Manufacturing Laboratory-I (ME207) Report

Date of submission: 14/09/2021 Name: Akshit Mehra

Group: G9 Entry No: 2019MEB1235

 Experiment No: 2
 Experiment title:
1. Metallographic sample preparation and Micro structural observation.

 Objective(s)
The objectives of the above performed experiment were:
1. To learn and understand different metallographic and Sample preparation
techniques along with optical microscopy.
2. To examine and analyze the optimal microstructure and measurement grain
size.
3. Compare the hardness of heat treated samples.

 Material and apparatus:

For conducting the above mentioned experiment, below mentioned apparatus is
required:
1. Sample Current
2. Sample mounting machine.
3. Belt Grinder
4. Polishing Machine
5. Optical Microscope
6. Micro-hardness testing machine

 Experimental procedure
For performing the experimentation, below mentioned steps are required to be
performed:
1. First, we cut and create a sample from the bulk material. This is done with the
help of metallographic cutting machine, where rather than heat treatment,
mechanical abrasion is performed, called grinding.
2. Place the bulk material in vice, and set the corresponding configuration in
machines. This includes setting up This is done on mounting machine.
3. Here, we set the settings for program 1 to Bakelite. And thus start out mounting
operation. Then, we mount our sample on machine on which, we put some
Bakelite powder on it.
4. Then, we power on the mounting process. We can see the variation of
temperature and pressure on the digital screen present on the machine.
5. Finally, when done, we take our sample out of the Machine. This process is
then followed by grinding and polishing step.
 6. When mounting is done, we move to the first step of grinding and polishing.
This is done in 2 steps.
7. First we perform grinding with coarse grade grinding paper, which is then
followed by find grade grinding. The grinding takes place with various different
paper categories like P-400, P-600, P-800, P-2000, and is done In the defined
order itself.
8. When completed, we perform cloth polishing to obtain a mirror finishing. This is
done on automatic cloth polishing machine.
9. On the machine, we then set the configuration. This include, the time for
polishing, the force to be applied, RPM for machine, diameter for colloidal
solution, etc.
10. When completed, the specimen goes through ultrasonic cleaning to obtain
mirror finish.
11. Now, we perform the etching process. This is done with NITAL Solution. Below
is the given composition:
NITAL = Nitric Acid (5 – 10ml), Alcohol (90 - 95ml)
12. For applying solution, we use the Cotton swab method.
13. Now, we perform micro-structural observation via Olympus microscope. For
this, we keep our specimen over the microscope, and give it proper x and y
coordinates.
14. Switch on the software to be used, i.e. Stream Basics. We then configure our
image obtained from microscope and change the threshold values to analyze
the grain structure.
15. This is then followed by Grain measurement process. This is done with the help
of grain formulae using software like ImageJ.
16. In the end, we perform Micro-hardness measurement testing. Here, we perform
Vickers hardness testing. This is done on each sample phase we have.
17. We set the configuration on the machine which includes the force applied, lens
resolution, etc. Correspondingly, we see the results and the values of hardness
over screen.

 Results and discussion

For calculating the area fraction, we have used the ImageJ software. Below are the
results obtained:

Below is the analyzed image attached:

For computing grain size, we use the below mentioned formulae:
Lbar = VAB * N * L / M * (Intersections)
G = - 6.6438log10L - 3.288
Where,
N is the number of lines which is 7, L is 13cm, M is the magnification, Intersections for
white = 73, Intersections of black = 29, and VAB is the area fraction = 0.254
Now, for magnification M,
M = length of scale bar on paper / length of scale bar mentioned
= 1.42cm / 0.0002cm
= 710
For white Ferrite:
LBAR = 0.254 * 7 * 130 / (710 * 73)
= 0.00446
ASTM Grain Number,
GWHITE = -6.6438 * log(0.000446) – 3.288
= 15.617 – 3.288 = 12.329 = 12
For black Pearlite
LBAR = 0.254 * 7 * 130 / (710 * 73)
= 0.0112
ASTM Grain Number,
GBLACK = -6.6438 * log(0.0.0112) – 3.288
= 12.964 – 3.288 = 9.96 = 10

Below are the attached results obtained from the Hardness Testing:

Sample Base Cold Annealed Normalized Normalized Quenche Quenched

Sample work (30mm) (30mm) (60mm) d (60mm)
s (30mm)
Hardness 167.5 297 154 187.2 173.5 235.8 250.2
Value
(HV)
In the above table, we observe the following trend:
a. The samples went through quenching is having the highest hardness value as
compared to other samples. This is so because, in quenching the specimen
goes via rapid cooling, and resulting in smaller grain size.
b. For annealing, due to a very small cooling rate (air), the grain size observed is
large, which can be attributed to the lowest value of hardness amongst other
samples.
c. In case of Normalizing, the grain sizes formed are of intermediate sizes (greater
than annealing and less than quenching). Thus the hardness level is also in
between the 2.
d. The cold worked sample shows higher strength than base metal, which is true
as cold working increases the strength. This is so because, when we perform
cold work, the dislocation in the sample increases, thus becoming unable to
move and piling up. This results in increases strength.

 Learning from the experiments

1. ASTM Grain Size: The number of grains are specified by the formulae:
N = 2G-1
Where, N is the number of grains per square inch at 100X magnification.
2. Hall-Patch Relation: Hall Patch relation is basically used to determine the strength
for the materials where phase/shape of all the grains is same. (eg. BCC), but the
orientation may be different. It is given by:
σ = σo + K*d-1/2
Where, d is the average grain size diameter.
3. Grinding and Polishing: Grinding Process and Polishing Process are basically further
divided into 2 steps.
a. Grinding: Belt Grinder + Coarse grade emery paper.
b. Polishing: Cloth Polishing + Fine grade emery paper.
4. Hardness Test: Hardness testing can be performed in 2 ways:
a. Knoop-Hardness Test: Consists of Rhombic shape based indenter tip. This is
defined HKN values.
b. Vickers-Hardness Test: It consists of square shape based pyramidal tip and is
represented by HVN values.
5. Hardness observed in Cold Worked sample is higher as compared to Base Sample.
This is so because the dislocations created gets piled up and becomes tangled, thus
making them unable to move.

 Safety Concerns
1. Always wear all the safety gears before starting the experiment. This may
include safety goggles, hand gloves, safety shoes, etc.
2. Do not touch any chemical without knowing, as this can lead to devastating
consequence.
3. Never perform the experiment in a sleep deprived condition. Always be active
and focused while conducting the experiment.