MSE 251 Lab Manual

MSE 251
Physical Metallurgy and Materials Characterization Lab

(2023-2024-II)
Lab Schedule: Tuesday and Thursday, 14:00 to 16:50hrs
Lab Start Date Tuesday 09/01/24 & Thursday 11/01/24
Venue: Physical Metallurgy Lab (WL-201& 202)
Course Website:
https://hello.iitk.ac.in/mse251sem22324/#/home
Instructors:
Shashank Shekhar, MSE Shivam Tripathi, MSE
Office: Western Lab 304A Office: 510, ESB-III
Email: shashank@ Phone: 6528 Email: shivamt@ Phone:2426
Lab In charges:
G P Bajpai
7933; gpbajpai@
Lab Staff:
Ajay P. Singh Satya P. Nath Harshit Agarwal
ajayps@ spnath@ harshitag@
TAs:
Day Name Email Contact Experiment No.
1 Amit Kumar Yadav amitky21@ 7488347093 6 (SEM)

2 Deepti Gangwar gdeepti@ 9927305994 5 (Kinetics)
Tuesday 3 Ankit Singh Negi asnegi@ 7983369952 4 (Carburizing)
4 Ayan Mullick ayanm23@ 9330659292 3 (HT)
5 Swagata Datta swagatad23@ 9804074322 7 (Wettability)
1 Abhinav Dixit adixit@ 9532017575 6 (SEM)
2 Peri Bala Kameshwar pbalak23@ 8886701588 5 (Kinetics)
Thursday 3 Abhishek Kumar Verma abhishekkv20@ 7376142903 4 (Carburizing)
4 Radhakrishnan Sriram sriamr23@ 6303310084 3 (HT)
5 Ruhi Syed ruhiagani23@ 7620087379 7 (Wettability)
Recommended Reading
✓ The Principles of Metallographic Laboratory Practice by George L. Kehl
✓ Physical Metallurgy by V. Raghavan
✓ Engineering Physical Metallurgy by Y. Lakhtin
List of Experiments
Combined Experiments
Lab Activity/Experiment Tuesday Thursday
Turn
1 Formation of Groups, Distribution of manual, Common instructions for First half First half
lab Sample preparation (mounting, polishing, and etching) and observing of the of the
the microstructure of).45% carbon steel in optical microscope (BF, DF, section section
etc.)
2 Sample preparation (mounting, polishing, and etching) and observing the Second Second
microstructure of soft metallic material (Brass) in optical microscope (BF, half of half of the
DF, etc.) section section
Experiments for Set-1

Turn
3 (i) Heat treatment of steel – Microstructure examination and hardness T1,T5,T Th1,Th5,T
measurement post-annealing, normalizing, hardening, tempering (ii) 4,T3,T2 h4,Th3,Th2
Optical microstructure examination of cast iron and steel (hypo
eutectoid, hypereutectoid)
4 (i) Hardenability – Jominy end quench test (ii) Carburization - T2,T1,T Th2,Th1,T
decarburization of steel and measurement of case depth 5,T4,T3 h5,Th4,Th3
5 (i) Optical microstructure examination of non-ferrous material: cold T3,T2,T Th3,Th2,T
work, recovery, recrystallization, grain growth (ii) Quantitative 1,T5,T4 h1,Th5,Th4
metallography – Grain growth kinetics/pearlitic growth in eutectoid
steel (JMAK relation)
6 (i) Sample preparation and demonstration of scanning electron T4,T3,T Th4,Th3,T
microscopy (imaging and EDS), (ii) Fractography of tensile, fatigue 2,T1,T5 h2,Th1,Th5
fractured samples
7 Wettability/contact angle measurement (ii) Optical microstructure T5,T4,T Th5,Th4,T
examination after arc welding and hardness measurement 3,T2,T1 h3,Th2,Th1
Experiments for Set-2

Turn
8 (i) Thermal etching and microstructure observation of ceramic T1,T5,T4, Th1,Th5,
materials, (ii) Etch pit technique for dislocation density measurement T3,T2 Th4,Th3,
(LiF, Fe-Si, Cu, etc.) Th2
9 (i) Cooling curve/DTA of a binary alloy – Application to phase diagram T2,T1,T5, Th2,Th1,
determination (ii) Macrostructure examination of an ingot section (e.g. T4,T3 Th5,Th4,
Zn, steel) Th3
10 (i) Creating and visualizing crystal-structures and related features using T3,T2,T1, Th3,Th2,
a crystallography software (ii) Identifying crystal orientation using T5,T4 Th1,Th5,
Laue pattern Th4
11 (i) Differential scanning calorimetry (DSC) - Phase transformation in T4,T3,T2, Th4,Th3,
metals and polymers (ii) X-Ray diffraction – Determination of T1,T5 Th2,Th1,
crystallite size/strain Th5
12 (i) Demonstration and analysis of FTIR, Raman and other advanced T5,T4,T3, Th5,Th4,
characterization technique, (ii) Demonstration of sample preparation for T2,T1 Th3,Th2,
TEM Th1
READING RELATED TO EXPERIMENT 1 & 2
SAMPLE PREPARATION (MOUNTING, POLISHING , AND ETCHING ) AND OBSERVING
MICROSTRUCTURE IN OPTICAL MICROSCOPE (BF, DF, ETC.)
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
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 convenient 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.
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
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
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.
EXPERIMENT 1
MICROSTRUCTURE OF CAST IRON AND STEEL IN OPTICAL MICROSCOPE (BF, DF,
ETC.)
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
4. Optical microscopy of 0.45% carbon steel
Methodology
• Mounting of a given sample

• Grinding
• Polishing (manual) with a set of 4 papers
• Cloth polishing with alumina solution
• Etching with 3% Nital solution
• Microstructure observation in BF and DF
• Completion of report
Brief description about iron carbon diagram:
Read: The Principles of Metallographic Laboratory Practice by George L. Khel

Physical Metallurgy by V. Raghvan 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 1). 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
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 austentic stainless steel. The microstructure
shows grains of austenite.
Figure 1.1: 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.
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. 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. Draw the structures what you see under microscope and label.
EXPERIMENT 2
MICROSTRUCTURE OF SOFT METALLIC MATERIAL IN OPTICAL MICROSCOPE (BF, DF,
ETC.)
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
4. Optical microscopy of brass
Methodology:
• Mounting of a given sample

• Grinding
• Polishing (manual) with a set of 4 papers
• Cloth polishing with water
• Etching with Ferric Chloride solution
• Microstructure observation in BF and DF
Introduction:
Read: Physical Metallurgy by V. Raghvan 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 2.1 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
freezing of the peritectic alloy, the reaction never goes to completion and hence, some amount
of primary  phase remains in the microstructure surrounded by the  phase.
Figure 2.1: Phase diagram of Cu-Zn system
To Report:
1. Draw the microstructures and label.

2. Calculate the phase fraction in Brass.
EXPERIMENT 3
(i) HEAT TREATMENT OF STEEL – MICROSTRUCTURE EXAMINATION AND

HARDNESS MEASUREMENT POST ANNEALING , NORMALIZING ,
HARDENING , TEMPERING
(ii) OPTICAL MICROSTRUCTURE EXAMINATION OF CAST IRON AND STEEL
(HYPOEUTECTOID , HYPEREUTECTOID )
Objective:
1. To examine the effect of the various heat treatments of steel by examining the
microstructure and study its effect on the hardness
2. To examine the optical microstructure of cast iron, hypo eutectoid and hyper eutectoid
steels
Methodology:
Material: Medium carbon steel
• 2 samples post annealing

• 10 samples anneal at 910 ℃ for 10 minutes
• 3 samples for air cooling
• 3 samples water quenching
• 2 samples for tempering at 400 ℃ for 10 minutes
• 2 samples for tempering at 400 ℃ for 30 minutes
• Hardness measurement with the Rockwell hardness tester
• Sample preparation for microscopy similar to Experiment 1
• Observation of microstructures
Introduction:
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 four 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:
c) Quenching the steel in water or oil to cause the soft initial material to transform to a
much harder, stronger structure (martensite).
Tempering
Often, the hardened material is very brittle and cannot be used without tempering to
improve their toughness. The process involves the following steps:
c) Quenching the steel in water or oil to cause the soft initial material to transform to a
much harder, stronger structure (martensite).
d) Reheating the quenched sample to higher temperature (Tempering temperature) and
keeping it there for definite period of time.
Tempering results in a decrease in hardness and an increase in the ductility and toughness
of the steel.
Brief description about iron carbon diagram:
Read: The Principles of Metallographic Laboratory Practice by George L. Khel

Physical Metallurgy by V. Raghvan 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 3.1). 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
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 austentic stainless steel. The microstructure
shows grains of austenite.
Figure 3.1: Phase diagram of Fe-C system
Microstructure of 304 stainless steel Colour mixture of austenite, ferrite and

sigma phases
To Report:
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.
EXPERIMENT 4
(i) HARDENABILITY – JOMINY END QUENCH TEST
(ii) CARBURIZATION - DECARBURIZATION OF STEEL AND MEASUREMENT OF
CASE DEPTH
Objective
1. To study hardness as a function of quench rate and investigate the hardenability of steels
2. Measure the case depth of hardened plain carbon steel during carburization
3. To study decarburization of steel
Methodology
Hardenability – Jominy end quench test
• Place a Jominy specimen into the furnace set at 950° C

• Adjust the water column height in the Jominy end quenching tank to 65 mm above the
orifice with faceplate valve wide open. Close the faceplate without changing the water
column height adjustment so that when the faceplate is opened later on the water
column will rise immediately to 65mm.
• After 30 minutes in the furnace transfer the Jominy specimen to the specimen holder of
the Jominy end quenching tank. Then after the Jominy specimen is in place, turn on the
water and quench the bottom end of the specimen Transfer from furnace to quench
should be rapid (in minor than 5 seconds).
• Measure hardness (using vicker’s micro-hardness tester) in the Jominy speciment at
several distances from the quenched bottom end
Carburization - decarburization of steel and measurement of case depth

Carburization
• One gear sample is already cut and mounted
• Before starting indentation, the sample has to be polished to remove rust &
indentation
• Put under Vickers hardness tester
• Align the base of the teeth with the horizontal crosshair line
• Move 50-micrometer steps (5 divisions) on the Vernier in the reverse direction and
take indentation ( example readings on micrometer positions: 15, 10, 5, 0, 45, 40, 35
….)
Decarburization
Material: 0.8% carbon steel

• Heat at 1000 ℃ for 1 hour
• Cut multiple cross-sections of the rod after decarburization (throw the end piece and
use other)
• Mount the samples
• Sample preparation for microscopy similar to Experiment 1
• Measure the decarburized layer (white layer without any pearlite)
• Take reading at 5 different positions
• Use the average “decarburized” depth (x) to calculate D as per the procedure in
manual: c(x,t) = 0.02, cs = 0, c0 = 0.5
Introduction:
Hardenability – Jominy end quench test
Hardenability is the ease with which a steel piece can be hardened. It is also the depth of
hardening produced under given condition of cooling. Hardenability depends on content of
alloying elements & grain size of the material. Coarse-grained material has better hardenability
than fine-grained material. This is due to the fact that grain boundary reduces the cooling rate.
Any factor that reduces the cooling rate will decrease the hardenability. Hardenability is
different than hardness. Hardenability is an ability to harden while hardness is a measure of the
resistance of material to plastic deformation. There are various methods to determine the
hardenability. For e.g. Grossman method, Jominy end quench method etc. When a piece of
steel of any appreciable size is heated to its austenization temperature & then quenched, the
cooling rates during quenching vary across the cross section. The cooling rate at the surface &
the center are not same. The difference in their rate increases with rise in severity of quenches
or decreases in the speed of heat absorption. At the center of the cross section, the cooling rate
is slowest. This may give rise to the formation of pearlite. The relatively permanent & most
common method of determining the hard ability of steel is the Quench test. This is also called
as ‘Jominy End Quench Test’.
Knowledge about the hardenability of steels is necessary to be able to select the

appropriate combination of alloy steel and heat treatment to manufacture components of
different size to minimize thermal stresses and distortion. 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.
Carburization - decarburization of steel and measurement of case depth
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 maintaining required chemical potential 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 forms 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 at 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) (4.1)
𝜕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,
t is the diffusion time and x is the depth below the surface. If D is taken as constant then,
𝜕𝑐 𝜕2 𝑐
= 𝐷 𝜕𝑥 2 (4.2)
𝜕𝑡
The solution to equation (4.2), 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 4.1) gives the
concentration, c(x,t) as a function of time (t) and depth (x):
𝐶(𝑥,𝑡)−𝐶0 𝑥
= [1 − 𝑒𝑟𝑓 2√𝐷𝑡 ] (4.3)
𝐶𝑠 −𝐶0
Figure 4.2 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 4.2(a)) at the surface. Figure 4.2(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 4.2(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 micr-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 4.1. 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)
(c)
Figure 4.2. Microstructure of carburized mild carbon steel sample at the following cross-
sections: (a) surface; (b) sub-surface; (c) core.
To Report:
1. Plot a hardenability curve of hardness vs. distance from the quenched end in Jominy
End Quench Test’
2. Depth of carburization and de-carburization observed in the samples.
3. Plot the variation of hardness as a function of depth.
4. 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.
EXPERIMENT 5
(i) OPTICAL MICROSTRUCTURE EXAMINATION OF NON -FERROUS MATERIAL :
COLD WORK , RECOVERY , RECRYSTALLIZATION , GRAIN GROWTH AND TWIN
OBSERVATIONS
(ii) QUANTITATIVE METALLOGRAPHY – GRAIN GROWTH KINETICS / PEARLITIC
GROWTH (JMAK RELATION )
Objective
1. To report microstructural changes in a cold worked single phase alloy during its
annealing, in particular observe changes during recovery, recrystallization and grain
growth
2. Determine grain growth kinetics in eutectoid steel by quantitative metallography
Methodology:
Material: Brass
• Rolled to 50%
• Recrystallize at 400 ℃ for 20 min & 40 min
• Sample preparation for microscopy of 4 samples ( as received, rolled, and annealed
for 20 min and 40 min)
• Measure the decarburized layer (white layer without any pearlite)
• Record microstructure of all 4 samples
• Use quantitative metallography to calculate number of grains per unit area as per
manual
Introduction:
Metals can be plastically deformed i.e. they will not come back to their original shape
and size when the load causing their deformation is removed. Thus, we can roll a metallic strip
to reduce its thickness. Similarly, there are many other metal working operations which are
industrially used to make components and parts of many engineering devices from metallic
materials.
A small percentage of the energy spent in plastically deforming a metal remains stored
in its structure and increases its internal energy. This increment in the internal energy is
associated with the generation of lattice defects such as vacancies, interstitials, dislocations and
stacking faults during plastic deformation of the crystal. On a microscopic scale the distribution
of these defects, however, is very inhomogeneous. For example, bulk of the deformed crystal
consists of relatively dislocation-free regions (called sub-grains or cells) separated by boundary
regions of high dislocation density in which many dislocations are arranged as tightly packed
tangles There may be many of such cells in each grain of the material. If the deformation occurs
at a low enough temperature so that the crystal has very little thermal energy to recover from
such a structure, dislocation tangles are retained in its structure, and we refer to such a structure
as the cold worked structure. What do you think will happen when such a structure is heated?
Obviously, the crystal acquires thermal energy and with its help several thermally activated
mechanisms, such as atomic diffusion begins to operate. Heating of a cold-worked (or cold-
deformed) structure at a given temperature for a given period of time is generally referred to as
annealing. Phenomena which occur during annealing are recovery, recrystallization, and grain
growth.
Recovery:
The first effect of reheating previously cold-worked metal is reduction of internal stress without
noticeable change of mechanical properties. Since this effect is not evident microscopically,
the importance of the recovery process has not been widely appreciated by engineers. Recovery
in a cold-worked structure occurs when the material is held at relatively lower temperatures for
a given time interval. It involves changes in the number and distribution of point defects and
dislocations present in the cold-worked structure. Since the temperature of annealing is low
during recovery, structural changes in the material occur by the clustering of point defects like
vacancies and interstitials and the migration of point defects to dislocations, grain boundaries
and/or external surfaces of the crystal. If the annealing is carried out at somewhat higher
temperature even dislocations (which are less mobile than point defects) may gain appreciable
mobility and move by glide and climb to relieve some of the internal strain accumulated in the
structure. Some of the dislocations may rearrange themselves while some others may get
annihilated by mutually canceling each other. Thus, during the process of recovery of a cold-
worked material the dislocation density of cells gets reduced and dislocation walls around these
cells become more sharply defined. Small changes in hardness which are usually observed
during later stages of recovery are due to decrease in the number of point defects and
dislocations.
Recrystallization
Recrystallization entails the complete formation of new and unstrained metal grains, with
simultaneous elimination of previously cold-worked and distorted metal. Recrystallization is
very evident because of its marked effect on mechanical properties. Strain hardening and work
strengthening which resulted from cold working are largely eliminated by recrystallization and
ductility is simultaneously restored. The microscopical appearance of cold-worked metal is
also greatly changed by recrystallization.
When annealing is carried out at even higher temperatures recrystallization occurs. During the
recrystallization process new strain-free grains crystallize in the earlier cold-worked structure.
The free energy of the system is lowered by these newly formed strain-free grains. In an
aggregate of deformed metal crystals, there are regions where the· atomic structure is most
highly disarranged, and such regions exhibit the strongest tendency for realignment into an
unstrained condition and the strongest desire for recrystallization. These regions are at grain
boundaries, at slip planes or twinning planes, at internal discontinuities, regions of stress
concentration caused by inclusions, and elsewhere with the crystal where internal strain is high.
These new grains grow at the expense of the deformed structure until the whole matrix is
consumed. This process occurs either by migration of original grain boundaries or by sub-grain
growth. The recrystallized matrix has much lower dislocation density than the deformed
material. The lowest temperature at which strain-free recrystallized grains appear in the
structure of the previously cold-worked structure is termed as the recrystallization temperature
of that material. The recrystallization temperature is influenced by the grain size, the severity
of cold-work, strain given during plastic deformation, the presence of solute atoms and the
second phase in the structure. complete, but it is usually much more satisfactory to think in
terms of the range of temperatures between the first appearance of a new grain and complete
recrystallization. This is called the recrystallization temperature range.
Greater prior cold working increases the number of recrystallization nuclei and ensures finer
grain size after complete recrystallization. Greater plastic deformation also creates greater
misalignment at grain boundaries and regions of internal strain, a factor which allows
recrystallization at lower temperature. The recrystallization temperature is lower because less
thermal agitation is necessary to obtain sufficient energy for the atoms to become rearranged
by recrystallization.
Finer initial grain size results in more strained regions in plastically deformed metal, which in
turn causes finer grain size in the fully recrystallized metal. Nucleation and growth of new
unstrained crystals are time and temperature dependent. For a given amount of plastic
deformation, the rate of nucleation and the growth rate of the newly formed grains are more
rapid at higher temperatures.
Recrystallization occurs by the continual formation of new unstrained grains and their growth
until all the strained metal is replaced by unstrained material. The recrystallization temperature
is defined as the temperature at which recrystallization is complete, but it is usually much more
satisfactory to think in terms of the range of temperatures between the first appearance of a
new grain and complete recrystallization. This is called the recrystallization temperature range.
It is not possible to cite particular recrystallization temperatures, since recrystallization depends

upon several variables. Increased plastic deformation allows recrystallization at a lower
temperature, as plotted in Fig. 5.1. The time of annealing also has an effect. Increased time
allows recrystallization at lower temperature (Fig.5.2). Coarse grained metal is not work-
hardened as much by a given amount of deformation as is finer-grained metal and will not have
as great an urge to recrystallize. Therefore, the recrystallization temperature will be higher for
coarse-grained metal
Fig 5.1 Effect of prior cold work on Fig 5.2 Effect of annealing time on
recrystallization temperature recrystallization temp of cold worked
metal
Grain Growth or Coalescence

When cold-worked metal is held above the recrystallization temperature after recrystallization
is complete, growth of some of the recrystallized grains at the expense of other grains occurs,
a process called grain growth or coalescence. This is a digestion process in which some grains
increase in size while others get smaller and finally disappear, resulting in a larger average
grain size and a smaller total number of grains.
Grain growth occurs because in doing so the total area of grain boundaries reduces and lowers,
in turn, the grain boundary energy of the system.
Because engineering properties of metals are related to grain size, control of grain growth is an
important feature of the metallurgy of cold working and annealing. Control of grain size of
cold-worked metal during heat treatment depends, to a large measure, upon control of prior
history of the material, but a fine-grained structure can be coarsened by coalescence during
annealing. Attempts to shorten the annealing time after cold working by utilizing a high furnace
temperature may result in excessive coalescence. Overloading furnaces so that some parts of
the charge are overheated before the entire charge is adequately softened may also result in
excessive coalescence in the overheated portions.
Why do some crystals grow during coalescence while others become smaller and disappear?
Grain-boundary migration is the fundamental feature that governs this condition, although the
driving force for boundary migration is not completely known. When the boundary between,
two metal grains is perfectly plane, it has little tendency to migrate, and there is little tendency
for one grain to digest its neighbor. However, boundaries that are not in plane appear to migrate
toward the center curvature of the boundary. This tends to make large grains larger small grains
smaller until they disappear. Also, there may be a tendency for grains to grow in certain
crystallographic directions preferentially to other directions.
A complete analysis of grain-boundary migration is not within the scope of engineering

metallurgy, but this brief statement of possible mechanisms is included as a means of
evaluating the effects of various working and heating cycles on boundary migration. Purer
metals or alloys coalesce extensively, while less pure material retains fine grain size for longer
annealing periods or at higher annealing temperatures. All metals, or even all heats of the same
metal, do not develop similar grain sizes during forming and reheating processes, and do
exhibit differences in subsequent operations and significant variation in final properties.
The Cold-work-Anneal Cycle
From the preceding discussion it is evident that cold working hardens and strengthens metals
at the expense of decreased ductility. However, when cold working is excessive, the metal may
fracture before reaching the desired size and shape. To avoid such defects, the total deformation
is produced in several steps with intermediate anneals to soften the hardened metal and to
regain lost ductility so that further deformation is possible. This process of repeated cold
working and annealing is called the cold-work- anneal cycle, which is illustrated for specific
conditions in Fig. 5.3.
Fig 5.3. Cold –worked anneal cycle.
Metal is hardened and strengthened by cold deformation and ductility is decreased. Before the
metal fractures, cold working is stopped as at X. If metal which has been previously deformed
to point X is reheated for 1 hr at temperature Y, the original ductility and strength will be
returned. To obtain intermediate properties, the stock is annealed when sufficiently oversize so
that the desired properties will be developed during a final working operation. Consideration
of these two operations, hardening and subsequent softening, as a unit is most important for
engineering applications, since they allow a shape to be formed with any prescribed degree of
work strengthening. When a completely softened product is desired, process annealing follows
cold working. Complete recrystallization and softening result. However, if the final product
must be stronger than the fully softened material, it becomes necessary that the last
recrystallization anneal precede final cold working.
Grain growth occurs because in doing so the total area of grain boundaries reduces and lowers,
in turn, the grain boundary energy of the system. In simple situations the occurrence of grain
growth can be expressed in terms of the following relationship:
𝐷𝑡 − 𝐷0 = 𝑘𝑡𝑛 (5.1)
Where 𝐷𝑡 is the average grain diameter after the annealing time of t, 𝐷0 is the initial grain
diameter before grain growth starts, and K is a constant. Usually, a value of n is estimated to
be 1/2.
Grain Size Measurement by Quantitative Metallography:
From the study of actual grain shapes, it has been found that while grains do not actually
possess regular or idealized forms the truncated octahedron is a reasonable approximation for
equiaxed grains. For the quantitative estimate of the average grain size of a single-phase
equiaxed grain structure the grains along a line, circle or within a known area are counted. In
Jeffries' Planimetric Method a circle surrounding a known area is superimposed on the
microstructure as shown in Fig.5.4. The grains cut by the circumference nc and grains
completely within the circle ni are counted. Half of the number of grains intersected by the
circumference is added to the number of completely included grains to get the number of
equivalent whole grains within the circle.
1
𝑛 𝑒𝑞 = 2 𝑛 + 𝑛𝑖 (5.2)
𝑐
Fig 5.4 Grains size measurement by Jefferies Planimetric method
𝑛
The number of grains per unit area (NA) is given by 𝑒𝑞⁄𝐴 where A is the actual area of the
specimen investigated. If the photomicrograph was taken at a magnification m, A = observed
area/𝑚2 .
To Report:
1. Draw the microstructures in the increasing order of time with all the details like
magnification, temperature, time.
2. Measure the number of grains per unit area in the increasing order of time.
Questions:
1. What factors are expected to raise the recrystallization temperature of a metal or alloy?
Why?
2. If we hold the cold worked sample in the furnace for a very long time at a temperature
above its recrystallization temperature, will the grain growth continue or will it stop at
some stage? Explain.
3. During recrystallization where do new grains will first form? Why?
4. Why is metal able to plastically deform under a given load, while glass breaks?
EXPERIMENT 6
(i) SAMPLE PREPARATION AND DEMONSTRATION OF SCANNING ELECTRON

MICROSCOPY (IMAGING AND EDS)
(ii) FRACTOGRAPHY OF TENSILE , FATIGUE FRACTURED SAMPLES
Objective:
1. Microstructure of sample in SE and BSE mode

2. Chemical composition of the sample in EDS mode
3. Fractography of tensile and fatigue fractured sample
Methodology:
Introduction:
Scanning Electron Microscopy (SEM)
Scanning electron microscopy (SEM) gives information about the crystal structure, the
chemical composition, and the topography of a sample. In scanning electron microscopy,
similar to X-Ray diffraction, collisions between an incident beam and the sample serve as the
primary function of image production. Whereby the incident beams must follow certain
criterion in order to be productive in x-ray diffraction, the different forms of collisions in
scanning electron microscopy are all useful in providing information. The collisions in SEM
determine what information is generated. Collisions of the incident beam and the sample
atom’s electrons give off secondary electrons, which creates an image displaying the
topography of the surface. Alternatively, collisions between the incident beam and the nucleus
of the sample atom gives off backscattered electrons, where collection creates an image using
contrast to distinguish areas of varying chemical composition. When the incident electrons
impinge on the surface of the sample, auger electrons and x-rays may also be produced, also
important in compositional analysis.
To generate electrons, a SEM passes a current through a filament producing an electron cloud.
A cathode and anode are then used to send the electron towards the specimen, completing the
system called an electron gun. The beam of electrons is then focused on the specimen using an
electromagnetic lens. Wires are coiled around an iron core cylinder that creates a magnetic
field after application of a current. This wire and core system makes up the lens. The SEM
column has two lenses, the condenser lens that determines the size of the beam and the
objective lens that focuses the beam on a 2 spot on the sample. The electrons that are given off
are picked up by various detectors included in the SEM, as seen in Figure 6.1. Figure 6.2
demonstrate the schematic of the basic construction of SEM. The secondary electron detector
utilizes a positive bias in order to attract these electrons due to their low energy. The electrons
then strike the scintillator on the detector, producing light that is then amplified with a
photomultiplier into a signal. The back scattered electron detector is a semiconductor detector
arranged around the objective lens. Lastly, the x-ray detector, not built into the SEM column,
the photons are collected according to their energy and used to determine chemical
composition. When a high energy incident electron collides with an inner shell electron, it can
cause the electron to eject, leading to the generation of x-rays. The emitted signals are captured
by the detectors and analyzed as part of electron dispersive spectroscopy (EDS). The energy of
the x-ray photon emitted is specific to the element from which it came, the higher the atomic
number the higher the respective energy. The intensity of the emission of the x-rays is
proportional to the concentration of the element. EDS quantification is done through
𝑵
comparison against a standard with a known concentration 𝑪𝒔𝒂𝒎𝒑𝒍𝒆 = 𝑵 𝒔𝒂𝒎𝒑𝒍𝒆 ∗ 𝑪𝒔𝒕𝒂𝒏𝒅𝒂𝒓𝒅
𝒔𝒕𝒂𝒏𝒅𝒂𝒓𝒅
(where C is weight concentration and N is the number of counts of an element). In order to
produce a more accurate quantification, three correction factors are applied. First, the atomic
number correction (Z) limits the effect of backscattered electrons that do not produce x-rays
and the loss of energy due to inelastic scattering. Secondly, the absorption correction (A)
accounts for the x-rays that are absorbed as they travel to the detector due to the amount of
matter that they must travel through. Lastly, the fluorescence effect (F) corrects for the
characteristic electrons that are emitted due to the ionization of the inner atomic shells.
𝑵
𝑪𝒔𝒂𝒎𝒑𝒍𝒆 = (𝒁𝑨𝑭) ∗ 𝑵 𝒔𝒂𝒎𝒑𝒍𝒆 ∗ 𝑪𝒔𝒕𝒂𝒏𝒅𝒂𝒓𝒅.
𝒔𝒕𝒂𝒏𝒅𝒂𝒓𝒅
Figure 6.1. SEM Chamber
Figure 6.2. Basic construction of SEM

Description of Components
1. Electron Beam: It has two variables i.e. energy and current. The voltage is variable from
about 1 - 60keV and the current from 1e-7 to 1e-12 A. These values are specific to the
instrument model.
2. Electron Gun: It is used to produce fine electron beam (and is also called as electron
probe). Several different types of electron guns used are:
a. TE (Thermionic- Emission) gun

b. FE (Field- Emission) gun
c. SE (Schottky- Emission) gun
TE (Thermionic- Emission) gun (Figure 6.3)
• A thin tungsten wire filament acts as cathode to generate thermo electrons by heating
the filament at 2800K.
• A positive voltage of about 1 to 30 KV is applied to the metal plate acting as anode, in
order to collect these thermo electrons.
• By applying negative voltage to the Wehnelt electrode placed between the anode and
the cathode, current of the electron beam is adjusted. This electrode also helps in
focusing the electron beam.
• Thinnest point of beam known as cross-over (15-20μm Diameter), regarded as actual
electron source.
• LaB6 crystal is used as a cathode. It used to reduce the spot size. It requires high vacuum
due to its higher activity.
Figure 6.3. Construction of TE gun
FE (Field- Emission) gun (Figure 6.4)
• Provides high resolution.

• Works on field-emission effect when high electric field is applied to the metal surface.
• A thin tungsten wire act as cathode wielded to the tungsten single crystal whose tip is
curved with the radius of about 100nm, and is known as emitter.
• Electrons are emitted from emitter through tunnelling effect when positive voltage is
applied to the extracting electrode.
• Hole is created in the extracting electrode to allow emitted electrons to flow through it.
Then electron beam containing some energy is obtained by applying voltage to the
accelerating electrode present beneath the extracting electrode.
• In FE gun energy spread is less because no heating is required and also electron beam
diameter is 5-10nm.
• Requires ultra-high vacuum of the order of 10-8 Pa.
Figure 6.4. Construction of FE gun
SE (Schottky- Emission) gun (Figure 6.5)
• Works on Schottky emission effect when high electric field is applied to heated metal
surface.
• A tungsten single crystal (tip radius – few hundred nm) coated with ZrO acts as cathode.
• ZrO coating reduces the work function to enhance the emission current at low cathode
temperature.
• Thermo electrons are shielded from emitter by applying negative voltage to the
suppressor electrode.
• Advantage: electron beam current is highly stable because emitter is placed in ultra high
vacuum of the order of 10-7 Pa.
• Produces larger probe current.
Figure 6.5. Construction of SE gun

Lenses
To produce finest beam of electron with desired crossover diameter, two- level lens
system, i.e., condenser and objective lens, made of metal cylinders with cylindrical
hole, operating in vacuum is used. These lenses are located beneath the electron gun.
Magnetic field is generated in the inner part of the lenses to focus or de-focus the beam.
Figure 6.6. Formation of electron probe by lenses
Role of condenser lens:
Condenser lens affects the probe size. If it is strengthened then probe size is narrowed with a
smaller ratio of b/a, whereas if it is weakened then probe size is broadened. C1 and C2 lenses
control the beam current by varying size and intensity of beam spot. Aperture is formed by
making a small hole in the metal placed between the two condenser lenses and the objective
lens to allow the beam to pass through it and reach the objective. Resolution is dependent upon
aperture as it controls the spot size.
Role of objective lens:
It is used for focusing and determines the final diameter of probe.
Scanning Coils-
These coils deflect the beam in X or Y directions in order to scan the sample surface in a raster
pattern.
Sample Stage-
It is a motorized plate which has movement in three directions X, Y and Z controlled by feeding
value in the software. The samples are supported on it and move smoothly in the required
direction. X and Y, the two horizontal movement are used to change the field of view whereas
Z, the vertical movement is required for image resolution as well as depth of focus. Along with
these movements rotation and tilting are also possible. Also, stage movement can be controlled
manually through mouse in the user interface of the software.
Detector–
Characteristics of sample are measured at different beam position to form image. Secondary
electrons emitted from the sample are measured using secondary electron detector.
• Secondary Electron Detector: It includes a Scintillator coating at the detector tip and high
positive voltage of 10 kV is applied to it. The secondary electrons emitted from the
specimen get magnetized towards this positive voltage, also this secondary electron
collection is supported by supplementary electrode (the collector) placed before scintillator
by applying few volts to this collector. When they hit the scintillator light is produced which
is guided to PMT (Photo multiplier tube) through light guide. Then light is converted to
electrons which are amplified as electric signal. This detector was fabricated by Everhart
and Thornley, and therefore named as ET detector. For higher resolution in some SEM TTL
(Through The Lens) detectors are used which consists of secondary electron detector above
the objective lens.
Figure 6.7. Construction of secondary electron detector
Display Unit and Recording system-
The output in the form of amplified electronic signal is send to the display unit. To form SEM
image, scanning is synchronized with electron beam scan and brightness (which depends upon
number of secondary electrons emitted) on the display unit. Originally, CRT (Cathode Ray
Tube) was used as a display unit but these days it is replaced by LCD (Liquid - Crystal Display).
Usually, very fast scan speed is used while focusing for observation, whereas slow speed is
used for capturing or saving the image.
Vacuum System-
The microscope column and the specimen chamber are kept under high vacuum i.e. 10-3 to 10-
4
Pa. Diffusion pump is used to evacuate these components. For oil-free environment – Turbo
molecular pump is used, for FE-SEM – sputter ion pump is used as Fe-SEM requires ultra-high
vacuum conditions.
Principle of SEM image formation-
When an electron beam is incident on the sample then many different types of signals are
generated which are eventually used to observe or analyze morphology/topology of the sample.
SEM is also used for elemental and state analysis. These signals includes: Secondary electrons,
Backscattered electrons, Auger electrons, Cathodoluminescence and X-rays.
Figure 6.8. Emission of various electrons and electromagnetic waves from the specimen
• Interaction of Electrons with Specimen: Electrons entering specimen gets scattered

within it and lose their energy gradually upon getting absorbed within the sample.
Scattering range within specimen depends upon-
▪ Energy of electrons – More Energy More Scattering.
▪ Element’s atomic number (Z) making the sample - More Z Less Scattering.
▪ Density of constituent atoms – More Density less scattering.
Acceleration Voltage effects:
Higher the voltage, higher is the penetration depth of the beam within the sample, thereby
providing the inside information of the specimen. However, it spoils the contrast at the
specimen’s surface due to broadening of the spot size inside the sample. Therefore, lower
acceleration voltages are used to view surface of the samples.
Magnification of SEM –
Magnification is yet another parameter of the performance of SEM. Magnification in a SEM

can vary in the range of around 6 orders of magnitude, or from ~10 - 500,000 times. Unlike the
optical and transmission electron microscopes, magnification in SEM does not depend on
objective lens power. The condenser and objective lenses only focus the beam to a spot, and
do not form image of object. Further, SEM can even work without the condenser and objective
since the electron gun itself generates a highly focused electron beam, but it may not be able
to achieve high resolutions. Like the scanning probe microscopy, magnification in SEM comes
from ratio of the dimensions of raster on specimen and display screen. For a fixed display
screen, reducing the dimensions of raster on object can lead to higher magnifications, and vice
versa. Thus, the magnification can be regulated by the current fed to x, y scanning coils, and
voltage applied on x, y deflector plates. The numerical value of magnification is determined by
𝑳
the ratio of the length of the monitor versus the length of the scan on the sample: 𝑴 = 𝑳𝒎𝒐𝒏 .
𝒔𝒑𝒆𝒄
Depth of Focus –
Sometimes when top side of the specimen is focused the bottom goes out of focus. For SEM
systems this depth of focus depends upon the two variables which are:
a. The aperture size

b. The working distance
When aperture or aperture angle is small, then the depth of focus will be larger. On the other
hand, when the aperture or aperture angle is larger, the depth of focus will be smaller. The
parallel electron probe entering through smaller aperture angle then the image remains focused
even though the focus is varied significantly and when electron probe entering is at an angle
larger than the aperture angle, then image goes out of focus even if the focus is varied slightly,
as shown in Figure 6.9.
Figure 6.9. Relation between the aperture angle of the electron probe and the depth of focus.
Fractography of tensile and fatigue fractured samples
Fracture in engineering alloys can occur by a transgranular (through the grains) or an

intergranular (along the grain boundaries) fracture path. However, regardless of the fracture
path, there are essentially only four principal fracture modes: dimple rupture, cleavage, fatigue,
and decohesive rupture. Each of these modes has a characteristics fracture surface appearance
and a mechanism or mechanisms by which the fracture propagates. In this lab, we will see the
fractography of tensile (dimple rupture) and fatigue fractured samples.
Dimple Rupture (Typical in tensile fractured samples)
When overload is the principal cause of fracture, most common structural alloys fail by a
process known as microvoid coalescence. The microvoids nucleate at regions of localized
strain discontinuity, such as that associated with second phase particles, inclusions, grain
boundaries, and dislocation pile-ups. As the strain in the material increases, the microvoids
grow, coalesce, and eventually form a continuous fracture surface (Figure 6.10). This type of
fracture exhibits numerous cuplike depressions that are the direct result of the microvoid
coalescence. The cuplike depressions are referred to as dimples, and the fracture mode is known
as dimple rupture.
The size of the dimple on a fracture surface is governed by the number and distribution of
microvoids that are nucleated. When the nucleation sites are few and widely spaced, the
microvoids grow to a large size before coalescing and the result is a fracture surface that
contains large dimples. Small dimples are formed when numerous nucleating sites are activated
and adjacent microvoids join (coalesce) before they have an opportunity to grow to a larger
size. Extremely small dimples are often found in oxide dispersion strengthened materials.
Dimple shape is governed by the state of stress within the material as the microvoids form and
coalesce. Fracture under conditions of uniaxial tensile load (Figure 6.10a) results in the
formation of essentially equiaxed dimples bounded by a lip or rim (Fig. 6.11 and 6.12a).
Depending on the microstructure and plasticity of the material, the dimples can exhibit a very
deep, conical shape (Figure 6.12a) or can be quite shallow (Fig. 6.12b).
Figure 6.10. Influence of direction of maximum stress (σmax) on the shapes of dimples
formed by microvoid coalescence. (a) In tension, equiaxed dimples are formed on both
fracture surfaces. (b) In shear, elongated dimples point in opposite directions on matching
fracture surfaces. (c) In tensile tearing, elongated dimples point toward fracture origin on
matching fracture surfaces
Figure 6.11. Intergranular dimple rupture in a steel specimen resulting from microvoid
coalescence at grain boundaries.
Figure 6.12. Different types of dimples formed during microvoid coalescence. (a) Conical
equiaxed dimples in a spring steel specimen. (b) Shallow dimples in a maraging steel
specimen
Fatigue
A fracture that is the result of repetitive or cyclic loading is known as a fatigue fracture. A
fatigue fracture generally occurs in three stages: it initiates during Stage I, propagates for most
of its length during Stage II, and proceeds to catastrophic fracture during Stage III.
Fatigue crack initiation and growth during Stage I occurs principally by slip-plane cracking
due to repetitive reversals of the active slip systems in the metal. Crack growth is strongly
influenced by microstructure and mean stress, and as much as 90% of the fatigue life may be
consumed in initiating a viable fatigue crack. The crack tends to follow crystallographic planes,
but changes direction at discontinuities, such as grain boundaries. At large plastic-strain
amplitudes, fatigue cracks may initiate at grain boundaries. A typical State I fatigue fracture is
shown in Figure 6.13. State I fatigue fracture surfaces are faceted, often resemble cleavage, and
do not exhibit fatigue striations. Stage I fatigue is normally observed on high-cycle low-stress
fractures and is frequently absent in low cycle high-stress fatigue.
Figure 6.13. Stage I fatigue appearance. (a) Cleavage like, crystallographically oriented
State I fatigue fracture in a cast Ni-14Cr-4.5Mo-1Ti-6Al-1.5Fe-2.0(Nb + Ta) alloy. (b) Stair-
step fracture surface indicative of Stage I fatigue fracture in a cast ASTM F75 cobalt-base
alloy (R. Abrams, Howmedica, Div. Pfizer Hospital Products Group Inc.)
The largest portion of a fatigue fracture consists of Stage II crack growth, which generally
occurs by transgranular fracture and is more influenced by the magnitude of the alternating
stress than by the mean stress or microstructure. Fatigue fractures generated during Stage II
fatigue usually exhibit crack-arrest marks known as fatigue striations (Figure 6.14), which are
a visual record of the position of the fatigue crack front during crack propagation through the
material.
Figure 6.14. High-magnification views of fatigue striations. (a) Striations (arrow) on the
fracture surface of an austenitic stainless steel. (C.R. Brooks and A. Choudhury, University of
Tennessee). (b) Fatigue striations on the facets of tantalum grains in the heat-affected zone of
a weldment. (M.E. Blum, FMC Corporation)
Stage III is the terminal propagation phase of a fatigue crack in which the striation-forming
mode is progressively displaced by the static fracture modes, such as dimple rupture or
cleavage. The rate of crack growth increases during Stage III until the fatigue crack becomes
unstable and the part fails. Because the crack propagation is increasingly dominated by the
static fracture modes, Stage III fatigue is sensitive to both microstructure and mean stress.
To Report:
(a) SE and BSE images of the given samples. Compare SEM and
optical microscopy and compare SE and BSE modes.
(b) EDS map and composition of the given samples. Comment on the
accuracy of the EDS technique for measuring composition.
(c) Fractographs at various magnification of the tensile-fractured
sample and fatigue-fractured sample. Comment on the type of
fracture.
EXPERIMENT 7
(i) WETTABILITY/CONTACT ANGLE MEASUREMENT

(ii) OPTICAL MICROSTRUCTURE EXAMINATION AFTER ARC WELDING AND
HARDNESS MEASUREMENT
Objective
1. To explore the concepts of surface free energy, adhesion and wetting by measuring the
contact angle of a series of liquids on a polytetrafluoroethylene (teflon) substrate.
2. To create a Zisman Plot from a series of contact angle measurements to determine the
surface tension of polytetrafluoroethylene (teflon).
3. To determine the macrostructure and microstructure characteristics related to arc
welding on mild steel
4. To measure the hardness on the three distinguished zones of arc welding structure
Methodology:
Introduction:
Wettability/contact angle measurement
The interaction between a liquid and a solid involves three interfaces: the solid-liquid
interface, the liquid-vapor interface, and the solid-vapor interface. Each of these interfaces
has an associated surface tension, γ, which represents the energy required to create a unit area
of that particular interface.
Figure 7.1. Diagram of the contact angle
The angle between a liquid drop and a solid surface, Young’s contact angle, is related to the
surface tensions of the three interfaces according to the relationship:
cos 𝜃𝑦 = (𝛾𝑆𝑜𝑙𝑖𝑑−𝑉𝑎𝑝𝑜𝑟 − 𝛾𝑆𝑜𝑙𝑖𝑑−𝐿𝑖𝑞𝑢𝑖𝑑 )/𝛾𝐿𝑖𝑞𝑢𝑖𝑑−𝑉𝑎𝑝𝑜𝑟 (7.1)
The magnitude of Young’s contact angle is a result of energy minimization. If the liquid-
vapor surface tension is smaller than the solid-vapor surface tension (𝛾𝐿𝑉 < 𝛾𝑆𝑉 ), the liquid-
solid interface will increase to minimize energy. As the drop wets the surface, the contact
angle approaches zero. The critical surface tension of a material, 𝛾𝑐 , is a measure of the
surface’s wettability and it is proportional to the surface free energy of the material. A liquid
with a surface tension less than or equal to the critical surface tension of a particular material
will “wet” that surface, i.e. the contact angle will be less than or equal to 90°. A material’s
critical 1surface tension can be determined from a Zisman Plot, which measures variation in
Young’s contact angle as a function of the surface tension of a series of liquids. Zisman
noticed empirically that a plot of cos(θ) versus 𝛾𝐿𝑉 is often linear. The value for which cos(θ)
extrapolates to 1 is termed the critical surface tension.
The Microstructure and Hardness of Arc Welding on Mild Steel
Welding is one of the fabrication processes where two pieces of metal can be joined together
through the use of extreme heat and sometimes the addition of other metals or gaseous
materials also can cause the metallic structures of the two pieces to join together as one. There
are a number of different welding methods, including spot welding, metal inert gas (MIG) ,
and tungsten inert gas which are the forms of gas metal arc welding, arc welding and gas
welding. Welding can also be done underwater. Welding is gaining popularity from time-to-
time because of some few reasons such as it is relatively inexpensive and economical.
Fusion welding processes, such as gas welding, arc welding and gas metal arc welding are
commonly used in most industries. Gas welding is a welding process that melts and joins
metals by heating them with a flame that is caused by a reaction of fuel gas and oxygen and
the metals are constantly heated above their melting point. With this, both metals will
effectively become one piece of metal. The examples for gas metal arc welding are metal inert
gas (MIG) and tungsten inert gas.
Arc welding is a type of welding process using an electric arc to create heat to melt and join
metals (as shown in Figure 7.2). Direct (DC) or alternating (AC) currents are either used to
create an electric arc between a consumable or non-consumable electrode and the base
material. After the welding process is done, there are typical fusion weld joints that consist of
several zones: (i)fusion or weld zone, (ii) weld interface, (iii) heat affected zone (HAZ) and
(iv) unaffected base metal. The fusion or weld zone consists of a mixture of filler metal and
base metal that have melted completely. This zone is distinguished by a high degree of
homogeneity among the component metals that have been melted during welding.
The second zone, weld zone, is a narrow boundary that separates the fusion zone from HAZ.
This consists of a thin band of base metal that was melted or partially melted (localized melting
within the grains) during welding but then immediately solidified before any mixing with the
metal in the fusion zone. The heat affected zone (HAZ) is a non-melted area of metal that has
changed in material properties due to high temperatures exposures. These changes in material
properties are commonly caused by welding or high-heat cutting. The amount of change
depends on factors such as amount of heat input and peat temperature reached, distance from
fusion zone, length of time, cooling rate and the metal’s thermal properties. Failure often
occurs in the HAZ region as it is often weaker than the fusion or base metals. The unaffected
base metal is a region where they are far enough from the fusion zone and no metallurgical
change has occurred.
Figure 7.2. Basics of arc welding process
To Report:
(a) Contact angle of the given materials. Comment on factors

affecting contact angle
(b) Zisman plot
(c) Hardness variation across the Weld zone. Demarcate the
important zones in welding. Comment on microstructural
transformations during welding

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MSE 251

Physical Metallurgy and Materials Characterization Lab

Day Name Email Contact Experiment No.

1 Amit Kumar Yadav amitky21@ 7488347093 6 (SEM)

Experiments for Set-1

Experiments for Set-2

A well prepared metallographic specimen is:

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

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

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

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

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

1. Metallographic sample preparation

• Mounting of a given sample

Brief description about iron carbon diagram:

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

Figure 1.1: Phase diagram of Fe-C system

1. Metallographic sample preparation

• Mounting of a given sample

Read: Physical Metallurgy by V. Raghvan and

Figure 2.1: Phase diagram of Cu-Zn system

1. Draw the microstructures and label.

(i) HEAT TREATMENT OF STEEL – MICROSTRUCTURE EXAMINATION AND

Material: Medium carbon steel

• 2 samples post annealing

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

Brief description about iron carbon diagram:

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

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

1. Typical Microstructures Observed label the various features

Hardenability – Jominy end quench test

• Place a Jominy specimen into the furnace set at 950° C

Carburization - decarburization of steel and measurement of case depth

Material: 0.8% carbon steel

Hardenability – Jominy end quench test

Knowledge about the hardenability of steels is necessary to be able to select the

Carburization - decarburization of steel and measurement of case depth

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

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

Cs Figure 4.1. Concentration

0 Depth below surface x

It is not possible to cite particular recrystallization temperatures, since recrystallization depends

Grain Growth or Coalescence

A complete analysis of grain-boundary migration is not within the scope of engineering

The Cold-work-Anneal Cycle

Grain Size Measurement by Quantitative Metallography:

(i) SAMPLE PREPARATION AND DEMONSTRATION OF SCANNING ELECTRON

1. Microstructure of sample in SE and BSE mode

Scanning Electron Microscopy (SEM)

Figure 6.1. SEM Chamber

Figure 6.2. Basic construction of SEM

a. TE (Thermionic- Emission) gun

TE (Thermionic- Emission) gun (Figure 6.3)

Figure 6.3. Construction of TE gun

FE (Field- Emission) gun (Figure 6.4)

• Provides high resolution.

Figure 6.4. Construction of FE gun

SE (Schottky- Emission) gun (Figure 6.5)

Figure 6.5. Construction of SE gun

Figure 6.6. Formation of electron probe by lenses

Role of condenser lens:

Role of objective lens:

It is used for focusing and determines the final diameter of probe.

Figure 6.7. Construction of secondary electron detector