HEAT TREATMENT & PHASE

TRANSFORMATIONS

Laboratory Manual cum Observation

Book

Name of the Student:

Roll Number:

Laboratory Coordinator -Dr. Manoj Chopkar

Department of Metallurgical & Materials

Engineering

National Institute of Technology Raipur

G E Road, Raipur 492010
 TABLE OF CONTENTS

S. No Experiment Title Page No

1. Concepts in Phase Transformations & Heat Treatment (Revisit) 01

2. Annealing & Normalizing 08

3. Spherodising & Hardening 16
4. Jominy End Quench Test 25
5. Carburization of Steel 32
6. Precipitation Hardening 37
 EXPERIMENT 1

CONCEPTS IN PHASE TRANSFORMATIONS & HEAT TREATMENT

Draw Fe-Fe3C Phase Diagram and identify the phases

01
Draw Fe-C Phase Diagram and identify the phases

02
Draw TTT Diagram for Hypo-Eutectoid, Eutectoid, Hyper-eutectoid Steels

03
Draw CCT Diagram for Hypo-Eutectoid, Eutectoid, Hyper-eutectoid Steels

04
Draw CCT Diagram for Hypo-Eutectoid, Eutectoid, Hyper-eutectoid Steels

05
Draw CCT Diagram for Hypo-Eutectoid, Eutectoid, Hyper-eutectoid Steels

06
Draw a schematic view of a laboratory furnace

07
 EXPERIMENT 2

ANNEALING & NORMALIZING

OBJECTIVE

To study the microstructure, grain size and hardness of Annealed and Normalized plain carbon
steel having ≤0.2%C and ≤0.4%C.

EQUIPMENT / MATERIALS

Steel samples of 0.2%C, 0.4%C and 1.2%C, Electric furnace, SiC papers of various grit sizes,
Polishing machine, Metallurgical microscope, Rockwell hardness tester.

THEORY

The heat treatment includes heating and cooling operations or the sequence of two or more such
operations applied to any material in order to modify its metallurgical structure and alter its
physical, mechanical and chemical properties. Usually it consists of heating the material to some
specific temperature, holding at this temperature for a definite period and cooling to room
temperature or below with a definite rate. Annealing, Normalizing, Hardening and Tempering are
the four widely used heat treatment processes that affect the structure and properties, and are
assigned to meet the specific requirements from the semi-fabricated and finished components.
Steels being the most widely used materials in major engineering fabrications undergo various
heat treatment cycles depending on the requirements.

Annealing refers to a wide group of heat treatment processes and is performed primarily for
homogenization, recrystallization or relief of residual stress in typical cold worked or welded
components. Depending upon the temperature conditions under which it is performed, annealing
eliminates chemical or physical non-homogeneity produced of phase transformations. Few
important variants of annealing are full annealing, isothermal annealing, spheroidise annealing,
recrystallization annealing, and stress relief annealing. In this experiment we will do full annealing
treatment of carbon steels.

Full annealing
Full annealing process consists of three steps. First step is heating the steel component to above
A3 (upper critical temperature for ferrite) temperature for hypo-eutectoid steels and above
o
A1(lower critical temperature) temperature for hypereutectoid steels by 30-50 C. The second step
is holding the steel component at this temperature for a definite holding (soaking) period of at least
20 minutes per cm of the thick section to assure equalization of temperature throughout the cross-
section of the component and complete austenization. Final step is to cool the hot steel component
to room temperature slowly in the furnace, which is also called as furnace cooling. The full

08
annealing is used to relieve the internal stresses induced due to cold working, welding, etc, to
reduce hardness and increase ductility, to refine the grain structure, to make the material
homogenous in respect of chemical composition, to increase uniformity of phase distribution, and
to increase machinability.

Normalizing

Normalizing process consists of three steps. The first step involves heating the steel component
above the A3 temperature for hypo eutectoid steels and above A cm (upper critical temperature for
0 0
cementite) temperature for hypereutectoid steels by 30 C to 50 C (Figure 4.7.5). The second step
involves holding the steel component long enough at this temperature for homogeneous
austenization. The final step involves cooling the hot steel component to room temperature in still
air. Due to air cooling, normalized components show slightly different structure and properties
than annealed components.

The properties of normalized components are not much different from those of annealed
components. However, normalizing takes less time and is more convenient and economical than
annealing and hence is a more common heat treatment in industries. Normalizing is used for high-
carbon (hypereutectoid) steels to eliminate the cementite network that may develop upon slow
cooling in the temperature range from point Acm to point A1. Normalizing is also used to relieve

internal stresses induced by heat treating, welding, casting, forging, forming, or machining.
Normalizing also improves the ductility without reducing the hardness and strength.

Schematic representation of annealing operation

09
PROCEDURE

10
OBSERVATIONS

Observe the microstructure and write down the phases present

Sample Identity:

Draw the microstructure in the circle given below and write down the phases

Magnification used

The phases present in the microstructure and the approximate % of major phases are

Phases Present Percentage

Etchant used Hardness

From the observation of microstructure & Hardness of the given sample

…………………………………………………………………………………………………..
…………………………………………………………………………………………………..
………………………………………………………………………………………………......
.............................

11
Observe the microstructure and write down the phases present

Sample Identity:

Draw the microstructure in the circle given below and write down the phases

Magnification used

The phases present in the microstructure and the approximate % of major phases are

Phases Present Percentage

Etchant used Hardness

From the observation of microstructure & Hardness of the given sample

…………………………………………………………………………………………………..
…………………………………………………………………………………………………..
………………………………………………………………………………………………......
..................................................................................................................................................

12
 Answer the following Questions
(1) Define the term “heat treatment”. Why are the steels heat treated?
Ans:- Heat treatment is a metallurgical process which involves heating a material (mostly, steels) up to a
predetermined temperature, holding at the same temperature for a definite period of time and cooling at a certain
rate to room temperature. All the physical and mechanical properties of steel depend on its microstructure and heat
treatment of steel allows us to fabricate microstructures according to over requirements.

(2) If one of the specimens of the same kind of steel is normalized and the other is annealed,which
will show more strength and why?
Ans:- Normalized steel will have more strength, as they will be having fine pearlite, while annealed steel
will have a weak structure consisting of coarse grains of pearlite.

(3) Out of the normalized and annealed samples, which one is more machinable and why?
Ans :- Machinability is the ease with which a material can be cut. Normalized samples would be hard and strong,
making them not suitable for machinability. Hence, annealed steel sample is more machinable.

(4) How does the hardness vary with cooling rate?

Ans :- Faster cooling rates produce hard and brittle phases with small grains. Slower cooling rates provide
sufficient time for grain growth thus grain coarsening reduces the overall hardness.

13
(5) How do your microstructures compare with standard microstructures?
Ans :-

(6) What temperature will be used for annealing and normalizing the mild steel specimen with
0.25%C?
Ans :- The temperature range for annealing process range from 260 to 760 degree Celsius whereas
normalizing process is done in temperature range 750 to 980 degree Celsius.

(7) What is the nature of the microstructure in spheroidized high carbon steel, normalized high
carbon steel, annealed high carbon steel?
Ans :- Microstructure in spheroidized high carbon steel, pearlite and spheroidized cementite.
Microstructure in normalized high carbon steel, uniform fine pearlite structure. Microstructure in
annealed high carbon steel, coarse pearlite and cementite network is observed.

14
(8) The microstructure of an iron-carbon alloy consists of proeutectoid ferrite and pearlite; the mass
fractions of these two micro constituents are 0.174 and 0.826, respectively. Determine the
concentration of carbon in this alloy.
0.8 − x
Ans :- 0.174 =
0.8 − 0.025
Therefore, the concentration of carbon in this alloy (x) = 0.665 wt % C.

(9) Explain the process of annealing?

Ans :- Annealing refers to a wide group of heat treatment processes and is performed primarily for
homogenization, recrystallization or relief of residual stress in typical cold worked or welded components. Few
important variants of annealing are full annealing, isothermal annealing, spheroidise annealing, recrystallization
annealing, and stress relief annealing.
Full annealing - Full annealing process consists of three steps. First step is heating the steel component to above
A (upper critical temperature for ferrite) temperature for hypo-eutectoid steel and above A (lower critical
temperature) temperature for hypereutectoid steels by 30-50 C. The second step 1 is holding the steel component
at this temperature for a definite holding (soaking) period of at least 20 minutes per cm of the thick section to
assure equalization of temperature throughout the cross section of the component and complete austenization.
Final step is to cool the hot steel component to room temperature slowly in the furnace, which is also called as
furnace cooling. The full annealing is used to relieve the internal stresses induced due to cold working,

(10) What is the significance of this experiment? How is it related to your course of study?
Ans :- By this experiment we will have a great knowledge about the annealing and the normalizing process. At
which temperature they occur and how they occur, what type of microstructure we get by the annealing and
normalizing which properties will be enhanced by the process, and it is totally related to our course of study,
because to heat treat any material we must have to great knowledge about annealing and normalizing.

15
 EXPERIMENT 3

SPHEROIDISING & HARDENING

OBJECTIVE

To study the microstructure and hardness of Hardened and Spheroidized plain carbon steel having
≤1.2%C steel.

EQUIPMENT / MATERIALS

Steel samples of 0.2%C, 0.4%C and 1.2%C, Electric furnace, SiC papers of various grit sizes,
Polishing machine, Metallurgical microscope, Rockwell hardness tester.

THEORY

One of the techniques to improve the ductility of the high carbon steels are spheroidised annealing.

Spheroidized annealing

Spheroidise annealing is one of the variant of the annealing process that produces typical
microstructure consisting of the globules (spheroid) of cementite or carbides in the matrix of ferrite.
The following methods are used for spheroidise annealing.

Holding at just below A1

Holding the steel component at just below the lower critical temperature (A1) transforms the
pearlite to globular cementite particles. But this process is very slow and requires more time for
obtaining spheroidised structure.

Thermal cycling around A1

In this method, the thermal cycling in the narrow temperature range around A1 transforms

cementite lamellae from pearlite to spheroidal. Figure depicts a typical heat treatment cycle to
produce spheroidised structure. During heating above A1, cementite or carbides try to dissolve and
during cooling they try to re-form. This repeated action spheroidises the carbide particles.
Spheroidised structures are softer than the fully annealed structures and have excellent
machinability. This heat treatment is utilized to high carbon and air hardened alloy steels to soften
them and to increase machinability, and to reduce the decarburization while hardening of thin
sections such as safety razor blades and needles.

16
 Figure 1: A typical heat treatment cycle to produce spheroidised structure

Different techniques to improve the hardness of the steels are conventional hardening, and
tempering.

Conventional hardening

Conventional hardening process consists of four steps. The first step involves heating the steel to
above A3 temperature for hypo-eutectoid steels and above A1 temperature for hypereutectoid steels

0
by 50 C. The second step involves holding the steel components for sufficient socking time for
homogeneous austenization. The third step involves cooling of hot steel components at a rate just
exceeding the critical cooling rate of the steel to room temperature or below room temperature.
The final step involves the tempering of the martensite to achieve the desired hardness. Detailed
explanation about tempering is given in the subsequent sections. In this conventional hardening
process, the austenite transforms to martensite. This martensite structure improves the hardness.
Following are a few salient features in conventional hardening of steel.
1. Proper quenching medium should be used such that the component gets cooled at a rate just
exceeding the critical cooling rate of that steel.
2. Alloy steels have less critical cooling rate and hence some of the alloy steels can be hardened
by simple air cooling.
3. High carbon steels have slightly more critical cooling rate and has to be hardened by oil
quenching.
4. Medium carbon steels have still higher critical cooling rates and hence water or brine quenching
is necessary.
Figure 2 depicts the conventional hardening process which involves quenching and tempering.
During quenching outer surface is cooled quicker than the center. Thinner parts are cooled faster
than the parts with greater cross-sectional areas. In other words, the transformation of the austenite
is proceeding at different rates. Hence there is a limit to the overall size of the part in this hardening
process.

17
 Figure 2: Heat treatment cycle for conventional hardening process

PROCEDURE

Conventional Hardening
1. In this experiment we have 3 steel samples all with different weight% of carbon 0.4%, 0.8% and 1.2%
respectively we will perform hardening with all the samples(before starting the experiment safety equipment
should be put on).
2. Hardness of all the samples should be measured before the heat treatment process using the Rockwell
hardness tester.
3. First we will take the 0.4% carbon steel and uniformally heat it to the A3 temperature and the 0.8% and 1.2%
carbon steel to A1 temperature by 500c.
4. And then as the sample reach their desired temperatures the samples are quickly put into the quenching
solution and are cooled down to obtain a much harder and high strength steel.
5. After quenching all the samples should be tested for their hardness using the Rockwell hardness tester to
confirm the increase in hardness due to the martensite formation.
6. After the hardness test, metallography will be done of the samples by first proper grinding of the sample by
Sic grinding paper will be done.
7. Proper polishing will also be done to obtain a good pictograph of the microstructure using polishing
machine.
8. Pictograph of the microstructure should be taken using the microscope for further inspection of the
microsturucture.

Spheroidized Annealing
1. In this experiment we have 3 steel samples all with different weight% of carbon 0.4%, 0.8% and 1.2%
respectively we will perform hardening with all the samples(before starting the experiment safety equipment
should be put on).
2. Hardness of all the samples should be measured before the heat treatment process using the Rockwell
hardness tester.
3. In Spheroidising the steel is heated to just below Ac1 temperature, and is holded at this temperature for a
very long time.

18
4. After that the sample is slowly cooled to obtain a microstructure consisting of coarse spheroidised cementite
particles embedded in the ferrite matrix.
5. After cooling all the samples should be tested for their hardness using the Rockwell hardness tester to
confirm the difference in hardness due to the formation of spheroidite.
6. After the hardness test, metallography will be done of the samples by first proper grinding of the sample by
Sic grinding paper will be done.
7. Proper polishing will also be done to obtain a good pictograph of the microstructure using polishing
machine.
8. Pictograph of the microstructure should be taken using the microscope for further inspection of the
microsturucture.

19
OBSERVATIONS

Observe the microstructure and write down the phases present

Sample Identity:

Draw the microstructure in the circle given below and write down the phases

Magnification used

The phases present in the microstructure and the approximate % of major phases are

Phases Present Percentage

Etchant used Hardness

From the observation of microstructure & Hardness of the given sample

…………………………………………………………………………………………………..
…………………………………………………………………………………………………..
………………………………………………………………………………………………......
.......................................................................................................................................................

20
Observe the microstructure and write down the phases present

Sample Identity:

Draw the microstructure in the circle given below and write down the phases

Magnification used

The phases present in the microstructure and the approximate % of major phases are

Phases Present Percentage

Etchant used Hardness

From the observation of microstructure & Hardness of the given sample

…………………………………………………………………………………………………..
…………………………………………………………………………………………………..
………………………………………………………………………………………………......
.......................................................................................................................................................

21
 Answer the Following Questions
(1) How do your tempered structures compare with standard microstructures of tempered
martensite and spheroidised steel?

Ans:- The microstructure of tempered martensite consists of extremely small and uniformly dispersed
cementite particles embedded within a continuous ferrite matrix. This is similar to the microstructure
of spheroidite except that the cementite particles are much, much smaller in tempered structure.

(2) Give the physical and mechanical changes that occur during the above phasetransformation.
Ans:- During Hardening of the steel a phase transformation of ferrite to austenite is seen and after
quenching martensite formation is seen which increases the hardness of the steel to a very high level
which in turn also makes it brittle. In Spheriodizing of the steel we can observe sphere like structures
called spheriodite formed from cementite in the steel microstructure which gives very high ductility and
machinability.

(3) Explain the nature of pearlite and cementite phase in spheroidised steel?
Ans:- In spheroidised steel due to the prolonged heating at a temperature below the eutectoid temperature the
pearlite, which is the lowest energy arrangement of steel, gets converted to ferrite and cementite and the graphite
content of steel assumes a spheroidal shape after spheroidizing and after prolonged heating the pearlite layers are
broken down and spherical lumps of cementite are formed.

(4) Why is tempering preceded by converting the steel into martensite phase?
Ans:- It is attributed to the formation of cementite particles at the martensite lath boundaries and within the laths.
During tempering, the particles coarsen and become large enough to crack, thus providing crack nuclei which may
then propogate into the matrix. As a consequence, untempered low carbon martensitic steels sometimes have a
better toughness than when they are tempered, even though the untempered steel is stronger. The cementite behaves
like a brittle inclusion.

22
(5) Which steel will be tougher, tempered high carbon steel or hardened medium carbon steel?
Ans :- Tempered high carbon steel will be much tougher than the hardened medium carbon steel because as stated
hardening is a process which makes steel much harder but also brittle. Therefore, Tempering is done after the
hardening process to reduce excess hardness and give more ductibility to the steel which in turn makes steel more
tough.

(6) What is the nature of the microstructure in Spheroidized high carbon steel, normalized high
carbon steel, annealed high carbon steel?
Ans:- In Spheroidized steel, sphere like structures called spheriodite formed from cementite is seen like
lumps in the microstructure. Whereas in normalized steel we can see a refine crystal structure and
produces a more uniform and desired grain distribution, fine grained pearlite and an absence of massive
proeutectoid ferrite in the microsturcture. The microstructure after annealing contains coarse ferrite and
pearlite , the main aim of annealing is to remove the internal stresses produced in the metal due to plastic
deformation.

(7) How does hardness vary with % carbon content in steels? Explain.
Ans :- Increasing carbon content increases hardness and strength and improves hardenability. But carbon also
increases brittleness and reduces weldability because of its tendency to form martensite. This means as the carbon
content increases, the proportion of cementite in the steel also increases. Since the cementite is relatively hard, the
hardness of the steel increases accordingly. This results in an almost linear relationship between the carbon content
and the hardness of the steel.

23
(8) Why it is necessary to be really quick in transferring the specimen from the austeniting furnace
to the water bath during quenching?
Ans:- In quenching to obtain proper hardness throughout the sample it is very important that the sample is cooled
faster as the rapid cooling changes the crystal structure of the steel, compared with a slow cooling. Depending on
the carbon content and alloying element of the steel, it can get left with a harder, more brittle microstructure such as
martensite or bainite, when it undergoes the quench hardening process. These microstructures result in increased
strength and hardness of the steel and a fast transport to the water bath is also helpful to prevent loss of heat from
the sample which could lead to non-uniform heating of the sample.

(9) How does the hardness of specimen tempered at 700oC compare with that of the furnace cooled
specimen? A Steel given such a tempering treatment is preferred to a furnace cooled specimen for
good machinability. Can you explain this on the basis of the difference in microstructure?
Ans :- During tempering of the steel at temperature of above 6500c the Sorbitic structure is formed which is fine
globular pearlite which results in a great combination of strength and toughness to the steel which leads to great
machinability of the steel whereas furnace cooling steel at such a high temperature will lead to temper
embrittlement as co-segregation takes place inside the steel microstructure this reduces the cohesion of grain
boundaries to cause intergranular fracture which causes brittleness.

(10) What is the significance of this experiment? How is it related to your course of study?
Ans:- In this experiment we learn how to perform conventional hardening and is one of the important heat
treatment techniques that is used to increase the hardness of steel that will be very useful as a metallurgist as we are
basically study metals and a technique which transforms the physical and mechanical properties of a metal is of
very much of our interest and so does spheroidized annealing as it is a process which increases the ductility of the
metal which is useful as to make metal parts more ductile and machinable to be used in our experiments and in so
many places.

24
 EXPERIMENT 4
HARDENABILITY: JOMINY END QUENCH TEST

OBJECTIVE

To study hardness and microstructure as a function as a function of quench rate, and investigate
the hardenability of steels by Jominy test.

EQUIPMENT / MATERIALS

Sample of medium or high carbon steel (the steel must have more than 0.35%C), or alloy steel,
Quenching tank, Electric furnace, Special tongs, Rockwell hardness tester, metallographic
polishing equipment, Metallurgical microscope.

THEORY

In a practical sense it is not possible to heat-treat all parts to the same degree. The difference is due
to the thickness or volume effect. Basically, when a part is quenched in water or some other fluid,
the heat must be conducted out through the surface. This leads to a temperature gradient dt/dx
between the surface and the center of the part being heat-treated. The temperature gradient varies
with time.
The temperature gradient is less steep between the center and the edge at later times. Therefore,
the temperature of the center lags in time behind the temperature of the surface. If we were to plot
a time profile of the center and the edge temperatures as shown in Figure 1, the time to reach a
given temperature T2 is definitely longer in the center than at the edge. This means that cooling
rate varies as a function of depth. The greater the depth the slower the cooling rate.
The situation with respect to the cooling rate can lead to a different hardness in the center than at
the edge. The edge could transform to martensite and the center to pearlite or bainite.

Figure 1: Cooling curves for the surface and center of a quenched specimen

In selecting a steel, the ability to cool the center depends upon the thickness of the part. The thicker
the part, the slower the cooling rate at the center. For a given thickness, one must select a steel that
can be hardened in the center if that is desired. The cooling rate in this case is fixed. The center
part of steel can be hardened by shifting the time-temperature transformation diagram through

25
alloying. Figure 2 shows that alloying elements added to plain carbon steel can shift the nose of
the TTT curve to longer times and raise the Ms temperature. This means a slower cooling rate can
be used to reach the martensitic state. A slower cooling rate means a thicker part can be heat-
treated.

Figure 2: TTT diagram for two different steels

To obtain standardized data on the hardness of steels as functions of cooling rates, the Jominy End
Quench test was developed. In the test, water is sprayed on one end of a bar of steel while it is hot.
This leads to a one dimensional heat transfer cooling. Except near the surface of the bar the
temperature is controlled by heat flow along the length of the bar (like thickness in the part).
Moving axially away from the quenched end of the bar, the temperature and the rate of change of
temperature are changing. The temperature is higher and the cooling rate is lower. If surface
hardness is measured as a function of distance from the end, a hardness profile can be obtained
which applies to any part made from the same steel, as shown in Figure 3.

26
 Figure 3: Quenched Tank and Hardness as a function of distance from quenched end for
two steels

PROCEDURE
In this test, a steel bar of 1 inch diameter and 4 inches long is heated to proper austenitizing temperature. After
being soaked for sufficient time, the specimen is quickly placed in a fixture. A water jet is opened quickly. Water
comes out at a constant pressure through an orifice of 1/2 inch diameter. The distance between orifice and the
bottom end of the steel bar is kept at 1/2 inch. The free jet height is 2.5 inches, and the temperature of water is kept
around 24°C. A stream of water strikes the lower end of the specimen. The end quenching is continued for about 20
minutes to cool the bar nearly to ambient temperature. The cooling rate is very rapid at the lower end and decreases
gradually with increase in distance from the lower end where complete martensitic formation occurs. After
quenching, two shallow flat surfaces of 0.02 inch deep are ground 180° apart on the test bar. The hardness is
determined at intervals of 1/16 inch along one end of the flat surface of the bar. Near the quenched end, this interval
is reduced to 1/32 inch as hardness impressions are smaller and hardness value may vary rapidly. Curves are then
plotted showing hardness against distance from the quenched end.

27
OBSERVATIONS

1. Measure hardness as a function of distance from the rapidly quenched end. Make a
hardness reading every 18 in. in the most rapidly quenched one inch, every 14 in

Distance Hardness Measurements Hardness

(inches) Trail 1 Trail 2 Trail 3 ( )

2. Draw the plot between distance vs. hardness of given sample

28
 Answer the Following Questions
(1) How do your hardness measurements correlate with your microstructural observations?
Ans :- Grain size is a contributing factor to hardness and hardenability. Micrographs can be taken and grain size
measured for another quantitative test. Hardness will tell us the size of the grain size in the sample and with the date
of size we can predict the phase of the metal present i.e maretensite or pearlite or ferrite.

(2) Give five applications for quench-hardened steels.

Ans :-
1. Machinery and in equipment where greater abrasion resistance is coupled with higher strength.
2. Low weight applications that require high carrying capacity as it has high yield strength.
3. This steel is also used in construction sites in dumping truck bodies, storage bins, and hoppers.
4. Consistent mechanical properties , therefore can be used for axle as well as moving parts of machinery.
5. Since it is less brittle, it can be used in impact machine as well.

(3) What will be the difference in hardness profile of a steel part quenched in water and in oil at the
same temperature?
Ans :- The faster the cooling rate the higher the hardness (in steels). Water-quenched steels will generally be harder
than oil-quenched steels. This is mainly because the thermal conductivity of water is higher than the thermal
conductivity of most oils ; consequently, the rates of cooling will be less rapid (or lower) in oils compared with
water.

29
(4) Steel gears are being quenched by dropping into a tank of room temperature oil. A competitor
makes gears of the same size and shape, apparently from the same raw material, but his gears last
longer than yours. What can you do to improve the quality of your productand cut down wear? What
is the danger in this course of action if you overdo it?
Ans :- Induction hardening is a heat treating technique that can be used to selectively harden portions of a
gear, such as the flanks, roots and tips of teeth, providing improved hardness, wear resistance, and contact
fatigue strength without affecting the metallurgy of the core and other parts of the component that don’t
require change.

(5) What is the ideal critical diameter and can it be determined with a Jominy test?
Ans :- The ideal size, or ideal diameter, of a steel can be defined as the size of bar hardened to 50% martensite in a
perfect quench medium. In this test, a steel bar of 1 inch diameter and 4 inches long is heated to proper austenitizing
temperature.

(6) How is the role of carbon and various alloy elements on the hardenability of steels?
Ans :- Increasing the carbon content tends to retard austenite transformation. This enables a slower quench for
reduced distortion while maintaining hardness. The as-quenched hardness of an alloy is only dependent on the
amount of carbon present. Additional alloying elements do not increase the achievable maximum as quenched
hardness of the steel. Alloying elements, such as nickel, chromium, and others, retard diffusion of carbon within the
steel. This diffusion of carbon is needed for the formation of pearlite. Martensite formation is promoted. Therefore,
alloying elements promote the formation of martensite and allow martensite formation at lower quenching rates.
This enables a part to be more deeply hardened.

30
(7) What effect does surface scale have on hardness measurements?
Ans :- Hardness testing is the surface quality on the test sample. This is where surface finish inspection star ts to
play a role. Contained within the literature of many hardness gages, a minimum surface finish requirement is
specified in order to assure proper hardness gage function. A surface finish of 80 microinches or better average
roughness (Ra) is often required to assure proper hardness measurements. Surface finish—also known as
profile—is composed of two elements: waviness and roughness. As the indenter is apt to be small compared to
the waviness component of the surface, it is the latter, short wavelength roughness pattern that influences
hardness values the most. However, when that surface is rough, a number of different forces come into play. If
the surface has a consistent pattern of roughness, then the indenter must work its way through a succession of
more or less evenly spaced peaks as its force is dissipated.

(8) You have three steels. Select the most appropriate steel to achieve the necessary levels of
mechanical properties, residual stress and distortion in a 1mm diameter wood-working drill.Why? 1%
C, 0.4% Si, 1% Mn, 5% Cr, 1% Mo and 0.4% C, 0.4% Mn, 0.3% Si, and 0.5% C, 4% Cr, 6% Mo.
Ans :- 1st type of steel should be used because for making drills, carbon percentage in steel should be in
between 0.7 to 1.5% (carbide formation would increase the hardness, red hardness and wear resistance)
whereas Chromium improves hardenability and prevents scaling, Molybdenum improves cutting efficiency
and hardness, as well as resistance to tempering, The use of silica fume increased both the mechanical
strength and the modulus of the elasticity of concrete and Manganese removes oxygen and sulfur
when iron ore (an iron and oxygen compound) is converted into iron. It also is an essential alloy that helps
convert iron into steel. As an alloy it decreases the brittleness of steel and imparts strength.

(9) As grain size increases, effect boron on hardenability decreases. Why?

Ans :- Boron is known to be an effective alloying element used to increase the hardenability. Generally speaking,
hardenability occurs because boron atoms easily segregate to prior austenite grain boundaries, lowering the grain
boundary energy while retarding the transformation of austenite to ferrite. But due to increase in grain size , number
of grain boundaries decreases and hence formation of pearlite increases and effect of boron of hardenability
decreases.

(10) What is the significance of this experiment? How is it related to your course of study?
Ans :- The Jominy end quench test is the standard method for measuring the hardenability of steels. This describes
the ability of the steel to be hardened in depth by quenching. The hardenability depends on the alloy composition of
the steel, and can also be affected by prior processing, such as the austenitisation temperature.

Knowledge of the hardenability of steels is necessary in order to select the appropriate combination of alloy and
heat treatment for components of different size, to minimise thermal stresses and distortion.

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 EXPERIMENT 5

CARBURIZATION OF STEEL

OBJECTIVE

Observe the carburized and decarburized layer (selective etching will be done due to gradual
carbon increment from surface to center.
To carburize the carbon steel and measure the diffusion coefficient

EQUIPMENT / MATERIALS

Samples of 0.2% Carbon steel alloy, 30-32% coke, 53-55% charcoal and 2-3% Na2Co3, Ba2Co3,
and 3-4% CaCo3, Stainless steel box, Electric furnace, SiC papers of various grit sizes, Polishing
machine, Metallurgical microscope, Rockwell hardness tester.

THEORY

Carburizing

If a steel is exposed to carbonaceous atmosphere (CO gas) at an elevated temperature, carbon

dissolves in the surface of the specimen building up the carbon concentrations at the surface and
diffuses inside under the influence of carbon concentration gradient (between the surface and
inside). Such a process is known as carburization. Here the following reaction takes place at the
surface.

If the carbon content of the carburizing atmosphere remains constant, it would give rise to a
constant carbon concentration Cs (Solubility limit of carbon in steel at the carburizing temperature)
at the surface of the steel. If we assume that the diffusion is unidirectional, the process of carbon
diffusion can be described by Fick’s second law,

Where D is the coefficient of diffusion of the diffusing element, dc/dt and dc/dx are concentration
gradients with time and distance, respectively. If D ≠ D(c)

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The solution to this equation is of the general form in case of the diffusion couple consisting of a
constant concentration on the surface (Cs i.e. for carburizing process) is given by

Where Cs is surface carbon concentration, C(x,t) is carbon concentration at depth “x” after time
“t”, C0 is initial carbon concentration of the given steel sample. Thus knowing C0 = 0.2, C(x,t) =
0.4, Cs = 0.8, erf (y) can be obtained by [y=x/2√Dt]. Hence knowing x & t from the experiment
D can be calculated.

0.2% Carbon steel is packed carburized in carburizing mixture (30-32% coke, 53-55% charcoal
and 2-3% Na2Co3, Ba2Co3, and 3-4% CaCo3) at 930oC for 4hrs, 6hrs, 8hrs, 10hrs, and 12hrs. For
this purpose, a stainless steel box is filled with the carburizing mixture and the samples are kept
inside the mixture. The box then is sealed with high temperature cement to prevent the exposure
of carburizing mixture and the samples to the atmosphere to prevent possible oxidation.

PROCEDURE

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 Answer the Following Questions
(1) Explain why the surface hardness of quenched high-carbon steel may be less than the
hardness under the surface.
Ans :- Carburizing is another form of case hardening that is widely used to improve the mechanical
properties of a steel substrate. During carburizing, a steel alloy is heated to an elevated temperature
and then is exposed to high amounts of carbon on its surface. The external carbon source can be a
gas, liquid, or solid depending on the application requirements. The high amounts of external
carbon will then form carbides with other elements on the surface of the steel. These carbides
provide increased hardness and wear resistance. Similar to nitriding, the heating requirements are
generally less, potentially resulting in less distortion.

(2) Cite three main reasons for surface hardening of steel.

Ans :-
1. To have hard surface but soft (tough) core in component like gears, shafts.
2. To overcome section size effects which make it difficult to get required surface hardness in large section by
quenching.
3. To get a favorable residue stress on the surface which would inhibits crack in it.

(3) Explain why core refining heat treatment may not be required for case carburized aluminium
killed steel.
Ans: Purpose of core refining treatment is to get fine austenite grain in case carburized steel. Aluminum killed steel
are resistant to austenitic grain growth. Aluminum reacts with dissolved oxygen to form oxide particles during
solidification. These are located along austenite grain boundaries and restrict their movements. In such steel grain
growth during carburization heat treatment may not be significant. This is why core refining treatment may not be
necessary.

(4) Can steel having 0.1% carbon be case carburized at 850⁰ C?

Ans :- It would carburize but the process would be too slow. At 850⁰C it will have ferrite austenite structure.
Solubility of carbon in ferrite is very small. Only the austenitic region will pick up carbon. The concentration
gradient for carbon to diffuse into austenite is also less. Since both temperature & concentration gradients are low
rate of carbon pick up will be extremely slow. Therefore, carburization at 850C is not recommended.

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(5) Show that the inter-lamellar spacing of pearlite is inversely proportional to the degree of under
cooling.

(6) List the factors that determine the strength of properly hardened steel.
Ans: A steel has maximum strength if has 100% martensite. This is obtained by quenching steel from austenitic
state. Strength of martensite depends primarily on its carbon content. However the cooling rate needed to get 100%
martensite in plain carbon steel is often difficult to achieve. Presence of additional alloy elements decreases critical
cooling rate. Alloy steels are easy to harden. Therefore strength of hardened steel would depend on its carbon
content, section size (thickness) and other alloy elements present & their amounts in the steel.

(7) Explain why thicker sections are more susceptible to cracking during hardening heat treatment.
Ans:- The difference in cooling rate between the centre and the surface is much more in a thicker section. As soon
as the temperature at the surface crosses Ms temperature, martensite forms accompanied by volume expansion. The
core is still soft austenite and can accommodate deformation if required. However later when its temperature goes
below Ms it would expand, when outer core which is already transformed is hard and cannot accommodate
deformation. A tensile stress therefore develops at the surface and it becomes prone to cracking. If thickness is less
the difference in temperature is not large. Transformation takes place almost simultaneously with little chance of
developing high tensile stress at the surface.

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(8) A hardened steel has become embrittled on tempering. Can this be de-embrittled?
Ans:- The difference in cooling rate between the centre and the surface is much more in a thicker section. As soon
as the temperature at the surface crosses Ms temperature, martensite forms accompanied by volume expansion. The
core is still soft austenite and can accommodate deformation if required. However later when its temperature goes
below Ms it would expand, when outer core which is already transformed is hard and cannot accommodate
deformation. A tensile stress therefore develops at the surface and it becomes prone to cracking. If thickness is less
the difference in temperature is not large. Transformation takes place almost simultaneously with little chance of
developing high tensile stress at the surface.

(9) Microstructure of isothermally transformed pearlite should have identical spacing in all colonies.
However often its microstructure often shows that lamellar spacing varies from colony to colony.
Why is it so?
Ans: Pealite is made of alternate layers of ferrite and cementite. Ferrite plates being 7 time wider than cementite.
Microstructure gives a sectional view. Colonies of Pearlite in a microstructure are randomly oriented. The plane of
microstructure may intersect these at different angles. Wherever the plane is perpendicular to ferrite / cementite
plates the spacing between two plates will be the minimum. Whereas those intersected at an angle will appear to
have larger spacing.

On plane B spacing would appear significantly larger. If transformation occurs at a fixed temperature the minimum
spacing is the correct estimate of lamellar distance.

(10) What is the significance of this experiment? How is it related to your course of study?
Ans :- A result of carburization which is taught in this experiment is an increase in hardness of the carburized
materials. Low alloy steels are often exposed to carbonaceous environments to produce hard surfaces to increase
wear resistance, corrosion resistance, and abrasion resistance. So, with the proper heat treatment in a gas
atmosphere, the consequence of carburization is beneficial. Carburization is also known as a corrosion process that
affects high temperature alloys.
Carburising is a thermochemical process in which carbon is diffused into the surface of low carbon steels to
increase the carbon content to sufficient levels so that the surface will respond to heat treatment and produce a hard,
wear-resistant layer. This process is widely used in the field of metallurgical engineering whenever steel is
produced. Production of high grade steel is the prime example of Carburising. There are three types of carburising
commonly used:

 gas carburising
 liquid carburising (or cyaniding)
 solid (pack) carburising

All three processes rely on the transformation of austenite into martensite on quenching. The increase in carbon
content at the surface must be high enough to give a martensitic layer with sufficient hardness, to provide a wear-
resistant surface.
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 EXPERIMENT 6

PRECIPITATION HARDENING

OBJECTIVE

To study the effect of precipitation hardening treatment on Al-4% Cu alloy on Isothermal ageing.

EQUIPMENT / MATERIALS

Samples of Al-4%Cu alloy, Electric furnace, SiC papers of various grit sizes, Polishing machine,
Metallurgical microscope, Rockwell hardness tester.

THEORY

Materials can be hardened by inhibiting the motion of crystal defects called dislocations. In pure
metals, the presence of defects (such as vacancies, interstitials, dislocations and grain boundaries)
can enhance the strength. In single phase alloys, additional resistance to deformation may arise
from the presence of foreign atoms. In two-phase alloys, additional stress is needed to enable the
dislocation to intersect the second-phase particles. A finely dispersed precipitate may, therefore,
strengthen the material. This phenomenon is termed precipitation hardening.

The thermodynamics of precipitation in 2014 Al can best be understood by referring to the binary
phase diagram of Aluminum-Copper in the aluminum-rich region in Figure 1.

Figure 1. Binary Phase Diagram for Al-Cu

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When the aluminum-copper alloy of less than 5 wt% copper is heated to a temperature just above
the solvus line, only one phase (alpha, α) is thermodynamically stable. Other solid phases dissolve
(disappear). This process is called solution treatment. The only requirement is that the specimen
must be kept at this temperature for a long enough time. To solution treat a sample of 2014 Al (4
wt% Cu), the sample should be heated to 9300F (5000C) and held for 30 minutes.

When a solution treated sample is rapidly cooled (quenched) to below the solvus line (Figure 1),
two phases are thermodynamically stable (alpha and theta). These phases are two different solids,
physically distinct, and separated by a phase boundary. The process is similar to precipitation of
salt in supersaturated brine.

The process of precipitation is not instantaneous, as is often the case in liquid-solid precipitation.
The process involves the formation of embryos of theta through thermal fluctuations and their
subsequent growth, once they achieve stability. With time, more and more precipitates form. This
process is called aging. Once the solution achieves an equilibrium composition given by the solvus
line for the aging temperature, precipitation stops. For example, the precipitation of the copper-
rich theta phase depletes the kappa phase of copper to approximately 1-1/2 wt% Cu at 715°F
(3800C).

The distribution of precipitates affects the hardness and yield strength. The hardness and yield
strength are greater when the precipitates are small and finely dispersed in the kappa matrix than
when the precipitates are large and not finely scattered. Therefore, to gain hardness in 2014 Al, the
specimen should be heat treated to produce a fine dispersion of small precipitates. Unfortunately,
there is a tendency when thermodynamic equilibrium is reached for large precipitates to grow and
small precipitates to shrink. This will lower the surface to volume ratio of the precipitates, the
surface energy, and therefore the energy of the system. As a result, at some point in the aging of
2014 Al, the precipitates begin to coarsen and (on average) the spacing between them gradually
increases. At this point, the hardness and the yield point will begin to decrease with time of aging.
The process of aging is a function of temperature; the higher the temperature, the wider the spacing
of the precipitates. They form initially on cooling from the solution treatment. Also, because
coarsening is dependent upon the movement of copper atoms in kappa, the maximum point is
generally reached sooner at a higher temperature than at a lower temperature, as shown in figure.

38
PROCEDURE

1. Stamp the five 2024 Al specimens with an identifying mark.

2. Measure the hardness of all of the specimens using Rockwell B.
3. Place all five in a heat-treatment crucible and into a furnace for solution treatment at 500°C (930°F) for 30
minutes.
4. Natural Aging - Remove one specimen and drop into a pail of water. Once the specimen is cool, measure
the Rockwell B hardness at intervals of approximately 30 min, 90 min, 1 day, and 1 week for this specimen.
It will be necessary for one member to come back to the lab during the week when the lab is in session to
measure the hardness.
5. Artificial Aging - Remove the remaining four specimens and drop them into a pail of water. Once the
specimens are cool remove them from the quenching bucket. Measure the Rockwell B hardness. Next
transfer the specimens to a furnace set at 190°C (370°F). Remove one sample after 3 min, 10 min, 60 min
and 90 min. Quench into water and measure the Rockwell B hardness. After one week, again measure the
Rockwell B hardness of the 3- and 10-minute artificially aged specimens.

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OBSERVATIONS

1. Record the date in following table

Solution treatment temperature:

Hardness of Quenched specimen:

Aging temperature:

Sl.No Ageing Time Hardness

2. Plot Hardness vs ageing time curve

40
 Answer the Following Questions
(1) Discuss the variation in hardness as a function of ageing time.
Ans:- In general, on aging, hardness first increases, attains a peak value and then decreases on further aging.
Subsequent aging further enhances the hardness and the aging curves again follow the same trend. Cold working
prior to aging reduces the time to reach the first hardness peaks.

(2) How will the peak hardness vary with ageing temperature?
Ans :- The peak-strength values of the alloy for the aging temperatures of (160, 180 and 190) °C were obtained
when the alloy was aged for (60, 10 and 5) h, respectively.

(3) How will the hardness vs ageing time curve shift for an alloy with 5 percent copper?
Ans :- The height of the initial peak varies directly as the square of the free-Copper concentration. So, during the
measurement of the peak on first cooling, the free copper concentration does not increase by more than 5 percent.

(4) Aluminum alloy rivets can be deformed easily when put in place but age-harden at room
temperature. How could one salvage a batch of rivets which had age-hardened before they had been
used?
Ans :- Once icebox rivet has been taken from the refrigerator, it should not be mixed with the rivets still in cold
storage. If more rivets are removed from the refrigerator than can be used in 15 minutes, they should be placed in a
separate container and stored for reheat treatment. Heat treatment of rivets may be repeated a number of times if
done properly.

(5) What methods other than hardness measurement could be used to study the precipitation
phenomenon? Discuss any of them.
Ans:- Strengthening Mechanism of the material can be used to study the precipitation phenomena. The
strengthening mechanisms give engineers the ability to tailor the mechanical properties of materials to suit a variety
of different applications. In most binary systems, alloying above a concentration given by the phase diagram will
cause the formation of a second phase. A second phase can also be created by mechanical or thermal treatments.
The particles that compose the second phase precipitates act as pinning points in a similar manner to solutes, though
the particles are not necessarily single atoms.

41
(6) What are the stages of precipitate formation in precipitation strengthened alloys?
Ans :-
1) Solution Treatment, or Solutionizing, is the first step in the precipitation-hardening process where the alloy is
heated above the solvus temperature and soaked there until a homogeneous solid solution (α) is produced. The θ
precipitates are dissolved in this step and any segregation present in the original alloy is reduced.

2) Quenching is the second step where the solid α is rapidly cooled forming a supersaturated solid solution of
αSS which contains excess copper and is not an equilibrium structure. The atoms do not have time to diffuse to
potential nucleation sites and thus θ precipitates do not form.

3) Aging is the third step where the supersaturated α, αSS, is heated below the solvus temperature to produce a
finely dispersed precipitate. Atoms diffuse only short distances at this aging temperature. Because the
supersaturated α is not stable, the extra copper atoms diffuse to numerous nucleation sites and precipitates grow.
The formation of a finely dispersed precipitate in the alloy is the objective of the precipitation-hardening
process. The fine precipitates in the alloy impede dislocation movement by forcing the dislocations to either cut
through the precipitated particles or go around them. By restricting dislocation movement during deformation,
the alloy is strengthened.

(7) What is the essential condition for age hardening?

Ans :- The metals and alloys need to be maintained at high temperatures for many hours for the precipitation to
occur; hence this process is called age hardening.

(8) What is the structural difference between GP zones and θ?

Ans :- The GP zones are (typically) about 10 nm in diameter, 2 atomic layers thick and are typically separated by
about 10 nm. The θ is tetragonal; it is a distorted fcc structure with alternating copper and aluminium atoms on the
(001) planes. It has a small misfit along the c direction which is accomodated by elastic strain. GP zones are formed
in a disk- or plate-shaped morphology on {100} matrix planes with typically single Cu-rich layer zones (GP(1)
zone) and two or more than two Cu-rich layers separated by three Al layers (GP(2) zone).

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(9) What’s the difference between a Coherent and a Non-Coherent Precipitate?
Ans :- Incoherent precipitates are truly distinct second-phase particles with their own crystal structure and separated
from the surrounding matrix by a well-defined interface. Incoherent precipitates are effective obstacles against
dislocation slip because the large distortion of the matrix surrounding the particles interacts strongly with the stress
field of the dislocations.

In coherent precipitates in a matrix, if the precipitate has a lattice parameter less than that of the matrix, then the
atomic match across the IPB leads to an internal stress field that interacts with moving dislocations.

(10) What is the significance of this experiment? How is it related to your course of study?
Ans :- This experiment helped in the study of the effect of precipitation hardening treatment on Al-4% Cu alloy on
Isothermal ageing. It also aimed to understand the variation in hardness as a function of ageing time, difference
between Coherent and a Non-Coherent Precipitate and variation of peak hardness with temperature. This helped us
to understand the stages of precipitate formation in precipitation strengthened alloys, the structural difference
between GP zones and θ and essential condition for age hardening.

43