Manual As On 10-1-22
Manual As On 10-1-22
(2021-2022 Sem 2)
Instructor
Prof. Kallol Mondal
Materials Science & Engineering
Ph. 6156 Email: kallol@
Lab In-charges:
Mr. G P Bajpai Mr. Ajay Pratap Singh
Materials Science & Engineering Materials Science & Engineering
Ph. 7933; Email: gpbajpai@ Ph. 7933; Email: ajayps@
TAs:
Name Roll number email Student Group
Basant Yadav 20106012 basant20@ A
Bishal Swanrankar 20106014 bishals20@ B
Akhil Kotha 20106004 akhilkotha20@ C
Arjun R 20106010 arjun20@ D
Sandipan Bhattacharyya 20106040 sandipan20@ E
1
General Information
Total Laboratory Turns: 12
1 turn will be reserved for introduction, turn distribution and general
policies.
1 turn will be reserved for Lab Exam/Lab Viva/Lab Quiz. Lab Exam/Lab
Quiz will be either after both sets of experiments or after each set of
experiment.
Viva for each person will be conducted twice in a semester; once before
mid-sem and once after mid-sem. Persons for viva will be selected
randomly on each lab-day. The viva will cover the running experiment or
any experiment that has been done so far.
RULES:
Follow the lab timing. There will be two attendances: Initial attendance (at
sharp 2 PM) to be taken by TAs at the beginning of lab session and final
one after the experiments are over. Late comers will not be allowed to join.
During virtual lab, your video must be on.
Details of experiment will be uploaded beforehand. Students must
carefully go through the shared material before it is performed online.
100% attendance is mandatory. Missing even one turn will lead to fail
grade
2
List of experiments & Lab Schedule
S. Date
Description
No.
1 Lab Introduction, Group Distribution etc 10-01-2022
2 Introduction of Various processes for metallographic sample preparation. 17-01-2022
Optical microscopy of ferrous samples (Steel & Cast Iron) Calculate the 24-01-2022
3
phase fraction in steel and nodules size in Cast Iron
Optical microscopy of nonferrous sample (Brass) Calculate the phase fraction 31-01-2022
4
in Brass
Through X-ray diffraction compare peaks from two samples & find the phase 07-02-2022
5
fraction
6 Annealing, Normalizing and Hardening treatment of Steel 14-02-2022
7 Jominy end quench for hardenability 07-03-2022
Thermal Analysis using DSC to study the phase transformations of Pb-Sn 21-03-2022
8
alloy
9 Recrystallization behavior of cold rolled mild steel. 28-03-2022
RECOMMENDED READING:
The Principles of Metallographic Laboratory Practice by George L. Khel
Physical Metallurgy by V. Raghvan
Engineering Physical Metallurgy by Yu. Lakhtin
Material Science by S P Gupta
3
EXPERIMENT 1
Objective:
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. 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
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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
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.
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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
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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
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
Objective
We shall now consider alloys of Iron and Carbon in our experiment. We will look at the
microstructures 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 hypo eutectoid 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 hypo
eutectoid 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
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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.
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,
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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. Calculate the phase fraction in steel and nodules size in Cast Iron.
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EXPERIMENT 3
Objective:
The metallography of non-ferrous metals are little tricky since they are soft and some of the
cases, special reagents are required for etching.
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.
To Report:
1. Calculate the phase fraction in Brass and grain size in Copper.
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EXPERIMENT No. 4
Objective
To measure the phase fractions of and phases based on the observed intensities of various
XRD peaks of the phases in an - brass sample.
Procedure:
1. Perform XRD measurements on given - brass sample and label all the peaks.
2. Measure intensities of two select peaks of each of the phases.
3. Determine the phase fractions of and from the measured intensities.
Background/Basic Principle:
To Report:
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EXPERIMENT No. 5
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.
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.
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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.
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Experiment 6
HARDENABILITY OF STEEL
Objective:
To study the susceptibility of a steel to hardening by quenching
Background:
Hardenability:
The influence of alloy composition on the ability of a steel alloy to transform to martensite for
a particular quenching treatment is related to a parameter called hardenability. For every steel
alloy there is a specific relationship between the mechanical properties and the cooling rate.
Hardenability is a term that is used to describe the ability of an alloy to be hardened by the
formation of martensite as a result of a given heat treatment. Hardenability is not “hardness,”
which is the resistance to indentation; rather, hardenability is a qualitative measure of the rate
at which hardness drops off with distance into the interior of a specimen as a result of
diminished martensite content. A steel alloy that has a high hardenability is one that hardens,
or forms martensite, not only at the surface, but also to a large degree throughout the entire
interior.
The Jominy End-Quench Test:
One standard procedure that is widely utilized to determine hardenability is the Jominy end-
quench test. With this procedure, except for alloy composition, all factors that may influence
the depth to which a piece hardens (i.e., specimen size and shape and quenching treatment) are
maintained constant. A cylindrical specimen 25.4 mm (1.0 in.) in diameter and 100 mm (4 in.)
long is austenitized at a prescribed temperature for a prescribed time. After removal from the
furnace, it is quickly mounted in a fixture as diagrammed in Figure 6.1a. The lower end is
quenched by a jet of water of specified flow rate and temperature. Thus, the cooling rate is a
maximum at the quenched end and diminishes with position from this point along the length
of the specimen. After the piece has cooled to room temperature, shallow flats 0.4 mm (0.015
in.) deep are ground along the specimen length, and Rockwell hardness measurements are made
for the first 50 mm (2 in.) along each flat (Figure 6.1b); for the first 12.8 mm hardness readings
are taken at 1.6-mm intervals, and for the remaining 38.4 mm every 3.2 mm. A hardenability
curve is produced when hardness is plotted as a function of position from the quenched end.
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Hardenability Curves:
Figure 6 Jominy End Quench Sample (a) with mounting fixture (b) flat ground bad measured hardness from the end
Hardenability
A typical hardenability curve is represented in Figure 6.2. The quenched end is cooled most
rapidly and exhibits the maximum hardness; 100% martensite is the product at this position for
most steels. Cooling rate decreases with distance from the quenched end, and the hardness also
decreases, as indicated in the figure. With diminishing cooling rate more time is allowed for
carbon diffusion and the formation of a greater proportion of the softer pearlite, which may be
mixed with martensite and bainite. Thus, steel that is highly hardenable will retain large
hardness values for relatively long distances; steel with low hardenability will not. Also, each
steel alloy has its own unique hardenability curve.
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Fig.6.2. Typical hardenability
plot of Rockwell C hardness as a
function of distance from the
quenched end
Sometimes, it is convenient to relate hardness to a cooling rate rather than to the location from
the quenched end of a standard Jominy specimen. Cooling rate [taken at 700oC (1300oF)] is
typically shown on the upper horizontal axis of a hardenability diagram; this scale is included
with the hardenability plots presented here. This correlation between position and cooling rate
is the same for plain carbon steels and many alloy steels because the rate of heat transfer is
nearly independent of composition. On occasion, cooling rate or position from the quenched
end is specified in terms of Jominy distance, one Jominy distance unit being 1.6 mm A
correlation may be drawn between position along the Jominy specimen and continuous-cooling
transformations. For example, Figure 6.3 is a continuous-cooling transformation diagram for a
eutectoid iron–carbon alloy onto which are superimposed the cooling curves at four different
Jominy positions, together with the corresponding microstructures that result for each. The
hardenability curve for this alloy is also included. Figure 6.4 shows the hardenability curves
for five different steel alloys all having 0.40 wt% C but differing amounts of other alloying
elements. One specimen is a plain carbon steel (1040); the other four (4140, 4340, 5140, and
8640) are alloy steels. The compositions of the four alloy steels are included in the figure. First,
all five alloys have identical hardnesses at the quenched end (57 HRC); this hardness is a
function of carbon content only, which is the same for all of these alloys.
Probably the most significant feature of these curves is shape, which relates to hardenability.
The hardenability of the plain carbon 1040 steel is low because the hardness drops off
precipitously (to about 30 HRC) after a relatively short Jominy distance (6.4 mm, By way of
contrast, the decreases in hardness for the other four alloy steels are distinctly more gradual.
For example, at a Jominy distance of 50 mm (2 in.), the hardnesses of the 4340 and 8640 alloys
are approximately 50 and 32 HRC, respectively; thus, of these two alloys, the 4340 is more
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hardenable. A water-quenched specimen of the 1040 plain carbon steel would harden only to a
shallow depth below the surface, whereas for the other four alloy steels the high quenched
hardness would persist to a much greater depth.
Severity of quench:
This is a term often used to indicate the rate of cooling; the more rapid the quench, the more
severe is the quench. Of the three most common quenching media i.e.water, oil, and air water
produces the most severe quench, followed by oil, which is more effective than air (Shown
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Fig.6.4. Hardenability curves for
five
different steel alloys, each
containing 0.4 wt% C.
Approximate alloy compositions
(wt%) are as follows: 4340–1.85 Ni,
0.80 Cr, and 0.25 Mo;
4140–1.0 Cr and 0.20 Mo; 8640–
0.55 Ni, 0.50 Cr, and 0.20 Mo;
5140–0.85 Cr; and 1040 is an
unalloyed steel.
The degree of agitation of each medium also influences the rate of heat removal. Increasing the
velocity of the quenching medium across the specimen surface enhances the quenching
effectiveness. Oil quenches are suitable for the heat treating of many alloy steels. In fact, for
higher-carbon steels, a water quench is too severe because cracking and warping may be
produced. Air cooling of austenitized plain carbon steels typically produces an almost
completely pearlitic structure. Severity of the quench of “H” is indicated by heat transfer
equivalent and is given by relation
H = f/k
f- is the heat transfer factor in cal/cm2.s.0C and the K the thermal conductivity in cal/cm.s.0C
The most rapid cooling rate would be with a severity of quench “H” = ∞. Therefore, the
inherent hardenability of a steel can be expressed as the diameter of the bar that will form a
structure with 50% martensite at the centre when quenched at “H” = ∞. This is called Ideal
critical diameter(D1).
The end quench test does not provide directly a single figure indicating the hardenability of the
steel. However, it is possible to calculate the Ideal critical diameter. This may be done by
determining the distance from water quenched end of the end – quench bar at which a structure
consisting of 50 % martensite is attained. The diameter of round bar that will produce the same
structure its centre when quenched with severity of the “H” = ∞ can then be determined by
using fig 6.5
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Fig.6.5 Ideal
Diameter Vs distance
from the quenched
end.
Hardenability of steel:
Equipment and materials:
1. Samples of medium or high carbon steel or alloy steel, machined to the shape show in
fig.9.1.
2. Quenching tank to hold the hot specimen vertically with its lower end above the open
end of vertical water tape.
3. Suitable tongs to hold the hot specimen vertically with its lower end above the open
end of the vertical water pipe.
4. Furnace with temperature controller, for temperature upto 1000oC.
5. Rockwell hardness tester.
6. Microscope.
7. Metallographic grinding and polishing equipment.
Procedure:
1. Heat the sample in the furnace and bring to temperature of 900oC
2. Soak for 15 minutes at the temperature and then remove it to the quenching apparatus.
3. Immediately turn on the water to impinge on the bottom of the hot bar at pre-set flow
rate.
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4. After the entire sample has cooled to room temperature, turn of the water, remove any
scale (Iron Oxide) and grind the sample along the axis to get a flat inside.
5. Measure hardness along the entire length at an interval of 1/8 inch (close to quenched
end) and interval of ¼ inch elsewhere. (as shown in figure 6.7 below).
6. Polish the flat side metallographically, observe the structure and determined the
approximately the distance from the quenched end at which the 50% martensite occurs.
22
EXPERIMENT NO 7
Objective:
Background:
Principle
DSC measures the differences in heat flow into a substance and a reference as
a function of sample temperature while both are subjected to a controlled temperature
program. DSC provides access to accurate thermodynamic data as well as information
regarding reactivity and phase transformations
DSC – types
DSC is the most sophisticated and advanced of the thermal methods. There are two
principal types:
power compensated DSC
heat-flux DSC
Working principle:
Samples are contained in shallow pans, with the aim of making a good thermal contact
between sample, pan and heat flux plate. Symmetrical heating of the cell are needed,
(Sample(S) and Reference(R)), and this can be achieved by constructing the furnace from a
metal of high thermal conductivity – for example, silver. Sample and reference material are
heated by separate heaters in two independent furnaces (Fig. 7.1). The furnaces are imbedded
in a large temperature - controlled heat sink. Sample holders are above the furnaces. Pt
resistance thermometers are imbedded in the furnaces to monitor the temperatures of
sample and reference continuously. There is provision for establishing gas flow through the
cell, to sweep away volatiles, provide the required atmosphere, and to assist in heat transfer.
23
Fig 7.1 Heat flux in DSC
Sample and Reference are heated by a single heater. Differential heat flow into the S
and R pans is monitored by thermocouple. Gas purging is done to avoid oxidation of the
sample.
Enthalpy changes:
The DSC curve of typical metallic glass shows (Fig. 7.2) glass transition and
crystallization. The area under the peak is the enthalpy for crystallization.
In our laboratory, we are using the model PerkinElmer STA 6000 for DSC analysis.
24
Some possible processes giving enthalpy peaks:
Description:
The STA 6000 features the innovative SaTurnA Sensor for high quality, simultaneous
TG and DTA/DSC measurements. This advanced sensor is optimized to achieve flat DTA
baselines and high sensitivity. Because both sample and reference are measured
simultaneously, you can be sure of the integrity of your analysis. The corrosion-resistant, pure
platinum pan holder and reference ring make the instrument suitable for a wide variety of
samples and applications. While many methods call for specific gas flow rates, others may
require a gas switching during the analysis. Either way, the STA 6000 with its built-in mass
flow controller both monitors and controls the purge flow rates.
25
An inside look at the STA 6000:
b
a
Fig. 7.3 Parts of perkinelmer STA 6000, b. Sample Holder and Reference ring
http://www.perkinelmer.com/Content/RelatedMaterials/Brochures/BRO_STA-6000.pdf
1. The small furnace enables accurate temperature control, minimizes the time to achieve
a pure gas environment and allows for the fastest cool down/turnaround times.
2. The SaTurnA sensor measures both the sample and reference temperature. The vertical
loading balance allows for easy operation and sample loading. For unattended
operation, equip your STA 6000 with an optional 45 position autosampler.
3. The rugged alumina furnace is corrosion-resistant allowing for a wide variety of
reactive gases to be used. Its large isothermal zone provides excellent temperature
reproducibility.
4. Experience unsurpassed furnace cool-down speed with the chiller and integral forced
air features and allow your laboratory to process more samples in less time.
5. The balance housing’s thick, stainless steel walls act as a large heat sink, thermally
isolating the balance from the furnace.
6. Balance purge gas maintains a constant environment for the balance and protects it
from the reactive sample purge gas as well as materials evolving from the sample.
7. Sample purge gas: the integrated mass flow controller provides accurate environmental
control and meets the needs of methods that call for specific gas flow rates, or for gas
switching during the analysis.
26
EXPERIMENT No 8
RECRYSTALLIZATION BEHAVIOUR OF COLD ROLLED MILD STEEL
RECOVERY
During recovery, some of the stored internal strain energy is relieved by dislocation climb
and glide (in the absence of an externally applied stress), as a result of enhanced atomic
diffusion at the elevated temperature. This leads to annihilation of some dislocations as well as
re-arrangement of dislocations into lower strain energy configurations (termed as
polygonization).
RECRYSTALLIZATION
Even after recovery is complete, the grains are still in a relatively high strain energy state.
Recrystallization is the formation of a new set of strain-free and equiaxed grains (i.e., having
approximately regular polyhedral shapes) that have low dislocation densities, i.e. 104-105
mm/mm3 as compared to the cold worked state having 109-1010 mm/mm3 dislocation densities.
The driving force for recrystallization is the reduction in the stored stain energy caused due to
formation of new strain-free grains. The new recrystallized grains form as very small nuclei
27
and grow until they completely consume the deformed parent material. Several stages in the
recrystallization and growth process are illustrated in photomicrographs presented in Figures.
Thus, recrystallization of cold-worked metals may be used to refine the grain structure.
Also, during recrystallization, the mechanical properties revert back to their pre-cold
worked values; that is, the metal becomes softer and weaker, but more ductile. Some heat
treatments are deliberately designed to allow recrystallization to occur with these modifications
in the mechanical characteristics.
28
The extent of recrystallization depends on both time and temperature. The time required
for fraction recrystallized follows the Avrami equation (just as in the case of austenite to
pearlite transformation).
The degree (or fraction) of recrystallization increases with time, as may be noted in the
microstructures shown in figures. The recrystallization temperature can be defined as the
temperature at which 50% recrystallization occurs in one hour. The time and temperature
required to recrystallize the material can be given by the equation shown below
1
= ke−Q/RT
𝑡
Plotting ln(1/t) vs 1/T, the effective activation energy Q for recrystallization can be
obtained from the slope of this plot.
The influence of temperature is demonstrated in figure, which plots tensile strength and
ductility (at room temperature) of a brass alloy as a function of the temperature and for a
constant heat treatment time of 1hr. The decrease in tensile strength and the increase in ductility
with temperature correlates with the reduction in the stored strain energy as recrystallization
proceeds. The grain structures found at the various stages of the process are also presented
schematically. From the figure it is evident that recrystallization reaches completion at about
450°C. Typically, for pure metals the recrystallization is generally found to be between 0.4Tm
29
to 0.5Tm (where Tm is the melting point). For some commercial alloys like alloy 718, alloys of
Al-Mg-Sc etc. it may be as high as 0.7Tm.
OBJECTIVE
PROCEDURE
Pre-treatment:
1. Make four sets of mild steel samples: (i) annealed at 800°C for 30min, followed with
(ii) deformation by 80% reduction; the deformed samples are to be annealed at 680°C
for a duration of (iii) 10 min. and (iv) 40 min.
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.
Hardness testing
5. Measure hardness (using the Vickers hardness tester) for all the samples. For each
sample report an average of three hardness values.
RESULTS
QUESTIONS
30
EXPERIMENT No 9
AGE HARDENING BEHAVIOR OF DURALUMIN
DURALUMIN
Duralumin generally consists of alloying elements like copper, manganese, magnesium,
added to Aluminium. In 1903, a researcher Wilma observed that when the Aluminium alloy
(containing 4% copper) is heated above the solvus temperature and quenched, then it can
exhibit “natural” ageing at room temperature or an accelerated ageing if aged “artificially” at
elevated temperature. Al-Cu phase diagram shows, on an Al-Cu phase diagram, the various
steps in the age hardening cycle. The change in the hardness of a material during age hardening
is due to the formation of a sequence of metastable precipitates, which are coherent or semi-
coherent with the matrix. The sequence of various transition phases during precipitation in
Duralumin is GP zones → θ″ → θ′ → θ (CuAl2). During the aging process, initially the
hardness increases and then decreases for transformation of phases from θ′ → θ (CuAl2 –
equilibrium phase) at longer aging times. The decrease in hardness is termed as over-aging.
During this, the average particle size increases, the number of particles decrease and the
interparticle distance increases, which results in the softening of alloys. The unusual feature of
duralumin is the fact, that it can be hardened quite appreciably by quenching from a temperature
slightly below its melting point followed by aging.
31
Figure 9 Al-Cu phase diagram.
OBJECTIVE
PROCEDURE
Hardness Measurement
4. Measure the Hardness using Vickers microhardness tester of all the samples. For each
sample report an average of three hardness values.
32
Results
0
(As quenched)
33
EXPERIMENT No 10
CHANGE OF SURFACE HARDENING BEHAVIOUR BY CARBURISING/
DECARBURIZING OF STEEL
34
DIFFUSION OF CARBON
In a carburizing furnace, steady state is maintained such that a constant carbon potential
is maintained a 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
= (𝐷 )
𝜕𝑡 𝜕𝑥 𝜕𝑥
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 and x is the depth below the surface. If D is taken as constant then,
𝜕𝑐 𝜕2 𝑐
= 𝐷 𝜕𝑥 2
𝜕𝑡
The solution to equation, in the case of a semi-infinite bar (with initial concentration c0) where
the surface concentration is kept constant at Cs gives the concentration, c(x,t) as a function of
time (t) and depth (x):
𝐶(𝑥,𝑡)−𝐶0 𝑥
= [1 − 𝑒𝑟𝑓 2√𝐷𝑡 ]
𝐶𝑠 −𝐶0
Figure 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 in the figure at the surface. Second figure 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 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.
35
C
t3 > t2 > t1
Carbon conc. (wt%)
(a)
(b)
(c)
Figure 10: Microstructure of carburized mild carbon steel sample at the following cross-
sections: (a) surface; (b) sub-surface; (c) core.
OBJECTIVE
36
PROCEDURE
Pre-treatment
1. Take a carbon steel specimen and apply hardening heat treatment to it.
2. Decarburize one eutectoid steel sample at 900°C in air atmosphere for 1hour followed
by air cooling.
Polishing
3. In order to reveal the microstructure, polish and etch the samples using the procedure
described in Experiment 1 in the first set of labs.
4. Etch the samples
QUESTIONS
37
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
38
1
2