National Institute of Technology Karnataka Surathkal

MT 304 Physical Metallurgy Lab – Manual

DEPARTMENT OF METALLURGICAL AND MATERIALS ENGINEERING

July 2024

Page 1 of 26
Contents

Sl. No. Experiment Name of the Experiment Page No.

No.

1 Exp. No. 1 Calibration of Thermocouple

2 Exp. No. 2 Metallography of Mild Steel

3 Exp. No. 3 Metallography of Grey Cast Iron

4 Exp. No. 4 Quantitative Metallography

5 Exp. No. 5 Construction of Phase Diagram by Thermal

Analysis
6 Exp. No. 6 Study on Cu-Zn Diffusion Couple

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Experiment No. 1. Calibration of Thermocouple

Aim: To Carry out Primary Calibration of the given Thermocouple

Procedure:
1. Take pure metal of known melting point and melt it in a in a crucible, the quantity of the melt should
be sufficient to permit immersion of the thermocouple into a depth at least equal to 10 times the
diameter
2. Insert the given thermocouple in the molten metal and connect the cold junction to EMF measuring
device
3. Switch off the power supply to the furnace and allow the molten metal to cool at a very slow rate.
4. Note down the EMF readings at regular intervals of time (every 15 secs)
5. Continue taking readings until the EMF reading remains constant for a long time.
6. As the EMF reading starts decreasing after constant reading, take 10 more readings.
7. Confirm that metal has solidified.
8. Plot the graph of EMF Vs Time
9. Identify the EMF value corresponding to the melting point of the metal (horizontal portion of the
curve)
10. Get similar values from other batches and finally plot the calibration curve for the thermocouple
(Temperature Vs. EMF plot)

Questions:
1. What is Peltier effect?
2. What is Thomson Effect?
3. What is Seeback effect?
4. What is the working principle of a thermocouple
5. List 5 Thermocouples along with the composition and Temperature range
6. What is meant by (i) Primary calibration (ii) Secondary calibration of thermocouples?
7. List the different instruments used to mesure temperature along with the temperature ranges
8. What is Cold junction or reference junction of a thermocouple?
9. What is Hot junction or measuring junction of a thermocouple?
10. What is meant by Cold junction correction ?

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Observations:
Pure Metal Taken: Its melting point :

Sl. No. Time (Sec) mV reading Sl. No. Time (Sec) mV reading
1 29
2 30
3 312
4 32
5 33
6 34
7 35
8 36
9 37
10 38
11 39
12 40
13 41
14 42
15 43
16 44
17 45
18 46
19 47
20 48
21 49
22 50
23 51
24 52
25 53
26 54
27 55
28 56

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57
58

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Page 6 of 26
Result: mV reading corresponding to the melting point of the pure metal (………..) =

Experiment 2: Metallography of Mild Steel

Aim: To practice the technique of specimen preparation for metallography and study of
microstructure of Mild Steel
Procedure:
1. Collect a cylindrical specimen of mild steel
2. Make one of the circular faces flat using belt grinder
3. Bevel (Chamfer) the edges of the flat surface
4. Polish the flat surface using polishing paper no.1. While polishing hold the paper firmly on a glass
plate and polish the sample, with light pressure, in only one direction (Forward Direction). This
polishing introduces scratches. If the scratches are uniform and parallel, wash the specimen, dry it
and go to the next finer paper 1/0.
5. While polishing on this new paper, turn the specimen through 90 degrees so that the new scratches
formed are perpendicular to the earlier scratches. Continue polishing until all the old scratches
disappear and the specimen contains only the new scratches. Once the specimen shows only new
scratches, wash, dry and go to next finer paper 2/0
6. Follow similar procedure and polish using 3/0 and 4/0 papers.
7. After polishing with 4/0 paper, wash the specimen and polish on polishing wheel using abrasives like
SiC or Al2O3
8. While polishing on the wheel, apply little pressure and keep rotating the sample.
9. Continue polishing until the sample is free from all the scratches and has attained a mirror finish.
Wash the specimen, dry it with hot air blower.
10. View the polished surface under the optical microscope. Draw the microstructure of this un-etched
specimen and label the various micro constituents. This un-etched specimen shows inclusions.
Identify these inclusions using the inclusion charts and declare the inclusion rating.
11. Now, Etch the specimen with 2% Nital. Observe the surface under the optical microscope. Identify
various features of the microstructure like the various phase, grains, grain boundaries etc. Draw the
microstructure and label the various micro constituents.

Questions:
1. Draw Fe-Fe3C phase diagram and label all the phase filelds
2. What are the microstructural constituents of Mild Steel?
3. How can you identify pearlite?
4. What could be the approximate composition of mild steel you have observed?
5. Other than Fe and C, what elements are expected in mild steel? In what quantity?
6. What are inclusions? What are the different types of inclusions that can be present in mild steel?
7. How inclusion rating in steel is done?

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Observations:

Material: Chemical Composition:

Condition: Un-etched Condition: Etched with …………….

Magnification: Magnification:

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Experiment 3: Metallography of Grey Cast Iron
Aim: To practice the technique of specimen preparation for metallography and study of
microstructure of Grey Cast Iron
Procedure:
1. Collect a cylindrical specimen of Grey Cast Iron
2. Make one of the circular faces flat using belt grinder
3. Bevel (Chamfer) the edges of the flat surface
4. Polish the flat surface using polishing paper no.1. While polishing hold the paper firmly on a glass
plate and polish the sample, with light pressure, in only one direction (Forward Direction). This
polishing introduces scratches on the specimen. If the scratches are uniform and parallel, wash the
specimen, dry it and go to the next finer paper 1/0
5. While polishing on this new paper, turn the specimen through 90 degrees so that the new scratches
formed are perpendicular to the earlier scratches. Continue polishing until all the old scratches
disappear and the specimen contains only the new scratches. Once the specimen shows only new
scratches, wash the specimen, dry it and go to the next finer paper 2/0
6. Follow similar procedure and polish using 3/0 and 4/0 papers.
7. After polishing with 4/0 paper, wash the specimen and polish on polishing wheel using abrasives like
SiC or Al2O3
8. While polishing on the wheel, apply little pressure and keep rotating the sample.
9. Continue polishing until the sample is free from all the scratches and has attained a mirror finish.
10. Wash the specimen, dry it with hot air blower.
11. View the polished surface under the optical microscope. Draw the microstructure of this un-etched
specimen and label the various micro constituents. This un-etched specimen shows graphite flakes.
Classify these flakes using the charts.
12. Now, Etch the specimen with 2% Nital. Observe the surface under the optical microscope. Identify
various features of the microstructure like the various phase, grains, grain boundaries etc. Draw the
microstructure and label the various micro constituents.

Questions:
1. What are Cast irons?
2. Name the elements which promote graphitization in Grey Cast Iron
3. How do graphite flakes affect mechanical properties of grey cast iron?
4. What is the general composition of Grey Cast Iron?
5. Why graphite flakes are visible even in the unetched condition?
5. Describe the types and distribution of graphite flakes in cast irons
6. Name the different types of cast irons

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Observations:

Material: Chemical Composition:

Condition: Un-etched Condition: Etched with …………….

Magnification: Magnification:

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Experiment 4: Quantitative Metallography
Aim: To determine (i) Grain size (ii) Amount of phases by different methods
I. Grain Size Measurement:

(a) ASTM Grain Size Number:

This is the most common method of designating the austenite grain size.
ASTM grain size is defined by the relation;

n = 2 N-1

Where, n = number of grains per square inch in a specimen viewed at 100X

N = ASTM Grain size number

Following table relates the ASTM grain size number to the size of the grains. The usual range of austenite
grain size number is 1 to 9.

Procedure:
1. Obtain a metallographically prepared sample in polished and etched condition clearly showing austenitic
grain structure.
2. Project the image on to a screen or get a photograph of the image magnified 100 times.
3. Mark 1 square inch area and count the number of grains in this area. For grains intersecting the perimeter,
If more than half of the grain is inside the square consider it as one grain and if less than half is inside the
square, omit that grain. Take several readings (at least 10) at different locations of the sample. More the
number of reading better will be the accuracy. Estimate the ASTM grain size number using the formula.

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4. Alternatively, We can also determine the ASTM grain size number by comparing the microstructure with
standard charts.

Observations:
Sl. No. Location No. No. of grains/sq. inch at 100 X
1 Location No. 1
2 Location No. 2
3 Location No. 3
4 Location No. 4
5 Location No. 5
6 Location No. 6
7 Location No. 7
8 Location No. 8
9 Location No. 9
10 Location No. 10
Average

Calculations: Average No. of grains/sq. inch at 100 X, n =

We have, n = 2 N-1

Result:
ASTM Grain size number, N = ………..
ASTM Grain size number, N from standard charts =

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(b) Jefferies Planimetric Method:
This method is developed for non-ferrous metals and alloys.

Procedure:
1. Project the image on to a screen or get a photograph of the image at known magnification
2. Mark a circle of 50 mm diameter on the image. In fact, we can choose any shape like square, rectangle
etc.
3. Count the number of grains intersected by the circumference of the circle, ne
4. Count the number of grains lying within the circle, na
5. Calculate the equivalent number of whole grains, neq, in the area of 5000 mm2 ;

neq = ne / 2+na
𝑛𝑒𝑞 2
The number of grains per unit area, NA = ×𝑚
𝐴

Where A is the area of the circle.

6. Repeat the procedure at other locations of the specimen (at least 5 locations) and calculate the mean
value.
7. Declare the grain size as grains/mm2

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Observations:
Sl. No. Location No. No. of grains No. of grains Equivalent
intersected by the lying within number of
circumference of the circle, na whole grains,
the circle, ne neq
1 Location No. 1
2 Location No. 2
3 Location No. 3
4 Location No. 4
5 Location No. 5
Average

Calculations: Average Equivalent No. of grains, neq =

Area of the Circle, A =

Magnification, m =
𝑛𝑒𝑞 2
∴ The number of grains per unit area, NA = ×𝑚 = ……………
𝐴

Result: The number of grains per unit area =

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(c) Heyn’s Intercept Method:
This is also called Linear Intercept Method.

Procedure:
1. Project the image on to a screen or get a photograph of the image at known magnification
2. Draw a line of known length L, on the image
3. Count the number, ng of grain boundaries intersected by the line
4. Calculate the number of grains per unit length is nL= ( ng – 1) / L
5. If m is the magnification, number of grains per unit length in the sample is , NL= nL× m.
6. Repeat the procedure in different orientations (directions) and obtain the mean value.
7. Declare the grain size as number of grains/mm

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Observations:
Length of the line considered, L:
Sl. No. Location No. No. of grain boundaries No. of grains per unit length, nL
intersected by the line, ng (ng-1) /L

1 Direction 1
2 Direction 2
3 Direction 3
4 Direction 4
5 Direction 5
Average
Calculations: Average No. of grains/unit length, nL =

Magnification, m =
∴ The number of grains per unit length, NL = nL × m

Result: The number of grains per unit length =

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II. Determination of amount of Phases:
Consider a 2-phase alloy like (α − β) Brass
(a) Linear intercept method:
Procedure:
1. Project the image of well-polished and etched specimen on to a screen or get a photograph.
2. Draw a line of known length L, on the image
3. Determine what length of the total length is covered by α phase. If this length is lα, then percentage of α
phase is ( lα / L ) X 100 . Rest is % β phase.
4. Repeat the procedure in different orientations (directions), at least 10 orientations and obtain the mean
value.
5. Declare the amount of each phase

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Observations:
Length of the line considered, L:
Sl. No. Location No. Length of the line covered % α phase =
𝑙α
×100
𝐿
by α phase, lα

1 Direction 1
2 Direction 2
3 Direction 3
4 Direction 4
5 Direction 5
6 Direction 6
7 Direction 7
8 Direction 8
9 Direction 9
10 Direction 10
Average

Result:
% α phase = ………..
% β phase = ………

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Phase counting:
Procedure:
1. Project the image of well-polished and etched specimen on to a screen or get a photograph.
2. Superimpose a square grid (of at least 100 squares i.e. 10x10) on the image
3. Count the number of squares covered by α phase and that by β phase. While counting, if more than half
of the square is covered by a phase then take it as one and if less than half of the square is covered by a
phase then take it as zero.
4. Calculate the Percentage of phases;

𝑇𝑜𝑡𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑠𝑞𝑢𝑎𝑟𝑒𝑠 𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝑏𝑦 α 𝑝ℎ𝑎𝑠𝑒

% of α phase = 𝑇𝑜𝑡𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑠𝑞𝑢𝑟𝑒𝑠 𝑖𝑛 𝑡ℎ𝑒 𝑔𝑟𝑖𝑑
×100

% 𝑜𝑓 β phase = 100 - % of α phase

5. Repeat the procedure at different locations (at least 5 locations)

Questions:
1. What is the effect of grain size on strength, hardness, ductility?
2. Why do grain boundaries etch dark compared to the grain interior?
3. What is the significance of austenitic grain size?
4. While using linear intercept method, why is it necessary to take readings in different directions?
5. Classify the grains into ultra-fine grains, fine grains and coarse grains.

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Observations:
Total number of squares in the grid, N = ……
Sl. No. Location No. Number of squares % α phase =
𝑛α
×100
𝑁
covered by α phase, nα

1 Direction 1
2 Direction 2
3 Direction 3
4 Direction 4
5 Direction 5
Average

Result:
% α phase = ………..
% β phase = ………

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Experiment 5: Construction of Phase Diagram by Thermal Analysis
Aim: To determine the Pb-Sn binary phase diagram by Thermal Analysis

Procedure:
1. Take Pb-Sn alloys of known compositions and melt it in a in a crucible [Note: each batch will take
alloys of different composition],
2. Insert a thermocouple in the molten alloy and connect the cold junction to EMF measuring device
3. Switch off the power supply to the furnace and allow the molten alloy to cool at a very slow rate.
4. Note down the EMF readings at regular intervals of time (every 10 secs)
5. Continue taking readings until the EMF reading reaches a value corresponding to 130-degree
Celsius.
6. Plot the graph of EMF Vs Time or Temperature Vs. time
7. Identify the temperature corresponding to the phase transformations.
8. Get similar values from other batches for other compositions and finally plot the Phase diagram
covering the entire composition.

Questions:
1. Draw the cooling curve for pure Fe
2. Why the temperature remains constant for a long period in cooling curve of pure metals?
3. How the phase transformations are indicated in cooling curves?
4. What are the limitations of Thermal Analysis for determination of phase diagrams?
5. List and briefly explain other methods of determination of phase diagrams

Page 21 of 26
Observations:
Composition of the Alloy Taken:

Sl. No. Time (Sec) mV reading Sl. No. Time (Sec) mV reading
1 29
2 30
3 312
4 32
5 33
6 34
7 35
8 36
9 37
10 38
11 39
12 40
13 41
14 42
15 43
16 44
17 45
18 46
19 47
20 48
21 49
22 50

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23 51
24 52
25 53
26 54
27 55
28 56
57
58

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Page 24 of 26
Result:
Critical Transformation Temperatures:
(i) L to α / β = (ii) Eutectic Temperature =

Experiment 6: Study on Cu-Zn Diffusion Couple

Aim: To study the diffusion Characteristics of Cu-Zn Diffusion Couple
Procedure:
1. Melt sufficient quantity of Pure Zinc in a crucible and maintain the melt at 500 ℃
2. Take a rod of pure copper and polish the surface to remove any oxide layer.
3. Immerse the copper rod into the molten Zn and fix the rod with a stand so that the rod remains
vertical throughout the experiment.
4. Leave this set up for 2 hours at 500 ℃
5. After 2 hours allow the set up to cool to room temperature
6. After cooling, cut the copper rod vertically into two halves along with the zinc.
7. Polish and etch the cut surface for metallographic examination using the standard procedure.
8. Observe the microstructural features of this Cu-Zn couple especially at the interface.
9. Draw the microstructure

Questions:
1. In Cu-Zn diffusion couple which elements diffuse faster?
2. What is Kirkendall effect?
3. Why cavities are observed towards the Zn-side of the interface
4. Why copper rod shows wrought structure whereas Zn shows dendritic structure?
5. Why two-phase regions are not seen in the interface of isothermal diffusion couple?

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Observations:
Material: Cu-Zn Diffusion Couple

Condition: Etched with …………….

Magnification:

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