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MATERIAL TESTING : MACRO/MICRO

HSEYN KASIRGA
030040323
GROUP

Instructor: Prof. Dr. Ahmet ARAN

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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.

Results & Discussion Of Results


1. Results of Microscopical Examination
2. Results of Macroscopical Examination

V.

Conclusion

VI.

References

VII.

Tables and Figures

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.

II. EXPERIMENTAL PROCEDURE


1. SPECIMEN PREPARATION
The purpose of specimen preparation is to prepare the material piece for analysis by
minimizing mechanical surface damages to obtain reproducible results. Preparation of a
metallographic specimen generally requires following major operations:
1. Grinding
2. Polishing
3. Etching
a. Grinding:
The purpose of grinding is to minimizing the mechanical damages on specimens
surface by lessening the depth of deformed metal to the point where the last vestiges of
damage can be removed by series of polishing steps. The scratch depth and the depth of cold
worked metal underneath the scratches decrease with decreasing particle size of abrasive.
Grinding is done using a machine carrying rotating discs covered with silicon carbide paper
and water. There are a number of grades of paper, with 180, 240, 320, 400, 600, 1000, 1200,

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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)

iron and steel

- Alcholic Ferric Chloride

copper alloys

- Mixed Acids

aluminum alloys

- Dilute HCl

zinc alloys

Etching times varies according to specimen, but a general procedure is to observe


the surface during the operation and to end the operation when evidence of the grains first
appears. Further etching then follows to strengthen up the details as required for a good
contrast in microscopical examination. After etching, the specimen should be thoroughly
washed and dried with acetone or alcohol.

Figure 1: Machine used for grinding and polishing

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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.

III. DATA ANALYSS


1. MICROSCOPICAL EXAMINATION

d = the average grain diameter


nL = the number of grain boundaries intersected
per unit length of a test line
M = magnification
C = constant (generally C=1,5)

d = C/nL .M

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IV. RESULTS & DISCUSSION OF RESULTS


1. RESULTS of MICROSCOPICAL EXAMINATION
1. The Sketch Of Microstructure:

Figure 2. Micrograph of the Microstructure of specimen.


Dark colored areas indicates perlits ( + Fe3C ) and other white areas ferrits ().
2. Carbon Content of the Steel:
Containing the compound of Carbon (C), the amount of the dark areas, perlits ( +
Fe3C ), per unit area can give the Carbon content of the steel. However, the microstructure of
the specimen in figure 2 is not clear enough to calculate this content, because the grain
boundaries are not distinct enough. The reason of this situation is inadequate time of the
operation for etchant to attack and resolve details!
3. Average Grain Diameter:
Average grain diameter of a microstructure can be calculated with Linear Intercept
Method. In this method, the grains intercepted by a theoretical line on the specimen surface
are counted. The average grain size is indicated by the inverse of the number of grain
boundaries intersected per unit length of the test line, corrected for the magnification of
micrograph. Then the average grain diameter is given by following formula:

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d = the average grain diameter


nL = the number of grain boundaries intersected
per unit length of a test line
M = magnification
C = constant (generally C=1,5)

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:

Figure 3. Sulphur Inclusions

As it is seen in the figure 3, sulphur inclusions are


not distributed homogeneously. They are distributed
as segregated points in the material. This distribution
affects mechanical properties of the material,
especially its strength. This inhomogenic distribution
of sulphur makes the material brittle where the
sulphur density is higher.
b. Flow Lines

3. Existence of Flow Lines:


Flow lines appear as a consequence of applied mechanical working on materials. For
example, when a plastic formation, for instance rolling is applied to the material, orientations
in the rolling direction are started in the microstructure of the material due to the movement of
dislocations.
Flow lines do not exist in casted materials, because in casting, the material in liquid
form is poured into a mold where it is allowed to solidify by cooling. The liquid and
homogeny form of the material prevents any lines inside the product while it cools slowly.
4. Flow Lines and Mechanical Properties:
Flow lines are the kind of discontinuousness in the constitution of the metals that
affects the mechanical properties of the metal. A pressure applied on the metal is transmitted
on the flow lines through the metal and according to the distribution and direction of the flow

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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.)

Figure 4. Flow lines

c. Welded Sections:
5. Welded Section

6. Welded Section and Mechanical Properties


By examining the welded-sections it is
found that the the material is not manufactured
as a whole. The elliptical projection of the
material is welded.
Because any distinction in appearance
cannot be seen with unaided eye without any
polishing and etching operation, it can be said
the weld quality is very good. The reason of this
is the similarity of two materials.

Figure 5. Welded Section of Specimen


There are some relations between the weld section and the mechanical properties
of the material. Welding causes a heat treatment process of which effect decreases according
to the distance from the welded section. Due to the high temperature, some grain growths
exist in and near the welded section. The growth of the grains means decline of the grain
boundaries that affect the hardness and strength of the material in a negative way. Because the
grain boundaries are amorphous, they prevent from the dislocations. Therefore a decrease in
the amount of the grain boundaries results in decreases in the hardness and strength of the
material.
V. CONCLUSION
In conclusion, the constitutional characteristics of a metal or an alloy can be
related to its physical and mechanical properties with the aid of methods contained in
metallography.

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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.