THANJAVUR – 613 401

SCHOOL OF MECHANICAL ENGINEERING

MEC202 - METALLURGY LABORATORY

 METALLURGY LABORATORY RECORD

BONAFIDE CERTIFICATE

Certified that this is the bonafide record of work done by

Chiranjeevi / Sowbagyavathi................................................................................................

with class roll no ................ who studied in........................................................................

in the Metallurgy laboratory during the year.........................

Staff in charge

UNIVERSITY REG. No.

 MEC202 - METALLURGY LABORATORY
List of Experiments

Cycle – I

1. Metallographic specimen preparation procedure

2. Study of Metallurgical microscope
3. Study of Iron - Iron carbide equilibrium diagram and TTT diagram
4. Micro structure identification of dead mild steel
5. Micro structure identification of mild steel
6. Micro structure identification of medium carbon steel
7. Micro structure identification of tor steel
8. Micro structure identification of grey cast iron
9. Micro structure identification of spheroidal graphite iron
10. Micro structure identification of white cast iron

Cycle – II

11. Study of heat treatment process – Annealing – Normalizing - Hardening

12. Micro structure identification of annealed steel
13. Micro structure identification of normalized steel
14. Micro structure identification of hardened steel
15. Micro structure identification of red brass
16. Micro structure identification of yellow brass
17. Micro structure identification of stainless steel
18. Determination of hardenability – Jominy end quench test
19. Introduction to Non-Destructive Testing (NDT) techniques
20. Introduction to basic powder metallurgy processing technique
 CONTENTS

Expt. Page
Date Name of the Experiment Remarks
No. No.
 CONTENTS

Expt. Page
Date Name of the Experiment Remarks
No. No.
Ex.No.1 Metallographic Specimen Preparation procedure

Aim: To study the procedure for preparation of a specimen for metallographic examination.

Introduction:

Metallographic or microscopy studies consist of the microscopic study of the structural

characteristics of the material or an alloy. The objective of the study is to determine microstructure,
grain size, shape & distribution of various phases & inclusions which have a great effect on the
mechanical properties of material.

The procedure to be followed for the preparation of a specimen is simple & involved with
various steps. The ultimate aim is to produce a flat, scratch free, mirror like surface finish on the
specimen. The steps involved to prepare a metallographic specimen properly are given below.

Fig.1 Steps in involved in specimen preparation

1. SAMPLE SELECTION

Selecting a sample for the micro structural study is an important first step. In general, micro
structure investigations are performed on transverse cross sections of the metal sample. The
sectioning of the test sample is performed carefully to avoid altering or destroying the structure of
the material. If the material is ductile or soft, for example non ferrous metals or alloys & non heat
treated steels, the section is attained by manual hack sawing or power saw operation. If the material
is hard, the section may be obtained by use of an abrasive cut off wheels. This wheel is in a thin
disk of suitable cutting abrasive rotating at high speed. The specimen should be kept cool during
the cutting operation.
2. SURFACE SELECTION

Whenever possible the specimen should be of a size & shape that is convenient to handle.
The specimen surface should be a flat, regular geometry and free from defects. If the specimen is
too little and awkwardly shaped, it will be complicated to clutch the sample during grinding and
polishing. So it is to be mounted to a specific shape by specimen mounting method with the
assistance of thermosetting plastics or cold mounting by polyester resins.

3. GRINDING

The rough grinding of mounted specimen is prepared in a flat belt grinder. The grinding
belt is embedded with abrasive powders which are mounted between wheels. The rough grinding
is performed for removal of all scratches due to hacksaw cutting or cut-off wheel, oxide layers in
specimen and to bring out the surface to be flat.

4.HAND POLISHING or INTERMEDIATE POLISHING

After the previous grinding operation, the specimen is polished on a series of emery sheets
encrusted with finer abrasives of Al2O3 or SiC. The grades of emery sheet in the order of 1/ 0, 2/0,
3/0, & finally 4/0 (i.e. coarse to fine). The intermediate polishing operation using emery paper is
usually done by dry conditions. First the specimen is to be rubbed (polished) in 1/0 grade of emery
in about 50 strokes (Note: the return stroke must be an idle) in a first direction (i.e.0º
orientation). After completion of 50 strokes in 0º, the specimen is to be tilted to 90º + 180º +270º
consecutively and to be polished for 50 strokes in each orientation. The similar procedures of
polishing are to be performed in other emery sheets by order.

5. FINE POLISHING or DISC POLISHING

The final conditions of specimen to the flat and scratch free surface are obtained by disc
polishing machine. Also the fine polishing brings out specimen in to grease, oil and fatty acid free.
The specimen is polished in a rotating wheel covered with soft velvet wet cloth and charged by
fine sized abrasive particles (Al2O3) kept in water. The fine polishing is prepared to bring out the
specimen’s surface alike a mirror finish.

6. ETCHING

The fine polished surface is exposed to chemical action with the application of etching
agent. The applied etching agent reacts with the chemical composition of the phases and shows
the micro structural characteristics as grain boundaries, valleys, dark and polished regions with the
assistance of light rays from microscope sources. The etching time is about 3 to 5 sec. Later, the
specimen is rinsed in water and dried out in air and equipped for micro structural investigations.

Ex.No.2 Study of Metallurgical Microscope

Aim: To study the construction details and working principles of metallurgical microscope

Introduction:

The metallurgical microscope is used for metallographic investigations. Its primary

function is to disclose the details of micro structure of metals. It is also used for the investigation
of defects and structure of a large area as opposed to a microscopic portion of that area. This study
is carried out to expose the solidification of structure, flow lines, segregation, and structural
changes due to welding, general distribution and size of inclusions, porosity, ingot defects and
fabricating defects.

Principle:

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

Fig.1 Working of principle of metallurgical microscope

Construction details:

In contrast with a biological microscope, the metallurgical microscope is different in the

mode by which the specimen is illuminated. Since a metallographic sample is opaque to light, the
sample must be illuminated by reflected light. Metallurgical samples and other not-
transparent subjects can only be observed with the help of reflected light. Since the metallurgical
microscope illuminates the subject from above, parallel to the viewing direction, the examination
light is reflected to the sample through mirrors. In the majority cases the illuminating mirrors are
built-up with the objective lens. The major construction of the metallurgical microscope is given
in Fig.1. It can based on bright-field or dark-field illumination principle.

The prepared surface of the specimen is located perpendicular to the optical axis of the
microscope. It is illuminated through the objective lens by the light source. It is focused by the
condenser lens into a beam that is made approximately parallel to the optical axis of the microscope
by the plane glass reflector. The light is then reflected from the surface of the specimen. This light
reflected from the specimen surface will be magnified in passing through the objective lens and
will persist upward through the plane glass reflector and gets magnified again by the eyepiece.

Fig.2 Construction details of metallurgical microscope

The light is reflected from the surface of the specimen in to objective lens from features
just about normal to the optical axis and away from objective lens from features inclined to the
optical axis. The ultimate image of the specimen, which is formed by the eyepiece, is therefore
bright for all features normal to the optical axis (grain) and dark for inclined features (grain
boundary). In this way, the various micro-structural features of a metallographic specimen such as
grain boundaries that have been etched to create grooves with inclined edges, precipitated particles
and inclusions that have either been etched or polished in such a way that their edges are inclined
are discovered. It is doable to mount a CCD or digital camera above the eyepiece and use the
microscope for photomicrography. The maximum magnification range achieved with optical
microscope is about 2000x. The limitation is due to the wavelength of visible light which limits
the resolution of fine detail in the metallographic specimen. For higher resolutions, electron
microscopes are used. In principle the electron microscope is similar to the light microscope. In
electron microscope, light rays are replaced by a beam of electrons. An electron microscope has a
basic magnification range of 1400 to 32000x, which may be extended to 200000x with accessory
lenses.

Ex.No.3 Study of Iron – Iron Carbide (Fe–Fe3C) Phase Diagram and

TTT diagram
Aim: To study the various phase transformation occurrences in Iron – Iron Carbide (Fe–Fe3C)
system and TTT diagram.

Introduction:

The study of phase relations plays a vital role in the better understanding of the properties
of materials. Much of the information about the control of microstructure or phase structure of a
particular alloy system is properly displayed in what is called a phase diagram, also called as an
equilibrium or constitutional diagram. Phase diagrams are clear maps that furnish the relations
between phases in thermodynamic equilibrium in a system as a function of temperature, pressure
and composition. The Time-Temperature-Transformation (TTT) diagram or S-curve refers to one
particular composition at a time. This diagram is also called as C-curve isothermal transformation
diagram and Bain’s curve. The effect of time and temperature on the microstructure changes of
steel can be shown by TTT diagram.

Iron – Iron Carbide (Fe–Fe3C) Phase Diagram

It is a map of the temperature at which different phase changes occur on heating and cooling
in relation to carbon, and is called Iron – carbon diagram. It shows the types of alloys formed
during cooling, proper heat treatment temperature and compositions of various steels and cast
irons.

Different phases in Fe–Fe3C Phase Diagram

 1.α-ferrite - solid solution of C in BCC Fe
• Stable form of iron at room temperature.
• The maximum solubility of C is 0.022 wt%
• Transforms to FCC γ-austenite at 912 ºC

2.γ-austenite - solid solution of C in FCC Fe

• The maximum solubility of C is 2.14 wt %.
• Transforms to BCC δ-ferrite at 1395 ºC
• Is not stable below the eutectic temperature (727ºC) unless cooled rapidly

3.δ-ferrite solid solution of C in BCC Fe

• The same structure as α-ferrite
• Stable only at high T, above 1394 ºC
• Melts at 1538 ºC

4. Fe3C (Iron carbide or cementite)

• This intermetallic compound is metastable, it remains as a compound indefinitely at
room T, but decomposes (very slowly, within several years) into α-Fe and C (graphite)
at 650 - 700 ºC.

A few observations on Fe–Fe3C system

 C is an interstitial impurity in Fe. It forms a solid solution with α,γ,δ phases of iron.
 Maximum solubility in BCC α-ferrite is limited (max. 0.022 wt% at 727 ºC)
 BCC has relatively small interstitial positions.
 Maximum solubility in FCC austenite is 2.14 wt% at 1147 ºC.
 FCC has larger interstitial positions.

Mechanical properties: Cementite is very hard and brittle - can strengthen steels. Mechanical
properties also depend on the microstructure, that is, how ferrite and cementite are mixed.

Magnetic properties: α -ferrite is magnetic below 768 ºC, austenite is non-magnetic.

Three types of ferrous alloys:

• Iron: less than 0.008 wt % C in α−ferrite at room T

• Steels: 0.008 - 2.14 wt % C (usually < 1 wt % ) α-ferrite + Fe3C at room T
• Cast iron: 2.14 - 6.7 wt % (usually < 4.5 wt %)

Phase compositions of the Iron-Carbon alloys at room temperature

  Hypo-eutectoid steels - (carbon content from 0 to 0.83%) consist of primary pro
eutectoid ferrite and pearlite.
 Eutectoid steel (carbon content 0.83%) entirely consists of pearlite.
 Hyper-eutectoid steels (carbon content from 0.83 to 2.06%) consist of primary (pro
eutectoid) cementite and pearlite.
 Cast irons (carbon content from 2.06% to 4.3%) consist of pro eutectoid cementite ejected
from austenite, pearlite and transformed ledeburite (ledeburite in which austenite
transformed to pearlite).

Various reactions in Iron – Iron Carbide (Fe–Fe3C) Phase Diagram

1. Eutectoid Reaction (Pearlite Formation)

2. Hypo-Eutectoid reaction
3. Hyper-eutectoid reaction

TTT - DIAGRAM
 T (Time) T (Temperature) T (Transformation) diagram is a plot of temperature versus the
logarithm of time for a steel alloy of definite composition. It is used to determine when
transformations begin and end for an isothermal (constant temperature) heat treatment of a
previously austenitized alloy. When austenite is cooled slowly to a temperature below LCT (Lower
Critical Temperature), the structure that is formed is Pearlite. As the cooling rate increases, the
pearlite transformation temperature gets lower. The microstructure of the material is significantly
altered as the cooling rate increases. By heating and cooling a series of samples, the history of the
austenite transformation may be recorded. TTT diagram indicates when a specific transformation
starts and ends and it also shows what percentage of transformation of austenite at a particular
temperature is achieved.
 As indicated when austenite is cooled to temperatures below LCT, it transforms to other
crystal structures due to its unstable nature. A specific cooling rate may be chosen so that the
transformation of austenite can be 50 %, 100 % etc. If the cooling rate is very slow such as
annealing process, the cooling curve passes through the entire transformation area and the end
product of this cooling process becomes 100% Pearlite. In other words, when slow cooling is
applied, all the Austenite will transform to Pearlite. If the cooling curve passes through the middle
of the transformation area, the end product is 50 % Austenite and 50 % Pearlite, which means that
at certain cooling rates we can retain part of the Austenite, without transforming it into Pearlite.
 Upper half of TTT Diagram Lower half of TTT Diagram
(Austenite-Pearlite Transformation Area) (Austenite-Martensite & Bainite Transformation)

If a cooling rate is very high, the cooling curve will remain on the left hand side of the
Transformation Start curve. In this case all Austenite will transform to Martensite. If there is no
interruption in cooling, the end product will be martensite.

1. Magnification
 2. Magnification

Ex.No:
Date: Identification of Metal

.............................................
Aim:
Identification and study of micro structure of the given specimen through metallurgical
microscope.
Apparatus Required:

1. Metallurgical Microscope
2. Emery sheets – Grade 1/0, 2/0, 3/0, & 4/0
3. Disc polishing machine
4. Etching Agent

Etching reagent used:.........................................................

Procedure:
1. The belt grinding is performed on the sample until the surface is flat and free from
scratches.
2. After the previous process the specimen is polished on a series of emery paper containing
successively finer abrasives, with the order of grades 1/ 0, 2/0, 3/0, & 4/0.
3. The specimen is polished in a rotating wheel covered with soft velvet wet cloth and charged
with fine sized abrasive particles (Al2O3) kept in water suspension. The fine polishing is
prepared up to five minutes to bring out the specimen’s surface alike mirror finish. After
the disc polishing the specimen is rinsed with water and dried in air.
 4. Later etching is carried out with proper reagent to make the structural characteristics of the
metal or alloy is noticeable by means of chemical action.
5. The micro structure of the metal is examined with the use of metallurgical microscope and
documented.
Observation:
The observed specimen is.......................................
and its micro structure is as shown at............................ magnifications.

The major properties of the identified metal specimen are:

1.
2.
3.
and has the following applications.
1.
2.
3.

Signature of staff

Ex.No:
Date: Study of heat treatment process - Annealing

Aim:
To study the procedure for heat treatment of steel by annealing process.

Apparatus Required:
1. Mild steel specimen
2. Muffle furnace

Procedure:
1. The micro structure of the given sample is analyzed before heat treatment.
2. The given metal sample is loaded in the muffle furnace.
3. Furnace is switched on and the temperature is allowed to increase.
4. The specimen is heated above upper critical temperature by 50oC for hypo-eutectoid steel
and above lower critical temperature by 50oC for hyper-eutectoid steel.
5. Sufficient time is given based on the thickness of the specimen for obtaining
homogeneous temperature.
6. Then the furnace is switched off and the material is allowed to cool inside the furnace till
room temperature.
 7. The specimen is prepared once again for metallographic examination.

Result:
Thus the annealing process is performed on the steel specimen.

Signature of staff

Ex.No:
Date: Study of heat treatment process - Normalizing

Aim:
To study the procedure for heat treatment of steel by normalizing process.

Apparatus Required:
1. Mild steel specimen
2. Muffle furnace

Procedure:
1. Micro structure of the given sample is analyzed before heat treatment.
2. The given metal sample is loaded in the muffle furnace.
3. Furnace is switched on and the temperature is allowed to increase.
4. The specimen is heated above upper critical temperature by 50oC.
5. Sufficient time is given based on the thickness of the specimen for obtaining
homogeneous temperature.
6. Then the specimen is taken out from the furnace and allowed to cool to in still / forced air
up to room temperature.
7. The specimen is prepared once again for metallographic examination.
Result:
Thus the normalizing process is performed on the steel specimen.

Signature of staff

Ex.No:
Date: Study of heat treatment process – Hardening

Aim:
To study the procedure for heat treatment of steel by hardening process.

Apparatus Required:
1. Mild steel specimen
2. Muffle furnace
3. Quenching medium
4. Hardness testing machine

Procedure:
1. The hardness value of the given sample is measured initially using hardness testing
machine.
2. The given metal sample is loaded in the muffle furnace.
3. Furnace is switched on and the temperature is allowed to increase.
4. The specimen is heated to the temperature to achieve austenite throughout.
5. The sample is retained in the furnace for sufficient time period to obtain homogeneous
temperature.
 6. After reaching of homogeneous temperature, the specimen is taken out from the furnace
and rapidly quenched in the quenching medium.
7. The specimen is taken out from the medium and desiccated properly.
8. After this treatment, the hardness value of the hardened specimen is determined.
9. The hardness values of the specimen after heat treatment is obtained and compared.
Result:

Thus the hardening process is performed on the steel specimen.

Signature of staff

Ex.No:
Date: Determination of hardenability – Jominy End Quench test

Aim:
To conduct the hardenability test in the given specimen.

Apparatus Required:
1. Steel bar - 25.4 mm in diameter and 100 mm length.
2. Muffle furnace
3. Jominy End Quench apparatus
4. Grinding machine
5. Hardness testing machine

Procedure:
1. A steel specimen of 25.4 mm in diameter and 100 mm length is selected for experiment.
2. The steel specimen is austenitized at a prescribed temperature for a prescribed time in the
muffle furnace.
3. After removal from the furnace, it is quickly mounted in a specimen holder of Jominy End
Quench test apparatus.
 4. The bottom end surface of the specimen is quenched by a jet of water of specified flow rate
and temperature.
5. After the piece has cooled to room temperature, flat surface is created using grinding
machine along the specimen length.
6. Few Rockwell hardness measurements are made from the quenched end to other end with
the distance interval of 0.5 mm.
7. A hardenability curve is plotted in the graph sheet with respect to the hardness values
positioned from the quenched end.
8. From graph plot, it is observed that quenched end is cooled most rapidly and exhibits the
maximum hardness; 100% martensite is the product at this position.
9. In addition, when the cooling rate decreases with distance from the quenched end, and the
hardness also decreases.

Result:
The hardenability test for the given specimen is carried out using Jominy End quench
apparatus.
Ex. No. Introduction to Non-Destructive Testing (NDT) techniques
– Study Exercise

Non-destructive testing (NDT) is a widespread defects recognition technique employed in

science and engineering industry to evaluate the properties of a material, component or product
without making damage. This technology also called with several terms such as Nondestructive
examination (NDE), Nondestructive inspection (NDI) and Nondestructive evaluation (NDE).
Since NDT does not eternally alter the object being inspected, it is a precious method that can save
both money and time in product evaluation. The common NDT techniques comprised with
ultrasonic, magnetic-particle, liquid penetrant, radiographic, remote visual inspection (RVI), eddy-
current testing and low coherence interferometry. The NDT techniques are commonly used in
various domains such as Mechanical Engineering, Electrical Engineering, Civil Engineering,
Systems Engineering, Aeronautical Engineering, Medicine, Etc.,
I. Magnetic particle inspection (MPI) method

Magnetic particle Inspection (MPI) is a non-destructive testing (NDT) method for detection
of surface and subsurface discontinuities and cracks in ferromagnetic materials such as iron, nickel,
cobalt, and some of their alloys. The test method establishes a magnetic field into the test piece.
The test piece can be magnetized by direct or indirect magnetization. Direct magnetization is
generated by passing electric current to the test piece and a magnetic field is created in the material.
Indirect magnetization takes place when no electric current is passed through the test piece, but a
magnetic field is applied from an outside source. The magnetic fields of force are perpendicular to
the direction of the electric current which may be either alternating current (AC) or some form of
direct current (DC) or (rectified AC). Fig.1 shows the principles of magnetic particles inspection.

Fig.1. Principles of magnetic particles Inspection

While inspection, the occurrence of surface or subsurface discontinuity in the material

permits the magnetic flux to leak, since air cannot hold up as much magnetic field per unit volume
as metals. Ferrous iron particles are then applied to the test piece surface. The iron particles could
be dry powder or in a wet suspension condition. If an area of flux leakage is to occur, the particles
will be attracted to this area. The particles will build up at the area of leakage and outward
appearance is known as a defect. The indication can then be appraised to conclude reasons for
above defect. Magnetic Particle Inspection (MPI) is the cost-effective and comparatively quicker
non-destructive test method.

Applications of Magnetic particle Inspection

It is extensively employed in Aerospace, automotive, power generation, nuclear,

locomotive, petrochemical industries etc. The most common examples are testing of crank shafts,
cam shafts, connecting rods, engine gears, bearings, bearing caps, engine blocks, motor shafts,
threaded bars, engine bolts, nuts, washers, studs and piping joints ( fabricated joints, welds).
II. Liquid Penetrant Inspection (LPI) method

Dye penetrant inspection (DPI), also known as liquid penetrant inspection (LPI) or
penetrant testing (PT), is a widely applied and low-cost inspection technique used to trace out the
surface defects in all non-porous materials such as metals, plastics, or ceramics. The penetrant may
be applied to all non-ferrous materials and ferrous materials for defect identifications. LPI is
employed to detect defects in casting, forging and welding surface defects such as hairline cracks,
surface porosity, leaks in new products and fatigue cracks on working components. Fig.2
illustrates the steps involved in liquid penetrant inspection.

Some proven applications of liquid penetrant inspection are:

1. Inspection of tools and dies.

2. Inspection of tank vessels, reactors, piping, driers and pumps in chemical, food and paper
industries.
3. Inspection of oil field drilling rigs, drill pipe, castings and drilling equipment.
4. Inspection of diesel locomotive truck and bus parts.
5. Inspection of aircraft engine parts, propellers, wing fittings, castings etc.
Fig.2 Steps involved in liquid penetrant inspection.