Department of Metallurgical and Materials Engineering

National Institute of Technology Warangal

Phase Transformation and Heat Treatment

Laboratory
(Course code: MM 255)

Laboratory Manual
2nd Year B.Tech. in Met & Mat Engineering
II Semester

Course Instructor

Dr. Asit Kumar Khanra

Department of Metallurgical and Materials Engineering

National Institute of Technology Warangal
Warangal-506 004, Telangana State

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

MM 255 Phase Transformation and Heat Treatment Lab PCC 0022 02

Pre-requisites: Physical Metallurgy

Course Outcomes: At the end of the course, student will be able to:
CO1 Determination of Grain size and Calculation of Phases
CO2 Heat Treatment of Samples
CO3 Microstructure and Hardness Study of Annealed, Normalised and Hardened Samples
CO4 Hardenability of Steel Samples by Jominy End Quench

Brief syllabus
Grain size measurement & Calculation of Volume fraction of Phases, Microstructure of Steels
and Composites, Microstructure of Annealed, Normalising, Hardened samples, Tempering,
Jominy End Quench Test and Scanning Electron Microscopy (SEM) Study of Different Samples

REFERENCES:
1. Introduction of Physical Metallurgy, Mc Graw Hill, 1987- S. H. Avner.
2. Materials Science and Engineering, Prentice Hall, 4th Edition, New Delhi, 1999- V. Raghavan.
3. Alloy Phase Diagrams, ASM Handbook, Volume 3.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

Experimental Plan

Necessary study before the start of Experiments

LAYOUT of Physical Metallurgy & Heat Treatment (PTHT) Laboratory

List out the various equipment required for PTHT Lab
Study of Different Phase Diagrams
Sl. No. List of Experiments
1 Calculation of Grain Size and Volume fraction of Phases of given Microstructure
2 Grain size Measurement by American Society for Testing and Materials (ASTM) Method
3 Observation of Microstructure of Iron based unknown Samples
4 Annealing, Normalising and Hardening of Steel samples
5 Observation of Microstructure of Heat Treated Steel Samples
6 Tempering of Hardened Steel and Study the Effect of Tempering Conditions
7 Determination of Hardenability by Jominy End Quench Test
8 Austempering of Spheroidal Graphite (SG)/ Nodular Cast Iron

Necessary Instructions

(i) Students should submit lab report in the next lab class.
(ii) Students are requested to maintain rules and regulation of lab as per instruction.
(iii) Students should have a minimum of 80% Attendance.

Scheme of Evaluation

Sub-components Weightage
Continuous Evaluation 50 Marks
End Semester Examination 50 Marks

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

LAYOUT of Physical Metallurgy & Heat Treatment (PTHT) Laboratory

List out the various equipment required for PTHT Lab

1. Please keep scale bar in the Layout of Lab.

2. Please write the details of Specification of each equipment with Manufacturer.
3. Please write basic principle of each equipment.
4. Submit the Layout in the form of drawing sheet.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

Study of Different Phase Diagrams

Materials to be used: Drawing Sheet and Drawing items etc.

Instruction:

Students are requested to make Phase Diagram as per discussion in the lab.

Procedure:

Draw/ Print of Phase Diagram as per discussion.

Precautions:

⮚ Try to maintain the size of Phase Diagram as per scale.

⮚ All the points, level etc. should be clearly visible.

Deliverable:

1. Submission of Phase Diagram in the form of Sheet with name and roll number of students
2. Define Phase. What is the Gibb’s Phase rule?
3. What is the importance of Phase Diagram from the Alloy Design point of view?

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

Experiment number – 1

a) Grain size measurement and

b) Calculation of Volume fraction of Phases of given Microstructure by Line Intercept Method

Basic Theory:
The grain size is one of the key parameter for the materials processing. The basic mechanical properties
such as yield strength, tensile strength, fatigue strength etc. are controlled by the grain size. Hall-Petch
equation deals the relationship between the grain size (D) and yield strength (YS) of materials:

Where, and K are friction stress and constant respectively.

High cooling rate in rapid solidification processing (RSP) leads to generation of fine grain structure. The
grain structure of materials can be refined by controlled mechanical working process such as rolling,
forging, extrusion etc. Therefore, it is necessary to measure the grain size of materials. Again, the
properties also depend on the shape, size and distribution of different phases in the matrix. The line
intercept method can be adopted in order to calculate the volume fraction of phases of the microstructure.

Materials and Apparatus to be used: Hard copy of microstructures, Scale bar, Pencil, Eraser and
Calculator etc.

Procedure:

1. Draw straight lines of different directions over the given microstructure

2. Measure the intercept for each gain and then find an average grain size for each line.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
3. Take an average of 30 to 40 lines
4. Find the average grain size with error (such as 10 ± 1.0) µm.
5. Similar principle is applicable in order to calculate the volume fraction of different phases.

Precautions:

Draw lines as maximum as possible in order to get better accuracy of results.

Deliverable:

1. Calculate the average grain size of given microstructures.

2. Calculate the volume fraction of different phases of given microstructures.
3. Calculate the grain size and volume fraction of phases of other given microstructures.
4. Please find the accuracy level for calculations.
5. What are the importances of measuring grain size and volume fraction of phases?

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

Experiment number - 2

Grain size measurement by American Society for Testing and Materials (ASTM) Method

Objective:
✔ Sample preparation for the metallographic study.
✔ To measure the grain size by ASTM method.

Basic Theory:
The grain size is one of the key parameter for the materials processing. The basic mechanical properties
such as yield strength, tensile strength, fatigue strength etc. are controlled by the grain size. Hall-Petch
equation deals the relationship between the grain size (D) and yield strength (YS) of materials:

Where, and K are friction stress and constant respectively.

High cooling rate in rapid solidification processing (RSP) leads to generation of fine grain structure. The
grain structure of materials can be refined by controlled mechanical working process such as rolling,
forging, extrusion etc. The ASTM method can be applied in order to measure the ASTM grain size
number.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
Materials and Apparatus to be used: Optical Microscope, Belt Grinder, Disc Polisher, Standard Eye
Piece for ASTM Grain size Measurement, Sample for metallographic study.

Procedure:

A) Metallographic Study:
1. Take a sample for microstructure study which is made by Lathe
machine.
2. Make the surface of sample flat using belt grinder.
3. Polish the samples by using 400 grit paper for 10 min (approx.) and get scratch in polishing
direction (one direction). Then rotate the sample by 90 degree before moving to next sand paper.

4. Polish the sample on 800 grit paper and get scratch in polishing direction (one direction) rotate 90
degree for every cases before moving to next grit paper.
5. Polish the sample on 1200 and then 1500 grit papers respectively and get fine scratch in one
direction only.
6. Clean the sample using distilled water and polish the samples in Disc Polisher for 5 min. Alumina
dispersed water should be added to disc during polishing as per instruction.
7. Clean and dry the surface after polishing and see the surface structure under OM. If there is any
scratch, please repeat the procedure (Sl. No. 3 to 7).
8. Etching of surface which is free from scratch etc.
9. Drying of samples.
10. Observation of microstructure under OM at different magnifications.

B) ASTM Grain size measurement:

1. Observation of microstructure of samples under optical microscope at different magnifications.

2. Find a better distribution of grain at 100X.
3. Take special eye piece for ASTM Grain size Measurement of given sample.
4. Match the grain size as per grid size and find the ASTM number.
5. Measure the grain size at different locations and find an average ASTM number.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

Precautions:
a) Grain boundary of sample should be visible properly as per discussion.
b) Try to locate a suitable position for ASTM grain size measurement wherein the uniform grain size
is visible.

Deliverable:

1. Find the grain size and its distribution for standard and unknown (sample given for study) samples.
2. Differentiate the grain size measurement between the Line Intercept and ASTM Method.
3. Calculate the number of grains/sq. cm for N = 3 and 10 respectively.

Experiment number - 3: Observation of Microstructure of Iron based Samples

Objective:
✔ Samples preparation for the metallographic study.
✔ Microstructure study of samples at different magnifications.

Basic Theory:
Unlike the crystal structure, the Microstructure is governed by the life history of the metals. This means
that by studying the microstructure, we can have an idea about the way the metal has been processed
(rapid solidification process, mechanical deformation or welding etc.). Properties such as yield strength,
tensile strength are largely dependent on the microstructure (structure-sensitive properties). Hence a study
of the microstructure gives significant information of samples.

Materials and Apparatus to be used: Optical Microscope, Belt Grinder, Disc Polisher, Different
Samples, Different items (sand paper, polishing cloths, Alumina powder etc.) for Metallographic Study.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
Procedure:
1. Take sample for microstructure study which is made by Lathe Machine.
2. Make the surface of sample flat using belt grinder.
3. Polish the samples by using 400 grit paper for 10 min (approx.) and get scratch in polishing
direction (one direction). Then rotate the sample by 90 degree before moving to next sand paper.
4. Polish the sample on 800 grit paper and get scratch in polishing direction (one direction) rotate 90
degree for every cases before moving to next grit paper.
5. Polish the sample on 1200 and then 1500 grit papers respectively and get fine scratch in one
direction only.
6. Clean the sample using distilled water and polish the samples in Disc Polisher for 5 min. Alumina
dispersed water should be added to disc during polishing as per instruction.
7. Clean and dry the surface after polishing and see the surface structure under OM. If there is any
scratch, please repeat the procedure (Sl. No. 3 to 7).
8. Etching of surface which is free from scratch etc. (Etchant: as per sample).

9. Drying of samples.
10. Observation of microstructure under OM at different magnifications.
11. Draw the microstructures in lab note book.
12. See and draw the microstructure of other samples.

Precautions:
a) Sample surface should be exactly flat to the polishing paper during the polishing.
b) Don’t add much alumina dispersed water on the Disc during the disc polishing.
c) Grain boundary of sample should be clearly visible.
d) Understand the role of etchant and the effect of over and under etched conditions carefully.
e) Observe the laminar structures of different samples carefully.

Some Practical Tips for Microstructure Study

⮚ Start always at lowest magnification i.e. 50X, then go to higher magnifications progressively.
⮚ Ask yourself if there are any scratch, etch pits or other foreign particles or any marks on surface.
⮚ Look for grain boundary and see the grain size, shape and distribution.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
⮚ Look for different features such as presence of twins, dendritic, elongated grain etc.
⮚ Ask yourself whether it consists of single phase or multi-phase.
⮚ Look for the shape and distribution of phases in the microstructure.

Deliverable:

1. Understand the microstructures at different level of carbons.

2. Classify the different steel and cast irons.
3. What is the effect of carbon on the properties of steel?
4. Calculate the volume fraction of phases at different levels of carbon by using lever rule.
5. What are the basic principle and application of Image Analyser?

Experiment number - 4: Annealing, Normalizing and Hardening of Steel Samples

Objective:
✔ Soaking of samples at fixed Temperature for Heat Treatment.
✔ Different Heat Treatment of Samples.

Basic Theory:
Heat Treatment is a process of heating, soaking and cooling of materials in order to modify the properties
of materials and it is a solid state process. Manufacturing industries need heat treatment as a secondary
process for the increase of hardness, strength etc. of components which find application in auto-sector,
aerospace etc. Annealing process is based on slow cooling whereas air cooling is adopted in Normalising
process. Hardening leads to transformation of austenite to martensite by a rapid quenching process. The
morphology of martensite is like needle structure which enhances hardness and strength of steels. Hence

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
the experiment of heat treatment of steel is necessary in order to study of the effect of different heat
treatment on the properties of steels.

Materials and Apparatus to be used: Muffle Furnace (Resistance heating type), Different Steel
Samples, Quenching tank with water, Bricks etc.

Procedure:
1. Make samples free from surface oxides, grease, dirt etc. for heat treatment.
2. Set a fixed temperature (1050° C) and switch on the muffle furnace.
3. Loading of samples after reaching the set temperature.
4. Soaking of samples as per discussion.
5. Rapid quenching of samples in water without any delay for Hardening.
6. Keep samples in normal air for Normalising.
7. Keeping samples in the furnace, switch-off the muffle furnace for slow cooling (Annealing).

Precautions:
i) Carefully handle the sample during loading and unloading of samples.
ii) Use heat resistance gloves and goggles.
iii) Stirring of water during water quenching.

Deliverable:

1. Define heat treatment process.

2. What are the main aims of heat treatment process?
3. Is there any other process which enhances mechanical properties of steel?
4. Differentiate Annealing, Normalizing and Hardening Processes.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal

Experiment number - 5: Observation of Microstructure of Heat Treated Steel Samples

Objective:
✔ Metallographic study of Heat Treated Samples.
✔ Identify the microstructural difference of different heat treated samples

Basic Theory:
Annealing, Normalizing and Hardening are the most common heat treatment process in order to alter the
microstructure of steels which finally changes the hardness etc. Annealing process is based on slow
cooling whereas air cooling is adopted in Normalizing process. Hardening leads to transformation of
austenite to martensite by a rapid quenching process. The morphology of martensite is like needle
structure which enhances hardness and strength of steels. The various cooling rate in the heat treatment

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
process results in formation of different level of microstructures. Therefore, the microstructure study of
heat treated samples is necessary in order to understand the structure-property correlation study.

Materials and Apparatus to be used: Optical Microscope, Belt Grinder, Disc Polisher, Different Heat
Treated Samples, Hardness tester, Different items (sand paper, polishing cloths, Alumina powder etc.) for
Metallographic Study.

Procedure:
1. Take heat treated samples for microstructure study.
2. Make the surface of sample flat using belt grinder.
3. Polish the samples by using 400 grit paper for 10 min (approx.) and get scratch in polishing
direction (one direction). Then rotate the sample by 90 degree before moving to next sand paper.
4. Polish the sample on 800 grit paper and get scratch in polishing direction (one direction) rotate 90
degree for every cases before moving to next grit paper.
5. Polish the sample on 1200 and then 1500 grit papers respectively and get fine scratch in one
direction only.
6. Clean the sample using distilled water and polish the samples in Disc Polisher for 5 min. Alumina
dispersed water should be added to disc during polishing as per instruction.
7. Clean and dry the surface after polishing and see the surface structure under OM. If there is any
scratch, please repeat the procedure (Sl. No. 3 to 7).

8. Etching of surface which is free from scratch etc (Etchant: as per instruction).
9. Drying of samples.
10. Observation of microstructure under OM at different magnifications.
11. Draw the microstructures in lab note book.
12. See and draw the microstructure of all heat treated samples.
13. Measure the average hardness (Rockwell C scale) of different heat treated samples.

Precautions:
a) Sample surface should be exactly flat to the polishing paper during the polishing.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
b) Don’t add much alumina dispersed water on the Disc during the disc polishing.
c) Grain boundary of sample should be clearly visible as per discussion.
d) Understand carefully the role of etchant and the effect of over and under etched conditions.
e) Observe carefully the laminar structures of different samples.

Some Practical Tips for Microstructure Study

⮚ Start always at lowest magnification i.e. 50X. Then go to higher magnifications progressively.
⮚ Ask yourself if there are any scratch, etch pits or other foreign particles or any marks on surface.
⮚ Look for grain boundary and see the grain size, shape and distribution.
⮚ Look for different features such as presence of twins, dendritic, elongated grain etc.
⮚ Ask yourself whether it consists of single phase or multi-phase.
⮚ Look for the shape and distribution of phases in the microstructure.

Deliverable:

1. Understand the microstructures of different heat treated samples.

2. What are the most common hardening defects and how do you minimize those defects?
3. Find the trend of hardness change of different heat treated samples.

Experiment number - 6: Tempering of Hardened Steel and Study the Effect of

Tempering Conditions

Objective:
✔ Metallographic study of Tempered Samples.
✔ Effect of Tempering Condition on the Hardness of Samples.

Basic Theory:
Hardening of steels leads to increase of excessive hardness, low ductility and generation of thermal stress
(residual stress) etc. Tempering heat treatment is carried out just after the hardening without any delay in
order to get an optimum combination of strength and toughness and to relieve the residual stress.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
Basically tempering is nothing but low temperature normalizing process which take care the bad effect of
hardening process. Tempering of hardened steels results in formation of temper martensite and
dissociation of martensite into other structures, which indicates unstable structure of martensite.
Therefore, the tempering of hardened steel samples is necessary in order to get optimum combination of
properties of steel without residual stress.

Materials and Apparatus to be used: Optical Microscope, Muffle furnace, Belt Grinder, Disc Polisher,
Hardened Samples, Hardness tester, Different items (sand paper, polishing cloths, Alumina powder etc.)
for Metallographic Study.

Procedure:
1. Take heat treated samples for microstructure study.
2. Make the surface of sample flat using belt grinder.
3. Polish the samples by using 400 grit paper for 10 min (approx.) and get scratch in polishing
direction (one direction). Then rotate the sample by 90 degree before moving to next sand paper.
4. Polish the sample on 800 grit paper and get scratch in polishing direction (one direction) rotate 90
degree for every cases before moving to next grit paper.
5. Polish the sample on 1200 and then 1500 grit papers respectively and get fine scratch in one
direction only.
6. Clean the sample using distilled water and polish the samples in Disc Polisher for 5 min. Alumina
dispersed water should be added to disc during polishing as per instruction.

7. Clean and dry the surface after polishing and see the surface structure under OM. If there is any
scratch, please repeat the procedure (Sl. No. 3 to 7).
8. Etching of surface which is free from scratch etc. (Etchant: as per instruction).
9. Drying of samples.
10. Observation of microstructure under OM at different magnifications.
11. Draw the microstructures in lab note book.
12. See and draw the microstructure of all heat treated samples.
13. Measure the average hardness (Rockwell C scale) of different heat treated samples.

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
Precautions:
i) Carefully handle the sample during loading and unloading of samples.
ii) Use heat resistance gloves and goggles.
iii) Take atleast 05 readings to get average hardness of tempered samples.

Deliverable:

1. Understand the importance of tempering heat treatment.

2. What is temper embrittleness?
.

Experiment number - 7: Determination of Hardenability by Jominy End Quench Test

Objective:
✔ To understand the importance of Hardenability measurement.
Basic Theory:
Hardenability can be defined as ability to harden and it is a very common test in the heat treatment
industries. It gives two information such as depth and distribution of hardness across the cross section of

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
sample and the rate at which given steel sample to be quenched. Therefore, the hardenability
measurement is necessary in order to see the ability of hardening of sample.

Materials and Apparatus to be used: Jominy End Quench unit, Heat Muffle furnace, Jominy bar etc.

Procedure:
1. Clean the surface of Jominy bar as per instruction.
2. Set a fixed temperature (1050o C) and switch on the muffle furnace.
3. Loading of Jominy bar after reaching the set temperature.
4. Soaking of samples as per discussion.
5. Place the Jominy bar quickly in the proper place of Jominy quench tank.
6. Switch on the water circulation and cool for 20 min.
7. Observe the colour change of the Jominy bar with the time.
8. Clean the surface after cooling.
9. Measurement of harness from the quench end of the sample.
10. Make a relationship between the hardness and distance from quench end.

Precautions:
i) Carefully handle the sample during loading and unloading of samples.
ii) Use heat resistance gloves and goggles.

Deliverable:

1. Understand the importance of hardenability measurement.

2. Differentiate hardness and hardenability.

Experiment number -8: Austempering of Spheroidal Graphite (SG)/ Nodular Cast Iron

Objective: Austempering/ Isothermal Quenching of Spheroidal Graphite (SG)/ Nodular Cast Iron

Basic Theory:

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 Department of Metallurgical and Materials Engineering
National Institute of Technology Warangal
Austempered Ductile Iron (ADI) has superior properties than other variety of cast iron and properties
even comparable with the steel also. The ADI is austempered as per the TTT plot in order to get Bainitic
Structure. Austempering treatment basically does not require the tempering treatment.

Materials and Apparatus to be used: Optical Microscope, Muffle furnace, Belt Grinder, Disc Polisher,
SG Iron Samples, Hardness tester, Different items (sand paper, polishing cloths, Alumina powder etc.) for
Metallographic Study.

Procedure:
1. Austempering of SG iron
7. Observation of microstructure before and after the treatment.
8. Observation of Hardness improvement after the treatment.

Deliverable:

1. Differentiate between the Austempering and Martempering.

2. What the application of ADI?

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