Characterization of

Materials – II
Laboratory

Sample preparation and metallography

Name: Arsalan Muhammad Khan

Department: BSMME 19-23
Email ID: [email protected]
Instructor: Sir Aqib Zahoor
Date: 20 August 2021
Abstract:
This experiment basically is about metallography of mild steel, but it involves many prior
steps to obtain a micrograph. We did sampling, grinding, polishing, etching and then finally
observed the sample under a microscope and studied the structure of it.

Introduction:
Almost all the properties of a metal are related to its structure on micro level. Material
properties like strength, hardness, toughness, ductility etc. depend on microstructure and
atomic arrangements. We can study the microstructure by techniques of metallography.
Metallography requires good sample preparation. In this experiment, we perform the full
procedure for it starting from scratch.

Objectives:
- Learn about sampling, grinding, and polishing.
- Creating an etchant solution.
- Learn how to operate a microscope.
- Learn how to do structural study of a metal.

Theory:
Microstructural study is the best tool for characterization of materials. A micrograph alone
can be used to predict much of the properties of a crystalline material. When we wish to
obtain a micrograph, we have to ensure that our sample surface is adequate. This means
that the surface is polished and free from scratches, rust and other aspects which may
obscure the microstructure.
To achieve this, we have to do proper sample preparation which involves sampling,
grinding, polishing, and etching in that order. The quality of our micrograph is dependent
on how well the sample preparation is done. Poorly prepared samples may fail to reveal
any meaningful information. The ultimate objective is to obtain a flat, scratch-free, mirror-
like surface. Only then we can observe individual grains and grain boundaries of a material
under a microscope.
As our sample is of a normalized mild steel , we expect to see pearlite and ferrite being
present. The pearlite will be present at grain boundaries separate from ferrite grains. Mild
steel has carbon content of 0.05% to 0.25% so pearlite would be in lesser amount and
ferrite would be more. Since the sample is normalized, we don’t expect the presence of
martensite. We have to be cautious as mild steel is very prone to rusting and our process
should take minimum time after grinding is done.
The steps of metallography will now be explained.
 Sampling
We start from a rough cylindrical mild steel rod. We have to sample it into smaller parts so
that further steps can be easily done on a smaller size. We use abrasive cut off machines or
hacksaws to do this. Lathe machines may also be used for more precise and smoother
cutting. The area we cut our sample from should be representative of the whole metal.
It should be mentioned that if sample is small or irregular, it may need to be mounted in
appropriate material or clamped.

Grinding
Grinding is done on a grinding machine which has a rotating disk. Different grades of
sandpapers are fitted on the disk and used in wet conditions facilitated with a constant
water flow. The higher the grade of sandpaper, the more abrasive/rough it is. We start from
150 grade and work our way up to 2000 grade. Grinding is done on one face of material we
desire to do metallography on. We force the material face down on rotating sandpaper
until we achieve a very smooth and scratch-free surface. Handheld files can also be used in
some cases.

Polishing
Polishing is the next step after grinding. It also involves a rotating disk. Alumina powder’s
paste with water is used in this case for fine polishing. The paste is spread over disk and
sample is pressed against the disk. It removes any grooves and residue left after grinding
This method can help achieve a mirror like polished surface. The sample should be cleaned
with a cloth after polishing.

Etching
Etching is the selective degradation of metal. An etchant acts on high energy areas and
grains such as grain boundaries and eats/corrodes them faster than low energy areas. This
creates a pattern in which different grains can be identified and differentiated from each
other under a light microscope. Different etchants are used for different metals. For out
mild steel sample, we use Nital which is just 1/10th parts Nitric acid and rest is methyl
alcohol.

Microscopy
This is the final step in metallography which gives actual data. We use a metallurgical
microscope. The areas the etchant has eaten are deeper from other areas. When light
strikes the sample, it reflects back from the sample into our eye piece creating an image.
Light doesn’t reflect back from the deeper areas. Those areas appear dark when observed
and other areas appear bright creating a contrast. This way, we obtain a detailed
micrograph where grains, grain boundaries and defects can be seen.
Procedure:
Sampling: We start from a Mild Steel (MS) rod. A 0.5 to 1 inch part is cut from it by
use of automated hacksaw or a lathe machine.
Grinding: We turn on the grinding machine. Several grades of sandpaper are
arranged and cut into circles according to size of grinding machine’s disk. First 150
grade paper is fitted. Water flow is turned on and appropriate rotation of disk rpm
are set. The sample is grinded by forcing one face of it against the rotating disk and is
held in place. After some time, the paper is changed with a higher grade and again
grinding is done. We work our way up to 2000 grade paper.
Polishing: Alumina powder is taken and mixed with water to form a polishing paste.
The paste is spread on the disk of polishing machine. The sample is forced against
this disk for fine polishing to occur.
Etching: The etchant solution is prepared by mixing 1/10th portion Nitric acid (say 5
ml) into Ethyl alcohol (say 50 ml). The desired surface of this sample is dipped into
this solution for 10-20 seconds. The sample is taken out and cleaned with ethyl
alcohol. The surface is then dried by a tissue or by an air dryer.
Microcopy: Proper magnification objective is adjusted. Light is turned on of the
microscope. The sample is placed under the lens and focus is adjusted by the knobs
until surface is clear. The micrograph obtained is to be photographed.
Calculations: The micrograph is studied, and total magnification is found. The
percentage of pearlite and ferrite present is found. We should also find the grain
size.

Observations:
After grinding on 600 grade

After grinding on 1000 grade

After grinding on 2000 grade

After Fine polishing

After Etching
 With scale (from Hardness microscope)

Results and Calculations:

The pearlite grains in our mild steel appear dark and ferrite grains appear bright as the
etchant we used targets pearlite grains. Unfortunately, due to limitations of our etchant
and magnification, we can not see the grain boundaries in the ferrite region.
By use of the Gwyddion software, we can study our micrograph and find the areas of
pearlite zone and ferrite zone.
By selecting the “Mark by Otsu’s” option, the bright (ferrite) areas in our micrograph get
highlighted and the total area of ferrite can be found. The pearlite area can be found by
subtracting the ferrite area from the total area of the micrograph.
As the individual ferrite grains are not visible, we cannot accurately calculate the grain size
by linear intercept method. But we can see the individual pearlite grains. So, we calculate
the grain size of pearlite by randomly selecting 15 grains and finding their mean grain size.
Using the given scale on our micrograph from hardness testing microscope, we can find
that the dimensions of our total micrograph are 383 x 383 μm and by measurement, image
size is about 12.65 x 12.65 cm. This gives magnification of:
𝟏𝟐.𝟔𝟓 ×𝟏𝟎−𝟒
Magnification = = 330x
𝟑𝟖𝟑
By “mark by Otsu’s” we get the area of bright ferrite region = 0.1122 mm2
The total area of micrograph is = 383 x 383 = 0.1466 mm2
By subtracting, we can find area of the dark pearlite region = 0.0344 mm2
So, the proportion of ferrite in our sample is:
𝟎.𝟏𝟏𝟐𝟐
% Ferrite = x 100 = ~ 76.53 %
𝟎.𝟏𝟒𝟔𝟔

And the proportion of Pearlite:

% Pearlite = 100 – 76.53 = ~ 23.46 %
For grain size of pearlite grains:
Grain Size
1 13.4
2 5.4
3 14.8
4 11.1
5 18.1
6 3.5
7 9.2
8 11.4
9 12.8
10 10
11 15.3
12 3.5
13 7.3
14 6.1
15 12.8
Mean 10.31333333

So mean grain size of pearlite grains is approx. 10.13 μm

Pearlite % = 23.46 %
Ferrite % = 76.53 %
Pearlite Grain size = 10.13 μm

Conclusion:
We successfully performed metallography and structural study on mild steel by the
micrograph we obtained. We produced meaningful results for composition of different
phases and grain size. Pearlite is much lesser than ferrite and that is what we expected
from mild steel because carbon composition is low in it. Grain size value is also comparable
to predicted literature values of grain size. But since the sample is normalized, we should be
expecting bigger grain sizes compared to quenching.