Annealing, normalizing and hardening, treatments of plain carbon steel

Aim:
Study the effect of Annealing Normalizing & hardening treatment of low carbon steel and
identify the different phases.

Equipment and Materials:

Muffle Furnace
Plain Carbon steels
Laboratory equipment such as tongs, gloves, Anvile, Hax-saw or cutting machine,
refractories
Rockwell/Vickers Hardness Tester.
Optical Microscopy

Theory:
Heat treatment is a process of heating the metal below its melting point and holding it at
that temperature for sufficient time and cooling at the desired rate to obtain the required
properties. The various heat treatment processes are annealing, normalizing, tempering,
hardening, mar tempering, austempering.
.
The final mechanical properties depend on the microstructure formed due to various heat
treatment processes (due to various cooling rates). An annealed specimen was cooled in the
furnace or any good heat insulating material; it obtains the coarse grain structure of ferrite
and pearlite in case of hypo eutectoid steels and coarse grain structure of ferrite and
cementite in case of hyper eutectoid steel. It possesses high ductility.

Annealing:
Annealing in general, involves heating the steel specimens to sufficient high
temperatures (Above A3-upper critical line for hypoeutectoid steel and above A1-
lower critical line for hypereutectoid steels). Holding at this temperature for
homogenisation & finally cooling at a very slow cooling rate (furnace cooling). The
temperature to which steel is heating & holding time are determined by various
factors such as the chemical composition of the steel, size & shape of steel component
& final properties desired. Microstructural change in the specimen during annealing
are as follows, on heating, when the temp of the specimen reaches 30 - 50oC above
the critical temperature and soaking it for definite period of time all pearlite
transforms into fine austenite, subsequent cooling in the furnace will result in small
areas of fine Pearlite surrounded by pro – eutectoid ferrite

Annealing process refines grain structure, induces softness, and improves electrical and
magnetic properties. Annealing can form either the final treatment or a preparatory step for
further treatment.

Temperature of annealing For hypo-eutectoid and eutectoid steel: Ac3 +50°C

Temperature of annealing For hyper-eutectoid steels: Ac1 + 50°C

The various purposes of this treatment are

 To relive internal stresses developed during solidification, machining, forging,
rolling or welding etc.
 To improve or restore ductility or toughness
 To enhance machinability.
 To eliminate chemical non-uniformity.
 To refine grain size
 To reduce gaseous content in steel.

Types of Annealing
 Full Annealing
 Isothermal Annealing
 Diffusion Annealing
 Partial Annealing
 Re crystallization Annealing

Normalizing:
It is the process of heating steel to about 400- 500C above upper critical temperature (A3)
holding for proper time & then cooling it in air or slightly agitated air to room temperature.
After normalizing the resultant microstructure should be ferrite and pearlitic for low carbon
steels. This is particularly important for some alloy steels which are air hardened by nature
for such steels, cooling in air don’t lead to normalized structure. Slower cooling rates are
read since the temperature involved in this process is more than that for normalizing, the
homogeneity as austenitic increases & it results in better dispersion. Results in enhanced
mechanical properties. The grain size in finer in normalized structure that in annealing grain
size of normalized steel is governed by section thickness. As cooling rates differ
considerably from case to case, there is variation in grain size of normalizing steel over its
cross section. Refinement of grain size is on of the most important objectives of
normalizing & it is to be a great extent due to high temperature involved in these operation
are subjected to a great extent .
Normalizing treatment is frequently applied to steel in order to grain refinement,
improvement in mach inability & enhanced mechanical properties such as hardness,
strength & toughness.

Aims of normalizing:
 To refine the coarse grains of steel casting.
 To increase machinability of low carbon steel.
 To improve the mechanical properties of plain carbon steel.

Temperature of normalizing For hypo- eutectoid steels: Ac3 + 50°C

Temperature of normalizing For hyper-eutectic and eutectoid steel: Ac1 +50°C
Hardening
Hardening is the one of the heat treatment Technique which involves heating the steel to
30 -500C above upper critical temperature (Ac3) for hypo-eutectoid steels and by the same
temperature above the lower critical temperature for hyper-eutectoid steels, austenizing for
a sufficient time and cooling with a rate just exceeding the critical cooling rate of that steel
to room temperature or below room temperature .Due to this, the usual diffusion
transformations are stopped and the austenite by a diffusion less process transforms to
martensite. The purposes of hardening are to increase the hardness of the metal and to make
suitable cutting tools.

Microstructural change in the specimen during quench hardening are as follows, on

heating, the specimen to austenizing temperature then soaking at this temperature (for
rapid diffusion of carbon) results in austenic grains of uniform composition cooling the
specimen in circulated water (i.e. providing cooling rate greater than critical cooling
rate), oil or brine solution result in hard martensite grains. The martensite has body
cantered tetragonal (BCT) crystal structure.

Aims of hardening:

 Main aim of hardening is to induce high hardness.

 Many machine parts are hardened to induce high wear resistance.
 To develop high yield strength with good toughness and ductility

Temperature of hardening: For hypo- eutectoid steels: Ac3 +50°C

Temperature of hardening: For hyper-eutectic and eutectoid steel: Ac1 +500C

Different Heat treatment Process:

Annealing:

 The specimen was heated to a temperature of AC3+500C (9300C)

 At 9000C the specimen was held for 1 hour
 Then the furnace was switched off so that the specimen temperature will decrease
with the same rate as that of the furnace

The objective of keeping the specimen at 9000C for 1 hrs is to homogenize the specimen.
The temperature 9000C lies above upper critical temperature. So that the specimen at that
temperature gets sufficient time to homogenized. The specimen was taken out of the
furnace after 1 days when the furnace temperature had already reached the room
temperature
Normalizing:

 At the very beginning the specimen was heated to the temperature of AC3+500C
(9300C)
 There the specimen was kept for 1 hour.
 Then the furnace was switched off and the specimen was taken out.
 Now the specimen is allowed to cool in the ordinary environment (air). i.e. the
specimen is air cooled to room temperature. The process of air cooling of specimen
heated above upper critical (Ac3) is called normalizing.

Quenching:

This experiment was performed to harden the plain carbon steel. The process involved
putting the red hot steel directly in to a liquid medium.

 The specimen was heated to the temp of around 9000C and were allowed to
homogenize at that temp for 1 hour (depend on the sample size).
 An water bath was maintained at a constant temperature in which the specimen had
to be put.
 After 2 hour the specimen was taken out of the furnace and directly quenched in the
water bath.
 After around half an hour the specimen was taken out of the bath and cleaned
properly.
 Now the specimen attains the liquid bath temp within few minutes. But the rate of
cooling is very fast because the liquid doesn’t release heat readily.

Sample Preparation for microstructure observation:

 The specimen being small, is mounted on bakelite using mounting press.

 The mounted specimen surface is ground until unevenness of surface is
eliminated using Belt Grinder.
 After the specimen surface is leveled it is polished on a successively fine
grades of emery papers (400, 600, and finally on 800 grit).
 Fine Polishing is done on a disc Polisher (Rotating Polishing Wheel), the
wheel is fitted with a Polishing cloth and suspension of fine alumina powder in
water used as a polishing medium.
 A Scratch free surface is obtained after fine polishing for sufficient period (15
minutes)
 After fine polishing specimen is thoroughly washed with water and dried.
 The specimen is Etched for specified time using a suitable etchant (2 % Nital 2 %
HNO3 and 98 % Ethyl or Methyl Alcohol) to preferentially reveals the
microstructure. An optical microscope is used to observe the microstructure under
100X to 500X magnification as required.
Hardness Measurement:

The heat treated specimens hardness were measured by means of Rockwell/Vickers

hardness tester. The procedure adopted can be listed as follows:

 First the indenter was inserted in the machine; the load is adjusted to10kg.
 The minor load of a 10 kg was first applied to seat of the specimen.
 Now the major load applied and the depth of indentation is automatically recorded
on a dial gage in terms of arbitrary hardness numbers. The dial contains 100
divisions. Each division corresponds to a penetration of .002 mm. The dial is
reversed so that a high hardness, which results in small penetration, results in a high
hardness number. The hardness value thus obtained was converted into C scale b y
using the standard converter chart.

Precautions:

 Grinding should be done on the emery papers only in one direction.

 While polishing the specimen uniform pressure should be exerted on the
specimen.
 While going to the next grade of emery papers, the specimen has to be
rotated through 900.
 While switching over to new emery paper, specimen should be thoroughly
washed with water to remove all loose particles.
 After etching the specimen should be washed away with in a few seconds.
 Operate the Microscope Knobs gently (without jerks)

Observation:
 Study the microstructure of plain carbon steels at different
cooling rate

Aim:
To find the microstructure of hardened steels with varying cooling rate

Equipment & Materials:

Muffle furnace
Different liquid bath
Rockwell testing machine
Plain carbon steel (0.4%C Steel)

Procedure:
This experiment was performed to harden the plain carbon steels in different quenching
medium. The process involved quenching the red hot steels directly in to a liquid medium.

 The specimen is heated to the temp of around 9000 and were allowed to homogenize
at that temp for 1 hour.
 After 1 hour the specimen was taken out from the furnace and directly quenched in
the water, brine solution and oil bath.
 After around half an hour the specimen was taken out of the bath and cleaned
properly.
 Now the specimen attains the liquid bath temp within few minutes. But the rate of
cooling is very fast because the liquid doesn’t release heat readily. The samples are
quenched in different liquid bath to maintain the different cooling rate.
.
Sample Preparation for microstructure observation:

 The specimen being small, is mounted on bakelite using mounting press.

 The mounted specimen surface is ground until unevenness of surface is
eliminated using Belt Grinder.
 After the specimen surface is leveled it is polished on a successively fine
grades of emery papers (400, 600, and finally on 800 grit).
 Fine Polishing is done on a disc Polisher (Rotating Polishing Wheel), the
wheel is fitted with a Polishing cloth and suspension of fine alumina powder in
water used as a polishing medium.
 A Scratch free surface is obtained after fine polishing for sufficient period (15
minutes)
 After fine polishing specimen is thoroughly washed with water and dried.
 The specimen is Etched for specified time using a suitable etchant (2 % Nital 2 %
HNO3 and 98 % Ethyl or Methyl Alcohol) to preferentially reveals the
 microstructure. An optical microscope is used to observe the microstructure under
100X and 500X magnification as required.

Hardness Measurement:

The hardness of hardened specimens are measured by using Rockwell or Vicker's hardness
tester. The procedure adopted can be listed earlier:

Observation:
 Tempering Treatment with Varying Temperature and Time
Aim:
To perform the tempering treatment on the given material C-40 steel, with varying
temperature and time to optimise the mechanical properties of the steels.

Apparatus required:
 Muffle furnace: tongs
 Given material: 0.4%C steel
 Quenching medium: water,
 Rockwell test setup

Tempering:

Quenching makes austenite to transform to martensite. Martensite is a hard and brittle.

Quenching stresses may cause cracks even later on when in use. We know that martensite is
a supersaturated solid solution of carbon in iron (BCT), it rejects on heating, carbon on the
form of fine carbide and these takes place some of decrease of hardness with increase with
ductility i.e. the properties of martensite can be modified. It is necessary, therefore, to warm
the steel below the critical range in order to relieve stresses and to allow the arrested
reaction of cementite precipitation to take place. This is known as tempering.

This process consists of reheating the hardened steel to some temperature below the lower
critical temperature such as 2000C or 6000C, followed by any desired rate of cooling. The
purpose is to relive internal stress, to reduce brittleness and to make steel tough to resist
shock and fatigue.

Aim of Tempering:

 To relieve quenching stresses developed during hardening.

 To restore ductility and toughness with decrease in hardness and strength.
 To improve magnetic properties

Stages of Tempering:

 150-250°C. The object is heated in an oil bath, immediately after quenching, to prevent
related cracking, to relieve internal stress and to decompose austenite without much
softening.

 200-450°C. Used to toughen the steel at the expense of hardness. Brinell hardness is 350-
450.

 450-700°C. The precipitated cementite coalesces into larger masses and the steel becomes
softer. The structure is known as sorbite, which at the higher temperatures becomes coarsely
spheroidised. Sorbite is commonly found in heat-treated constructional steels, such as axles,
shafts and crankshafts subjected to dynamic stresses.
 Procedure:
Quenching:
It is an operation of rapid cooling by immersing a hot piece into a quenching bath
(water).
 The specimen is placed inside the heating chamber of muffle furnace and is heated
upto 9000C
 Then the specimen is soaked for 1 hr at the same temperature 900˚C.
 After soaking it is taken out from the furnace and it is quenched in the water, brine
water and Oil bath.
 Again the specimen is subjected to Rockwell hardness test and Rockwell
hardness number is measured.
 Followed by tempering treatment

Tempering:
It is defined as the process of reheating the hardened specimen to some temperature
below lower critical time with varying holding time to transform martensile to a
softer phase and relieve the internal stresses.

This is the one of the important experiment carried out with the objectiv to relief internal
stress and optimise the mechanical properties with varying tempering temperature and time

 First the ‘6’ specimen were heated to 9000C for 1 hour and then quenched in the
water bath maintained at room temp.
 Among the 6 specimen 2 were heated at 2000C for different time period of 1 hour
and 2 hour respectively.
 Now another 2 more specimens are heated at 4500C for the time period of 1 hour 2
hour respectively.
 The remaining specimens are heated to 6500C for same time interval of 1 hour. 2
hour respectively. After the specimens got heated to a particular temperature for a
particular time period, they are air cooled. The heat treatment of tempering at
different temp for different time periods develops variety of properties within them.

Observation:
 Jominy End Quench Test
Aim:
 How to harden the steel alloy by carrying out the Jominy End Quench Test.
 To evaluate the hardenability of the low carbon steel or medium carbon steel by
Jominy end quench test Method.
 Effect of alloying element on the microstructure
 Phase transformation of steel

Theory:
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. Knowledge about
the hardenability of steels is necessary to select the appropriate combination of alloy steel and
heat treatment to minimize thermal stresses and distortion in manufacturing components of
different sizes. Hardenability depends on the chemical composition of the steel and also be
can affected by prior processing conditions, such as the austenitizing temperature. It is not
only necessary to understand the basic information provided from the test, but also to
understand how the information obtained from the Jominy test can be used to understand the
effects of alloying in steels and the steel microstructure. Hardening of steels can be
understood by considering that on cooling from high temperature, the austenite phase of the
steel can transform to either martensite or a mixture of ferrite and pearlite. The ferrite/pearlite
reaction involves diffusion, which takes time. However, the martensite transformation does
not involve diffusion and essentially is instantaneous. These two reactions are competitive,
and martensite is obtained if the cooling rate is fast enough to avoid the slower formation of
ferrite and pearlite. In alloyed steels, the ferrite/ pearlite reaction is further slowed down,
which allows martensite to be obtained using slower cooling rates. Transformation to another
possible phase (bainite) can be understood in a similar way. Steels having high hardenability
are required to make large high-strength components, such as large extruder screws for
injection molding of polymers, pistons for rock breakers, mine-shaft supports, aircraft
undercarriages, as well as for small, high precision components, such as die-casting molds,
drills and presses for stamping coins. Steels having low hardenability may be used for smaller
components, such as chisels and shears, or for surface-hardened components, such as gears,
where there is a desire to maintain a ferrite/pearlite microstructure at the core to improve
toughness. The Jominy end-quench test is the standard method to measure the hardenability
of steels.
High hardness occurs where high volume fractions of martensite develop. Lower hardness
indicates transformation to bainite or ferrite/pearlite microstructures. Microstructures
observed in the Jominy end-quench test of a 0.4wt% carbon steel: (a) untempered martensite;
(b) ferrite and pearlite. Pearlite, the darker constituent, is a eutectoid mixture of ferrite and
iron carbide. Effects of alloying and microstucture

Apparatus:
 Heat treatment furnace
 Jominy end quench apparatus,
 Test specimen,
 Rockwell test setup

Specimen: Medium carbon (0.4%C ) steel.

Procedure:
Take the specimen, place it in the furnace and supply the power. Wait till the temperature
reaches to the austenising temperature. Heat the specimen at the austenising temperature
9000C for 2 hrs) until it is completely transformed in to Austenite. Remove the specimen
from the furnace with the help of tongs and gloves and place it in the Jomny end quench
apparatus and allow the jet of water to strike one end of the specimen.

When the specimen reaches to the room temperature remove it from the apparatus and find
the Rockwell hardness at 0.5cms along the length of the specimen. Plot the graph between the
hardness and distance from the quenched end.

Observation:
 Carburization Treatment

Carburization is a technique used to harden the surface of steels by diffusing of carbon atoms
into the crystal lattice. The carbon enters the interstitial spaces between the iron atoms. It
strengthens the metal by distorting the crystal lattice, thus making it difficult for dislocations
to move. Carburization is a surface hardening technique because, even at high temperatures,
diffusion is a slow process. The source of carbon can either be a gas or solid carbon. The
purposes of hardening are to increase the hardness of the metal and to make suitable cutting
tools.

Aim/Objectives
The practical aims to familiarize you with a solution of Fick's Second Law of diffusion by
studying the diffusion of carbon into iron. You will gain experience of heat treatment in
furnaces, preparation of metallographic sections and etching, The microscopy will require
interpretation of more complicated microstructures.

Carburizing:-
Carburizing is a process of adding carbon to surface. This is done by exposing the part to
carbon rich atmosphere at the elevated temp (nearly melting point) and allows diffusion to
transfer the carbon atoms in the steel. This diffusion work on the principle of differential
concentration.

2CO ↔C (in Fe) +CO2

CO+H2 ↔C (in Fe) +H2O

Types of carburizing process:-

 Gas carburizing
 Liquid carburizing
 Vacuum carburizing
 Plasma(ion) carburizing
 Salt bath carburizing
 Pack carburizing

Pack carburizing:
In this process, the part that is to be carburized is packed in a steel container, so that it is
completely surrounded by granules of charcoal. The charcoal is treated with an alternating
chemical such as barium carbonate (BaCO3) that promotes the formation of carbon dioxide
(CO2). This gas in turns reacts with the excess carbon in the charcoal to produce carbon
monoxide (CO) .carbon monoxide reacts with low carbon steel surface to form atomic carbon
which diffuses into the steel. Carbon monoxide supplies the carbon gradient that is necessary
for diffusion. The car bruising process does not harden the steel. It only increases the carbon
content to some predetermined depth below the surface to a sufficient level to allow
subsequent quench hardening.

CO2+C → 2CO
↓
2CO+3Fe → Fe3C+CO2
The oxygen of the entrapped air (in the carburizing box) initially reacts with the carbon of the
carburizing medium as follows:

C+O2 → CO2………… (1)

2C+O2 → 2CO………... (2)

As the temperature rises the following reactions take place and the equilibrium shifts towards
right that is gas becomes progressively richer in CO. at high temperature (> 800°c) the
boudoirs reaction occurs as follows

CO2+C ↔ 2CO ……… (3)

At the steel surface the decomposition of CO gas occurs as follows:

2C+O2 → CO2+C (atomic)

Fe+C (atomic) → Fe(C)

Where Fe(C) is carbon dissolved in austenite. This atomic and nascent carbon is radially
absorbed by the steel surface, and subsequently it diffuses towards the centre of steel sample.
CO2 thus formed react with the carbon (C) of the carburizing medium (reaction 3) to produce
CO, and thus, the cycle of the reaction continues. Charcoal is the basic source of carbon
during pack carburization. As entrapped air inside the box may be less to produce enough
CO2 (reaction 1) particularly in the beginning of the carburization, it is thus it is common
practice to add energizer (usually BaCO3) which decomposes during the heating up period as:

BaCO3 → BaO+CO2
CO2+C → 2CO

The CO2 thus formed then react with the carbon of the carburizer to produce CO gas. Thus
BaCO3 makes CO2 available at an early stage of carburization and hence it is called
energizer.

The case depth increases with rise in carburization temperature and time. The best
carburizing temperature is 900°C, the steel surface absorbs carbon at a faster rate and the rate
at which it can diffuse inside, thus producing super saturated case which may produce cracks
during quenching. In pack carburization it is difficult to control exactly the case depth
because of many factors affecting it, such as density of packing amount of air present inside
the box, reactivity of carburizer, etc….

Advantages of Pack Carburizing:

1) It is a cheap and simple method if only few parts are to be carburized.
2) Very large and massive parts which are too large for gas or salt carburization can be
carburized if a furnace of that size is available. Pack carburization can be done in large
variety of furnaces if these are having uniformity of the temperature.
3) In comparison to liquid and gas carburization, this method carburization involves less
capital investment.
4) No atmosphere-controlled furnace is required.
5) No poisonous cyanide or gas is used in this process.
6) It can be done any workshop.
Disadvantages of Pack Carburizing:
1) Carburizing time is very long, as carburizing boxes as well as bad heat conducting
carburizing materials need to be heated.
2) It is difficult to control the surface carbon and the carbon gradient.
3) It is difficult to control the case depth exactly.
4) Handling carburizing material and packing is dirty and dusty job.
5) In pack carburization it is difficult to quench the carburized parts.

Procedure
Two low carbon steels are taken for pack carburising experiment. One will be as blank (for
comparison) and the other is required for carburizing at 950ºC. Heat the samples in a muffel
furnace at 950oC for one hour. At the end turn off the furnace and let the samples cool in air
to room temperature. This process is caused normalization, and can be done several days or
weeks before the experiment; however the sample should be at room temperature for at least
24 hours before proceeding to the next step. To carburize the sample. Clean the surface of the
specimen by polishing using emery paper up to grade 800. The samples is packed in a steel
made box with a mixture of charcoal powder and barium carbonate activator (20 % max).
The carbonate releases carbon dioxide that reacts with C (charcoal) to give carbon monoxide
and form a carburizing gas. A lid is needed to exclude air. Place your crucible in the furnace
at 900°C for 4-6 hours. Remove from the furnace and quench the sample (hot) in water.
Perform a Vickers hardness test, and examine the surface under the optical microscopy.
Compare the data before and after carburizing and describe the microstructure. Note: after
carburizing the sample need to be polished; in particular it is important that the rusted (oxide)
surface is removed to expose a bulk cross-section. After grinding and polishing, the
specimens need to be etched, in 2% Nital. Check that the etch time is sufficient to show the
structure clearly across the whole carbon profile.

Safety
Care is needed in handling hot materials; use proper tongs, wear suitable protection (gloves
and visor) and don't leave hot materials on the bench without a notice that they are hot.
Normal safety precautions are adequate for etches used here, i.e. lab coat, gloves and eye
protection.

Observation: