30 s.
After cleaning" specimens may be dried rapidly by rinsing in alcohol,
benzene, or other low-boiling-point liquids, then placed under a hot-air
drier for sufficient time to vaporize liquids remaining in cracks and
pores.
i
Etching (Fig. 18)

'"
25
'1- - - - -.J - - - - - - 1
J
Rinsing
Although ceJi~in information may be obtained from as-polished specimens, the microstructure is usualIy visible only after etching. Only
features which. exhibit a significant difference in reflectivity (10% or
greater) can be viewed without etching. This is true of microstructural
features with strong color differences or with large differences in hardness
causing relief formation. Cracks, pores, pits, and nonmetallic inclusions
may be observed in the as-polished condition.
In most cases, a polished specimen will not exhibit its microstructure
because incident light is uniformly reflected. Since small differences
Fiel~
Dark
Polarized Light
Phase Contrast
Interference Contrast
Surfaee
of
With
Mierosedion
I
Elec!roehemical
Etching
Anodizing
Physieal
Etehing
IClassical Chem. Ion

Etehif1g
Etehing
Potentiostatie
Etching
Thermal
Etehing
Evaporation 01
I nterference
Layers
Fig. 18. Methods of metallographic etching.
in reflectivity cannot be recognized by the human eye, some means

of producing image contrast must be employed. A1though this has become
known as "etching" in metallography, it does not aIways refer to seIective
chemical dissolution of various structural features.
There are numerous ways of achieving contrast. These methods may
be classified as "optical," "eIectrochemicaI (chemicaI)," or "physicaI,"
depending on whether the process alte"rs the surface oi leaVes it intact.
Optical Etching
"OpticaI etching" is based on the appIication of certain illumination
methods, alI of which use the "KohIer" illumination principIe. This
principIe also underIies common bright-fieId illumination. These illumination modes are dark fieId, poIarized Iight, phase contrast, and interference
contrast. Theyare available in many commercially produced microscopes,
and in most cases, the mode may be put into operation with a few
simple manipulations; in other cases, it involves the addition of accessories. Image quality is not reduced significant1y, although the intensity
of the light at the image pIane is affected considerabIy by using different
illumination modes. These illumination possibilities are not yet as fully
exploited as one would assume, judging from the simplicity of manipulation and the dependability of the results. There is a distinct advantage
in employing optical etching rather than those techniques which alter
the specimen surface. Chemical and physical etching require considerable
time and effort and there is always a danger of producing artifacts
which lead to misinterpretations.
Electrochemical (Chemical) Etching

During the process of electrochemical etching (often termed "chemical"
etching) of metallic specimens, reduction and oxidation pro ces ses (redox
24
CLEANING
I
Blow-Off
Wipe-Off
Dissolving
Electrolytie
ETCHING
Ultrasonic
Drying
Without
Changing
Optical
Etehing
Emulsifying
Fig. 17. Methods of cleaning metallographic specimens.
and polishing step must be completely removed from the specimen to

avoid contamination, which would reduce the efficiency of the next
preparation step. Thorough cleaning is particularly critical after rme
grinding and before rough polishing and all subsequent steps.
CIean, grease-free surfaces are essentiaI for subsequent chemical or
electrolytic treatment. Residues, fingerprints, and inconspicuous ftlms
may interfere with etching, causing various areas to be attacked at
different rates. Every single microsection-preparation procedure must
be followed by thorough cleaning, which can be performed in different
ways.
Rnsing is inost frequent1y used and consists of holding the specimen
under a stream of running water and wiping the surface wth a soft
brush or cotton swab.
Ultrasonic cleaning is the most effective and thorough method of
cleaning. Not only are surface contaminants removed, but particulate
matter held in crevices, cracks, or pores is removed by the action of
cavitation. UsualIy this ultrasonic cleaning needs only 10 to 30 s.
After cleaning" specimens may be dried rapidly by rinsing in alcohol,
benzene, or other low-boiling-point liquids, then placed under a hot-air
drier for sufficient time to vaporize liquids remaining in cracks and
pores.
i
Etching (Fig. 18)

'"
25
'1- - - - -.J - - - - - - 1
J
Rinsing
Although ceJi~in information may be obtained from as-polished specimens, the microstructure is usualIy visible only after etching. Only
features which. exhibit a significant difference in reflectivity (10% or
greater) can be viewed without etching. This is true of microstructural
features with strong color differences or with large differences in hardness
causing relief formation. Cracks, pores, pits, and nonmetallic inclusions
may be observed in the as-polished condition.
In most cases, a polished specimen will not exhibit its microstructure
because incident light is uniformly reflected. Since small differences
Fiel~
Dark
Polarized Light
Phase Contrast
Interference Contrast
Surfaee
of
With
Mierosedion
I
Elec!roehemical
Etching
Anodizing
Physieal
Etehing
IClassical Chem. Ion

Etehif1g
Etehing
Potentiostatie
Etching
Thermal
Etehing
Evaporation 01
I nterference
Layers
Fig. 18. Methods of metallographic etching.
in reflectivity cannot be recognized by the human eye, some means

of producing image contrast must be employed. A1though this has become
known as "etching" in metallography, it does not aIways refer to seIective
chemical dissolution of various structural features.
There are numerous ways of achieving contrast. These methods may
be classified as "optical," "eIectrochemicaI (chemicaI)," or "physicaI,"
depending on whether the process alte"rs the surface oi leaVes it intact.
Optical Etching
"OpticaI etching" is based on the appIication of certain illumination
methods, alI of which use the "KohIer" illumination principIe. This
principIe also underIies common bright-fieId illumination. These illumination modes are dark fieId, poIarized Iight, phase contrast, and interference
contrast. Theyare available in many commercially produced microscopes,
and in most cases, the mode may be put into operation with a few
simple manipulations; in other cases, it involves the addition of accessories. Image quality is not reduced significant1y, although the intensity
of the light at the image pIane is affected considerabIy by using different
illumination modes. These illumination possibilities are not yet as fully
exploited as one would assume, judging from the simplicity of manipulation and the dependability of the results. There is a distinct advantage
in employing optical etching rather than those techniques which alter
the specimen surface. Chemical and physical etching require considerable
time and effort and there is always a danger of producing artifacts
which lead to misinterpretations.
Electrochemical (Chemical) Etching

During the process of electrochemical etching (often termed "chemical"
etching) of metallic specimens, reduction and oxidation pro ces ses (redox
26
processes)* take place. AH metals in contact with the solutions ha ve

a pronounced tendency to become ionized by releasing (losing) electrons.
The degree to which this reaction takes place may he recorded by
measuring the electrochemical potental. This i8 done by comparing the
potental of metal versus the standard potental of a reference electrode. t
The fabulation of various metals results in the electromotive series of
elements:
Li+, Na+, K+, Ca++, Ba++, Be++, Mg++, AI+++, Mn++, Zn++, Cr+++,
Cd++, TI+, Co++, Ni++, Pb++, Fe+++, H+, Sn ++++ , Sb+++', Bi+++, As+'>+,
Cu++, Ag+, Hg++, Au+++, Pt+++ .
The elements are listed in order of decreasing electroaffinity. AH

elements preceding hydrogen ar~ attacked by acids with the evolution
of hydrogen (Hz). AH elements following hydrogen cannot be attacked
without the addition of an oxidizing agent. Thus, microstructural elements
of different electrochemical potental are attacked at different rates.
This produces differental etching, resulting in microstructural contrast.
Electrochemical etching maybe considered as "forced corrosion."
The differences in potential of the microstructural elements cause a
'subdivision into a network of very small anodic or cathodic regions
(local elements). These miniature ceHs cannot orginate from differences
in phase composition only, but also have to come from irregularities
in the crystal structure as they are present-for example, at grain
boundaries and from other inhomogeneities such as:
Inhomogeneities resulting fromdeformation (deformed zones), which
are less resistant to attack than undeformed material.
Unevenness in the formation of oxidation layers (glossy areas are
les s resistant).
Concentration fluctuation in the electrolyte (low concentration is
less resistant).
Differences in elctrolyte velocity (higher circulation rates reduce
resistance to atta:ck).
Differenc~s in tlie oxygen content of the electrolyte (aerated solutions
are more resistint).
'
',.
* Reduction
...
= absorption of electrons (cathodic reaction)

Oxidation = emission of eletrons (anodic reaction)
Oxidizing
agent + electron ~ reducing agent
Fe 3 +
+ 'e "
~
Fe 2 +
Electrolytic grinding and polishing, chemical polishing, and some of the combined
methods are based on redox processes. This is not always obvious from convention&1
terminology.
'
tHydrogen electrode: a sheet of platnum surrounded by hydrogen at 1 atm pressure
and imrnersed into an aqueous solulion ofhydrogen-ion activity aH = l.
f
27
Differences in the illuminaton intensity, which can initiate differences in potential.

Because of differences in potential between microstructural features,
dissolutibn of the surface proceeds at differentrates, producing contrast.
Contrast can also originate from layers formed simultaneously with
material dissolution. This is true in precipitation etching and ,heat tinting
where surface reactions are involved. In precipitation (deposit) etching,
the material is first dissolved at the surface; it then reacts with certain
components of the etchant to form insoluble compounds. These
compounds precipitate selectively on the surface, causing interference
colors or heavy layers of a specific color. During heat tinting, coloration
of the surface takes place at different rates according to the reaction
characteristics of different microstructural elements under the given
conditions of atmosphere and temperature.
A wide variety of etchants is available, including acids, bases, neutral
solutions, mixtures of solutions, molten salts and gases; many examples
of these are given in Chapters 2 and 3. Most of these formulas were
derived empirically. Their composition and mode of application can
be easily varied and modified, and so also be usefulfor materials other
than those mentioned in the formulas. The rate of attack is mainly
determined by the degree of dissociation of the etchant and its electrical
conductvity. Both are often influenced in a certain way by small additions
of other chemicals. This may explain why many formulas contain small
amounts of substances whose significance is not immediately apparent.
The stability of many etching solutions is limited; redox potentials
change with time. Changes may also occur while the etchant is in use,
such that it must be discarded after a limited time.
Btching times range from several seconds to some hours. When no
instructions are given, progress is judged by the appearance of the surface
during etching. Usually, the surface will become less refIective (duHer)
as etching proceeds. Etching time and temperature are closely related;
by increasing the temperature, the time can usually be decreased.
However, this may not be advisable because the contrast could become
uneven when the rate of attack is too rapid. Most etching is performed
at room temperature.
Sources of error are numerous, especially in electrochemical etching.
Etching errors may lead to microstructural misinterpretation. For exampie, precipitates from etching or washing solutions could be interpreted
as additional phases.
Conventional chemical etching is the oldest and most commonly applied
technique for producing microstructural contrast. In this technique, the
JI' ..
!Iij
't
26
processes)* take place. AH metals in contact with the solutions ha ve

a pronounced tendency to become ionized by releasing (losing) electrons.
The degree to which this reaction takes place may he recorded by
measuring the electrochemical potental. This i8 done by comparing the
potental of metal versus the standard potental of a reference electrode. t
The fabulation of various metals results in the electromotive series of
elements:
Li+, Na+, K+, Ca++, Ba++, Be++, Mg++, AI+++, Mn++, Zn++, Cr+++,
Cd++, TI+, Co++, Ni++, Pb++, Fe+++, H+, Sn ++++ , Sb+++', Bi+++, As+'>+,
Cu++, Ag+, Hg++, Au+++, Pt+++ .
The elements are listed in order of decreasing electroaffinity. AH

elements preceding hydrogen ar~ attacked by acids with the evolution
of hydrogen (Hz). AH elements following hydrogen cannot be attacked
without the addition of an oxidizing agent. Thus, microstructural elements
of different electrochemical potental are attacked at different rates.
This produces differental etching, resulting in microstructural contrast.
Electrochemical etching maybe considered as "forced corrosion."
The differences in potential of the microstructural elements cause a
'subdivision into a network of very small anodic or cathodic regions
(local elements). These miniature ceHs cannot orginate from differences
in phase composition only, but also have to come from irregularities
in the crystal structure as they are present-for example, at grain
boundaries and from other inhomogeneities such as:
Inhomogeneities resulting fromdeformation (deformed zones), which
are less resistant to attack than undeformed material.
Unevenness in the formation of oxidation layers (glossy areas are
les s resistant).
Concentration fluctuation in the electrolyte (low concentration is
less resistant).
Differences in elctrolyte velocity (higher circulation rates reduce
resistance to atta:ck).
Differenc~s in tlie oxygen content of the electrolyte (aerated solutions
are more resistint).
'
',.
* Reduction
...
= absorption of electrons (cathodic reaction)

Oxidation = emission of eletrons (anodic reaction)
Oxidizing
agent + electron ~ reducing agent
Fe 3 +
+ 'e "
~
Fe 2 +
Electrolytic grinding and polishing, chemical polishing, and some of the combined
methods are based on redox processes. This is not always obvious from convention&1
terminology.
'
tHydrogen electrode: a sheet of platnum surrounded by hydrogen at 1 atm pressure
and imrnersed into an aqueous solulion ofhydrogen-ion activity aH = l.
f
27
Differences in the illuminaton intensity, which can initiate differences in potential.

Because of differences in potential between microstructural features,
dissolutibn of the surface proceeds at differentrates, producing contrast.
Contrast can also originate from layers formed simultaneously with
material dissolution. This is true in precipitation etching and ,heat tinting
where surface reactions are involved. In precipitation (deposit) etching,
the material is first dissolved at the surface; it then reacts with certain
components of the etchant to form insoluble compounds. These
compounds precipitate selectively on the surface, causing interference
colors or heavy layers of a specific color. During heat tinting, coloration
of the surface takes place at different rates according to the reaction
characteristics of different microstructural elements under the given
conditions of atmosphere and temperature.
A wide variety of etchants is available, including acids, bases, neutral
solutions, mixtures of solutions, molten salts and gases; many examples
of these are given in Chapters 2 and 3. Most of these formulas were
derived empirically. Their composition and mode of application can
be easily varied and modified, and so also be usefulfor materials other
than those mentioned in the formulas. The rate of attack is mainly
determined by the degree of dissociation of the etchant and its electrical
conductvity. Both are often influenced in a certain way by small additions
of other chemicals. This may explain why many formulas contain small
amounts of substances whose significance is not immediately apparent.
The stability of many etching solutions is limited; redox potentials
change with time. Changes may also occur while the etchant is in use,
such that it must be discarded after a limited time.
Btching times range from several seconds to some hours. When no
instructions are given, progress is judged by the appearance of the surface
during etching. Usually, the surface will become less refIective (duHer)
as etching proceeds. Etching time and temperature are closely related;
by increasing the temperature, the time can usually be decreased.
However, this may not be advisable because the contrast could become
uneven when the rate of attack is too rapid. Most etching is performed
at room temperature.
Sources of error are numerous, especially in electrochemical etching.
Etching errors may lead to microstructural misinterpretation. For exampie, precipitates from etching or washing solutions could be interpreted
as additional phases.
Conventional chemical etching is the oldest and most commonly applied
technique for producing microstructural contrast. In this technique, the
JI' ..
!Iij
't
28
lO
etchant reacts witb the specimen surface without tbe use of an external
cur-ent supply. Etching proceeds by selective dissolution according to
the electrocbemical cbaracteristic of the component areas.
'
In e/ectrolytic or anodic etching, an electrical potential is applied to
the specimen by means of an external circuit. Figure 12 illusttates a
typical setup consisting of tbe specimen (anode) and its counterelectrode
(cathode) immersed in an electrolyte (etchant). During anodic etching,
positive metal ions leave the specimen surface and diffuse into the
electrolyte with an equivalent number of electrons remaining in the
material. This results in a direct etching ,process shown as segment A-B
of the current density versus voltage curve in Fig. 14. Sample dissolution
of material without the formation of a layer occurs in this instance.
If, however, the metal ions leaving the material react with nonmetal
ions from the electrolyte with formation of an insoluble compound,
precipitated layers ofvarying thickness will form on the specimen surface.
The thickness of these layers is a function of the composition and
orientation of the microstructural features exposed to the solution. These
layers may reveal interference color hues due to variation ,in thickness,
determined by the underlying microstructure. When this variation of
electrolyticetcbingoccurs, it isreferred to as anodizing. Comparable
nonelectrolytic processes are heat tinting and deposit etching.
Potentiostatic etching is an advanced form of electrolytic etching, which
produces the ultimate etching contrast through highly controlled conditions. The potential of the specimen, which would usually change with
changes of electrolyte concentration, is maintained at a fixed level through
the use of a potentiostat and suitable reference standards. Clearly
pronounced contrast can be obtained with this method where tbis is
otherwise not p0ssible. In some cases, tbe cell current can be maintained
with a coulombmeter to determine the extent of etching (controlled
etching).
On completion of any chemical or electrochemical etching process,
the specimen ihould be rinsed in clean water to remove the chemicals
and Stol" any reactions from proceeding further. Sometimes, for example,
in etching for, segregations usg the Oberhoffer metbod, it is advisable
to rinse in alohol first. Otherwise, copper could precipitate on the
specimen surface because of the change in the degree of dissociation.
After specimens are water rinsed, they should be rinsed in alcohol and
dried in a stre,a m of warm air. The use of alcohol speeds up the drying,
action and prevents the formation of water spots. If etching produces
water-soluble layers, water must be avoided in the rinsing step. Mounted
specimens mus be cleaned thorougbly to avoid the destructive effects
of etchants and solvents seeping from pores, cracks, or clamp interfaces.
Technical Tips for Preparaion of Specimens
29
It may be helpful to use an ultrasonic cleaner to avoid these problems.

If specimens are of a high porosity or if highly concentrated acids are
used for etching (as for example, for deep etching), it is advisable to
neutralize the chemicals befo re rinsing and drying the specimen.
Physical Etching
Basic physical phenomena are also oH en used to develop structural

contrast, mainly when conventional chemical or electrolytic techniques
fail. They have the advantage of leaving surfaces free from chemical
residues and also offer advantages where electrochemical etching is
difficult-for example, when there is an extremely large difference in
electrochemical potential between microstructural elements, or when
chemical etchants produce ruinous stains or residues. Some probable
applications of these methods are plated layers, welds joining highly
dissimilar materials, porous materials, and ceramics.
Cathodic vacuum etching, also referred to as ion etching, produces
structural contrast by selective removal of atoms from the sample surface.
This is accomplished by using high-energy ions (such as argon) accelerated
by voltages of 1 to 10 kV. Individual atoms are removed at various
rates, depending on the microstructural details such as crystal orientation '
of the individual grains, grain boundaries, etc.
Thermal etching, used in high-temperature (hot-stage) microscopy, is
also partly based on atoms leaving the material surface, as a result
of additional energy. The predominant force in thermal etching, however,
is the formation of slightly curved equilibrium surfaces having individual
grains with minimum surface tension.
Structural contrast produced by evaporated interference /ayers is often
considered to be an optical method. Since no modification in the optical
path of the microscope is made, it is considered here as a physical
technique. Tbis is rational since the polished specimen is treated in
a way which distinguishes it from optical etching. The surface of tbe
speciInen is coated under vacuum with an evaporated layer of material,
producing interference effects. High refractive index materials, such
as ZnSe, Ti0 2 , etc., are commonly used. The effect of the evaporated
interference layer is caused by multiple light reflection produced at the
interface between object and evaporated layer (Fig. 19).
Gas-reaction chambers are a recent development which permit precise
control of evaporation during simultaneous microscopic observation.
Specimen Storage
When polished and etched specimens are to be stored for long periods
of tiIlle, they must be protected from atmospheric corrosion. Desiccators
28
lO
etchant reacts witb the specimen surface without tbe use of an external
cur-ent supply. Etching proceeds by selective dissolution according to
the electrocbemical cbaracteristic of the component areas.
'
In e/ectrolytic or anodic etching, an electrical potential is applied to
the specimen by means of an external circuit. Figure 12 illusttates a
typical setup consisting of tbe specimen (anode) and its counterelectrode
(cathode) immersed in an electrolyte (etchant). During anodic etching,
positive metal ions leave the specimen surface and diffuse into the
electrolyte with an equivalent number of electrons remaining in the
material. This results in a direct etching ,process shown as segment A-B
of the current density versus voltage curve in Fig. 14. Sample dissolution
of material without the formation of a layer occurs in this instance.
If, however, the metal ions leaving the material react with nonmetal
ions from the electrolyte with formation of an insoluble compound,
precipitated layers ofvarying thickness will form on the specimen surface.
The thickness of these layers is a function of the composition and
orientation of the microstructural features exposed to the solution. These
layers may reveal interference color hues due to variation ,in thickness,
determined by the underlying microstructure. When this variation of
electrolyticetcbingoccurs, it isreferred to as anodizing. Comparable
nonelectrolytic processes are heat tinting and deposit etching.
Potentiostatic etching is an advanced form of electrolytic etching, which
produces the ultimate etching contrast through highly controlled conditions. The potential of the specimen, which would usually change with
changes of electrolyte concentration, is maintained at a fixed level through
the use of a potentiostat and suitable reference standards. Clearly
pronounced contrast can be obtained with this method where tbis is
otherwise not p0ssible. In some cases, tbe cell current can be maintained
with a coulombmeter to determine the extent of etching (controlled
etching).
On completion of any chemical or electrochemical etching process,
the specimen ihould be rinsed in clean water to remove the chemicals
and Stol" any reactions from proceeding further. Sometimes, for example,
in etching for, segregations usg the Oberhoffer metbod, it is advisable
to rinse in alohol first. Otherwise, copper could precipitate on the
specimen surface because of the change in the degree of dissociation.
After specimens are water rinsed, they should be rinsed in alcohol and
dried in a stre,a m of warm air. The use of alcohol speeds up the drying,
action and prevents the formation of water spots. If etching produces
water-soluble layers, water must be avoided in the rinsing step. Mounted
specimens mus be cleaned thorougbly to avoid the destructive effects
of etchants and solvents seeping from pores, cracks, or clamp interfaces.
Technical Tips for Preparaion of Specimens
29
It may be helpful to use an ultrasonic cleaner to avoid these problems.

If specimens are of a high porosity or if highly concentrated acids are
used for etching (as for example, for deep etching), it is advisable to
neutralize the chemicals befo re rinsing and drying the specimen.
Physical Etching
Basic physical phenomena are also oH en used to develop structural

contrast, mainly when conventional chemical or electrolytic techniques
fail. They have the advantage of leaving surfaces free from chemical
residues and also offer advantages where electrochemical etching is
difficult-for example, when there is an extremely large difference in
electrochemical potential between microstructural elements, or when
chemical etchants produce ruinous stains or residues. Some probable
applications of these methods are plated layers, welds joining highly
dissimilar materials, porous materials, and ceramics.
Cathodic vacuum etching, also referred to as ion etching, produces
structural contrast by selective removal of atoms from the sample surface.
This is accomplished by using high-energy ions (such as argon) accelerated
by voltages of 1 to 10 kV. Individual atoms are removed at various
rates, depending on the microstructural details such as crystal orientation '
of the individual grains, grain boundaries, etc.
Thermal etching, used in high-temperature (hot-stage) microscopy, is
also partly based on atoms leaving the material surface, as a result
of additional energy. The predominant force in thermal etching, however,
is the formation of slightly curved equilibrium surfaces having individual
grains with minimum surface tension.
Structural contrast produced by evaporated interference /ayers is often
considered to be an optical method. Since no modification in the optical
path of the microscope is made, it is considered here as a physical
technique. Tbis is rational since the polished specimen is treated in
a way which distinguishes it from optical etching. The surface of tbe
speciInen is coated under vacuum with an evaporated layer of material,
producing interference effects. High refractive index materials, such
as ZnSe, Ti0 2 , etc., are commonly used. The effect of the evaporated
interference layer is caused by multiple light reflection produced at the
interface between object and evaporated layer (Fig. 19).
Gas-reaction chambers are a recent development which permit precise
control of evaporation during simultaneous microscopic observation.
Specimen Storage
When polished and etched specimens are to be stored for long periods
of tiIlle, they must be protected from atmospheric corrosion. Desiccators
30
and desiccator cab~ets are the most common means of specimen storage,
although plastic coatings and cellophane tape are sometimes used.
Reproducibility in, Etching

For the most part, metallographic etching continues to be an empirical
method with overtones of black magic. This condition is the result of
the' abundance of etching methods, nonuniform nomenclature and,
frequentIy, the lack of knowledge concerning etchant mechanisms. For
these reasons, it is difficult to present a cIear review of etching processes.
Conventional etching, in particular, is difficult to reproduce, regardless
of its simplicity. During the electrochernical processes, numerous side
effects must be taken into account. For example, changes in the electrolyte
and inhibiting reactions at the specimen surface must be considered,
which cause polarization phenomena, overpotential, etc.
With the goal of achieving more reproducible and dependable structural
contrast, various new methods have been developed in recent years.
Electrolytic potentiostatic etching, ion etching, and evaporation of interference layers are advanced methods gradually becoming accepted. The
principIes by which these techniques operate are illustrated in Fig. 19.
In the frst two methods, the microstructure becomes visible through
selective removal of the surface. In the last method, the contrast is
produced by multiple refIection of the light beam in the evaporated
layer of a material with high refractive indexo
The development of more reproducible and contrasting etching methods
is of particular importance for quantitative image analysis. These instruments are used to automatically determine the area fraction of various
phases and are not sensitive to subtle differences. Therefore, sharply
reproducible etching. contrast is necessary to obtain accurate information.
+
C<Jlomel
Electl'ode
lans
~llL
l
'i;i
,.
.
'i
(,,) Somple Rotenfjo! Ep
Sampfe
Efectrolyt(; Potentiostafie
Efching
tJR I tJR O
R::: ReflecfMfy
,.
'"
1 1 1
I~
Sample
Ion Etching
Sampfe
Evaporafion of Interference
Layers
Fig. 19. Three methods for reproducible metallographic etching.

-{
31
Etching Nomenclature
A cIassification of the most commonly used terms is possible on the
basis of distinctive features. A distinction has already been made between
optical, electrochemical, and physical etching on the basis of the kinetic
phenomena occurring at the sample surface. Further distinctions are
listed in Table 3, and explained in the next section. Often, terms are
used which refer to the major component of the etchant (for example,
dilute nitric acid, aqua regia, sodium thiosulfate, etc.), to the originator
of the etchant (for example, Oberhbff~r, Vilella, Murakami, Heyn, etc.),
or to alloys or chief constituents for which the etchant is intended (for
example, carbide, phosphide, steel etchant, etc.).
The multiplicity of terms is confusing because several different terms
may apply to the same phenomenon. The same phenomena can be named
according to different viewpoints, without converse limitation or exclusion
of notation. Steels, for example, may be etched using either chemical
or electrochemical tnethods; the microstructure may be revealed either
by dissolution or precipitation phenomena; it may display distinct grain
boundaries and / or colored grains, microstructures and / or macrostructures; combinations of etching procedures may be used, usually in order
of increasing ' severity. Steel etchlng, therefore, can be generated by
practically any of the etching methods, using one of the many suitable
etchants under one of the many suitable conditions. AH have one ultimate
goal: to produce a structure with sufficient contrast to delineate as much
detail as possible. Table 3 summarizes the etching terminology and how
the terms are related.
I
ti"
Explanation 01 Etching Terms

anodic etching. Developmenl of microstruclure by selective dissolulion of the
polished surface under application of a direct current. Variation with layer
formation: anodizing.
attack-polishing. Simultaneous etching and mechanical polishing.
cathodic etching. See ion etching.
cold etching. Development of microstructure at room temperature and below.
controlled etching. Electrolytic etching with selection of suitable etchant and
voltage resulting in a balance between current and dissolved metal ions.
crystal-figure ''etching. Discontinuity in etching depending on crystal orientation.
Distinctve sectional figures form at polished surface. Closely re1ated to
dislocation etching.
deep etching. MacroetchiIig, especially for steels, to determine the over-all
character of the material (presence of imperfections such as seams, forging
bursts, shrinkage-void remnants, cracks, coring).
dislocation etching. Etching of exit points of dislocations on a surface. Depends
on the strain fie1d ranging over a distan ce of several atoms. Crystal figures
(etch pits) are formed at exit points. For example, etch pits for cubic materials
are cube faces .
1"
i:
tl',l .
30
and desiccator cab~ets are the most common means of specimen storage,
although plastic coatings and cellophane tape are sometimes used.
Reproducibility in, Etching

For the most part, metallographic etching continues to be an empirical
method with overtones of black magic. This condition is the result of
the' abundance of etching methods, nonuniform nomenclature and,
frequentIy, the lack of knowledge concerning etchant mechanisms. For
these reasons, it is difficult to present a cIear review of etching processes.
Conventional etching, in particular, is difficult to reproduce, regardless
of its simplicity. During the electrochernical processes, numerous side
effects must be taken into account. For example, changes in the electrolyte
and inhibiting reactions at the specimen surface must be considered,
which cause polarization phenomena, overpotential, etc.
With the goal of achieving more reproducible and dependable structural
contrast, various new methods have been developed in recent years.
Electrolytic potentiostatic etching, ion etching, and evaporation of interference layers are advanced methods gradually becoming accepted. The
principIes by which these techniques operate are illustrated in Fig. 19.
In the frst two methods, the microstructure becomes visible through
selective removal of the surface. In the last method, the contrast is
produced by multiple refIection of the light beam in the evaporated
layer of a material with high refractive indexo
The development of more reproducible and contrasting etching methods
is of particular importance for quantitative image analysis. These instruments are used to automatically determine the area fraction of various
phases and are not sensitive to subtle differences. Therefore, sharply
reproducible etching. contrast is necessary to obtain accurate information.
+
C<Jlomel
Electl'ode
lans
~llL
l
'i;i
,.
.
'i
(,,) Somple Rotenfjo! Ep
Sampfe
Efectrolyt(; Potentiostafie
Efching
tJR I tJR O
R::: ReflecfMfy
,.
'"
1 1 1
I~
Sample
Ion Etching
Sampfe
Evaporafion of Interference
Layers
Fig. 19. Three methods for reproducible metallographic etching.

-{
31
Etching Nomenclature
A cIassification of the most commonly used terms is possible on the
basis of distinctive features. A distinction has already been made between
optical, electrochemical, and physical etching on the basis of the kinetic
phenomena occurring at the sample surface. Further distinctions are
listed in Table 3, and explained in the next section. Often, terms are
used which refer to the major component of the etchant (for example,
dilute nitric acid, aqua regia, sodium thiosulfate, etc.), to the originator
of the etchant (for example, Oberhbff~r, Vilella, Murakami, Heyn, etc.),
or to alloys or chief constituents for which the etchant is intended (for
example, carbide, phosphide, steel etchant, etc.).
The multiplicity of terms is confusing because several different terms
may apply to the same phenomenon. The same phenomena can be named
according to different viewpoints, without converse limitation or exclusion
of notation. Steels, for example, may be etched using either chemical
or electrochemical tnethods; the microstructure may be revealed either
by dissolution or precipitation phenomena; it may display distinct grain
boundaries and / or colored grains, microstructures and / or macrostructures; combinations of etching procedures may be used, usually in order
of increasing ' severity. Steel etchlng, therefore, can be generated by
practically any of the etching methods, using one of the many suitable
etchants under one of the many suitable conditions. AH have one ultimate
goal: to produce a structure with sufficient contrast to delineate as much
detail as possible. Table 3 summarizes the etching terminology and how
the terms are related.
I
ti"
Explanation 01 Etching Terms

anodic etching. Developmenl of microstruclure by selective dissolulion of the
polished surface under application of a direct current. Variation with layer
formation: anodizing.
attack-polishing. Simultaneous etching and mechanical polishing.
cathodic etching. See ion etching.
cold etching. Development of microstructure at room temperature and below.
controlled etching. Electrolytic etching with selection of suitable etchant and
voltage resulting in a balance between current and dissolved metal ions.
crystal-figure ''etching. Discontinuity in etching depending on crystal orientation.
Distinctve sectional figures form at polished surface. Closely re1ated to
dislocation etching.
deep etching. MacroetchiIig, especially for steels, to determine the over-all
character of the material (presence of imperfections such as seams, forging
bursts, shrinkage-void remnants, cracks, coring).
dislocation etching. Etching of exit points of dislocations on a surface. Depends
on the strain fie1d ranging over a distan ce of several atoms. Crystal figures
(etch pits) are formed at exit points. For example, etch pits for cubic materials
are cube faces .
1"
i:
tl',l .
32
x
~
v
"...
~
...:;
'"::.
.g
.~
::os
t 00:.0
'O' 8 g .S ~
~ .~ 'S ~ - o
~
><!.~
"'" . ... c: G) CIJ
g,~
8.
'g;S
8",,,,:; os ...
r-o'"
",1
~~++
c.o
.5
..c
~
~
y
-==f
.-
<1)
N~
()- ~UI\4l""'00
;::+++++++
:::+I++++++
~ 1 + 1 1 1 1 ++ 1
:::++++++ 1 +++
::: + 1 + + + + + 1 + 1 +.
~+II+++++I+I+
~++ 11 +++++ 1 +++
::)+++I I ++II+I+++
~ 1 +++ 111111111 + 1
;::;1111++1++111++11
.sbD
-; 'El
-
~
~
.5
~:.a.g] g o :;
bO=""-,,8
.$ asC)~
bO o 6b s" ..c:
.;::: "
O"as .... "' ..... b08 bObOC:: osOS
~ 0=
= C:: ' ~ '" c::
; ~ :a 13 :a :a Sg
~III++III+I+++II++
~III++++II++II+++++
S
cd~U1B.Bot~
'"c:> ..d,
=
uri~:;:~~u.... . !::
'"
'"
'C
;>
l.'"
-==
'"'"
:a='"=
",1++
1 1 1+
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;;; + + 1 1 1 +
='=-0,>
:;~] o [~~.~
",!:!os~ ..cqi~g
cQ)o~~~Q./
0 ..... S8_"
K
.::;:O ..... '-''''C''tjf.nG)
u::':=-gc::os S
~9V1o==~a
o '...... =.~ rJl Q) ... ~
t) gb.g td "'C E3 ~ E
c;g~-
00 111 11+++ 1 1+++1+1+++

~
11+++++++++++++++++
~+
11111+++1++++++1+ 1 1
~++1 1 1 111+++1++++++1+++
~1 1 1 I 1111++++1++++++1+++
-:> _::::::_:>:>+1
~1 1 1 111111++++1++++++++++
~I 1 1 1111111++++1++++++++++
=11+11111111++++1++++++++++
S++++++++++I+++++++++I 1 1 1++1
'" 1 +++++++++++ 1 +++++ 1 +++++++ 1 +
00+++++++++++++++++++++++++++++
r- 1 ++++++++++ 11 +++++++++++++++++
-0+++++++++++++++++++++++++++++++
~I+++++++++++++++++++++++++++++++
~++++++I 1 1 1++1+++11++++11+++++1+++
~I+++++++++++++I 1 1+++++++++++++++++
",+++++++++++++++1+1+1++++11++11+++++
_1++++++++++++++++11++1++++++++++1+++
.~
l !:!
Q
:c'"
QI)
bO
=
.f
_ j : au
bD
t)
bI)""
.SbD,-.. ~Su
bO
:au c::bO
bO
,S ~ bO
= ~ .9tIO bO
~ fj:a
_ u . ~..
..c: c::
U "'..c::: wu
(.) bI) ' -
d " : : : ' oooI
bO .
~
bO
I
.o
.S
_
~ c::
c::bO
..s= o
:.aC:lti
.- " '_~13
.=
bO .... .
B'Q)
bO.5' o~
~_vB 5bOvd-5
Q)
.... ....
b.O bO..... b.Q
...
..::: = d
..d o
=..c::
bO t..:I CIl el.) u..d = '- ...
c::bObO""bObOc::C::"=bO<I)
",:aObOU~
:auo<l)c::~os~
u_=fj"
,S1g
3.5 E 8 ~.$ ,~:fi :E.~ OS) ~ ~ o.
~~ '~ -g:a
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~ 8 as
..... =-..dQ,) .... o.J:: 't "' .... .-I()c::._=O"
0t::;-O
b,Q
uo_ooo
:- 1 .E
~ B 4' ~ t)" 2
g ~ i> oc: ~:.E ~.~:ti ',= '-= ~ =~ -al:: 'O G).o o ca ~ 8.!a4 ' ::: ~]
i~_"~!~~bb<l)~..c:<I)i~~]~ ... 5i~~ti~S.S=2!5~~0
.~ . ~ ~ e] o o o:.:;; ~ ~ ~ !:! ~ t ::: c:: ~ ,,1l (5 'C ~ o ~ o <1) ~ ~ c.~ <I).E :;'C
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~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
,
________
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NNNNNNNNNMMM~MMMMM
:;:
33
dissolution etching. Development of microstructure by surface removal.

double etching. Use of two etching solutions in sequence. The second etchant
stress es a particular microstructural feature.
drop etching. Placing of a drop of etchant on the polished surface. Suitable
forprecious etchants.
dry etching. Development of microstructure under the influence of gases .
electrochemical (chemical) etching. General expression for a11 developments of
microstructure through reduction and oxidation processes (redox reactions).
electrolytic etching. See anodic etching.
etch rinsing. Pouring etchant over tilted surface until desired degree of attack
is achieved. Used for etchants witli severe gas formation.
eutectic-cell etching. Development of eutectic cells (grains).
grain-boundary etching. Development of intersections of grain faces with the
polished surface. Because of severe, localized crystal deformation, grain
boundaries have higher dissolution potential than grains themselves. Accumulation of impurities in grain boundaries increases this effect .
grain-contrast etching. Development of grain surfaces lying in the polished surface
of the microsection. These become visible through differences in reflectivity
caused by reaction products on the surface or by differences in roughness.
heat tinting. Formation of colors (interference colors) in air or other gases,
mostly at elevated temperature.
hot etching. Development and stabilization of the microstructure at elevated
temperature in etchants or gases.
.identification etching. Etchingtoexpose particular microconstituents;all others
remain unaffected.
immersion etching. Method in which a microsection is dipped into etching solution
face up and is moved around during etching. This is the most common etching
method.
immersion etching, cyclic. Alternate immersion into two etchants: (1) actual
etchant; (2) solution used to dissolve layer formed during process l.
ion etching. Surface remo val by bombarding with accelerated ions in vacuum
(1 to 10 kV).
long-term etching. Etching times of a few minutes to hours.
macroetching. Development .of macrostructure for viewing with the unaided eye,
or under lens magnifications up to 25 x (50x in Europe).
microetching. Development of microstructure for microscopic examination.
Usual magnification of more than 25x (50x in Europe).
multiple etching. Treatment of microsection sequentially with specific reagents
attacking distinct microconstituents.
network etching. Formation of networks, especially in mild steels, after etching
in nitric acid. These networks relate to subgrain boundaries .
optical etching. Development of microstructure under application of special
illumination techniques (dark field, phase contrast, interference contrast,
polarized light).
physical etching. Development of microstructure through removal of atoms from
surface or lowering the grain-surface potential.
potentiostatic etching. Anodic development of microstructure at a constant
potential. By adjusting thepotential, a defined etching of singular phases
is possible.
precipitation etching. Development of microstructure through formation of reac-
~' I 'll,
32
x
~
v
"...
~
...:;
'"::.
.g
.~
::os
t 00:.0
'O' 8 g .S ~
~ .~ 'S ~ - o
~
><!.~
"'" . ... c: G) CIJ
g,~
8.
'g;S
8",,,,:; os ...
r-o'"
",1
~~++
c.o
.5
..c
~
~
y
-==f
.-
<1)
N~
()- ~UI\4l""'00
;::+++++++
:::+I++++++
~ 1 + 1 1 1 1 ++ 1
:::++++++ 1 +++
::: + 1 + + + + + 1 + 1 +.
~+II+++++I+I+
~++ 11 +++++ 1 +++
::)+++I I ++II+I+++
~ 1 +++ 111111111 + 1
;::;1111++1++111++11
.sbD
-; 'El
-
~
~
.5
~:.a.g] g o :;
bO=""-,,8
.$ asC)~
bO o 6b s" ..c:
.;::: "
O"as .... "' ..... b08 bObOC:: osOS
~ 0=
= C:: ' ~ '" c::
; ~ :a 13 :a :a Sg
~III++III+I+++II++
~III++++II++II+++++
S
cd~U1B.Bot~
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=
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-==
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u::':=-gc::os S
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t) gb.g td "'C E3 ~ E
c;g~-
00 111 11+++ 1 1+++1+1+++

~
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~1 1 1 I 1111++++1++++++1+++
-:> _::::::_:>:>+1
~1 1 1 111111++++1++++++++++
~I 1 1 1111111++++1++++++++++
=11+11111111++++1++++++++++
S++++++++++I+++++++++I 1 1 1++1
'" 1 +++++++++++ 1 +++++ 1 +++++++ 1 +
00+++++++++++++++++++++++++++++
r- 1 ++++++++++ 11 +++++++++++++++++
-0+++++++++++++++++++++++++++++++
~I+++++++++++++++++++++++++++++++
~++++++I 1 1 1++1+++11++++11+++++1+++
~I+++++++++++++I 1 1+++++++++++++++++
",+++++++++++++++1+1+1++++11++11+++++
_1++++++++++++++++11++1++++++++++1+++
.~
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Q
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bO
=
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_ j : au
bD
t)
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bO
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= ~ .9tIO bO
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=..c::
bO t..:I CIl el.) u..d = '- ...
c::bObO""bObOc::C::"=bO<I)
",:aObOU~
:auo<l)c::~os~
u_=fj"
,S1g
3.5 E 8 ~.$ ,~:fi :E.~ OS) ~ ~ o.
~~ '~ -g:a
~.-~uo
~ 8 as
..... =-..dQ,) .... o.J:: 't "' .... .-I()c::._=O"
0t::;-O
b,Q
uo_ooo
:- 1 .E
~ B 4' ~ t)" 2
g ~ i> oc: ~:.E ~.~:ti ',= '-= ~ =~ -al:: 'O G).o o ca ~ 8.!a4 ' ::: ~]
i~_"~!~~bb<l)~..c:<I)i~~]~ ... 5i~~ti~S.S=2!5~~0
.~ . ~ ~ e] o o o:.:;; ~ ~ ~ !:! ~ t ::: c:: ~ ,,1l (5 'C ~ o ~ o <1) ~ ~ c.~ <I).E :;'C
'-r
. ....
.-1
'8
's,.
,oof
=_
aE
'
C~~Q~~u=~~_c~_~u=....~~~C~_UQCCUCZ~~~~
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
,
________
_~
=:::
==
2:: . :>
NNNNNNNNNMMM~MMMMM
:;:
33
dissolution etching. Development of microstructure by surface removal.

double etching. Use of two etching solutions in sequence. The second etchant
stress es a particular microstructural feature.
drop etching. Placing of a drop of etchant on the polished surface. Suitable
forprecious etchants.
dry etching. Development of microstructure under the influence of gases .
electrochemical (chemical) etching. General expression for a11 developments of
microstructure through reduction and oxidation processes (redox reactions).
electrolytic etching. See anodic etching.
etch rinsing. Pouring etchant over tilted surface until desired degree of attack
is achieved. Used for etchants witli severe gas formation.
eutectic-cell etching. Development of eutectic cells (grains).
grain-boundary etching. Development of intersections of grain faces with the
polished surface. Because of severe, localized crystal deformation, grain
boundaries have higher dissolution potential than grains themselves. Accumulation of impurities in grain boundaries increases this effect .
grain-contrast etching. Development of grain surfaces lying in the polished surface
of the microsection. These become visible through differences in reflectivity
caused by reaction products on the surface or by differences in roughness.
heat tinting. Formation of colors (interference colors) in air or other gases,
mostly at elevated temperature.
hot etching. Development and stabilization of the microstructure at elevated
temperature in etchants or gases.
.identification etching. Etchingtoexpose particular microconstituents;all others
remain unaffected.
immersion etching. Method in which a microsection is dipped into etching solution
face up and is moved around during etching. This is the most common etching
method.
immersion etching, cyclic. Alternate immersion into two etchants: (1) actual
etchant; (2) solution used to dissolve layer formed during process l.
ion etching. Surface remo val by bombarding with accelerated ions in vacuum
(1 to 10 kV).
long-term etching. Etching times of a few minutes to hours.
macroetching. Development .of macrostructure for viewing with the unaided eye,
or under lens magnifications up to 25 x (50x in Europe).
microetching. Development of microstructure for microscopic examination.
Usual magnification of more than 25x (50x in Europe).
multiple etching. Treatment of microsection sequentially with specific reagents
attacking distinct microconstituents.
network etching. Formation of networks, especially in mild steels, after etching
in nitric acid. These networks relate to subgrain boundaries .
optical etching. Development of microstructure under application of special
illumination techniques (dark field, phase contrast, interference contrast,
polarized light).
physical etching. Development of microstructure through removal of atoms from
surface or lowering the grain-surface potential.
potentiostatic etching. Anodic development of microstructure at a constant
potential. By adjusting thepotential, a defined etching of singular phases
is possible.
precipitation etching. Development of microstructure through formation of reac-
~' I 'll,
34
Technical Tips for Preparation 0# Specimens
ton products at the ~urface of the microsection. (See also staining. )

primary etching. Deve!opment of cast structures including coring.
printing. A method in which a carrier material is soaked with an etchant and
pressed againsl the surfa~e of the specimen. The etchant reacts with one
of the phases. Substances form which react with the carrier material. These
eave behind a life-size image. Used for exposing particular elements-for
example, sulfur (sulfur prints).
secondary etching. Development of microstructures deviating from primary
structure through transformation and heat treatment in the solid state.
segregation (coring) etching. Development of segregation (coring) mainly in
macrostructures and microstructures of castings.
short-term etching. Etching times of seconds to a few minutes.
shrink etching. Precipitation on grain surfaces. Shrinkage takes place during
drying, which causes a cracking of the layer formed during etching. Crack
orientation depends on the underlying structure.
staining. Precipitation etching that causes contrast by distinctive staining of
microconstituents; different interference colors originate from surface layers
of varying thickness. Proof of inhomogeneities.
strain etching. Etching that renders information on deformed and undeformed
areas ifpresent side by side. In strained areas, more compounds are precipitated.
swabbing. Wiping of the specimen surface with a cotton ball saturated with
etchant to simultaneously remove reaction products.
thermal etching. Annealing of the specimen in vacuum or inert atmosphere .
Used primarily in high-temperature microscopy.
.
tinting. See heat tinting.
wet etching. Development of microstructure with liquids (acids, bases, neutral
solutions, mixtures of solutions).
wipe etching. See swabbing.
Nondestructive Metallographic Testing

Large structures or machines may be tested metallographically without
destructive preparation. This may be accomplished by using portable
devices which are either electrolytic or abrasive in principIe. Surfaces
prepared in thi!i manner must then be examined at the site by using
a portable micro~cope placed on, or attached to, the object.
Replicas are sometimes an advantage because they may be made in
situ, and then taken to the laboratory for observation under more favorable
"' conditions. Witli this technique, pie ces of cellulose acetate or nitrate
are softened on one face with a suitable solvent and pressed against
a polished ' surface. The soft plastic surface flows to conform to the
features o the,-sample. When it is dry, the plastic replica is removed
from the su'rface and taken to the laboratory for viewing by transmitted
and incident light. For increased contrast, carbon or metal may be
evaporated onto the surface to produce shadowing. Another method
of producing replicas employs an aluminum strip coated with plastic.
35
This product yields excellent image quality with no preparation other

than the in~tial contact step .
Other applications of the replication technique include determinations
of surface roughness and the making of observations in otherwise
inaccessible areas. Radioactiye materials are a particularly interesting
application, since the replicas are practically unaffected by the radiation
and can be handled with greater safe~y . As soon as the replicas are
moved from the otherwise hazardous environment, they are much safer
to use. Fractures are still another nseful application, although considerable
ca re must be taken when stripping replicas from coarse fracture surfaces.
Curved surfaces can behandled more easily because the replica may
be flattened out for use under the microscope.
ChapteF 2:
Preparation of Metals and Alloys

The preparation procedures and e'tching reagents described in the tables
that follow have be en used successfully in rnany applications. Naturally,
sorne modifications may be desirable or neeessary under certain circumstances. Because of normal variations in any individual technique and
the many variables in the processes, even proven etchants may fail.
The metallographer must be prepared to rnake any adjustments required
to find a satisfactory solution to his immediate problem. Etchant compositions which contain directions within parentheses-for example, "(concentration is variable)" - may require sorne experimentation to determine
the exact formula. The general material headings are only a guideline
for locating the best family of etch~nts. Wide variations in alloy composition within these areas will strongly affeet the final choice of etChing
reagents. Only etchants with proven instruetions for use have be en listed.
Many of the listed reagents and test materials are hazardous; these
are identified by three exclamation marks (!!I). Appendix A contains
more extensive directions, which must be earefully observed.
Sil ver
Silver is extremely ductile. Deeply damaged layers are easily formed during
preparation of microsections. Abrasive particles and polishing compounds tend
tobecome embedded in the surface. Care must be taken during mechanical
grinding and polishing. Silver forms water-insoluble halides, hydroxides, and
carbonates (avoid tap water). Silver alloys usualIy do not cause as much difficulty.
Silver compounds are often explosive, particularly in the dry state.
Macroetching
'A'
Preparation:
Wet grinding (using distilled water) on already used silicon carbide papers down to 600
grit (coating the paper with wax possibly helps).
Etching:
No.
Etchant
Ag
MI
Methanol (95%)
Nitric acid (1.40)
95 inl
10 mI
37
Conditions
Remarks
Several mino
Pure Ag and lowalloy Ag.

Grain contras!.
Preparation of Al
38
Ag
Microetching
m3
Preparation:
Grinding:
a. Wet on silieon earbide papers down to 600 grit (eoat papers with wax; use distilled
water).
b. Prepare by mierotome, using eutters of eemented earbides or, better stiU, diamond.
AIso useful for aU silver aUoys with a hardness below 150 HV.
polishing:
a. Usealumina or diamond paste down to fmest particle size. An eteh-polishing sequenee
or multiple polishing, using one of the listed mieroetehants, helps to deerease the
deformed layer.
b. Eleetrolytie:
1000 mi 10 min,
!!! See Appendix A.
l . Dist. water
37 g 2.5-3 V de,
Potassium eyanide
38 g . Ag cathode.
Potassium carbonate
35 g
Silver eyanide
200 mi 4-6 min, approx 40 oC
2. Dist. water
380 mi (100 F),
Ethanol (96%)
400 mi 2.5- 3 V de,
Phosphorie acid (1.71)
Al eathode.
!!! See Appendix A.
1000
mi
Approx I min,
3. Dist. water
2.5
V
de,
100
g
Sodium eyanide
100 g graphite eathod~ .
potassium ferrocyanide
e . Eleetrolytie lapping:
1000 mi 2-5 min,
Dist. water
2
12 g 6-8 mA/em
Sodium thiosulfate
2g
Thiourea
I g
Copper (H) nitrate
d. Chemieal:
!!! See Appendix A.
800 mI
Dist. water
Sal. aqueous sol. of
100 mi
ehromium (VI) oxide
45 mi
Hydroehlorie aeid ~IO%)
Etching:
No.
Ag
mi
A-
Ag
m2
39
Preparation?f Ag
I
Etehan~1
;
Dist. water '.jo

Sulfurie acid ( .84)
ChroIrlium (VI) oxide
(Coneentratiop. variable)
Sulfurie aeid (1. 84)
Sal. aqueous sol. oC
potassium dichromate
sodium ehloride
Conditions
lOO mI Up to I mino
2-11 mi !!! See Appendix A.
2g
10 mI Sees to mins, 1:9

dilution with dist.
water. Possibly
100 ml without sulfurie aeid.
Remarks
Predominantly used
for Ag alloys, espeeiaUy Ag-Ni alloys
and Ag-Mg-Ni
alloys .
Pure Ag and Ag
alloys .
Ag solders.
Ag
m4
Ag
mS
Ag
m6
Ag
rr;.7
Ag
m8
Ag
m9
Ammonia water
Potassium eyanide
100 mi 30 s to 2 min o
Mix (a) and (b) imlO g mediately before
100 mi etehing in proportion
10 g 1: 1.
!!! See Appendix A.
100 mi Several sees .
S-JO g !!! See Appendix A.
Ag and low-alloy Ag.
Pure Ag and Ag
eomposites with
other metals.
Ammonia water
Hydrogen p~roxide
(3%)
50 mi Up to I mino
.
Use fresh!
50 mi
Pure Ag. Ag-Ni

alloys.
Ag-Pd alloys .
Dist. water
Hydrogen peroxide
(3%)
Ammonia water
25 mi Up to I mino
Use fresh!
50 mi
25 mi
Ag-rieh Ag-Cd
alloys.
Ag solders. Ag-Cu
alloys.
Dist. water
lron (III) ehloride
Aqueous sol. of sodium hydroxide (10%)
Aqueous sol. of potassium ferrieyanide
(30%)
Electrolytic:
Dist. water
Citrie acid
lOO mi 5-30
2_g_ _
f~
f,
g
~h
~,
Ag solders.
kt
5-15 S.
10 mi If attaek too rapid,
dilute 50% with disto
water.
JO mi
Ag-Mo alloys.
Ag-W alloys.
Ag-W carbides.
f1
10ml 15 s to I mino
IOg 6 V de, Ag eathode.
Possibly 2-3 drops
nitrie acid (1.40).
Ag alloys .
S.
Ir~
!'
1"J
Aluminum
@]
Aluminum and many of its alloys are soft and ductile and have a tendency
to form deformed layers. Grinding and polishing compounds are easily embedded.
Anodic layer. lacqllers, galvanic layers, and soldered, brazed, or welded joints
must be examined unetched.
Macroetching
Preparation:
'';'11 ,
:,
Coarse grinding is normally sufficient (wet on silieon earbide paper).

Etching:
No.
Al
2ml
a. Dist. water
Ammonium persulfate
b. Dist. water
Potassium eyanide
MI
.,.,
F~
Etehant
Dist. water
Sodium hydroxide
Conditions
100 mi 5-15 min, 60-70 oC
JO-20 g (140-160F).
More eoneentrated
solutions work also at
room temperature.
Remarks
Suitable for most
types of Al and Al
alloys.
I'~
; -~1
Preparation of Al
38
Ag
Microetching
m3
Preparation:
Grinding:
a. Wet on silieon earbide papers down to 600 grit (eoat papers with wax; use distilled
water).
b. Prepare by mierotome, using eutters of eemented earbides or, better stiU, diamond.
AIso useful for aU silver aUoys with a hardness below 150 HV.
polishing:
a. Usealumina or diamond paste down to fmest particle size. An eteh-polishing sequenee
or multiple polishing, using one of the listed mieroetehants, helps to deerease the
deformed layer.
b. Eleetrolytie:
1000 mi 10 min,
!!! See Appendix A.
l . Dist. water
37 g 2.5-3 V de,
Potassium eyanide
38 g . Ag cathode.
Potassium carbonate
35 g
Silver eyanide
200 mi 4-6 min, approx 40 oC
2. Dist. water
380 mi (100 F),
Ethanol (96%)
400 mi 2.5- 3 V de,
Al eathode.
!!! See Appendix A.
1000
mi
Approx I min,
3. Dist. water
2.5
V
de,
100
g
Sodium eyanide
100 g graphite eathod~ .
potassium ferrocyanide
1000 mi 2-5 min,
Dist. water
2
12 g 6-8 mA/em
Sodium thiosulfate
2g
Thiourea
I g
Copper (H) nitrate
d. Chemieal:
!!! See Appendix A.
800 mI
Dist. water
100 mi
ehromium (VI) oxide
45 mi
Hydroehlorie aeid ~IO%)
Etching:
No.
Ag
mi
A-
Ag
m2
39
Preparation?f Ag
I
Etehan~1
;
Dist. water '.jo

Sulfurie acid ( .84)
ChroIrlium (VI) oxide
(Coneentratiop. variable)
Sal. aqueous sol. oC
potassium dichromate
sodium ehloride
Conditions
lOO mI Up to I mino
2g
10 mI Sees to mins, 1:9

dilution with dist.
water. Possibly
100 ml without sulfurie aeid.
Remarks
Predominantly used
for Ag alloys, espeeiaUy Ag-Ni alloys
and Ag-Mg-Ni
alloys .
Pure Ag and Ag
alloys .
Ag solders.
Ag
m4
Ag
mS
Ag
m6
Ag
rr;.7
Ag
m8
Ag
m9
Ammonia water
Potassium eyanide
100 mi 30 s to 2 min o
Mix (a) and (b) imlO g mediately before
100 mi etehing in proportion
10 g 1: 1.
!!! See Appendix A.
100 mi Several sees .
S-JO g !!! See Appendix A.
Ag and low-alloy Ag.
Pure Ag and Ag
eomposites with
other metals.
Ammonia water
Hydrogen p~roxide
(3%)
50 mi Up to I mino
.
Use fresh!
50 mi
Pure Ag. Ag-Ni

alloys.
Ag-Pd alloys .
Dist. water
Hydrogen peroxide
(3%)
Ammonia water
25 mi Up to I mino
Use fresh!
50 mi
25 mi
Ag-rieh Ag-Cd
alloys.
Ag solders. Ag-Cu
alloys.
Dist. water
lron (III) ehloride
Aqueous sol. of sodium hydroxide (10%)
Aqueous sol. of potassium ferrieyanide
(30%)
Electrolytic:
Dist. water
Citrie acid
lOO mi 5-30
2_g_ _
f~
f,
g
~h
~,
Ag solders.
kt
5-15 S.
10 mi If attaek too rapid,
dilute 50% with disto
water.
JO mi
Ag-Mo alloys.
Ag-W alloys.
Ag-W carbides.
f1
10ml 15 s to I mino
IOg 6 V de, Ag eathode.
Possibly 2-3 drops
nitrie acid (1.40).
Ag alloys .
S.
Ir~
!'
1"J
Aluminum
@]
Aluminum and many of its alloys are soft and ductile and have a tendency
to form deformed layers. Grinding and polishing compounds are easily embedded.
Anodic layer. lacqllers, galvanic layers, and soldered, brazed, or welded joints
must be examined unetched.
Macroetching
Preparation:
'';'11 ,
:,
Coarse grinding is normally sufficient (wet on silieon earbide paper).

Etching:
No.
Al
2ml
a. Dist. water
Ammonium persulfate
b. Dist. water
Potassium eyanide
MI
.,.,
F~
Etehant
Dist. water
Sodium hydroxide
Conditions
100 mi 5-15 min, 60-70 oC
JO-20 g (140-160F).
More eoneentrated
solutions work also at
room temperature.
Remarks
Suitable for most
types of Al and Al
alloys.
I'~
; -~1
Preparation of Al
40
Al
M2
Hydrochloric acid
(1.I9)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Secs to mins. Use

75 mI fresh!
25 mI Possibly diluted with
25 mI disto water.
5 mi Rinse in warm water.
!!! See Appendix A.
Al alloys containing
Cu, Mn, Si, Mg, Ti.
Al cast alloys with
high Si content.
Al
M3
Ois!. water
Hydrochloric acid
(1.l9)
Hydrofluoric acid
(40%)
(Flick's reagent)
90 mI 5 s to 3 mino
!!! See Appendix A.
15 mi
Al-base materials in
general. Pure Al.
Cu-Al alloys.
. Al
M4
Al
M5
Prepararon of Al
Oist. water
Hydrochloric acid
(1.l9)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
(Concentration variable)
(Keller's reagent)
20 (50) mi 1-3 min o

!!! See Appendix A.
20(15)ml
20(25) mi
5 (10) mi
.c.
Ois!. water
Hydrochloric acid
(1.l9)
Nitric acid (1.40)
Hydrofluoric acid
25 mi Secs to mins.
Use fresh!
45 mi !!! See Appendix A.
15 mI
(40%)
15 mi
(Tucker's reagent)
Al
M6
10 mi
Oist. water
Sulfuric acid (1.84)
Al7base materials in
general. High-purity
Al.
Alloys cif AI-Mn,
AI-Mg, AI-Mg-Mn,
and AI-Mg-Si.
Grain size. Rolling direction. Welded
joints.
Also useful for microetching.
High-purity Al.
Mn-Al, Si-Al, Mg-Al,
and Mg-Si-Al alloys.
100 mi Secs to mins.

5.5 mi
Surface imperfections
of pure Al.
lf macroetching results in a coated surface, the coating can be removed by a strong
solution of nitric acid.
Microetching
Preparation:
Grinding:
Wet on silicon carbide p!pers down to 600 grit.
Polishing:
41
950 mi
15 mi
50ml
10-60 s,
30-60 V dc,
stainless steel cathode.
!!! See Appendix A.
140 mi
15-60 s,
3. Oist. water
800 mi
30-80 V dc,
Ethanol (96%)
60 mi
Perchloric acid (60%)
!!! See Appendix A.
1-2min,
4. Oist. water
220 mI
1.5-12 V dc,
200 mi
Glycerine
580 mi stainIess steel cathode.
Sulfuric acid (1 .84)
c. With diamond paste (particle size 6 f..Lm).
Then chemically:
25 mi
30 s to 2 min,
1. Sulfuric acid (1.84)
70 mi
85 oC (185F) .
Phosphoric acid (1.71)
5 mI
Nitric acid (1.40)
65-80 mi
5-30 s,
2. Oist. water
50-60 oC (120-140 F).
ammonium hydrogen
fluoride
10-20 mi
10-20 mi
Nitric acid (1.40)
d. With alumina slurry No. 1 (5 /L m ) a~d No. lC (1 Lm; Linde C) on a fast-running
felt-covered wheel, followed by a1umma slurry No. 2 (0.3 f..Lm; Linde A) on cotton
velvet. For fmal polishing, alumina slurry No. 3 (0.05 Lm gamma a1umina; Linde
B) diluted with alcohol on silk velvet.
e. Electrolytic lapping:
95 mI
2-6 min,
Oist. water
Pure Al. Ouralumin.
1-10 mA/6.5 cm 2 , dc.
No. 3 alumina slurry
10 mI
Change poIarity
(0.05 Lm)
Al with small
every 1.5 S .
5 mi
additions of Zn,
0.5g
Velvet cloth.
Sodium fluoride
Mg, Cu, Fe, Ti, Mn,
Si. Al-Si alloys
up to 18%.
f. Milling wtth diamond cutting tool. Possibly followed by (b). Methanol for lubrication
and cooIing; only for harder alloys.
2. Methanol (95%)
Nitric acid (1.40)
PerchIoric acid (60%)
Etching:
No.
Conditions
Reagent
Al
mi
Ois!. water
Hydrofluoric acid
(40%)
If necessary, increase
content of hydrofluoric acid to 10 mI.
Al
m2
Oist. water
Nitric acid (1.40)
Hydrochloric acid
o"
a . . With diamond paste' (particle size 6-1 Lm, possibly 0.25 Lm), followed by 1-5 min
'bn a soft cloth with 'S: suspension: 120 mi hot distilled water, 20 mi aqueous solution
of ammonium tartrate (5%), and I g magnesium oxide. Suspension is filtered prior
to use. Oense nylon.9r cotton webbing is a suitable filter material. Copper-free samples
should not be polished on the same cloth as samples containing copper (formation
of dark precipitate may occur).
b. With diamond paste (particle size 6 Lm).
Then electrolytically:
l. Oist. water
250 mi
4-6 min, 40 oC (100 F),
Ethanol (96%)
380 mI
40-60 V dc,
Phosphoric acid (1.71) 400 mi
Al cathode.
(1.19)
100 mi 10-60 S.
!!! See Appendix A.
0.5 mi Minutes to 1 h.
Alternate polishing
and etching.
' l'41.
190(190)ml 10-30 S.
5(IO)ml Use fresh only!
!!! See Appendix A.
3 (6) mI
Hydrofluoric acid
(40%)
(Oix-Keller's reagent)
Remarks
For most types of Al
and Al alloys.
Grain boundaries. Slip
lines in high-purity Al.
2 (4) mi
For mos! types of Al

and Al aIloys. Exception: Al aIloys with
high Si content.
Preparation of Al
40
Al
M2
Hydrochloric acid
(1.I9)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Secs to mins. Use

75 mI fresh!
25 mI Possibly diluted with
25 mI disto water.
!!! See Appendix A.
Al alloys containing
Cu, Mn, Si, Mg, Ti.
Al cast alloys with
high Si content.
Al
M3
Ois!. water
Hydrochloric acid
(1.l9)
Hydrofluoric acid
(40%)
(Flick's reagent)
90 mI 5 s to 3 mino
!!! See Appendix A.
15 mi
Al-base materials in
general. Pure Al.
Cu-Al alloys.
. Al
M4
Al
M5
Prepararon of Al
Oist. water
Hydrochloric acid
(1.l9)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
(Keller's reagent)
20 (50) mi 1-3 min o

!!! See Appendix A.
20(15)ml
20(25) mi
5 (10) mi
.c.
Ois!. water
Hydrochloric acid
(1.l9)
Nitric acid (1.40)
Hydrofluoric acid
25 mi Secs to mins.
Use fresh!
15 mI
(40%)
15 mi
(Tucker's reagent)
Al
M6
10 mi
Oist. water
Al7base materials in
general. High-purity
Al.
Alloys cif AI-Mn,
AI-Mg, AI-Mg-Mn,
and AI-Mg-Si.
Grain size. Rolling direction. Welded
joints.
Also useful for microetching.
High-purity Al.
Mn-Al, Si-Al, Mg-Al,
and Mg-Si-Al alloys.

5.5 mi
Surface imperfections
of pure Al.
lf macroetching results in a coated surface, the coating can be removed by a strong
solution of nitric acid.
Microetching
Preparation:
Grinding:
Wet on silicon carbide p!pers down to 600 grit.
Polishing:
41
950 mi
15 mi
50ml
10-60 s,
30-60 V dc,
!!! See Appendix A.
140 mi
15-60 s,
3. Oist. water
800 mi
30-80 V dc,
Ethanol (96%)
60 mi
!!! See Appendix A.
1-2min,
4. Oist. water
220 mI
1.5-12 V dc,
200 mi
Glycerine
580 mi stainIess steel cathode.
c. With diamond paste (particle size 6 f..Lm).
Then chemically:
25 mi
30 s to 2 min,
1. Sulfuric acid (1.84)
70 mi
85 oC (185F) .
5 mI
Nitric acid (1.40)
65-80 mi
5-30 s,
2. Oist. water
50-60 oC (120-140 F).
ammonium hydrogen
fluoride
10-20 mi
10-20 mi
Nitric acid (1.40)
d. With alumina slurry No. 1 (5 /L m ) a~d No. lC (1 Lm; Linde C) on a fast-running
felt-covered wheel, followed by a1umma slurry No. 2 (0.3 f..Lm; Linde A) on cotton
velvet. For fmal polishing, alumina slurry No. 3 (0.05 Lm gamma a1umina; Linde
B) diluted with alcohol on silk velvet.
e. Electrolytic lapping:
95 mI
2-6 min,
Oist. water
Pure Al. Ouralumin.
1-10 mA/6.5 cm 2 , dc.
No. 3 alumina slurry
10 mI
Change poIarity
(0.05 Lm)
Al with small
every 1.5 S .
5 mi
additions of Zn,
0.5g
Velvet cloth.
Sodium fluoride
Mg, Cu, Fe, Ti, Mn,
Si. Al-Si alloys
up to 18%.
f. Milling wtth diamond cutting tool. Possibly followed by (b). Methanol for lubrication
and cooIing; only for harder alloys.
2. Methanol (95%)
Nitric acid (1.40)
PerchIoric acid (60%)
Etching:
No.
Conditions
Reagent
Al
mi
Ois!. water
Hydrofluoric acid
(40%)
If necessary, increase
content of hydrofluoric acid to 10 mI.
Al
m2
Oist. water
Nitric acid (1.40)
Hydrochloric acid
o"
a . . With diamond paste' (particle size 6-1 Lm, possibly 0.25 Lm), followed by 1-5 min
'bn a soft cloth with 'S: suspension: 120 mi hot distilled water, 20 mi aqueous solution
of ammonium tartrate (5%), and I g magnesium oxide. Suspension is filtered prior
to use. Oense nylon.9r cotton webbing is a suitable filter material. Copper-free samples
should not be polished on the same cloth as samples containing copper (formation
of dark precipitate may occur).
b. With diamond paste (particle size 6 Lm).
Then electrolytically:
l. Oist. water
250 mi
4-6 min, 40 oC (100 F),
Ethanol (96%)
380 mI
40-60 V dc,
Phosphoric acid (1.71) 400 mi
Al cathode.
(1.19)
100 mi 10-60 S.
!!! See Appendix A.
0.5 mi Minutes to 1 h.
Alternate polishing
and etching.
' l'41.
190(190)ml 10-30 S.
5(IO)ml Use fresh only!
!!! See Appendix A.
3 (6) mI
Hydrofluoric acid
(40%)
(Oix-Keller's reagent)
Remarks
and Al alloys.
Grain boundaries. Slip
lines in high-purity Al.
2 (4) mi
For mos! types of Al

and Al aIloys. Exception: Al aIloys with
high Si content.
Al
m3
Oist. water
Sodium hydroxide
For shrink etehing.
Oist. water
Nitric aeid (1040)
75 mi 40 s,
25 mi 70 oC (160F).

and Al alloys, espeeially those eontaining
CU .
Oist. water
Nitrie acid (1.40)
Hydrofluorie aeid
(4Q%)
(Kroll's reagent)
92 mi "5 s.
6 mI !!! See Appendix A.
Espeeially Cor Cu-AI

alloys. (AIso useful in
maeroetehing) .
Ois!. water
Sulfurie acid (1.84)
80 mI 30 s to 3 min,
20 mI 70 oC (160F).
Al
m5
Al
m6
Al
m9
Pure Al. Alloys o'

Cu-AI, Mg-Si-AI,
Mg-AI, and Zn-AJ.
If etehing times are
short, AI 2 Cu is not
eolored.

and Al alloys.
Oist. water
Sodium hydroxide
Zinc ehloride
Al
m8
100 mi a. 5-10 s, possiblyat

1-2 g 50 oC (120F).
Use fresh only!
Rinse in mixture: 95
mI dist. water, 5 mI nitrie acid (1.40).
b. Eteh 15 min, rinse
in water approx. 10
min o
100 mi Few sees to mins.
0.5-25 g
Ig
Al
m4
Al
m7
_:.
Preparation 01 Al
42
Same as Al m8
Anneal sample to
100 oC (212F) and
slow eool before
etching.
I!'
Al
Methanpl (95%)
mIO Hydroehlorie aeid
(1.19) '
Nitrie aeid (L;4Q~
:~
Hydrofluorie 'aid
(40%)
Al
Oist. water
mIl Sodium hydrdxjde
Potassium.ferrieyanide
Oist. water
Al
ml2 Phosphorie aeid (1.71)
Electrolytic:
Al
ml3 Oist. water
Fluoborie aeid (35 %)
(Barker's reagent)
/ 43
90 mI a. 1-3 min, 50 oC
10 mi (120 F).
b. Electrolytic:
5- 10 s,
1- 8 V de, stainless
steel eathode
Pure Al.
AI-Cu, AI-Mn, AI-Mg,
AI-Mg-Si alloys.
200 mi 1-2 min,

10 mi 20-40 V de.
00 not wipe during
"rinsing.
Catliode and anode
fixtures should be
made of high-purity
Al, Pb, or stainless
steel.
PUre Al. AI-Zn,

AI-Mn, AI-Mg-Si,
AI-Zn-Mg, AI-Mn-Mg
alloys.
Oiffieult with Al-CuMg alloys.
View in polarized
light.
2ml
100 mi 30 min o
9g
Oist. water
Phosphorie aeid
(1.88 erystal)
Preparation of Au, Ir, Os, Pd, Pt, Rh, Ru
25 (50) mI 10-60s.
!!! See Appendix A.
25 (30) mi
25 (20) mI
Oifferentiation of intermediate phases in

Al alloys with high
. eorttents 6C" Cil, Mn,
Mg, Fe, Be, Ti.
Fe,A!.
Oeteetion of suseeptibility to intererystalline eorrosion of AIMg - base alloys. Oistinet grain boundaries
in eorrosion-sensitive
alloys .
Preeipitates of betaAl. Mg s or Al, Mg 2 ,
respeetively. Shows
strain in AI-Mg - base
alloys .
Pure Al. AI-Mg and
AI-Mg-Si alloys .
Eteh figures.
Gold, Iridium, Osmium, Palladium,

Platinum, Rhodium, Ruthenium
These rnetals are usually soft. They have a tendency to produce deforrned
layers (although iridiurn, osrniurn, rhodiurn and rutheniurn represent exceptions
depending on purity). The alloys do not pose particular difficulties in preparing
metallographic specirnens.
Macroetching
Preparation:
Speeimen preparation for maeroetehing is identieal to that detailed below for mieroetehing.
Etching:
No.
Hydroehlorie aeid
(\.19)
Nitric acid (1.40)
Au
M2
Lactic aeid (90%) or

Hydroehlorie acid
(1.l9)
Nitric acid (1.40)
Hydrofluorie aeid
(40%)
I drop
60ml 2 min
IOg
5g
Precipitates. Grain
boundaries. Al-Si and
AI-Cu alloys.
Au
M3
Conditions
Etchant
Au
MI
Electrolytic:
sodium ehloride
Hydrochloric aeid
(\.19)
Few mins.
66 mI Use hot! Use fresh!
Few mins.
!!! See Appendix A.
50 mI
20 mi
Remarks
Au . Pt alloys.
Pd alloys.
Ru and Ru alloys.
Os and Os alloys.
Rh and Rh alloys.
30 mi
Few mins,
80 mi 6 V de,
Pt cathode.
20 mi
Pt and Pt alloys .
Au
Ir
Os
Pd
Pt
Rh
Ru
Al
m3
Oist. water
Sodium hydroxide
For shrink etehing.
Oist. water
Nitric aeid (1040)
75 mi 40 s,
25 mi 70 oC (160F).

and Al alloys, espeeially those eontaining
CU .
Oist. water
Nitrie acid (1.40)
Hydrofluorie aeid
(4Q%)
(Kroll's reagent)
92 mi "5 s.
Espeeially Cor Cu-AI

alloys. (AIso useful in
maeroetehing) .
Ois!. water
80 mI 30 s to 3 min,
20 mI 70 oC (160F).
Al
m5
Al
m6
Al
m9
Pure Al. Alloys o'

Cu-AI, Mg-Si-AI,
Mg-AI, and Zn-AJ.
If etehing times are
short, AI 2 Cu is not
eolored.

and Al alloys.
Oist. water
Sodium hydroxide
Zinc ehloride
Al
m8
100 mi a. 5-10 s, possiblyat

1-2 g 50 oC (120F).
Use fresh only!
Rinse in mixture: 95
mI dist. water, 5 mI nitrie acid (1.40).
b. Eteh 15 min, rinse
in water approx. 10
min o
100 mi Few sees to mins.
0.5-25 g
Ig
Al
m4
Al
m7
_:.
Preparation 01 Al
42
Same as Al m8
Anneal sample to
100 oC (212F) and
slow eool before
etching.
I!'
Al
Methanpl (95%)
mIO Hydroehlorie aeid
(1.19) '
Nitrie aeid (L;4Q~
:~
Hydrofluorie 'aid
(40%)
Al
Oist. water
mIl Sodium hydrdxjde
Potassium.ferrieyanide
Oist. water
Al
ml2 Phosphorie aeid (1.71)
Electrolytic:
Al
ml3 Oist. water
Fluoborie aeid (35 %)
(Barker's reagent)
/ 43
90 mI a. 1-3 min, 50 oC
10 mi (120 F).
b. Electrolytic:
5- 10 s,
1- 8 V de, stainless
steel eathode
Pure Al.
AI-Cu, AI-Mn, AI-Mg,
AI-Mg-Si alloys.
200 mi 1-2 min,

10 mi 20-40 V de.
00 not wipe during
"rinsing.
Catliode and anode
fixtures should be
made of high-purity
Al, Pb, or stainless
steel.
PUre Al. AI-Zn,

AI-Mn, AI-Mg-Si,
AI-Zn-Mg, AI-Mn-Mg
alloys.
Oiffieult with Al-CuMg alloys.
View in polarized
light.
2ml
100 mi 30 min o
9g
Oist. water
Phosphorie aeid
(1.88 erystal)
25 (50) mI 10-60s.
!!! See Appendix A.
25 (30) mi
25 (20) mI
Oifferentiation of intermediate phases in

Al alloys with high
. eorttents 6C" Cil, Mn,
Mg, Fe, Be, Ti.
Fe,A!.
Oeteetion of suseeptibility to intererystalline eorrosion of AIMg - base alloys. Oistinet grain boundaries
in eorrosion-sensitive
alloys .
Preeipitates of betaAl. Mg s or Al, Mg 2 ,
respeetively. Shows
strain in AI-Mg - base
alloys .
Pure Al. AI-Mg and
AI-Mg-Si alloys .
Eteh figures.
Gold, Iridium, Osmium, Palladium,

Platinum, Rhodium, Ruthenium
These rnetals are usually soft. They have a tendency to produce deforrned
layers (although iridiurn, osrniurn, rhodiurn and rutheniurn represent exceptions
depending on purity). The alloys do not pose particular difficulties in preparing
metallographic specirnens.
Macroetching
Preparation:
Speeimen preparation for maeroetehing is identieal to that detailed below for mieroetehing.
Etching:
No.
Hydroehlorie aeid
(\.19)
Nitric acid (1.40)
Au
M2
Lactic aeid (90%) or

Hydroehlorie acid
(1.l9)
Nitric acid (1.40)
Hydrofluorie aeid
(40%)
I drop
60ml 2 min
IOg
5g
Precipitates. Grain
boundaries. Al-Si and
AI-Cu alloys.
Au
M3
Conditions
Etchant
Au
MI
Electrolytic:
sodium ehloride
Hydrochloric aeid
(\.19)
Few mins.
66 mI Use hot! Use fresh!
Few mins.
!!! See Appendix A.
50 mI
20 mi
Remarks
Au . Pt alloys.
Pd alloys.
Ru and Ru alloys.
Os and Os alloys.
Rh and Rh alloys.
30 mi
Few mins,
80 mi 6 V de,
Pt cathode.
20 mi
Pt and Pt alloys .
Au
Ir
Os
Pd
Pt
Rh
Ru
44
P'eparation of Au, Ir, Os, Pd, Pt, Rh, Ru

Au
m2
Microetching
Prepara tion:
Grinding:
a. Dist. water
Potassium eyanide
b . Dist. water
Ammonium persulfate
a . Wet on silieon earbide papers down to 600 grit (eoat papers with wax).
b. Prepare by mierotome using diamond knife. Also useful for all alloys with hardness
below 150 HV.
Polishng:
Au
m3
a. Alumina slurry or diamond paste down to finest particle size. Multiple polishing with
one of tlle mieroetehants listed for eleetrolytie etehing eliminates the deformed layer
more quiekly.
b. Eleetrolytie:
1. Dist. water
Mostly Au.
1000 mi
2-4 min,
Potassium eyanide
80 g
7.5 V de,
Potassium carbonate
40 g
grapbite eathode.
Gold (111) ehloride
50 g
!!! See Appendix A.
8-12 V de,
Mostly Au.
2. Dist. Water
3 mi
Glacial aeetie acid
75 mi
stainless steel eatbode.
Chromium (VI) oxide
15 g
Mixing of eleetrolyte at
65 oC (150F), 1 h.
!!! See Appendix A.
1. Dist. water
820 mi
Pd and Pd
2-3 min,
SodiuII! thiosulfate
alloys.
50 g
. U-U A/em' de,
Potassium thioeyaAu-Pt 90
150 rpm .
nate
70 g
!!! See Appendix A.
alloy.
Ammonium ebloride 60 g
2. Dist. water
940 mi
4- 5 min,
Au.
2
Potassium thioeya55 mA/em de.
nate
20 g
!!! See Appendix A.
Ammonium ehloride 20 g
Ammonium thiosulfate
20 g
3. Dist. water
610 mi
Approx 15 min,
PI.
Hydroehlorie aeid
Au-Pt
0.5 A/0.25 cm'
(1.l9)
50 mi
alloys
ae.
Sodium fluoride !
150 g
!!! See Appendix A.
70/30 and
Potassium ehlorid~
lOO g
50/50.
Potassium nitrate t 50 g
Potassium thiocyanate
'.
40 g
Dist. water
Hydrogen peroxide
(3%)
Iron (JII) ehloride
Au
mI
Etehant '
Nitrie aeid (1.40)
Hydroehlorie aed
(1.19)
(Coneentration' variable)
Conditions
40 (1) mI Few sees to 1 min o
May require heating.
60 (lO) mI Use fresh only!
!!! See Appendix A.
..
lOO mi 30 s to 2 min o
IOg (a) and (b) are mixed
in proportion 1: I before use.
lOO mi Double amount of
potassium cyanide
IOg and ammonium persulfate.
!!! See. Appendix A.
Pd, Pt. Au alloys

with less than 90%
eontent of preeious
metals.
For Au alloys with
high eontent of precious metals. White
gold. Pd and Pt
alloys.
Au-Cu-Ag alloys .
100 mi
32 g
30 (50) mi 1-5 mino
Use hot!
25 (100) mi Remove precipitate
5 (10) mI of gold ehloride with
ammonia water.
Pure Pt and Pd.

Au alloys.
Proportions in
parentheses especialIy useful for Pt.
Dist. water
Hydroeblorie aeid
(l.l9)
Nitrie aeid (1.40)
(Coneentration variable)
Au
m5
Hydroehlorie acid
(1.19)
Chromium (VI) oxide
Sees to mins.
1-5 g
Pure Au a'n d Au-rich

alloys. Pd and Pd
alloys.
Au
m6
Dist. water
Potassium ferrieyanide
Sodium hydroxide
ISO mi Few mins.

!!! See Appendix A.
3.5 g
1g
Os and Os-W alloys.
Au
m7
Dist. water
Hydroehlorie aeid
(\.19)
Hydrogen peroxide
(3%)
Au
m8
ElectrQlytic:
Dist. water
Potassium eyanide
Au
m9
Electrolytic:
Dist. water
Hydroehlorie aeid
(1.19)
Sodium ehloride
Remarks
Pure Au and Pd.
Au-Pt, Pd alloys with
more tban 90% content of precious
metals. Rh alloys.
45
Au
m4
Etching:
No.
Au
mIO
Electrolytic:
Ethanol (96%)
Hydroehlorie aeid
(1.l9)
Au
mil
Electrolytic:
Hydroebloric aed
(L19)
80 mi Few mins.
Ru-rieb alloys.
Ru-Mo alloys.
20 mi
Iml
lOO mI 1- 2 min,
5g 1- 5 V ae, 0.5-1.5
A/ cm', Pt eatbode.
!!! See Appendix A.
Pt and Pt alloys.
Au and Au alloys .
65 mi 25 see, 10 V ae.
I min, 1.5 V ae.
20 mi 1-2 min, 20 V ae.
25 g 1 min, 6 Vae.
1 min, 5-20 V ae.
Graphite or Pt
eathode.
Rh-base alloys.
Pt- IO% Rh alloys .
Ir alloys.
Pure Pt and Pt alloys.
Ru-base alloys.
90 mI 30 s,
10 V de, grapbite
10 mi eathode.
Os-base alloys. Pure

Pd and Pd alloys.
Pt-Au alloys. Ir.
1-2 min, 5 V ae, Pt

cathode.
Rh-base alloys. Au
and Pt. Grain-eontrast eteh .
I
' ~ ~h
44
P'eparation of Au, Ir, Os, Pd, Pt, Rh, Ru

Au
m2
Microetching
Prepara tion:
Grinding:
a. Dist. water
Potassium eyanide
b . Dist. water
Ammonium persulfate
a . Wet on silieon earbide papers down to 600 grit (eoat papers with wax).
b. Prepare by mierotome using diamond knife. Also useful for all alloys with hardness
below 150 HV.
Polishng:
Au
m3
a. Alumina slurry or diamond paste down to finest particle size. Multiple polishing with
one of tlle mieroetehants listed for eleetrolytie etehing eliminates the deformed layer
more quiekly.
b. Eleetrolytie:
1. Dist. water
Mostly Au.
1000 mi
2-4 min,
Potassium eyanide
80 g
7.5 V de,
Potassium carbonate
40 g
grapbite eathode.
Gold (111) ehloride
50 g
!!! See Appendix A.
8-12 V de,
Mostly Au.
2. Dist. Water
3 mi
Glacial aeetie acid
75 mi
stainless steel eatbode.
Chromium (VI) oxide
15 g
Mixing of eleetrolyte at
65 oC (150F), 1 h.
!!! See Appendix A.
1. Dist. water
820 mi
Pd and Pd
2-3 min,
SodiuII! thiosulfate
alloys.
50 g
. U-U A/em' de,
Potassium thioeyaAu-Pt 90
150 rpm .
nate
70 g
!!! See Appendix A.
alloy.
Ammonium ebloride 60 g
2. Dist. water
940 mi
4- 5 min,
Au.
2
Potassium thioeya55 mA/em de.
nate
20 g
!!! See Appendix A.
Ammonium ehloride 20 g
20 g
3. Dist. water
610 mi
Approx 15 min,
PI.
Hydroehlorie aeid
Au-Pt
0.5 A/0.25 cm'
(1.l9)
50 mi
alloys
ae.
Sodium fluoride !
150 g
!!! See Appendix A.
70/30 and
Potassium ehlorid~
lOO g
50/50.
Potassium nitrate t 50 g
'.
40 g
Dist. water
Hydrogen peroxide
(3%)
Iron (JII) ehloride
Au
mI
Etehant '
Nitrie aeid (1.40)
Hydroehlorie aed
(1.19)
(Coneentration' variable)
Conditions
40 (1) mI Few sees to 1 min o
May require heating.
60 (lO) mI Use fresh only!
!!! See Appendix A.
..
lOO mi 30 s to 2 min o
IOg (a) and (b) are mixed
in proportion 1: I before use.
lOO mi Double amount of
potassium cyanide
IOg and ammonium persulfate.
!!! See. Appendix A.
Pd, Pt. Au alloys

with less than 90%
eontent of preeious
metals.
For Au alloys with
high eontent of precious metals. White
gold. Pd and Pt
alloys.
Au-Cu-Ag alloys .
100 mi
32 g
30 (50) mi 1-5 mino
Use hot!
25 (100) mi Remove precipitate
5 (10) mI of gold ehloride with
ammonia water.
Pure Pt and Pd.

Au alloys.
Proportions in
parentheses especialIy useful for Pt.
Dist. water
Hydroeblorie aeid
(l.l9)
Nitrie aeid (1.40)
Au
m5
Hydroehlorie acid
(1.19)
Chromium (VI) oxide
Sees to mins.
1-5 g
Pure Au a'n d Au-rich

alloys. Pd and Pd
alloys.
Au
m6
Dist. water
Sodium hydroxide
ISO mi Few mins.

!!! See Appendix A.
3.5 g
1g
Os and Os-W alloys.
Au
m7
Dist. water
Hydroehlorie aeid
(\.19)
Hydrogen peroxide
(3%)
Au
m8
ElectrQlytic:
Dist. water
Potassium eyanide
Au
m9
Electrolytic:
Dist. water
Hydroehlorie aeid
(1.19)
Sodium ehloride
Remarks
Pure Au and Pd.
Au-Pt, Pd alloys with
more tban 90% content of precious
metals. Rh alloys.
45
Au
m4
Etching:
No.
Au
mIO
Electrolytic:
Ethanol (96%)
Hydroehlorie aeid
(1.l9)
Au
mil
Electrolytic:
Hydroebloric aed
(L19)
80 mi Few mins.
Ru-rieb alloys.
Ru-Mo alloys.
20 mi
Iml
lOO mI 1- 2 min,
5g 1- 5 V ae, 0.5-1.5
A/ cm', Pt eatbode.
!!! See Appendix A.
Pt and Pt alloys.
Au and Au alloys .
65 mi 25 see, 10 V ae.
I min, 1.5 V ae.
20 mi 1-2 min, 20 V ae.
25 g 1 min, 6 Vae.
1 min, 5-20 V ae.
Graphite or Pt
eathode.
Rh-base alloys.
Pt- IO% Rh alloys .
Ir alloys.
Pure Pt and Pt alloys.
Ru-base alloys.
90 mI 30 s,
10 V de, grapbite
10 mi eathode.
Os-base alloys. Pure

Pd and Pd alloys.
Pt-Au alloys. Ir.
1-2 min, 5 V ae, Pt

cathode.
Rh-base alloys. Au
and Pt. Grain-eontrast eteh .
I
' ~ ~h
46
Au
ml2
Au
ml3
Preparation of Be
E/ectro/ytic:
Dist. water
Hydrochloric acid
(1.19)
E/ectro/ytic:
Dist. water
Preparation 0# Be
90 mi 30 min to 3 h,
0.1 A/cm\ graphite
5-10 mi or Pt cathode.
Preparation:
Compare technical tips for macroetching.
Polishing:
80 mi Up to 1 h,
20 mi 1-5 V ac, 0.05-0.2
A I cm \ graphite
cathode.
Pt alloys. Rh, Ir.
Preparation steps generate toxic dust, which must be carried out in a glove
box. Beryllium must never be inhaled. (!!! See Appendix A and references
on safety and toxicology in Appendix C.)
Maeroetching
Always wet on silicon carbide papers down to 600 grit, which is sufficient for coarse-grain
material. Beryllium with small grain size must be polished.
Polishing:
Diamond paste (6-0.25 J.Lm), followed by alumina suspension on a finely woven, sturdy
cloth. AIso valid for microetching.
Etching:
MI
Be
~2
Be
M3
a. Concentrated slurry of magnesium oxide in hydrogen peroxide (30%) on billiard cloth.

b. Alumina slurry in oxalic acid (10%) on silk. Final polish (15-30 s) on nylon with
long nap using No. 3 (0.05 J.Lm, Linde B) alumina slurry in a solution of 100 mI
water, 14 mi phosphoric acid (1.71), I mi sulfuric acid (1.84), and 20 g chromium
(VI) oxide, diluted with 10 parts distiYed water (!!! See Appendix A.). Solution is
added in drops during polishing.
c. Electrolytic:
1. Dist. water
200 mi
250 A/cm\
900 mi
70-80 oC (160-180 F),
Sato sol. of chromium (VI)
oxide in disto water
240 mi
!!! See Appendix A.
2. Phosphoric acid (1.71)
100 mi
2-4 A/cm 2 ,
30 mi
Glycerol
30 mi
!!! See Appendix A.
Ethanol (96%)
30 mi
d. Electrolytic lapping:
Ethylene glycol (1.11)
97 mi
1-1.5 Al cm 2
Hydrochloric acid (l.l9)
Iml
Nylon cloth.
. Nitric acid (1.40)
2m!.
Etching:
Preparation:
Grinding:
No.
Beryllium is suitable for observations in polarized light.

No.
Etchant
Conditions
Be Dist. water
Secs to mins.
mi or ethanol (96%)
lOO mi !!! See Appendix A.
Hydrofluoric acid
(40%)
2-10 mi
Be Dist. water
lOO mi 1-15 S.
m2 Sulfuric acid (1.84)
5 mI
Remarks
Be
Dist. water
Hydrochloric acid
(1.19)
. l
Ammonillm chloride
90 mi Few mins.
Immerse or swab.
10 mi
4g
Technical types of Be.

Especially with large
grain size.
m3
Dist. water
Hydrochloric ~~i4
(1.19)
Arnrnonium chloride
Picric acid
90 mi Few mins.
Immerse or swab.
10 mI
2g
2g

grain size. Low-alloy
Be.
25 mi Secs to mins,
500 mi 45 oC (110 F)
59 g !!! See Appendix A.
Grain-boundary etch.
Conditions
Etchant
Sulfuric acid (1 . 81)

Chromium (VI) oxide
(Possibly sorne disto
water)
47
Microetching
Ir.
Beryllium
Be
With fine-grain Be, macroetching is difficult.
Be
m4
Be
m5
Be
m6
Be
m7
Remarks
Be alloys.
For most types of Be

and Be alloys.
Dist. water
Ammonia water
Hydrogen peroxide
(30%)
50 mi Secs to mins.
20 mi Use fresh only!
Glycerol
Hydrofluoric acid
(40%)
Nitric acid (1.40)
25 mi Approx 15 S.
HF content may be
5 mI raised to 15 mI.
Be and Be alloys.
Lactic acid (90%)

Nitric acid (1.40)
Hydrofluoric acid
(40%)
50 mI Secs to mins.
Be-U, Be-Nb, Be-Y,

and Be-Zr alloys.
Dist. water
Oxalic acid
Sat. sol of copper (JI)
sulfate in dist. water
Be-Ag and Be-Al-Ti

alloys.
3 mi
>"'11',
50 mi
100 mI 2 mino
IOg 16 mino Boiling.
30 s.
Precipitates.
Grain boundaries.
Precipitates.
46
Au
ml2
Au
ml3
Preparation of Be
E/ectro/ytic:
Dist. water
Hydrochloric acid
(1.19)
E/ectro/ytic:
Dist. water
Preparation 0# Be
0.1 A/cm\ graphite
5-10 mi or Pt cathode.
Preparation:
Compare technical tips for macroetching.
Polishing:
80 mi Up to 1 h,
20 mi 1-5 V ac, 0.05-0.2
A I cm \ graphite
cathode.
Pt alloys. Rh, Ir.
Preparation steps generate toxic dust, which must be carried out in a glove
box. Beryllium must never be inhaled. (!!! See Appendix A and references
Maeroetching
Always wet on silicon carbide papers down to 600 grit, which is sufficient for coarse-grain
material. Beryllium with small grain size must be polished.
Polishing:
Diamond paste (6-0.25 J.Lm), followed by alumina suspension on a finely woven, sturdy
cloth. AIso valid for microetching.
Etching:
MI
Be
~2
Be
M3
a. Concentrated slurry of magnesium oxide in hydrogen peroxide (30%) on billiard cloth.

b. Alumina slurry in oxalic acid (10%) on silk. Final polish (15-30 s) on nylon with
long nap using No. 3 (0.05 J.Lm, Linde B) alumina slurry in a solution of 100 mI
water, 14 mi phosphoric acid (1.71), I mi sulfuric acid (1.84), and 20 g chromium
(VI) oxide, diluted with 10 parts distiYed water (!!! See Appendix A.). Solution is
added in drops during polishing.
c. Electrolytic:
1. Dist. water
200 mi
250 A/cm\
900 mi
70-80 oC (160-180 F),
Sato sol. of chromium (VI)
oxide in disto water
240 mi
!!! See Appendix A.
100 mi
2-4 A/cm 2 ,
30 mi
Glycerol
30 mi
!!! See Appendix A.
Ethanol (96%)
30 mi
d. Electrolytic lapping:
97 mi
1-1.5 Al cm 2
Hydrochloric acid (l.l9)
Iml
Nylon cloth.
. Nitric acid (1.40)
2m!.
Etching:
Preparation:
Grinding:
No.
Beryllium is suitable for observations in polarized light.

No.
Etchant
Conditions
Be Dist. water
Secs to mins.
mi or ethanol (96%)
Hydrofluoric acid
(40%)
2-10 mi
Be Dist. water
lOO mi 1-15 S.
m2 Sulfuric acid (1.84)
5 mI
Remarks
Be
Dist. water
Hydrochloric acid
(1.19)
. l
Ammonillm chloride
90 mi Few mins.
Immerse or swab.
10 mi
4g

grain size.
m3
Dist. water
Hydrochloric ~~i4
(1.19)
Arnrnonium chloride
Picric acid
90 mi Few mins.
Immerse or swab.
10 mI
2g
2g

grain size. Low-alloy
Be.
25 mi Secs to mins,
500 mi 45 oC (110 F)
Conditions
Etchant
Sulfuric acid (1 . 81)

Chromium (VI) oxide
(Possibly sorne disto
water)
47
Microetching
Ir.
Beryllium
Be
With fine-grain Be, macroetching is difficult.
Be
m4
Be
m5
Be
m6
Be
m7
Remarks
Be alloys.
For most types of Be

and Be alloys.
Dist. water
Ammonia water
Hydrogen peroxide
(30%)
50 mi Secs to mins.
Glycerol
Hydrofluoric acid
(40%)
Nitric acid (1.40)
25 mi Approx 15 S.
HF content may be
5 mI raised to 15 mI.
Be and Be alloys.
Lactic acid (90%)

Nitric acid (1.40)
Hydrofluoric acid
(40%)
50 mI Secs to mins.
Be-U, Be-Nb, Be-Y,

and Be-Zr alloys.
Dist. water
Oxalic acid
Sat. sol of copper (JI)
sulfate in dist. water
Be-Ag and Be-Al-Ti

alloys.
3 mi
>"'11',
50 mi
100 mI 2 mino
IOg 16 mino Boiling.
30 s.
Precipitates.
Grain boundaries.
Precipitates.
Preparation of Bi, Sb
48
Be
mS
Electrolylic:
Ethanol (96%)
Butyl glycol
Be
m9
Electrolytic:
Hydrochloric acid
(1.19)
Nitric acid (1.40)

Be Electro/y tic:
mIO Phosphoric acid (1.71)
Glycerol
Ethanol (96%)
Sulfuric acid (i.84)
[!O
~ Preparation:
35 mi 30-45 s, below
10 mi 35 oC (95F), 50 V
10 mi dc, stainless steel
cathode .
!!! See Appendix A.
Be and Be alloys.
Rapid attack.
294 mi 6 min,
30 oC (85F), 13-20 V
4 mi dc, stanless steel
2 mi cathode.
Be and Be alloys .
Bi
M2
a. Dist. water
Nitric acid (1.40)
b. Dist. water
Ammonium molybdate
Bi
M3
Dist. water
Citric acid
Ammonium molybdate
100 mi
30 mi
30 mi
2.5 mi
I min,
cool (10 oC; 50F),
25 V dc, stainless
.steel or Mo cathode.
Be. Grain-boundary
etch.
AIso used to increase
contrast in polarized
light.
Macroetching
Wet on silicon carbide papers down to 320 grit; if necessary, down to 600 grit.
No.
Etchant
a. Dist. water
Nitric acid' (l.40)
Glacial acetic acid
b. Dist. water
Glacial acetic acid
lOO mi Secs to mins.

25 g
Crystal arrangement.
Casting imperfections
in Sb and Bi.
lO g
Same as for macroetching.
Etching:
No.
Bi
mi
Conditions
160 mi First with (a) at
40 mi 40 oC (100F). Re30 mi polish untl surface
has become bright.
400 mi Repeat etching with
I mi (b) 1-2 h
Remarks
Sb-Pb, Bi-Sn alloys.
Etchant
Dist . water
Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
Conditions
70 mi Secs to mins .
30 mi
Glacial acetic acid

Hydrogen peroxide
(30%) '
30 mi Secs to mins.
Bi
m3
Dist. water
Hydrochloric acid
(1.19)
Iron (I1I) chloride
For pure and technically pure types of Sb.

Low-alloy Sb.
Sb and Sb alloys.
10 mi
30 mi
2g
Dist. water
Hydrochloric acid
(1.19)
Aqueous sol. of sodium thiosulfate (16%)
Aqueous sol. of chromium (VI) oxide
(10%)
(Czochralski's
etchant)
30 mi Add chromium (VI)

oxide shortly before
15 mi use. Chromium (VI)
oxide content can be
50 mi raised.
!!! See Appendix A.
Bi
m5
Dist. water
Hydrochloric acid
(1.19)
50 mi 1-10 mino
Bi
m6
Ethanol (96%)
Nitric acid (1.40)
5 mi
Bi
m7
Glycerol
Nitric acid (1.40)
Glacial acetic acid
Bi
m8
Dist. water
Silver nitrate
Bi
m4
Remarks
5 mi
Bi
m2
Polishing:
a. See composition bl for polishing aluminum in preparation for microetching. AIso with
alumina on velvet (approx. 150 rpm).
b. Electrolytic:
Special for Bi.
l. Glycerol
I
75 mi
1-5 min,
!!! See Appendix A.
Glacial acetic acid 12.5 mi 12 V dc.
Nitric acid (I.M) 12.5 mi Do not store!
2. Sat. aqueous se!. of
30 s, several times,
potassium iodide
98 mi 5-7 V dc, 0.2
Hydrochloric .acid
A/cm 2
(1.19)
,
2ml
Bi
MI
Technically pure Sb.

Sb-Bi alloys.
MicrfJetching
Bismuth and Antimony

80 mi Equal amounts of (a)
300 mi and (b) are mixed
before use .
45 g
Preparation:
Grinding:
' ''Etching:
/ 49
Sb and Sb alloys.
Pb-Sb, Bi-Sn, and
Bi-Cd alloys.
Sb alloys .
Grain contrast etch.
3 mi
Sb, Bi, and their

alloys.
50 mi
100 (100) mi Secs to mins.

25 (9) mi
25 (9) mi

5g
Bi-Sn eutectic.
Bi-Cd alloys.
Sb-Pb alloys.
Bi.
48
Be
mS
Electrolylic:
Ethanol (96%)
Butyl glycol
Be
m9
Electrolytic:
Hydrochloric acid
(1.19)
Nitric acid (1.40)

Be Electro/y tic:
mIO Phosphoric acid (1.71)
Glycerol
Ethanol (96%)
Sulfuric acid (i.84)
[!O
~ Preparation:
35 mi 30-45 s, below
10 mi 35 oC (95F), 50 V
cathode .
!!! See Appendix A.
Be and Be alloys.
Rapid attack.
294 mi 6 min,
30 oC (85F), 13-20 V
4 mi dc, stanless steel
2 mi cathode.
Be and Be alloys .
Bi
M2
a. Dist. water
Nitric acid (1.40)
b. Dist. water
Ammonium molybdate
Bi
M3
Dist. water
Citric acid
Ammonium molybdate
100 mi
30 mi
30 mi
2.5 mi
I min,
cool (10 oC; 50F),
25 V dc, stainless
.steel or Mo cathode.
Be. Grain-boundary
etch.
AIso used to increase
contrast in polarized
light.
Macroetching
Wet on silicon carbide papers down to 320 grit; if necessary, down to 600 grit.
No.
Etchant
a. Dist. water
Nitric acid' (l.40)
Glacial acetic acid
b. Dist. water
Glacial acetic acid

25 g
Casting imperfections
in Sb and Bi.
lO g
Same as for macroetching.
Etching:
No.
Bi
mi
Conditions
160 mi First with (a) at
40 mi 40 oC (100F). Re30 mi polish untl surface
has become bright.
400 mi Repeat etching with
I mi (b) 1-2 h
Remarks
Sb-Pb, Bi-Sn alloys.
Etchant
Dist . water
Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
Conditions
30 mi
Glacial acetic acid

Hydrogen peroxide
(30%) '
30 mi Secs to mins.
Bi
m3
Dist. water
Hydrochloric acid
(1.19)
Iron (I1I) chloride
For pure and technically pure types of Sb.

Low-alloy Sb.
Sb and Sb alloys.
10 mi
30 mi
2g
Dist. water
Hydrochloric acid
(1.19)
Aqueous sol. of sodium thiosulfate (16%)
Aqueous sol. of chromium (VI) oxide
(10%)
(Czochralski's
etchant)
30 mi Add chromium (VI)

oxide shortly before
15 mi use. Chromium (VI)
oxide content can be
50 mi raised.
!!! See Appendix A.
Bi
m5
Dist. water
Hydrochloric acid
(1.19)
50 mi 1-10 mino
Bi
m6
Ethanol (96%)
Nitric acid (1.40)
5 mi
Bi
m7
Glycerol
Nitric acid (1.40)
Glacial acetic acid
Bi
m8
Dist. water
Silver nitrate
Bi
m4
Remarks
5 mi
Bi
m2
Polishing:
a. See composition bl for polishing aluminum in preparation for microetching. AIso with
alumina on velvet (approx. 150 rpm).
b. Electrolytic:
Special for Bi.
l. Glycerol
I
75 mi
1-5 min,
!!! See Appendix A.
Glacial acetic acid 12.5 mi 12 V dc.
Nitric acid (I.M) 12.5 mi Do not store!
2. Sat. aqueous se!. of
30 s, several times,
potassium iodide
98 mi 5-7 V dc, 0.2
Hydrochloric .acid
A/cm 2
(1.19)
,
2ml
Bi
MI
Technically pure Sb.

Sb-Bi alloys.
MicrfJetching
Bismuth and Antimony

80 mi Equal amounts of (a)
300 mi and (b) are mixed
before use .
45 g
Preparation:
Grinding:
' ''Etching:
/ 49
Sb and Sb alloys.
Pb-Sb, Bi-Sn, and
Bi-Cd alloys.
Sb alloys .
Grain contrast etch.
3 mi
Sb, Bi, and their

alloys.
50 mi

25 (9) mi
25 (9) mi

5g
Bi-Sn eutectic.
Bi-Cd alloys.
Sb-Pb alloys.
Bi.
50
Preparaton of Cd, In, TI
~
In
TI
Preparaton of Co
Cadmium, Indium, Thallium
Cadrniurn, indiurn, and thalliurn, as welI as rnany of their alIoys, are soft
and have a low recrystallization temperature. Pressure during grinding and
polishing, and heating through friction should be kept as low as possible; otherwise,
deformed layers may forrn or fictitious microstructures may be observed.
Cdmium and thallium are toxic (!!! see Appendix A).
Cd
m5
Cd
m6
Ethanol (96%)
Hydrochloric acid
(l.I9)
Picric acid
Electrolylic:
Dist. water
Glycerol
Phosphoric aeid (1.71)
lOO m'! Secs to mins.
51
In and In-rich alloys.
5 mI
Ig
lOO mi 5-10 min,
200 mi 8-9 V dc,
200 mi Cd cathode.
Cd, TI.
Microetching
Preparation:
Orinding:
a. Use a special me for lighl and soft metals.
b. Wel on SiC papers (coat with wax) down to grit size 600.
c. Use lathe, deplh of cul below 25 .a.m.
d . Prepare by microtome using cutters of cemented carbides or, better still, diamond;
eliminates polishing.
Polishing:
a. With alumina slurry or diamond paste down to fmest particle size on rotating wheel,
200-300 rpm. If surface appears milky, add I g ammonium acetate lo 1000 mi distilled
water, and rinse specimen.
b. EleelrolYlie:
l. Oist. waler
. 550 mi
30min,
Cd, TI.
Phosphorie acid (1.71) 450 mi
2 V de, Ni ealhode.
2. Methanol (95%)
670 mi
1-2min,
In.
330 mi
Nitrie acid (1 .40)
40-50 V dc, stainless steel cathode.
e. Chemical:
Oist. water
25 mI
5-10 s.
Cd.
Nitric aeid (1 .40)
75 mi
Etching:
Pure cobalt is tough and has a tendency to produce deformed layers. Cobalt
alloys do not usually pose these difficulties. The distinctly heterogeneous alloys,
such as Stellite, have a tendency to form relief structures, since the hardness
of the individual phases differs greatly.
Macroetching
Preparation:
Wet grinding o~ silicon carbide pap~rs d~wn to 600 grit.
Etching:
No.
Cd
mi
Cd
m2
Cd
:'hI3
Cd
m4
Elchant
Ethanol (96%)'
Nitric acid (1.40)
Oist. water
~
Chromi\!m (VI) oxide
Conditions
98 mi Secs lo mins.
2 mi
100 mi 1-10 mino
IOg !!! See Appendix A.
Cd and solder alloys

eontaining Cd. TI.
Oist. water
Hydroehloric 'add
(1.19)
Iron (III) chlor~de
100 mi Secs lO mins.
Cd-Sn and Cd-Zn

euteetics.
Oist. water
.
Hydrofluorie acid
(40%)
Hydrogen peroxide
(30%)
40 mi 5-10 S .
!!! See Appendix A.
10 mi
25 mi
8g
10 mi
Cd, In, TI. In-Sb and

In-As alloys.
Conditions
Oist. water
Hydroehloric acid
(1.19)
Co
M2
Dist. water
Nitric aeid (1.40)
Hydrochloric acid
(1.19)
Iron (III) chloride
100 mi Swab.
Oist. water
Hydrochloric acid
(1.19)
Nitric acid (1.40)
25 mi Secs to mins.
Remarks
Cd and Cd alloys.
TI.
Etchant
Co
MI
Cd is suitable for obser.vations in polarized light.

No.
Ico I
Cobalt
Co
M3
50 mI 30--60 min, hoto

Rinse in hot water
50 mI
50 mi
IOg
50 mi
25 mi
Remarks
Co-Cr alloys, also
Stellite.
Co-25Cr-IONi-8W,
Co-2ICr-20Ni, and
Co-3Cr-3Mo-INb
alloys.
Other Stellites.
Co-Ni-Fe - base
alloys.
High-temperature
alloys.
Microetching
Preparation:
Grinding:
Same as for macroetching. For cemented carbides use silicon carbide slurries (grit size
in distilled water on cast iron wheel.
220~8(0)
Polishing:
a. Oiamond paste (particle size 15-1 .a.m).
'~~I '.
50
Preparaton of Cd, In, TI
~
In
TI
Preparaton of Co
Cadmium, Indium, Thallium
Cadrniurn, indiurn, and thalliurn, as welI as rnany of their alIoys, are soft
and have a low recrystallization temperature. Pressure during grinding and
polishing, and heating through friction should be kept as low as possible; otherwise,
deformed layers may forrn or fictitious microstructures may be observed.
Cdmium and thallium are toxic (!!! see Appendix A).
Cd
m5
Cd
m6
Ethanol (96%)
Hydrochloric acid
(l.I9)
Picric acid
Electrolylic:
Dist. water
Glycerol
Phosphoric aeid (1.71)
lOO m'! Secs to mins.
51
In and In-rich alloys.
5 mI
Ig
lOO mi 5-10 min,
200 mi 8-9 V dc,
200 mi Cd cathode.
Cd, TI.
Microetching
Preparation:
Orinding:
a. Use a special me for lighl and soft metals.
b. Wel on SiC papers (coat with wax) down to grit size 600.
c. Use lathe, deplh of cul below 25 .a.m.
d . Prepare by microtome using cutters of cemented carbides or, better still, diamond;
Polishing:
a. With alumina slurry or diamond paste down to fmest particle size on rotating wheel,
200-300 rpm. If surface appears milky, add I g ammonium acetate lo 1000 mi distilled
water, and rinse specimen.
b. EleelrolYlie:
l. Oist. waler
. 550 mi
30min,
Cd, TI.
Phosphorie acid (1.71) 450 mi
2 V de, Ni ealhode.
2. Methanol (95%)
670 mi
1-2min,
In.
330 mi
Nitrie acid (1 .40)
40-50 V dc, stainless steel cathode.
e. Chemical:
Oist. water
25 mI
5-10 s.
Cd.
Nitric aeid (1 .40)
75 mi
Etching:
Pure cobalt is tough and has a tendency to produce deformed layers. Cobalt
alloys do not usually pose these difficulties. The distinctly heterogeneous alloys,
such as Stellite, have a tendency to form relief structures, since the hardness
of the individual phases differs greatly.
Macroetching
Preparation:
Wet grinding o~ silicon carbide pap~rs d~wn to 600 grit.
Etching:
No.
Cd
mi
Cd
m2
Cd
:'hI3
Cd
m4
Elchant
Ethanol (96%)'
Nitric acid (1.40)
Oist. water
~
Chromi\!m (VI) oxide
Conditions
98 mi Secs lo mins.
2 mi
100 mi 1-10 mino
Cd and solder alloys

eontaining Cd. TI.
Oist. water
Hydroehloric 'add
(1.19)
Iron (III) chlor~de
100 mi Secs lO mins.
Cd-Sn and Cd-Zn

euteetics.
Oist. water
.
Hydrofluorie acid
(40%)
Hydrogen peroxide
(30%)
40 mi 5-10 S .
!!! See Appendix A.
10 mi
25 mi
8g
10 mi
Cd, In, TI. In-Sb and

In-As alloys.
Conditions
Oist. water
Hydroehloric acid
(1.19)
Co
M2
Dist. water
Nitric aeid (1.40)
Hydrochloric acid
(1.19)
Iron (III) chloride
100 mi Swab.
Oist. water
Hydrochloric acid
(1.19)
Nitric acid (1.40)
25 mi Secs to mins.
Remarks
Cd and Cd alloys.
TI.
Etchant
Co
MI
Cd is suitable for obser.vations in polarized light.

No.
Ico I
Cobalt
Co
M3
50 mI 30--60 min, hoto

Rinse in hot water
50 mI
50 mi
IOg
50 mi
25 mi
Remarks
Co-Cr alloys, also
Stellite.
Co-25Cr-IONi-8W,
Co-2ICr-20Ni, and
Co-3Cr-3Mo-INb
alloys.
Other Stellites.
Co-Ni-Fe - base
alloys.
High-temperature
alloys.
Microetching
Preparation:
Grinding:
Same as for macroetching. For cemented carbides use silicon carbide slurries (grit size
in distilled water on cast iron wheel.
220~8(0)
Polishing:
a. Oiamond paste (particle size 15-1 .a.m).
'~~I '.
52
Preparation of Co
Preparation ot Co
b. Electrolytic:
1. Methanol (95 %)
Nitric acid (1.40)
2. Phosphoric acid
(1.71)
;l . Dis!. water
Phosphoric acid
(1.71)
c. Chemical:
Lactic acid (90%)
Hydrochloric acid
(1.I9)
Nitric acid (1.40)
600 mi 10-60 s, 40-70 V de,

l!! See Appendix A.
330 mi stainless steel cathode .
3- 5 min, 1.5 V de, stainless steel cathode .
600 mi 1- 15 min, 1- 2 V dc, stainless steel or Co cathode.
400 mi
40 mi Secs to mins.
Etchant
30 mi
S mi
Conditions
Remarks
Co
mi
Methanol (95 %)
Nitric acid (1.40)
Co
m2
Dis!. water
Glacial acetic acid
Hydrochloric acid
(1.19)
Nitric acid (1 .40)
15 mi 5-30 S.
15 mi Wait at least 1 h
before use .
15 mi
Pure and low-alloy

CO. Co-B alloys.
Co-Ti alloys, and
Co-Mn alloys. WCTiC-TaC-Co - type cemented carbides.
Co
m3
Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
Few secs .
!!! See Appendix A.
5 mi
Wear-resistant alloys.
Alloys used for Cobase cutting tools.
Superalloys.
Co
m4
Dis!. water
Ammonium persuIfate
Co
m5
Dist. water
Potassium hydroxide
Potassium fenlcyanide
Co
m6
Hydrochloric atid
(1.19) ,
Nitric acid (1.40)
' ''Co
m7
Dis!. water
Hydrochloric acid
(1.19)
.,
Methanol (95%)
Nitric acid (1.40)
Iron (III) chloride
Copper (H) chloride
100 mi . Secs to mins.

1- 100 mI S min o
!!! See Appendix A.
100 mI Secs to mins.

20- 30 g
IOg
Secs to 5 min o
75 mI Use fresh only.
100 mi 10-15 S .
Immerse or swab.
looml
200 mi
5 mi
7g
2g
Dist. water
Nitric acid (1.40)
Co
m9
Hot etching in air
Co Dis!. water
m 10 Glacial acetic acid
Nitric acid (1 .40)
Etching:
No .
Co
m8
Pure CO. Co-Fe

alloys.
WC-TiC-NbC-Cotype cemented carbides.
Cemented carbides
and other Co-base
alloys.
WC-TiC-TaC-Co and
WC-NbC-Co - type
cemented carbides.
WC-TiC-NbC-Co type cemented
carbides.
Co-Pt alloys.
Co-Fe alloys.
Magnetic alloys.
Co Electrolytic:
mil Dis!. water
Potassium hydroxide
Sodium carbonate
Co Electrolytic:
ml2 Dist . water
Hydrochloric acid
(1.19)
Iron (IlI) chloride
loofml 90 s.
SO mI
53
Co-Ga alloys.
30 min, 400-450 oC
(750-850 F).
WC-TiC-(Ta, Nb)CCo - type cemented

carbides.
Carbide phases are
easily distinguishable
from binder phases by
differences in colors.
100 mI Few secs .

Iml
Iml
Co-Sm alloys.
100 mi 10 s, 3 V de, stainless

3g steel cathode .
2g Increase of sodium
carbonate content increases removal rate
of WC phase. Deposit
removed with diluted
hydrochloric acid.
Cemented carbides
with Co binder phase .
100 mi Few secs, 6 V de,

stainless steel
5 mI' cathode.
IOg
Pure CO.
_Co-AI alloys . .
Co Electroly tic:
ml3 Dist. water or Hydrochloric acid (1.19)
Chromium (VI) oxide
2- 20 s , 3 V dc, stain100 mi less steel cathode.

2- 10 g !!! See Appendix A.
Stellite up to 70% CO.

Co-base superalloys .
Co silicides.
Co Electrolytic:
ml4 Dis!. water
HydrochIoric acid
(1.19)
100 mi 2- 10 s, 3 V de, graphite cathode.

5-10 mI
Pure CO.
Co Electrolylic:
miS Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
3-5 s, 4 V de, stainlOO mi less steel cathode.

!!! See Appendix A.
5ml
Co-base wear-resistant
alloys and materials
used for cutting tools.
Superalloys.
52
Preparation of Co
Preparation ot Co
b. Electrolytic:
1. Methanol (95 %)
Nitric acid (1.40)
2. Phosphoric acid
(1.71)
;l . Dis!. water
Phosphoric acid
(1.71)
c. Chemical:
Lactic acid (90%)
Hydrochloric acid
(1.I9)
Nitric acid (1.40)
600 mi 10-60 s, 40-70 V de,

l!! See Appendix A.
330 mi stainless steel cathode .
3- 5 min, 1.5 V de, stainless steel cathode .
600 mi 1- 15 min, 1- 2 V dc, stainless steel or Co cathode.
400 mi
40 mi Secs to mins.
Etchant
30 mi
S mi
Conditions
Remarks
Co
mi
Methanol (95 %)
Nitric acid (1.40)
Co
m2
Dis!. water
Glacial acetic acid
Hydrochloric acid
(1.19)
Nitric acid (1 .40)
15 mi 5-30 S.
15 mi Wait at least 1 h
before use .
15 mi
Pure and low-alloy

CO. Co-B alloys.
Co-Ti alloys, and
Co-Mn alloys. WCTiC-TaC-Co - type cemented carbides.
Co
m3
Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
Few secs .
!!! See Appendix A.
5 mi
Wear-resistant alloys.
Alloys used for Cobase cutting tools.
Superalloys.
Co
m4
Dis!. water
Ammonium persuIfate
Co
m5
Dist. water
Potassium hydroxide
Potassium fenlcyanide
Co
m6
Hydrochloric atid
(1.19) ,
Nitric acid (1.40)
' ''Co
m7
Dis!. water
Hydrochloric acid
(1.19)
.,
Methanol (95%)
Nitric acid (1.40)
Iron (III) chloride
Copper (H) chloride
100 mi . Secs to mins.

1- 100 mI S min o
!!! See Appendix A.

20- 30 g
IOg
Secs to 5 min o
75 mI Use fresh only.
100 mi 10-15 S .
Immerse or swab.
looml
200 mi
5 mi
7g
2g
Dist. water
Nitric acid (1.40)
Co
m9
Hot etching in air
Co Dis!. water
m 10 Glacial acetic acid
Nitric acid (1 .40)
Etching:
No .
Co
m8
Pure CO. Co-Fe

alloys.
WC-TiC-NbC-Cotype cemented carbides.
Cemented carbides
and other Co-base
alloys.
WC-TiC-TaC-Co and
WC-NbC-Co - type
cemented carbides.
WC-TiC-NbC-Co type cemented
carbides.
Co-Pt alloys.
Co-Fe alloys.
Magnetic alloys.
Co Electrolytic:
mil Dis!. water
Potassium hydroxide
Sodium carbonate
Co Electrolytic:
ml2 Dist . water
Hydrochloric acid
(1.19)
Iron (IlI) chloride
loofml 90 s.
SO mI
53
Co-Ga alloys.
30 min, 400-450 oC
(750-850 F).
WC-TiC-(Ta, Nb)CCo - type cemented

carbides.
Carbide phases are
easily distinguishable
from binder phases by
differences in colors.
100 mI Few secs .

Iml
Iml
Co-Sm alloys.
100 mi 10 s, 3 V de, stainless

3g steel cathode .
2g Increase of sodium
carbonate content increases removal rate
of WC phase. Deposit
removed with diluted
hydrochloric acid.
Cemented carbides
with Co binder phase .
100 mi Few secs, 6 V de,

stainless steel
5 mI' cathode.
IOg
Pure CO.
_Co-AI alloys . .
Co Electroly tic:
ml3 Dist. water or Hydrochloric acid (1.19)
Chromium (VI) oxide
2- 20 s , 3 V dc, stain100 mi less steel cathode.

2- 10 g !!! See Appendix A.
Stellite up to 70% CO.

Co silicides.
Co Electrolytic:
ml4 Dis!. water
HydrochIoric acid
(1.19)
100 mi 2- 10 s, 3 V de, graphite cathode.

5-10 mI
Pure CO.
Co Electrolylic:
miS Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
3-5 s, 4 V de, stainlOO mi less steel cathode.

!!! See Appendix A.
5ml
Co-base wear-resistant
alloys and materials
used for cutting tools.
Superalloys.
54
Preparation of Cr, Mo, Nb, Re, Ta, V, W
Chromium, Molybdenum, Niobium, Rhenium,

Tantalum, Vanadium, Tungsten
Cr
Mo
Nb
Re
Ta
In the pure state, these materials are soft and tough. In the commercially
pure state, however, they are hard to brittle because of nonmetallic impurities.
Wet grinding on silicon carbide papers down to 600 grit.
Etching:
Macroetching
Preparation:
No.
Etchant
Conditions
Remarks
Cr
MI
Oist. water
90 mi 2-5 mino
10 mi Boiling.
Cr.
Cr
M2
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Secs to mins.
15 mi
Mo, W, V, Nb, Ta,

and their alloys .
Cr
M3
Oist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
30 mi
75 mi 10-20 min o
Mo, W, and V.
15ml
Microetching
Preparation:
Grinding:
Same as for maeroetehing.
e. Eleetrolytic lapping:
1. Oist. water
Sodium hydroxide
2. Oist. water with
alumina slurry
No. 3 (0.05 f.Lm ,
Linde B)
Potassium ferricyanide
3. Dist. water with
alumina slurry
No . 3 (0.05 f.Lm,
Linde B)
Hydrogen peroxide (30%)
4. Methanol (95%)
Nitric aeid (1.40)
Hydrofluoric acid
(40%)
Citric acid
d. Chemical:
Sulfuric aeid
(1.84)
Nitric aeid (1.40)
Hydrofluorie aeid
(40%)
55
W.
Mo.
1g
20 mion, 1- 10 mAj cm'.
stainless steel eathode.
Nb.
300 mi
10 mi
510 mi 40 s, 5 mA j cm', stain170 mi less steel eathode.
!!! See Appendix A.
50 mi
5g
5-10 s .
20 mi
Nb .
Preferentially for Ta
and Nb.
20 mi
Etching:
\[0 .
Reagent
Cr
mi
Nitric acid (1.40)

Hydroehloric acid
(1.19)
Conditions
20 mi 5-60 s.
00 not store!
60 mi
Cr
m2
Nitric aeid (1.40)

Hydrofluoric acid
(40%)
20 mi Approx 10 s.
!! ! See Appendix A.
60 mi
Cr
m3
a. Oist. water
Potassium hydroxide
100 mi 15-60 s.
10 g Equal amounts of (a)
and (b).
For Mo and W, sodi10 g um hydroxide and sodium ferrieyanide
may also be used.
Polishing:
a. With diamond paste or alumina slurry down to finest particle size; best on wheel
with hardwood cover. In mosl cases, attack-polishing with oneof the eleetrolyles
listed under (b) iSbf advantage .
I
b. Eleetrolytic:
1. MethanQI (95%t or
30 s t02 min, 6-18 V
Mo
dist. w.ter
!!! See Appendix A.
Sulfurie aeid
eathode .
(1.84)
125 mi
'J i"
2. Sulfuric acid . ,
5-10 min, approx 40 oC Nb, Ta.
(1.84)
900 mi (100 F)
!!! See Appendix A.
Hydrofluorie acid
(40%)
100 mi
3. Oist. water
1000 mi 10-25 min, 6 V dc,
W, Cr.
Sodium hydroxide
100 mi graphite eathode.
4. Glacial acetie aeid 900-950 mi Secs to 2 min , 25-30 V Cr, V, Re.
Perchlorie acid
dc.
(60%)
100 mi 1- lOmin, 10-20 V de,

2g stainless steel cathode .
Velvet cloth.
5-10 min, 40 V de,
Tough nylon cloth.
30 mi
b. Oist. water
Cr
m4
Oist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)

50 (25) mi !!! See Appendix A.
50(5)ml
Remarks
Cr and Cr-base
alloys.
Cr, Nb. and alloys.
Cr. Mo, Mo-Cr alloys

(up to 80% Cr).
Mo-Fe alloys.
W and W-base
alloys.
Mo-Re alloys. Re and
Re-base alloys .
Ta, Nb, and their
alloys. Cr and Cr silicide. Re silicide.
W-Th alloys.
'~~ I"
54
Chromium, Molybdenum, Niobium, Rhenium,

Tantalum, Vanadium, Tungsten
Cr
Mo
Nb
Re
Ta
In the pure state, these materials are soft and tough. In the commercially
pure state, however, they are hard to brittle because of nonmetallic impurities.
Wet grinding on silicon carbide papers down to 600 grit.
Etching:
Macroetching
Preparation:
No.
Etchant
Conditions
Remarks
Cr
MI
Oist. water
90 mi 2-5 mino
10 mi Boiling.
Cr.
Cr
M2
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Secs to mins.
15 mi
Mo, W, V, Nb, Ta,

and their alloys .
Cr
M3
Oist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
30 mi
75 mi 10-20 min o
Mo, W, and V.
15ml
Microetching
Preparation:
Grinding:
Same as for maeroetehing.
e. Eleetrolytic lapping:
1. Oist. water
Sodium hydroxide
2. Oist. water with
alumina slurry
No. 3 (0.05 f.Lm ,
Linde B)
3. Dist. water with
alumina slurry
No . 3 (0.05 f.Lm,
Linde B)
Hydrogen peroxide (30%)
4. Methanol (95%)
Nitric aeid (1.40)
Hydrofluoric acid
(40%)
Citric acid
d. Chemical:
Sulfuric aeid
(1.84)
Nitric aeid (1.40)
Hydrofluorie aeid
(40%)
55
W.
Mo.
1g
20 mion, 1- 10 mAj cm'.
Nb.
300 mi
10 mi
510 mi 40 s, 5 mA j cm', stain170 mi less steel eathode.
!!! See Appendix A.
50 mi
5g
5-10 s .
20 mi
Nb .
Preferentially for Ta
and Nb.
20 mi
Etching:
\[0 .
Reagent
Cr
mi
Nitric acid (1.40)

Hydroehloric acid
(1.19)
Conditions
20 mi 5-60 s.
00 not store!
60 mi
Cr
m2
Nitric aeid (1.40)

Hydrofluoric acid
(40%)
20 mi Approx 10 s.
!! ! See Appendix A.
60 mi
Cr
m3
a. Oist. water
Potassium hydroxide
100 mi 15-60 s.
10 g Equal amounts of (a)
and (b).
For Mo and W, sodi10 g um hydroxide and sodium ferrieyanide
may also be used.
Polishing:
a. With diamond paste or alumina slurry down to finest particle size; best on wheel
with hardwood cover. In mosl cases, attack-polishing with oneof the eleetrolyles
listed under (b) iSbf advantage .
I
b. Eleetrolytic:
1. MethanQI (95%t or
30 s t02 min, 6-18 V
Mo
dist. w.ter
!!! See Appendix A.
Sulfurie aeid
eathode .
(1.84)
125 mi
'J i"
2. Sulfuric acid . ,
5-10 min, approx 40 oC Nb, Ta.
(1.84)
900 mi (100 F)
!!! See Appendix A.
Hydrofluorie acid
(40%)
100 mi
3. Oist. water
1000 mi 10-25 min, 6 V dc,
W, Cr.
Sodium hydroxide
100 mi graphite eathode.
4. Glacial acetie aeid 900-950 mi Secs to 2 min , 25-30 V Cr, V, Re.
Perchlorie acid
dc.
(60%)
100 mi 1- lOmin, 10-20 V de,

2g stainless steel cathode .
Velvet cloth.
5-10 min, 40 V de,
Tough nylon cloth.
30 mi
b. Oist. water
Cr
m4
Oist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)

50(5)ml
Remarks
Cr and Cr-base
alloys.
Cr, Nb. and alloys.
Cr. Mo, Mo-Cr alloys

(up to 80% Cr).
Mo-Fe alloys.
W and W-base
alloys.
Mo-Re alloys. Re and
Re-base alloys .
Ta, Nb, and their
alloys. Cr and Cr silicide. Re silicide.
W-Th alloys.
'~~ I"
56
Cr
m5
Cr
m6
Cr
m7
Cr
m8
Cr
m9
Dist. water
Hydrogen peroxide
(3%)
Ammonia water
Dist. water
Hydrofluoric acid
(40%)
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Lactic acid (90%)
Glacial acetic acid
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Dist. water
Hydrogen peroxide
(30%)
Cr
mIO
Glycerol
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Cr
mll
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Glycerol
Cr
ml2
Hydrochloric acid
f
(l.l9)
Hydrogen p$iroxide
(3%)
Cr
ml3
' 'Cr
ml4
Cr
ml5
t.
Dist., water
Picric acid
Sodium hydroxide
.
50(70) mI Secs to mins.

10 min, boiling.
50 (20) mi
50(10) mi
50 mIlOs.
!!! See Appendix A.
50 mI
15-20 sec
10 (10) mI Do not store!
30(10)mI !!! See Appendix A.
60 (30) mI
50 mI 10-30 S.
20 nil !!! See Appendix A.
Dist. water
Sodium hydroxide
Cr
ml6
Eleetroly tic:
Dist. water
Sodium hydroxide
Cr
ml7
Eleetrolytie:
Dist. water
Oxalic acid
Ta and Ta-base
alloys.
100 mI 2-5 s, 6 V dc, stainIOg less steel cathode.

1 min
Nb, Ta, Mo and

their aIloys. Propor~
tions in parentheses
for Ta and Nb alloys.
Cr
ml8
Eleetroly tic:
Dist. water or
ethanol (96%)
Hydrochloric acid
(1.19)
lOO mI 30-90 S.
Boiling.
Iml
Cr
ml9
Eleetrolytie:
Cr
m20
10-20 mI Up to 5 mino
!!! See Appendix A.
10ml
10 mi
Mo, Ta, Nb, Mo-Ti

alloys. Ta-Nb alloys.
Pure V and V-base
alloys.
Secs to mins.
Cr and Cr alloys.
Secs to mins.
W-Co alloys containing 10-70% W.
30 mI
15 mI
45 mI
lO mI
10 mI
100 mI 15 s.
2g Boiling.
25 g
50 (O) mI Secs to mins.
!!! See Appendix A.
20 (20) mI
10 (20) mI
15 (50) mI
lOO mI Secs to mins.

IOg
Eutectic W-Co
alloys.
W component turns
black.
Ta and Ta-base
alloys. Nb and Nbbase alloys.
Nb-Cr alloys.
Mo and Mo alloys.
Pure Ta.
Mo (grain contrast)
Pure V and V-base
alloys. Cr and Crbase alloys.
Re and Re-base
aIloys.
Secs to mins, 5-10 V

95 mI dc, stainless steel
cathode.
5 mI
V and V-base alloys.

AIloys of high Cr
content. Mo-Cr-Fe
aIloys. Mo and Mo
alloys. U-Nb alloys.
Ferrovanadium.
Cr silicides. Galvanic
Cr layers.
95 mI 15 s, 30-50 V dc,
5 mI stainless steel or Pt
cathode.
!!! See Appendix A.
Cr and Crcbase
alloys.
Fe-Cr alloys. V.
Eleetrolytie:
Methanol (95%)
Hydrofluoric acid
(40%)
lOO mI 10-20 s,
5 mI 50-60 V dc.
!!! See Appendix A.
I mi
W and W-base
alloys.
Mo and Mo-base
alloys.
Cr
m21
Eleetrolytie:
Methanol (95%)
Hydrochloric acid
(1.19)
75 mI 30 s, 30 V dc,
10 mi stainless steel
cathode.
Ta and Ta-base
alloys. Mo and Mobase alloys. V and
V-base alloys.
Cr
m22
Eleetrolytie:
Dist. water
Nitric acid(1.40)
Hydrofluoric acid
(40%)
65 mI Secs to mins,
17 mI 12-30 V dc,
Pt cathode.
Pure Nb.
Mo.
Ta-base alIoys.
Nb-base aIloys.
W and W-base
alloys.
57
lOO mI Secs to mins, 1.5-6 V W and W-base

alloys.
10 g dc, stainless stee1
Ta and its alloys.
cathode.
5 mI
"
Dist. water
. Hydrofluor.ic acid
(40%)
Nitricacid (1,40)
S ulfuric acid (1. 84)
Mo and Mo-Ni
alloys.
W and W alloys.
Proportions in parentheses for Nb and its
alloys.
Glacial acetic acid

'i~
56
Cr
m5
Cr
m6
Cr
m7
Cr
m8
Cr
m9
Dist. water
Hydrogen peroxide
(3%)
Ammonia water
Dist. water
Hydrofluoric acid
(40%)
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Lactic acid (90%)
Glacial acetic acid
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Dist. water
Hydrogen peroxide
(30%)
Cr
mIO
Glycerol
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Cr
mll
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Glycerol
Cr
ml2
Hydrochloric acid
f
(l.l9)
Hydrogen p$iroxide
(3%)
Cr
ml3
' 'Cr
ml4
Cr
ml5
t.
Dist., water
Picric acid
Sodium hydroxide
.

10 min, boiling.
50 (20) mi
50(10) mi
50 mIlOs.
!!! See Appendix A.
50 mI
15-20 sec
10 (10) mI Do not store!
30(10)mI !!! See Appendix A.
60 (30) mI
50 mI 10-30 S.
20 nil !!! See Appendix A.
Dist. water
Sodium hydroxide
Cr
ml6
Eleetroly tic:
Dist. water
Sodium hydroxide
Cr
ml7
Eleetrolytie:
Dist. water
Oxalic acid
Ta and Ta-base
alloys.
100 mI 2-5 s, 6 V dc, stainIOg less steel cathode.

1 min
Nb, Ta, Mo and

their aIloys. Propor~
tions in parentheses
for Ta and Nb alloys.
Cr
ml8
Eleetroly tic:
Dist. water or
ethanol (96%)
Hydrochloric acid
(1.19)
lOO mI 30-90 S.
Boiling.
Iml
Cr
ml9
Eleetrolytie:
Cr
m20
10-20 mI Up to 5 mino
!!! See Appendix A.
10ml
10 mi
Mo, Ta, Nb, Mo-Ti

alloys. Ta-Nb alloys.
Pure V and V-base
alloys.
Secs to mins.
Cr and Cr alloys.
Secs to mins.
W-Co alloys containing 10-70% W.
30 mI
15 mI
45 mI
lO mI
10 mI
100 mI 15 s.
2g Boiling.
25 g
50 (O) mI Secs to mins.
!!! See Appendix A.
20 (20) mI
10 (20) mI
15 (50) mI
lOO mI Secs to mins.

IOg
Eutectic W-Co
alloys.
W component turns
black.
Ta and Ta-base
alloys. Nb and Nbbase alloys.
Nb-Cr alloys.
Mo and Mo alloys.
Pure Ta.
Mo (grain contrast)
Pure V and V-base
alloys. Cr and Crbase alloys.
Re and Re-base
aIloys.
Secs to mins, 5-10 V

cathode.
5 mI
V and V-base alloys.

AIloys of high Cr
content. Mo-Cr-Fe
aIloys. Mo and Mo
alloys. U-Nb alloys.
Ferrovanadium.
Cr silicides. Galvanic
Cr layers.
95 mI 15 s, 30-50 V dc,
5 mI stainless steel or Pt
cathode.
!!! See Appendix A.
Cr and Crcbase
alloys.
Fe-Cr alloys. V.
Eleetrolytie:
Methanol (95%)
Hydrofluoric acid
(40%)
lOO mI 10-20 s,
5 mI 50-60 V dc.
!!! See Appendix A.
I mi
W and W-base
alloys.
Mo and Mo-base
alloys.
Cr
m21
Eleetrolytie:
Methanol (95%)
Hydrochloric acid
(1.19)
75 mI 30 s, 30 V dc,
10 mi stainless steel
cathode.
Ta and Ta-base
alloys. Mo and Mobase alloys. V and
V-base alloys.
Cr
m22
Eleetrolytie:
Dist. water
Nitric acid(1.40)
Hydrofluoric acid
(40%)
65 mI Secs to mins,
17 mI 12-30 V dc,
Pt cathode.
Pure Nb.
Mo.
Ta-base alIoys.
Nb-base aIloys.
W and W-base
alloys.
57
lOO mI Secs to mins, 1.5-6 V W and W-base

alloys.
10 g dc, stainless stee1
Ta and its alloys.
cathode.
5 mI
"
Dist. water
. Hydrofluor.ic acid
(40%)
Nitricacid (1,40)
S ulfuric acid (1. 84)
Mo and Mo-Ni
alloys.
W and W alloys.
Proportions in parentheses for Nb and its
alloys.
Glacial acetic acid

'i~
58
Preparation of
Preparation of Cu
Pure copper is very soft, and metallographic preparation often results in

deformed layers. Grinding and polishing residues are easily embedded into the
surface .of the microsection. The pteparation of copper alloys generally does
not pos.e any difficulties.
Macroetching
Preparation:
Coarse grinding is sufficient (wet on silieon carbide papers down to 400 grit).
Polishing:
a. With alumina slurry or diamond paste down to finest particle size , Possibly under
addition of a solution of ammonium hydroxide or eopper ammonium persulfate; this
frequentIy eliminates etehing.
b. Same as under (a) but additional eteh-polishing sequenee with etehant No. Cu m6.
e. Eleetrolytie:
l. Oist. water
Phosphoric aeid
(1.71)
15 min, 2 V de, Cu
cathode.
For all types of Cu and

Cu aIJoys, with exeeption
of Sn bronzes.
After polishing, rinse in
a 20% aqueous solution
of phosphorie aeid.
Same as for (c. 1) above.
AIso used for Sn bronzes.
3-6 s, 6 V dc, Al eathode.
Al and Be bronzes.
5-7 min,
2
5 mA/O.4 em
2
8-9 mA/0.64 em
2
\O mA/0.8 cm
High-purity CU .
RoIled Cu.
80Ag-20Cu.
1-2 min, up to 80 oC
(180F).
AIJ types of Cu and Cu

alloys .
Oxide Iayer formed during polishing is removed

with \0% hydrofluoric
aeid.
!!! See Appendix A.
Grain boundaries.
Cu-AI aIloys ,
Alpha, gamma phase.
300 mI 5-15 min, L5-2 V de,

Cu athode.
700 mi
Etching:
Conditions
Etehant
Oist. water or
ethanol (96%)
Hydroehloric aeid
(1.19)
Iron (IlI) ehloride
Cu
MI
Few mins .
120 (100) mI
30(6) mi
1O(20)g
lOO mI
1g
100 mi
1 mi
Mix (a) and (b) in

equal amounts. Time
untihample begins to
crack is an indication
of stresses.
!!! See Appendix A.
Verification of
stresses in brass.
Samples with sfresses
begin to crack after
sorne time.
a. Oist. water
Mereury (H) nitrate
b. Oist. water
Nitric acid (1.40)
eu
M3
Oist. water
Nitric acid (1.40)
90 mI Few mins.
10-60 mi
Cu
M4
Oist. water
Nitrie acid (1.40)
50 mI Few mins.
50 mi
Cu and brasses.
Grain eontrast.
Cu
M5
Oist. water
Nitrie aeid (1.40)
Silver nitra te
50 mi Sees to mins.
50 mi Oeep etehing.
5g
.
AH types of Cu and
Cu alIoys.
Cu
M6
Oist. water
~.
Nitrie aeid (1.40)
Sulfuric a~id (1.84)
Ammonium ehIorlde
Chromium (VI) o,cide
Cu '".
M7
Oist. water
Ammonium persul.rate
Cu and all types of

brasses. Grains and
eraeks.
100 mi Sees to mins.

8 mI
7.5 g
40 g
Brasses eontaining
Si.
Si bronzes.
100 mi Sees to mins .
Brasses. Espeeially
brasses containing
CO.
25 g
Microetching
Preparation:
Grinding:
a . Wet on silicon earbide papers down to 600 grit.
,:< JI
Remarks
Cu and all types of
brasses. Grain eontrast. Bronzes. Al
bronze. Formation of
dendrites in alpha
alloys .
Cu
M2
59
b. Prepare by microtome using eutters of eemented earbides or, still better, diamond;
eliminates polishing. For all eopper alloys with a hardness of les s than 150 HV.
Copper
No.
eu /
300 mi
2. Oist. water
Phosphoric acid
670 mi
(1.71)
100 mi
100 mI
3. Oist. water
Chromium (VI)
1g
oxide
d. Eleetrolytie lapping:
885 mi
Oist. water
12 g
. Sodium thiosulfate
Ig
Copper (11) nitrate
2g
Thiourea
e. Chemieal:
30 mi
1. Nitrie acid (1.40)
Hydroehloric acid
10 mi
(1.19)
Phosphorie aeid
\O mI
. (1.71)
50 mI
Glacial aeetic aeid
(Coneentration
variable)
35 (\00) mI
2. Oist. water
40 (7) mi
Nitrie acid (1.40)
Chromium (VI)
25 (27) g
oxide
(Coneentration
variable)
';,[1'
Etching:
No.
Cu
mi
Etehant
Oist. water or ethanol
(95%)
Hydroehlorie aeid
(1.19)
Iron (III) ehloride
.
Proeedure
Sees to mins .
100- 120 mi Possibly followed by
Cum4.
20-50 mi
5~10 mI
Remarks
AIl types of Cu.
Cu-Be alloys. Brasses
(colors beta brass).
Special bronzes.
Al bronze with euteetoid. German silver.
'~~
:~l
~;i
58
Preparation of
Preparation of Cu
Pure copper is very soft, and metallographic preparation often results in

deformed layers. Grinding and polishing residues are easily embedded into the
surface .of the microsection. The pteparation of copper alloys generally does
not pos.e any difficulties.
Macroetching
Preparation:
Coarse grinding is sufficient (wet on silieon carbide papers down to 400 grit).
Polishing:
a. With alumina slurry or diamond paste down to finest particle size , Possibly under
addition of a solution of ammonium hydroxide or eopper ammonium persulfate; this
frequentIy eliminates etehing.
b. Same as under (a) but additional eteh-polishing sequenee with etehant No. Cu m6.
e. Eleetrolytie:
l. Oist. water
Phosphoric aeid
(1.71)
15 min, 2 V de, Cu
cathode.
For all types of Cu and

Cu aIJoys, with exeeption
of Sn bronzes.
After polishing, rinse in
a 20% aqueous solution
of phosphorie aeid.
Same as for (c. 1) above.
AIso used for Sn bronzes.
3-6 s, 6 V dc, Al eathode.
Al and Be bronzes.
5-7 min,
2
5 mA/O.4 em
2
8-9 mA/0.64 em
2
\O mA/0.8 cm
High-purity CU .
RoIled Cu.
80Ag-20Cu.
1-2 min, up to 80 oC
(180F).
AIJ types of Cu and Cu

alloys .
Oxide Iayer formed during polishing is removed

with \0% hydrofluoric
aeid.
!!! See Appendix A.
Grain boundaries.
Cu-AI aIloys ,
Alpha, gamma phase.
300 mI 5-15 min, L5-2 V de,

Cu athode.
700 mi
Etching:
Conditions
Etehant
Oist. water or
ethanol (96%)
Hydroehloric aeid
(1.19)
Iron (IlI) ehloride
Cu
MI
Few mins .
120 (100) mI
30(6) mi
1O(20)g
lOO mI
1g
100 mi
1 mi
Mix (a) and (b) in

equal amounts. Time
untihample begins to
crack is an indication
of stresses.
!!! See Appendix A.
Verification of
stresses in brass.
Samples with sfresses
begin to crack after
sorne time.
a. Oist. water
Mereury (H) nitrate
b. Oist. water
Nitric acid (1.40)
eu
M3
Oist. water
Nitric acid (1.40)
90 mI Few mins.
10-60 mi
Cu
M4
Oist. water
Nitrie acid (1.40)
50 mI Few mins.
50 mi
Cu and brasses.
Grain eontrast.
Cu
M5
Oist. water
Nitrie aeid (1.40)
Silver nitra te
50 mi Sees to mins.
50 mi Oeep etehing.
5g
.
AH types of Cu and
Cu alIoys.
Cu
M6
Oist. water
~.
Nitrie aeid (1.40)
Sulfuric a~id (1.84)
Ammonium ehIorlde
Chromium (VI) o,cide
Cu '".
M7
Oist. water
Ammonium persul.rate
Cu and all types of

brasses. Grains and
eraeks.
100 mi Sees to mins.

8 mI
7.5 g
40 g
Brasses eontaining
Si.
Si bronzes.
100 mi Sees to mins .
Brasses. Espeeially
brasses containing
CO.
25 g
Microetching
Preparation:
Grinding:
a . Wet on silicon earbide papers down to 600 grit.
,:< JI
Remarks
Cu and all types of
brasses. Grain eontrast. Bronzes. Al
bronze. Formation of
dendrites in alpha
alloys .
Cu
M2
59
b. Prepare by microtome using eutters of eemented earbides or, still better, diamond;
eliminates polishing. For all eopper alloys with a hardness of les s than 150 HV.
Copper
No.
eu /
300 mi
2. Oist. water
Phosphoric acid
670 mi
(1.71)
100 mi
100 mI
3. Oist. water
Chromium (VI)
1g
oxide
d. Eleetrolytie lapping:
885 mi
Oist. water
12 g
. Sodium thiosulfate
Ig
Copper (11) nitrate
2g
Thiourea
e. Chemieal:
30 mi
1. Nitrie acid (1.40)
Hydroehloric acid
10 mi
(1.19)
Phosphorie aeid
\O mI
. (1.71)
50 mI
Glacial aeetic aeid
(Coneentration
variable)
35 (\00) mI
2. Oist. water
40 (7) mi
Nitrie acid (1.40)
Chromium (VI)
25 (27) g
oxide
(Coneentration
variable)
';,[1'
Etching:
No.
Cu
mi
Etehant
Oist. water or ethanol
(95%)
Hydroehlorie aeid
(1.19)
Iron (III) ehloride
.
Proeedure
Sees to mins .
100- 120 mi Possibly followed by
Cum4.
20-50 mi
5~10 mI
Remarks
AIl types of Cu.
Cu-Be alloys. Brasses
(colors beta brass).
Special bronzes.
Al bronze with euteetoid. German silver.
'~~
:~l
~;i
Preparation oi Iron, Steel, Cast Iron

Preparation of Cu
60
Cu
m2
Oist. water
Ammonium persulfate
(possibly)
Hydrochloric acid
( 1.19)
Ammonium persulfate
Cu
m3
Oist. water
Copper (11) ammonium chlotide
Add ammonia water;
precipita te dissolves
Cu
m4
Oist. water
Sodium or potassium
dichromate
Cu
tn5
Cu
m6
Cu
m7
Sat. aqueous sol. of

sodium thiosulfate
Potassium metabisulfite
(Klemm' s reagent)
Oist. water
Ethanol (96 %)
lren (II) nitrate

Possibly heated.
lOg Use fresh only!
10 mi Mixing of Cu mi and
Cu m2 in equal
amounts or 3:1, or
cycIic immersion
etching in Cu mI and
Cu m2.
20 g
120 mi 5-60 S.
If dissolution too se10 g vere, dilute with dist.
water.
80 mi 3-30 s.
5 mI Immediately before
use, add two drops of
lOg hydrochloric acid
(1.19)
6-8 min
50 mi
'~
Cu
m9
Verification of (100)
rolling texture in CU.
CU. Alpha-beta brass.
Special brass.
Al brass. Red-cast
bronze. German
silver.
Cu-Sn alloys.
Brasses. Alpha
bronze.
German silver. Cu-Be,
Cu-Cr, Cu-Ni, Cu-Mn,
Cu-Si alloys.
lg
3 min
30 (100) mi Secs to mins .

10 (8) mi
10 (25) mI
Oist. we:r
Cold, sat. aqueous
sol. of sodium thlosulfate
chromium (\11) oxide
45 mi 3- 5 min o
Cu Dist. water
mIl Ammonia water
Hydrogen peroxide
(3%)
25 mi Secs to mins.
Possibly addition of
5- 25 mi 1-5 mi solution of potassium hydroxide
(20%).
Little hydrogen peroxide

More hydrogen peroxide
Cu Oist. water
ml2 Nittic acid (1.40)
Cu Electrolytic:
ml3 Aqueous sol. of chromium (VI) oxide (1%)
Grain contrast.
50 mi Secs to mins.
50 mi
3-6 s, 6 V dc, Al
cathode.
90 mi 5-10 s, 1-8 V dc, Cu

10 mi cathode.
Cu Electro1ytic:
ml6 Oist. water
Phosphoric acid (1.71 )
Hydrofluoric acid
(40%)
Chromium (VI) oxide
480 mi 30 s, \.1 A/cm 2 , 5 V

cathode.
9g
Color etchant and

grain contrast of
bronzes,.
20 g
Grain boundaries .
Pure CU. Brasses.
Bronzes. German
silver.
Most types of Cu and

Cu alloys.
Cu-Ag solder layers .
Mn, P, Be, Al-Si
bronzes. Alpha
brasses.
Grain boundaries.
Alpha and beta brass.
Multiple constituent
Sn bronzes. Oeltaphase. Proportions in
parentheses for Cu-Ga
alloys.
Al bronzes which are

difficult to etch otherwise.
6.6 mi
Cu Electrolytic:
ml5 Oist. water
5 mi
5- 30 S .
111 See Appendix A.
100 mi Few mins.

Color and grain contrast etchat f or CU .
100 mi Attack-polishing with- Fast, good polish and

100 mi out adding abrasive on etch for Cu and Cu
with oxide and sulfide
10 g velvet.
incIusions.
Oist. water
Hydrochloric acid,
(1.19)
;
Nitric acid (1.40) '
Cu Oist. water
mlO Nitric acid(1.40)
Hydrofluoric acid
(40%)
Cu ElectrolyUc:
ml4 Oist. water
Sodium hydroxide '
Iron (11) sulfate
5g
~
Cu
m8
CU. Brasses. Bronzes .

Al bronzes. 'Cu-Ni and
Cu-Ag alloys.
German silver.
Grain contrast of
alpha brasses .
Cu welds,
AIso useful for
macroetching.
/ 61

Cu alloys. Flow lines
in brass.
Al bronzes. Cu-Be
alloys.
950 mi Up to 15 s, 8-10 V dc, Beta brass. German

50 mi Cu cathode.
silver. Monel and
'2g
tu-Ni alloys.
15 g
Bronzes.
AIl types of CU.
Cartridge brass.
Tombac. Muntz metal.
Easily machinable
brasses.
Brasses.
Iron, Steel, Cast Iron

The preparation of iron, steel, and ferrous alloys usually does not give rise
to particular difficulties . However, the pronounced multiplicity of properties
and microstructures in tbis category requires differing methods of preparation.
Unalloyed irons and low-carbon steels are easily deformable, and therefore
deform,ation layers frequently formo Steels, as well as cast irons (2-4.5% C)
vary from tough to brittle. Hardened steels should not be heated during preparation
since this might cause hanges in microstructure . In addition, in materials that
'\1\-,
Preparation oi Iron, Steel, Cast Iron

Preparation of Cu
60
Cu
m2
Oist. water
Ammonium persulfate
(possibly)
Hydrochloric acid
( 1.19)
Ammonium persulfate
Cu
m3
Oist. water
Copper (11) ammonium chlotide
Add ammonia water;
precipita te dissolves
Cu
m4
Oist. water
Sodium or potassium
dichromate
Cu
tn5
Cu
m6
Cu
m7

sodium thiosulfate
(Klemm' s reagent)
Oist. water
Ethanol (96 %)
lren (II) nitrate

Possibly heated.
lOg Use fresh only!
10 mi Mixing of Cu mi and
Cu m2 in equal
amounts or 3:1, or
cycIic immersion
etching in Cu mI and
Cu m2.
20 g
120 mi 5-60 S.
If dissolution too se10 g vere, dilute with dist.
water.
80 mi 3-30 s.
5 mI Immediately before
use, add two drops of
lOg hydrochloric acid
(1.19)
6-8 min
50 mi
'~
Cu
m9
Verification of (100)
rolling texture in CU.
CU. Alpha-beta brass.
Special brass.
Al brass. Red-cast
bronze. German
silver.
Cu-Sn alloys.
Brasses. Alpha
bronze.
German silver. Cu-Be,
Cu-Cr, Cu-Ni, Cu-Mn,
Cu-Si alloys.
lg
3 min
30 (100) mi Secs to mins .

10 (8) mi
10 (25) mI
Oist. we:r
Cold, sat. aqueous
sol. of sodium thlosulfate
chromium (\11) oxide
45 mi 3- 5 min o
Cu Dist. water
mIl Ammonia water
Hydrogen peroxide
(3%)
25 mi Secs to mins.
Possibly addition of
5- 25 mi 1-5 mi solution of potassium hydroxide
(20%).
Little hydrogen peroxide

More hydrogen peroxide
Cu Oist. water
ml2 Nittic acid (1.40)
Cu Electrolytic:
ml3 Aqueous sol. of chromium (VI) oxide (1%)
Grain contrast.
50 mi Secs to mins.
50 mi
3-6 s, 6 V dc, Al
cathode.
90 mi 5-10 s, 1-8 V dc, Cu

10 mi cathode.
Cu Electro1ytic:
ml6 Oist. water
Phosphoric acid (1.71 )
Hydrofluoric acid
(40%)
Chromium (VI) oxide
480 mi 30 s, \.1 A/cm 2 , 5 V

cathode.
9g
Color etchant and

grain contrast of
bronzes,.
20 g
Grain boundaries .
Pure CU. Brasses.
Bronzes. German
silver.

Cu alloys.
Cu-Ag solder layers .
Mn, P, Be, Al-Si
bronzes. Alpha
brasses.
Grain boundaries.
Alpha and beta brass.
Multiple constituent
Sn bronzes. Oeltaphase. Proportions in
parentheses for Cu-Ga
alloys.
Al bronzes which are

difficult to etch otherwise.
6.6 mi
Cu Electrolytic:
ml5 Oist. water
5 mi
5- 30 S .
111 See Appendix A.
100 mi Few mins.

Color and grain contrast etchat f or CU .
100 mi Attack-polishing with- Fast, good polish and

100 mi out adding abrasive on etch for Cu and Cu
with oxide and sulfide
10 g velvet.
incIusions.
Oist. water
Hydrochloric acid,
(1.19)
;
Nitric acid (1.40) '
Cu Oist. water
mlO Nitric acid(1.40)
Hydrofluoric acid
(40%)
Cu ElectrolyUc:
ml4 Oist. water
Sodium hydroxide '
Iron (11) sulfate
5g
~
Cu
m8
CU. Brasses. Bronzes .

Al bronzes. 'Cu-Ni and
Cu-Ag alloys.
German silver.
Grain contrast of
alpha brasses .
Cu welds,
AIso useful for
macroetching.
/ 61

Cu alloys. Flow lines
in brass.
Al bronzes. Cu-Be
alloys.
950 mi Up to 15 s, 8-10 V dc, Beta brass. German

50 mi Cu cathode.
silver. Monel and
'2g
tu-Ni alloys.
15 g
Bronzes.
AIl types of CU.
Cartridge brass.
Tombac. Muntz metal.
Easily machinable
brasses.
Brasses.
Iron, Steel, Cast Iron

The preparation of iron, steel, and ferrous alloys usually does not give rise
to particular difficulties . However, the pronounced multiplicity of properties
and microstructures in tbis category requires differing methods of preparation.
Unalloyed irons and low-carbon steels are easily deformable, and therefore
deform,ation layers frequently formo Steels, as well as cast irons (2-4.5% C)
vary from tough to brittle. Hardened steels should not be heated during preparation
since this might cause hanges in microstructure . In addition, in materials that
'\1\-,
62
Preparation of Iron, Steel, Cast Iron
Preparation of Iron, Steel, Cast lron
have undergone a forming process, the direction of deformation should be taken

into consideration. Fiber orientation, grain elongation, banded structure, and
nonmetallic inclusions are better judged in longitudinal sections.
Oist. water
Sulfuric acid (1. 84)
(Sulfur-printing test)
(Baumann print)
100 mi Silver bromide papee

5 mi is saturated with solution, and firmly
pressed against the
prepared surface .
After 1-5 min, rinse,
fix (6 g sodium thiosulfate in 100 mi
water), wash and dry.
Verification, arrangement, and distribution

of Fe and Mn sulfide
inc1usions. Sulfide
reacts with sulfuric
acid, forming hydrogen sulfide which
combines to darkish
silver suiCide with the
silver from the sil ver
bromide in the photogrl!-phic paper.
Fe
M6
Oist. water
Ethanol (96%)
Hydrochloric acid (1.19)
Iron (III) chloride
Tin (11) chloride
Add hydrochloric acid
last
(Oberhoffer's reagent)
500 mi
500 mi
42 mi
30 g
0.5 g
Steels and special

steels. Fe-enriched
areas appear dark.
Blowhole segregation.
Primary structure.
Fiber orientation.
Fe
M7
Oist. water
Copper (11) ammonium
chloride
(Heyn's reagent)
120 mi 2- 10 min .
Cu precipitates wiped
20 g with water.
Phosphorus segregation in low-carbon

steels.
Fiber orientation.
Welding zones . Grain
contrast. Primary
structure.
Fe
M8

sodium thiosulfate
(Klemm's reagent)
Secs to mins.
Phosphorus distribution in cast steel and

cast iron.
Macroetching
oc sectioning is often
400 grit is satisfactory.
wet grinding down to
grit is required. When
Etching:
No .
Fe
MI
Fe
M2
Fe
M3
Fe
M4
Conditions
Etchant
90 mi 1-5 min o
\O mi . Oeep etching.
Ethanol (96%)
Nitric acid (1.40)
50 mi 10-30 min, up to 80 oC Versatile etchant for

alloyed and unalloyed
(180F) .
steels. Oeep etchant
50 mi Remove film under
for surface 'control
running water. For
and segregation. Pocorrosion-resistant
rosity, hardness insteels, immerse in
dentations, fractures,
warm, 20% aqueous
inclusions, densol. of nitric acid
drites, flow lines,
(1.40) .
ferrite .
Oist. water
Hydrochloric acid
(1.l9)
Secs to mins .
Hydrochloric acid
(1.19)
copper (11) sulfate
(Marble's reagent)
50 mi
25 mi
100 mi
Ois!. water
Hydrochloric acid
1
(1.19)
1\ 120- 180 mi
45-90 g
Copper (11) chloride ,
(Fry's reagent)
'lt\
.
'.
--:\
.}1
Remarks
Versatile, useful for
Fe and steel.
Carburized, or decarburized zones.
Segregation. AIso usefui for ncroetching.
5-20 min.
Prior to etching, heat
at 150-200 oC
(300-400 F) for
5-30 min. After
etching, immerse in
conc. hydrochloric
acid, rinse in water,
and neutralize in
ammonia water.
Austenitic and hightemperature steels.

Fe-Cr-Ni cast alloys.
Oepth of nitriding .
Flow lines in low-carbon N 2 steels. Thomas
steel.
Compare microetchant
Fe mB.
63
Fe
M5
Preparation:
The surface quality resulting from machining, coarse grinding,
sufficient. Usually, wet grinding on silicon carbide papers down to
In special cases, for verification of segregation and flow lines,
600 grit or lapping with silicon carbide powders from 320 to 800
examining surface imperfections, etching is done directly.
Secs to mins.
Microsection must be
polished.
After etching, rinse in
a 4: I mixture of ethanol and hydrochloric
acid.
50 mi
I g
Microetchant Fe m22 is also used for macroetching.
Microetching
Preparation:
Compare suggestions for macroetching.
Grinding:
Wet on silicon carbide papers down to 600 grit. For hardened steels, avoid heating .
Polishing:
a. Alumina slurry on felt (billiard cloth or wool). Toward the end of the polishing cyc1e,
add a lot of water (possibly 0.1 % aqueous solution of ammonium tartrate) to wash
off adhering alumina partic1es .
b. Oiamond paste, particle size 6-1 J..l.m; 0.25 J..l.m only for extreme requirements in surface
quality (danger of overpolishing). Oiamond polishing is particularly suitable for heterogeneous materials with microstructural components of differing hardness such as cast
iron, malleable cast iron, steels containing carbides. Oiamond polishing helps avoid
relief formation. Graphite formation and nonmetallic inclusions can be studied in the
unetched state. Try to avoid pull-outs!
''}<J '.
62
Preparation of Iron, Steel, Cast lron
have undergone a forming process, the direction of deformation should be taken

into consideration. Fiber orientation, grain elongation, banded structure, and
nonmetallic inclusions are better judged in longitudinal sections.
Oist. water
(Sulfur-printing test)
(Baumann print)
100 mi Silver bromide papee

5 mi is saturated with solution, and firmly
pressed against the
prepared surface .
After 1-5 min, rinse,
fix (6 g sodium thiosulfate in 100 mi
water), wash and dry.
Verification, arrangement, and distribution

of Fe and Mn sulfide
inc1usions. Sulfide
reacts with sulfuric
acid, forming hydrogen sulfide which
combines to darkish
silver suiCide with the
silver from the sil ver
bromide in the photogrl!-phic paper.
Fe
M6
Oist. water
Ethanol (96%)
Hydrochloric acid (1.19)
Iron (III) chloride
Tin (11) chloride
Add hydrochloric acid
last
(Oberhoffer's reagent)
500 mi
500 mi
42 mi
30 g
0.5 g
Steels and special

steels. Fe-enriched
areas appear dark.
Blowhole segregation.
Primary structure.
Fiber orientation.
Fe
M7
Oist. water
Copper (11) ammonium
chloride
(Heyn's reagent)
120 mi 2- 10 min .
Cu precipitates wiped
20 g with water.
Phosphorus segregation in low-carbon

steels.
Fiber orientation.
Welding zones . Grain
contrast. Primary
structure.
Fe
M8

sodium thiosulfate
(Klemm's reagent)
Secs to mins.
Phosphorus distribution in cast steel and

cast iron.
Macroetching
oc sectioning is often
400 grit is satisfactory.
wet grinding down to
grit is required. When
Etching:
No .
Fe
MI
Fe
M2
Fe
M3
Fe
M4
Conditions
Etchant
90 mi 1-5 min o
\O mi . Oeep etching.
Ethanol (96%)
Nitric acid (1.40)
50 mi 10-30 min, up to 80 oC Versatile etchant for

alloyed and unalloyed
(180F) .
steels. Oeep etchant
50 mi Remove film under
for surface 'control
running water. For
and segregation. Pocorrosion-resistant
rosity, hardness insteels, immerse in
dentations, fractures,
warm, 20% aqueous
inclusions, densol. of nitric acid
drites, flow lines,
(1.40) .
ferrite .
Oist. water
Hydrochloric acid
(1.l9)
Secs to mins .
Hydrochloric acid
(1.19)
copper (11) sulfate
(Marble's reagent)
50 mi
25 mi
100 mi
Ois!. water
Hydrochloric acid
1
(1.19)
1\ 120- 180 mi
45-90 g
Copper (11) chloride ,
(Fry's reagent)
'lt\
.
'.
--:\
.}1
Remarks
Versatile, useful for
Fe and steel.
Carburized, or decarburized zones.
Segregation. AIso usefui for ncroetching.
5-20 min.
at 150-200 oC
(300-400 F) for
5-30 min. After
etching, immerse in
conc. hydrochloric
acid, rinse in water,
and neutralize in
ammonia water.
Austenitic and hightemperature steels.

Fe-Cr-Ni cast alloys.
Oepth of nitriding .
Flow lines in low-carbon N 2 steels. Thomas
steel.
Compare microetchant
Fe mB.
63
Fe
M5
Preparation:
The surface quality resulting from machining, coarse grinding,
sufficient. Usually, wet grinding on silicon carbide papers down to
In special cases, for verification of segregation and flow lines,
600 grit or lapping with silicon carbide powders from 320 to 800
examining surface imperfections, etching is done directly.
Secs to mins.
Microsection must be
polished.
After etching, rinse in
a 4: I mixture of ethanol and hydrochloric
acid.
50 mi
I g
Microetchant Fe m22 is also used for macroetching.
Microetching
Preparation:
Compare suggestions for macroetching.
Grinding:
Wet on silicon carbide papers down to 600 grit. For hardened steels, avoid heating .
Polishing:
a. Alumina slurry on felt (billiard cloth or wool). Toward the end of the polishing cyc1e,
add a lot of water (possibly 0.1 % aqueous solution of ammonium tartrate) to wash
off adhering alumina partic1es .
b. Oiamond paste, particle size 6-1 J..l.m; 0.25 J..l.m only for extreme requirements in surface
quality (danger of overpolishing). Oiamond polishing is particularly suitable for heterogeneous materials with microstructural components of differing hardness such as cast
iron, malleable cast iron, steels containing carbides. Oiamond polishing helps avoid
relief formation. Graphite formation and nonmetallic inclusions can be studied in the
unetched state. Try to avoid pull-outs!
''}<J '.
64
Preparaton of Iron, Steel, Cast Iron
c. Electrolytic:
l . Dist. water
2. Dist. water
Chromium (VI)
oxide
400 mI 2-6 min, 1.5- 6 V dc, Ni

600 mi cathode.
830 mi 2-10 min, 1.5- 9 V dc, Ni
cathode.
620 g n! See Appendix A.
Corrosion-resistant steels.
Pure iron.
Corrosion-resistartt steels.
High-alloy steels.
Fe
m7
Etching:
Pure iron: Fe ml , 3, 4, 9, 19, 20, 21
Structural steels and heat treated steels: Fe ml-9, 12, 13,
14, 16, 17, 19, 20, 21 , 24
High-temperature steels: Fe ml- l2, 17, 18, 22-25
Tool steels : Fe mi-lO, 14, 15, 18
Stainless steeIs : Fe m5, 6, 10, 11 , 12,21- 25
No.
Etchant
Conditions
Fe
m8
Remarks
Fe
mi
Ethanol or methanol
(95%)
Nitric acid (1.40)
(Nital)
See note at Fe m3.
Fe
m2
Ethanol or methanol
(95 %)
Hydrochloric acid
(1.19)
5-30 mino
Possible addition of
20 mi hydrogen peroxide
(30%).
Differentiation of
cubic and tetragonal
martensite. Ni-containing Cr steels.
High-temperature
steels.
Fe
m3
Ethanol (96 %)
Picric acid
(Picral)
Nital and Picral (Fe
mi and Fe m3) may
be mixed 1:1
lOO mi Secs to mins .

2-4 g n! See Appendix A.
Generally used for

iron and heat treated
steels.
Pearlite, martensite,
and bainite.
Lower contrast than
Fe mI.
Uniform etching, even
with segregations.
Fe J C stained light
yeIlow.
. Secs to mins.
Most common etchant
100 mi Caution: not to exceed for pure iron, low-car1-10 mi 10% solution.
bon steels, alloy
Explosive!
steels, and gray cast
iron. Segregations can
cause uneven attack.
.
;
Fe
m4
'}\
Fe
m5
Methapol or ettanol
(96%) ,
Nitric acid (1<40)
Picric acid " '.
Ethanol (96 o/a.) .

Hydroehlorie acid
(1.19)
Pierie aeid
Possibly a few drops
hydrogen peroxide
(3 %).or wetting agent
Secs to mins.
100 mi
0.2 mi
0.3 mi

To bring out grain
1-5 mi boundaries, heat for
1-4 g 10 min at 300-500 oC
(570- 930 F) before
etehing.
!n See Appendix A.
Fe Ethanol or methanol
m6 (95 %)
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Compare Fe mi and
m3 .
Improvement of contrast over Fe m3 .
Sometimes prevents
uneven attack of Fe
mI.
Inereases attaek of Fe
m2 in alloyed steels.
Grain-boundary preeipitates in Cr-Ni
steeIs beeome visible :
Fe
m9
Up to several mins .
85 mi n! See Appendix A.
1-10 mi
1-5 mi
/ 65
Grain boundaries in
heat treated tool
steels.
Alloyed Cr steels.
Ethanol (96%)
Nitric acid (1.40)
Hydrochloric acid
(1.19)
Picric acid
wetting agent
80 mi Secs to mins.
Dist. water
"
Sodium hydroxide
Picric acid
75 mi 3- 15 min, 50 oC
25 g (120 F).
2g n! See Appendix A.
Cementite (Fe J C) with

up to 10% Cr is
stained dark.
For more than 10%
Cr, no staining.
(Fe,Cr)7 C J ,
(Fe,Cr)23 C 6 , WC
and VC are not
stained.
100 mi 2-20 min, 20-50 oC

(70-120 0F).
IOg Use fresh only!
IOg !n See Appendix A.
Fe J C with more than

10% Cr is stained dark
more rapidly than
Fe J C with lessCr;
(Fe,Cr)7C J ,
(Fe,<;:r)23 C 6 , and
iron phosphide are
stained.
lOO mi Secs to mins, room

temperature to 50 oC
100 mi (120F).
10 mi
Mn-alloyed Cr-Ni
steels. Sigma phase
and ferrite .
Fine microstructures
in alloyed steels.
Dist. water
Potassium or sodium
hydroxide
' (Concentration variable)
(Murakami's reagent)
Fe Dist. water
mIO Hydrochloric acid
(1.19)
Nitric acid (1.40)
Vogel's special
reagent
(V2A etchant)
, Fe Glycerol
mil Nitric acid (1.40)
Hydrochloric acid
(1.19)
(Vilella's reagent)
Fe Glycerol
ml2 Nitrie aeid (1.40)
Hydrofluoric acid
(40%)
Grain boundaries in
martensitic microstructures.
10 mi
Ig
0.3 mi
Stainless steels with

high Cr content.
Cr-Ni cast steeIs.
30 mi
20-40 mi Secs to mins.

20 mi
SteeIs with high Si

content.
:~I
64
c. Electrolytic:
l . Dist. water
2. Dist. water
Chromium (VI)
oxide
400 mI 2-6 min, 1.5- 6 V dc, Ni

600 mi cathode.
830 mi 2-10 min, 1.5- 9 V dc, Ni
cathode.
620 g n! See Appendix A.
Corrosion-resistant steels.
Pure iron.
Corrosion-resistartt steels.
High-alloy steels.
Fe
m7
Etching:
Pure iron: Fe ml , 3, 4, 9, 19, 20, 21
Structural steels and heat treated steels: Fe ml-9, 12, 13,
14, 16, 17, 19, 20, 21 , 24
High-temperature steels: Fe ml- l2, 17, 18, 22-25
Tool steels : Fe mi-lO, 14, 15, 18
Stainless steeIs : Fe m5, 6, 10, 11 , 12,21- 25
No.
Etchant
Conditions
Fe
m8
Remarks
Fe
mi
Ethanol or methanol
(95%)
Nitric acid (1.40)
(Nital)
See note at Fe m3.
Fe
m2
Ethanol or methanol
(95 %)
Hydrochloric acid
(1.19)
5-30 mino
20 mi hydrogen peroxide
(30%).
Differentiation of
cubic and tetragonal
martensite. Ni-containing Cr steels.
High-temperature
steels.
Fe
m3
Ethanol (96 %)
Picric acid
(Picral)
Nital and Picral (Fe
mi and Fe m3) may
be mixed 1:1
lOO mi Secs to mins .

2-4 g n! See Appendix A.
Generally used for

iron and heat treated
steels.
Pearlite, martensite,
and bainite.
Lower contrast than
Fe mI.
Uniform etching, even
with segregations.
Fe J C stained light
yeIlow.
. Secs to mins.
Most common etchant
100 mi Caution: not to exceed for pure iron, low-car1-10 mi 10% solution.
bon steels, alloy
Explosive!
steels, and gray cast
iron. Segregations can
cause uneven attack.
.
;
Fe
m4
'}\
Fe
m5
Methapol or ettanol
(96%) ,
Nitric acid (1<40)
Picric acid " '.
Ethanol (96 o/a.) .

Hydroehlorie acid
(1.19)
Pierie aeid
Possibly a few drops
hydrogen peroxide
(3 %).or wetting agent
Secs to mins.
100 mi
0.2 mi
0.3 mi

To bring out grain
1-5 mi boundaries, heat for
1-4 g 10 min at 300-500 oC
(570- 930 F) before
etehing.
!n See Appendix A.
Fe Ethanol or methanol
m6 (95 %)
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Compare Fe mi and
m3 .
Improvement of contrast over Fe m3 .
Sometimes prevents
uneven attack of Fe
mI.
Inereases attaek of Fe
m2 in alloyed steels.
Grain-boundary preeipitates in Cr-Ni
steeIs beeome visible :
Fe
m9
Up to several mins .
1-10 mi
1-5 mi
/ 65
Grain boundaries in
heat treated tool
steels.
Alloyed Cr steels.
Ethanol (96%)
Nitric acid (1.40)
Hydrochloric acid
(1.19)
Picric acid
wetting agent
80 mi Secs to mins.
Dist. water
"
Sodium hydroxide
Picric acid
75 mi 3- 15 min, 50 oC
25 g (120 F).
2g n! See Appendix A.
Cementite (Fe J C) with

up to 10% Cr is
stained dark.
For more than 10%
Cr, no staining.
(Fe,Cr)7 C J ,
(Fe,Cr)23 C 6 , WC
and VC are not
stained.
100 mi 2-20 min, 20-50 oC

(70-120 0F).
IOg Use fresh only!
IOg !n See Appendix A.
Fe J C with more than

10% Cr is stained dark
more rapidly than
Fe J C with lessCr;
(Fe,Cr)7C J ,
(Fe,<;:r)23 C 6 , and
iron phosphide are
stained.
lOO mi Secs to mins, room

temperature to 50 oC
100 mi (120F).
10 mi
Mn-alloyed Cr-Ni
steels. Sigma phase
and ferrite .
Fine microstructures
in alloyed steels.
Dist. water
Potassium or sodium
hydroxide
' (Concentration variable)
(Murakami's reagent)
Fe Dist. water
mIO Hydrochloric acid
(1.19)
Nitric acid (1.40)
Vogel's special
reagent
(V2A etchant)
, Fe Glycerol
mil Nitric acid (1.40)
Hydrochloric acid
(1.19)
(Vilella's reagent)
Fe Glycerol
ml2 Nitrie aeid (1.40)
Hydrofluoric acid
(40%)
Grain boundaries in
martensitic microstructures.
10 mi
Ig
0.3 mi
Stainless steels with

high Cr content.
Cr-Ni cast steeIs.
30 mi
20-40 mi Secs to mins.

20 mi
SteeIs with high Si

content.
:~I
66
25 mI to 150-200 oC
(300-400F).
40 mI Compare macroetchant
5 g Fe M4.
Fe
Oist. water
ml3 Ethanol or menthanol
(95%)
Hydrochloric acid
(1.19)
Copyer (H) chloride
(Fry's reagent)
Fe SaL sol. of aqueous

. mI4 picric acid, possibly
diluted
Copper (11) chloride
Wetting agent
Same as Fe ml4 plus
mI5 HydrochIoric acid
(1.19)
Austenite grain
boundaries in tempered steels and
case-hardened
steels .
Secs to mins.
Austenite grain
boundaries in cold
work steels.
Iml
Fe Oist. water
ml6 Ethanol (96%)
Saturated picrie acid
(in alcohol)
Wetting agefit
lron (H) chloride
Zinc (II) chloride
25 mi Secs to mins.
7S mi
Fe
Ethanol (96%) .
m 17 Wetting agent
Ammonia water
Hydrochlorie acid (1.19)
Picric acid
Copper (11) ammonium chloride
50 mi Secs to mins.
10 mi
Iml
Iml
3g
Fe
48 mi Secs to mins.
10ml
6g
l
Oist. water
I
ml9 Potassium hydroxide~ '
Potassium ferricyanidi
Fe Dist. water
m20 'S odium thiosulfate . \,
Citric acid
Cadmium chloride ..,
(Beraha' s reagent)
'.
JI
Fe
Oist. water
m21 Potassium metabisulfite
Fe Dist. water
m22 Ammonium persulfate
Used also'\as a
macroetchant.
Austenite grain
boundaries in casehardened steels.
Austenite grain
boundaries in valve
steels, tempered
steels, case-hardened
steels .
Electrolytic:
m23 Oist. water
Lead acetate
1g
Austenite grain
boundaries in cold
work steels.
Ig
60 mi 20-40 s, 50 oC
30 g (120 F).
30 g Use fresh only!
!!! See Appendix A.
lOO mi
24 g
3g
2-2.5 g
20-40 S.
Oissolve chemicals in
given sequence. Each
constituent must be
completeIy dissolved
before the next one is
added. Store in dark
bottle, max 20 oC
(70 F). Filter solution
before use. Remains
useful for 4 h.
Sigma phase is
stained,
Austenite remains unchanged. Ferrite turns
yellow-brown.
Tint etchant for pure
iron and carbon steeIs,
cast iron, and alloyed
steels. Oifferentiation
of ferrte (brown to violet), carbides, phosphides, and nitrides
(light) .
lOO mi 5-20 S .
IOg Use fresh only!
Electrolylic:
Secs to mins, 6 V de,
Ni cathode .
Fe
Fe
Electrolytic:
m24 Ammonium hydroxide
conc.
Fe
Electrolylic:
m25 Dist. water
Chromium (VI) oxide
67
Pure iron, carbon

Possible pre-etching in steels, low-alloy
steels .
IOg Fe mI
Tinting of ferrite, martensite, bainite, and
sorbite.
Eteh pits, subgrain
boundaries, twins.
Carbides, nitrides,
phosphides, and sulfides are not attacked .
Approx 2 min
20 mi
14ml
IOg
3g
Ethanol (96%)
m 18 Wetting agent
Picric acid
Copper (II) ammonium chloride
In normalized, lowcarbon steels eontaining nitrogen, deformed

areas can be distinguished next to undeformed areas.
Flow lines in forgings .
30--60 s, 75-85 oC
(160-185 F) .
lOO mi Wipe black film on
80 mg specimen with
60 mi aqueous sol. of ammonium hydroxide on
cotton
Fe
Fe
"
,:t'
'~
-~
Grain contrast of ferrite in low-carbon

steels. Transformer
sheet metals, austenitie Ni-steels.
Carbides and phosphides in low-alloy
steels.
Only matrix is attacked.
High-alloy Cr-Ni
steels. (Transformation and precipitation
microstructure~ , carbides).
Hardened steeIs with
martensite.
100 mi Secs, 2 V dc, stainless Fe-Cr-Ni cast alloy.

Sigma phase (blue10 g steel cathode.
red), ferrite (dar k
blue), austenite (light
blue), and carbide
"' (yellow) in stainless
and high-alloy heat-resistant steels.
30-60 s , 1.5-6 V dc,
Pt cathode.
High-alloy steels.
Etches carbides only .
Leaves sigma phase
unchanged.
100 mI 3-{0 s, 3-6 V de, Pt

IOg cathode .
!!! See Appendix A.
Cr and Cr-Ni steels.

Cernen tite is attacked
rapidly, austenite less
rapidly, ferrite and
phosphide are attacked least. Carbide
etchant.
Corrosion-resistant
malleable steel.
Cast iron.
Immersion etching
~'it\
66
25 mI to 150-200 oC
(300-400F).
40 mI Compare macroetchant
5 g Fe M4.
Fe
Oist. water
ml3 Ethanol or menthanol
(95%)
Hydrochloric acid
(1.19)
Copyer (H) chloride
(Fry's reagent)
Fe SaL sol. of aqueous

. mI4 picric acid, possibly
diluted
Wetting agent
Same as Fe ml4 plus
mI5 HydrochIoric acid
(1.19)
Austenite grain
boundaries in tempered steels and
case-hardened
steels .
Secs to mins.
Austenite grain
boundaries in cold
work steels.
Iml
Fe Oist. water
ml6 Ethanol (96%)
Saturated picrie acid
(in alcohol)
Wetting agefit
lron (H) chloride
Zinc (II) chloride
25 mi Secs to mins.
7S mi
Fe
Ethanol (96%) .
m 17 Wetting agent
Ammonia water
Hydrochlorie acid (1.19)
Picric acid
50 mi Secs to mins.
10 mi
Iml
Iml
3g
Fe
48 mi Secs to mins.
10ml
6g
l
Oist. water
I
ml9 Potassium hydroxide~ '
Potassium ferricyanidi
Fe Dist. water
m20 'S odium thiosulfate . \,
Citric acid
Cadmium chloride ..,
(Beraha' s reagent)
'.
JI
Fe
Oist. water
m21 Potassium metabisulfite
Fe Dist. water
m22 Ammonium persulfate
Used also'\as a
macroetchant.
Austenite grain
boundaries in casehardened steels.
Austenite grain
boundaries in valve
steels, tempered
steels, case-hardened
steels .
Electrolytic:
m23 Oist. water
Lead acetate
1g
Austenite grain
boundaries in cold
work steels.
Ig
60 mi 20-40 s, 50 oC
30 g (120 F).
30 g Use fresh only!
!!! See Appendix A.
lOO mi
24 g
3g
2-2.5 g
20-40 S.
Oissolve chemicals in
given sequence. Each
constituent must be
completeIy dissolved
before the next one is
added. Store in dark
bottle, max 20 oC
(70 F). Filter solution
before use. Remains
useful for 4 h.
Sigma phase is
stained,
Austenite remains unchanged. Ferrite turns
yellow-brown.
Tint etchant for pure
iron and carbon steeIs,
cast iron, and alloyed
steels. Oifferentiation
of ferrte (brown to violet), carbides, phosphides, and nitrides
(light) .
lOO mi 5-20 S .
IOg Use fresh only!
Electrolylic:
Secs to mins, 6 V de,
Ni cathode .
Fe
Fe
Electrolytic:
m24 Ammonium hydroxide
conc.
Fe
Electrolylic:
m25 Dist. water
Chromium (VI) oxide
67
Pure iron, carbon

Possible pre-etching in steels, low-alloy
steels .
IOg Fe mI
Tinting of ferrite, martensite, bainite, and
sorbite.
Eteh pits, subgrain
boundaries, twins.
Carbides, nitrides,
phosphides, and sulfides are not attacked .
Approx 2 min
20 mi
14ml
IOg
3g
Ethanol (96%)
m 18 Wetting agent
Picric acid
Copper (II) ammonium chloride
In normalized, lowcarbon steels eontaining nitrogen, deformed

areas can be distinguished next to undeformed areas.
Flow lines in forgings .
30--60 s, 75-85 oC
(160-185 F) .
lOO mi Wipe black film on
80 mg specimen with
60 mi aqueous sol. of ammonium hydroxide on
cotton
Fe
Fe
"
,:t'
'~
-~
Grain contrast of ferrite in low-carbon

steels. Transformer
sheet metals, austenitie Ni-steels.
Carbides and phosphides in low-alloy
steels.
Only matrix is attacked.
High-alloy Cr-Ni
steels. (Transformation and precipitation
microstructure~ , carbides).
Hardened steeIs with
martensite.
100 mi Secs, 2 V dc, stainless Fe-Cr-Ni cast alloy.

Sigma phase (blue10 g steel cathode.
red), ferrite (dar k
blue), austenite (light
blue), and carbide
"' (yellow) in stainless
and high-alloy heat-resistant steels.
30-60 s , 1.5-6 V dc,
Pt cathode.
High-alloy steels.
Etches carbides only .
Leaves sigma phase
unchanged.
100 mI 3-{0 s, 3-6 V de, Pt

IOg cathode .
!!! See Appendix A.
Cr and Cr-Ni steels.

Cernen tite is attacked
rapidly, austenite less
rapidly, ferrite and
phosphide are attacked least. Carbide
etchant.
Corrosion-resistant
malleable steel.
Cast iron.
Immersion etching
~'it\
f
68
Preparation of Ge, Se, Si, Te
Fe
Electro/y tic:
m26 Dist. water
Sodium hydroxide
lOO mi 5-60 s, 1-3 V de, Pt

40 g eathode.
Potentiostafie:
at +450 mV
at -700 mV
Ge
Se
Si
Te
Verifieaton of sigma
phase. First, stains
yellow to dark brown.
Then, staining of ferrite eommenees.
Continued etehing develops earbides.
More uniform, better
quality etehing.
Staining of eementite.
Germanium, Selenium, Silicon, Tellurium,

Am By and AIJ BYI Alloys
Microetching
Lapping 'with silieon eilrbide, 'bofon carbide", 'or aluminum oxide slurries in water (grit
size 320-800).
'
Polishing:
Etchiong:
No.
.~~
Picric acid
Elehant
.,
5 mi
1g
Ge-In alloys with Ag,

Au, Bi, Cu additions.
Grain boundaries.
Hydrofluorie acid
(40%)
Nitrie acid (1.40)
Sees lo mins .
10 mi
Si, Ge, and their

alloys. InSb.
Eteh pits on (111)
planes, p-n junetions.
Ge
m4
Dist. water
Hydrofluorie acid
(40%)
Hydrogen peroxide
(30%)
40 mI 1-3 min o
J!! See Appendix A.
10 mi
Se, Ge, and their

alloys.
InAs, InSb, GaSb,
GaAs, AISb, ZnTe,
CdTe,InP.
Ge
m5
Nitrie acid (1.40)

I:!ydrofluoric acid
(4b%)
Glacial aeetie aeid

Bromine
(CP4 soIution)
Without bromine
Ge
m6
Nitrie aeid (1.40)

PossibIy diIuted with
dist. water, and/or
mixed with hydrohlorie aeid (1.9)
Ge
m7
Dist. water
Hydroehlorie acid
10 mi
50 mi 3-25 S.
Mix 30 min before
30 mi use.
0.6 mi
Si, Ge, and their

alloys.
GaSb. InSb. DisIoeations on (100) and
(111) planes of Si.
Sees to mins.
Ge, Te, Se. Tellurides.

Selenides and Zr silicide.
InAs.
Iron (IlI) chloride
50 mI Sees to mins .
Boiling.
50 mi
20 g
Ge and its alloys.

Grain eontrast.
Also suitable as a
maeroetehant.
Ge
m8
Dist. water
Hydrofluorie acid
(40%)
Nitric acid (1.40)
Silver nitrate
40 mI 30 s to 2 min
!!! See Appendix A.
40 mi
20 mi
2g
Ge and its alloys.

GaAs, InAs, AlAs.
Grain boundaries.
Dislocations on (111)
planes.
Ge
m9
Dist. water
Sodium hydroxide
Ge Eleetrolytie:
mIO Dist. water
Oxalie acid

50-100 g
100 mI 10-20 s, 4-6 V de,
lO g stainless steel
eathode.
Si, Te, Se.
Ge and its alloys.

Grain boundaries.
"h
. \.
Dist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
lOO mi Sees to mins.
69
Ge
m3
(1.19)
a. USe diamond paste or alumina slurries down to finest particle size. Eteh,polishing
sequenee with soIutions used for ehemicaI polishing (c. 1) or (c. 2).
b. ElectroIytie:
590 mI
30-60 s,
MethanoI (95%)
Butyl gIyeol
350 mI
25-35 V de,
60 mi
!!! See Appendix A.
e. Chemieal:
Ge.
5-10 s.
1. Hydrofluorie aeid (4<1%)
15 mi
Nitrie aeid (1.40) , 1
!!! See Appendix A.
25 mi
15 mi
Glacial aeetie acid 't
3-4 drops
Bromine
Si.
5-10 s
2. Nitrie aeid (~.40)
20 mI
!!! See Appendix A.
5 mI
Hydrofluoric aeid (40%)
Ge
mi
Ethanol (96%)
Hydrochlorie acid
(1.19)
Selenium and its compounds are toxico (!!! See Appendix A and references
Preparation:
Grinding:
Ge
m2
Conditions
5 (90) mi 5-20 s.
25 (5) mI
Remarks
Si, Ge, and their
alloys. InSb.
ProportioIis in parenIheses especially for
Si.
AIso used for chemical poIishing al approx
50 oC (120F)
f
68
Fe
Electro/y tic:
m26 Dist. water
Sodium hydroxide
lOO mi 5-60 s, 1-3 V de, Pt

40 g eathode.
Potentiostafie:
at +450 mV
at -700 mV
Ge
Se
Si
Te
Verifieaton of sigma
phase. First, stains
yellow to dark brown.
Then, staining of ferrite eommenees.
Continued etehing develops earbides.
More uniform, better
quality etehing.
Staining of eementite.
Germanium, Selenium, Silicon, Tellurium,

Am By and AIJ BYI Alloys
Microetching
Lapping 'with silieon eilrbide, 'bofon carbide", 'or aluminum oxide slurries in water (grit
size 320-800).
'
Polishing:
Etchiong:
No.
.~~
Picric acid
Elehant
.,
5 mi
1g
Ge-In alloys with Ag,

Au, Bi, Cu additions.
Grain boundaries.
Hydrofluorie acid
(40%)
Nitrie acid (1.40)
Sees lo mins .
10 mi
Si, Ge, and their

alloys. InSb.
Eteh pits on (111)
planes, p-n junetions.
Ge
m4
Dist. water
Hydrofluorie acid
(40%)
Hydrogen peroxide
(30%)
40 mI 1-3 min o
J!! See Appendix A.
10 mi
Se, Ge, and their

alloys.
InAs, InSb, GaSb,
GaAs, AISb, ZnTe,
CdTe,InP.
Ge
m5
Nitrie acid (1.40)

I:!ydrofluoric acid
(4b%)
Glacial aeetie aeid

Bromine
(CP4 soIution)
Without bromine
Ge
m6
Nitrie aeid (1.40)

PossibIy diIuted with
dist. water, and/or
mixed with hydrohlorie aeid (1.9)
Ge
m7
Dist. water
Hydroehlorie acid
10 mi
50 mi 3-25 S.
Mix 30 min before
30 mi use.
0.6 mi
Si, Ge, and their

alloys.
GaSb. InSb. DisIoeations on (100) and
(111) planes of Si.
Sees to mins.
Ge, Te, Se. Tellurides.

Selenides and Zr silicide.
InAs.
Iron (IlI) chloride
50 mI Sees to mins .
Boiling.
50 mi
20 g
Ge and its alloys.

Grain eontrast.
Also suitable as a
maeroetehant.
Ge
m8
Dist. water
Hydrofluorie acid
(40%)
Nitric acid (1.40)
Silver nitrate
40 mI 30 s to 2 min
!!! See Appendix A.
40 mi
20 mi
2g
Ge and its alloys.

GaAs, InAs, AlAs.
Grain boundaries.
Dislocations on (111)
planes.
Ge
m9
Dist. water
Sodium hydroxide
Ge Eleetrolytie:
mIO Dist. water
Oxalie acid

50-100 g
100 mI 10-20 s, 4-6 V de,
lO g stainless steel
eathode.
Si, Te, Se.
Ge and its alloys.

Grain boundaries.
"h
. \.
Dist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
69
Ge
m3
(1.19)
a. USe diamond paste or alumina slurries down to finest particle size. Eteh,polishing
sequenee with soIutions used for ehemicaI polishing (c. 1) or (c. 2).
b. ElectroIytie:
590 mI
30-60 s,
MethanoI (95%)
Butyl gIyeol
350 mI
25-35 V de,
60 mi
!!! See Appendix A.
e. Chemieal:
Ge.
5-10 s.
1. Hydrofluorie aeid (4<1%)
15 mi
Nitrie aeid (1.40) , 1
!!! See Appendix A.
25 mi
15 mi
Glacial aeetie acid 't
3-4 drops
Bromine
Si.
5-10 s
2. Nitrie aeid (~.40)
20 mI
!!! See Appendix A.
5 mI
Hydrofluoric aeid (40%)
Ge
mi
Ethanol (96%)
Hydrochlorie acid
(1.19)
Selenium and its compounds are toxico (!!! See Appendix A and references
Preparation:
Grinding:
Ge
m2
Conditions
5 (90) mi 5-20 s.
25 (5) mI
Remarks
Si, Ge, and their
alloys. InSb.
ProportioIis in parenIheses especially for
Si.
AIso used for chemical poIishing al approx
50 oC (120F)
70
Preparation of Hf, Ir
. Hafnium and Zirconium

[iill
Pure hafnium and zirconium are soft, and metallographic preparation often
~ results
in deformation layers. Their alloys usually do not pose any particular
difficulties.
c. Chemical:
l. Oist. water or hydrogen peroxide (30%)
Hydrofluoric acid (40%)
Nitric acid (1.40)
Wet grinding on silicon carbide papers down to 600 grit. Possible coating of grinding
paper with wax.
Conditions
Etchant
Remarks
Hf
MI
Oist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
70 ml Secs to mins.
30 mi Swab.
!H See Appendix A.
5 mi
Zircaloy-2 and Hf.
Hf
M2
Ois!. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
45 mI Sees to mins.
45 mi Swab.
H! See Appendix A.
10 mi
Zr and Hf and their

alloys with high additional alloying constituents.
With smaller amounts
of additional alloying .
constituents, use ethanol(96%) instead of
water.
Secs to mins.
45 mi Swab.
45 ml !!! See Appendix A.
Hydrogen peroxide
(30%)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Zr and Hf and their

alloys with small additional constituents
Preparation:
Grinding:
-:\
JI
l'
a. With diamond paste arldlumina slurry down to finest particle size. Possible etch-polish
sequence with one of the microetchants.
b. Electrolytic:
..:
"
90 mi 30 s to 8 min, 12-18 V de,
l. Glacial aeetic acid .
Perchlorie acid (70%") ."
10 mi
!!! See Appendix A.
870 mI 1-10 min, 9-12 V de, stain2. Glycerol
43 mi less steel cathode.
Hydrofluorie acid (40%)
Nitric acid (1.40)
Do not store!
H! See Appendix A.
Remarks
15 ml 3-10 s, swab.
2-min immersion etch.
30 ml n! See Appendix A.
30 mi
Zr and Hf-base alloys

Zr-Nb alloys.
Hf
Oist. water
Nitric acid (1.40)
lfydrofluoric acid
(40%)
45 mi 5- 20 s.
45 mi H! See Appendix A.
Pure and low-alloy Hf

and Zr for observations in polarized
Iight. Zr-U, Zr-AI,
Hf-Re alloys.
m2
Hf
m3
Oist. water
Hydrofluoric acid
(40%)
Aqueous sol. of silver
nitrate (5%)
with disto water
10 mi
200 mi 5-60 s.
n! See Appendix A.
5ml
2ml
100 mI 10-60 s.
(pprox)
Hf-base alloys.
l;r-base alloys.
Hf
m4
Oist. water
Hydrofluoric acid
100 mI 1-5 s.
5-10 mi !H See Appendix A.
Hf
mS
Nitric acid
Hydrofluoric acid
(40%)
(Concentration
variable)
90 mI Secs to mins.
!!! See Appendix A.
10 mI
With equal parts of
the constituents
Zr-Th, Zr-Sn, Zr-Nb,

Zr-Cu, Zr-Si, Zr-Ni
alloys.
Zr alloys with Al, Be,
Fe, Ni, Si .
HI
n6
Glycerol
Nitric acid (1.40)
Hydrofluoric acid
(40%)
(Concentration
variable)

10 (45) ml 00 not stoTe!
H! See Appendix A.
5 (10) mI
Zr-Mg, Zr-Mo, Zr-Sn,

Zr-U, Zr-B, Zr-Fe,
Zr-Ni alloys.
Proportions in parentheses for alloys with
lowadditions.
'If
n7
Electrolytic:
Glycerol
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Same as under macroetcruhg. AIso, prepare by rnicrotome using eutters of cemented

earbide; diamond e~tters tep.d to roughen the surface.
Conditions
Nitrie acid (1.40)

Hydrofluoric acid
(40%)
Nitric acid (1.19)
lO mi
Microetching
Etchant
Hf
mi
Etching:
Polishing:
5-10 s repeatedly .
!!! See Appendix A.
Hafnium and zirconium are suitable for investigations under polarized light.
No.
Preparation:
Hf
M3
71
Etching:
Macroetching
No.
45 mi
10 mi
45 mi
100 mIl-lO min, 9-12 V de,

10 mi Pt cathode.
00 not store!
S mi !n See Appendix A.
Zr, Zr-Be, Zr-H, and

Zr-Nb alloys.
Zircaloy.
Zr and its alloys.
Mercury Alloys (Amalgamates)

Amalgamates are heat sensitve. They have a tendency to smear. Use only
lery light pressure, with external cooling of specimen. Microscopy should
mmediately follow preparation. Amalgamates are toxie (!!! See Appendix A.)
~h
IHg I
70
. Hafnium and Zirconium

[iill
Pure hafnium and zirconium are soft, and metallographic preparation often
~ results
in deformation layers. Their alloys usually do not pose any particular
difficulties.
c. Chemical:
l. Oist. water or hydrogen peroxide (30%)
Hydrofluoric acid (40%)
Nitric acid (1.40)
Wet grinding on silicon carbide papers down to 600 grit. Possible coating of grinding
paper with wax.
Conditions
Etchant
Remarks
Hf
MI
Oist. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
70 ml Secs to mins.
30 mi Swab.
!H See Appendix A.
5 mi
Zircaloy-2 and Hf.
Hf
M2
Ois!. water
Nitric acid (1.40)
Hydrofluoric acid
(40%)
45 mI Sees to mins.
45 mi Swab.
H! See Appendix A.
10 mi
Zr and Hf and their

alloys with high additional alloying constituents.
With smaller amounts
of additional alloying .
constituents, use ethanol(96%) instead of
water.
Secs to mins.
45 mi Swab.
45 ml !!! See Appendix A.
Hydrogen peroxide
(30%)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Zr and Hf and their

alloys with small additional constituents
Preparation:
Grinding:
-:\
JI
l'
a. With diamond paste arldlumina slurry down to finest particle size. Possible etch-polish
sequence with one of the microetchants.
b. Electrolytic:
..:
"
90 mi 30 s to 8 min, 12-18 V de,
l. Glacial aeetic acid .
Perchlorie acid (70%") ."
10 mi
!!! See Appendix A.
870 mI 1-10 min, 9-12 V de, stain2. Glycerol
43 mi less steel cathode.
Hydrofluorie acid (40%)
Nitric acid (1.40)
Do not store!
H! See Appendix A.
Remarks
15 ml 3-10 s, swab.
2-min immersion etch.
30 ml n! See Appendix A.
30 mi
Zr and Hf-base alloys

Zr-Nb alloys.
Hf
Oist. water
Nitric acid (1.40)
lfydrofluoric acid
(40%)
45 mi 5- 20 s.
45 mi H! See Appendix A.
Pure and low-alloy Hf

and Zr for observations in polarized
Iight. Zr-U, Zr-AI,
Hf-Re alloys.
m2
Hf
m3
Oist. water
Hydrofluoric acid
(40%)
Aqueous sol. of silver
nitrate (5%)
with disto water
10 mi
200 mi 5-60 s.
n! See Appendix A.
5ml
2ml
100 mI 10-60 s.
(pprox)
Hf-base alloys.
l;r-base alloys.
Hf
m4
Oist. water
Hydrofluoric acid
100 mI 1-5 s.
5-10 mi !H See Appendix A.
Hf
mS
Nitric acid
Hydrofluoric acid
(40%)
(Concentration
variable)
90 mI Secs to mins.
!!! See Appendix A.
10 mI
With equal parts of
the constituents
Zr-Th, Zr-Sn, Zr-Nb,

Zr-Cu, Zr-Si, Zr-Ni
alloys.
Zr alloys with Al, Be,
Fe, Ni, Si .
HI
n6
Glycerol
Nitric acid (1.40)
Hydrofluoric acid
(40%)
(Concentration
variable)

10 (45) ml 00 not stoTe!
H! See Appendix A.
5 (10) mI
Zr-Mg, Zr-Mo, Zr-Sn,

Zr-U, Zr-B, Zr-Fe,
Zr-Ni alloys.
Proportions in parentheses for alloys with
lowadditions.
'If
n7
Electrolytic:
Glycerol
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Same as under macroetcruhg. AIso, prepare by rnicrotome using eutters of cemented

earbide; diamond e~tters tep.d to roughen the surface.
Conditions
Nitrie acid (1.40)

Hydrofluoric acid
(40%)
Nitric acid (1.19)
lO mi
Microetching
Etchant
Hf
mi
Etching:
Polishing:
5-10 s repeatedly .
!!! See Appendix A.
Hafnium and zirconium are suitable for investigations under polarized light.
No.
Preparation:
Hf
M3
71
Etching:
Macroetching
No.
45 mi
10 mi
45 mi
100 mIl-lO min, 9-12 V de,

10 mi Pt cathode.
00 not store!
S mi !n See Appendix A.
Zr, Zr-Be, Zr-H, and

Zr-Nb alloys.
Zircaloy.
Zr and its alloys.
Mercury Alloys (Amalgamates)

Amalgamates are heat sensitve. They have a tendency to smear. Use only
lery light pressure, with external cooling of specimen. Microscopy should
mmediately follow preparation. Amalgamates are toxie (!!! See Appendix A.)
~h
IHg I
72
Preparation of Mg
Preparation of Hg Alloys (Amalgamates)
Preparation:
Grinding:
No.
Etchant
Mg
MI
Dist. water
Sol. of picric acid
(64%) in ethanol (96%)
Glacial acetic acid
Possibly higher water
content
Mg
M2
Dist. water
Acetic aeid
100 mI 30 s to 3 min
10 mI Swab
Internal defeets in
cast ingots.
Segregations.
Flow lines in forged
parts.
Mg
M3
Dist. water
Nitric acid (1.40)
20 ml
Internal defects in
cast ingots. Segregations. Flow lines in
forged parts.
Mg-Mn and Mg-Zr
alloys
Wet on .already used silicon carbide paper (possibly coated with wax). Grit size 320-600;
subsequently, 600-grit soft, already used.
.
Polishing:
Diamond paste (particle size 3-0.25 !Lm, approx 5- 15 min). Subsequently, alumina slurry
No. 3 (0.05 ,..m, Linde B)-or, even better, magnesia slurry on velvet or soft leather.
Use light pressure, fast mov~ment. Rinse in distilled water. Dry by pressing against blotting
papero Cool-air stream (hair drier) can also be used. Possible etch-polishing sequence.
Grinding and polishing can be replaced by preparation with microtome.
Etching:
Hg
mI
Condition
Etchant
a. Dist. water or ethanol (96%)

Hydrochloric acid
(1.19)
b. Dist. water
Aqueous sol. of iron
(I1I) chloride (5%)
Hydrochloric acid
1.19)
Hg
m2
Glacial acetic acid
Hg
m3
Amrnonia water
Hydrogen peroxide
(30%)
(possibly dist. water)
1-3 min.
90 mI
10 mI
90 mI Dip briefly.
10 mI
Iml
Approx 15 min
100 mI Secs to mins
Remarks
. Usually, (a) is sufficient.

Double etching in (a)
and (b) results in
greater contrast.
Hg-Sn and Hg-Sn-Cu
alloys.
Ag-Sn-Hg alloys.
25 mI
(100 mi)
""
Magnesium
~
Deforfuation' layers frequently form on rnagnesium. AIso, there is a tendency
toward mechanical twinning at relatively low deformation. Abrasives and polishing
compounds are \embedded into the surface. Sorne phases containing magnesium
are attacked by water. Therefore, extended treatment involving water should
be avoided. ~agnesium dust and shavings are pyrophoric (!!! See Appendix
A).
.,
~..
Conditions
20 mI 30s to 3 min
Precipitate is washed
50 mI off in hot water.
For most amalgamates.
Etching sqlutions for the respective alloying metals of mercury are suitable in diluted
form for amalgamates.
IMgl
73
Etching:
Microetching
No.
Remarks
Grain size and flow
lines in cast and
forged parts .
Microetching
Preparation:
Grinding:
a. Observe instruetions for macroetching.
b. Wet with distilled water on silicon earbide papers down to grit size 600 (for specimens
which are insensitive to water).
C. Prepare by microtome using eemented carbide blade or, even better,diamond blade;
Polishing:
a. With alumina slurry on Mierocloth, or with diamond (particle size 6-1 !Lm). Subsequently,
on soft c10th with a suspension of 120 mI hot distilled water, 20 mI of aqueous solution
of ammonium tartrate (5 %), and I g MgO. Suspension should be filtered before use
. (through a fme eotton or nylon c1oth).
b. Electrolytic:
250 mi 2 min, 25-50 oC (75-120 F), \O
Dist. water
Ethanol (96%)
300 mI V de, Mg or Al cathode.
c. Chemieal
Nitric acid (1.40)
Imerse for 3-s periods. Polish- Pure Mg.
ing effect after about I mino
Then etching eommences.
Etching:
Magnesium is suitable for observations in polarized Iight.
..~
Macroetching
Preparation:
Coarse grinding on siliconcarbide paper is.usually sufficient. If water-sensitive components
are prl=sent, grinding has to be carried out dry, or by using alcohol or kerosine as a
lubricant with proper ventilation precautions.
No.
Etchant
Mg Ethanol, methanol
mi (95%), or dist. water
Nitric acid (1.40)
Conditions
Sees to mins.
100 mI
1-8 mI
Remarks
Pure Mg and most Mg
alIoys, also in cast and
forged state.
72
Preparation of Mg
Preparation of Hg Alloys (Amalgamates)
Preparation:
Grinding:
No.
Etchant
Mg
MI
Dist. water
Sol. of picric acid
(64%) in ethanol (96%)
Glacial acetic acid
Possibly higher water
content
Mg
M2
Dist. water
Acetic aeid
10 mI Swab
Internal defeets in
cast ingots.
Segregations.
Flow lines in forged
parts.
Mg
M3
Dist. water
Nitric acid (1.40)
20 ml
Internal defects in
cast ingots. Segregations. Flow lines in
forged parts.
Mg-Mn and Mg-Zr
alloys
Wet on .already used silicon carbide paper (possibly coated with wax). Grit size 320-600;
subsequently, 600-grit soft, already used.
.
Polishing:
Diamond paste (particle size 3-0.25 !Lm, approx 5- 15 min). Subsequently, alumina slurry
No. 3 (0.05 ,..m, Linde B)-or, even better, magnesia slurry on velvet or soft leather.
Use light pressure, fast mov~ment. Rinse in distilled water. Dry by pressing against blotting
papero Cool-air stream (hair drier) can also be used. Possible etch-polishing sequence.
Grinding and polishing can be replaced by preparation with microtome.
Etching:
Hg
mI
Condition
Etchant
a. Dist. water or ethanol (96%)

Hydrochloric acid
(1.19)
b. Dist. water
(I1I) chloride (5%)
Hydrochloric acid
1.19)
Hg
m2
Glacial acetic acid
Hg
m3
Amrnonia water
Hydrogen peroxide
(30%)
(possibly dist. water)
1-3 min.
90 mI
10 mI
90 mI Dip briefly.
10 mI
Iml
Approx 15 min
100 mI Secs to mins
Remarks
. Usually, (a) is sufficient.

Double etching in (a)
and (b) results in
greater contrast.
Hg-Sn and Hg-Sn-Cu
alloys.
Ag-Sn-Hg alloys.
25 mI
(100 mi)
""
Magnesium
~
Deforfuation' layers frequently form on rnagnesium. AIso, there is a tendency
toward mechanical twinning at relatively low deformation. Abrasives and polishing
compounds are \embedded into the surface. Sorne phases containing magnesium
are attacked by water. Therefore, extended treatment involving water should
be avoided. ~agnesium dust and shavings are pyrophoric (!!! See Appendix
A).
.,
~..
Conditions
20 mI 30s to 3 min
Precipitate is washed
50 mI off in hot water.
For most amalgamates.
Etching sqlutions for the respective alloying metals of mercury are suitable in diluted
form for amalgamates.
IMgl
73
Etching:
Microetching
No.
Remarks
Grain size and flow
lines in cast and
forged parts .
Microetching
Preparation:
Grinding:
a. Observe instruetions for macroetching.
b. Wet with distilled water on silicon earbide papers down to grit size 600 (for specimens
which are insensitive to water).
C. Prepare by microtome using eemented carbide blade or, even better,diamond blade;
Polishing:
a. With alumina slurry on Mierocloth, or with diamond (particle size 6-1 !Lm). Subsequently,
on soft c10th with a suspension of 120 mI hot distilled water, 20 mI of aqueous solution
of ammonium tartrate (5 %), and I g MgO. Suspension should be filtered before use
. (through a fme eotton or nylon c1oth).
b. Electrolytic:
250 mi 2 min, 25-50 oC (75-120 F), \O
Dist. water
Ethanol (96%)
300 mI V de, Mg or Al cathode.
c. Chemieal
Nitric acid (1.40)
Imerse for 3-s periods. Polish- Pure Mg.
ing effect after about I mino
Then etching eommences.
Etching:
Magnesium is suitable for observations in polarized Iight.
..~
Macroetching
Preparation:
Coarse grinding on siliconcarbide paper is.usually sufficient. If water-sensitive components
are prl=sent, grinding has to be carried out dry, or by using alcohol or kerosine as a
lubricant with proper ventilation precautions.
No.
Etchant
Mg Ethanol, methanol
mi (95%), or dist. water
Nitric acid (1.40)
Conditions
Sees to mins.
100 mI
1-8 mI
Remarks
Pure Mg and most Mg
alIoys, also in cast and
forged state.
Preparation of Mn and Ni
74
Mg
m2
Dist. water
Oxalie aeid
75
Preparation of Mg
Manganese
Mg Dist. water
m3 -Tartarie aed
Mg
m4
Mg
m5
Mg
m6
Flow tines. Grain size

in east material.
Mg-AI, Mg-Mn, and
Mg-Mn-AI-Zn aIloys.
Most types of Mg and

its aIloys.
AIso eastings and
forgings.
Dist. water
Ethylene glyeol (1.11)
Nitrie aed (1.40)
24 mI 30-<i0 s.
75 mi
Iml'
All types of Mg alloys

in east or heat treated
state.
Grain-boundary eteh.
Dist. water
Hydrofluorie aeid
(40%)
Possibly less hydrofluorie aeid
Mg
m8
Dist. water
Nitrie aeid (1.40)
Chromium (VI) oxide
Eleclrolylic:
Oslo water
Sodium hydroxide
Mg Electro/y tic:
miO Oslo water
Ethanol (96%) ~
Phosphore aeid (1.71)
90 mi 3-30 s.
!!! See Appendix A.
10 mi
100 mi 30 s
2-11 g
85 mi 10-30 s.
15 mi Inerease water content
12 g for alloys with high Al
content.
!!! See Appendx A.
Microetching
Preparation:
Grinding:
Wet on silieon earbide papers down to 600 grit.
Teehnieally pure Mg,

Mg-AI-Zn, Mg-Zn-ThZr, Mg-Rare Earth-Zr
alloys.
Mg and Mg-Cu alloys.
Mg die-easting aIloys.
Mg-AI aIloys.
Grain eontrast in heat
treated eastings.
Flow lines in forgings.
a. With diamond paste (particle size 6-0.25 J.Lm), or alumina slurry on Microcloth.
b. Eleetrolytie:
Ethanol (96%)
Glyeerol
Phosphorie aeid (1.71)
20 mi 1-10 min, 10-35 V de,

20 mi Mg cathode.
40 mi !!! See Appendx A.
Complex Mg alloys
eontaining Al, Zn, Cd,
Bi.
50 mI 18 V de, stainless
25 mI steel eathode.
Mn. Mn-Cu alloys.
Etching:
No.
Etehant
.Mn
mi
Dist. water
Hydrofluorie aed
(40%)
Mn
m2
Ethanol (96%)
Nitric aeid (1.40)
(Nital)
Mn
m3
Glycerol
Hydrofluorie aed
(40%)
Hydroehlorie aeid
(1.19)
Nitre aed (1.40)
Mn
100 mi 2-4 min, 4 V de, Cu
IOg eathode.
Eteh immediately
after polishing.
\Mnl
polishing:
19m1 1-30 s.
60 mi Swab.
20 mI Rinse hot.
I mi
Ethanol (96%)
Citrie aeid'
'lO-
90 mi 10 sto 2 min
2-10 g Polish dry only!
Intense eteh rinsing.
Subsequently, rinse in
alcohol. Dry in eold
air stream.
Pure Mg, Mg-Mn, MgAl, Mg-AI-Zr, Mg-ThZr, Mg-Zn-Zr alloys.

AIso extruded types.
Dist. water
Glacial aeetie aed
Nitrie aeid (1.40)
Mg
m7
Mg
m9
100 mi 6-10 s
2g
Aeetelyne aeetone
Ntrie aed (1.40)
Conditions
Remarks
90 mi Sees to mins.
!!! See Appendix A.
10 mI
98 mi Sees to mins.
2ml
Mn-Si-Ca alloys.
Ferromanganese.
40 mi 1-3 s.
!!! See Appendix A.
30 mi
Mn-Ge, Mn-Si,
Mn-Sn-Ge,
Mn-Sn-Si
alloys.
25 mi
10ml
200 mI 2-18 mino
1-2 mi If possible, ultrasonieally, to destroy oxide
film.
Mn-Fe, Mn-Ni, MnCu, Mn-Co alloys.
Pure Mn.
Low-alloy Mn eontaining Ni, Co, Fe,
Ge, and Cu .
Mg and Mg-base
alloys.
Nickel
Pure nickel is tough, and deformation layers frequently formo Nickel alloys
do not pose any particular difficulties. Skin and respiratory poisoning may result
from contact with nickel.
Macroetching
Preparation:
Wet grinding on silcon earbide papers down to 400 grit is normally suffieient.
\ Ni
1"
Preparation of Mn and Ni
74
Mg
m2
Dist. water
Oxalie aeid
75
Preparation of Mg
Manganese
Mg Dist. water
m3 -Tartarie aed
Mg
m4
Mg
m5
Mg
m6
Flow tines. Grain size

in east material.
Mg-AI, Mg-Mn, and
Mg-Mn-AI-Zn aIloys.
Most types of Mg and

its aIloys.
AIso eastings and
forgings.
Dist. water
Nitrie aed (1.40)
24 mI 30-<i0 s.
75 mi
Iml'
All types of Mg alloys

in east or heat treated
state.
Grain-boundary eteh.
Dist. water
Hydrofluorie aeid
(40%)
Possibly less hydrofluorie aeid
Mg
m8
Dist. water
Nitrie aeid (1.40)
Chromium (VI) oxide
Eleclrolylic:
Oslo water
Sodium hydroxide
Mg Electro/y tic:
miO Oslo water
Ethanol (96%) ~
Phosphore aeid (1.71)
90 mi 3-30 s.
!!! See Appendix A.
10 mi
100 mi 30 s
2-11 g
85 mi 10-30 s.
15 mi Inerease water content
12 g for alloys with high Al
content.
!!! See Appendx A.
Microetching
Preparation:
Grinding:
Wet on silieon earbide papers down to 600 grit.
Teehnieally pure Mg,

Mg-AI-Zn, Mg-Zn-ThZr, Mg-Rare Earth-Zr
alloys.
Mg and Mg-Cu alloys.
Mg die-easting aIloys.
Mg-AI aIloys.
Grain eontrast in heat
treated eastings.
Flow lines in forgings.
a. With diamond paste (particle size 6-0.25 J.Lm), or alumina slurry on Microcloth.
b. Eleetrolytie:
Ethanol (96%)
Glyeerol
Phosphorie aeid (1.71)
20 mi 1-10 min, 10-35 V de,

20 mi Mg cathode.
40 mi !!! See Appendx A.
Complex Mg alloys
eontaining Al, Zn, Cd,
Bi.
50 mI 18 V de, stainless
25 mI steel eathode.
Mn. Mn-Cu alloys.
Etching:
No.
Etehant
.Mn
mi
Dist. water
Hydrofluorie aed
(40%)
Mn
m2
Ethanol (96%)
Nitric aeid (1.40)
(Nital)
Mn
m3
Glycerol
Hydrofluorie aed
(40%)
Hydroehlorie aeid
(1.19)
Nitre aed (1.40)
Mn
100 mi 2-4 min, 4 V de, Cu
IOg eathode.
Eteh immediately
after polishing.
\Mnl
polishing:
19m1 1-30 s.
60 mi Swab.
20 mI Rinse hot.
I mi
Ethanol (96%)
Citrie aeid'
'lO-
90 mi 10 sto 2 min
2-10 g Polish dry only!
Intense eteh rinsing.
Subsequently, rinse in
alcohol. Dry in eold
air stream.
Pure Mg, Mg-Mn, MgAl, Mg-AI-Zr, Mg-ThZr, Mg-Zn-Zr alloys.

AIso extruded types.
Dist. water
Glacial aeetie aed
Nitrie aeid (1.40)
Mg
m7
Mg
m9
100 mi 6-10 s
2g
Aeetelyne aeetone
Ntrie aed (1.40)
Conditions
Remarks
90 mi Sees to mins.
!!! See Appendix A.
10 mI
98 mi Sees to mins.
2ml
Mn-Si-Ca alloys.
Ferromanganese.
40 mi 1-3 s.
!!! See Appendix A.
30 mi
Mn-Ge, Mn-Si,
Mn-Sn-Ge,
Mn-Sn-Si
alloys.
25 mi
10ml
200 mI 2-18 mino
1-2 mi If possible, ultrasonieally, to destroy oxide
film.
Mn-Fe, Mn-Ni, MnCu, Mn-Co alloys.
Pure Mn.
Low-alloy Mn eontaining Ni, Co, Fe,
Ge, and Cu .
Mg and Mg-base
alloys.
Nickel
Pure nickel is tough, and deformation layers frequently formo Nickel alloys
do not pose any particular difficulties. Skin and respiratory poisoning may result
from contact with nickel.
Macroetching
Preparation:
Wet grinding on silcon earbide papers down to 400 grit is normally suffieient.
\ Ni
1"
76
Preparation of Ni
Preparation of Ni
Etching:
No.
Ni
MI
N'
M2
Dislo water
Nitric acid (1.40)
(Concentration
variable)
Dist. water
Ethanol (96%)
Hydrochloric acid
(1.19)
Copper (II) sulfate
Ni
M3
Dist. water
Nitric acid (1.40)
Copper (I1) sulfate
Ni
M4
Glacial acetic acid

Nitric acid (1.40)
Hydrochloric acid
(1.19)
Ni
M5
Dist. water
Nitric acid (1.40)
Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
(Concentration
variable)
Ni
M6
Conditions
Etchant

(IlI) chloride
Hydrochloric acid
(1.19)
Nitric acid (1.40)
50 mi 20-30 mino
50-100 mi
50 mi Secs to mins.
50 mi
50 mi
IOg
10 (lOO) mI 20-30 min o
20(100) mI
10 (20) g
50 mi Secs to mins.
50 mI ' Swab.
(75) mi Hydrochloric acid
may possibly be
omitted.
20-30 mi 2 mino
0-20 mI Use fresh onIy!
20 mi
10 mI
2. Dist. water
Sulfuric aeid (1.84)
3. Methanol (95%)
Nitric acid (1.40)
Remarks
High-alloy Ni.
Ni-Cu alloys (Monel).
Ni-Al, Ni-Fe alloys .
Porosity. Flow lines .
Ni and Ni-base alloys.
Ni-Cu alloys. Ni-CrFe aUoys.
Grain size in superalloys.
Low-alloy Ni.
Cracks. Porosity.
Ni alloys containing
Cr and Fe. Welding
joints.
Inconel-type alloys on
Ni-Cr and Ni-Fe-Cr
basis. Ni-Nb, Ni-Ta,
Ni-Si, Ni-Co-Cr
alloys. High abrasion
in superalloys.
d . Eleetrolytic lapping:
1. Dst. water
Disodium hydrogen
phosphate
Sodium fluoride
2. Dist. water
Sodium thiosulfate
Copper (I1) nitrate
Thiourea
3. Dist. water
Alumina slurry No. 3
(0.05 ILm; Linde B)
Arnmonium ehloride
Potassium nitrate
e. Chemical
Nitrie aeid (1.40)
Sulfurie acid (1 .84)
Glacial acetic acid
',.
mI
mi
mI
mi
2-6 min, 1.5-6 V de, Ni eathode.

10-60 s, 40-70 V de, Ni cathode.
!!! See Appendix A.
840 mi Approx 5 min, 1.3 A/O.4 cm 2 ,

50 g ac
50 g.
60 g
985 mi
12 g
1g
2g
100 mi
3-4 min, 4-6 mA/0.7 em

Can be used with and without
the addition of alumina abrasive.
0.5-1 min, 0.05-0.1 mA/0.08
cm 2 , NiCrlO eathode.
Cast Ni.
10 mI
5g
2g
30 mI 30-60 s, 80-90 oC (180-200
10 mI F) ,
10 mi
50 mI
Etching:
AU macroetehants are suitable for mieroetehing if etehing time is shortened.
5-10 mino
125 mI Boiling.
Superalloys.
No.
Etchant
Ni
mi
Dist. water or
ethanol (96%)
Hydroehlorie aeid
(1.19)
!ron (1Il) ehloride
600 mI
18.5 mI
Microetching
Preparation:
Grinding:
400
600
660
330
I 77
I
>
a. Wet on silicon carbide papers down to 600 grito

b. Prepare by mic[-otome using cemented carbide blade or diamond blade; eliminates
polishing. Hardness of specimen should not be greater than 150 HV.
Polishing:
a. Alumina slurfY'No. 1 (5 ILm) and No. I C (1 ILm; Linde C) on felt. Toward the
end of the polishing cycle, add water to remove adhering abrasive particles.
b . Diamond Paste, particle size 6 to I Lm. For hghest quality, also 0.25 Lm. Etch-polishing
sequence with solutions (c. 2) and (e) is of advantage for removal of deformed layer.
e . Eleetrolytie:
l . Glacial aeetie acid
700 mI l-j min, 40-100 V de, Ni
300 mI eathode.
!!! See Appendix A.
Ni
m2
Ni
m3
Ni
m4
Conditions
5-6 S .
20-100 mI Swab .
2-25 mi
5-8 g
Remarks
Ni,Fe, Ni-Cu, and
Ni-Ag alloys.
Ni-base superalloys ....
Monel.
Dist. water
Nitric acid
Glacial acetie aeid
(Coneentration
variable)
O (10) mI 5-30 s.
50 (38) mI Use fresh only!
Grain boundaries.
Pure types of Ni and
alloys with high Ni'
contento Ni-Ti and
Ni-Cu alloys.
Nitric aeid (1.40)

Hydroehloric acid
(1.19)
20 mi 5-6 s.
Does not keep!
lOO mI !!! See Appendix A.
Ni-base superalloys.
95 mi Secs to mins.
5g Use fresh onIy!
100 mI Mix equal amounts
of (a) and (b).
Ni-Zn-Ag, Ni-Ag-NiCu, and Ni-AI-Mo

alloys.
Nonmetallie inclusions are not
attaeked.
a. Dist. water
Potassium cyanide
b. Dist. water
Ammonium persulfate
Hydrogen peroxide
(3 %)
few drops
1;
76
Preparation of Ni
Preparation of Ni
Etching:
No.
Ni
MI
N'
M2
Dislo water
Nitric acid (1.40)
(Concentration
variable)
Dist. water
Ethanol (96%)
Hydrochloric acid
(1.19)
Copper (II) sulfate
Ni
M3
Dist. water
Nitric acid (1.40)
Copper (I1) sulfate
Ni
M4
Glacial acetic acid

Nitric acid (1.40)
Hydrochloric acid
(1.19)
Ni
M5
Dist. water
Nitric acid (1.40)
Hydrochloric acid
(1.19)
Hydrogen peroxide
(30%)
(Concentration
variable)
Ni
M6
Conditions
Etchant

(IlI) chloride
Hydrochloric acid
(1.19)
Nitric acid (1.40)
50 mi 20-30 mino
50-100 mi
50 mi Secs to mins.
50 mi
50 mi
IOg
10 (lOO) mI 20-30 min o
20(100) mI
10 (20) g
50 mi Secs to mins.
50 mI ' Swab.
(75) mi Hydrochloric acid
may possibly be
omitted.
20-30 mi 2 mino
0-20 mI Use fresh onIy!
20 mi
10 mI
2. Dist. water
3. Methanol (95%)
Nitric acid (1.40)
Remarks
High-alloy Ni.
Ni-Cu alloys (Monel).
Ni-Al, Ni-Fe alloys .
Porosity. Flow lines .
Ni and Ni-base alloys.
Ni-Cu alloys. Ni-CrFe aUoys.
Grain size in superalloys.
Low-alloy Ni.
Cracks. Porosity.
Ni alloys containing
Cr and Fe. Welding
joints.
Inconel-type alloys on
Ni-Cr and Ni-Fe-Cr
basis. Ni-Nb, Ni-Ta,
Ni-Si, Ni-Co-Cr
alloys. High abrasion
in superalloys.
d . Eleetrolytic lapping:
1. Dst. water
Disodium hydrogen
phosphate
Sodium fluoride
2. Dist. water
Sodium thiosulfate
Copper (I1) nitrate
Thiourea
3. Dist. water
Alumina slurry No. 3
(0.05 ILm; Linde B)
Arnmonium ehloride
Potassium nitrate
e. Chemical
Nitrie aeid (1.40)
Sulfurie acid (1 .84)
Glacial acetic acid
',.
mI
mi
mI
mi
2-6 min, 1.5-6 V de, Ni eathode.

10-60 s, 40-70 V de, Ni cathode.
!!! See Appendix A.
840 mi Approx 5 min, 1.3 A/O.4 cm 2 ,

50 g ac
50 g.
60 g
985 mi
12 g
1g
2g
100 mi
3-4 min, 4-6 mA/0.7 em

Can be used with and without
the addition of alumina abrasive.
0.5-1 min, 0.05-0.1 mA/0.08
cm 2 , NiCrlO eathode.
Cast Ni.
10 mI
5g
2g
30 mI 30-60 s, 80-90 oC (180-200
10 mI F) ,
10 mi
50 mI
Etching:
AU macroetehants are suitable for mieroetehing if etehing time is shortened.
5-10 mino
125 mI Boiling.
Superalloys.
No.
Etchant
Ni
mi
Dist. water or
ethanol (96%)
Hydroehlorie aeid
(1.19)
!ron (1Il) ehloride
600 mI
18.5 mI
Microetching
Preparation:
Grinding:
400
600
660
330
I 77
I
>
a. Wet on silicon carbide papers down to 600 grito

b. Prepare by mic[-otome using cemented carbide blade or diamond blade; eliminates
polishing. Hardness of specimen should not be greater than 150 HV.
Polishing:
a. Alumina slurfY'No. 1 (5 ILm) and No. I C (1 ILm; Linde C) on felt. Toward the
end of the polishing cycle, add water to remove adhering abrasive particles.
b . Diamond Paste, particle size 6 to I Lm. For hghest quality, also 0.25 Lm. Etch-polishing
sequence with solutions (c. 2) and (e) is of advantage for removal of deformed layer.
e . Eleetrolytie:
l . Glacial aeetie acid
700 mI l-j min, 40-100 V de, Ni
300 mI eathode.
!!! See Appendix A.
Ni
m2
Ni
m3
Ni
m4
Conditions
5-6 S .
20-100 mI Swab .
2-25 mi
5-8 g
Remarks
Ni,Fe, Ni-Cu, and
Ni-Ag alloys.
Ni-base superalloys ....
Monel.
Dist. water
Nitric acid
Glacial acetie aeid
(Coneentration
variable)
O (10) mI 5-30 s.
50 (38) mI Use fresh only!
Grain boundaries.
Pure types of Ni and
alloys with high Ni'
contento Ni-Ti and
Ni-Cu alloys.
Nitric aeid (1.40)

Hydroehloric acid
(1.19)
20 mi 5-6 s.
Does not keep!
lOO mI !!! See Appendix A.
95 mi Secs to mins.
5g Use fresh onIy!
100 mI Mix equal amounts
of (a) and (b).
Ni-Zn-Ag, Ni-Ag-NiCu, and Ni-AI-Mo

alloys.
Nonmetallie inclusions are not
attaeked.
a. Dist. water
Potassium cyanide
b. Dist. water
Ammonium persulfate
Hydrogen peroxide
(3 %)
few drops
1;
78
Preparation of Pb
Preparation of Ni
Ni
m5
Hydroehlorie aeid
(1.l9)
Chromium (VI) oxide
Ni
m6
Nitric acid (1.40)

Hydrofluoric aeid
(40%)
Sees to mins.
0.01-1 g
Ni-Al, Mo-Ni, Ni-Ti

alIoys.
Mieroseetion should
3 mi be heated in boiling
water prior to etehing.
!!! See Appendix A.
Ni and Ni-base
alIoys .
Ni-Cr alIoys.
Ni
m7
Methanol (95%)
Nitrie acid (1.40)
lO mi 5 mino
10 mi
WC-Mo, C-TiC-Ni cemented earbides.
Ni
m8
Amrnonia water
Hydrogen peroxide
(30%)
85 mI 5-15 S.
Does not keep!
15 mi
Ni-Zn alIoys.
Ni
m9
Dist. water
Hydrochloric aeid
(1.l9)
Chromium (VI) oxide
Ni
mIO
Hydroehloric aeid
(1.l9)
40 mI
Nitric acid (1.40)
30 mI
Glyeerol
10 mi
Glacial aeetie acid
20.. mi
(Conentration variable)
Sees to mins.
Do not store!
!!! See Appendix A.
Ni-Fe and Ni-Al

alloys.
Without aeetic acid
Ni-base superalloys .
Ethanol or methanol
(95%)
Hydrochlorie aeid
(1.19)
Copper (H) ehloride
Sees to mins.
Ni-Cu alloys.
Ni-base superalIoys. !
Ni
mlI
50 mi 5-20 s.
!!! See Appendix A.
150 mi
25 g
40-80 mi
40 mi
2g
Ni
ml2
Dist. water
Nitrie aeid (1.40)
Hydrofluorie acid
(40%)
80 mi Sees to mins.
Ni
ml3
Dist. water
I
Nitric acid (1.40),
50 mi 30-60 S .
50 mi 90-100 oC
(200-210 F) .
Ni
ml4
E/eetro/yUe:
Dist. water
Potassium eyani6e
'.
Ni
mI5
</l
i..
E/ectro/ytje:
. Dist. water
Sulfurie aeid (1 .84)
".
EspeeialIy suitable
for HastelIoy types.
Ni
ml6
E/eetrolytie:
Dist. water
Ammonium persulfate
or .chromium (VI)
oxide
Ni
ml7
Eleetrolytie:
Dist. water
Nitrie acid (1.40)
Glacial aeetie acid
Ni
ml8
Electro/y tic:
Dist water
Glycerol
Hydrofluorie acid
Ni
ml9
E/eetro/ytje:
Dist. water
Oxalie aeid
Ni
m20
E/ectrolytie:
Dist water
Phosphoric aeid (171)
Possibly:
Sulfuric aeid (1. 84)
NI
m21
E/eetrolytje:
Phosphoric aeid
(\. 71)
Chromium (VI) oxide
79
lOO mi Secs to mins, 6 V de, Ni and Ni-base

Ni eathode.
alloys.'
Ni-Cr and Ni-Fe
alIoys.
6g
Cast alloys.
85 mi 20- 60 s, 1.5 V de, Pt
10 mI eathode:
5 mi Do not store!
'!!! See Appendix A.
Grain eontrast in Ni.

Ni-Ag, Ni-Al, Ni-Cr,
Ni-Cu, Ni-Fe, and
Ni-Ji alIoys.
85 mi 2-10 s, 2-3 V de, Ni

10 mi cathode.
Ni-Al alIoys .
lOO mI 10-15 s, 6 V de,

IOg stainless steel cathode.
Ni-Au, Ni-Mo, and

Ni-Cr alloys.
Micro-inhomogeneities in superalloys.
30 mi 5-60 s, 2-10 V de, Ni Ni and Ni-base

70 mi eathode.
alloys. ,
Ni-Cr, Ni-Fe alloys.
15 mi
Superalloys of the
(max:)
Nimonie type.
5-30 s, 10 V de, Pt
85 mi eathode.
8g
Gamma precipitates.
Ti and Nb mierosegregations .
Ni-silicides.
10 mi
100 mi Approx 3 min, 6 V

10 g de, Pt eathode.
!!! See Appendix A.
100 mi 5-15 s, 6V de, Pt
2-50 mi eathode.
80Ni-2OCr and 35Ni20Cr-45Fe alloys.
Lead
Carbides in Ni-Cr
alloys.
Ni and Ni-base
alloys . ..
Ni-Cu and Ni-Cr
alloys.
Carbtde inc1usions .
Because of the low hardness and low recrystallization temperature of lead,

deformation layers are difficult to avoid, and erroneous mierostruetures forrn
easily. Preparation methods whieh do not genera te meehanieal strain or heat
are preferred. Respiratory poison and stomaeh poisoning may oeeur upon ingestion
of lead into the human body (!!! See Appendix A).
-'
;" ..',.
Macroetching
Preparation:
J1
In general, either dressing with a speeial file for light and soft metals, or coarse grinding,
.. . is suffieient. Areas of the surfaee not of interest are eovered with plastie spray.
~"."
Ipb I
~/;"
78
Preparation of Pb
Preparation of Ni
Ni
m5
Hydroehlorie aeid
(1.l9)
Chromium (VI) oxide
Ni
m6
Nitric acid (1.40)

Hydrofluoric aeid
(40%)
Sees to mins.
0.01-1 g
Ni-Al, Mo-Ni, Ni-Ti

alIoys.
Mieroseetion should
3 mi be heated in boiling
water prior to etehing.
!!! See Appendix A.
Ni and Ni-base
alIoys .
Ni-Cr alIoys.
Ni
m7
Methanol (95%)
Nitrie acid (1.40)
lO mi 5 mino
10 mi
WC-Mo, C-TiC-Ni cemented earbides.
Ni
m8
Amrnonia water
Hydrogen peroxide
(30%)
85 mI 5-15 S.
Does not keep!
15 mi
Ni-Zn alIoys.
Ni
m9
Dist. water
Hydrochloric aeid
(1.l9)
Chromium (VI) oxide
Ni
mIO
Hydroehloric aeid
(1.l9)
40 mI
Nitric acid (1.40)
30 mI
Glyeerol
10 mi
Glacial aeetie acid
20.. mi
(Conentration variable)
Sees to mins.
Do not store!
!!! See Appendix A.
Ni-Fe and Ni-Al

alloys.
Without aeetic acid
Ethanol or methanol
(95%)
Hydrochlorie aeid
(1.19)
Copper (H) ehloride
Sees to mins.
Ni-Cu alloys.
Ni-base superalIoys. !
Ni
mlI
50 mi 5-20 s.
!!! See Appendix A.
150 mi
25 g
40-80 mi
40 mi
2g
Ni
ml2
Dist. water
Nitrie aeid (1.40)
Hydrofluorie acid
(40%)
80 mi Sees to mins.
Ni
ml3
Dist. water
I
Nitric acid (1.40),
50 mi 30-60 S .
50 mi 90-100 oC
(200-210 F) .
Ni
ml4
E/eetro/yUe:
Dist. water
Potassium eyani6e
'.
Ni
mI5
</l
i..
E/ectro/ytje:
. Dist. water
Sulfurie aeid (1 .84)
".
EspeeialIy suitable
for HastelIoy types.
Ni
ml6
E/eetrolytie:
Dist. water
Ammonium persulfate
or .chromium (VI)
oxide
Ni
ml7
Eleetrolytie:
Dist. water
Nitrie acid (1.40)
Glacial aeetie acid
Ni
ml8
Electro/y tic:
Dist water
Glycerol
Hydrofluorie acid
Ni
ml9
E/eetro/ytje:
Dist. water
Oxalie aeid
Ni
m20
E/ectrolytie:
Dist water
Phosphoric aeid (171)
Possibly:
NI
m21
E/eetrolytje:
Phosphoric aeid
(\. 71)
Chromium (VI) oxide
79
lOO mi Secs to mins, 6 V de, Ni and Ni-base

Ni eathode.
alloys.'
Ni-Cr and Ni-Fe
alIoys.
6g
Cast alloys.
85 mi 20- 60 s, 1.5 V de, Pt
10 mI eathode:
5 mi Do not store!
'!!! See Appendix A.
Grain eontrast in Ni.

Ni-Ag, Ni-Al, Ni-Cr,
Ni-Cu, Ni-Fe, and
Ni-Ji alIoys.
85 mi 2-10 s, 2-3 V de, Ni

10 mi cathode.
Ni-Al alIoys .
lOO mI 10-15 s, 6 V de,

IOg stainless steel cathode.
Ni-Au, Ni-Mo, and

Ni-Cr alloys.
Micro-inhomogeneities in superalloys.
30 mi 5-60 s, 2-10 V de, Ni Ni and Ni-base

70 mi eathode.
alloys. ,
Ni-Cr, Ni-Fe alloys.
15 mi
Superalloys of the
(max:)
Nimonie type.
5-30 s, 10 V de, Pt
85 mi eathode.
8g
Gamma precipitates.
Ti and Nb mierosegregations .
Ni-silicides.
10 mi
100 mi Approx 3 min, 6 V

10 g de, Pt eathode.
!!! See Appendix A.
100 mi 5-15 s, 6V de, Pt
2-50 mi eathode.
80Ni-2OCr and 35Ni20Cr-45Fe alloys.
Lead
Carbides in Ni-Cr
alloys.
Ni and Ni-base
alloys . ..
Ni-Cu and Ni-Cr
alloys.
Carbtde inc1usions .
Because of the low hardness and low recrystallization temperature of lead,

deformation layers are difficult to avoid, and erroneous mierostruetures forrn
easily. Preparation methods whieh do not genera te meehanieal strain or heat
are preferred. Respiratory poison and stomaeh poisoning may oeeur upon ingestion
of lead into the human body (!!! See Appendix A).
-'
;" ..',.
Macroetching
Preparation:
J1
In general, either dressing with a speeial file for light and soft metals, or coarse grinding,
.. . is suffieient. Areas of the surfaee not of interest are eovered with plastie spray.
~"."
Ipb I
~/;"
P.reparation of Pu, Th, U
80
Pb
m3
Etching:
No.
Etchant
Pb
MI
Dist. water
Nitric acid (1.40)
80 mi lO min.
20 mi Swab.
Grain contrast.
Welded seams.
Layers.
Pb
M2
Glycerol
Glacial acetic acid
Nitric acid (1.40)
68 mi Few mino
16 mi Useful as microetchant (few secs).
Grain contrast.
Pb containing Sb.
Pb
M3
Conditions
a. Dist. water
Ammonium molybdate
b. Dist. water
Nitric acid (1 AO)
lOO mI Mix (a) and (b) in

equal proportions.
15 g 10-30 S.
42 mi Swab.
58. mI Rinse in running
water.
Remarks
Dis1. water or ethanol

(96%)
Hydrochloric aed
(1.19)
Iron (I1I) chloride

1-10 min
90(90) mi
20(30) mi
0(10) g
Preparation:
80 mi 14-30 min, 40 oC
15 mi (lOO F) ..
Lead solders.
Pb-Sn alloys.
Pb
m5
Glacial acetic acid

Hydrogen peroxide
(30%)
75 mi 50-15
Pure Pb. Pb-Sb, Pb-Ca

alIoys.
Grain boundaries.
S.
25 mi

5-10 g Etch-rinsing.
Pb
m6
Dist. water
Silver nitrate
Pb
m7
Electrolytic:
Perchloric aed (60%)
Glacial acetic acid
Mix drop by drop in
ice bath for eooling.
Pb
m8
Electrolytic:
Dist. water
Grinding:
a. Dry on silicon carbide papers down to 600 grit; coat papers wth wax.
b. Dressing by lathe, less than 25 ILm per cut.
C. Prepare by microtome using cemented carbide blade or, even better, diamond blade;
Polishing:
a. Electrolytic: 300 mi perchloric acid (60%), 700 mi glacial acetic acid; mix drop by
drop, cool with ice. 3-4 min at 15 C (60F). 8 Y, dc. (!!! See Appendix A.)
b. Alumina slurry. Add I g arnmonium acetate per litre in case of surface-fIlm formation.
Soft polishing cloth. Low rotation speed (200-300 rpm).
C. Hard lead, lead-rich white metals and type metals, speeimen preparation same as for
steel.
,
After polishing, rinse in ,distilled water. Tap water may etch surfaee.
Etching:
No.
't
Etc)ant
Conditions
Pb Glycerol or ethan)
mi,,,, (96%)
. ' \
Glacial aeetic acid
Nitric acid (1 AO)
. (Concentration variable)
~:,
,JI
Ethanol or methanol
(95%)
Nitric acid (1.40)
Can also be used as
macroetchant.
Lead sold~r. Pb,Sb

alloys and high-Pb
whit~ metals and type
metals.
Dis1. water
Glacial aeetic aeid
Nitric acid (1.40)
Removal of deformed
layers. Pure and lowalIoy Pb.
Observe specifications for macroetching.
,ot;
81,
Pb
m4
Microetching
Pb
m2
Preparation of Pb
30 mi I min, 1-2 Y dc, Pb

70 mi or Cu cathode.
!!! See Appendix A.
AII Pb alloys.
Hard lead. High-Pb
white metals and type
metals. Friction
metals. Bearing
metals.
Grain contrast.
40 milOs, 2 Y dc, Pt anode, Pb. Pb-Sb and Pb-Sn

60 mi sample as cathode.
alIoys.
!!! See Appendix A.
Care is advised! Radioactive materials! (!!! See Appendix A.) Work should
be carried out in glove boxes with proper ventilation or "hot cells" if critical
radiation limit is surpassed. In any case, check radiation! These materials must
not be inhaled and are to be handled by properly trained authorized personnel.
Remarks
Pb, Pb-Sb, Pb-Cd,

Few secs.
84(76) mi Possibly 80 oC (180F). Pb-Ca alIoys. Pb-con8(16) mi Use fresh only!
taining Cu and
bronzes .
8 mi
High-Pb white metals.
Grain boundaries and
precipitates.
1-10 min.
Pb and Pb alloys.
lOO mi After etching, store in Hard lead and high-Pb
1-5 mi tap water for short
time.
metals.
Pb solid-solution crystals are etched dark.
Macroetching
Preparation:
Coarse grinding down to 400 grit, wet on silicon carbide papers.
Etching:
No.
Conditions
Etchant
Pu
MI
Nitric acid (1 AO)
Pu
M2
Electrolytic:
Dis1. water
1-5
S.
90 mi Up to 15 min, 20 Y
10 ml de, Al cathode,
~
u
Plutonium, Thorium, Uranium
Remarks
U and U alloys.
U and most U alloys.
Th
P.reparation of Pu, Th, U
80
Pb
m3
Etching:
No.
Etchant
Pb
MI
Dist. water
Nitric acid (1.40)
80 mi lO min.
20 mi Swab.
Grain contrast.
Welded seams.
Layers.
Pb
M2
Glycerol
Glacial acetic acid
Nitric acid (1.40)
68 mi Few mino
16 mi Useful as microetchant (few secs).
Grain contrast.
Pb containing Sb.
Pb
M3
Conditions
a. Dist. water
Ammonium molybdate
b. Dist. water
Nitric acid (1 AO)
lOO mI Mix (a) and (b) in

equal proportions.
15 g 10-30 S.
42 mi Swab.
58. mI Rinse in running
water.
Remarks
Dis1. water or ethanol

(96%)
Hydrochloric aed
(1.19)
Iron (I1I) chloride

1-10 min
90(90) mi
20(30) mi
0(10) g
Preparation:
80 mi 14-30 min, 40 oC
15 mi (lOO F) ..
Lead solders.
Pb-Sn alloys.
Pb
m5
Glacial acetic acid

Hydrogen peroxide
(30%)
75 mi 50-15
Pure Pb. Pb-Sb, Pb-Ca

alIoys.
Grain boundaries.
S.
25 mi

5-10 g Etch-rinsing.
Pb
m6
Dist. water
Silver nitrate
Pb
m7
Electrolytic:
Perchloric aed (60%)
Glacial acetic acid
Mix drop by drop in
ice bath for eooling.
Pb
m8
Electrolytic:
Dist. water
Grinding:
a. Dry on silicon carbide papers down to 600 grit; coat papers wth wax.
b. Dressing by lathe, less than 25 ILm per cut.
C. Prepare by microtome using cemented carbide blade or, even better, diamond blade;
Polishing:
a. Electrolytic: 300 mi perchloric acid (60%), 700 mi glacial acetic acid; mix drop by
drop, cool with ice. 3-4 min at 15 C (60F). 8 Y, dc. (!!! See Appendix A.)
b. Alumina slurry. Add I g arnmonium acetate per litre in case of surface-fIlm formation.
Soft polishing cloth. Low rotation speed (200-300 rpm).
C. Hard lead, lead-rich white metals and type metals, speeimen preparation same as for
steel.
,
After polishing, rinse in ,distilled water. Tap water may etch surfaee.
Etching:
No.
't
Etc)ant
Conditions
Pb Glycerol or ethan)
mi,,,, (96%)
. ' \
Glacial aeetic acid
Nitric acid (1 AO)
. (Concentration variable)
~:,
,JI
Ethanol or methanol
(95%)
Nitric acid (1.40)
Can also be used as
macroetchant.
Lead sold~r. Pb,Sb

alloys and high-Pb
whit~ metals and type
metals.
Dis1. water
Glacial aeetic aeid
Nitric acid (1.40)
Removal of deformed
layers. Pure and lowalIoy Pb.
Observe specifications for macroetching.
,ot;
81,
Pb
m4
Microetching
Pb
m2
Preparation of Pb
30 mi I min, 1-2 Y dc, Pb

70 mi or Cu cathode.
!!! See Appendix A.
AII Pb alloys.
Hard lead. High-Pb
metals. Friction
metals. Bearing
metals.
Grain contrast.
40 milOs, 2 Y dc, Pt anode, Pb. Pb-Sb and Pb-Sn

60 mi sample as cathode.
alIoys.
!!! See Appendix A.
Care is advised! Radioactive materials! (!!! See Appendix A.) Work should
be carried out in glove boxes with proper ventilation or "hot cells" if critical
radiation limit is surpassed. In any case, check radiation! These materials must
not be inhaled and are to be handled by properly trained authorized personnel.
Remarks
Pb, Pb-Sb, Pb-Cd,

Few secs.
84(76) mi Possibly 80 oC (180F). Pb-Ca alIoys. Pb-con8(16) mi Use fresh only!
taining Cu and
bronzes .
8 mi
High-Pb white metals.
Grain boundaries and
precipitates.
1-10 min.
Pb and Pb alloys.
lOO mi After etching, store in Hard lead and high-Pb
1-5 mi tap water for short
time.
metals.
Pb solid-solution crystals are etched dark.
Macroetching
Preparation:
Coarse grinding down to 400 grit, wet on silicon carbide papers.
Etching:
No.
Conditions
Etchant
Pu
MI
Nitric acid (1 AO)
Pu
M2
Electrolytic:
Dis1. water
1-5
S.
90 mi Up to 15 min, 20 Y
10 ml de, Al cathode,
~
u
Plutonium, Thorium, Uranium
Remarks
U and U alloys.
Th
82
Preparation of Lant.hanum and Rare Earths
Preparation of Pu, Th, U
Microetching
Preparation:
Grinding:
Pu
mS
Electrolytic:
Glacial acetic acid
Perchloric aeid
Pu
m9
Electrolytic:
Methanol (95%)
Nitric acid (1.40)
Wet on silicon carbide papers down to 600 grit.
Polishing: a. Aluminaslurry or diamond paste down to finest particle size .

b. Electrolytic:
l. Glacial acetie acid
900 mI 30 s to mins, 12-20 V
Especially for Pu-AI
lOO mI de, stainless steel cath- aUoys.
ode.
!!! See Appendix A.
2. Ethanol (96%)
300 mI 4-6 min, 20-30 V dc,
Phosphorie acid (1.71) 300 mi Al cathode .
Glycerol
3. Etltanol (96%)
445 mI 1-5 min, 18-20 V dc,
275 mi stainless steel eathode.
Phosphorie aeid (1.71) 275 mI !!! See Appendix A.
Etching:
No.
Pu
m2
Pu
m3
Pu
m4
.~ l
:~ '
Etehant
Conditions
30 mi 5-30 s
30 mi
Nitrie aeid (1.40)

Glacial acetic aeid
Glyeerol
Dist. water
Nitric acid (1.40) or
Hydrofluorie acid
(40%)

38 (25) mI !!! See Appendix A.
1 (25) mi
Gwcerol
Nitric acid (1.40) ,
Hydrofluorie acid
(40%)
Pu
m6
Hydrofluorie acid
(40%)
Nitrie acid (1.40)
Pu
m7
Laetic acid (90%)

Nitric acid (1.40)
Hydrofluoric aeid
(40%)
..
70 mi Secs to mins.
25 mi
5 mI
5-30 s.
I mI !!! See Appendix A.
30 mI
10 mi
~"
U-Al alloys . UAl 2

(light blue). UAI) (yellow). UAI. (gray).
20 mI 2 min, 0.05 Ajcm 2 ,

50 mI stainless steel cath5 mi ode.
Pu and Pu-base alloys.
Microetching
Preparation:
Grinding:
Polishing:
With diamondpaste andjor alumina slurry down to finest particle size on felt or velvet.
Etching:
U alloys
U-Be alloys.
U-beryllides, U-Zr,
and U-Nb alloys.
RE
'mI
30 mi Secs lo mins.
30 mi
U-silicides.
Conditions
75 mi 5-15 s.
Remarks
For most RE metals
and their alloys.
25 mI
Mins to hours
For mosl alloys of RE

metals.
m2
room lemperature to
200 oC (390 F)
RE
Nitric acid (1.40)

Glacial acetic acid
Laetic acid (90%)
15 mI 10-15
10 mi
5 mi
20 mI
Iml
Ethanol (96%)
Nitric acid (1.40)
49 mi 2-3 mino
Pure Gd. RE-Co
1 mI Possible pre-etehing
alloys.
with solution made of Grain-boundary etch.
30 mI nitrie acid (1.40)
and 70 mi glyeerol.
Heat solution in water
bath.
Gamma phase stabilized U-Mo and U-Zr

alloys.
Th and Th-base
alloys.
Etehant
Glacial acetic acid
Hydrogen peroxide
(30%)
RE Heat tinting inair,
m3
Few seco
50 mi
3 drops
Pure U and Th.
Wet on silicon carbide papers down to 600 grit. Exceptions: europium, lanthanum, and
rare-earth-eobalt alloys grind dry.
30 mi
40 mi 5-10 S .
90 mi 5-15 min, 18-20 V

cathode.
!!! See Appendix A.
Cerium, dysprosiurn, erbiurn, europiurn, gadoliniurn, holrniurn, lanthanurn,

lutetiurn, neodyrniurn, prornethiurn, praseodyrniurn, sarnariurn, terbiurn, thuliurn,
ytterbium.
No .

Nitric acid (1.40)
r
Hydrofluorie acid
,.,I
(40%)
, i
Nitrie acid (1 .4~
Laetic acid (90 o) or
Dist. water
Pu
m5
Remarks
83
Lanthanum and Rare Earths (Lanthanides)
Uranium is suitable for observation in polarized light.

Heat tinting at 100-200 oC (21O-390F) for several hours gives good results for most
types of uranium and uranium alloys.
Pu
mI
RE
m4
S.
Dy, Er, Gd, Ho-base

alloys. RE-Co alloys.
RE
Ce
Dy
Er
Eu
Gd
Ho
La
Lu
Nd
Pro
Pr
Sm
Tb
Tm
Yb I
'j-
82
Preparation of Lant.hanum and Rare Earths
Preparation of Pu, Th, U
Microetching
Preparation:
Grinding:
Pu
mS
Electrolytic:
Glacial acetic acid
Perchloric aeid
Pu
m9
Electrolytic:
Methanol (95%)
Nitric acid (1.40)
Wet on silicon carbide papers down to 600 grit.
Polishing: a. Aluminaslurry or diamond paste down to finest particle size .

b. Electrolytic:
l. Glacial acetie acid
900 mI 30 s to mins, 12-20 V
Especially for Pu-AI
lOO mI de, stainless steel cath- aUoys.
ode.
!!! See Appendix A.
2. Ethanol (96%)
300 mI 4-6 min, 20-30 V dc,
Phosphorie acid (1.71) 300 mi Al cathode .
Glycerol
3. Etltanol (96%)
445 mI 1-5 min, 18-20 V dc,
275 mi stainless steel eathode.
Phosphorie aeid (1.71) 275 mI !!! See Appendix A.
Etching:
No.
Pu
m2
Pu
m3
Pu
m4
.~ l
:~ '
Etehant
Conditions
30 mi 5-30 s
30 mi
Nitrie aeid (1.40)

Glacial acetic aeid
Glyeerol
Dist. water
Nitric acid (1.40) or
Hydrofluorie acid
(40%)

38 (25) mI !!! See Appendix A.
1 (25) mi
Gwcerol
Nitric acid (1.40) ,
Hydrofluorie acid
(40%)
Pu
m6
Hydrofluorie acid
(40%)
Nitrie acid (1.40)
Pu
m7
Laetic acid (90%)

Nitric acid (1.40)
Hydrofluoric aeid
(40%)
..
70 mi Secs to mins.
25 mi
5 mI
5-30 s.
I mI !!! See Appendix A.
30 mI
10 mi
~"
U-Al alloys . UAl 2

(light blue). UAI) (yellow). UAI. (gray).
20 mI 2 min, 0.05 Ajcm 2 ,

50 mI stainless steel cath5 mi ode.
Pu and Pu-base alloys.
Microetching
Preparation:
Grinding:
Polishing:
With diamondpaste andjor alumina slurry down to finest particle size on felt or velvet.
Etching:
U alloys
U-Be alloys.
U-beryllides, U-Zr,
and U-Nb alloys.
RE
'mI
30 mi Secs lo mins.
30 mi
U-silicides.
Conditions
75 mi 5-15 s.
Remarks
For most RE metals
and their alloys.
25 mI
Mins to hours
For mosl alloys of RE

metals.
m2
room lemperature to
200 oC (390 F)
RE
Nitric acid (1.40)

Glacial acetic acid
Laetic acid (90%)
15 mI 10-15
10 mi
5 mi
20 mI
Iml
Ethanol (96%)
Nitric acid (1.40)
49 mi 2-3 mino
Pure Gd. RE-Co
1 mI Possible pre-etehing
alloys.
with solution made of Grain-boundary etch.
30 mI nitrie acid (1.40)
and 70 mi glyeerol.
Heat solution in water
bath.
Gamma phase stabilized U-Mo and U-Zr

alloys.
Th and Th-base
alloys.
Etehant
Glacial acetic acid
Hydrogen peroxide
(30%)
RE Heat tinting inair,
m3
Few seco
50 mi
3 drops
Pure U and Th.
Wet on silicon carbide papers down to 600 grit. Exceptions: europium, lanthanum, and
rare-earth-eobalt alloys grind dry.
30 mi
40 mi 5-10 S .
90 mi 5-15 min, 18-20 V

cathode.
!!! See Appendix A.
Cerium, dysprosiurn, erbiurn, europiurn, gadoliniurn, holrniurn, lanthanurn,

lutetiurn, neodyrniurn, prornethiurn, praseodyrniurn, sarnariurn, terbiurn, thuliurn,
ytterbium.
No .

Nitric acid (1.40)
r
Hydrofluorie acid
,.,I
(40%)
, i
Nitrie acid (1 .4~
Laetic acid (90 o) or
Dist. water
Pu
m5
Remarks
83
Lanthanum and Rare Earths (Lanthanides)
Uranium is suitable for observation in polarized light.

Heat tinting at 100-200 oC (21O-390F) for several hours gives good results for most
types of uranium and uranium alloys.
Pu
mI
RE
m4
S.
Dy, Er, Gd, Ho-base

alloys. RE-Co alloys.
RE
Ce
Dy
Er
Eu
Gd
Ho
La
Lu
Nd
Pro
Pr
Sm
Tb
Tm
Yb I
'j-
84
Preparation of Ti
Preparation of Sn
No.
Because of the tendency of tin toward deformation and low recrystallization

temperature, deformation layers may also form in pure tin as well as in some
ofits alloys. Artifacts and mechanical twinning occur commonly. Use preparation
methods which do not generate mechanical strain and heat.
Su
mi
Sn
m2
Macroetching
Etehant
100 mI
(1.19)
2-5 mI
Dist. water or
methanol (5%)
Hydrochloric acid
10-30 s (possibly up
100 mI to 5 min).
Preparation:
(1.19)
Iron (III) ehloride
Etching:
Conditions
Sn
MI

arnmonium polysulfide
Sn
M2
Dist. water
Hydroehlorie acid
(\.19)
Iron (III) ehloride
20-30 mino
. Wipe off with eotton
after etehing.
100 mi 30 sto 5 min
Sn
m3
Sn-rieh bearing metals

and white metals.
2 mI
lOg
Microetching
Preparation:
Observe instruetions foc maeroetehing.
Glyeerol
Hydrofluoric acid
Nitric acid (1.40)
Sn
m4
Ethanol (96%)
Nitric acid (1.40)
(Nital)
lOO mi 2-3 S .
1-5 mi Possibly followed by
stronger nital etchant.
So
mS
Dst. water
Arnmonium persulfate
So
m6
Cold sat. aqueous sol.

oC sodium thiosulfa,,, "
So
m7
Ethanol (96%)
Picric acid
(Pieral)
(40%)
Grinding:
a. Wet on silieon earbide papers down to 600 grit (eoat with wax).
b. Prepare by mierotome using eemented earbide blade or diamond blade; eliminates
polishing.
e. For high-tin white metals, use same method as for steel.
Sn Electrolytic:
m8 ' Dist. water
Polishing:
So
m9
a . Eleetrolytie:
1. Dist. water
,
Perehlorie acid (70%) I
Glacial aeetie acid ~ ,
2. Dist. water
t
Fluoborie aeii1 (35%)
Sulfurie aeid (1.84);'
13 mi
63 mi
300 mi
780 mi
200 mi
20 mi
Approx 10 min, 20-30 V de,

Sn eathode.
!!! See Appendix A.
3-5 s, 20-40 oC (70-100 0F),
15-17 V de, stainless steel
eathode.
!!! See Appendix A.
b. wlth alumina slurry <pos~ible eteh-polishing sequenee) on Mierocloth, or with diamond
paste (particle size 6~.25 .Lm). Subsequently on soft cloth with a suspension of 120
mi hot distilled water, 2P mraqueous solution of tartarie aeid (5%), and I g magnesia.
Suspension should be filtered before use (through a fine nylon cloth or eotton material).
5-25 mI
lOg
25 mI I mino
!!! See Appendix A.
2ml
I drop
Remarks
For all types of Sn
and Sn-base alloys.
Grain distributiori.
Conditions
Few mins.
Ethanol or methanol
(95%) or dist. water
Hydrochloric aeid
Coarse grinding (wet) On silieon earbide paper is often sufficient. A special file can also
be used for light and soft metals. Possibly diamond polishing down to 6 .Lm.
Etehant
Electrolytic:
Dist. water
, Glacial acetic acid

5-10 g
60-90 S .
50 mi
5g
lOO mI Sees to mins.
4g
Remarks
Pure Sn, Sn-Cd, SnFe, Sn-Pb, and Sn-SbCu alloys.
and white metals.
Sn-Cu alloys and
Bi-Sn euteetie.
Sn layers on steel.
Sn-Pb alloys.
Pure Sn. Sn-rich

alloys with Cd, Fe,
Sb, Cu.
Sn layers. Sn bearing
metals.
Grain .contrast,(eplpr)
in pure Sn and most
Sn alloys.
Sn layers on steel and
cast iron.
80 mi Sees to mins, 30 V de, Pure Sn. Withdraw

sample while current
20 mI Al eathode.
is on.
25 mi lO min, 20-30 V de,

300 mi Sn cathode.
Sn and Sn-rich alloys.
Titanium
Pure titanium is soft and deformation layers easi1y formo Titanium alloys
usual1y do not pose any particular problems.
""' , '>;:
Macroetching
Preparation:
Wet grinding on silicon earbide papers down to 600 grit.
~1
85
Etching:
Tin
No.
Ti I
.''J.
84
Preparation of Ti
Preparation of Sn
No.
Because of the tendency of tin toward deformation and low recrystallization

temperature, deformation layers may also form in pure tin as well as in some
ofits alloys. Artifacts and mechanical twinning occur commonly. Use preparation
methods which do not generate mechanical strain and heat.
Su
mi
Sn
m2
Macroetching
Etehant
100 mI
(1.19)
2-5 mI
Dist. water or
methanol (5%)
Hydrochloric acid
10-30 s (possibly up
100 mI to 5 min).
Preparation:
(1.19)
Iron (III) ehloride
Etching:
Conditions
Sn
MI

arnmonium polysulfide
Sn
M2
Dist. water
Hydroehlorie acid
(\.19)
Iron (III) ehloride
20-30 mino
. Wipe off with eotton
after etehing.
100 mi 30 sto 5 min
Sn
m3

and white metals.
2 mI
lOg
Microetching
Preparation:
Observe instruetions foc maeroetehing.
Glyeerol
Hydrofluoric acid
Nitric acid (1.40)
Sn
m4
Ethanol (96%)
Nitric acid (1.40)
(Nital)
lOO mi 2-3 S .
1-5 mi Possibly followed by
stronger nital etchant.
So
mS
Dst. water
Arnmonium persulfate
So
m6
Cold sat. aqueous sol.

oC sodium thiosulfa,,, "
So
m7
Ethanol (96%)
Picric acid
(Pieral)
(40%)
Grinding:
a. Wet on silieon earbide papers down to 600 grit (eoat with wax).
b. Prepare by mierotome using eemented earbide blade or diamond blade; eliminates
polishing.
e. For high-tin white metals, use same method as for steel.
Sn Electrolytic:
m8 ' Dist. water
Polishing:
So
m9
a . Eleetrolytie:
1. Dist. water
,
Perehlorie acid (70%) I
Glacial aeetie acid ~ ,
2. Dist. water
t
Fluoborie aeii1 (35%)
Sulfurie aeid (1.84);'
13 mi
63 mi
300 mi
780 mi
200 mi
20 mi
Approx 10 min, 20-30 V de,

Sn eathode.
!!! See Appendix A.
3-5 s, 20-40 oC (70-100 0F),
15-17 V de, stainless steel
eathode.
!!! See Appendix A.
b. wlth alumina slurry <pos~ible eteh-polishing sequenee) on Mierocloth, or with diamond
paste (particle size 6~.25 .Lm). Subsequently on soft cloth with a suspension of 120
mi hot distilled water, 2P mraqueous solution of tartarie aeid (5%), and I g magnesia.
Suspension should be filtered before use (through a fine nylon cloth or eotton material).
5-25 mI
lOg
25 mI I mino
!!! See Appendix A.
2ml
I drop
Remarks
For all types of Sn
and Sn-base alloys.
Grain distributiori.
Conditions
Few mins.
Ethanol or methanol
(95%) or dist. water
Hydrochloric aeid
Coarse grinding (wet) On silieon earbide paper is often sufficient. A special file can also
be used for light and soft metals. Possibly diamond polishing down to 6 .Lm.
Etehant
Electrolytic:
Dist. water
, Glacial acetic acid

5-10 g
60-90 S .
50 mi
5g
lOO mI Sees to mins.
4g
Remarks
Pure Sn, Sn-Cd, SnFe, Sn-Pb, and Sn-SbCu alloys.
and white metals.
Sn-Cu alloys and
Bi-Sn euteetie.
Sn layers on steel.
Sn-Pb alloys.
Pure Sn. Sn-rich

alloys with Cd, Fe,
Sb, Cu.
Sn layers. Sn bearing
metals.
Grain .contrast,(eplpr)
in pure Sn and most
Sn alloys.
Sn layers on steel and
cast iron.
80 mi Sees to mins, 30 V de, Pure Sn. Withdraw

sample while current
20 mI Al eathode.
is on.
25 mi lO min, 20-30 V de,

300 mi Sn cathode.
Sn and Sn-rich alloys.
Titanium
Pure titanium is soft and deformation layers easi1y formo Titanium alloys
usual1y do not pose any particular problems.
""' , '>;:
Macroetching
Preparation:
Wet grinding on silicon earbide papers down to 600 grit.
~1
85
Etching:
Tin
No.
Ti I
.''J.
86
Preparation of Ti
Preparation of Ti
Etching:
Etching:
Remarks
Conditions
Etchant
No.
/ 87
Oist. water
Ti
Ml Nitric acid (1.40)
Hydrofluoric acid
(40%)
'Content of hydrofluoric acid may be
decreased
50 mi 5- 8 min, 60--80 oc
40 mi (140--180 F).
!!! See Appendix A.
10 mi
Ti and Ti-base alloys.

Ti-AI-Mo alloys.
Ti
M2
Oist. water
Hydrofluoric acid
(40%)
Hydrogen peroxide
(30%)
30 mi Swab until desired

contrast is obtained.
10 mi
lodide Ti.
Ti
M3
Oist. water
Hydrofluoric acid
(40%)
Iron (111) nitrate
Oxalic acid
Ti
M4
Oist. water
Hydrochloric acid
(1.19)
60 m!
200 mi Secs to mins, 50-60 oC Welded seams .
(120--140 F).
2 m! !!! See Appendix A.
lOg
35 g
Oifferentiation of
50 m! Secs to mins.
alpha and beta Ti.
50 mi
Titanium is suitable for observations in polarized light.

No.
Oist. water
Hydrofluoric acid
(40%)
Nitric acid (1.40)
(KroU's reagent)
Ti
m2
Oist. water
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Ti
m3
Oist. water
Hydrofluoric acid
(40%)
or
Ti
m4
Oist. water
Hydrogen peroxide
(30%)
Aqueous sol. of potassium hydroxide
Microetching
Preparation:
Grinding:
a. Same as for macroetching. Starting with 400 grit, coat papers with wax.
b. Prepare by microtome using cemented carbide blade. Only final polishing needed after
this treatment. Oiamond blades are not suitable, because they tend to leave a rough
surface.
Polishing:
a. Electrolytic:
1. Glacial acetic l/-cid
..
900 mi
60 m!
1-5 min, 20-60 V dc,

!!! See Appendix A .
1-6 min, 20--25 V dc,
!!! See Appendix A.
90 mi
2. Ethanol (96%'
10m!
n-Butyl alcohol
6g
Aluminum c~loride
28 g
Zinc chloride
.... b. With diamond" >~te or alumina slurry down to fmest partic1e size. P.os~ible multiple
polishing with one of the electrolytes mentioned aboye o~ ~tch-polishmg se.quence
with one of the elctrolytes mentioned aboye or etch-polishing sequence W1th one
of the microe~chants listed.
c. Chemical:
l. With nacroetchant Ti M2
Approx 5-20 S.
2. With microetchant Ti mi
10m! Secs to mins.
3. Hydrofluoric acid (40%)
Nitric acid (1.40)
30 m!
Lactic acid(90%)
't.~ _-....
Etchant
Ti
mi
Conditions
Remarks
100 mi 3- 10 s.
!!! See Appendix A.
1-3 mi
2-6 mi
For many Ti raw materials. EspeciaUy for

Ti-AI-VaUoys.
85(96)ml 2- 3 s.
!~! See Appendix A.
10(2) mi
5 (2) mi
Most types of Ti and

Ti aUoys. Ti-Mn, TiV-Cr-AI aIIoys.

Ti aUoys.
Glycerol instead of
Alpha Ti is attacked.
1-10 mi water decreases attack
rate.
1-10 m! !!! See Appendix A.
78 (20) mi 3-20 S.
Swab.
15 (5) mi
12(IO)ml
Ti. Ferro-Ti.
Ti-AI-V-Sn aIIoys.
Alpha Ti is attacked;
beta Ti is left unchangeil.
Ti
m5
Oist. water
Glycerol
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Ti-AI-S n and Ti-Al-Ni

20 mi 3- 20 S.
45 m! Swab.
alloys.
Use 3 m! hydrochloric
1 m! acid (1.19) instead of
water.
Ti-Si alloy.
Ti
m6
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Lactic acid (90%)
(Concentration yariable)
5- 30 S .
1 mi 00 not store!
30 mi See Appendix A.
30 mi
Ti
m7
Oist. water
Hydrofluoric acid
(40%)
Hydrogen peroxide
(30%)
Ti
m8
Electrolytic:
Oist. water
Methanol (95 %)
100 m! 30-60 s.
!!! See Appendix A.
2m!
Attacks hydrides in Ti
preferentially.
Ti and Ti aIIoys.
Grain boundary
etchant.
5 mi
25 m!
390 mi
350 m!
35 m!
10--40 s, 5"-10 oC (40Pure Ti.

50F), 30- 50 V dc,
!!! See Appendix A.
86
Preparation of Ti
Preparation of Ti
Etching:
Etching:
Remarks
Conditions
Etchant
No.
/ 87
Oist. water
Ti
Ml Nitric acid (1.40)
Hydrofluoric acid
(40%)
'Content of hydrofluoric acid may be
decreased
50 mi 5- 8 min, 60--80 oc
40 mi (140--180 F).
!!! See Appendix A.
10 mi

Ti-AI-Mo alloys.
Ti
M2
Oist. water
Hydrofluoric acid
(40%)
Hydrogen peroxide
(30%)
30 mi Swab until desired

contrast is obtained.
10 mi
lodide Ti.
Ti
M3
Oist. water
Hydrofluoric acid
(40%)
Iron (111) nitrate
Oxalic acid
Ti
M4
Oist. water
Hydrochloric acid
(1.19)
60 m!
200 mi Secs to mins, 50-60 oC Welded seams .
(120--140 F).
lOg
35 g
Oifferentiation of
50 m! Secs to mins.
alpha and beta Ti.
50 mi
Titanium is suitable for observations in polarized light.

No.
Oist. water
Hydrofluoric acid
(40%)
Nitric acid (1.40)
(KroU's reagent)
Ti
m2
Oist. water
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Ti
m3
Oist. water
Hydrofluoric acid
(40%)
or
Ti
m4
Oist. water
Hydrogen peroxide
(30%)
Aqueous sol. of potassium hydroxide
Microetching
Preparation:
Grinding:
a. Same as for macroetching. Starting with 400 grit, coat papers with wax.
b. Prepare by microtome using cemented carbide blade. Only final polishing needed after
this treatment. Oiamond blades are not suitable, because they tend to leave a rough
surface.
Polishing:
a. Electrolytic:
1. Glacial acetic l/-cid
..
900 mi
60 m!
1-5 min, 20-60 V dc,

1-6 min, 20--25 V dc,
!!! See Appendix A.
90 mi
2. Ethanol (96%'
10m!
n-Butyl alcohol
6g
Aluminum c~loride
28 g
Zinc chloride
.... b. With diamond" >~te or alumina slurry down to fmest partic1e size. P.os~ible multiple
polishing with one of the electrolytes mentioned aboye o~ ~tch-polishmg se.quence
with one of the elctrolytes mentioned aboye or etch-polishing sequence W1th one
of the microe~chants listed.
c. Chemical:
l. With nacroetchant Ti M2
Approx 5-20 S.
2. With microetchant Ti mi
10m! Secs to mins.
3. Hydrofluoric acid (40%)
Nitric acid (1.40)
30 m!
Lactic acid(90%)
't.~ _-....
Etchant
Ti
mi
Conditions
Remarks
100 mi 3- 10 s.
!!! See Appendix A.
1-3 mi
2-6 mi
For many Ti raw materials. EspeciaUy for

Ti-AI-VaUoys.
85(96)ml 2- 3 s.
!~! See Appendix A.
10(2) mi
5 (2) mi
Most types of Ti and

Ti aUoys. Ti-Mn, TiV-Cr-AI aIIoys.

Ti aUoys.
Glycerol instead of
Alpha Ti is attacked.
1-10 mi water decreases attack
rate.
1-10 m! !!! See Appendix A.
78 (20) mi 3-20 S.
Swab.
15 (5) mi
12(IO)ml
Ti. Ferro-Ti.
Ti-AI-V-Sn aIIoys.
Alpha Ti is attacked;
beta Ti is left unchangeil.
Ti
m5
Oist. water
Glycerol
Nitric acid (1.40)
Hydrofluoric acid
(40%)
Ti-AI-S n and Ti-Al-Ni

20 mi 3- 20 S.
45 m! Swab.
alloys.
Use 3 m! hydrochloric
1 m! acid (1.19) instead of
water.
Ti-Si alloy.
Ti
m6
Hydrofluoric acid
(40%)
Nitric acid (1.40)
Lactic acid (90%)
(Concentration yariable)
5- 30 S .
1 mi 00 not store!
30 mi See Appendix A.
30 mi
Ti
m7
Oist. water
Hydrofluoric acid
(40%)
Hydrogen peroxide
(30%)
Ti
m8
Electrolytic:
Oist. water
Methanol (95 %)
100 m! 30-60 s.
!!! See Appendix A.
2m!
Attacks hydrides in Ti
preferentially.
Ti and Ti aIIoys.
Grain boundary
etchant.
5 mi
25 m!
390 mi
350 m!
35 m!
10--40 s, 5"-10 oC (40Pure Ti.

50F), 30- 50 V dc,
!!! See Appendix A.
88
T
m9
Electrolytic:
Glacial acetic acid
Preparation of Zn
Preparation of Zn
80 mI 1-5 min, 20-60 V dc,

5mI stainless steel cathode.
!!! See Appendix A.
Electrolylic:
mIO Dist. water
Ethnol (96%)
Lactic acid (90%)
Citric acid
Oxalic acid
Pure Ti and Ti-base

alloys.
Ti
35 mI
60 mI
10 mi
5 mi
5g
5g
10 s, 30-50 V dc,
stainless steel cathode. Tint etching.
Possible dilution with Precipitates.
equal amount of glycerol. Then, use 130
V dc, 60 s.
!!! See Appendix A.
If a deposit forms during etching, immediately clean sample in aqueous solution of sulfuric
acid (10-30%).
IZn
Zinc
During metallographic preparation of zinc, deformation layers may easily formo

False microstructures are also cornmon. Therefore, mechanical strain and heat
formation should be avoided during preparation.
, Macroetching
Preparation:
Coarse grinding is sufficient. Possibly pre-polishing with diamond paste, particle size
6 Lm.
Etching:
No.
Etchant
Zn
MI
Dist. water
Hydrochloric acid
(1.19) or concentrated
hydrochloric acid only
or concentrated nitric f
acid (1.40) only
I
Zn
M2
Dist. water
'
Chromium (VI) oxide~
Sodium sulfate (anhy,
drous)
(Palmerton's reagent)
Remarks
Conditions
50 mi Approx 15 s.
Rinse off film under
running water.
Pure Zn.
Zn alloys without Cu.
Cast materials.
',,"
.
'.
Polishing:
a. With alumina slurry on Microcloth, or with diamond paste (particle size: 6, 3, 1,
and possibly 0.25 Lm, followed by polishing with a suspension of 120 mi warm distilled
water, 20 mi of aqueous solution of ammonium tartrate (5%), and 1 g magnesium
oxide. Before use, suspension should be ftltered through a fme nylon or cotton cloth.
b. To eliminate the deformed layer originated in gri,nding, a pre-polishing may be useful.
Soap is added to an alumina slurry, and the specimen is polished with this mixture
on a soft wool cloth. Attack-polishing m~y also be suitable. Here, mechanical polishing
with alumina or diamond alternates with etching, employing etchant Zn mi. The following
sequence has proven successful: 4 min diamond (6 Lm), 3.5 min etch, 6 min diamond
(3 Lm), 1.5 rnin etch, 8 min diamond (1 Lm), 30 s etch, 10 min diamond (0.25 Lm),
10 s etch, polishing with alumina slurry No. 3 (0.05 Lm, Linde B), 5 sec etch.
c. Electrolytic:
lOO mI 40-50 s, 60 V dc, Pt or
1. Dist. water
Zn cathode.
20 g
Chromium (VI) oxide
!!! See Appendix A.
l h and longer, 4-6 V dc,
50 mI
50 mI stainless steel cathode.
Ethanol (96%)
!!! See Appendix A.
d. Chemical:
lOO mi Up to 30 mino
Dist. water
Layer of reaction products
5 mi
Nitric acid (1.40)
is water soluble.'
I.5g
Sodium sulfate
!!! See Appendix A.
20 g
Chromium (VI) oxide
Etching:
Zinc is suitable for observation in polarized light.
Conditions
Etchant
No.
Zn
mi
Dist. water
Chromium (VI) oxide
Sodium sulfate
Zn
m2
Dist. water, ethanol,

methanol, or amyl
alcohol (95%)
Nitric acid (1.40)
50 mI
~.
Microetching
Preparation:
See recommendations for macroetching.
Grinding:
a. Wet on silicon carbide papers down to 600 grit (coat papers with wax).
~
,~l
89
b. Prepare by microtome using cemented carbide blade or diamond blade; eliminates

polishing.
Zn alloys containing
Cu. Dilute with lOO mI
20 g If using sodium sulfate containing crystal water if used as microetchant.
I.5g water (Na2 S04
IOH2 0) increase to
3.5 g.
!!! See Appendix A.
lOO mi 2-3 mino

20 g For alloys containing
l.5g Cu, use half the
amount of sodium sulfate.
Rinse in:
lOO mi disto water
20 g chromium (VI)
oxide
!!! See Appendix A.
Secs to mins.
Etching solution
lOO mi should not be older
0.5-1 mi than I h. To avoid
stains, rinse specimen
in aqueous sol. of
chromic acid (20%)
after etching
Remarks
F or most types of Zn
and Zn alloys. Especially for rolled Zn
containing Pb and
Zn-Cu alloys.
If chromium (VI)
oxide content is
lowered to 5 g and the
sodium sulfate to 0.5
g, etchant can be used
f or pressure-cast
parts, and Zn platings.
Zn-Fe layers of galvanized steel or ferrous materials.
Zn-AI and Zn-Cr
alloys.
Grain boundaries.
88
T
m9
Electrolytic:
Glacial acetic acid
Preparation of Zn
Preparation of Zn
80 mI 1-5 min, 20-60 V dc,

5mI stainless steel cathode.
!!! See Appendix A.
Electrolylic:
mIO Dist. water
Ethnol (96%)
Lactic acid (90%)
Citric acid
Oxalic acid
Pure Ti and Ti-base

alloys.
Ti
35 mI
60 mI
10 mi
5 mi
5g
5g
10 s, 30-50 V dc,
stainless steel cathode. Tint etching.
Possible dilution with Precipitates.
equal amount of glycerol. Then, use 130
V dc, 60 s.
!!! See Appendix A.
If a deposit forms during etching, immediately clean sample in aqueous solution of sulfuric
acid (10-30%).
IZn
Zinc
During metallographic preparation of zinc, deformation layers may easily formo

False microstructures are also cornmon. Therefore, mechanical strain and heat
formation should be avoided during preparation.
, Macroetching
Preparation:
Coarse grinding is sufficient. Possibly pre-polishing with diamond paste, particle size
6 Lm.
Etching:
No.
Etchant
Zn
MI
Dist. water
Hydrochloric acid
(1.19) or concentrated
hydrochloric acid only
or concentrated nitric f
acid (1.40) only
I
Zn
M2
Dist. water
'
Chromium (VI) oxide~
Sodium sulfate (anhy,
drous)
(Palmerton's reagent)
Remarks
Conditions
50 mi Approx 15 s.
Rinse off film under
running water.
Pure Zn.
Zn alloys without Cu.
Cast materials.
',,"
.
'.
Polishing:
a. With alumina slurry on Microcloth, or with diamond paste (particle size: 6, 3, 1,
and possibly 0.25 Lm, followed by polishing with a suspension of 120 mi warm distilled
water, 20 mi of aqueous solution of ammonium tartrate (5%), and 1 g magnesium
oxide. Before use, suspension should be ftltered through a fme nylon or cotton cloth.
b. To eliminate the deformed layer originated in gri,nding, a pre-polishing may be useful.
Soap is added to an alumina slurry, and the specimen is polished with this mixture
on a soft wool cloth. Attack-polishing m~y also be suitable. Here, mechanical polishing
with alumina or diamond alternates with etching, employing etchant Zn mi. The following
sequence has proven successful: 4 min diamond (6 Lm), 3.5 min etch, 6 min diamond
(3 Lm), 1.5 rnin etch, 8 min diamond (1 Lm), 30 s etch, 10 min diamond (0.25 Lm),
10 s etch, polishing with alumina slurry No. 3 (0.05 Lm, Linde B), 5 sec etch.
c. Electrolytic:
lOO mI 40-50 s, 60 V dc, Pt or
1. Dist. water
Zn cathode.
20 g
Chromium (VI) oxide
!!! See Appendix A.
l h and longer, 4-6 V dc,
50 mI
50 mI stainless steel cathode.
Ethanol (96%)
!!! See Appendix A.
d. Chemical:
lOO mi Up to 30 mino
Dist. water
Layer of reaction products
5 mi
Nitric acid (1.40)
is water soluble.'
I.5g
Sodium sulfate
!!! See Appendix A.
20 g
Chromium (VI) oxide
Etching:
Zinc is suitable for observation in polarized light.
Conditions
Etchant
No.
Zn
mi
Dist. water
Chromium (VI) oxide
Sodium sulfate
Zn
m2
Dist. water, ethanol,

methanol, or amyl
alcohol (95%)
Nitric acid (1.40)
50 mI
~.
Microetching
Preparation:
See recommendations for macroetching.
Grinding:
a. Wet on silicon carbide papers down to 600 grit (coat papers with wax).
~
,~l
89
b. Prepare by microtome using cemented carbide blade or diamond blade; eliminates

polishing.
Zn alloys containing
Cu. Dilute with lOO mI
20 g If using sodium sulfate containing crystal water if used as microetchant.
I.5g water (Na2 S04
IOH2 0) increase to
3.5 g.
!!! See Appendix A.
lOO mi 2-3 mino

20 g For alloys containing
l.5g Cu, use half the
amount of sodium sulfate.
Rinse in:
lOO mi disto water
20 g chromium (VI)
oxide
!!! See Appendix A.
Secs to mins.
Etching solution
lOO mi should not be older
0.5-1 mi than I h. To avoid
stains, rinse specimen
in aqueous sol. of
chromic acid (20%)
after etching
Remarks
F or most types of Zn
and Zn alloys. Especially for rolled Zn
containing Pb and
Zn-Cu alloys.
If chromium (VI)
oxide content is
lowered to 5 g and the
sodium sulfate to 0.5
g, etchant can be used
f or pressure-cast
parts, and Zn platings.
Zn-Fe layers of galvanized steel or ferrous materials.
Zn-AI and Zn-Cr
alloys.
Grain boundaries.
90
Zn
m3
Dist. water
Sodium hydroxide
Zn
m4
Zn
m5
Preparation 01 Zn
Aqueous sol. of sodium thiosulfate

Potassium metabisul-fite
Dist. water or
ethanol (96%)
Hydrochloric acid
(1.19)
Possibly increase
water content
100 mI 1-5 s.
10 g
50 mi 30 s.
Ig
Secs to mins.
100 mi
1-5 mi
Dist. water
Ethanol (96%)
Picric acid
Zn
m7
Dist. water
Hydrochloric acid
(1.19)
Iron (111) chloride
Dist. water
Saturated sol. of copper (11) nitrate
Potassium hydroxide
Potassium cyanide
Citric acid
(Schramm's reagent)

Let precipitating crys60 mi tals settle.
75 g
6.5 g
Fe, Pb, Mg, Cu, and

Ni-Zn alloys. Zn-rich
phase dark.
AIso suited as macroetchant.

Ig
II g
Fiber structure in extruded Zn alloys.
100 mi 15 min, 6 V dc, Cu

25 g cathode.
Pure and low-alloy

Zn.
Zn
m9
Dist. water
Citric acid
Ammonium persulfate
Zn Electrolytic:
mIO Dist. water
I
Sodium hydroxid~
Zn Electrolytic:
t
mIl Dist. wate~

Chromium '(VI) oxide
:....
70 mi. Secs to mins.

30 mI
0.3 g
30 mi
4g
Zn alloys with metals

of the iron group.
Zn platings.
Zn alloys with much

nobler constituents,
for example, Cu, Ag,
Au.
100 mI Secs to mins, 12 V dc, Zn-Cu alloys to distin10 g Pt cathode.

guish between gamma
!!! See Appendix A.
and epsilon phase.
.~
.n I
~ .:10
Chapter 3:
Preparation of Special Ceramics and

Cermets (Ceramography)
Zn and Zn-rich alloys.

Zn-Cu-AI alIoys.
Zn
m6
Zn
mS
Technically pure Zn.

Zn-Co and Zn-Cu
alIoys.
GeneralIy for lowalloy Zn.
Tint etching of Zn and
10w-alIoy Zn.
Most engineering ceramics and cermets are examined by reflected-light

microscopy. Silicate ceramics, however, are more frequently examined
as thin sections, using transmitted-light microscopy. Preparing suitable
specimens requires certain deviations from the usual metallographic
procedure (refer to Chapters 1 and 2), thereby creating the expression
"ceramography. "
Porosity and plucking are the greatest problems in preparing ceramics.
The hardness differential between the ceramic and metallic components
is the major problem when preparing cermets. Macroscopic examinations
of special ceramics and cermets is normally not neccessary. In any
case, the preparation methods for macroscopic investigations are idtmtical
to those for microscopic observations.
Ceramics are often porous and contain cracks and therefore should
be impregnated with a resin to preserve the specimen (refer to Chapter
1). Toxic mat,erials such as beryIlium oxide, uranium compounds, and
plutonium compounds should be handled carefully according to precautions in Appendix A. The need for these precautions is indicated by
the (!!!) notation.
Preparation:
Grinding:
a. Wet on silicon carbide papers down lo 320 grit or 600 grit.
b. Beginning with grit size 320, fine grinding on diamond wheels.
c. Lapping with silicon carbide slurries of particle size 7-1 .tm on a cast iron wheel.
Polishing:
a. With diamond paste of particle size 15-1 .tm for one to two days or longer on automatic
polishers (for example, vibrating polishers).
b. With diamond paste of particle size 6-1 .tm on a fast-rotating hardwood wheel.
c. With diamond paste of partcle size 6-1 .tm with a stick of rosewood of approx 15
mm diameter in a hand drill machine. Fast polishing action. Polished surface area
is equal to diameter ofwood stick and is not flat. Wood stck should not touch embedding
material (smearing).
d. With alumina slurry No. I (5 .tm) and No. IC (1 .tm, Linde C) on a fast-rotating
wheel covered with strong, smooth felt.
e. Alumina slurry (0.05 .tm; 30 g in 140 mi hydrogen peroxide, 3%) on a fast-rotating
91
90
Zn
m3
Dist. water
Sodium hydroxide
Zn
m4
Zn
m5
Preparation 01 Zn
Aqueous sol. of sodium thiosulfate

Potassium metabisul-fite
Dist. water or
ethanol (96%)
Hydrochloric acid
(1.19)
Possibly increase
water content
100 mI 1-5 s.
10 g
50 mi 30 s.
Ig
Secs to mins.
100 mi
1-5 mi
Dist. water
Ethanol (96%)
Picric acid
Zn
m7
Dist. water
Hydrochloric acid
(1.19)
Iron (111) chloride
Dist. water
Saturated sol. of copper (11) nitrate
Potassium hydroxide
Potassium cyanide
Citric acid
(Schramm's reagent)

Let precipitating crys60 mi tals settle.
75 g
6.5 g
Fe, Pb, Mg, Cu, and

Ni-Zn alloys. Zn-rich
phase dark.
AIso suited as macroetchant.

Ig
II g
Fiber structure in extruded Zn alloys.
100 mi 15 min, 6 V dc, Cu

25 g cathode.
Pure and low-alloy

Zn.
Zn
m9
Dist. water
Citric acid
Ammonium persulfate
Zn Electrolytic:
mIO Dist. water
I
Sodium hydroxid~
Zn Electrolytic:
t
mIl Dist. wate~

Chromium '(VI) oxide
:....
70 mi. Secs to mins.

30 mI
0.3 g
30 mi
4g
Zn alloys with metals

of the iron group.
Zn platings.
Zn alloys with much

nobler constituents,
for example, Cu, Ag,
Au.
100 mI Secs to mins, 12 V dc, Zn-Cu alloys to distin10 g Pt cathode.

guish between gamma
!!! See Appendix A.
and epsilon phase.
.~
.n I
~ .:10
Chapter 3:
Preparation of Special Ceramics and

Cermets (Ceramography)
Zn and Zn-rich alloys.

Zn-Cu-AI alIoys.
Zn
m6
Zn
mS
Technically pure Zn.

Zn-Co and Zn-Cu
alIoys.
GeneralIy for lowalloy Zn.
Tint etching of Zn and
10w-alIoy Zn.
Most engineering ceramics and cermets are examined by reflected-light

microscopy. Silicate ceramics, however, are more frequently examined
as thin sections, using transmitted-light microscopy. Preparing suitable
specimens requires certain deviations from the usual metallographic
procedure (refer to Chapters 1 and 2), thereby creating the expression
"ceramography. "
Porosity and plucking are the greatest problems in preparing ceramics.
The hardness differential between the ceramic and metallic components
is the major problem when preparing cermets. Macroscopic examinations
of special ceramics and cermets is normally not neccessary. In any
case, the preparation methods for macroscopic investigations are idtmtical
to those for microscopic observations.
Ceramics are often porous and contain cracks and therefore should
be impregnated with a resin to preserve the specimen (refer to Chapter
1). Toxic mat,erials such as beryIlium oxide, uranium compounds, and
plutonium compounds should be handled carefully according to precautions in Appendix A. The need for these precautions is indicated by
the (!!!) notation.
Preparation:
Grinding:
a. Wet on silicon carbide papers down lo 320 grit or 600 grit.
b. Beginning with grit size 320, fine grinding on diamond wheels.
c. Lapping with silicon carbide slurries of particle size 7-1 .tm on a cast iron wheel.
Polishing:
a. With diamond paste of particle size 15-1 .tm for one to two days or longer on automatic
polishers (for example, vibrating polishers).
b. With diamond paste of particle size 6-1 .tm on a fast-rotating hardwood wheel.
c. With diamond paste of partcle size 6-1 .tm with a stick of rosewood of approx 15
mm diameter in a hand drill machine. Fast polishing action. Polished surface area
is equal to diameter ofwood stick and is not flat. Wood stck should not touch embedding
material (smearing).
d. With alumina slurry No. I (5 .tm) and No. IC (1 .tm, Linde C) on a fast-rotating
wheel covered with strong, smooth felt.
e. Alumina slurry (0.05 .tm; 30 g in 140 mi hydrogen peroxide, 3%) on a fast-rotating
91
92
/ Preparation of Oxides
Oxides
Etchant
Conditions
Rot etching in air
2h, 1100-1500 oC
(2000-2730 F), 4
mino
AI2 O,.
AI20,-MgO mixture.
SriO,.
O
m2
Rot etching in pure,

dry hydrogen
1-3 min, 700-1600

OC) (1300-2900 F)
500 torr, 3 min,
1200 oC (2200 F).
!!! See Appendix A.
AlzO,. BeO (!!!).

V0 2 (!!!).
Rot etching in dry

hydrogen
500 torr, 3-10 min,

1200 oC (2200 F)..
VO, (!!!).
O
m4
Rot etching in al :1
mixture of water
vapor and argon
2 h, 1250 oC (2300
F).
VO, (!!!).
Grain size.
O
m5
Thermal etching .
1 h,IO.torr, 1600 oC .
(2900 F).
O
m6
Potassium hydrogen
fluoride melt
5- lO min, molten salt

in Pt crucible.
!!! See Appendix A.
AI,O,. Al,SiOs'
Rinse sample in
phosphoric acid.
O
'm7
Potassium hydrogen
sulfate melt
3-10 min, molten salt

in Pt crucible.
15- 25 S.
!!! See Appendix A.
Cr,O,. CeO,.
AI,O,.
O
m8
Hydrochloric acid
(1.19)
3st06min
CaO, MgO.
O
m9
Os!. water
Hydrochloric acid
(1.19)
'l
2 s to 6 min.
!!! See Appendix A.
. VO, (!!!).
ThO, -Y2 0 , mixtures

(!!!)
BeO (!!!). Zr,O, ..
BaO, MgO.
Ca,Zr l , Oy.
lO(loo)ml 10-20 min, 60-80 oC

O
O~ . water
mIl Hydrofluoric acd
(140-180 P)
40%
.. , IlO(l)ml !!! See Appendix A.
A120, , SiO, .
BeO-VO,-Y2 0 , mixtures (!!!).
Ois!. water
O
ml2 Rydrochloric acid
(1.19)
Sato aqueous sol. of
copper (H) sulfate
Eu2 O, .
'1"
10 m! Secs to mins.
Boiling.
10m!
~.
10 mI 5 S .
10m!
10m!
I_r
Phosphoric acia
O
m13 (1.71)
1- 30 mino
Boiling.
"
''
1li
m14
Oist. water
Phosphoric acid
(1.71)
Oist. water
miS Nitric acid (1.40)
O
m16
Dist . .water
O
ml7 Sulfuric acid (1.84)
O
m3
O
Hydrofluoric aci.,d
mIO (40%)
.
"
Remarks
O
mI
I
>,
~:.''"
93
1"
"
wheel covered by moistened velvet or felt. Finish with high pressure. Clean sample
under running water inimediately after polishing.
f. With electrically conductive ceramics (for example, carbides), electrolytic polishing
is possible. The etchants listed below are often suitable for electrolytic polishing.
Polishing times are six to ten times the 'etching time.
No.
.'
Preparation of Oxides
Oist. water
O
m18 Glacial acetic acid
(1.84)
Hydrofluoric acid
O
ml9 (40%)
Nitric acid (1.40)
(Concentration variab1e)
15 mi 5 min to 2 h.
Boiling.
85 mI
10(100) mI 3s to 5 min, room
10(15)ml tempe'rature to 60 oC
(140 F).
1 min to 2 h.
1-2 min, 60 OC (140F).
50(1O)m! 1-5 min, boiling.
50(1)ml 1-5 min, 30 oC (85 P).
lO sec, 30 oC (85 P).
MgO. Th02 (!!!).

Al,NiO., Pu0 2
(gamma, sintered)
(!!!).
yp,-ZrO, and
Srn,O,-ZrO, mixtures.
AI20,. Relief formation.
MgO, V0 2 (!!!).
AlzO" VO, (!!!).

ThO,(!!!),
AI,O,-MgO mixtures
ZrO z
V,08 (!!!).
Conceritration in parentheses for Nd,O,.
ZnO.
5m!
S- lO min, 60-80 oC
10(l) ml (140-180F).
50(30) mi !!! See Appendix A.
10 min, boiling.
30 s to 1 min, boiling.
20 (100) mI 5-15 min.

Oist. water
O
20(90)m! !!! See Appendix A.
m20 Nitric acid (1.40)
Rydrofluoric acid
1O(10)rn1
(40%)
7 min to 2 h.
Rydrochloric acid
O
m21 (1.19)
Rydrofluoric acid
3 mI
(40%)
1-11 min
Rydrogen
peroxide
O
1 (10) mI
m22 .(30%)
10(1) m!
9 mi Secs to mins.
Oist. water
O
1 mI
Rydrogen peroxide
2m!
(30%)
15-70 sec
aqueous
sol.
of
Sato
O
m24 sodium sulfide
VO, (!!!). Th,VP2

(!!!).
PuO" cast (!!!).

PuO, (gamma, sintered) (!!!)
CeO" SrTiO, . AI,O, .
ZrO-ZrC mixtures.
BaTiO, . BaTi,07'
VO,. VO,-PuF,.
VO,-V.O. and V0 2CeO, mixtures (!!!).
V.o. (!!!).
CaO.
92
/ Preparation of Oxides
Oxides
Etchant
Conditions
Rot etching in air
2h, 1100-1500 oC
(2000-2730 F), 4
mino
AI2 O,.
AI20,-MgO mixture.
SriO,.
O
m2
Rot etching in pure,

dry hydrogen
1-3 min, 700-1600

OC) (1300-2900 F)
500 torr, 3 min,
1200 oC (2200 F).
!!! See Appendix A.
AlzO,. BeO (!!!).

V0 2 (!!!).
Rot etching in dry

hydrogen
500 torr, 3-10 min,

1200 oC (2200 F)..
VO, (!!!).
O
m4
Rot etching in al :1
mixture of water
vapor and argon
2 h, 1250 oC (2300
F).
VO, (!!!).
Grain size.
O
m5
Thermal etching .
1 h,IO.torr, 1600 oC .
(2900 F).
O
m6
Potassium hydrogen
fluoride melt
5- lO min, molten salt

in Pt crucible.
!!! See Appendix A.
AI,O,. Al,SiOs'
Rinse sample in
phosphoric acid.
O
'm7
Potassium hydrogen
sulfate melt
3-10 min, molten salt

in Pt crucible.
15- 25 S.
!!! See Appendix A.
Cr,O,. CeO,.
AI,O,.
O
m8
Hydrochloric acid
(1.19)
3st06min
CaO, MgO.
O
m9
Os!. water
Hydrochloric acid
(1.19)
'l
2 s to 6 min.
!!! See Appendix A.
. VO, (!!!).
ThO, -Y2 0 , mixtures

(!!!)
BeO (!!!). Zr,O, ..
BaO, MgO.
Ca,Zr l , Oy.
lO(loo)ml 10-20 min, 60-80 oC

O
O~ . water
mIl Hydrofluoric acd
(140-180 P)
40%
.. , IlO(l)ml !!! See Appendix A.
A120, , SiO, .
BeO-VO,-Y2 0 , mixtures (!!!).
Ois!. water
O
ml2 Rydrochloric acid
(1.19)
Sato aqueous sol. of
copper (H) sulfate
Eu2 O, .
'1"
10 m! Secs to mins.
Boiling.
10m!
~.
10 mI 5 S .
10m!
10m!
I_r
Phosphoric acia
O
m13 (1.71)
1- 30 mino
Boiling.
"
''
1li
m14
Oist. water
Phosphoric acid
(1.71)
Oist. water
miS Nitric acid (1.40)
O
m16
Dist . .water
O
ml7 Sulfuric acid (1.84)
O
m3
O
Hydrofluoric aci.,d
mIO (40%)
.
"
Remarks
O
mI
I
>,
~:.''"
93
1"
"
wheel covered by moistened velvet or felt. Finish with high pressure. Clean sample
under running water inimediately after polishing.
f. With electrically conductive ceramics (for example, carbides), electrolytic polishing
is possible. The etchants listed below are often suitable for electrolytic polishing.
Polishing times are six to ten times the 'etching time.
No.
.'
Oist. water
O
m18 Glacial acetic acid
(1.84)
Hydrofluoric acid
O
ml9 (40%)
Nitric acid (1.40)
(Concentration variab1e)
15 mi 5 min to 2 h.
Boiling.
85 mI
10(100) mI 3s to 5 min, room
10(15)ml tempe'rature to 60 oC
(140 F).
1 min to 2 h.
1-2 min, 60 OC (140F).
50(1O)m! 1-5 min, boiling.
50(1)ml 1-5 min, 30 oC (85 P).
lO sec, 30 oC (85 P).
MgO. Th02 (!!!).

Al,NiO., Pu0 2
(gamma, sintered)
(!!!).
yp,-ZrO, and
Srn,O,-ZrO, mixtures.
AI20,. Relief formation.
MgO, V0 2 (!!!).
AlzO" VO, (!!!).

ThO,(!!!),
AI,O,-MgO mixtures
ZrO z
V,08 (!!!).
Conceritration in parentheses for Nd,O,.
ZnO.
5m!
S- lO min, 60-80 oC
10(l) ml (140-180F).
50(30) mi !!! See Appendix A.
10 min, boiling.
30 s to 1 min, boiling.
20 (100) mI 5-15 min.

Oist. water
O
20(90)m! !!! See Appendix A.
Rydrofluoric acid
1O(10)rn1
(40%)
7 min to 2 h.
Rydrochloric acid
O
m21 (1.19)
Rydrofluoric acid
3 mI
(40%)
1-11 min
Rydrogen
peroxide
O
1 (10) mI
m22 .(30%)
10(1) m!
9 mi Secs to mins.
Oist. water
O
1 mI
Rydrogen peroxide
2m!
(30%)
15-70 sec
aqueous
sol.
of
Sato
O
m24 sodium sulfide
VO, (!!!). Th,VP2

(!!!).
PuO" cast (!!!).

PuO, (gamma, sintered) (!!!)
CeO" SrTiO, . AI,O, .
ZrO-ZrC mixtures.
BaTiO, . BaTi,07'
VO,. VO,-PuF,.
VO,-V.O. and V0 2CeO, mixtures (!!!).
V.o. (!!!).
CaO.
94
100 mI 3- 5 min, 60 oC
(140 F).
25-50 g Prewarm sample in
water.
Dist. water
O
m25 Ammonium hydrogen fluoride
Lactic acid (90%)
O
Hydrofluorie aeid
(40%)
15 mi 65 oC (150 F) .
!!! See Appendix A.
5 ml
Dist. water
O
m27 Nitrie aeid (1.40)
Hydrofluorie aeid
(40%)
Cerium (IV) nitrate
80 mi Secs to mins ,
100 mI 1 mino
!!! See Appendix A.
3 mI
15 mI
10 mi
20 mi
Ig
O
Elllctrolytic:
m30 Dist. water
Cone. aqueous oxalie
acid
Cone. aqueous eitrie
aeid
Laetie aeid (90%)
Ethanol (96%)
Phosphoric aeid
(1.71)
Hydrofluorie acid
(40%)
Glacial aeetie ~eid
""..
No.
10-15 V de, I
Ajcm2, stainless
steel eathode .
60-90 s (eteh).
30-50 s (polish).
!!! See Appendix A.
35 mi 3 s to 6 min, 17- 20
V de, stainless 'steel
30 mi eathode.
!!! See Appendix A.
30 mi
10 mi
60 mi
U02 -PU02 mixtures

(!!!).
MgO-AI, 0 3-SiO, Zr02 mixtures.
U0 2 (!!!).
Hydrogen sulfide
C
m4
Thermal etching
C
m5
Sodium or potassium
bcarbonate melt
!!! See Appendix A.
C
m6
Sodium tetraborate
melt
Few mins.
!!! See Appendix A.
C
m7
Nitrie acid (1.40)
Sees to mins.
C
m8
Dist. water
Nitrie acid (1.40)
C
m9
Nitrie aeid (1.40)

Hydrofluorie aeid
(40%)
10(30) mI Sees to mins.

!!! See Appendix A.
10 (10) mi
Dist. water
C
mIO Nitrie acid (1.40)
Hydrofluorie acid
(40%)
10 mi Secs to mins.
10 mI GlyeeroI instead of
disto water.
cre, HCC .
Hydrofluoric acid
C
mll (40%)
Nitrie aeid (1.40)
Lactie acid (90%)
Secs to mins.
10 mi !!! See Appendix A .
10 mi
20 mi
Ta(C,N,O).
60-70 mi 30-45 s, 2-4

mA/em2 ,
I
'.
6-12 V de, stainless
25 mi steel eathode
~
" l.
Etehant
Conditions
. ....
Air
Dry, high-purity argon
~-
_ t
Carbides
Remarks
10 min to 24 h, 20- 25
oC (70-80 0F).
ThC (!!!).
20min to 24 h, 20-25
oC (70-80 0 F).
Th02 (!!!).
I
:
'~ '.
\\;
95
KC.
3
:$ 10- torr, 1200 oC
(2200 F).
SiC.
10 min, molten salt.
SiC.
SiC.
UC-Cr23 C6 mixtures
(!!!).
lO mi Secs to mins .
10 mi
1-45 min o
10 mi Sees to mins.
10 mi
10 mi
Swab.
Few drops oC oxalic
aeid or hydrofluorie
aeid (40%).
!!! See Appendix: A .
NiO.
!!! See Appendix A.
Dist. water
C
ml2 Nitrie acid (1.40)
Glacial acetic acid
Nb oxides .
NbO (blue), Nb0 2
(eyan), Nb2 0 S (reddish-brown).
12-30 s.
C
m3
5 mi
C
mi
m2
BeO (! !!).
0.5 mi
Electrolytic:
O
m29 Dist. water
Glacial aeetie acid
Chromium (VI) oxide
Electrolytic:
O
m31 Dist. water
BeO (!!!).
3 drops
1g
MethanoI (95 %)
O
rD28 Hydroehlorie acid
(1.l9)
Hydrofluorie acid
(40%)
{I
Preparation of Carbides
(Th,U)C (!!!) with

U jTh ratio < 3.
ThC2 (!!!).
(Fe,Si)C. Coneentration in parentheses for
TaC.
VC, (Al, Ti)C.
UC, U(C,O), UCUC UC,-U2C3

"
mixtures.
(U,Pu)C high in C.
U(C,N), UC-ZrC mixtures (!!!).
Dist. water
C.
m 13 Nitrie acid (1.40)
Hydroehlorie aeid
(1.l9)
25 mi Sees to mins.
25 mi
Nitrie acid (1.40)

C
ml4 Hydroehlorie acid
(1.19)
Sulfurie aeid (1.84)
10 mi Sees to mins.
Hydrofluorie aeid
10 mi (40%) can be used in10 mi stead of hydroehlorie
acid.
TaC.
Secs to mins .
Wc.
C
Hydrochlorie aeid
mI5 (1.19)
Hydrogen peroxide
(30%)
Dist. water
C
ml6 Formie aeid (1.22)
ThC (!!!).
Iml
10 mi
10 mi
10 mi 4
10 mi
S.
UC-Pu mixtures (!!!).
94
100 mI 3- 5 min, 60 oC
(140 F).
25-50 g Prewarm sample in
water.
Dist. water
O
m25 Ammonium hydrogen fluoride
Lactic acid (90%)
O
Hydrofluorie aeid
(40%)
15 mi 65 oC (150 F) .
!!! See Appendix A.
5 ml
Dist. water
O
m27 Nitrie aeid (1.40)
Hydrofluorie aeid
(40%)
Cerium (IV) nitrate
80 mi Secs to mins ,
100 mI 1 mino
!!! See Appendix A.
3 mI
15 mI
10 mi
20 mi
Ig
O
Elllctrolytic:
m30 Dist. water
Cone. aqueous oxalie
acid
Cone. aqueous eitrie
aeid
Laetie aeid (90%)
Ethanol (96%)
Phosphoric aeid
(1.71)
Hydrofluorie acid
(40%)
Glacial aeetie ~eid
""..
No.
10-15 V de, I
Ajcm2, stainless
steel eathode .
60-90 s (eteh).
30-50 s (polish).
!!! See Appendix A.
35 mi 3 s to 6 min, 17- 20
V de, stainless 'steel
30 mi eathode.
!!! See Appendix A.
30 mi
10 mi
60 mi
U02 -PU02 mixtures

(!!!).
MgO-AI, 0 3-SiO, Zr02 mixtures.
U0 2 (!!!).
Hydrogen sulfide
C
m4
Thermal etching
C
m5
Sodium or potassium
bcarbonate melt
!!! See Appendix A.
C
m6
Sodium tetraborate
melt
Few mins.
!!! See Appendix A.
C
m7
Nitrie acid (1.40)
Sees to mins.
C
m8
Dist. water
Nitrie acid (1.40)
C
m9
Nitrie aeid (1.40)

Hydrofluorie aeid
(40%)
10(30) mI Sees to mins.

!!! See Appendix A.
10 (10) mi
Dist. water
C
mIO Nitrie acid (1.40)
Hydrofluorie acid
(40%)
10 mi Secs to mins.
10 mI GlyeeroI instead of
disto water.
cre, HCC .
Hydrofluoric acid
C
mll (40%)
Nitrie aeid (1.40)
Lactie acid (90%)
Secs to mins.
10 mi !!! See Appendix A .
10 mi
20 mi
Ta(C,N,O).
60-70 mi 30-45 s, 2-4

mA/em2 ,
I
'.
6-12 V de, stainless
25 mi steel eathode
~
" l.
Etehant
Conditions
. ....
Air
Dry, high-purity argon
~-
_ t
Carbides
Remarks
10 min to 24 h, 20- 25
oC (70-80 0F).
ThC (!!!).
20min to 24 h, 20-25
oC (70-80 0 F).
Th02 (!!!).
I
:
'~ '.
\\;
95
KC.
3
:$ 10- torr, 1200 oC
(2200 F).
SiC.
10 min, molten salt.
SiC.
SiC.
UC-Cr23 C6 mixtures
(!!!).
lO mi Secs to mins .
10 mi
1-45 min o
10 mi Sees to mins.
10 mi
10 mi
Swab.
Few drops oC oxalic
aeid or hydrofluorie
aeid (40%).
NiO.
!!! See Appendix A.
Dist. water
C
ml2 Nitrie acid (1.40)
Glacial acetic acid
Nb oxides .
NbO (blue), Nb0 2
(eyan), Nb2 0 S (reddish-brown).
12-30 s.
C
m3
5 mi
C
mi
m2
BeO (! !!).
0.5 mi
Electrolytic:
O
m29 Dist. water
Glacial aeetie acid
Chromium (VI) oxide
Electrolytic:
O
m31 Dist. water
BeO (!!!).
3 drops
1g
MethanoI (95 %)
O
rD28 Hydroehlorie acid
(1.l9)
Hydrofluorie acid
(40%)
{I
Preparation of Carbides
(Th,U)C (!!!) with

U jTh ratio < 3.
ThC2 (!!!).
(Fe,Si)C. Coneentration in parentheses for
TaC.
VC, (Al, Ti)C.
UC, U(C,O), UCUC UC,-U2C3

"
mixtures.
(U,Pu)C high in C.
U(C,N), UC-ZrC mixtures (!!!).
Dist. water
C.
m 13 Nitrie acid (1.40)
Hydroehlorie aeid
(1.l9)
25 mi Sees to mins.
25 mi
Nitrie acid (1.40)

C
ml4 Hydroehlorie acid
(1.19)
10 mi Sees to mins.
Hydrofluorie aeid
10 mi (40%) can be used in10 mi stead of hydroehlorie
acid.
TaC.
Secs to mins .
Wc.
C
Hydrochlorie aeid
mI5 (1.19)
Hydrogen peroxide
(30%)
Dist. water
C
ml6 Formie aeid (1.22)
ThC (!!!).
Iml
10 mi
10 mi
10 mi 4
10 mi
S.
UC-Pu mixtures (!!!).
96
P'.patal;o. o. Ca,b;d.,
C
m 17
C
ml8
Glacial acetic acid .

Ethanol (96%)
C
Dis!. water
ml9 SodiUIn hydroxide
C
E/ectro/ytic:
m20 Aqueous sol. (8%) of
sodium hydroxide
Sulfuric acid (1 84)
Copper (11) sulfate
'C
E/ectrolytic:
m21 Same as C ml2
C
E/ectrolytic:
m22 Same as C m17
.l
10 mi
10 mi
8 mi
5 mi
5 mi
100 mi
10 mi
10 g
8-10 min
(Th,U)C 2 (!!!).
5.,.60 s.
Swab.
n! See Appendix A.
2- 20 min, 50 oC
(120 0 P).
!!! See Appendix A.
(U,Pu)C (!!!).
. Up to 50 s, 80
mAlcm2 , stainless
steel cathode.
3-5 s, 5-7 V, dc,

C
E/ectro/ytic:
m24 Lactic acid (90%)
o
Nitric acid(1.40)
Hydrofluoric acid
(40%)
50 m1 S
.
ecsto mms.
30 mi 20-25 "C (70-80 0F),
17-20 V dc, stain8 mi less steel cathode.
!!! See Appendix A.
C
Electro/y tic:
m25 Dist. water
Potassium hydroxide
,
:'
. .t
.
C
'~ectrolytlc:
" \.
m26 DIst.. water..
GlacIal. acetlc aCld. .
ChromlUm (VI) OXIde'
C
Electroly lic:
'" :'
m27 Dist. water
Butyl glycol
~~I
p.uC (dend")
ntIc (",)
... .
tio. of NII,ld..
NItndes
l.
No.
Etchant
Conditions
Remarks
N
Hot etching in dry
5 h, 1600 oc (2900 P). Si3N.
mi high-purity
Variable.
___
nt_tr_o.:::g:.-en_ _ _ _~_ _ _ _ _ _ _ _ _ _ _ _ _ _ __
N
Hot etching in dry
3 h, 1650 oC (3000 P). UN (!!!).
m2 high-purity
!!! See ~ppendix A.
_ _-,hy:...d_r~o:::.ge_n_
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
N
m3
N
m4
N
m5
N
m6
ThC2 (!!!).
.......
m7
N
m8
(U,Pu)C highin U.
UC-PuN mixtures
(!!!).
NbC , NbC'2'
N
m9
Thermal etching
-18 h, 1650 oC (3000 P)

:S 10-5 torr
. "
PotasslUm carbonate
95.4 g 1-4 mm, molten salto
Sodium fluoride
5-1.5. min.
BoIlmg.
Hydrofluoric acid
10-15 mino
(40%)
!!! See Appendix A.
Dist. water
10 mi Secs to mins.
Glacial acetic acid
10 mi
Nitric acid (1.40)
10 mi
Lactic acid (90%)
10 mi 30 s to I mino
Nitric acid (1.40)
10 mi After etching Cor 30 s,
add 7 drops oC hydrofluoric acid (40%).
!!! See Appendix A.
3 ~in, 40 oC (100 o~
wlthout hydrofluoflc
ac'd
I .
Dist. water
60 mi 30 s, lO oC (50 P).
Glacial acetic acid
Chromium (VI) oxide
50 g
E/eclrolytic:
mIO Sulfuric acid (1.84)
Glycerol
N
Electrolytic:
mil Glacial acetic acid
Chromium (VI) oxide
UN (!!!).
SI3N.
Si3N. UN (!!!).
Si3 N.
(AI,Ti)N.
UN, UN-U 2N)

tures (!!!).
ffiX-
U~-U(N2?{-U2N3
mIXtures ( ... )
UN (!!!).
PotasslUm hY~,roXlde .
.'\
..
N
I min, 30-35 V, dc,
C
E/ectro/ytic:
m23 Sato aqueous sol. of
arnmonium acetate
30 s, 25 oC (80 P), 3.5 TiC.

80 mi V dc, 0.9 Alcm1 ,
80 mi Cu cathode.
10 l
10 :
. .
MoC , CrC
10 mi 2-30 s, 2 V dc, 302 g 60 mAlcm2 Pt cathode. Move specimen.

20 ~, 6 V dc, I Al
cm .
2
0.1 g 40 ':1 dc, 3 Al cm ,
7 mi I min, 20 V dc, stain133 mi less steel cathode.
TiC, TaC.
.
SIC.
B,C.
PuC (!!!).
I mi 20-40 s, 5-10 V de,

(U,Pu)C high in Pu
6 mi 10-15 mAlcm2 ,
(!!!).
3 mi stainless steel cathode.
Electrolytic:
ml2 Dist. water
Ethanol (96%)
oxalic acid
Sat. aqueous sol. oC
citric acid
Lactic acid (90%)
10 mi 3-10 s, 4 V dc, stain30 mi less steel cathode.

30 nIi !!! See Appendix A.
UN (!!!).
18 mi 4 s, 40 V dc, stainI g less steel cathode.

!!! See Appendix A.
UN-U2 N) mixtures
35 mi Secs to mins.
60 mi 17-20 V dc, stainless steel cathode.
NbN (yeUow).
Nb2N (light red).
(!!!).
3 mi
lO mi
5 mi
'TI
96
P'.patal;o. o. Ca,b;d.,
C
m 17
C
ml8
Glacial acetic acid .

Ethanol (96%)
C
Dis!. water
ml9 SodiUIn hydroxide
C
E/ectro/ytic:
m20 Aqueous sol. (8%) of
sodium hydroxide
Sulfuric acid (1 84)
Copper (11) sulfate
'C
E/ectrolytic:
m21 Same as C ml2
C
E/ectrolytic:
m22 Same as C m17
.l
10 mi
10 mi
8 mi
5 mi
5 mi
100 mi
10 mi
10 g
8-10 min
(Th,U)C 2 (!!!).
5.,.60 s.
Swab.
n! See Appendix A.
2- 20 min, 50 oC
(120 0 P).
!!! See Appendix A.
(U,Pu)C (!!!).
. Up to 50 s, 80
mAlcm2 , stainless
steel cathode.
3-5 s, 5-7 V, dc,

C
E/ectro/ytic:
m24 Lactic acid (90%)
o
Nitric acid(1.40)
Hydrofluoric acid
(40%)
50 m1 S
.
ecsto mms.
30 mi 20-25 "C (70-80 0F),
17-20 V dc, stain8 mi less steel cathode.
!!! See Appendix A.
C
Electro/y tic:
m25 Dist. water
Potassium hydroxide
,
:'
. .t
.
C
'~ectrolytlc:
" \.
m26 DIst.. water..
GlacIal. acetlc aCld. .
ChromlUm (VI) OXIde'
C
Electroly lic:
'" :'
m27 Dist. water
Butyl glycol
~~I
p.uC (dend")
ntIc (",)
... .
tio. of NII,ld..
NItndes
l.
No.
Etchant
Conditions
Remarks
N
Hot etching in dry
5 h, 1600 oc (2900 P). Si3N.
mi high-purity
Variable.
___
nt_tr_o.:::g:.-en_ _ _ _~_ _ _ _ _ _ _ _ _ _ _ _ _ _ __
N
Hot etching in dry
3 h, 1650 oC (3000 P). UN (!!!).
m2 high-purity
!!! See ~ppendix A.
_ _-,hy:...d_r~o:::.ge_n_
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ __
N
m3
N
m4
N
m5
N
m6
ThC2 (!!!).
.......
m7
N
m8
(U,Pu)C highin U.
UC-PuN mixtures
(!!!).
NbC , NbC'2'
N
m9
Thermal etching
-18 h, 1650 oC (3000 P)

:S 10-5 torr
. "
PotasslUm carbonate
95.4 g 1-4 mm, molten salto
Sodium fluoride
5-1.5. min.
BoIlmg.
Hydrofluoric acid
10-15 mino
(40%)
!!! See Appendix A.
Dist. water
10 mi Secs to mins.
Glacial acetic acid
10 mi
Nitric acid (1.40)
10 mi
Lactic acid (90%)
10 mi 30 s to I mino
Nitric acid (1.40)
10 mi After etching Cor 30 s,
add 7 drops oC hydrofluoric acid (40%).
!!! See Appendix A.
3 ~in, 40 oC (100 o~
wlthout hydrofluoflc
ac'd
I .
Dist. water
60 mi 30 s, lO oC (50 P).
Glacial acetic acid
Chromium (VI) oxide
50 g
E/eclrolytic:
mIO Sulfuric acid (1.84)
Glycerol
N
Electrolytic:
mil Glacial acetic acid
Chromium (VI) oxide
UN (!!!).
SI3N.
Si3N. UN (!!!).
Si3 N.
(AI,Ti)N.
UN, UN-U 2N)

tures (!!!).
ffiX-
U~-U(N2?{-U2N3
mIXtures ( ... )
UN (!!!).
PotasslUm hY~,roXlde .
.'\
..
N
I min, 30-35 V, dc,
C
E/ectro/ytic:
m23 Sato aqueous sol. of
arnmonium acetate
30 s, 25 oC (80 P), 3.5 TiC.

80 mi V dc, 0.9 Alcm1 ,
80 mi Cu cathode.
10 l
10 :
. .
MoC , CrC
10 mi 2-30 s, 2 V dc, 302 g 60 mAlcm2 Pt cathode. Move specimen.

20 ~, 6 V dc, I Al
cm .
2
0.1 g 40 ':1 dc, 3 Al cm ,
7 mi I min, 20 V dc, stain133 mi less steel cathode.
TiC, TaC.
.
SIC.
B,C.
PuC (!!!).
I mi 20-40 s, 5-10 V de,

(U,Pu)C high in Pu
6 mi 10-15 mAlcm2 ,
(!!!).
3 mi stainless steel cathode.
Electrolytic:
ml2 Dist. water
Ethanol (96%)
oxalic acid
Sat. aqueous sol. oC
citric acid
Lactic acid (90%)
10 mi 3-10 s, 4 V dc, stain30 mi less steel cathode.

30 nIi !!! See Appendix A.
UN (!!!).
18 mi 4 s, 40 V dc, stainI g less steel cathode.

!!! See Appendix A.
UN-U2 N) mixtures
35 mi Secs to mins.
60 mi 17-20 V dc, stainless steel cathode.
NbN (yeUow).
Nb2N (light red).
(!!!).
3 mi
lO mi
5 mi
'TI
98
l'
/ Preparation of Borides, Phosphides and Sulfides
"
Borides
No .
Etehant
Conditions
Remarks
B
mi
Laetie aeid
Nitrie aed (1.40)
Hydrofluorie aeid
(40%) -
30 mi Sees to mins.
10 mI Instead .of laetic aeid,
lO mi glycerol can be
10 mi used.
ZrB2 TiB 2
B
m2
Hydrohlorie aeid
(1.19)
Nitrie aed (1.40)
1-5 min
10 mi 40 oC (lOO F), vapor
10 mi etehing.
CrB2 MoB 2
B
m3
Hydroehlorie aed
(1.19)
Nitrie aeid (1.40)
B
m4
Hydroehlorie aeid
(1.19)
Nitrie aed (1.40)
Hydrofluore aeid
(40%)
B
m5
Oist. water
Hydrofluorie aeid
(40%)
Nitrie aed (1.40)
10 mi Sees to mins.
!!! See Appendix A.
10 mi
10 mi
ZrB
B
m6
Oist. water
IOml 15
Iml
TiB 2
B
m7
Electrolytic:
Oist. water
Sodium hydroxide
15 s
9 s, 3{).4() oC (85-100
6 mi ~F) .
10 mI Sees to mins, 10-15

1-2 g V de, stainless steel
cathode.
HfB 2 -NbB 2 mixtures.
TaB 2 LaB .
P
mi
p
m2
,
t
Laetie aeid (90%)
(40~)
Nitrie aeid (1.40)

p
m3
Hydroehloric aed
(1.19)
Hydrogen peroxide
(30%)
m4
,;1
' '
"l,
'.,
lO mi Sees to mins.
10 mi
20 mi
. 20 mi
Secs to mins.
10 mI
I mi
Etehant
Conditions
Remarks
2.5 h, 1500 oC (2730

F).
!!! See Appendix A.
U02 -Mo (!!!).
el
m2
Hydrogen sulfide
15-30 s, room temperature.

!!! See Appendix A.
U0 2-Cr (!!!).
et
m3
a. Oist. water
b. Oist. water
Potassium or sodum
hydroxide
(Coneentration var- '
able)
et
m4
Nitrie aeid (1.40)
et
m5
Oist. water
Nitrie aed (1.40)
Hydrofluorie aed
(40%)
100 mi Mix (a) and (b) in

ratio 1: 1 before use.
IOg 1-4 mino
IOg
Sees to mins.
Zr0 2-W. Th0 2-W

(!!!).
W2C-W. UC-Cr (!!!).
UC-Fe (!!!). UC-Ni
(!!!).
UC-UFe2 (l!!).
Cr23 C.-UFe2 (!!!).

US-U (!!!). UC2-UN,
US (!!!).
50 (10) mi Sees to mins.

30(10)ml !!! See Appendix A.
10 (10) mi
TiN-Co, TiN-Fe.
TiN-Mo, TiN-W.
eoneentrations in parentheses for HfCHf.
et
m6
Oist. water
Nitrie aeid (1.40)
Glacial aeetie aeid
US-Co, UC2 -Fe,

lO mI Sees to mins.
lO mI Possibly several
(UZr)C-Nb, (UZr)C10 mi drops oC hydrofluorie Ta, (UZr)C-W (!!!) .
aeid (40%)
!!! See Appendix A.
et
m7
Nitrie aeid (1.40)

Hydrofluorie aeid
(40%)
lO mi Sees to mins.
et
m8
Ois!. water
Nitrie aed (1.40)
Hydroehlorie aeid
(1 .19)
50 mI Sees to mins.
47 mi
et
m9
Hydrofluorie aeid
(40%)
Nitrie acid (1.40)
Laetie aed (90%)
1-5 mino
50 mi
3 mI
UO (!!!).
6-12 S .
CdS.
Boiling, vapor etehing.
't_. , ''''
PbS.
Hot etehing in dry,

high-purity
hydrogen
Remarks
PuP (!!!), PuS (!!!).
Oist. water
Hydrofluorie aeid
99
(!!!).
eonditions
Sees to mins.
30 mi 1- 10 min, 60 oC
(140 F)
10 mi
Ig
Ct
mi
Etehant
Cermets
No.
Phosphides and SuJfides

No.
Oist. water
Hydroehlorie aed
(1.19)
Oimethylene thiourea
_,o
Iml
S.
p
m5
~;;'
TiB 2
100 mi
10 mi
Preparation of Cermets
, ..
:;
NbCz-NbFe-Nb.
10 mI
TiC-Ni.
3 mI
U02 -Nb (!!!).
98
l'
/ Preparation of Borides, Phosphides and Sulfides
"
Borides
No .
Etehant
Conditions
Remarks
B
mi
Laetie aeid
Nitrie aed (1.40)
Hydrofluorie aeid
(40%) -
30 mi Sees to mins.
10 mI Instead .of laetic aeid,
lO mi glycerol can be
10 mi used.
ZrB2 TiB 2
B
m2
Hydrohlorie aeid
(1.19)
Nitrie aed (1.40)
1-5 min
10 mi 40 oC (lOO F), vapor
10 mi etehing.
CrB2 MoB 2
B
m3
Hydroehlorie aed
(1.19)
Nitrie aeid (1.40)
B
m4
Hydroehlorie aeid
(1.19)
Nitrie aed (1.40)
Hydrofluore aeid
(40%)
B
m5
Oist. water
Hydrofluorie aeid
(40%)
Nitrie aed (1.40)
10 mi Sees to mins.
!!! See Appendix A.
10 mi
10 mi
ZrB
B
m6
Oist. water
IOml 15
Iml
TiB 2
B
m7
Electrolytic:
Oist. water
Sodium hydroxide
15 s
9 s, 3{).4() oC (85-100
6 mi ~F) .
10 mI Sees to mins, 10-15

1-2 g V de, stainless steel
cathode.
HfB 2 -NbB 2 mixtures.
TaB 2 LaB .
P
mi
p
m2
,
t
Laetie aeid (90%)
(40~)
Nitrie aeid (1.40)

p
m3
Hydroehloric aed
(1.19)
Hydrogen peroxide
(30%)
m4
,;1
' '
"l,
'.,
lO mi Sees to mins.
10 mi
20 mi
. 20 mi
Secs to mins.
10 mI
I mi
Etehant
Conditions
Remarks
2.5 h, 1500 oC (2730

F).
!!! See Appendix A.
U02 -Mo (!!!).
el
m2
Hydrogen sulfide
15-30 s, room temperature.

!!! See Appendix A.
U0 2-Cr (!!!).
et
m3
a. Oist. water
b. Oist. water
Potassium or sodum
hydroxide
(Coneentration var- '
able)
et
m4
Nitrie aeid (1.40)
et
m5
Oist. water
Nitrie aed (1.40)
Hydrofluorie aed
(40%)
100 mi Mix (a) and (b) in

ratio 1: 1 before use.
IOg 1-4 mino
IOg
Sees to mins.
Zr0 2-W. Th0 2-W

(!!!).
W2C-W. UC-Cr (!!!).
UC-Fe (!!!). UC-Ni
(!!!).
UC-UFe2 (l!!).
Cr23 C.-UFe2 (!!!).

US-U (!!!). UC2-UN,
US (!!!).
50 (10) mi Sees to mins.

30(10)ml !!! See Appendix A.
10 (10) mi
TiN-Co, TiN-Fe.
TiN-Mo, TiN-W.
eoneentrations in parentheses for HfCHf.
et
m6
Oist. water
Nitrie aeid (1.40)
Glacial aeetie aeid
US-Co, UC2 -Fe,

lO mI Sees to mins.
lO mI Possibly several
(UZr)C-Nb, (UZr)C10 mi drops oC hydrofluorie Ta, (UZr)C-W (!!!) .
aeid (40%)
!!! See Appendix A.
et
m7
Nitrie aeid (1.40)

Hydrofluorie aeid
(40%)
lO mi Sees to mins.
et
m8
Ois!. water
Nitrie aed (1.40)
Hydroehlorie aeid
(1 .19)
50 mI Sees to mins.
47 mi
et
m9
Hydrofluorie aeid
(40%)
Nitrie acid (1.40)
Laetie aed (90%)
1-5 mino
50 mi
3 mI
UO (!!!).
6-12 S .
CdS.
Boiling, vapor etehing.
't_. , ''''
PbS.
Hot etehing in dry,

high-purity
hydrogen
Remarks
PuP (!!!), PuS (!!!).
Oist. water
Hydrofluorie aeid
99
(!!!).
eonditions
Sees to mins.
30 mi 1- 10 min, 60 oC
(140 F)
10 mi
Ig
Ct
mi
Etehant
Cermets
No.
Phosphides and SuJfides

No.
Oist. water
Hydroehlorie aed
(1.19)
Oimethylene thiourea
_,o
Iml
S.
p
m5
~;;'
TiB 2
100 mi
10 mi
Preparation of Cermets
, ..
:;
NbCz-NbFe-Nb.
10 mI
TiC-Ni.
3 mI
U02 -Nb (!!!).
100
Preparation of lron Oxide Layers on Iron

Preparation of Iron Oxide Layers on Iron
Ct
mIO
Sulfunc acid (1.84)

Lactic acid (90%)
Glacial acetic acid
Ct a. Dist. water
mil
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
b. Dist. water
Nitric acid (1.40)
Ct
mI2
Lactic acid (90%)
Ct
m13
Hydrogen peroxide
(30%)
Ammonia water
10 mI Secs to mins.
10 mI
10 mI
100 mIlOs, 50 oC (120F).
!!! See Appendix A.
6 mI
2ml
PuC-Pu (!!!).
U02 -AI (!!!).
5ml
10 mI 3 min, 25 oC (80F).
10 mI Use (a) tirst, then
(b).
Secs to mins.
(Y3AI)C-Y3 C-Y.
Secs to mins.
UN-U, UN-W (!!!).
10m!.
10 mI
Iron Oxide Layers on Iron

No.
OFe
mI
Etchant
Dist. water
Aqueous sol.of nitric .
acid (1%)
Aqueous sol of citric
acid (5%)
Aqueous sol. of
thioglycolic acid (5%)
OFe
m2
Aqueous sol. of citric

acid (10%)
Aqueous sol. of sodium thiocyanate (10%)
OFe a. Dist. water
m3
Formic acid (1.22)
b. Dist. water
Fluoboric acid
OFe
m4
Conditions
10 mI 15-60 S.
Swab.
5ml
5ml
5 mI
45-90 S.
5 mI Swab.
5 mI
15 mI 5 S.
5 mI Swab, followed by
15 mI (b)' 2 S.
5ml
Thioglycolic aeid
(5%)
Aqueous sol. of po- I
tassium diphthalate " \.
(5%)
Aqueous sol. of ammonium citrate (5%>""'
Aqueous sol. of citric.,
acid (5%)
Remarks
Fe2 0 3
Fe3 0. and Fe are not
attacked.
30--60 S.
10 mI Swab.
5mI
2ml
3 mI
Fe2 0 3
Fe3 0. is not attacked.
Fe3 O.
If Fe2 0 3 is to be
etched simultaneously, use OFe m2
rust and follow up
with OFe m3.
FeO.
OFe
m5
101
Electrolylc:
Thioglycolic acid
(5%)
Aqueous sol. of potassium diphthalate
(5%)
Aqueous sol. of ammonium citrate (5%)
Aqueous sol of sodium chromate (0.5%)
15 s, 2-4 mA/cm2 , 9
10 mI V dc, stainless steeI
cathode.
Add sodium chro5 mI mate solution only
shortly before use.
2 mi
50 mI
Fe3 0 .
Fe and Fe2 0 3 are not
attacked.
100
Preparation of lron Oxide Layers on Iron

Preparation of Iron Oxide Layers on Iron
Ct
mIO
Sulfunc acid (1.84)

Lactic acid (90%)
Glacial acetic acid
Ct a. Dist. water
mil
Hydrochloric acid
(1.19)
Nitric acid (1.40)
Hydrofluoric acid
(40%)
b. Dist. water
Nitric acid (1.40)
Ct
mI2
Lactic acid (90%)
Ct
m13
Hydrogen peroxide
(30%)
Ammonia water
10 mI Secs to mins.
10 mI
10 mI
100 mIlOs, 50 oC (120F).
!!! See Appendix A.
6 mI
2ml
PuC-Pu (!!!).
U02 -AI (!!!).
5ml
10 mI 3 min, 25 oC (80F).
10 mI Use (a) tirst, then
(b).
Secs to mins.
(Y3AI)C-Y3 C-Y.
Secs to mins.
UN-U, UN-W (!!!).
10m!.
10 mI
Iron Oxide Layers on Iron

No.
OFe
mI
Etchant
Dist. water
Aqueous sol.of nitric .
acid (1%)
Aqueous sol of citric
acid (5%)
Aqueous sol. of
thioglycolic acid (5%)
OFe
m2
Aqueous sol. of citric

acid (10%)
Aqueous sol. of sodium thiocyanate (10%)
OFe a. Dist. water
m3
Formic acid (1.22)
b. Dist. water
Fluoboric acid
OFe
m4
Conditions
10 mI 15-60 S.
Swab.
5ml
5ml
5 mI
45-90 S.
5 mI Swab.
5 mI
15 mI 5 S.
5 mI Swab, followed by
15 mI (b)' 2 S.
5ml
Thioglycolic aeid
(5%)
Aqueous sol. of po- I
tassium diphthalate " \.
(5%)
Aqueous sol. of ammonium citrate (5%>""'
Aqueous sol. of citric.,
acid (5%)
Remarks
Fe2 0 3
Fe3 0. and Fe are not
attacked.
30--60 S.
10 mI Swab.
5mI
2ml
3 mI
Fe2 0 3
Fe3 0. is not attacked.
Fe3 O.
If Fe2 0 3 is to be
etched simultaneously, use OFe m2
rust and follow up
with OFe m3.
FeO.
OFe
m5
101
Electrolylc:
Thioglycolic acid
(5%)
Aqueous sol. of potassium diphthalate
(5%)
Aqueous sol. of ammonium citrate (5%)
Aqueous sol of sodium chromate (0.5%)
15 s, 2-4 mA/cm2 , 9
10 mI V dc, stainless steeI
cathode.
Add sodium chro5 mI mate solution only
shortly before use.
2 mi
50 mI
Fe3 0 .
Fe and Fe2 0 3 are not
attacked.
Appendix A:
Suggestions for Handling

Hazardous Materials
AH chemicals, including many metals and oxides, pose sorne degree
of danger to the human organismo This may come about by ingestion
through the respiratory or digestive tracts or by external contact with
the skin or eyes. Basically, the same precautions apply to the metallographic laboratory as to all chemical laboratories, except that certain
specific areas are particularly critical.
Sorne significant precautions are:
t
'/
.,..
,.1,.
CIearly IabeI all storage containers.

Dilute eoneentrated ehemieaIs before disposal and observe alllocal
waste-disposal regulations.
CritieaI substanees (flammable, explosive, toxic, or corrosive) should
be stored in approved containers in cool, fireproof, isolated areas.
Caustie materiaIs, such as acids, bases, peroxides, and sorne salts,
should be handled only when wearing protective de vices such as
safety glasses, rubber gloves, and laboratory coats or aprons. Vapors
of such materials are often harmful, too. Actual work should be
carried out in an effective fume hood with an additional gas mask
if evolution of toxic gases and vapors is suspected.
When preparing etchants containing aggressive ehemieals such as
sulfuric acid, the chemical should always be added to the solvent
(water, alcohol, glycerol, etc.) slowly with gentle stirring. External
cooling may also be required if heat evolution is particularly strong.
VoIatile, flainmabIe, and explosive materials, such as benzene,
acetone, ether, perchlorate, nitrate, etc. , should not be heated or
kept near open flames.
When preparing microsections of toxe materals such as beryIlium,
and radioaetve substances or alloys containing uranium, thorium,
and plutonium, a glove box or hot cell must be used.
'"
...., ".
Particularly hazardous chemicals listed in the etchant compositions

(Chapters 2 and 3) and in Appendix B are indicated by (!!!). These
de serve additional comments ..
Perchlorie acid in concentrations exceeding 60% is highly flammable
and explosive. This danger is greatly iucreased by the presence
!,: 1
103
104
Handling Hazardous Materials
of organic materials or metals such as bismuth, which oxidizes readily.

Avoid the higher concentration and heating of these solutions,
particularly in electrolytic polishing and etching; never store highconcentration perchloric solutions in plastic containers. When mixing
perchloric acid and alcohol, highly explosive alkyl perchlorates may
form : Perchloric acid should be added slowly under constant stirring.
Keepthe temperature of the solution below 35 oC (95 P) and, if
necessary, use a coolant bath. Wearing safety glasses is helpful,
but working behind a safety shield is preferable.
Mixtures of alcohol and hydrochloricacid can react in various ways .
to produce aldehydes, fatty acids, explosive nitrogen compounds,
etc. The tendency toward explosion increases with increasing molecule size. Hydrochloric acid content should not exceed 5% in ethanol
or 35% in methanol. These mixtures shduld not be stored.
Mixtures of alcohol and phosphoric acidcan result in the formation
of esters, some of which are potent nerve poisons. If absorbed
through the skin or inhaled, severe personal damage may result.
Mixtures of methanol and sulfuric acid may form dimethylene sulfate,
an odorless, tasteless compound that may be fatal if absorbed in
. sufficient quantities into the skin' or respiratory tract. Even gas
masks do not offer adequate protection. Sulfates of the higher
alcohols, however, are not potentially dangerous poisons.
Mixtures of chromium (VI) oxide and organic materials are explosive.
Mix with care and do not store.
Lead and lead salts are highly toxic, and the damage produced
is cumulative. Care is also recommended when handling cadmium,
thallium, nickel, mercury, and other heavy metals.
Al! cyanide compounds (eN) are highly dangerous because hydrocyanic acid (HCN) may easily formo They are fast-acting poisons
that can cause death, even in relatively low concentrations.
Hydrofluoric acid i~ a very strong skin and respiratory poison that
is hard to control. " should be handled with extreme care, beca use
sores resulting f;oIp. its attack on skin do not heal readily. Hydrofluoric acid also a:ttacks glass, and fumes .from specimensetched
~ HP solution c"uld easily damage front elements of microscope
lenses. Specimens 'should be rinsed thoroughly and in sorne cases
placed in a vacuum desiccator for one to two hours before examination.
.
Picric acid anhydri'a~ is an explosive.
The references on safty and toxicology in Appendix C contain
information on potential poisons, symptoms of poisoning, treatment,
and prevenon.
~
1)1
Appendix B:
Chemicals Used to Prepare Etchants

in Chapters 2 and 3
F = flammable, !!!
D = density.
toxic, E
Name
Acetic acid
Acetylacetone
(2,3-pentanedione, diacetylmethane)
Aluminum chloride
Ammonia
Ammonia water
Ammonium acetate
Ammonium chloride
Ammonium dicitrate
(diammonium hydrogen citrate)
Ammonium ditartrate
Ammonium hydrogen fluoride
Ammonium paramo!ybdate
(mo!ybdic acid)
Ammonium peroxydisu!fate
Ammonium polysulfide
Argon
Bromine
!-Butano!
Cadmium chloride
Cerium (IV) nitrate
Chromium (IlI) oxide
Chromium (VI) oxide (chromic acid)
Citric acid
Copper ammonium persulfate
Copper (I1) nitrate
Copper (11) sulfate
.(
explosiv, L
liquid, G
Formula
CH,COOH
C 5 H~02
(NH.). M0 7 2. , 4H 2
(NH.)2 S 2O~
(NH')2 Sx
(NH.)2 S20)
Ar
Br 2
CH j (CH 2 OH
CdCI 2 ' H,O
Ce(NO4
Cr,O)
CrO,
C.H ~ 07H,O
(NH4)2 [CuCl412H,O
[Cu(NH,).] S2 O.
CuCl,'H, O
Cu(No,),'6H,O
CuS04 '5H 2O
105
crystalline,
Remarks
!!! (caustic)
F, L, D 0.972
(CH, COCH 2eOCH

AICl)
NH)
NH) + H 20
CH)COONH.
NH.Cl
C.H,.N20 7
[(NH.)2 HC.H,071
(NH')2 C. H. O.
(NH.)HF 2
gas, C
C
!!!, G, D 0.596
!!!, L, 00.91
C
C
C
C
C
C
C
!!!, L
C
C
!!! (vapor), L,
D 3.11
F, L
!!l, C
C
C
!!! (caustic), e
C
l!!, C
C
!!!,e
l!!, C
!l!, C
104
Handling Hazardous Materials
of organic materials or metals such as bismuth, which oxidizes readily.

Avoid the higher concentration and heating of these solutions,
particularly in electrolytic polishing and etching; never store highconcentration perchloric solutions in plastic containers. When mixing
perchloric acid and alcohol, highly explosive alkyl perchlorates may
form : Perchloric acid should be added slowly under constant stirring.
Keepthe temperature of the solution below 35 oC (95 P) and, if
necessary, use a coolant bath. Wearing safety glasses is helpful,
but working behind a safety shield is preferable.
Mixtures of alcohol and hydrochloricacid can react in various ways .
to produce aldehydes, fatty acids, explosive nitrogen compounds,
etc. The tendency toward explosion increases with increasing molecule size. Hydrochloric acid content should not exceed 5% in ethanol
or 35% in methanol. These mixtures shduld not be stored.
Mixtures of alcohol and phosphoric acidcan result in the formation
of esters, some of which are potent nerve poisons. If absorbed
through the skin or inhaled, severe personal damage may result.
Mixtures of methanol and sulfuric acid may form dimethylene sulfate,
an odorless, tasteless compound that may be fatal if absorbed in
. sufficient quantities into the skin' or respiratory tract. Even gas
masks do not offer adequate protection. Sulfates of the higher
alcohols, however, are not potentially dangerous poisons.
Mixtures of chromium (VI) oxide and organic materials are explosive.
Mix with care and do not store.
Lead and lead salts are highly toxic, and the damage produced
is cumulative. Care is also recommended when handling cadmium,
thallium, nickel, mercury, and other heavy metals.
Al! cyanide compounds (eN) are highly dangerous because hydrocyanic acid (HCN) may easily formo They are fast-acting poisons
that can cause death, even in relatively low concentrations.
Hydrofluoric acid i~ a very strong skin and respiratory poison that
is hard to control. " should be handled with extreme care, beca use
sores resulting f;oIp. its attack on skin do not heal readily. Hydrofluoric acid also a:ttacks glass, and fumes .from specimensetched
~ HP solution c"uld easily damage front elements of microscope
lenses. Specimens 'should be rinsed thoroughly and in sorne cases
placed in a vacuum desiccator for one to two hours before examination.
.
Picric acid anhydri'a~ is an explosive.
The references on safty and toxicology in Appendix C contain
information on potential poisons, symptoms of poisoning, treatment,
and prevenon.
~
1)1
Appendix B:
Chemicals Used to Prepare Etchants

in Chapters 2 and 3
F = flammable, !!!
D = density.
toxic, E
Name
Acetic acid
Acetylacetone
(2,3-pentanedione, diacetylmethane)
Aluminum chloride
Ammonia
Ammonia water
Ammonium acetate
Ammonium chloride
Ammonium dicitrate
(diammonium hydrogen citrate)
Ammonium ditartrate
Ammonium hydrogen fluoride
Ammonium paramo!ybdate
(mo!ybdic acid)
Ammonium peroxydisu!fate
Ammonium polysulfide
Argon
Bromine
!-Butano!
Cadmium chloride
Cerium (IV) nitrate
Chromium (IlI) oxide
Chromium (VI) oxide (chromic acid)
Citric acid
Copper ammonium persulfate
Copper (I1) nitrate
Copper (11) sulfate
.(
explosiv, L
liquid, G
Formula
CH,COOH
C 5 H~02
(NH.). M0 7 2. , 4H 2
(NH.)2 S 2O~
(NH')2 Sx
(NH.)2 S20)
Ar
Br 2
CH j (CH 2 OH
CdCI 2 ' H,O
Ce(NO4
Cr,O)
CrO,
C.H ~ 07H,O
(NH4)2 [CuCl412H,O
[Cu(NH,).] S2 O.
CuCl,'H, O
Cu(No,),'6H,O
CuS04 '5H 2O
105
crystalline,
Remarks
!!! (caustic)
F, L, D 0.972
(CH, COCH 2eOCH

AICl)
NH)
NH) + H 20
CH)COONH.
NH.Cl
C.H,.N20 7
[(NH.)2 HC.H,071
(NH')2 C. H. O.
(NH.)HF 2
gas, C
C
!!!, G, D 0.596
!!!, L, 00.91
C
C
C
C
C
C
C
!!!, L
C
C
!!! (vapor), L,
D 3.11
F, L
!!l, C
C
C
!!! (caustic), e
C
l!!, C
C
!!!,e
l!!, C
!l!, C
106
Chemicals for Etchants in Chapters 2 and 3
1,2-ethanediol (dihydroxy ethane,

ethylene glycol, glycol) .
C, H. O,
(HOCH 2 CH 2OH)
L, D 1.11
Ethanethiol
Ethanol
C6 H,.02
C2 H, OH
L, D 0.90
F,L,D
0.81-0.79
Ethylene glycol
Fluoboric acid
(See 1,2-ethanediol)
HBF.
Formic acid
Glycerol
(glycerine)
Gold (111) chloride
Hydrochloric acid
HCOOH
C,H.03
(HOCH 2CHOHCH 2 OH)
AuCI 3H 20
HCI
!!! (caustic), L,
D 1.23
L, D 1.22
L, D 1.26
C
!!! (caustic), L,
D 1.19
Hydrofluoric acid
HF
+ H2 0
!!! (caustic), L,
40%
Hydrogen
Hydrogen peroxide
Hydrogen sulfide
Iron (I1I) chloride
lron (III) nitrate
Iron (H) sulfate
Lactic acid
Lead acetate
Magnesium oxide (magnesia)
Mercury (11) nitrate
. Methanol
Nitric acid
H,
H 2 0,
H2 S
FeCI 36H 2 0
Fe(N0 3)3 9H 2
FeSO.7H 20
C 3 H. O,
Pb(CH 3COO),
MgO
Hg(N3)2 8H 20
CH 30H
HN03
N2
Nitrogen
Oxalic acid
Perchloric acid
>,
C 2 H 20.2H 2
HCIO.
~.
Phosphoric acid
H 3 PO.
Picric acid
Potass~m bicarbonate
Potassium carbonate
Potassium chloride
P~tassium cyanide
Potassium dichromate
Potassium ferrocyanide
~
:P
'
., ','
'!. ... . ....
C. H3 N 30,
KHCO,
K 2 C03
KCI
KCN
K 2Cr,O,
K) [Fe(CN).l
K. [Fe(CN).l
E, F,G
L, D 1.11
!!!,G
C
C
C
L, D. 1.21
!!!, C
C
!!!, C
!!! L, D 0.76
!!!(caustic), L,
D 1.19
G
JI!, C
!!! (caustic), L,
E, D 1.67
!!! (caustic), L,
D 1.71
!!! (caustic),
E,C
C
Potassium hydrate solution

Potassium hydrogen fluoride
Potassium hydrogen sulfate
Potassium hydroxide
Potassium iodide
Potassium nitrate
Potassium phthalate (di-)
Silver cyanide
Silver nitrate
Sodium bicarbonate
Sodium carbonate
Sodium chloride
Sodium chromate
Sodium cyanide
Sodium dichromate
Sodium f1uoride
Sodium hydrogen phosphate
Sodium hydroxide
Sodium sulfate
Sodium sulfate, anhydrous
Sodium sulfide
Sodium tetraborate
Sodiumthiocyanate
Sodium thiosulfate (fixer)
Spirits of ammonia
Sulfuric acid
Trtaric acid
Thioglycolic acid
Thiourea
1,3-dimethyl
2-thiourea
Tin (11) chIoride
Vogel's special reagent
(stainless steel etchant)
C
!!!,C
!!! (caustic), C
C
C
Wetting agents
Zinc chloride
107
!!!(caustic), L
C
C
!l! (caustic), C
KOH+H 20
KHF,
KHSO.
KOH
KI
K,S,O,
KN03
C. H. K,O"
KSS::;N
AgCN
AgN0 3
NaCHO)
Na 2 CO, 10H,O
NaCl
Na 2 CrO.
NaCN
Na 2 Cr 2 07 2H ,
NaF
Na, HPO. 12H 2

NaOH
Na, SO.' IOH,
Na 2 SO.
Na 2 S
Na 2 B.O,
NaSCN
Na, S2 0, . 5H,O
NH,+H 2 0
H 2 SO.
C.H.O.
HSCH 2COOH
CS(NH 2)2
C,H.N 2S
(CH) NHCSNHCH,)
SnCI 2 2H,O
Mixture of tar and
sulfurous acid, boiled and
filtered; protected trade
product
Additives for lowering
surface tension
ZnCI 2
C
C
C
!l!, C
!l!, C
C
C
C
C
C
!!!, C
!!! (caustic),C
C
C
!l! (caustic), C
C
C
':C
C
C
C
!!!, L, D 0.91
!!! (caustic), L,
DI.84
L
L
C
C
!!! (caustic), C
L
!!! (caustic), C
106
1,2-ethanediol (dihydroxy ethane,

ethylene glycol, glycol) .
C, H. O,
(HOCH 2 CH 2OH)
L, D 1.11
Ethanethiol
Ethanol
C6 H,.02
C2 H, OH
L, D 0.90
F,L,D
0.81-0.79
Ethylene glycol
Fluoboric acid
(See 1,2-ethanediol)
HBF.
Formic acid
Glycerol
(glycerine)
Gold (111) chloride
Hydrochloric acid
HCOOH
C,H.03
(HOCH 2CHOHCH 2 OH)
AuCI 3H 20
HCI
!!! (caustic), L,
D 1.23
L, D 1.22
L, D 1.26
C
!!! (caustic), L,
D 1.19
Hydrofluoric acid
HF
+ H2 0
!!! (caustic), L,
40%
Hydrogen
Hydrogen peroxide
Hydrogen sulfide
Iron (I1I) chloride
lron (III) nitrate
Iron (H) sulfate
Lactic acid
Lead acetate
Magnesium oxide (magnesia)
Mercury (11) nitrate
. Methanol
Nitric acid
H,
H 2 0,
H2 S
FeCI 36H 2 0
Fe(N0 3)3 9H 2
FeSO.7H 20
C 3 H. O,
Pb(CH 3COO),
MgO
Hg(N3)2 8H 20
CH 30H
HN03
N2
Nitrogen
Oxalic acid
Perchloric acid
>,
C 2 H 20.2H 2
HCIO.
~.
Phosphoric acid
H 3 PO.
Picric acid
Potass~m bicarbonate
Potassium carbonate
Potassium chloride
P~tassium cyanide
Potassium dichromate
Potassium ferrocyanide
~
:P
'
., ','
'!. ... . ....
C. H3 N 30,
KHCO,
K 2 C03
KCI
KCN
K 2Cr,O,
K) [Fe(CN).l
K. [Fe(CN).l
E, F,G
L, D 1.11
!!!,G
C
C
C
L, D. 1.21
!!!, C
C
!!!, C
!!! L, D 0.76
!!!(caustic), L,
D 1.19
G
JI!, C
!!! (caustic), L,
E, D 1.67
!!! (caustic), L,
D 1.71
!!! (caustic),
E,C
C
Potassium hydrate solution

Potassium hydrogen fluoride
Potassium hydrogen sulfate
Potassium hydroxide
Potassium iodide
Potassium nitrate
Potassium phthalate (di-)
Silver cyanide
Silver nitrate
Sodium bicarbonate
Sodium carbonate
Sodium chloride
Sodium chromate
Sodium cyanide
Sodium dichromate
Sodium f1uoride
Sodium hydrogen phosphate
Sodium hydroxide
Sodium sulfate
Sodium sulfate, anhydrous
Sodium sulfide
Sodium tetraborate
Sodiumthiocyanate
Sodium thiosulfate (fixer)
Spirits of ammonia
Sulfuric acid
Trtaric acid
Thioglycolic acid
Thiourea
1,3-dimethyl
2-thiourea
Tin (11) chIoride
Vogel's special reagent
(stainless steel etchant)
C
!!!,C
!!! (caustic), C
C
C
Wetting agents
Zinc chloride
107
!!!(caustic), L
C
C
!l! (caustic), C
KOH+H 20
KHF,
KHSO.
KOH
KI
K,S,O,
KN03
C. H. K,O"
KSS::;N
AgCN
AgN0 3
NaCHO)
Na 2 CO, 10H,O
NaCl
Na 2 CrO.
NaCN
Na 2 Cr 2 07 2H ,
NaF
Na, HPO. 12H 2

NaOH
Na, SO.' IOH,
Na 2 SO.
Na 2 S
Na 2 B.O,
NaSCN
Na, S2 0, . 5H,O
NH,+H 2 0
H 2 SO.
C.H.O.
HSCH 2COOH
CS(NH 2)2
C,H.N 2S
(CH) NHCSNHCH,)
SnCI 2 2H,O
Mixture of tar and
sulfurous acid, boiled and
filtered; protected trade
product
Additives for lowering
surface tension
ZnCI 2
C
C
C
!l!, C
!l!, C
C
C
C
C
C
!!!, C
!!! (caustic),C
C
C
!l! (caustic), C
C
C
':C
C
C
C
!!!, L, D 0.91
!!! (caustic), L,
DI.84
L
L
C
C
!!! (caustic), C
L
!!! (caustic), C
References
109
la, Ausg. Dez. 1965 jMarz 1969, Hauptverband dergewerblichen Berufsgenossen_

schaften, C. Heymanns Ver!. KG, Kiiln.
Appendix C:
15. Registry of Toxic Effects of Chemical Substances, U. S. Department of Hea1th,

Education, and Welfare. Public Hea1th Service - Center for Disease Control- National
Institute for Occupational Safety and Health (NIOSH), Rockville, Md., June 1976.
(Published every year.)
References
The references listed in this appendix are suggested for obtaining a better
understanding. Only selected texts are represented; not all sources used to prepare
the manual are listed.
Safetyand Toxicology
1. W. Braun, A. Donhardt, Poisoning Register (in German) Vergiftungsregister, Georg
Thieme Verl., Stuttgart, 1970.
2. L. V. Cralley, L. J. Cralley, G. D. Clayton, J. A. Jurgiel, Ed., Industrial Environmental
Health, The Worker and the Community, Academic Press, New York and London,
1972.
3. A. Hamilton, H. L. Hardy, Industrial Toxicology, Publishing Sciences Group, Inc.,

Acton, Mass., 1974.
4. A. Loomis, Essentials of Toxicology, Lea & Febinger, Philadelphia, 1974.
5. F. A. Patty, Ed., Industrial Hygiene and Toxicology, Interscience Publishers; New

York, 1963.
6. N. 1. Sax, Dangerous Properties of Industrial Materials, Van Nostrand Reinhold Co.,
New YorkjCincinnatijTorontojLondonjMelbourne, 1975.
7. G. Sorbe, Toxins and Explosives (in German) Gifte und explosive Substanzen, Berufskundliche Reihe zur Fachzeitschrift Chemie fr Labor und Betrieb, Bd. 7. Umschau
Verl., Frankfurt am Main, 1968.
8. P. G. Stecher, The Merck Index of Chemicals and Drugs, Merck & Co., Inc., Rahway,
N. J. (Get newest edition. Useful for identification of unknown materials).
9. H. E. Stockinger, Ed., Beryllium: Its Industrial Hygiene, Aspects, Academic Press,
N ew York j London, 1966.
I
lO. C. Xinteras, B. C. J04nson, 1. de Groot, Ed., Behavioral Toxicology, Early Detection

of Occupational Hazards, U. S. Department of Health, Education,and Welfare. Public
Hea1th Service-Cenker for Disease Control-National Institute for Occupational
Safety and Hea1th '(N,IOSH), Rockville, Md., 1974.
,
11. F'ederal Controls on <ccupational Exposures to Beryllium: A Rapid Reference Compli,ance Guide. Rules a,n.d Regulations. Federal Register, Vol. 36, No. 157, Aug 13,
"1971.
,1
12. Guide for Safety in the Chemical Laboratory, Manufacturing Chemists Assn., Van
Nostrand Reinhold '(;:0.; New YorkjCincinnatijToronto/LondonjMelbourne, 1972.
13. Guidelinesfor Cheinical Laboratories (in German)
Richtlinien fr chemische Laboratorien, Laboratoriumsrichtlinien Ausgabe 1972,
Hauptverband der gewerblichen Berufsgenossenschaften, Zentralstelle fr Unfallverhtung, Bonn.
.
14. Protection Against Dangerous Materials (in German)
Schutz gegen gefiihrliche Stoffe, Sammlung der Unfallverhtungsvorschriften, Nr. VBO
~,1
108
16. The Industrial Environment-Its Evaluation & Control, U. S. Department of Hea1th,

Education, and Welfare. Public Hea1th Service -Center for Disease Control- National
Institute for Occupational Safety and H~a1th (NIOSH), Rockville, Md., 1973.
17. There is a whole list of information available on individual subjects from NIOSH
Standards Library, U. S. Department of Hea1th, Education, and Welfare, Public Health

Service-Center for Disease Control-National Institute for Occupational Safety
and Health (NIOSH), Rockville, Md.
a) Technical
b) Surveys
e) Research Reports
d) Full Criteria Documents
e) Mini Criteria Documents
f) NIOSH Miscellaneous.
General Textbooks and Reviews

1. D. G. Brandon, Modern Techniques in Metal/ography, Butterworth Pub!. Co., London,
1966.
2. H. E. Exner, Ed., "Quantitative Analysis of Microstructures in Medicine, Biology

and Materials Development," Special Issue 5. of Practical Metal/ography, Dr. RiedererVerlag GmbH, Stuttgart, 1975.
3. R. M. Fulrath, J. A. Pask, Ed., Ceramic Microstructures, John Wiley and Sons,
Inc., New YorkjLondonjSydney, 1968.
4. R. C. Gifkins, Oplical Microscopy of Metals, American Elsevier Publishing Co., Inc.,
New York, 1970.
5. H. Gleiter, Structure and Properties of High-Angle Grain Boundaries in Metals (in

German)
Struktur und Eigenschaften von Grosswinkelkorngrenzen in Metal/en, Materialkundlich_
Technische Reihe. G. Petzow, Ed., Gebr. Borntrager Verlag, BerlinjStuttgart, 1977.
6. E. Hornbogen, G. Petzow, "Metallography" (in German)
"Metallographie," Zeitschriftfr Metal/kunde, Vo!. 61 (1970), pp. 81-94.
7. W. Jahnig, Metallography of Cast Al/oys (in German)
Metallographie der Gusslegierungen, VEB Deutscher Verlag fr Grundstoffindustrie,
Leipzig, 1971.
8. E. Kauczor, Metal in the Microscope. Introduction to Metallographic Microstructures

(in German)
Metal/ unter dem Mikroskop, Einfhrung in die Metallographische Gejgelehre. Fertigung
und Betrieb, Vo!. 3. H. Determann, W. Malmberg, Ed., Springer Verlag, BerlinjHeidelbergjNew York, 1974.
9. H. Modin, Metallurgical Microscopy, Butterworth Pub!. Co., London, 1973.
lO. V. A. Phillips, Modern Metallographic Techniques and Their Application, Wiley

Interscience, New YorkjLondonjSydney/Toronto, 1971.
11. E. P. Poluschkin, Structural Characteristics of Metals, Elsevier Pub!. Co., Amsterdam,
1964.
References
109
la, Ausg. Dez. 1965 jMarz 1969, Hauptverband dergewerblichen Berufsgenossen_

schaften, C. Heymanns Ver!. KG, Kiiln.
Appendix C:
15. Registry of Toxic Effects of Chemical Substances, U. S. Department of Hea1th,

Education, and Welfare. Public Hea1th Service - Center for Disease Control- National
Institute for Occupational Safety and Health (NIOSH), Rockville, Md., June 1976.
(Published every year.)
References
The references listed in this appendix are suggested for obtaining a better
understanding. Only selected texts are represented; not all sources used to prepare
the manual are listed.
Safetyand Toxicology
1. W. Braun, A. Donhardt, Poisoning Register (in German) Vergiftungsregister, Georg
Thieme Verl., Stuttgart, 1970.
2. L. V. Cralley, L. J. Cralley, G. D. Clayton, J. A. Jurgiel, Ed., Industrial Environmental
Health, The Worker and the Community, Academic Press, New York and London,
1972.
3. A. Hamilton, H. L. Hardy, Industrial Toxicology, Publishing Sciences Group, Inc.,

Acton, Mass., 1974.
4. A. Loomis, Essentials of Toxicology, Lea & Febinger, Philadelphia, 1974.
5. F. A. Patty, Ed., Industrial Hygiene and Toxicology, Interscience Publishers; New

York, 1963.
6. N. 1. Sax, Dangerous Properties of Industrial Materials, Van Nostrand Reinhold Co.,
New YorkjCincinnatijTorontojLondonjMelbourne, 1975.
7. G. Sorbe, Toxins and Explosives (in German) Gifte und explosive Substanzen, Berufskundliche Reihe zur Fachzeitschrift Chemie fr Labor und Betrieb, Bd. 7. Umschau
Verl., Frankfurt am Main, 1968.
8. P. G. Stecher, The Merck Index of Chemicals and Drugs, Merck & Co., Inc., Rahway,
N. J. (Get newest edition. Useful for identification of unknown materials).
9. H. E. Stockinger, Ed., Beryllium: Its Industrial Hygiene, Aspects, Academic Press,
N ew York j London, 1966.
I
lO. C. Xinteras, B. C. J04nson, 1. de Groot, Ed., Behavioral Toxicology, Early Detection

of Occupational Hazards, U. S. Department of Health, Education,and Welfare. Public
Hea1th Service-Cenker for Disease Control-National Institute for Occupational
Safety and Hea1th '(N,IOSH), Rockville, Md., 1974.
,
11. F'ederal Controls on <ccupational Exposures to Beryllium: A Rapid Reference Compli,ance Guide. Rules a,n.d Regulations. Federal Register, Vol. 36, No. 157, Aug 13,
"1971.
,1
12. Guide for Safety in the Chemical Laboratory, Manufacturing Chemists Assn., Van
Nostrand Reinhold '(;:0.; New YorkjCincinnatijToronto/LondonjMelbourne, 1972.
13. Guidelinesfor Cheinical Laboratories (in German)
Richtlinien fr chemische Laboratorien, Laboratoriumsrichtlinien Ausgabe 1972,
Hauptverband der gewerblichen Berufsgenossenschaften, Zentralstelle fr Unfallverhtung, Bonn.
.
14. Protection Against Dangerous Materials (in German)
Schutz gegen gefiihrliche Stoffe, Sammlung der Unfallverhtungsvorschriften, Nr. VBO
~,1
108
16. The Industrial Environment-Its Evaluation & Control, U. S. Department of Hea1th,

Education, and Welfare. Public Hea1th Service -Center for Disease Control- National
Institute for Occupational Safety and H~a1th (NIOSH), Rockville, Md., 1973.
17. There is a whole list of information available on individual subjects from NIOSH
Standards Library, U. S. Department of Hea1th, Education, and Welfare, Public Health

Service-Center for Disease Control-National Institute for Occupational Safety
and Health (NIOSH), Rockville, Md.
a) Technical
b) Surveys
e) Research Reports
d) Full Criteria Documents
e) Mini Criteria Documents
f) NIOSH Miscellaneous.
General Textbooks and Reviews

1. D. G. Brandon, Modern Techniques in Metal/ography, Butterworth Pub!. Co., London,
1966.
2. H. E. Exner, Ed., "Quantitative Analysis of Microstructures in Medicine, Biology

and Materials Development," Special Issue 5. of Practical Metal/ography, Dr. RiedererVerlag GmbH, Stuttgart, 1975.
3. R. M. Fulrath, J. A. Pask, Ed., Ceramic Microstructures, John Wiley and Sons,
Inc., New YorkjLondonjSydney, 1968.
4. R. C. Gifkins, Oplical Microscopy of Metals, American Elsevier Publishing Co., Inc.,
New York, 1970.
5. H. Gleiter, Structure and Properties of High-Angle Grain Boundaries in Metals (in

German)
Struktur und Eigenschaften von Grosswinkelkorngrenzen in Metal/en, Materialkundlich_
Technische Reihe. G. Petzow, Ed., Gebr. Borntrager Verlag, BerlinjStuttgart, 1977.
6. E. Hornbogen, G. Petzow, "Metallography" (in German)
"Metallographie," Zeitschriftfr Metal/kunde, Vo!. 61 (1970), pp. 81-94.
7. W. Jahnig, Metallography of Cast Al/oys (in German)
Metallographie der Gusslegierungen, VEB Deutscher Verlag fr Grundstoffindustrie,
Leipzig, 1971.
8. E. Kauczor, Metal in the Microscope. Introduction to Metallographic Microstructures

(in German)
Metal/ unter dem Mikroskop, Einfhrung in die Metallographische Gejgelehre. Fertigung
und Betrieb, Vo!. 3. H. Determann, W. Malmberg, Ed., Springer Verlag, BerlinjHeidelbergjNew York, 1974.
9. H. Modin, Metallurgical Microscopy, Butterworth Pub!. Co., London, 1973.
lO. V. A. Phillips, Modern Metallographic Techniques and Their Application, Wiley

Interscience, New YorkjLondonjSydney/Toronto, 1971.
11. E. P. Poluschkin, Structural Characteristics of Metals, Elsevier Pub!. Co., Amsterdam,
1964.
110
References
References
12. J. H. Richardson, "Optical Microscopy for the Materials Sciences," Monographs

and Textbooks in Materials Science, Vol. 3, Marcel Dekker, Inc., New York and
Basel, 1970.
13. W. Rostocker, J. R. Dvorak, Interpretation
Press, New York, London, 1965.
01 Metallographic
Structures, Aeademic
14. H. Schllinann, Metallography (in German)

Metallographie, VEB Deutscher Verlag fr Grundstoffindustrie, Leipzig, 1967.
15. R: E. Smallman, Modern Physical Metallurgy, Butterworth International, Woburn,
Mass., 1970.
16. C. S. Smith, A History
01 Metallography,
University of Chicago Press, 1960.
111
11. J. A. Nelson, E. D. Albrecht, "The Basics of Metallography" (Parts I and 11), Heat
Treating, Apr/June 1976, pp. 19-23.
12. L. E. Samuels, Metallographic Polishing by Mechanical Methods, Pitman Publ. Corp.,

London and Melbourne, 1971.
13. Me. G. Tegart, The Electrolytic and Chemical Polishing
Industry, Pergamon Press, London, 1959.
01 Metals
in Research and
14. B. Tuck, "The Chemical Polishing of Semiconductors," J. Mat. Science, Vol. 10,
1957, pp. 321-339.
15. R. S. Williams, V. O. Homerberg, PrincipIes 01 Metallography, Metallurgy and
Metallurgical Engineering Series, McGraw-Hill Book Co., New York, 1948.
.17. H. Thompson, Microscopical Techniques in Metallurgy, Sir Isaac Pitman & Sons,
Ltd., London, 1954.
16. J. L. Woodbury, E. D. Albrecht, "The Reflective Decision Maker," Industrial Research,

May 1976, pp. 78-81.
18. Applications 01 Modern Metallographic Techniques, American Society for Testing

and Materials (ASTM) Special Tec,hnicaI Pub!. No. 480, Symposium Philadelphia,
1966.
17. ANALYST: Preparation 01 Metallographic, Ceramic, and Petrographic Samples,

Buehler Ltd. and A. 1. Buehler Inc., Evanston, m.
19. Fifty Years 01 Progress in Metallographic Techniques, American Society for Testing
and Materials (ASTM) Special Technical Publ. No. 430, Symposium Atlantic City
1966, Philadelphia.
.
20. Symposium on Metallography in Color, American Society for Testing and Materials
(ASTM) Special Technical Publ. No. 86, Symposium Detroit, 1948, Philadelphia.
18. "Metallographic Reagents for Iron and Steel," Metal Progress Data Book, Vol. 106,
No. 1, American Society for Metals, Metals Park, Ohio, 1974.
19. "Metallographic Sample Preparation," Metal Digest, Buehler Ltd., Vol. 11, No. 2/3.
20. METALOG: Preparation 01 Metallographic, Ceramic, and Petrographic Samples,

Struers Scientific Instruments, Copenhagen, Denmark.
21. "Petrographic Sample Preparation," Metal Digest, Buehler Ltd., Vol. 12/13, No. 1.
Metallographic Preparation
1. M. Beckert, H. Klemm, Handbook 01 Metallographic Etching Techniques (in German)
Handbuch der metallographischen Atzverfahren, VEB Deutscher Verlag fr Grundstoffindustrie (2nd Ed.), Leipzig, 1976.
23. 1975 Annual Book 01 ASTM Standards, Part 11: Metallography; Nondestructive Tests,
American Society for Testing and Materials, Philadelphia, 1975.
2. A. F. Bogenschtz, Etching Semiconductors (in German)

Atzpraxislr Halbleiter, Carl Hanser Verlag, Mnchen, 1967.
Handbooks, Compilations, and Tables
3. P. M. French, J. L. MeCall, Ed., Interpretive Techniqueslor Microstructural Analysis,

Plenum Press, New York, 1977.
4. H. Freund, Ed., Metallographic Specimen Preparationlor Optical Microscopy-Handbooklor Technical Microscopy, Vol. III/Part I (in German)
Metallographische Probenpriiparation lr die mikroskopische Untersuchung- Handbuch der Mikroskopie il'/ der Technik, Bd. III/Teil 1, Umsehau Verlag, Frankfurt
I
am Main, 1968.
..
5. R. Galopin, N.F.M., Mi:roscopic Study

Sons Ltd., Cambridge, 1'72.
\
01 Opaque Minerals,
Henry W. Heffer and
6. G. L. Kehl, The PrincipIes 01 Metallographic Laboratory Practice, Metallurgy and

Metallurgical Engineerilig Series, McGraw-Hill Book Co., New York, 1949.
7. H:":E. Knechtel, W. F>icindle, J. L. McCall, R. D. Buchheit, Tools and Techniques
in Physical Metallurgy, . Vol. 1, F. Weinberg (Ed.); pp. 321-399, M. Dekker Inc.,
New York, 1970..,
8. J. L. McCall, W. M. Mu'eller, Ed., Microstructural Analysis, Tools and Techniques,
Plenum Press, New YorlC; 1973.
9. J. L. McCall, W. M. Mueller, Ed., Metallographic Specimen Preparation, Plenum
Press, New York, 1971.
10. J. A. Nelson, "Metallographic Techniques in the Electronics Industry," Metallography,
Vol. 9, No. 2, American EIsevier Publishing, 1976, pp. 109-122.
~
,p
22. 1973 Annual Book 01 ASTM SJandards, Part. 31, AmericanSociety for Testing and
Materials, Philadelphia, 1973.
1. R. J. Gray, J. L. McCall and others (Ed.), Microstructural Science, Vol. 1-5, Proceedings
of Annual Meetings of the International Metallographic Society, American EIsevier
Pub!. Co., Inc., New York, 1974-1977.
2. L. Habraken, J. L. deBrouwer, Basic Metallography (in German)
De Ferri Metallographia, Grundlagen der Metallographie, Teil 1, Presses Acadmiques
Europennes, Bruxelles, 1966.
3. H. Hanemann, A. Schrader, Atlas 01 Microstructures, Vol. I Iron-Carbon Steels (1933),
Vo!. 11 Cast Irons (1936), Vol. III Binary AluminumAlloys (1952) (in German)
Atlas Metallographicus, Gebr. Borntrager Verlag, Braunschweig.
4. V. Horn in cooperation with W. Bernhardt, K. Buness, E. Kretzschmar and H.
Stein, Atlas 01 Microstructures in Welding (in German)
Schweisstechnischer Gelgeatlas, VEB Verlag Technik, Berlin, 1974.
5. F. Jeglitsch, G. Petzow, "Progress in Metallography," Practical Metallography, Special
Edition 4 (in German)
"Fortschritte in der Metallographie," Dr. Riederer-Verlag GmbH, Stuttgart, 1975.
6. R. Mitsche, F. Jeglitsch, G. Petzow, "Progress in Metallography," Practical Metallography, Special Edition 3 (in German)
7. F. K. Naumann, The Book 01 Failures (in German)
Das Buch der Schadensliille, Dr. Riederer-Verlag GmbH, Stuttgart, 1976.
110
References
References
12. J. H. Richardson, "Optical Microscopy for the Materials Sciences," Monographs

and Textbooks in Materials Science, Vol. 3, Marcel Dekker, Inc., New York and
Basel, 1970.
13. W. Rostocker, J. R. Dvorak, Interpretation
Press, New York, London, 1965.
01 Metallographic
Structures, Aeademic
14. H. Schllinann, Metallography (in German)

Metallographie, VEB Deutscher Verlag fr Grundstoffindustrie, Leipzig, 1967.
15. R: E. Smallman, Modern Physical Metallurgy, Butterworth International, Woburn,
Mass., 1970.
16. C. S. Smith, A History
01 Metallography,
University of Chicago Press, 1960.
111
11. J. A. Nelson, E. D. Albrecht, "The Basics of Metallography" (Parts I and 11), Heat
Treating, Apr/June 1976, pp. 19-23.
12. L. E. Samuels, Metallographic Polishing by Mechanical Methods, Pitman Publ. Corp.,

London and Melbourne, 1971.
13. Me. G. Tegart, The Electrolytic and Chemical Polishing
Industry, Pergamon Press, London, 1959.
01 Metals
in Research and
14. B. Tuck, "The Chemical Polishing of Semiconductors," J. Mat. Science, Vol. 10,
1957, pp. 321-339.
15. R. S. Williams, V. O. Homerberg, PrincipIes 01 Metallography, Metallurgy and
Metallurgical Engineering Series, McGraw-Hill Book Co., New York, 1948.
.17. H. Thompson, Microscopical Techniques in Metallurgy, Sir Isaac Pitman & Sons,
Ltd., London, 1954.
16. J. L. Woodbury, E. D. Albrecht, "The Reflective Decision Maker," Industrial Research,

May 1976, pp. 78-81.
18. Applications 01 Modern Metallographic Techniques, American Society for Testing

and Materials (ASTM) Special Tec,hnicaI Pub!. No. 480, Symposium Philadelphia,
1966.
17. ANALYST: Preparation 01 Metallographic, Ceramic, and Petrographic Samples,

Buehler Ltd. and A. 1. Buehler Inc., Evanston, m.
19. Fifty Years 01 Progress in Metallographic Techniques, American Society for Testing
and Materials (ASTM) Special Technical Publ. No. 430, Symposium Atlantic City
1966, Philadelphia.
.
20. Symposium on Metallography in Color, American Society for Testing and Materials
(ASTM) Special Technical Publ. No. 86, Symposium Detroit, 1948, Philadelphia.
18. "Metallographic Reagents for Iron and Steel," Metal Progress Data Book, Vol. 106,
No. 1, American Society for Metals, Metals Park, Ohio, 1974.
19. "Metallographic Sample Preparation," Metal Digest, Buehler Ltd., Vol. 11, No. 2/3.
20. METALOG: Preparation 01 Metallographic, Ceramic, and Petrographic Samples,

Struers Scientific Instruments, Copenhagen, Denmark.
21. "Petrographic Sample Preparation," Metal Digest, Buehler Ltd., Vol. 12/13, No. 1.
Metallographic Preparation
1. M. Beckert, H. Klemm, Handbook 01 Metallographic Etching Techniques (in German)
Handbuch der metallographischen Atzverfahren, VEB Deutscher Verlag fr Grundstoffindustrie (2nd Ed.), Leipzig, 1976.
23. 1975 Annual Book 01 ASTM Standards, Part 11: Metallography; Nondestructive Tests,
American Society for Testing and Materials, Philadelphia, 1975.
2. A. F. Bogenschtz, Etching Semiconductors (in German)

Atzpraxislr Halbleiter, Carl Hanser Verlag, Mnchen, 1967.
Handbooks, Compilations, and Tables
3. P. M. French, J. L. MeCall, Ed., Interpretive Techniqueslor Microstructural Analysis,

Plenum Press, New York, 1977.
4. H. Freund, Ed., Metallographic Specimen Preparationlor Optical Microscopy-Handbooklor Technical Microscopy, Vol. III/Part I (in German)
Metallographische Probenpriiparation lr die mikroskopische Untersuchung- Handbuch der Mikroskopie il'/ der Technik, Bd. III/Teil 1, Umsehau Verlag, Frankfurt
I
am Main, 1968.
..
5. R. Galopin, N.F.M., Mi:roscopic Study

Sons Ltd., Cambridge, 1'72.
\
01 Opaque Minerals,
Henry W. Heffer and
6. G. L. Kehl, The PrincipIes 01 Metallographic Laboratory Practice, Metallurgy and

Metallurgical Engineerilig Series, McGraw-Hill Book Co., New York, 1949.
7. H:":E. Knechtel, W. F>icindle, J. L. McCall, R. D. Buchheit, Tools and Techniques
in Physical Metallurgy, . Vol. 1, F. Weinberg (Ed.); pp. 321-399, M. Dekker Inc.,
New York, 1970..,
8. J. L. McCall, W. M. Mu'eller, Ed., Microstructural Analysis, Tools and Techniques,
Plenum Press, New YorlC; 1973.
9. J. L. McCall, W. M. Mueller, Ed., Metallographic Specimen Preparation, Plenum
Press, New York, 1971.
10. J. A. Nelson, "Metallographic Techniques in the Electronics Industry," Metallography,
Vol. 9, No. 2, American EIsevier Publishing, 1976, pp. 109-122.
~
,p
22. 1973 Annual Book 01 ASTM SJandards, Part. 31, AmericanSociety for Testing and
Materials, Philadelphia, 1973.
1. R. J. Gray, J. L. McCall and others (Ed.), Microstructural Science, Vol. 1-5, Proceedings
of Annual Meetings of the International Metallographic Society, American EIsevier
Pub!. Co., Inc., New York, 1974-1977.
2. L. Habraken, J. L. deBrouwer, Basic Metallography (in German)
De Ferri Metallographia, Grundlagen der Metallographie, Teil 1, Presses Acadmiques
Europennes, Bruxelles, 1966.
3. H. Hanemann, A. Schrader, Atlas 01 Microstructures, Vol. I Iron-Carbon Steels (1933),
Vo!. 11 Cast Irons (1936), Vol. III Binary AluminumAlloys (1952) (in German)
Atlas Metallographicus, Gebr. Borntrager Verlag, Braunschweig.
4. V. Horn in cooperation with W. Bernhardt, K. Buness, E. Kretzschmar and H.
Stein, Atlas 01 Microstructures in Welding (in German)
Schweisstechnischer Gelgeatlas, VEB Verlag Technik, Berlin, 1974.
5. F. Jeglitsch, G. Petzow, "Progress in Metallography," Practical Metallography, Special
Edition 4 (in German)
6. R. Mitsche, F. Jeglitsch, G. Petzow, "Progress in Metallography," Practical Metallography, Special Edition 3 (in German)
7. F. K. Naumann, The Book 01 Failures (in German)
Das Buch der Schadensliille, Dr. Riederer-Verlag GmbH, Stuttgart, 1976.
112
References
8. J. Orlich, A. Rose, p, Wiest, Atlaslor Heat Treatment 01 Steels (in German)

Atlas zur Wiirembehandlung der Stiihle, Band 3, Verlag Stahleisen, Dsseldorf, 1973.
9. A. Schrader, A. Rose, Microstructures 01 Steels (in German)
De Ferri Metallographia, Teil 11, Gefge der Stiihle, Verlag Stahleisen, Dsseldorf,
1966.
10. R. W. ",ilson, Metallurgy and Heat Treatment 01 Tool Steels, McGraw-HilI Company
(U.K.) Ltd., Maidenhead, Berkshire, 1975.
11. "Atlas of Microstructures of Industrial AIIoys," Metals Handbook, 8th Ed., Vol.
7, American Society for Metals, Metals Park, Ohio, 1972.
Appendix D:
Some Suppliers of Metallographic

Equipment and Materials
12. "Fractography and Atlas of Fractographs," Metals Handbook, 8th Ed., Vol. 9,
American Society for Metals, Metals Park, Ohio, 1974.
13. "MetaIlography, Structures and Phase Diagrams," Metals Handbook, 8th Ed., Vol.
14. So urce Book in Failure Analysis, American Society for Metals, Metals Park, Ohio,
1974.
15. Translormation and Hardenability in Steels, Climax Molybdenum Corp., Ann Arbor,
Mich., 1967.
Journals of Mostly Metallographic Content

1.
Metallography. An International Journal, English, 4 issues/year. Since 1968. American

Elsevier Publishing Co., Inc., 52 Vanderbilt Ave., N:ew York, N.Y. 10017.
In Cooperation with the International MetaIlographic Society.
2.
Microstructural Science. Proceedings of the Annual Technical Meetings of the International MetaIlographic Society. Since 1972. American Elsevier Publishing Co., Inc.,
52 Vanderbilt Ave., New York, N. Y. 10017.
3.
Praktische Metallographie / Practical Metallography. Bilingual (German-English). 12

issues/year. Detailed comprehensive index for each year, also every ten years. Since
1964. Dr. Riederer-Verlag GmbH, 60 Johannesstrasse, 7000 Stuttgart 1, Germany.
In Cooperation with the German Society for Metals (Deutsche GeseIlschaft fr
MetaIlkunde).
4.
Special Edition Series 01 Practical Metallography. Lecture Compilations of MetaIlographic Meetings. Mostly in German. Published irregularly since 1970. Dr. RiedererVerlag GmbH, 60 Johan1l.esstrasse, 7000 Stuttgart 1, Germany.
,I
.~
'.-
\.
NORTH AMERICA
Canada
Anglo Canadian Scientific Co.
P. O. Box 691
Don Mills, Ontario
AH materials and equipment for metaHographic and ceramographic specimen

preparation.
Tech-Met Canada Ltd.jLtee.

31 Progress Ave. 5
Scarborough (Toronto)
Ontario MIP 4S6
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Chemicals, microscopes, and apparatus foc miCrostructural anaysis.
.
Mexico
Tecnicos Argostal, S.A.
Apdo. Postal M-2511
Mexico 1, D.F.
United States
Buehler Ltd.
2120 Greenwood SI.
P. O. Box 1459
Evanston, Ill. 60204
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Chemicals, microscopes, and apparatus for microstructural analysis.
Buehler Ltd.
2525 North Loop West
Suite 124
Houston, Tex. 77008
AH materials and equipment for metallographic, petrographic, and ceramographic specimen preparation. Chemicals, microscopes, and apparatus for microstructural analysis.
Buehler Ltd.
9010 Reseda Blvd.
Suite liO
Northridge, Calif. 91324
'1.~ ._~:'
"
J!
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Chemicals,
microscopes, and apparatus for microstructural analysis.
113
112
References
8. J. Orlich, A. Rose, p, Wiest, Atlaslor Heat Treatment 01 Steels (in German)

Atlas zur Wiirembehandlung der Stiihle, Band 3, Verlag Stahleisen, Dsseldorf, 1973.
9. A. Schrader, A. Rose, Microstructures 01 Steels (in German)
De Ferri Metallographia, Teil 11, Gefge der Stiihle, Verlag Stahleisen, Dsseldorf,
1966.
10. R. W. ",ilson, Metallurgy and Heat Treatment 01 Tool Steels, McGraw-HilI Company
(U.K.) Ltd., Maidenhead, Berkshire, 1975.
11. "Atlas of Microstructures of Industrial AIIoys," Metals Handbook, 8th Ed., Vol.
Appendix D:
Some Suppliers of Metallographic

Equipment and Materials
12. "Fractography and Atlas of Fractographs," Metals Handbook, 8th Ed., Vol. 9,
American Society for Metals, Metals Park, Ohio, 1974.
13. "MetaIlography, Structures and Phase Diagrams," Metals Handbook, 8th Ed., Vol.
14. So urce Book in Failure Analysis, American Society for Metals, Metals Park, Ohio,
1974.
15. Translormation and Hardenability in Steels, Climax Molybdenum Corp., Ann Arbor,
Mich., 1967.
Journals of Mostly Metallographic Content

1.
Metallography. An International Journal, English, 4 issues/year. Since 1968. American

Elsevier Publishing Co., Inc., 52 Vanderbilt Ave., N:ew York, N.Y. 10017.
In Cooperation with the International MetaIlographic Society.
2.
Microstructural Science. Proceedings of the Annual Technical Meetings of the International MetaIlographic Society. Since 1972. American Elsevier Publishing Co., Inc.,
52 Vanderbilt Ave., New York, N. Y. 10017.
3.
Praktische Metallographie / Practical Metallography. Bilingual (German-English). 12

issues/year. Detailed comprehensive index for each year, also every ten years. Since
1964. Dr. Riederer-Verlag GmbH, 60 Johannesstrasse, 7000 Stuttgart 1, Germany.
In Cooperation with the German Society for Metals (Deutsche GeseIlschaft fr
MetaIlkunde).
4.
Special Edition Series 01 Practical Metallography. Lecture Compilations of MetaIlographic Meetings. Mostly in German. Published irregularly since 1970. Dr. RiedererVerlag GmbH, 60 Johan1l.esstrasse, 7000 Stuttgart 1, Germany.
,I
.~
'.-
\.
NORTH AMERICA
Canada
Anglo Canadian Scientific Co.
P. O. Box 691
Don Mills, Ontario

preparation.
Tech-Met Canada Ltd.jLtee.

31 Progress Ave. 5
Scarborough (Toronto)
Ontario MIP 4S6
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Chemicals, microscopes, and apparatus foc miCrostructural anaysis.
.
Mexico
Tecnicos Argostal, S.A.
Apdo. Postal M-2511
Mexico 1, D.F.
United States
Buehler Ltd.
2120 Greenwood SI.
P. O. Box 1459
Evanston, Ill. 60204
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Chemicals, microscopes, and apparatus for microstructural analysis.
Buehler Ltd.
2525 North Loop West
Suite 124
Houston, Tex. 77008
Buehler Ltd.
9010 Reseda Blvd.
Suite liO
Northridge, Calif. 91324
'1.~ ._~:'
"
J!
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Chemicals,
113
114
Suppliers of Metallographic Equipment
Max Erb Instrument Co.

2112 W. Burbank Blvd.
Burbank, Calif. 91506
AH materials and equipment for

graphic, petrographic, and
graphic specimen preparation.
scopes and optical instruments.
Excel Metallurgical
P. O. Box 1838
Springfield,. Mass. 01101
metaHoceramoMicrometaHoceramoMicro-
Fisher Scientific
711 Forbes Ave.
Pittsburgh, Pa. 15219
Offices throughout the U.S.A.
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation.
T. C. Jarrett Co.
P. O. Box 15397
Denver, Colo. 80215
115
Brazil
Panambra S.A.
Av. Senador Queiroz 150
Sao Paulo
AH materials and equipment for metallographic and ceramographic specimen

preparation.
POLITEC
Importacao e Comercia Ltda.
Rua Correa de Lemos 309
04140 Sao Paulo
Chile
Complete system in preparing metaHurgical and geological specimens.
Forestier-Intrumentos Scientificos
G. Busch & Cia. Ltda.
Casilla 191-V
Valparaiso
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Microscopes and optical instruments.
Leco Corp.
3000 Lakeview A ve.
St. Joseph, Mich. 49085

preparation.
Erwin Schneuer K
Casilla 9339
Moneda 1137/85-87
Santiago de Chile

preparation.
Struers Inc.
20102 Progre ss Drive
Cleveland, Ohio 44136
VWR Scientific IIlc.
3745 Bayshore Blvd.
Brisbane, Calif. 94005
Wilkens Anderson
4525 W. Division St.
Chicago, Ill. 60651

preparation. Chemicals, microscopes.
AH materials arid equipment for metaHographic, petrographic, and ceramographic specimen preparation.
Argentina
SOUTH AMERICA
,I
~
Lutz, Ferrando y Cia. S:A.
Florida ( R 5 )
Buenos
Aires
'Ji.
" \ ..
SIREX
Libertad 836
Buenos Aires
.... ,

preparation.
All materials and equipment for metaHographic, petrographic, and ceramographic
specimen preparation .
<.;"
GAMMA
Casilla No. 4316
La Paz
Colombia
Instrumentacin
H. A. Langebaek & Kier S.A.
Carrera 7 No. 48-59
Bogota

preparation.
Pantecnica S.A.
Apartado Aereo 7189
Bogota
Milciades Sanchez
Apartado Aereo 4675
Bogota
AH materials and equipment for metallographic, petrographic, and ceramographic specimen preparation.
Ecuador
Panandina Cia. Ltda.
P. O. Box 3882
Quito
SUMITEC
Suministros Tecnicos Ltda.
P. O. Box 259-4492
Guyaquil
preparation.
Peru
Bolivia
ji
AH materials and equipment for metaHographic, petrographic, and ceramographic sepcimen preparation.
H. W. Kessel
Apartado 552
Lima
114
Max Erb Instrument Co.

2112 W. Burbank Blvd.
Burbank, Calif. 91506

Excel Metallurgical
P. O. Box 1838
Springfield,. Mass. 01101
metaHoceramoMicrometaHoceramoMicro-
Fisher Scientific
711 Forbes Ave.
Pittsburgh, Pa. 15219
T. C. Jarrett Co.
P. O. Box 15397
Denver, Colo. 80215
115
Brazil
Panambra S.A.
Av. Senador Queiroz 150
Sao Paulo

preparation.
POLITEC
Importacao e Comercia Ltda.
Rua Correa de Lemos 309
04140 Sao Paulo
Chile
Complete system in preparing metaHurgical and geological specimens.
Forestier-Intrumentos Scientificos
G. Busch & Cia. Ltda.
Casilla 191-V
Valparaiso
AH materials and equipment for metaHographic, petrographic, and ceramographic specimen preparation. Microscopes and optical instruments.
Leco Corp.
3000 Lakeview A ve.
St. Joseph, Mich. 49085

preparation.
Erwin Schneuer K
Casilla 9339
Moneda 1137/85-87
Santiago de Chile

preparation.
Struers Inc.
20102 Progre ss Drive
Cleveland, Ohio 44136
VWR Scientific IIlc.
3745 Bayshore Blvd.
Brisbane, Calif. 94005
Wilkens Anderson
4525 W. Division St.
Chicago, Ill. 60651

preparation. Chemicals, microscopes.
AH materials arid equipment for metaHographic, petrographic, and ceramographic specimen preparation.
Argentina
SOUTH AMERICA
,I
~
Lutz, Ferrando y Cia. S:A.
Florida ( R 5 )
Buenos
Aires
'Ji.
" \ ..
SIREX
Libertad 836
Buenos Aires
.... ,

preparation.
<.;"
GAMMA
Casilla No. 4316
La Paz
Colombia
Instrumentacin
H. A. Langebaek & Kier S.A.
Carrera 7 No. 48-59
Bogota

preparation.
Pantecnica S.A.
Apartado Aereo 7189
Bogota
Milciades Sanchez
Apartado Aereo 4675
Bogota
Ecuador
Panandina Cia. Ltda.
P. O. Box 3882
Quito
SUMITEC
Suministros Tecnicos Ltda.
P. O. Box 259-4492
Guyaquil
preparation.
Peru
Bolivia
ji
AH materials and equipment for metaHographic, petrographic, and ceramographic sepcimen preparation.
H. W. Kessel
Apartado 552
Lima
116

Uruguay
Belgium
Casa Stapff
Casilla Correo 640
Montevideo
VenezuelaFerrum C .k ..
P. O. Box 70.624
Caracas
AH materials and equipment for me tallographic, petrographic, and ceramographic specimen preparation.
C. Hellmund & Cia. S.A.

A venida Pantin
Edificio Casa Hellmund
Caracas

preparation.
CENTRAL AMERICA
Dominican Republic
Quimico Industrial
Apartado de Correos No. 2058
Santo Domingo
AIl materials and equipment for metallographic, petrographic, and ceramographic specimen preparation.
Nicaragua
Roberto Teran G.
Apartado Postal 689
Managua, D.N.
All materials and equipment for me tallographic, petrographic, and ceramographic specinien preparation.
Panama
Promed, S.A.
Apartado 6281
Panama 5
All materials and equipment for me tallographic, petrographic, and ceramographic specimen preparation.
I
"
EUROPE
','
Austria
~
i ., \
Buehler-Met Handels GmbH

Rainerring 22
A-2500 Baden bei Wien
.. ....
~
C. Reichert Optische Werke AG

Hernalser Hauptstr. 219
A-1l70 Wien
J'
f 117
All materials and equipment for me taIlographic, petrographic, and ceramographic specimen preparation. Chemicals,
Special metaHographic equipment and
microscopes .
S. A. Analis
Rue Dewez, 14
B-5000 Namur
AH materials and equipment for metaHographic, petrographic, and ceramographic

specimen preparation.
BODSON (tablissements)
6, Quai St. Leonard
B-4000 Liege
AIl materials and equipment for metallographic and ceramographic specimen

preparation.
Denmark
Struers KfS
38 Skindergade
DK-1l59 Kopenhagen K
AH materia1s and equipment for nietallographic and ceramographic specimen

preparation. Chemicals and microscopes.
Finland
AB Axel von Knorringin
Tekn. BYRA
P. O. Box 20
Helsinki 38
AH materials and equipment for metallographic, petrographic, and ceramographic

Kaukomarkkinat Oy
F abianinka vt 9
He1sinki 13
All materials and equipment for me tallographic and ' ceramographic specimen
preparation.
France
ISI
Les Instruments Scientifiques
et Industriels
'
77, Avenue Parmentier
B. P. 254
75526 Paris
All materials and equipment for metallographic and ceramographic specimen

preparation.
Presi
2 Avenue Hector-Berlioz
F PoisatfGrenoble
38310 Eybens

preparation .
TestweH, S.A.
B. P. 176-09
Paris 75
All materials and equipment for metallographic, petrographic, and ceramographic

East Germany
Jenoptik Jena GmbH
Carl-Zeiss-Str. 1
DDR 69 Jena
Electropolishers and microscopes.
VEW Rathenower Optische Werke

DDR Rathenow
Grinding and polishing equipment.
116

Uruguay
Belgium
Casa Stapff
Casilla Correo 640
Montevideo
VenezuelaFerrum C .k ..
P. O. Box 70.624
Caracas
AH materials and equipment for me tallographic, petrographic, and ceramographic specimen preparation.
C. Hellmund & Cia. S.A.

A venida Pantin
Edificio Casa Hellmund
Caracas

preparation.
CENTRAL AMERICA
Dominican Republic
Quimico Industrial
Apartado de Correos No. 2058
Santo Domingo
AIl materials and equipment for metallographic, petrographic, and ceramographic specimen preparation.
Nicaragua
Roberto Teran G.
Apartado Postal 689
Managua, D.N.
All materials and equipment for me tallographic, petrographic, and ceramographic specinien preparation.
Panama
Promed, S.A.
Apartado 6281
Panama 5
All materials and equipment for me tallographic, petrographic, and ceramographic specimen preparation.
I
"
EUROPE
','
Austria
~
i ., \
Buehler-Met Handels GmbH

Rainerring 22
A-2500 Baden bei Wien
.. ....
~
C. Reichert Optische Werke AG

Hernalser Hauptstr. 219
A-1l70 Wien
J'
f 117
All materials and equipment for me taIlographic, petrographic, and ceramographic specimen preparation. Chemicals,
Special metaHographic equipment and
microscopes .
S. A. Analis
Rue Dewez, 14
B-5000 Namur

BODSON (tablissements)
6, Quai St. Leonard
B-4000 Liege
AIl materials and equipment for metallographic and ceramographic specimen

preparation.
Denmark
Struers KfS
38 Skindergade
DK-1l59 Kopenhagen K
AH materia1s and equipment for nietallographic and ceramographic specimen

preparation. Chemicals and microscopes.
Finland
AB Axel von Knorringin
Tekn. BYRA
P. O. Box 20
Helsinki 38

Kaukomarkkinat Oy
F abianinka vt 9
He1sinki 13
All materials and equipment for me tallographic and ' ceramographic specimen
preparation.
France
ISI
Les Instruments Scientifiques
et Industriels
'
77, Avenue Parmentier
B. P. 254
75526 Paris

preparation.
Presi
2 Avenue Hector-Berlioz
F PoisatfGrenoble
38310 Eybens

preparation .
TestweH, S.A.
B. P. 176-09
Paris 75

East Germany
Jenoptik Jena GmbH
Carl-Zeiss-Str. 1
DDR 69 Jena
Electropolishers and microscopes.
VEW Rathenower Optische Werke

DDR Rathenow
Grinding and polishing equipment.
118
Suppliers of MetalJographic Equipment
West Germany
Ernst Winter & Sohn

58 Osterstr.
D-2000 Hamburg 21
Polishing equipment, diamond pastes, and

tools.
AlI materials and equipment for metallographic and ceramographic specimen
preparation. Chemicals. Apparatus for
microstructural analysis and microscopes.
Buehler-Met GmbH
Lessingstr. 66 j 68
D-46 Dortmund
All materials and equipment for me tallographic, petrographic, and ceramographic

specimen preparation. Chemicals, microscopes, and apparatus for microstructural
analysis.
Jean Wirtz
73 CharIottenstr.
D-4000 Dsse1dorf I
P. F. Dujardin & Co.

16 Wiesenstr.
D-4000 Dsse1dorf-Heerdt
Materials and equipment for me tallographic specimen preparation. Chemicals.

Vogel's special reagent.
Great Britain
Elektroschmelzwerk Kempten
GmbH
P. O. Box 609
D-8000 Mnchen 33
Diamond pastes of polycrystalline diamonds.
K. & B. Grubbs Instrument

GmbH & Co. KG
15 Froschkonig-Weg
D-4000 Dsseldorf

preparation. Chemicals.
Iminex
14 Hauptstr.
D-6145 Lindenfels 2
Jenoptik Jena GmbH
6 Weender Landstr.
D-3400 Gottingen
Materials and equipment for metallographic specimen preparation.
R. Jung
P. O. Box 1120
D-6901 NusslochjHeidelberg
Microtome and micromilling devices.
Kontron GmbH
"
I Oskar v. Millerstr.
~;
D-8057 EchingjMnchent
Kulzer & Co. GmbH '
P. O. Box 1749
D-63/W Bad Homburg i " \"
Leco Instrumente GmbH
'"
Benzstr.
8011 Kirchheim bei M~chen
Special materials for metallographic specimen preparation. Microscopes and apparatus for microstructural analysis.
Multi Metal
P. O. Box 2705
D-4150 Krefeld
....'~ ,.~..
Plastics for cold mounting. Metal grinding

and polishing system.
preparation .
119
Materials and equipment for me tallographic specimen preparation.

analysis.
Electropolishers. Microscopes.
Sean Dia
P. O. Box 3031
D-5800 Hagen
Buehler-Met GmbH
35 Zeppe1instr.
D-n03 Ostfildern (Kemnat)j
Stuttgart . ~
Ernst Leitz GmbH

P. O. Box 2020
D-6330 Wetzlar
$1
Banner Scientific Ltd.

3, Three Spires Ave.
Coventry CV6 ILE

analysis.
Metallurgical Services
Reliant Works
Brockham, Betchworth
Surrey j England
Special metallographic
equipment.
Vickers Ltd.
Vickers Instruments
Haxby Rd.
York Y03 7SD

preparation.
materials
and
Greece
Carco-Technica Ltd.
23-24 Eleftherias
Sq. Athens 113

M. J. Priniotakis
5 Evrydikis Street
Athens 516

preparation.
lreland
Thomas H. Mason & Sons Ltd.
Crane Lane (off Dame St.)
Dublin 2

preparation.
ltaly
Etching chamber for evaporating of interference layers. Microscopes.
Gagliani & sas

Via Edolo 19
20125 Milano

Plastics for embedding specimens.
W. Pabisch S.p.A.
Via Borromei I B j 4
1-20123 Milano

preparation.
118
Suppliers of MetalJographic Equipment
West Germany
Ernst Winter & Sohn

58 Osterstr.
D-2000 Hamburg 21
Polishing equipment, diamond pastes, and

tools.
AlI materials and equipment for metallographic and ceramographic specimen
preparation. Chemicals. Apparatus for
microstructural analysis and microscopes.
Buehler-Met GmbH
Lessingstr. 66 j 68
D-46 Dortmund

analysis.
Jean Wirtz
73 CharIottenstr.
D-4000 Dsse1dorf I
P. F. Dujardin & Co.

16 Wiesenstr.
D-4000 Dsse1dorf-Heerdt
Materials and equipment for me tallographic specimen preparation. Chemicals.

Vogel's special reagent.
Great Britain
Elektroschmelzwerk Kempten
GmbH
P. O. Box 609
D-8000 Mnchen 33
Diamond pastes of polycrystalline diamonds.
K. & B. Grubbs Instrument

GmbH & Co. KG
15 Froschkonig-Weg
D-4000 Dsseldorf

preparation. Chemicals.
Iminex
14 Hauptstr.
D-6145 Lindenfels 2
Jenoptik Jena GmbH
6 Weender Landstr.
D-3400 Gottingen
Materials and equipment for metallographic specimen preparation.
R. Jung
P. O. Box 1120
D-6901 NusslochjHeidelberg
Microtome and micromilling devices.
Kontron GmbH
"
I Oskar v. Millerstr.
~;
D-8057 EchingjMnchent
Kulzer & Co. GmbH '
P. O. Box 1749
D-63/W Bad Homburg i " \"
Leco Instrumente GmbH
'"
Benzstr.
8011 Kirchheim bei M~chen
Special materials for metallographic specimen preparation. Microscopes and apparatus for microstructural analysis.
Multi Metal
P. O. Box 2705
D-4150 Krefeld
....'~ ,.~..
Plastics for cold mounting. Metal grinding

and polishing system.
preparation .
119
Materials and equipment for me tallographic specimen preparation.

analysis.
Electropolishers. Microscopes.
Sean Dia
P. O. Box 3031
D-5800 Hagen
Buehler-Met GmbH
35 Zeppe1instr.
D-n03 Ostfildern (Kemnat)j
Stuttgart . ~
Ernst Leitz GmbH

P. O. Box 2020
D-6330 Wetzlar
$1
Banner Scientific Ltd.

3, Three Spires Ave.
Coventry CV6 ILE

analysis.
Metallurgical Services
Reliant Works
Brockham, Betchworth
Surrey j England
Special metallographic
equipment.
Vickers Ltd.
Vickers Instruments
Haxby Rd.
York Y03 7SD

preparation.
materials
and
Greece
Carco-Technica Ltd.
23-24 Eleftherias
Sq. Athens 113

M. J. Priniotakis
5 Evrydikis Street
Athens 516

preparation.
lreland
Thomas H. Mason & Sons Ltd.
Crane Lane (off Dame St.)
Dublin 2

preparation.
ltaly
Etching chamber for evaporating of interference layers. Microscopes.
Gagliani & sas

Via Edolo 19
20125 Milano

Plastics for embedding specimens.
W. Pabisch S.p.A.
Via Borromei I B j 4
1-20123 Milano

preparation.
120
Liechtenstein
Balzers AG. High-Vacuum Techn.
and Thin Film Techn.
FL-9496 Balzers
Apparatus for evaporation of interferencu

layers (Pepperhoff etch).
Netnerlands
Lameris Instrumenten N . V.
Biltstraat 149
Utrecht
VIBA, N .V.
Koningin Emmakade 199
The Hague
AIl materials and equipment for metallo

graphic and ceramographic specimcn
preparation.
AH materials and equipment for metallo
graphic, petrographic, and ceramographio
specimen preparation. Microscopes and
optical instruments.
Norway
A/S Christian Falchenberg
N edre Slottsgate 23
Oslo
Nerliens Kemisk-Tekniske
Aktieselskap
Tollbugt. 32
Oslo 1
All materials and equipment for metallo

graphic, petrographic, and ceramographio
All materials and equipment for metallo
graphic and ceramograpbic specimoll
, preparation.
Portugal
Equipamentos de Laboratorio Lda.
Apartado 1, 100
Lisbon 1
Viara Comercail (Mquinas) Lda.
Rua Delfim Ferreira, 509
Porto
Spain
!
I
All materials and equipment for metallo.

graphic, petrographic, and ceramographiu
All materials and equipment for metallo .
grapbic and ceramographic specirnllll .
preparation.
) .
C. R. Mars\ S.A. , ~
Calle Valencia 333
Barcelona-9
P":A.C.I.S.A. , , , \.,
P. O. Box 7023
Madrid 5
AIl materials and equipment for metallo.

graphic and ceramographic specirnllll
preparation.
AIl materials and equipment for metallu.
grapbic, petrographic, and ceramographl\l
Sweden
Bergman & Beving AB,
Karlavagen 76
Stockholm 10
All materials and equipment for metnll'h

graphic and ceramographic specimtlll
preparation.
Brandt Optik AB
P. O. Box 27053
S 102 51 Stockholm
121
All materials and equipment ror metallographic, petrographic, and ceramographic

specimen preparation. Microscopes and
optical instruments.
Switzerland
Carl Bittmann
Herzogenmhlestr. 14
CH-8015 Zrich .
BuehIer-Met AG
Zollfreilager Dreispitz
CH-4023 Basel
All materials and equipment for me tallographic and ceramographic specimen

preparation.
AH materials and equipment for metallographiC, petrographic, and ceramographic
analysis.
Yugoslavia
HERMES
Mosa Pijade 27
61000 Ljubljana
Jugolaboratorija
VI. 7 Jula No . 44
11000 Beograd

preparation.
ASIA
Beas Enterprises
GPO Box 787
acca 2

HongKong
;:~ Schmidt & Co.
'1',
t,;
!'.
;~i
P. O. Box 297
Hong Kong
AH materials and equipment for me tallographic, petrographic, and ceramographic

~!. India
~;;
J . T. Jagtiani
National House
" Tulloch Rd.
~\ Apollo Bunder
(r Bombay 1
1',
{-

preparation.
122
123
Malaysia
Indonesia
P. T. Ahrend Indonesia
Djalan Kapten P. Tendean 19
(Hegarmanah Kulon)
Bandung
Schmidt Scientific (Pte) Ltd.
Katong P.-O.Box 76
Singapore 15

preparation.
Jebsen & Jessen (M) Sedn. Bhd.

Denmark House
84 Jalan Ampong
Kuala Lumpur
AH material s and equipment for metallographic and ceramographic specimen

preparation.

Schmidt Scientific Sdn. Bhd.

P. O. Box 592
Kuala Lumpur 08-03

Nepal
Jopan
Kasai Shoko Co.
5-6-37 Tsanashimahigashi
Kohoku-ku
Yokohama 223
Marumoto Kogyo Co.
2-1 Kyobashi
Chuo-ku
Tokyo 104

preparation.
Maruto Co.
1-1-10 Yushima
Bunkyo-ku
Tokyo 113
Rigaku Denki Co.
2-9-8 Sotokanda
Chiyoda-ku
Tokyo 101
Sankei Co. Ltd.
Tsunashima Dai-2 Bldg.
No. 20-12, 3-Chome, Jushima
Bunkyo-ku
Tokyo
Yamamoto Kagaku
Kogu Kenkyusha
'~
2-15-4 Sakaemachi
\
Hunabashi
Chiba 273
Yuni& Kogaku Co. '. \.
2-20-9 Shimura
Itabashi-ku
Tokyo 174
Precise cutting machines. Apparatus for

determination of the crystal orientation by
etch figures.
All materials and equipment for metallographic and ceramograpruc specimen

preparation. Standard specimens for metallography (for example, grain size, carbon content).
Portable metallography apparatus.

analysis.
Standard specimens for metaHography (for
example, grain size, carbon content.
hardness).
".,..

Pakistan
Nazer & Co.
Habib Bank Building
Victoria/Bunder Road
Karacru 3

preparation.
Philippines
Engineering Equip. Inc.
P. O. Box 7160
Airmail Exchange Office
Manila Int'l. Airport 3120

Inhelder-Don Baxter Lab. lnc.

41, Pioneer St.
Mandeluyong
Rizal D-713

preparation.
Singapore
Jebsen & Jessen (S) Pte. Ltd.
10th Floor Supreme House
Penang Road
Singapore

preparation.
South Korea
"
":...
Gita Trading Co.

GPO Box 479
Katmandu
Optical microscopes. Abrasives and polishing machines.
Shin Han Scientific Co. Ltd.

Int'l P. O. Box 1250
Seoul

Sri Lanka
Laboratory Equipment Co.
3rd Floor, Y.M.B.A. Bldg.
Colombo 1

122
123
Malaysia
Indonesia
P. T. Ahrend Indonesia
Djalan Kapten P. Tendean 19
(Hegarmanah Kulon)
Bandung
Schmidt Scientific (Pte) Ltd.
Katong P.-O.Box 76
Singapore 15

preparation.
Jebsen & Jessen (M) Sedn. Bhd.

Denmark House
84 Jalan Ampong
Kuala Lumpur
AH material s and equipment for metallographic and ceramographic specimen

preparation.

Schmidt Scientific Sdn. Bhd.

P. O. Box 592
Kuala Lumpur 08-03

Nepal
Jopan
Kasai Shoko Co.
5-6-37 Tsanashimahigashi
Kohoku-ku
Yokohama 223
Marumoto Kogyo Co.
2-1 Kyobashi
Chuo-ku
Tokyo 104

preparation.
Maruto Co.
1-1-10 Yushima
Bunkyo-ku
Tokyo 113
Rigaku Denki Co.
2-9-8 Sotokanda
Chiyoda-ku
Tokyo 101
Sankei Co. Ltd.
Tsunashima Dai-2 Bldg.
No. 20-12, 3-Chome, Jushima
Bunkyo-ku
Tokyo
Yamamoto Kagaku
Kogu Kenkyusha
'~
2-15-4 Sakaemachi
\
Hunabashi
Chiba 273
Yuni& Kogaku Co. '. \.
2-20-9 Shimura
Itabashi-ku
Tokyo 174
Precise cutting machines. Apparatus for

determination of the crystal orientation by
etch figures.
All materials and equipment for metallographic and ceramograpruc specimen

preparation. Standard specimens for metallography (for example, grain size, carbon content).
Portable metallography apparatus.

analysis.
Standard specimens for metaHography (for
example, grain size, carbon content.
hardness).
".,..

Pakistan
Nazer & Co.
Habib Bank Building
Victoria/Bunder Road
Karacru 3

preparation.
Philippines
Engineering Equip. Inc.
P. O. Box 7160
Airmail Exchange Office
Manila Int'l. Airport 3120

Inhelder-Don Baxter Lab. lnc.

41, Pioneer St.
Mandeluyong
Rizal D-713

preparation.
Singapore
Jebsen & Jessen (S) Pte. Ltd.
10th Floor Supreme House
Penang Road
Singapore

preparation.
South Korea
"
":...
Gita Trading Co.

GPO Box 479
Katmandu
Optical microscopes. Abrasives and polishing machines.
Shin Han Scientific Co. Ltd.

Int'l P. O. Box 1250
Seoul

Sri Lanka
Laboratory Equipment Co.
3rd Floor, Y.M.B.A. Bldg.
Colombo 1

124
Taiwan

Thailand
Sis Company. Ltd.
1248 Nakornchaisri Rd.
Bangkok 3

AUSTRALIA
H. B. Selby & CO. Pty. Ltd.
352-368 Ferntree Gully Rd.
N otting Hill, Victoria 3168
Watson Victor Ltd.
P. O. Box 100
North Ryde, NSW 2113

preparation.
NEW ZEALAND
Watson Victor Ltd.
Physics & Engin.
P. O. Box 1180
Wellington

Geo. W. Wilton & CO. Ltd.

77 CarHon Gore Rd.
New Market
Auckland, C.l

preparation.
Soofer CO.
Khark & Shahreza Avenue
Teheran

IMACO Ltd.
Chiaban Seza~ar lit
Teheran
All materials and equipment for metaIlographic and ceramographic specimen

preparation.
Iraq
Leon Kouyoumdijan & CO.
Fixit House
Sa' Adoon St.
Alwiya
Baghdad
Cyprus
,
Advanced Technical Services.
.
Egypt
Johs. Rieckermann
140, Tehrir St., 6th Floor
Cairo, A.R.E.
\
' ...
":.~,

Agentex Ltd.
3 Bograshov
Tel-Aviv
L. Kardos
P. O. Box 11033
TelcAviv

AH materials and equipment for metaIlographic and ceramographic specimen

preparation.
AH materials and equipment for me taIlographic, pe~rographic, and ceramographic
Jordan
Mouasher Cousins
P. O. Box 1387
Amman
AIl materials and equipment for metallographic, petrographic, and ceramographic

Lebanon
Comptoir D'lectricit
AV. Bechara Khoury
Beirut

Saudi Arabia
Abduhnajeed Y. AI-Reshaid
P. O. Box 363
AI-Khobar
AIl material s and equipment for metallographic, petrographic, and ceramographic

Syria
The Arab Trad. & Eng. Office
Port Said St. 137
Damascus
",-
AH materials and equipment for me taIlographic and ceramographic specimen

preparation.
Israel
:~MIDDLE EAST
.p
125
Iran
San Kwang Instr. CO. Ltd.

No. 20, Yung Sui Rd.
Taipei 100
GmbH. :.
P. O. Box 2349
Nicosia

124
Taiwan

Thailand
Sis Company. Ltd.
1248 Nakornchaisri Rd.
Bangkok 3

AUSTRALIA
H. B. Selby & CO. Pty. Ltd.
352-368 Ferntree Gully Rd.
N otting Hill, Victoria 3168
Watson Victor Ltd.
P. O. Box 100
North Ryde, NSW 2113

preparation.
NEW ZEALAND
Watson Victor Ltd.
Physics & Engin.
P. O. Box 1180
Wellington

Geo. W. Wilton & CO. Ltd.

77 CarHon Gore Rd.
New Market
Auckland, C.l

preparation.
Soofer CO.
Khark & Shahreza Avenue
Teheran

IMACO Ltd.
Chiaban Seza~ar lit
Teheran
All materials and equipment for metaIlographic and ceramographic specimen

preparation.
Iraq
Leon Kouyoumdijan & CO.
Fixit House
Sa' Adoon St.
Alwiya
Baghdad
Cyprus
,
Advanced Technical Services.
.
Egypt
Johs. Rieckermann
140, Tehrir St., 6th Floor
Cairo, A.R.E.
\
' ...
":.~,

Agentex Ltd.
3 Bograshov
Tel-Aviv
L. Kardos
P. O. Box 11033
TelcAviv

AH materials and equipment for metaIlographic and ceramographic specimen

preparation.
AH materials and equipment for me taIlographic, pe~rographic, and ceramographic
Jordan
Mouasher Cousins
P. O. Box 1387
Amman
AIl materials and equipment for metallographic, petrographic, and ceramographic

Lebanon
Comptoir D'lectricit
AV. Bechara Khoury
Beirut

Saudi Arabia
Abduhnajeed Y. AI-Reshaid
P. O. Box 363
AI-Khobar
AIl material s and equipment for metallographic, petrographic, and ceramographic

Syria
The Arab Trad. & Eng. Office
Port Said St. 137
Damascus
",-
AH materials and equipment for me taIlographic and ceramographic specimen

preparation.
Israel
:~MIDDLE EAST
.p
125
Iran
San Kwang Instr. CO. Ltd.

No. 20, Yung Sui Rd.
Taipei 100
GmbH. :.
P. O. Box 2349
Nicosia

126
Teehnieal & Laboratory .

Applianees
Pardoss Street 79
Kassas & Sadate Building
Damaseus
AH materials and equipment fOI metallographie and eeramographic speeimen

preparaton.
Turkey.
Alemdar Enternasyonal A.S.
Veli Alemdar Han 717
Karakoy, Istanbul

preparation.
AFRICA
Algeria
Scientifix
3, Boulevard Colonel
Amirouehe
AIger

preparation.
Ango/a
Equipamentos Teenieos Lda.
Rua Serpa Pinto 391
Caixa Postal 6319
Luanda
All materials and equipment for metallographic, petrographic, and ceramographie

Morocco
Chimilabo
193 , Avenue des Porees
Atmes Royales
Casablanea
Jaeques Guy-Moyat \
Passage Sumica
Casablat}.ea
>,
, \ "
AIl materials and equipment for metallographic, pettographie, and ceramographie

speeimen preparation.
preparation.
Mozambique
Artur Ballossini
P. O . Box 288
Lourenco Marques
Teleeom-Equipal
Telecomunicacoes de Mocambique
C. Postal 310
Maputo
All materials and equipment for metallographic, petrographic, and ceramographie

speeimen preparation.
127
Rhodesia
Taeuber & Corssen (Pty) Ltd.
P. O. Box 3190
Salisbury
AH materials and equipment ror metaHographic, petrographic, and ceramographic

South Africa
OPTOLABOR
3rd Floor, Standard House
40 de Korte St.
Braamfontain
Johannesburg
T & C Scientific
Suppliers (Pty) Ltd.
P. O. Box 1366
Johannesburg
AH materials and equipment for metallographic . and ceramographic specimen

preparation.

Zambia
Baird & Tatlock
(Zambia) Ltd.
P. O. Box 1097
BruneH Rd.
Ndola

Index
AmBy and ArrBYI compounds, 68-69
Aluminum and aluminum alloys, 39-43
Amalgamates, 71
Antimony and antimony alloys, 48-49.
Cobalt and cobalt alloys, 51-53

Copper and copper alloys, 58-61
Corrosion-resistant steels, 61-68
Current-voltage characteristics, 18-19
Cutting tools, cobalt-base, 52, 53
Bearing alloys, 81, 84, 85

Bearing metaIs, 81
Beryllium and beryllium alloys, 46-48
Bibliographic references, 108-112
general textbooks and reviews, 109-110
handbooks, compilations and tables,
111-112
joumals of mostly metallographic
content, 112
metaIlographic preparation, 11O-111
safety and toxicology, 108-109
Bismuth and bismuth alloys, 48-49
Borides,98
Brasses, 58-61
Bronzes
aluminum bronzes, 58-61
beryllium bronzes, 59
copper bronzes, 58-61
lead bronzes, 80
silicon bronzes, 58
special bronzes, 59
tin bronzes, 59, 60
I
>
t
j'
:lO-
i.
",
' .... ,,~
"
cI1
Cadmium and cadmium aIloys, 50-51

Carbides,94-96
Cast iron, 61-68
Cathodic vacuum etching, 29
Cemented carbides, 52, 53, 78
Cerium,83
Cermets, 99-100
Chemical polishing solutions, 20
Chemicals used to prepare eichants in
Chapters 2 and 3, 105-107
Chromium and chromium alloys, 54-57
Cleaning, 23-24
drying after, 24
rinsing, 28
ultrasonic cleaning, 24
129
Drying of specimens after cleaning, 24

Duralumin, 41
Dysprosium, 83
Electrolytes, 16-18
Electrolytic polishing, 16-20
Erbium, 83
Etching, 24-34
anodic etching (anodizing), 25, 28, 31,
32 (see also electrolytic etching)
attack-polishing, 21, 31, 32
cathodicetching, 31, 32
chemical etching (see- '
electrochemical etching)
cold etching, 31, 32
controlled etching, 28,31,32
conventional (classical) chemical
etching, 25, 27, 30
crystaI-figure etching, 31, 32
deep etching, 31,32
dislocation etching, 31, 32
dissolution etching, 32, 33
double etching, 32,33
drop etching, 32, 33
drop etching, 32, 33
dry etching, 32, 33
electrochemicaI etching, 25-29, 33
electrolytic etching, 28, 30 (see also
anodic etching)
etch rinsing, 32, 33
eutectic-cell etching,' 32, 33
grain-boundary etching, 32, 33
grain-contrast etching, 32, 33
heat tinting, 27, 32, 33
hot etching, 32, 33
identification etching, 32, 33
immersion etching, 32, 33
immersion etching, cycJic, 32, 33
130/lndex
Etching (continued)
ion etching , 25, 29 , 30
long-tenn etching, 32, 33
macroetching, 32, 33
microetching, 32, 33
multiple etching, 32, 33
networkekhing, 32, 33
optical etching, 25, 33
physical etching, 25, 29, 33
potentiostatic etching, 25, 28, 30, 33
precipitation etching, 27, 32, 33
prirnary etching, 32, 34
printing, 32, 34
reproducible etching, 30
secondary etching, 32, 34
segregation etching; 34
short-tenn etching, 32, 34
shrink etching, 32, 34
staining, 32, 34
strain etching, 34
swabbing, 32, 34
thennal etching, 25, 29, 32, 34
wet etching, 32, 34
wipe etching, 39
Etching nomenclature; explanation of
etching terms, 31-34
Etching, post-treatment, 28-29
Europium, 83
Evaporation of interference layers,
25, 29, 30
Flow lines in steeI forgings, 66
Gadolinium, 83
Gennan silver, 60
f
Germanium and gennanium ~Ioys, 68-69
Gold and gold alloys, 43-46 ~
Grinding, 8-16, 22 \
'
automatic grinding, 22 . ,
coarse grinding, 8, 9, 11 I
fine gtinding, 8, 11 , ' ., t
mechanical grinding, 9
...'
pre-grinding, 11
pressure, time, velocity, .15 '.
specimen motion in, .15 "',.'"
substrates, 15-16
Grinding compounds, 11-15
Grinding substrate materials, 15
Hafnium and hafnium a!loys, 70-71
Hardened steels, 61, 64-67
Hazardous materials, precautions

in handling, 103-104
Heat-resistant steels, 61-68
Holmium, 83
Indium and indium alloys, 50-51
Iridium and iridium alloys, 43-46
Iron and iron alloys, 61-68
Iron oxide layers, 100
Lanthanum and lanthanum alloys, 83
Lead and lead alloys, 79
Lutetium, 83
Magnesium and magnesium alloys, 72-74
Magnetic aIloys, 52
Manganese and manganese alloys, 75
Marking of specirnens for identification,
7-8
Mercury amalgamates, 71 , 72
Metal compounds
borides, 98
carbides, 94-96
nitildes, 97
.
oxides, 92-94
phosphides and sulfides, 98-99
Metallog~aphic equipment and materials,
suppliers, 113-127
Africa, 126-127
Asia, 121-124
Australia, 124
Central America, 116
Europe, .116-121
Middle East, 124-126
New Zealand, 124
North merica, 113-114
South America, 114-116
Microtome cutting, 8, 16, 23
. Molybdenum and molybdenwn alloys,
.
54-57
Monel metal, 61, 76, 77
Mounting of specimens, 3-7
c1amping, 3, 4
plastic embedding, 4-6
properties of mounting materials, 6-7
Multiple polishing, 21
Muntz metal, 61
Neodyrnium, .83
Nickel and nickeI alloys, 75-79
Niobium and niobium alloys, 54-57
Index /131
Nitride metal compounds, 97
Nondestructive metallographic testing,
34-35
Rhenium and rhenium a1loys, 54-57

Rhodium and rhodium a1loys, 43-46
Ru~henium and ruthenium alloys, 43-46
Osmium and osmium alloys, 43-46

Oxide metal compounds, 92-94
Samarium, 83
Selenium and selenium alloys, 68-69
Semiconductors, 68-69
Silicon and silicon alloys, 68-69
Silver and sil ver alloys, 37-39
Silver solders , 38 , 39
Solder alloys containing cadmium, 50
Special steels, 63
Specimen preparation, general, l
Specimen sectioning, 2-3
Specimen storage, 29-30
Stainless steels, 64-67
Steels, 61-68
Stellite, 51, 53
Structural steels, 61-68
Sulfide inc\usions in steel, 63
Sulfide-metal compounds, 98-99
Superalloys, 52, 53, 76-79
Palladium and palladium alloys, 43-46

Phosphide and sulfide compounds, 98-99
Phosphorus distribution in steel , 63
Platinum and platinum alloys, 43-46
Plutonium and plutonium alloys, 81-83
Polishing, 8-23
anodic polishing, 16-21 (see also
electrolytic polishing)
attack-polishing, 21 , 31, 32
automatic polishing , 22
chemical polishing, 20-21
coarse polishing, 8, 11 .
electrolytic lapping, 21-22
electrolytic polishing, 16-21 (see also
anodic polishing)
etch-polishing, 21
final polishing, 1I
fine polishing, II
mechanical polishing, 9-11
pre-polishing, 11
pressure, time, velocity, 15
specimen motion in, 15
substrates, 15
Polishing compounds, 10-14
Polishing fluids, 14-15
Polishing methods, combinations, 21-22
Polishing methods, evaluation , 22-23
Polishing substrate materials, 15-16
Praseodyrnium, 83
Precautionary measures
in handling hazardous materials, 103-104
with perchloric acid, 17-18
Precious metals, 43-46
Preparation ofmetaIs and alloys, 37-90 (see
also entries under specific metals)
Preparation of special ceramics and cermets
(ceramography) , 91-101 (see al so
entries under Metal compounds)
Primary grain structure in steels, 63
Promethium, 83
Pure iron, 64, 66, 67
Rare earth metals, 83
Redox processes , 25-26
Talitalum and tantalum a1loys, 54-S7

Taper sectioning of specimens, 5-6
Tellurium and tellurium a1loys, 68-69
Terbium, 83
Thallium and thallium alloys, 50, 51
Thorium and thorium a1loys, 81-83
Thulium, 83
Tin and tin alloys, 84-85
Titanium and titanium a1loys, 85-88
Tombac, 61
Tool steels , 64-66
Tungsten and tungsten alloys, 54-57
Type metal, ,80, 81
Ultrasonic cleaning, 24
Uranium and uranium alloys, 81-83
Vacuum impregnation, 5
Vanadium and vanadium alloys, 54-57
White metals (babbitts), 80, 81, 84, 85
Ytterbium, 83
Zinc and zinc alloys, 88-90
Zinc platings, 90
Zircaloy, 70, 71
Zirconium and zirconium a110ys, 70-71

Metallographic Etching-Gunter Petzow

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Metallographic

Translators from the German version:

Rosemarie Koch and James A. Nelson

AMERICAN SOCIETY FOR METALS

~ Metals Park, 0hio 44073

A I" ON., ....

OriginaUy published in 1976 as

Enlarged English translation copyright ' 1978 - ,.--- ..: . ", .. -- . ~

No part of this book may be reproduced , stored in a

To Robert 1. Gray and E. Daniel A lbrecht,

Library of Congress Cataloging in Publication Data

PRINTED IN TH E UNITED STATES OF AMERICA

A I" ON., ....

OriginaUy published in 1976 as

Enlarged English translation copyright ' 1978 - ,.--- ..: . ", .. -- . ~

No part of this book may be reproduced , stored in a

To Robert 1. Gray and E. Daniel A lbrecht,

Library of Congress Cataloging in Publication Data

PRINTED IN TH E UNITED STATES OF AMERICA

In the last few years, metallographic prepara.tion techniques have been

Preface to the German Edition

2. Preparation of Metals and Alloys-37

3. Preparation of Special Cerarnics and Cermets

APPENDIX A: Suggestions for Handling Hazardous

APPENDIX D: Sorne Suppliers oC Metallographic Equipment

3. Preparation of Special Cerarnics and Cermets

APPENDIX A: Suggestions for Handling Hazardous

APPENDIX D: Sorne Suppliers oC Metallographic Equipment

Technical Tips Cor Preparation oC

The methods of preparing metallographic sections for macroscopic

Technical Tips for Preparation of Specimens

Technical Tips for Preparation of Specimens

Specimen Sectioning (Fig. 1)

Ult rasonic _1 '

.ow Speed Oiamond

The first step in specimen preparation-selection and separation of

Metals and AUOYS1

Flg. l. Methods of metallographic specimen sectioning.

Fig. 2. Methods of metallographic mounting.

Technical Tips for Preparation of Specimens

Technical Tips for Preparation of Specimens

Specimen Sectioning (Fig. 1)

Ult rasonic _1 '

.ow Speed Oiamond

The first step in specimen preparation-selection and separation of

Metals and AUOYS1

Flg. l. Methods of metallographic specimen sectioning.

Fig. 2. Methods of metallographic mounting.

Technical Tips for Preparation of Specimens

in a single mount or when automatic devices are to be used in further

Fig. 3. Examples of fixtures used

Resin + Pressure + Heat

Hot mounting (compression molding) requires the use of a press which

gene rally have similar mechanical and chemical characteristics so that

Technical Tips for Preparation of Specimens

Fig. 4. Cold mounting of metallographie

Room-temperature-curing piastics are also advantageous when mounting

Technical Tips for Preparation of Specimens

in a single mount or when automatic devices are to be used in further

Fig. 3. Examples of fixtures used

Resin + Pressure + Heat

Hot mounting (compression molding) requires the use of a press which

gene rally have similar mechanical and chemical characteristics so that

Technical Tips for Preparation of Specimens