Manufacturing Laboratory-I (ME207) Report

Date of submission: 7/09/2021 Name: Md Athar Hassan

Group: G10 Entry No: 2019MEB1278

Experiment-02
Title of the Experiment
Metallographic sample preparation and Microstructural observation.

Objective of the Experiment

 The purpose of this course is to learn how to prepare metallographic samples.
 To comprehend the optical microscope.
 Examine and analyse the optical microstructure, as well as grain size measurement.
 To measure and compare the hardness of heat-treated samples.

Material and the Apparatus used

 Mild steel
 Sample cutter
 Sample mounting machine
 Belt grinder
 Optical Microscope
 Microhardness testing machine

Procedure of the Experiment

 Procedure of Cutting process-

 The sample to be cut was measured.
 Sample that had been cut, placed in clamps and clamped it slowly until tight.
 The machine cover has been closed for safety. The machine was turned on and the
blade was rotating, waiting for the fluid to rise at the blade.
 When the sample has been cut, the machine was turned off, the cover machine was
opened after the blade had stooped rotating. Then clamps were loosed, and sample
have been taken.

 Procedure of the Mounting-

 The mounting cup was raised, and the sample was placed, then the mounting cup was
lowered slightly.
 Some amount of bakelite powder that fully covered the sample is put into it and then
the mounting cup was lowered to the bottom.
 Bayonet cover was pressed and locked to the left.
 Then set the Parameter: Solidity Time : 10 min ,Cooling Time : 5 min ,Pressure : 200
bar ,Temperature : 1800c
 Start button pressed.
 After the process was over, the bayonet cover was pulled up, and the mounting cup
was lifted, and the completed mount sample have been removed for proceed with
grinding.

 Procedure for the grinding-

 First we grind the samples in belt grinder for coarse grinding.
 And for fine grinding we use emery paper with grit 400 was attached on the grinder.
 The machine was turned on, then the water pump and motor have been turned on.
 The sample was held and pressed in the grinding in the opposite direction.
 Next, turn specimen 90 degrees and repeat above procedure on the 600 Grit surface.
 Again turn specimen 90 degrees and repeat procedure now on the 800 Grit surface.
 Finally, turning specimen 90 degrees and repeat procedure now on the 1200 Grit
surface.
 After completing the step up to grit 1200, a smooth sample surface was produced.

 Procedure for polishing-

 Polished cloth was placed on the plate and spread diamond paste and spray.
 The machine was turned on. 9-micron alumina powder was placed on a cloth.
 Distilled water was turned on.
 After completing the polishing sample surface like a mirror has been produced.
 Now we clean the sample by ultra sonic cleaner.
 And by using the dry blower we dry the sample.

 Procedure for etching-

 Firstly Nital liquid was made by mixing the alcohol (90 to 95%) and Nitric acid (5 to
10 %).
 And with the use of cotton and nital liquid we etched the samples.
 After finishing the etching process, the sample was washed with water, then dried
using a pressure air gun.
 Then, the sample was placed under microscope, do the microscopic observation.
 These all process is done on all the samples(base,cold work, annealing, tempering,
quenching, normalization) is obtained from the Experiment1 and do the microscopic
observation by the uses of microscopic lens.
 And finally we calculate the hardness value with the use the Vickers indenter and
software named minuteman of all the samples in hardness testing machine.

Result and Discussion-

Grain Size Calculation-

L-- = (No.of lines) x (Volume Fraction) x Length of the line (L)/(No of intersections) x
Magnification(M)

G = 6.643 * log(L-- ) - 3.228

We take annealed sample microstructure-

Volume Fraction = 0.2536
Magification = 100(approx)
Total number of intersection = 98(12,13,12,15,10,12,10,13)
L-- = (8x 0.2536x10)/(98x 100) = 0.0020702
G = -6.643xlog(0.0020702) - 3.228 = 12(approx)
For this value of G, the grain size is coming out to be 0.008 mm
Drawbacks of such estimation of grain size-
 This method is not very accurate because manually drawing lines and counting
intersection can result in inaccuracies, hence we got some error in ‘G'(Grain size)
value.
 For industrial uses, this approach is labor-intensive.

Microscopic observation of all samples-

Base sample Cold work Annealed Sample

Normalizing(30min) Normalizing(60min) Quenching(30min) Quenching(60min)

Hardness observation-
After experimenting on Vickers’s hardness machine, we observed the following data for 7
specimens.

Base Cold Normalized Normalized Quenching Quenching

Annealed
Sample worked (30min) (60min) (30 min) (60min)

Micro-
Hardness 167.5
297HV 154HV 187.2HV 173.5HV 235.8HV 250.2HV
(Load- HV
200gf)

Hardness value of all samples which is obtainef

from heat process of mild steel
350
300
250
HARDNESS(HV)

200
150
100
50
0
Base sample-
This sample has the second-lowest hardness value among all other specimens because it
has not been subjected to any heat treatment methods. You can also observe that it has a
higher ferrite concentration than perlite in its microstructure, making it more ductile and
easily malleable (low hardness). Because the annealed sample has a stable austenite
phase, which increases the ferrite content in the microstructures, the annealed sample has
lower hardness than the base metal, despite its greater hardness value.

Cold work
A cold work sample has a high hardness value because its crystal structure is deformed
(compressed, twisted, and rotated) during the cold work process, resulting in
homogeneous crystalline plane movement to one another.
This causes a microstructure discontinuity known as a dislocation, which acts as a
deformation resistance when the load is applied. As you can see in the photograph, the
content of pearlites is higher than ferrite with some discontinuities, making the specimen
harder and more brittle.

Annealed
It has an extremely low hardness value compared to all other samples, indicating excellent
ductility and poor yield strength. According to our theoretical research, annealing has a
slow cooling rate (because to the fact that it is done in a furnace), which leads to the
stability of the austenite phase. The amount of ferrite in the specimen grows while the
amount of pearlite decreases, as indicated in the image. In addition, as the dislocation
density drops, the resistance to deformation reduces, lowering the hardness value.

Normalizing
After heating to austenite temperature, the specimen is cooled to room temperature in the
presence of air only during normalisation. As a result, the cooling rate of the specimen
treated by the annealing process is faster. This enhances the hardness of the material and
results in a finer pearlitic microstructure.

Quenching
After cold work, it has the second-highest hardness values. The cooling rate in quenching
is substantially higher than in annealing and normalizing because the specimen is cooled
in the presence of water, which speeds up the cooling process.

 Order of hardness(annealed<base sample< normalized< quenched<cold work).

Learning from the experiments

Learn about the various metallographic preparation processes.
Learned how the material's microstructure is affected by the cleaning process.
To calculate the micro hardness of samples, I learned the Vickers method.
With the help of microstructure, I learned how to analyse the material's impact properties.

Safety concern
 Before beginning the experiment, you must wear all of your safety equipment, such as
goggles, lab coats, hand gloves, and safety shoes.
 Always be cautious in the lab or workshop since metal cutting equipment can easily cut
your body.
 Do not handle any chemical until you know what it is, as it can be quite harmful.