Experiment 5

Metallographic Specimen
Preparation and Examination

Amirehsan Barzegarsedigh
C1700064
ABSTRACT

The experiment was performed to know the method of preparing metallographic

samples and the fundamental function and operation of the optical microscope. Analysis of a
material microstructure helps to determine whether the material has been properly processed
and is therefore a critical step in determining product reliability and determining why a
material has failed. In addition, the experiment was performed to analyse the observation of
the microstructure and to understand the theoretical background of sample preparation and
metallographic specimens. Six Processes that are sectioning, mounting, grinding, polishing,
etching and microscopic analysis were performed during the experiment. The results can be
obtained during microscopic analysis which is the grain structure of ferrite and pearlite.

INTRODUCTION

Metallographic research, or metallography, is the testing of topographic or

microstructural characteristics on prepared material surfaces. Metallography studied
buildings are reflective of the characteristics and efficiency of the studied materials. Planar
surfaces are ready for a polished finish in this method. Chemical or other techniques of
etching are often used to delineate the characteristics of macrostructure and microstructure.
Once prepared, the unassisted eye, light microscopy and/or electron microscopy will examine
samples. [ CITATION Met18 \l 1033 ]. Analysis of a microstructure of products enables us to
determine whether the material has been processed properly and is therefore a critical step in
determining the reliability of the product and determining why a material failed. The
fundamental steps for adequate preparing of the metallographic specimen are:

1) Sectioning and Cutting

- Careful sectioning of the test sample to prevent changing or destroying the
material composition. Therefore, if an abrasive saw is used, keeping the
sample cool with lubricant or coolant is essential. However, a tiny quantity of
deformation happens on the sample surface regardless of how closely abrasive
sawing or electrical discharge machining is done. During later sample
 preparation steps, this deformation must be removed. [ CITATION Met181 \l
1033 ].

2) Mounting
- After the specimen has been cut to a convenient size, it is installed in a plastic
or epoxy material to facilitate handling during the grinding and polishing
steps. In terms of hardness and abrasion resistance, the mounting media must
be consistent with the sample.[ CITATION Met181 \l 1033 ].

3) Grinding
- The next step is to grind the sample with a water lubricated abrasive wheel for
a flat, smooth and scratch-free surface. To remove the surface damage that
happened during sectioning, this step is needed. The grinding process involves
that use of a sequence of gradually finer abrasive grids. [ CITATION
Met181 \l 1033 ].

4) Polishing

- In metallographic preparing, the polishing step removes the last thing layer of
deformed metal for a smooth reflective surface. It leaves a proper prepared
sample ready to examine unetched features, such as content of incorporation
or any porosity that may occur [ CITATION Met181 \l 1033 ].

5) Etching
- The final stage that could be used to etch a suitable acidic or basic solution to
determine the micro-structural information of the test sample. This step shows
characteristics such as grain boundaries, twin and second phase particles not
seen in the un-etched sample.

6) Microscopic analysis
- After etching these samples for further evaluation, go through the microscope.
OBJECTIVES

i. To prepare metallographic samples.

ii. To study the important of the various steps in sample preparation
iii. To understand the need of mounting, polishing and etching
iv. To study the microstructure of ferrous and non-ferrous metal.

MATERIALS

i. Mild steel
ii. Copper
iii. Brass
iv. Alcohol
v. Distilled water
vi. Diamond Paste
vii. Acylic resin etching solutions

APPARATUS

i. Grinders
ii. Different size of sand paper
iii. Polishing wheels
iv. Drying fans (Hair Dryer)
v. Optical microscopes

PROCEDURE

1. Using hacksaw in the workshop, a tiny portion of the steels sample from various
kinds of steel rods was separated.
2. Different metals were put in the mounting solution (RESIN-5) in each separate
small container after waiting for it to be melted for 15 minutes.
3. The metals were waiting to be hardened again inside the mounting solution.
 4. The surface of the samples was grinded with various sand paper types beginning
with the roughest P320, P800, and then using the flat disc grinder P1200.
5. The surface of the specimens was polished with diamond pasted using the
polishing wheel in a scratch-free condition by rotating in the opposite direction to
that of the rotation of the wheel to minimize the polishing effects of the direction.
6. After the grinding and polishing method, the samples were plunged into alcohol
for 2 minutes.
7. The samples were then dried for about 30 seconds using the drying fan.
8. After drying process, the samples were immersed in etching solution for 1 minute.
9. By dipping into distilled water for 10 seconds, the samples were washed and then
dried with a drying fan.
10. The sample is shifted to the final phase after etching, which is metallographic
evaluation by using the optical microscope to view the specimen at different
11. Magnifications and note the material’s microstructure elements.

RESULTS

Figure 1: Microstructure of brass specimen

Figure 2: Microstructure of copper specimen.

Figure 3: Microstructure of mild steel specimen.

Figure 4: Phase diagram of steel.

DISCUSSION

Figure 1 demonstrates the brass microstructure acquired after adequate metallographic

sample preparing by watching under the optical microscope. Brass is known to be a copper-
zinc to its high strength and resistance to corrosion. Single phase alloys consisting of a strong
solution of zinc and alpha copper are alloys comprising up to roughly 35% zinc. These brass
types have excellent ductility and are easy to cold work. Brass has a larger grain boundary
than mild steel based on the outcomes acquired from the optical microscope.

Figure 2 indicates that copper specimen microstructure after etching. Copper and
copper alloys are hard to prepare because they tend to harden and have inclusions of oxide.
Copper is examined to determine the extent to which the stainless steel is diffused into the
copper. This is undesirable because the copper’s electrical conductivity is considerably
reduced. The key to polishing copper is to minimize smearing during cutting and original
grinding and retain the integrity of the copper and stainless steel inclusions. The outcome is
that they can dislodge the oxide inclusions and scratch the surface. This scratching becomes
more evident after etching[ CITATION Cop18 \l 1033 ].

By using fine grit alumina building documents and polishing with polycrystalline
diamond for the intermediate polishing step, preparation damage can be minimized, followed
by polishing with polycrystalline alumina [ CITATION Cop18 \l 1033 ].

In figure 3, the optical microscopic is used to obtain the microstructure of mild steel.
Based on figure figure 4, ferrite and pearlite are found in the microstructure of mild steel.
Mild steel is also referred to as low carbon steel, containing about 0.25 to 0.4% of carbon.
CONCLUSION

In conclusion, metallography is one of the most significant parts of physical

metallurgy that uses an optical microscope to imagine the sort of material and its physical
characteristics from microstructure. The observation for mild steel microstructure is not clear
due to the optical microscope’s low magnification. Therefore, it is not possible to obtain
much data. Therefore, the microstructure of pearlite and ferrite cannot be seen as well. The
grain boundary is more difficult to see, there it is not possible to obtain grain size. A finer
grain size will definitely enhance the finished product’s yield strength and stress relaxation
resistance. In general, smaller grains will also enhance a material’s formability. As a results,
these changes in the properties of the material for the micro structure are very important.
Metallography thus plays a significant modifications that affect the physical characteristics of
materials.

COMMENTS

1. What is mounting? Explain two types of mounting.

Specimens are integrated in resin to make processing easier and enhance the outcome
of the preparing. Before loading, samples should be washed for the highest feasible
consequence. Resin's highest feasible adhesion to the sample needs that the surface is
free of grease and other contaminants. Specimens requiring ideal edge preservation or
layer safety involve installation. However, it is worth wondering whether holding
would be pointless or even hard due to the size or geometry of the sample. If this is
the situation, mounting it may be better not.

Two kinds of assembly are cold and warm assembly. Hot mounting requires place
under stress in a mounting cabinet where, together with the suitable mounting resin,
 the sample is put in a cylinder. When the specimen is embedded, a temperature of up
to 200 ° C and a stress of up to 50kN are then introduced. There are two kinds of
procedures for warm storage: thermoplastic resins and resins for thermo setting.

When boiled, thermoplastic resins dissolve, providing the chance to repeat the method
with the same sample if the first time the outcome is unsatisfactory. Thermoplastic
resins are hardened with or without stress during a chemical response. This implies
that elevated stress during heating and ventilation is not essential. This process is
good when mounting fragile specimens.

Cold holding or embedding occurs when the holding compound is blended with a
hardener (or accelerator) and then the method of polymerization occurs to create the
block. This method gives off warmth in some instances. However, using ice or cold
air blow environment can control this thermal generation. Cold mounting compounds
are chosen for heat- or pressure-sensitive samples used during the warm mounting
phase.

2. Define terms of polishing, grinding, and etching.

Grinding removes saw marks and levels and cleans the specimen surface. Polishing
removes the artefacts of grinding but very little stock. Grinding uses fixed abrasives
(the abrasive particles are bonded to the paper or platen) for fast stock removal.
Polishing Free abrasives are used on a cloth by polishing; that is, the abrasive
components are held in a lubricant and can fold or glide across the cloth and sample.
Etching In microfabrication, etching is used to chemically extract pieces from a
wafer's surface during fabrication. Etching is a critical system module, and before it is
full, every wafer undergoes many etching measures.

3. Explain the importance of etchant.

etchant is the method of exposing microstructural information on the as-polished
sample that would otherwise not be apparent. Etching is not always needed as some
characteristics, such as porosity, gaps and inclusions, are noticeable in the as-polished
situation. A properly prepared specimen will reveal properties such as grain size,
segregation, and the shape, size, and distribution of the present phases and inclusions,
 while other aspects such as mechanical deformation and thermal treatments may also
be identifiable.

4. Which type of precautions should be taken care of before etching?

i. Goggles for safety. The etching solution may splash, and in your eyes, you
don't want it.
ii. Apron. Your clothes will be stained by the etchant and anything else it touches.
iii. Good ventilation (open a window or exhaust fan if necessary). Never etch in a
tiny room that is contained. In a tiny room, chemical fumes and gasses that are
not visible in the correct configuration can create up to hazardous
concentrations. Outdoors is a excellent location to etch, allowing the climate.
iv. Plastic or glass containers for the "bath" etchant. We like to use the spinach or
salad mixed transparent plastic tubes.
v. To neutralize the acid, use baking soda.
vi. Secure plastic screw-top container to dispose of the enchantment used.

5. Why metallographic samples are sometimes mounted in plastic?

It is necessary to level and polish metallographic samples well. It is best to polish a
device with a mechanical holder (to apply uniform motion and a constant down force)
that can maintain only normal cylindrical diameter samples. But the sample material
can't be sliced into that form very often or the sample is just too tiny. So casting the
sample inside plastic is simpler. The back part of the sample can also be readily
levelled in this manner. Lastly, metallographic microscope phases are generally laid to
fit such samples.

6. What is the difference between Eutectoid steel and Hypoeutectoid steel?

Based on the proportion of carbon, the iron carbon equilibrium ranking of steel
1. Hypo eutectoid steel: less than 0.8 % carbon
2. Eutectoid steel: 0.8 % Carbon
 3. Hypereutectoid steel: higher than 0.8 but less than 2 %

7. At room temperature:
i. What are the phases of eutectoid steel?
Iron Carbide
ii. What are the constituents of eutectoid steel?
Pearlite which is a mixture of ferrite and cementite.
iii. What are the phases of hypo eutectoid steel?
Steel according to Fe-Fe3C
iv. What are the constituents of hypo eutectoid steel?
Ferrite (alpha iron) and Pearlite (gamma iron)

8. Briefly explain the effect of grain size on the strength of a metal.

Most metals ' strength depends on the average size of grain in a polycrystalline
material and the sample size in a monocrystalline material. You need to think what
determines the material strength in order to comprehend this. For larger grains,
statistically speaking, they are more likely to have longer dislocations as the stress
required to activate some of these (longest) dislocations is lower than the stress
required to activate the dislocations that would normally occur in a smaller crystal
where the longest dislocations are significantly shorter.
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APPENDIX

Figure 5: Second Microstructure of Brass Specimen

Figure 6: Second Microstructure of Mild Steel Specimen

Figure 6: Second Microstructure of Copper Specimen