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HSEYN KASIRGA
030040323
GROUP
Kasrga,
TABLE OF CONTENTS
I.
Introduction
1. Definitions
a. Metallography
b.
Microscopy
c. Macroscopy
II.
Experimental Procedure
1. Specimen Preparation
a. Grinding
b. Polishing
c. Etching
2. Microscopical Examination
a. Objective
b. Experiment
3. Macroscopical Examination
a. Objective
b. Experiment
i. Sulphur Printing
ii. Flow Lines
iii. Welded Sections
III.
Data Analysis
1. For Microscopical Examination
2. For Macroscopical Examination
IV.
V.
Conclusion
VI.
References
VII.
VIII. Appendix
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I. INTRODUCTION
1. DEFINITIONS
a. Metallography:
Metallography is the science and art of preparing a metal surface for analysis by
grinding, polishing, and etching to reveal microstructural constituents. After preparation, the
sample can easily be analyzed using optical or electron microscopy. A skilled technician is
able to identify alloys and predict material properties, as well as processing conditions by
metallography alone. There are two examination methods in Metallography:
1. Microscopy
2. Macroscopy
b. Microscopy:
In microscopy, the examination of the prepared specimen is done with the optical
microscopes applying magnifications from 10x to 2000x. This examination provides
information regarding the morphology and distribution of constituent phases as well as the
nature and pattern of crystal imperfections.
c. Macroscopy:
In this method the examination of the material (generally metals and alloys) is done
by the unaided eye or a low-power microscope with a magnification up to 10x. This
examination method provides information about the nature of inhomogenities, flow lines,
segregations, and fabricating defects that cannot be examined by microscopy. However, these
data represents the characteristics only at a particular section of the material.
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grains of silicon carbide per square inch in the order from coarser to finer. Most grinding of
metallographic specimen is performed by manually holding the specimen with its surface
against that grinding material covering discs. To establish and maintain a flat surface over the
entire area being ground, equal pressure must be applied on both sides of the specimen
avoiding any rocking motion that will produce a convex surface. Success in grinding depends
in part on the pressure applied to the specimen. A very light pressure removes insufficient
metal. Somewhat heavier pressure produce polishing, while still heavier pressure brings about
the desired grinding action. Very heavy pressure results in nonuniform scratch size, deep
gouges, and embedded abrasive particles. Generally, a medium to moderately heavy pressure
applied firmly gives the best results. To avoid from excessive warm of the specimen water is
used as cooler.
The grade of the silicon carbide paper to begin the grinding operation is the coarsest
paper, 180 grade. Always light pressure is used, applied at the centre of the specimen and
continued grinding until all the blemishes have been removed, the sample surface is flat, and
all the scratches are in a single orientation. Then the sample is washed in water and moved to
the next finer grades, orienting the scratches from the previous grade normal (90) to the
rotation direction. This makes it easy to see when the coarser scratches have all been
removed. After the final grinding operation on 1000 paper, the sample is washed in water and
dried before moving to the polishing operation.
b. Polishing:
Polishing is the final step in production a surface that is flat, scratch free, and mirror
like in appearance. Such a surface is necessary for subsequent accurate metallographic
interpretation, both qualitative and quantitative. The polishers consist of rotating discs
covered with soft cloth (broadcloth) impregnated with diamond particles and an oily
lubricant. Typically, a sample is polished with slurry of alumina (Aluminum oxide is a
chemical compound of aluminum and oxygen with the chemical formula Al 2O3. It is also
commonly referred to as alumina in the materials science communities.), silica, or diamond as
polishing agent to produce a scratch free mirror surface. In polishing operation, alumina is
used to prevent excessive warm of specimen instead of water in grinding operation. During
polishing the specimen should be rotated or moved around the wheel so as to give an even
polish, but excessive pressure should be avoided. After polishing the specimen should be
thoroughly cleaned and dried without any contact of hands directly with the polished surface
of specimen.
c. Etching:
The purpose of etching is two-fold. Grinding and polishing operations produce a
highly deformed, thin layer on the surface which is removed chemically during etching.
Secondly, after polishing, the microstructural constituents of the sample are revealed by using
a suitable chemical or electrolytic etchant .The etchant attacks the surface with preference for
those sites with the highest energy, leading to surface relief which allows different crystal
orientations, grain boundaries, precipitates, phases and defects to be distinguished in reflected
light microscopy. There are many tried and tested etchants available, but the ideal etchant is
dependent on sample composition, and the microstructural feature(s) of interest. As a quide
following etchants are commonly used:
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- Nital (ethyl alcohol + 2% HNO3)
copper alloys
- Mixed Acids
aluminum alloys
- Dilute HCl
zinc alloys
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2. MICROSCOPICAL EXAMINATION
After the specimen prepared for examination, the microstructural study of the
material can begin. With this examination information can be provided about the distribution
and morphology of the phases and if their properties are known, a quantitative analysis of the
micrographs provides information about the bulk properties of the specimen. Microstructural
examination can provide quantitative information about the following parameters:
Specimens grain size
Interfacial area per unit volume
Dimensions of constituent phases
Amount and distribution of phases
a. Objective:
To examine the microstructural characteristics of prepared metal specimen
employing magnifications with an optical microscope.
b. Experiment:
First, the specimen is prepared as said in the section of specimen preparation. That is
the specimen grinded, polished and finally etched. Then with the aid of microscope
successively magnifications are used to resolve the fine details and obtain a good image with
a good contrast. In focusing, the stage is gradually moved towards the objective and when the
image appears, focusing is completed with the fine adjustment. However, something
important that must be considered is that the prepared surface represents a two-dimensional
picture whereas the structure of specimen exists in three dimensions.
3. MACROSCOPICAL EXAMINATION
In this method the examination of the material (generally metals and alloys) is done
by the unaided eye or a low-power microscope with a magnification up to 10x. This
examination method provides information about the nature of inhomogenities, flow lines,
segregations, and fabricating defects that cannot be examined by microscopy. However, these
data represents the characteristics only at a particular section of the material.
a. Objective:
To examine the nature of inhomogenities, flow lines and welded sections of a metal
by unaided eye (or with a low-power microscope).
b. Experiment:
i. Sulphur Printing
ii. Flow Lines
iii. Welded Sections
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i. Sulphur Printing:
The purpose of this experiment is to examine the impurities that may exist in steel
products. The importance of these impurities is because of their amount and distribution in the
steel. These impurities degrade steels mechanical properties especially its strengthen.
Sulphur existence is one of these impurities and makes the steel brittle.
Sulphur printing is a common method to detect and record the distribution of
Sulphur in steel. To prepare the surface of rail material to the experiment it must be cleaned
from the foreign matters on the surface by grinding and polishing. Because it is a macroscopic
examination with unaided eye, etching is not required. Preparing the surface, a special photo
paper, photographic bromide paper, is soaked in a 2% aqueous solution of sulphuric acid for
approximately 3-4 min. After the paper is removed from the solution and allowed to drain
from excess solution, prepared surface of the specimen is pressed on the paper with a pressure
for 1-2 min to let the chemical reactions between the surface and acid solution proceed. Then
it removed and the paper is placed into a photographic fixing solution for about 15 min. to fix
it permanently. When fixation completed the paper is washed in running water and dried.
Presence of darkly colored areas on paper indicates the presence of sulphur on the material
and distribution of these areas provides information about the mechanical properties of rail
material.
ii. Flow Lines
Flow lines are the natural consequences of applied mechanical working on material.
Flow lines provide information about the defects of material and excessive amount of
inclusions and segregated areas as well as the direction of metal flow during deformation. In
this method, because the elongated inclusions of impurities, such as oxides and other
heterogeneous areas are selectively attacked by etching reagent, flow lines are made visible.
iii. Welded Sections:
The purpose of welded section experiment is to find the locations of weld sections of
a welded material. After the surface of the specimen cleared from foreign matters and
deformations by grinding and polishing, prepared surface is etched with nital for 10-20 sec.
This operation is repeated several times until some relief of the macrostructure is produced.
Finally the specimen is rinsed in alcohol and dried.
d = C/nL .M
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d = C/nL .M
However, because of the unclear micrograph above, the average grain diameter
cannot be calculated for this figure (Figure 2.).
2. RESULTS of MACROSCOPICAL EXAMINATION
a. Sulphur Printing
1. Sulphur Inclusions in Rail Material:
As explained above in the sulphur printing
section, a consequence of the chemical reaction
between the sulphuric acid on the photographic
bromide paper and the sulphide regions of the
specimens surface, darkly colored stains and areas
exist on the paper. That is, dark colored points
indicate sulphur inclusions of the rail material.
2. Distribution of Sulphur Inclusions:
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lines, some stress stacks appears in particular sections of metal where have the risk of brittle
fracture. (See the figure 4.)
c. Welded Sections:
5. Welded Section
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VI. REFERENCES
[1] University of Cambridge, retrieved from http://www.msm.cam.ac.uk, September 28, 2006.
[2] D.R. Askeland, The Science and Engineering Materials, P.P Phule Thomson Pub., 5th
edition 2006.
[3] Wikipedia, the free encyclopedia, retrieved from http://en.wikipedia.org, September 28,
2006.
[4] Arnes Corporation, retrieved from http://www2.arnes.si, September 29, 2006.
[5] Aran, A., Malzeme Bilgisi Ders Notlar, Makina Fakltesi, T.
[6] Material Testing Laboratory Manual, ITU, 2006.
[7] Aran, A., Manufacturing Prop. of Materials, ITU, 2006.
[8] Materials Evaluation and Engineering, inc, retrieved from http://www.mee-inc.com,
September 30, 2006.