Amrita Vishwa Vidyapeetham University

Laboratory Manual
Metallurgy and Material Testing Lab
MEC – 291

Department of Mechanical Engineering

School of Engineering, Bangalore Campus, Bangalore.
 Metallurgy and Material Testing Laboratory – MEC 291

List of Experiments

Exp No. Experiment Title Page No

Introduction 1
1 Study of Metallurgical Microscope 4
2 Preparation of Mounted Samples with the help of Mounting Press 7
3 Preparation of Specimen for Microscopic Examination 9
4 Microstructure of Engineering Materials 13
5 Study of effect of Heat Treatment on Properties of Mild Steel 16
6 Jominy End Quench Test 19
7

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Introduction

Metallurgy is a domain of materials science that studies the physical andchemical behaviour of
metallic elements, their intermetallic compounds, andtheir mixtures, which are called alloys. It is
also the technology of metals, theway in which science is applied to their practical use.

Extraction or Extractive metallurgy is the practice of removing valuable metals from an ore
and refining the extracted raw metals into a purer form. In order to convert a metal oxide or
sulfide to a purer metal, the ore must be reduced physically, chemically, or electrolytically.

Metal is an element that is a good conductor of both electricity and heat. Metals are usually
shiny, malleable and ductile.

Alloysare a mixture or metallicsolid solution composed of two or more elements. An alloy will
contain one or more of the three: a solid solution of the elements; a mixture of metallic phases;
an intermetallic compound with no distinct boundary between the phases. Alloys are used as
their properties are superior to those of the pure component elements.

Heat treatmentof metals can be done to alter the properties of metals like strength, ductility,
toughness, hardness or resistance to corrosion. Common heat treatment processes include
annealing, precipitation strengthening, quenching, and tempering. The annealing process softens
the metal by heating it and then allowing it to cool very slowly, which gets rid of stresses in the
metal and makes the grain structure large and soft-edged so that when the metal is hit or stressed
it dents or perhaps bends, rather than breaking; it is also easier to sand, grind, or cut annealed
metal. Quenching is the process of cooling a high-carbon steel very quickly after you have
heated it, thus "freezing" the steel's molecules in the very hard martensite form, which makes the
metal harder. There is a balance between hardness and toughness in any steel, where the harder it
is, the less tough or impact-resistant it is, and the more impact-resistant it is, the less hard it is.
Tempering relieves stresses in the metal that were caused by the hardening process; tempering
makes the metal less hard while making it better able to sustain impacts without breaking

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Experiment No. 1
Study of Metallurgical Microscope
Aim: - To study the optical metallurgical microscope in detail.

Principle: - A horizontal beam of light from the light source is reflected by means of a plane
glass reflector downwards through the microscope objective on the surface of the specimen some
of this incident light reflected from the specimen surface will be magnified and passing through
the plane glass reflector and magnified again by upper lens system of the eye-piece.

Theory:- The science of metallography is essentially the study of the structural characteristic of
a constitution of a metal/alloy in relation to the physical and mechanical properties.

Metallography consists of macroscopy and microscope. Microscopic examination

involves study of metal either by necked eye or with the aid of low magnification (<10X). This
type of examination reveals some of the important details such as uniformity of structural and
presence of defects.

In a metallurgical polished and flat surface will appear bright light rays falling on rough
surfaces will get reflected out of the objective region and are lost because of these light lose, the
region when viewed with eye-piece appears dark. The type of illumination in which flat and
polished surface appears bright and lustrous rough or curved surface appears dark is called bright
field illumination.

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Instrumentation designed for both visual examination of metal specimens and

photography of metallography. It consists of essentially a metallurgical microscope of intensity
vertical illumination and photographic camera. The pictures of metallurgical structure are called
photomicrographs.

The important terms related to all optical metallurgical microscopes are –

a) Magnifying power of objective: -

It is the ability of a objective to magnify the real object by definite number of times
without the aid of an eye-piece. The is engraved on the objective mount objective are available
with magnifying powers of 5X, 10X, 40X, 50X, 90X,or 100X ( X sign denotes linear
magnification )

b) Magnifying power of eye-piece: -

It is the ability of an eye-piece to magnifying the real object by definite number of turns. This is
engraved on the eye-piece mount. Eye-pieces are available with magnifying powers 5X, 10X,
15X, 20X, or 25X.

The total magnifying obtained by the combination of given eye-piece and objective
depends only on initial magnifying power but also on the distance by which these two are
separated in the microscope. Almost all the objectives are designed for use at a definite tube
length, which is about 250mm. when a given combination of objective and eye-piece is used at
appropriate tube length. The total magnification is the product of their initial magnification.
When the image is projected onto a screen, total magnification is given by M= D* (M1M2)/250x.

c) Numerical aperture of the objects:

It is the right collection or light gathering capacity of an objective. It consists for a given
objective and is a function of a design.

The purpose of object is to objective is to receive and combine into an image large solid
from of light that can normally be received by the objective is influenced by the refractive index
of the medium between the objective and the specimen surface.

In a dry objective that is an objective having air (__=1) between the objective and the
specimen. Light rays upto R1 are received by the objective. If the medium between objective and

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the specimen is oil, such as cedar oil it will be seen from the figure that the light rays R2will bend
whilepassing through oil and now will received by the objective i.e, the greater amount of light is
received by the oil is immersion objectives on the cone of light (m) enteringthe objective and the
refractive index of the medium between the objective and the specimen surface

d) Resolving Power (or) Resolving of an objective: -

It is the ability of an objective to produce sharply defined separate images of closely

spaced details in the object fineness details or limit of resolution is the minimum clearance
distance that can be seen clearly by that objective at some suitable magnification for a narrow
beam of light

Fitness details or resolution limit = λ /NA

Whereλ wave length of illumination

NA  numerical aperture of the objective

Resolving power of resolution is inversely proportional to the fineness detail.

Resolving power of a given microscope can be increased by using visible light beam of
smaller wave length and by oil immersion objective. Desired light can be obtained by inserting
an appropriate filter in the illumination screen.

Uses – The metallurgical microscope is useful in quality control departmentin Industries to

observe & study1) Differential phases 2) Porosity or defects.

All these have a great effect on mechanical properties of material

List of Modern Microscopes

i. Watson Royal Microscope.

ii. Van Lanes Hock Microscope.
iii. Glass led Microscope.
iv. Baker series Microscope.

Result:

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Experiment No – 2

Preparation of Mounted Samples with the help of Mounting Press

Aim:- Preparation of Mounted samples with the help of mountingpress/cold setting resins.

Theory:- Specimens that are very small or awkwardly shaped should bemounted to favorite,
intermediate & final polishing wires small rods steel, sheetmetal specimens, thin sections etc.
must be approximately mounted in a suitablematerial or rigidly damped in a mechanical mount.

Synthetic plastic materials applied in a special mounting press will yield amount of
uniform convenient size (usually 1 inch or 1.25 inch or 1.5 inch. indiameter) for handling in
subsequent polishing operation. These mounts whenproperly made are very resistant to attack by
etching reagent ordinarily used. Themost common thermosetting resin for mounting is
‘Bakelite’. Bakelite moldingpowders are available in variety of colors which simplifies the
identification ofmounted specimen. The specimen & the correct amount of bakelite powder
areavailable in variety of cloves which simplifies the identification of mountedspecimen. The
specimen & the correct amount of bakelite powder are placed inthe cylinder of the mounting
press. The temperature is gradually150° C & amolding pressure of about 4000 PSI is applied
simultaneously since bakelite isset & curved when this temperature is reached, the specimen
mount may beejected from the molding die which is still hot.

Lucite is the most common thermosetting plastic resin for mounting. It iscompletely
transparent when properly mounted. This transparency is useful whenit is polished or when it is
desirable for any other reason to see the entirespecimen in the mould mount unlike the
thermosetting plastic, the thermosettingresin don’t undergo curing at the molding temperature,
rather they set oncooling. The specimen & a proper amount of Lucite powder are placed in
themounting press & are subjected to the same temperature & pressure as forBakelite (150°C,
4000 PSI) After this has been reached, the heating coil isremoved & cooling fins are placed
around the cylinder to cool the mount to about75°C in about 7 minutes while the molding
pressure is maintained. Then themount be rejected from the mould, ejecting the mount while still
hot, or allowing itto cool slowly in the molding cylinder to ordinary temperature before ejection
willcause mount to remain opaque.

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Small specimens may be continently mounted for metallographicpreparation in a

laboratory made damping device. Thin sheet specimens whenmounted in a damping device, are
usually alternated with metal. ‘Filler’ sheetwhich have approximately the same hardness as these
specimens. The use offiller sheet will preserve surface irregularities of the specimen & will
prevent tosome extent the edges of the specimen from becoming rounded during polishing.

Result:

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Experiment No – 3

Preparation of Specimen for Microscopic Examination

Aim: - To prepare the given specimen for metallographic examination.

Principal: - met allograph is the science of studying metallic strictures using optical (or) electron
microscope. Here we confine ourselves to optical metallography. It is possible to determine grain
size and shape and distribution of various phases and inclusion which have a great effect on the
mechanical properties of metal alloy. The microstructure will reveal the mechanical and thermal
treatment of metal alloy and it may be possible to predict the expected behavior under a given set
of condition.

Preparation of specimen:-Success in microscopic examination depends largely upon the care

taken in the preparation of the specimen. The objective is to produce a flat, scratch,-free, mirror-
like surface.

The step required to prepare a specimen for metallographic examination are

1. Selection: - when investigating the prop of a metal/alloy it is essential that the specimen used
must be representative of the whole mass. There are different ways of taking samples from a
sheet, which is illustrated in the figure and if the materials is perfectly uniform each will yield
50% the result when the sheet is rolled. The 50% of the structure revealed is different in each
case. This may lead to wrong interpretation of the grain size and degree of cold work

a) If a failure is to be investigated the sample should be chosen as close as possible to the

area of failure and should be compared with the one taken from the manual selection.
b) In cutting and grinding of specimen the structure of metal/alloy should not be distributed
by excessive pressure or heating.

2. Rough Grinding: -the sample for microscopic examination of metal alloy is cutwith the help of
specimen cutting machine to suitable size, say measuring about 20 x 20mm. the surface of the
specimen is first made flat by means of a file r an a motor driven energy belt. The specimen
should be cooled by dipping in water. Frequently otherwise the stricture of the specimen is likely
to be altered superficially. In all grinding and polishing operation the specimen should be moved
perpendicular to the existing scratches. This will facilitate the removal of the deeper by

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shallower ones. During rough grinding operation the sharp edge and corners are to be leveled to
prevent tearing of emery sheets and polishing clothes in lather operations.

a) Very small specimens are difficult to polish they require mounting in a plastic material
like Bakelite, Luciteetc. Bakelite moulding powder is available in a variety of colors the
specimen and the correct amount of power are placed in the cylinder of the moulding
press.
b) The temperature is gradually raised to 150o c and the moulding pressure of about the 25-
30 MPais applied simultaneously since Bakelite cures at this temp and pressure.

3. Intermediate Polishing: - The specimen is then polishing on a series of a emery paper of

increasing fitness the first paper is1/0 and 2/0,3/0 and finally 4/0 then this intermediate polishing
operation would be completed.

1/0 paper is placed on a glass plate the specimen is held in such a way that the scratches
produced by the belt grinder is perpendicular to the movement of specimen on 1/0 paper under
moderately applied measure the specimen is gently drawn back and forth across the full length of
the paper, until all the deep scratches produced by the belt grinder are removed and a new set of
scratches perpendicular to the earlier once, produced by the 1/0 are formed throughout the face.
The specimen is then polished till the scratches produced by 1/0 are completely removed and a
new set of shallow scratches is formed the procedure is then repeated on 3/0 and 4/0.
4. Final Polishing: - Fine polishing of metallographic specimen is for the purpose of removing
from the surface of the specimen, the fine scratches introduced during the last grinding operation
and for producing a highly polished scratch free mirror like surface. The time consumed and
success of the fine polishing depends largely upon the care that was exercised during the
previous steps.
a) The polishing operation is performed on a rotating wheel. A special polishing cloth is
spread on the wheel on the polishing compound such as alumina or magnesia is
employed. The polishing media is smeared on the cloth and the specimen isheld against
the rotating wheel only a moderate pressure is to be employed here the specimen an be
rotates opposite to the rotation of the wheel
b) When the final polishing is completed the specimen is washed in running water and
swabbed with water wet cotton to remove the last traces of abrasive and finally dried in

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warm stream of air. Polished surface of the specimen should not be touched with figures
which would case staining and eventual uneven attack by the etching regent also, the
prepared surface should not come in contact with foreign objects that may case scratches.
c) After this the specimen should be observed under the microscope certain details can be
observed because of the difference in inherent respectively of the constituent. For
examples dark graphite flakes can be seen in the case gray cast iron. The observation in
stage in recommended for determining the size, shape, and distribution of the graphite.
5. Etching: - The next step is etching specimen is necessary in order to make visible of the
structural characteristic of metal in alloys composed of two or more phases structural component
or revealed are revealed. During etching by a preferential attack or staining of one or more of this
constituent by the reagent, owing to the different in chemical composition of the phases in the
case of pure metals and homogeneous single phase alloys structural contrast is established and
grain boundaries are revealed mainly because of differences in the rate at which the grains are
attacked by the regent a circumstance directly associated with the orientation of the different
grains sections with respect to the plain of the polished surface.
a. The prepared specimen etched or unetched may be temporally preserved in desiccators
with solid desiccants like dehydrate calcium sulphate or anhydrouscalcium or magnesium
chloride.
6. Etching Regents: - The etching regents or etchant to be used depends on the composition of
specimen and structural phases present in it. The list ofetchantis: -
7. Etchingprocedure: - To secure satisfactorily etched surface the etching should be performed as
recommended this involves.

a) The selection of proper etchant.

b) Method of etching.

c) Temperature of which etching is carried out.

d) Approximate time duration of etching.

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It is necessary that the specimensurface to clean to ensure uniform wetting of the surface
by the etchant. Hence before etching wash the specimen surface in warm water swab the surface
with wet cotton and dry in a blast of warm air.

Depending upon the metal/alloy to be etched and the regnant selected, etching time may
vary from few seconds to 30 minutes or longer.

Etching Reagents for Microscopic Examination

Etching reagent Composition Metal & alloys Etching time (sec)

which can be etched

Nitric acid (nital) Cone metric acid Carbon steels and 10-30
cast iron
Picric acid(picral) Picric acid Carbon steel & alloy 15-60
4ccAbsolute ____ steel (etched)
alcohol 96cc pearlite do never
reveal ferrite grains
HC1 +HNO3+H2O Hydrochloric acid 18/8 Stainless steel 15-60
10cc nitric acid 3cc
water 100cc (pickling
rest airier 70/80 cc
Ferric chloride Ferric chloride 10g Copper & __ alloy
cone hydrochloride such as bronzes, high
and 30 cc water 200cc zinc brasses &
aluminum.
NH4OH + H2O2 Ammonium hydroxide Copper and its alloy.
5 parts, water 5 parts
hydrogen peroxide 2
parts
Hydrofluoric acid + Hydrofluoric acid 5cc Aluminum and its 15-60 (use freshly
HNO3 Nitric acid 5cc water alloy. prepared __)
100cc.

Result:

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Experiment No – 4

Microstructure of Engineering Materials

Aim: -To study the microstructure of Engineering Materials (specimen).

Apparatus: - bench grinder, finisherpolish,emery paper, 4/0, 3/0, 2/0, 1/0 double disc polisher,
enchant, microscope, dryer.

Simple producer: - The given specimen is taken and its surface is made flat by using a bench
grinder. After making the surface flat, it is then polished with the help of _______ polisher. After
subjecting it to _______ polisher the specimen was firmly polished with the help of emery paper
of different grades (1/0, 2/0, 3/0, and 4/0). There the specimen was subjected to double disc
polisher where it was polished to a higher degree of fineness, then an etching-reagent-nitol-was
swabbed on the surface of the specimen and was observed under the microscope and the
microstructure was drawn and studied.

Characteristics: -Low carbon steel of 0.05% to 0.3% carbon content are classified into three: -

1. Dead mild steel: - carbon content- 0.05% to 0.15%

It has tensile strength of 390N/mm2 and the hardness of 115 BHN.

2. Mild steel: - carbon content- 0.15% to 0.2%.

It has high tensile strength of 420N/mm2 and the hardness of 125 BHN

3. Mild steel: - carbon content- 0.2% to 0.3%.

a. It has tensile strength of 555N/mm2 and the hardness of 140 BHN

Applications:

1. Dead mild steel: - make steel wire, shells, pipes, and rivets.

2. Mild steel (0.15% to 0.2%): - making composite, sheets, strips for fan blades, forging.

3. Mild steel (0.2% to 0.3%): - making valves, gears, crank shaft, connecting rod etc.

Result: The given specimen was observed under the microscope and its microstructure was
studied and drawn.

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Microstructure Observation Sheet

MATERIAL: ____________________________________________________________

COMPOSITION: ________________________________________________________

_______________________________________________________________________

MICROSCOPE: _____________________________________

MAGNIFICATION: __________________________________

MICROSTRUCTURE WITHOUT ETCHANT:

OBSERVATIONS: _______________________________________________________

_______________________________________________________________________

MICROSTRUCTURE WITH ETCHANT:

ETCHANT USED: ____________________________________

DURATION: _________________________________________

OBSERVATIONS: ______________________________________________________

_______________________________________________________________________

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Microstructure Observation Sheet

MATERIAL: ____________________________________________________________

COMPOSITION: ________________________________________________________

_______________________________________________________________________

MICROSCOPE: _____________________________________

MAGNIFICATION: __________________________________

MICROSTRUCTURE WITHOUT ETCHANT:

OBSERVATIONS: _______________________________________________________

_______________________________________________________________________

MICROSTRUCTURE WITH ETCHANT:

ETCHANT USED: ____________________________________

DURATION: _________________________________________

OBSERVATIONS: ______________________________________________________

_______________________________________________________________________

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Experiment No – 5

Study of effect of Heat Treatment on Properties of Mild Steel

Aim: Study of effect of Annealing, Normalizing and Quenching properties of mild steel.

Equipment used for Heat Treatment:Muffle Furnace

Equipment for checking Hardness afterHeat Treatment: Brinell’s Hardness Tester

Definition: Heat Treatment can be defined as a combination of Heating and Cooling Operations
carried out on a metal or alloy in the solid state so as to produce a Particular Microstructure and
hence the Desired Properties.

Generally the Composition is fixed and the Solidification is also completed the only way
to change the properties is by Heat Treatment.Heat Treatment effectively alters the Size and
Shape of the Grains and also type (SCC, BCC, FCC, HCP etc) and Distribution of grains hence
the PROPERTIES.

Objectives Heat Treatment:

 To improve the Mechanical Properties

 To improve Machinability

 To increase Wear Resistance

 To modify Electrical & Magnetic Properties

 To Refine the Grains

 To produce Hard Surfaces & Soft Inner Core

 To Relieve Internal (Residual) Stress due to Mechanical Working

 To Overcome effects of Strain Hardening & Restore Ductile Property

Various Stages of Heat Treatment Process:

Stage 1: Heating the metal or the alloy to the prescribed temperature

Stage 2: Holding the specimen at that temperature for a known time period (holding time or
soaking time-depends upon the thickness of the specimen)

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Stage 3: Cooling at a rate (Slow or Rapid rate) necessary to obtain a specific microstructure for
the desired properties (Furnace Cooling, Air cooling, Water Cooling, Oil cooling, & Ice cooling)

Theory– Annealing in general, involves heating to sufficient high temperaturesHolding at this

temperature & finally cooling at a very slow rate. Thetemperature to which steel is heating &
holding time are determined byvarious factors such as the chemical composition of the steel, size
& shapeof steel component & final properties desired. Annealing can form either thefinal
treatment or a preparatory step for further treatment. The variouspurposes of this treatment are

 To improve the Mechanical Properties

 To improve Machinability

 To increase Wear Resistance

 To modify Electrical & Magnetic Properties

 To Refine the Grains

 To produce Hard Surfaces & Soft Inner Core

 To Relieve Internal (Residual) Stress due to Mechanical Working

Types of Annealing

1. Full Annealing

2. Isothermal Annealing

3. Diffusion Annealing

4. Partial Annealing

5. Re crystallization Annealing

Normalizing– It is the process of heating steel to about 40° - 50°C aboveupper critical
temperature ( A 3) holding for proper time & then cooling it in airor slightly agitated air to room
temperature or air volume. After normalizingthe resultant microstructure should be pearlitic.
This is particularly importantfor some alloy steels which are air hardened by nature for such
steels, coolingin air don’t lead to normalized structure. Slower cooling rates are read sincethe
temperature involved in this process is more than that for normalizing, thehomogeneity as
austenitic increases & it results in better dispersion. Resultsin enhanced mechanical properties.

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The grain size in finer in normalizedstructure that in annealing grain size of normalized steel is
governed bysection thickness. As cooling rates differ considerably from case to case,there is
variation in grain size of normalizing steel over its cross section.Refinement of grain size is one
of the most important objectives of normalizing& it is to be a great extent due to high
temperature involved in these operationare subjected to a great extent .

Normalizing treatment is frequently applied to steel in order to gainrefinement,

improvement in mach inability & enhanced mechanical propertiessuch as hardness, strength &
toughness.

Quenching:

Quenching (sudden cooling by immersion in water or oil) is the rapid cooling of a work
piece to obtain certain material properties. It prevents low-temperature processes, such as phase
transformations, from occurring by only providing a narrow window of time in which the
reaction is both thermodynamically favorable and kinetically accessible. For instance, it can
reduce crystallinity and thereby increase toughness of both alloys and plastics.

Tabular Column:

Serial No. Heat Treatment Process BHN Remarks

1 Annealing

2 Normalizing

3 Ice Quenching

4 Oil Quenching

5 Water Quenching

* Plot the Bar Chart on the Graph Sheet.

Result:

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Experiment No – 6

Jominy End Quench Test

Aim: To conduct the jominy harden ability test and to utilize the test result to determine harden
ability of steel.

Equipment and Material Required: -

1. Furnace that attains required hardening temperature.

2. Jominy end quench apparatus.

3. Brinell’s hardness testing machine.

4. Proper tongs and hand gloves.

5. Specimen.

Specimen of Furnace Used: -

Power- 2 KW

Voltage- 250 V

Max temperature- 850o C

Definition: - Hardness of a material is defined as the ability of a material to resist plastic

deformation. Whereas Hardenability of materials is its ability to get hardened as a result of
hardening heat treatment.

A steel that has highest hardenability is one that has martensite, not only at the surface
but throughout the entire interior or core of the steel.

The Hardenability of steels depends on

a. Composition of the steel and method of manufacture

b. Quenching medium and the method of quenching

c. Section (thickness) of steel

Working Principle: - The test consistsof heating astandardsteel specimen to a given quenching
temperature for a specific period of time follower by a water, quenching at one end under

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specified conditions. The specimen must be a BS4437 (or) IS: 3848-1966. the quenched
specimen is subjected to hardness test of various parts from the quenched end along the length of
the piece from the quenched end.

Specimen std: - BS 3337 (or) IS 3848-1966

Process parameter

 Water inlet orifice dia 12.5mm

 Free jet height 62.5mm
 Distance between orifice & bottom
 End of steel bar 12.5mm
 Temp of water 21-25° C
 Quenching time 10 min

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Sl No. Distance from Quenched End (mm) BHN

1 5

2 10

3 15

4 20

5 25

6 30

7 35

8 40

9 45

10 50

* Plot the graph of Distance Vs Hardness

Result: - From jominy test the hardening curve for specimen is obtained for different steel,
kinds, and shapes of the curve varies.

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