Experiment No.

3: MICROSTRUCTURE AND HARDNESS TEST

MATERIAL SCIENCE AND ENGINEERING (GEL102)

LABORATORY REPORT
on
Experiment No. 3
“MICROSTRUCTURE AND HARDNESS TEST"

Submitted by :-
1. Ambarish Borah (2016eeb1069)
2. Amit Kumar (2016eeb1070)
3. Avinash Gupta (2016eeb1071)
4. Bhavesh Meena (2016eeb1072)

Group no.: - LG (2)

Experiment Performed On: 12 October 2017

Report Submitted On: 12 October 2017

Supervised by:
Dr. Ravi Mohan Prasad
1st Semester, Session 2017-2018

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

Table of Contents
1. Introduction................................................................................................. 3
2. Apparatus Details/ Equipment Specifications..............................................3
3. Experiments................................................................................................. 3
3.1. Aim of the experiment.......................................................................3
3.2. Theory related to the experiment..................................................... 4
3.3. Experimental Procedure................................................................... 5
3.4. Data Analysis......................................................................................7
3.4.1. Calculation of hardness:…………………………………………………….7
3.4.2. Photos Obtained.........................................................................10
4. Conclusion and Discussions.......................................................................15
5. Precautions..................................................................................................15
6. References...................................................................................................15

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

1. Introduction:

In this experiment, we study the properties of the allotted material using

the knowledge obtained by analyzing its microstructure and its
hardness.

2. Apparatus Details/Equipment specifications:

a) Mild Steel sample,

b) Emery paper,
c) Fiber Glass sheet,
d) Belt Grinder,
e) Diamond based Polish Alumina,
f) Grinding and polishing machine,
g) Etchant (90% ethanol + 10% nitric acid)

3. Experiment:

Many properties of metallic materials such as yield strength, tensile

strength as well as the electric resistance are more or less directly
related to the microstructure. The understanding of the relationship
between microstructure and properties therefore plays an important
role in the control and development of metallic materials. For this we
perform two sets of experiments which are as follows.

3.1. Aim of the experiment:

To study the microstructure of the given specimen using the data
obtained from the microscope.

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Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

3.2. Theory related to the experiment:

The examination of the microstructure, metallography, is an important
test method for the determination of the applications for the materials
involved. Metallography tells us a lot about the different properties of
the given specimen viz. lusture, electric conductance, heat conductivity,
ductility, coercivity, thermal conductivity, etc.

While carrying out our experiments, preparation of the specimen is of

utmost importance.There are some sectioning techniques which are
material preserving but they are time consuming and not economic for
routine work. However, they are useful for special applications like that
for semi-conductors, brittle materials.A soft cutting wheel is used in
caseof hard material for faster removal of the used grains. This also
leads to exposure of new abrasive grains. A hard-cutting wheel on the
other hand is used for soft materials. Other criteria determining this
selection are grain size, concentration of abrasive particles, thickness of
the wheel, durability of the wheel. highly concentrated and coarse

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

abrasive particles produce small areas of contact while lowly

concentrated produce large area of contact. The speed of the wheel is
also taken into account.

Mounting is also done for irregular and small materials to use as a

specimen. Mounting depends on shape, size, brittleness, porosity,
electrical conductance, transparency, chemical resistance to etchants or
solvents. The technique for mounting is decided based on the materials
properties.

There are also some special mounting techniques viz. taper techniques,
infiltration, mounting of powders, etc.

3.3. Experimental Procedure:

The basic processes involved in this experiment are as follows:

a) Sample Selection: We have selected mild steel as the material for our
specimen.
b) Sample Preparation: There is no universal technique that meets all the
demands of metallographic specimen preparation. Metallographic
preparation includes sectioning, mounting, identification, grinding,
polishing, cleaning, etching. A satisfactory specimen must include a
representative plain surface area; this area must be free from changes

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Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

caused by surface deformation, flowed materials (smears), plucking (

pullouts), scratches.
The first step involves selection and separation of the sample from the
bulk material. Sectioning should render a plain surface for the following
preparation without causing any critical changes in the material.
Alterations in the microstructure can be produced by deformation,
creation and development of cracks and breakouts, heat generation,
recrystallization, partial melting; which can be lessened using inert
lubricants, coolants (water, oil, compressed air), so care should be taken
in this regard.
We then mount our sample onto a epoxy resin in order to further work
on our sample; as our sample is very small so it would be nearly
impossible to work on our sample provided the dimensions it now has.
This mounting is done on the mounting press. The mounting process
involved here is hot mounting, though we haven’t come across the cold
mounting procedure until now.

Fig.- Sample Mounting Press

We now perform grinding on our given specimen to attain a better

surface finish. We start with lower grades of silicon carbide paper
starting from 60 on the belt grinder and then manually proceeding to
2000. We follow a basic alignment while doing this grinding. We start

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

from a specific direction and then after orienting the lines of scratches
along this direction we move on to its perpendicular one with the paper
of higher grade.
The next step is polishing which is done on the polishing machine. We
apply micro polish alumina on the surface of the specimen. We continue
this till we attain a polished surface. Now, we are to perform etching.
We apply an etchant mixture of 90% ethanol and 10% nitric acid. We
also dried our specimen by blowing hot air onto it. Our specimen is now
ready to be analysed for its microstructure.

c) Working on the microscope: We take our specimen to the microscope

and place the polished surface on the panel in order to study its
microstructure. We view the microstructure shown in the display and
record the pictures obtained. We use this pictures for our further study
of the material’s properties.

3.4. Data Analysis:

3.4.1. Calculation of hardness:

Vicker’s Hardness Tests : The Vickers hardness test method, also referred
to as a microhardness test method, is mostly used for small parts, thin
sections, or case depth work.
The Vickers method is based on an optical measurement system. The
Microhardness test procedure, ASTM E-384, specifies a range of light
loads using a diamond indenter to make an indentation which is
measured and converted to a hardness value. It is very useful for testing
on a wide type of materials, but test samples must be highly polished to
enable measuring the size of the impressions. A square base pyramid
shaped diamond is used for testing in the Vickers scale.
The Microhardness methods are used to test on metals, ceramics,
composites - almost any type of material.Since the test indentation is very
small in a Vickers test, it is useful for a variety of applications: testing very

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

thin materials like foils or measuring the surface of a part, small parts or
small areas, measuring individual microstructures, or measuring the depth
of case hardening by sectioning a part and making a series of indentations
to describe a profile of the change in hardness.
Sectioning is usually necessary with a microhardness test in order to
provide a small enough specimen that can fit into the tester. Additionally,
the sample preparation will need to make the specimen’s surface smooth
to permit a regular indentation shape and good measurement, and to
ensure the sample can be held perpendicular to the indenter.
Often the prepared samples are mounted in a plastic medium to facilitate
the preparation and testing. The indentations should be as large as
possible to maximize the measurement resolution.

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

F - Load in kgf
D - Arithmetic mean of the two diagonals, d1 and d2 in mm

HV - Vickers hardness

136°
2𝐹𝑠𝑖𝑛
2
HV = 2
𝑑

Fig.- Vicker’s Micro-Hardness Tester

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

3.4.2. Photos Obtained:

HV =28.7

Microstructure of top part of Aluminium casted in brick mold.

Magnification = 10X.

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

HV = 31.1

Microstructure of centre part of Aluminium casted in steel mould.

Magnification = 10X.

HV = 27.7

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Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

Fig. (4): - Microstructure of central part of Aluminium casted in brick mold.

Magnification = 10X.

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Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

Fig. (5): - Microstructure of middle part of Aluminium casted in brick mold.

Magnification = 10X.

Fig. (6): - Microstructure of top part of Aluminium casted in brick mold.

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Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

Magnification = 10X.

Fig. (7): - Microstructure of top part of Aluminium casted in steel mould.

Magnification = 10X.

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

Fig. (8): - Microstructure of centre part of Aluminium casted in steel mould.

Magnification = 10X.

Fig. (9): - Microstructure of middle part of Aluminium casted in steel mould.

Magnification = 10X.

4. Conclusion and discussion:

1) The average grain size at the centre is greater than that of the
grains at the edges.
2) As the edges of the Aluminium is in contact of the mould, the Avg.
Grain Size of Aluminium at its edges can be controlled by casting on
different moulds(different rate of cooling); thus the properties of
Aluminium can hence be altered as per our requirements.
3) Aluminium is composed of minute crystals made of grains which are
oriented in different directions, separated by grain boundaries due
to crystal defects.
4) The hardness of aluminium with smaller grain size is greater than
the hardness of aluminium with larger grain size.

The rate of cooling is a dominant factor for variation of physical properties

of a material. The microstructure of various samples with different rate of

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 Experiment No.3: MICROSTRUCTURE AND HARDNESS TEST

cooling differs significantly. If the rate of cooling is higher, the grain

formed has finer grain size and such material has higher strength and
hardness. The grain size influences the strength of a material. Smaller
grains help prevent hot tearing or crack in the casting. Also while
moulding a material the rate of cooling is different for different part of the
material so the hardness also varies within the material. Hence, the
hardness is greater at the centre and least at the middle.

5. Precautions:
1) Always wear Acid Resistant gloves when Etching!
2) If the choice of a sample is not representative of the material, it
cannot be corrected later. It is also difficult to compensate later for
improper sectioning, because additional, time-consuming corrective
steps are necessary to remove the initial damage.
3) The abrasive grains become rapidly worn out during cutting of hard
materials and must be continuously replaced by newly exposed grains.
4) Do not touch, wipe or swab the specimen following etching.
5) Care should be taken while dealing with Hydrofluoric Acid ; use of
gloves is

6. References:
a) Metallographic Etching, 2nd Edition, ASM International

b) Materials Science and Engineering- an Introduction, William D. Callister, Jr.

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