EXPERIMENT 1

Introduction of Metallographic Specimen Preparation

Objective:

1. Metallographic Sample Preparation.

2. To study the importance of the various steps in sample preparation.
3. To understand the need of mounting, polishing and etching.

Introduction:

Metallography is the study of the microstructure of metals and alloys by means of microscopy.
It is an art and science of preparing, interpreting, and analyzing microstructures in materials,
to better understand materials behavior and performance. The method is used for the
evaluation of metallic materials in the various industries, including the aerospace industry,
the automotive industry and parts of the construction industry. It is also used for process
control including the examination of defects that appear in finished or partly finished
products, as well as the studies of parts that have failed during service. It is an important
branch of the Metallurgical Engineering.

A well prepared metallographic specimen is:

a. A representative sample
b. Sectioned, ground and polished so as to minimize disturbed or flowed surface metal
caused by mechanical deformation, and thus to allow the true microstructure to be
revealed by etching.
c. Free from polishing scratches and pits and liquid staining
d. Flat enough to permit examination by optical microscope or SEM

Various steps involved in the specimen preparation, and the significance of each step:

Many steps in the preparation of metallographic specimens described here are also applicable
in other types of metallographic studies, such as electron microscopy, micro hardness testing,
quantitative measurement of constituents of structures, and electron microprobe analysis.
Preparation of metallographic specimens generally requires five major operations:

a. Sectioning
b. Mounting (which is necessary when the sample cannot be held properly due to its
shape and/or size, while polishing)
c. Grinding
d. Polishing
e. Etching

These operations are listed below in the order they are performed

▪ Sectioning

Separate test pieces or coupons attached to castings or forgings should be designed so that a
minimum of sectioning is required for producing metallographic specimens. Sectioning

4
 becomes necessary when studying parts that have failed in service where specimen has to be
taken from a large block of material. Therefore, metallographic studies of such samples
often involve more than one sectioning operation.

Many metallographic studies require more than one specimen. For example, a study of
deformation in wrought metals usually requires two sections- one perpendicular to, and the
other parallel to, the major axis of the direction of deformation. Failed parts may best be
studied by selecting a specimen that intersects the origin of the failure, if the origin can be
identified on the surface. Depending on the type of failure, it may be necessary to take
several specimens from the area of failure and from adjacent areas.

▪ Mounting of Specimens

The primary purpose of mounting is to make it convincement to handle specimens of arbitrary

shape and/or small sizes during various steps of metallographic sample preparation and
examination. A secondary purpose is to protect and preserve extreme edges or surface
defects during metallographic preparation. Specimens may also require mounting to
accommodate various types of automatic devices used in metallographic laboratories or to
facilitate placement on the microscope stage. An additional benefit of mounting is the
identification of the sample (name, alloy number or laboratory code number) without
damaging the specimen.

Compression mounting: It is most common mounting method, which involves molding

around the metallographic specimen by heat and pressure using the molding materials such
as Bakelite, Diallyl Phthalate resins, and acrylic resins. Bakelite and Diallyl phthalate are
thermosetting, and acrylic resins are thermoplastic.

Not all materials or specimens can be mounted in thermosetting or thermoplastic mounting.

The heating cycle may cause changes in the microstructure, or the pressure may cause
delicate specimens to collapse or deform. The size of the selected specimen may be too large
to be accepted by the available mold sizes. These difficulties are usually overcome by cold
mounting.

Cold Mounting requires no pressure and little heat, and is a mean of mounting large
numbers of specimens more rapidly than possible by compression mounting. Epoxy resins
are most widely used cold mounting materials. They are hard, and adhere tenaciously to
most metallurgical, mineral and ceramic specimens.

▪ Grinding

Grinding is a most important operation in specimen preparation. During grinding, the operator
has the opportunity of minimizing mechanical surface damage, that can be removed by
subsequent polishing operations. Even if sectioning is done in a careless manner resulting into
a severely damaged surface, the damage can be eliminated by prolonged grinding. However,
prolonged grinding should be avoided since it might lead to excess heating or surface damage.

5
Grinding is accomplished by abrading the specimen surface through a sequence of operations
using progressively finer abrasive grits. Grit sizes ranging from 6 0 mesh to 150 mesh are
usually regarded as coarse abrasives, and grit sizes r a n g i n g f r o m 1 8 0 mesh to 600
mesh as fine abrasives. Grinding should commence with the coarse grit size for making
initial flat surface and remove the effects of sectioning. Hack-sawed, band-sawed, or other
rough surfaces usually require abrasive grit sizes in the range of 80 to 150 mesh. Grinding
should be done sequentially starting from the coarser one to finer one. A satisfactory
grinding sequence might involve grit sizes of 180, 240, 400 and 600 mesh. The purpose of
grinding is to remove the oxide layer or damaged layer or uneven surfaces that might have
formed during last sectioning operation. However, the depth of cold worked metal is roughly
inversely proportional to the hardness of the specimen and may be 10 to 50 times the depth
of penetration of the abrasive particle.

To ensure the complete elimination of the previous grinding scratches found by visual
inspection, the direction of grinding must be changed by 90o from the one stage of grinding
to the next stage. In addition, microscopic examination of the various ground surfaces during
the grinding sequence may be worthwhile in evaluating the effect of grinding. Each ground
surface should have scratches that are clean-cut and uniform in size, with no evidence of
previous grinding scratches. Cleaning before going to next stage grinding is always helpful.

Grinding Mediums

Grinding media are silicon carbide (SiC), aluminium oxide (Al2O3), emery (Al2O3-Fe3O4),
and diamond particles. All except diamond are generally bonded to paper or cloth backing
material of various weights in the form of sheets, disks, and belts of various sizes. The
abrasives may be used also in t h e powder form by charging the grinding surfaces with
loose abrasive particles.

Automatic grinding, as the name implies, is done without hand assistance. All automatic
grinding devices use lap surfaces on which paper-based disks are placed or abrasive
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 powder is charged. The lap is either a rotating or a vibrating disk, where the use of the
latter is described as vibratory grinding.

▪ Polishing

Polishing is the final step in producing a surface that is flat, scratch free, and mirror-like in
appearance. Such surface is necessary for subsequent accurate metallographic
interpretation, both the qualitative and quantitative. The polishing technique used should
not introduce extraneous structure, such as disturbed metal, pitting, dragging out of
inclusions, and staining.

Mechanical Polishing

Mechanical polishing is frequently used to describe the various final polishing procedures
involving the use of cloth-covered laps and suitable polishing abrasives basically Al2O3
slurry. The laps have either a rotating or a vibrating motion, and the specimens are held
by hand, held mechanically, or merely confined within the polishing area. Polishing should
be done in a relatively dust-free area, preferably removed from the area for sectioning,
mounting and rough grinding. Any contamination of a polishing lap by abrasive particles
carried over from preceding operations or by dust, dirt or other foreign matter in the air
cannot be tolerated. Carryover as a result of improper cleaning between final polishing steps
is another prime source of contamination. It is just as important for the operator to wash
his/her hands meticulously as it is for him/her to remove all traces of polishing abrasive from
the specimen before proceeding to the next finer polishing operation.

Electrolytic Polishing

Even with the most careful mechanical polishing, some disturbed metal, even very small
the amount, will remain after preparation of a metallographic specimen. This is no problem if
the specimen is to be etched for structural investigation because etching is usually sufficient
to remove the slight layer of disturbed metal. However, if the specimen is to be examined
in the as polished condition, or if no surface disturbance can be tolerated, then either
electrolytic polishing or chemical polishing is preferred. The basic principle involved in this
technique is anodic dissolution of surface of the sample which results in a leveling and
brightening of its surface.

Electro polishing does not disturb any metal on the specimen surface, and therefore, ideally
suited for the metallographic preparation of soft metals, most single phase alloys, and alloys
that works harden readily. The disadvantages of electro polishing include preferential attack
in multiphase alloys caused by differences in electrical potential between phases. Proper
choice of electrolyte and operating conditions will minimize these disadvantages.

▪ Etching

Metallographic etching is used to reveal particular structural characteristics of a metal. This

is essential since these structural characteristics are not visible in the as polished mirror like
surface in the metal. It can be used for phase identification, for dislocation density
calculation (etch pitting), and for orientation studies. The principle of etching multiphase
alloys is based on the preferential attack (different rates of electrochemical dissolution of

7
phases in the etchant) or preferential staining of one or more phases, because of differences
in chemical composition and, because of differences in grain-orientation. Before being
etched, a specimen should be inspected for polishing defects, such as scratches, pits, relief
polish, comet tails, pulled out inclusions, and voids.

Chemical Etching

Chemical etching is accomplished by immersing the specimen in (or swabbing it with) a

suitable etchant until the required structure is revealed. Etching is done in Petri-dishes or
in other suitable containers with loose covers to prevent excessive evaporation of the
solvent, particularly alcohol solutions. Glass containers can be used for all etchants except
hydrofluoric acid solutions, where the container should be made of polyethylene or other
suitable material. By the use of tongs or other convenient handling device, the surface of the
specimen is immersed in the etchant with some agitation to ensure that fresh etchant is in
contact with the specimen all the times. During etching, most metals lose their bright
appearance, indicating that etching is taking place. With practice, one can ascertain the
completion of etching by the degree of dullness of the surface. If the etching procedure calls
for swabbing, the surface of the specimen can be swabbed with cotton saturated with the
etchant, or the specimen can be immersed and swabbed while in the solution. When etching
is complete, the specimen is rinsed in running water and then in alcohol, followed by drying
in a stream of warm air (hand dryer). After etching the specimen surface is observed under
the optical-microscope for studying its microstructure. Care should be taken while etching
so that the hand is not affected by the etching.

To report:

1. What is mounting?
2. Differentiate between hot and cold mounting?
3. Define terms polishing, grinding, and mesh size?
4. Explain the importance of etchant?
5. Which types of materials are basically polished by electrolytic polishing?
6. What are the affects you have observed on changing etchant time?
7. Which type of precaution should be taken care of before etching?

8
 EXPERIMENT 2

Preparation and optical microscopy of nodular cast iron and determination of nodules
size; Demonstration of illustrative microstructures of ferrous metallic samples; Students
are required to make comparisons.

Objective

Optical Microscopy of different ferrous samples of Steel and Cast Irons

Methodology

• Follow all the steps for making the specimen for etching (as per first day lab)
• Etch with the proper etchant (list of etchants is given in the Appendix)
• See the microstructure with appropriate magnification.
• Draw the microstructure and label.

Brief description about iron carbon diagram:

Read: The Principles of Metallographic Laboratory Practice by George L. Khel

Physical Metallurgy by V. Raghavan and Engineering
Physical Metallurgy by Yu. Lakhtin

We shall now consider alloys of Iron and Carbon in our experiment. We will look at the
microstrucrures of Fe–C alloys, which undergo solid state transformations, such as eutectoid
transformations, martensitic transformations, etc. Fe-C alloys with C content less than 2 wt.
%C are known as plain carbon steels. There are many reasons for studying the microstructure
of plain carbon steels. Carbon steels by far find the maximum use in industries and daily life.
With the variation of different phases, the processing, properties and use of the Fe-C alloys
also vary. Hence, Fe-C phase diagram and the microstructure in carbon steels are to be studied
so extensively.

Let us first look at the Fe rich portion of classical Fe-C phase diagram (Figure 2). Cementite is
an intermetallic compounds orthorhombic crystal structure. This phase diagram depicts a
number of invariant points. If we consider an alloy with 0.8wt% C and heat it to 9500C (1223K),
it forms single phase austenite having FCC crystal structure. Austenite has high solubility of
carbon (max. 2.11wt% at about 11500C) On cooling such an alloy below 723 0C , the alloy
undergoes eutectoid transformation forming two phases, ferrite(α) and cementite,
simultaneously. This structure is known as pearlite, which consists of alternate lamellae of α
and Fe3C. Steels having composition less than 0.8 wt.% C (known as hypoeutectoid steels) has
primary α and pearlite in the microstructure because on cooling such a steel from γ region, it
forms α first until the composition of the remaining γ reaches 0.8 wt.% at temperature of 7230C,
and this austenite undergoes eutectoid transformation. Therefore, microstructure of
hypoeutectoid steels consists of proeutectoid α with lamellar pearlite in varying proportions
depending on the alloy composition. Similarly, Fe-C alloy compositions more than 0.8 wt.% C
are termed as hypereutectoid steels. The microstructure of such steels consists of pro eutectoid
Fe3C with lamellar pearlite.

The microstructure of steels depends on heat treatment conditions. If we heat a steel with
0.7wt% C to 950 0 C and suddenly quench the steel in water (or brine solution), the steel

9
becomes very hard. Quenching of steel is the rapid cooling from a suitably elevated
temperature. This is because, γ transforms to a new phase called martensite, which is a
metastable phase with body center tetragonal crystal structure. Martensite has lath shaped
morphology, which are internally twinned. The microstructures shows twin laths in different
orientations. The most important alloy steel is stainless steel. Stainless steels are stainless as
they have minimum 11.5wt% Cr, which forms very thin, protective, adherent and stable oxide
(preferably Cr2O3) film on the surface. This film is continuous, impervious and passive to stop
further reaction between steels and atmosphere. Stainless steels can be of different types
depending on the microstructure: ferrite, austenitic, martensitic, duplex types. We will study
18 wt.% Cr and 8 wt.% Ni, famously known as 18-8 austenitic stainless steel. The
microstructure shows grains of austenite.

Figure 2: Phase diagram of Fe-C system

Cast Irons

Gray Cast iron: When a cast iron is solidified slowly, the tendency of carbon to separate out
as graphite increases. In gray cast iron the graphite precipitates as irregular, elongated, curved
and interconnected plates. Although the flakes appear as if separated in the two dimensional
microstructure, they are interconnected in three dimensional structures. The large graphite
flakes not only interrupt the continuity of the matrix but also act as stress risers. As a result, the
strength and ductility of the gray cast iron decreases. However, the presence of flake graphite
provides good wear and thermal properties along with good damping capacity. Gray cast iron
is widely used for gear and pump housings, machines beds, brake drums, motor frames and
electrical equipment.

10
White cast iron: White cast irons are very brittle and contain eutectic mixture of austenite and
cementite (known as leduburite) upon cooling. A typical microstructure of white cast iron
consists of dendrites of transformed austenite (later to pearlite) in white interdendritic network
of cementite. Cementite is a hard, brittle interstitial compound. Since white cast iron contains
relatively large amounts of cementite in the form of continuous interdentritic network, it makes
the white cast iron “hard” and “wear resistant”. However, it is extremely brittle and difficult to
machine. White cast irons have limited in engineering applications, because of inherent
brittleness and lack of machinability. They are used where wear resistance is most important,
and service condition does not require ductility such as liners for cement mixtures, ball mills,
certain type of drawing dies and extrusion nozzles.

Nodular/ Spheroidal cast iron: In the nodular cast iron the graphite is present as tiny balls or
nodules. Nodular iron is produced by the addition of one or more elements, such as as Mg, Ce,
Ca, Li, Na, and Ba to the molten metal. Mg plays an important role in the formation of graphite
nodules. The spheroids result in higher strength and toughness compared to gray cast iron.
Some typical application of nodular iron includes crank shafts, pistons, cylinder heads, fly
wheels, work rolls, lever, etc.

Microstructure of 304 stainless steel Colour mixture of austenite, ferrite and sigma
phases

To report:

1. Draw the structures what you see under microscope and label.
2. Calculate the nodules size in Cast Iron.

11
 EXPERIMENT 3

Preparation and Optical microscopy of non-ferrous sample (Brass); determine the

phase fraction
Demonstration of illustrative microstructures of non-ferrous metallic samples

Objective:

Optical Microscopy of different non-ferrous samples

Methodology

• Follow all the steps for making the specimen for etching (as per first day lab)
• Etch with the proper solutions (list of etchant is given at the end of the document)
• See the microstructure with appropriate magnification.
• Draw the microstructure and label.

Brief description about eutectic alloys.

Read: Physical Metallurgy by V. Raghavan and

Engineering Physical Metallurgy by Yu. Lakhtin

The metallography of non-ferrous metals are little tricky since they are soft and some of the
cases, special reagents are required for etching.

Copper (Cu):

Copper is a face centered cubic (FCC metal) with very high ductility, electrical and thermal
conductivity. This is very soft too. It is used in electrical applications, industrial machinery,
hearth for arc furnaces. In the alloyed form, it also finds enormous importance. One such
application is duralumin (Al-4.5% Cu), which is common material for airplane body material.
When it is alloyed with Zn, it is called brass. 70:30 brass is very common in making pipe lines
for water.

Brass:

Figure 3 shows the Cu-Zn phase diagram with different phases. Cu-rich portion of the phase
diagram reveals a cascade of peritectic reactions. The peritectic reactions corresponding to +
brass is marked. In the laboratory exercise, you will study the microstructure of composition
of alloy Cu:Zn = 60:40. The microstructure will reveal presence of both the  and  phases
because of incomplete peritectic reaction. Apart from Brass, many other technically important
alloy systems such as steels, CuSn (Bronze), rare earth permanent magnets (Nd-Fe-B) and high
Tc superconductors (Yb-B-Cu-O) display peritectic reactions, where phase and microstructure
selection plays an important role for the processing and the properties of the material. The
peritectic reaction can be written as a + L →  on cooling, where  and  are solid phases and
L stands for liquid. Therefore, a primary solid phase reacts with liquid leading to formation of
another solid phase. The second solid phase is called peritectic phase. The equilibrium
microstructure of such alloys will show  as dendrites (tree like structure). During normal
 the reaction never goes to completion and hence, some amount
freezing of the peritectic alloy,
of primary  phase remains in the microstructure surrounded by the  phase.

12
 Figure 3: Phase diagram of Cu-Zn system

To Report:

1. Draw the microstructures and label.

2. Calculate the phase fraction in Brass.

13
 EXPERIMENT No. 4

Annealing, Normalizing and Hardening with 0.4% C steel

Preparation, microscopy, hardness measurements and comparison among all students
w.r.t. microstructure

A heat treatment of an alloy involves three basic steps: heating, soaking and cooling with
desired rate. Heat treatments are usually carried out to alter the microstructure of metals and
alloys, which in turn is required to obtain certain properties for particular applications. Heat
treatment can also be used to alter certain manufacturability objectives such as to improve
machining, improve formability, and restore ductility after a cold working operation. The
method chosen depends on the desired characteristics of the material. Steels have become most
widely used engineering material mainly because properties of steels can be varied over a wide
range by employing suitable heat treatments. This experiment focuses on three very common
heat treatment practices used for steels.
FULL ANNEALING
Annealing is a heat treatment process generally used to increase the ductility and reduce the
hardness of steel to make it more workable (the material can be cold-worked for larger strains
without fracture). The process involves the following steps:
a) Heating the steel to above its A3 temperature, at which the steel exists as single phase
austenite.
b) Keeping the material at the above mentioned temperature for definite time period to
achieve homogenous austenitization.
c) Furnace cooling of the material so as to make the material nearly stresses free (by
reducing the number of defects and internal stresses of the material) and the phases
reach their equilibrium compositions and phase fractions as per the phase diagram.
NORMALIZING
Normalizing is a heat-treatment process that is often used to provide uniformity in grain size
and composition throughout bulk material. The process involves the following steps:
a) Heating the steel to above its A3 temperature.
b) Keeping the steel at the above-mentioned temperature for definite time period to
achieve homogenous austenitization
c) Cooling of the material in air (termed as air-cooling) so as to get uniform and relatively
fine-grained distribution.

Normalizing produces higher amount of pearlite than annealing in a steel of same

carbon content. Normalizing gives harder and stronger steel, but with less ductility for the
same composition than full annealing.
HARDENING
Hardening process often results in increase in the level of hardness, producing a stronger
material. The process involves the following steps:
a) Heating the steel to above its A3 temperature.
b) Keeping the steel at the above mentioned temperature for definite time period to achieve
homogenous austenitization.
c) Quenching the steel in water or oil to cause the soft initial material to transform to a
much harder, stronger structure (martensite).
Often, the hardened material is very brittle and cannot be used without tempering to improve
their toughness.

14
OBJECTIVE
1. To observe the micro structural changes in hypo eutectoid steels during annealing,
normalizing and hardening heat treatments.
2. To examine the effect of the above treatments on the hardness of the steel.

PROCEDURE
Sample Preparation
1. Annealing of the hypo eutectoid steel specimen by heating the sample to about 910°C
temperature and hold the specimen at this temperature for a definite time period
followed by furnace cooling to room temperature in the furnace.
2. Normalizing of the hypo eutectoid steel specimen by heating the sample to about 910°C
temperature and hold it 1hr at this temperature for homogeneous austenitization
followed by cooling to room temperature in air.
3. Hardening of the hypo eutectoid steel specimen by heating the sample to about 910°C
temperature and hold it 1hr at this temperature followed by quenching in water.
Polishing
1. In order to reveal the microstructure, polish and etch the samples using the procedure
described in Experiment 1 in the first set of labs.

RESULTS
1. Typical Microstructures Observed label the various features
2. Explain the observed microstructures based on the CCT diagram.
3. Compare and comment on the hardness of the different samples.

QUESTIONS

Q1. What could be temperature range for annealing and normalizing for a eutectoid steel?
Q2. How the size of the sample and carbon content affect the formation of martensite during
normalizing.
Q3. Arrange the following quenching media with increasing order of cooling rate that they
can yield: (i) water (ii) oil and (iii) brine.

15
 EXPERIMENT 5

Measurement of case depth in carburizing (gear sample) and decarburizing in 0.45% C steel,
hardness and microstructure evaluation

If steel is exposed to carbonaceous atmosphere (e.g., CO gas) at an elevated temperature,

carbon dissolves in the surface of the specimen building up the carbon concentration at the
surface and subsequently diffuses inside the steel under the influence of carbon concentration
gradient. Such a process is known as carburizing. There three types of carburizing processes.
In Pack Carburizing, the steel to be carburized is packed inside a box, which is a rich source of
carbon such as coke. In liquid carburizing, the steel is dipped in a salt containing carbon. In
Gas Carburizing, an appropriate gaseous environment is maintained on the surface of the steel
such that high chemical potential of carbon exists on the surface of steel and hence carbon can
diffuse from surface into the interior of the steel.

Gas carburizing is the most industrially used process because of its low coast and
ability to be scaled to a large and continuous production of parts. Although various reaction
equilibria exist in the gaseous atmosphere of carburizing, the most basic reaction responsible
for maintainng required chemcial pontial of carbon on top of steel is as follows:

2CO (g) = CO2 (g) + C (steel) ...............(1)

The steels used in carburized process are typically low carbon steels (carbon content
between 0.15-0.25 wt%). The carburization process is used to increase the carbon content to
a desired depth (called case depth) below the surface. Since the process depends upon
diffusion of carbon in austenite, the case depth is controlled by temperature and time. Once
the carburizing is over, the steel is quenched in oil so that the case transforms to martensite
whereas the core of the steel, which is still low in carbon, transforms to a mixture of fine
pearlite, bainite and small fraction of low carbon martensite. Thus, the resulting sample has a
very hard and wear-resistant surface and tough core. This process is usually employed in
applications like transmission gears and shafts

It is necessary to maintain the carburizing atmosphere such that reaction (1) is driven
from left to right. If the atmosphere is disturbed or not maintained properly, the reaction may
reverse, and this may lead to loss of carbon from steel instead of addition of carbon into the
steel. This is referred to as “decarburizing” and is not desirable. Precaution have to be taken
to avoid decarburizing that may occur during annealing of various types of steels such as in
high and medium carbon steels or during soaking of carburized steels for further hardening.

DIFFUSION OF CARBON
In a carburizing furnace, steady state is maintained such that a constant carbon
potential is maintained the surface of the carbon, which corresponds to a constant carbon
concentration on the surface of the carbon (Cs) during the entire carburizing process. This
value of CS is typically kept at 0.8 wt. If we assume that the diffusion is unidirectional, the
process of carbon diffusion can be described by the following diffusion equation:

𝜕𝑐 𝜕 𝜕𝑐
= 𝜕𝑥 (𝐷 𝜕𝑥) (5.1)
𝜕𝑡

Where D is the diffusion coefficient of carbon in austenite (since the process is carried
out at a temperature at which steel exists in austenite phase), c is the concentration of carbon,

16
 t is the diffusion time and and x is the depth below the surface. If D is taken as constant then,
𝜕𝑐 𝜕2 𝑐
= 𝐷 𝜕𝑥 2 (5.2)
𝜕𝑡

The solution to equation (5.2), in the case of a semi-infinite bar (with initial concentration c0)
where the surface concentration is kept constant at Cs (as shown in figure 5.1) gives the
concentration, c(x,t) as a function of time (t) and depth (x):

𝐶(𝑥,𝑡)−𝐶0 𝑥
= [1 − 𝑒𝑟𝑓 2√𝐷𝑡 ] (5.3)
𝐶𝑠 −𝐶0

Figure 10.2 shows the typical microstructure of carburized and hardened mild carbon
steel sample at cross-sections obtained at different depths. Martensite and retained austenite
phases can be seen (figure 5.2(a)) at the surface. Figure 5.2(b) shows the fine pearlite (dark)
and martensite phases at the sub-surface with lower C than surface. Further going deep into
the sample, proeutectoid ferrite (white) and low carbon martensite phases can be observed
(figure 5.2(c)) in the core part of the sample.

Case depth is usually taken as the depth at which the carbon concentration falls to 0.4
wt% or in terms of micro-hardness, the depth at which the micro-hardness falls to 550 Hv.
The latter standard is more common as it is easy to measure by taking micro hardness profile
from surface to the core.

C
t3 > t2 > t1
Carbon conc. (wt%)

Cs Figure 5.1. Concentration

profile for non-steady state
t3 diffusion in a semi-infinite
t1 bar taken at three different
t2 times t1, t2, t3

0 Depth below surface x

(a) (b)

17
 (c)
Figure 5.2. Microstructure of carburized mild carbon steel sample at the following cross-
sections: (a) surface; (b) sub-surface; (c) core.

OBJECTIVE
1. Measure the case depth of harden plain carbon steel.
2. To study decarburization of steel.

PROCEDURE
1. Decarburize one eutectoid steel sample at 900°C in air atmosphere for 1 hour followed
by air cooling.

Polishing
2. In order to reveal the microstructure, polish and etch the samples using the procedure
described in Experiment 1 in the first set of labs.
3. Etch the samples with Beraha’s sulfamic acid (100ml water, 3g potassium
metabisulfite, 1g sulfamic acid).

Observations under Microscope

4. Observe the specimen under an optical microscope.
5. Sketch the typical microstructures obtained and label all important features neatly.
Hardness measurement
6. Measure hardness (using Vickers micro-hardness tester) in the carburized sample at
several depths below the surface.

RESULTS
1. Depth of carburization and de-carburization observed in the samples.
2. Plot the variation of hardness as a function of depth.
3. Estimate diffusion coefficient of carbon in austenite from the depth of decarburized
layer assuming that the solubility of carbon in ferrite is 0.02 wt%. Also assume that
carbon content of air is kept constant at zero.

18
 Appendix

List of Etchants

Sr Etching Regent Composition Suitable for

1 Nitric Acid (Nital) HNO3 1 to 5 ml For low carbon and
Ethyl or methyl Alcohol 100 ml mediam carbon steel
2 Picric Acid (Picral) Picric Acid 4 gm For all grades of
Ethyl or methyl alcohol 100ml carbon steel
3 Ferric Chloride and FeCl3 5g
Hydrochloric acid HCl 50 ml Stainless Steel
H2O 100 ml
4 Ferric Chloride FeCl3 5 to 10 g
HCl 15 to 20 ml Copper, Brass
Water 100 ml
5 Mixed Acids HNO3 5ml
Water 95ml Lead Tin Alloy
6 Mixed Acids HCl 50 ml
Water 50 ml Zinc and its alloys

19