Metallurgy Lab.

Materials Science-MECH 2006Y

UNIVERSITY OF MAURITIUS
FACULTY OF ENGINEERING
MECHANICAL AND PRODUCTION ENGINEERING DEPARTMENT

METALLURGY LAB.
MATERIALS SCIENCE MODULE- MECH 2006Y
Prepared by S. Venkannah

METALLOGRAPHY:
Metallography is the study of metals by optical and electron microscopes. Structures which are
coarse enough to be discernible by the naked eye or under low magnifications are termed
macrostructures. Useful information can often be gained by examination with the naked eye of
the surface of metal objects or polished and etched sections.

Those which require high magnification to be visible are termed microstructures. Microscopes
are required for the examination of the microstructure of the metals. Optical microscopes are
used for resolutions down to roughly the wavelength of light (about half a micron) and electron
microscope are used for detail below this level, down to atomic resolution.

The most commonly used microscope is the conventional light microscope. In principle, optical
microscopes may be used to look through specimens (in transmission) as well as at them (in
reflection). Many materials, however, do not transmit light and so we are restricted to looking
at the surface of the specimens with an optical microscope. Electron microscope can be used in
the transmission e.g. Transmission Electron Microscope (TEM) and to look at the surfaces e.g.
Scanning Electron Microscope (SEM)

Microscopy can give information concerning a materials composition, previous treatment and
properties. Particular features of interest are
(I) grain size
(II) phases present
(III) Chemical homogeneity
(IV) distribution of phases
(V) elongated structures formed by plastic deformation

Optical Microscopy:
With optical microscopy, the light microscope is used to study the microstructure; optical
illumination systems are its basic elements. For materials that are opaque to visible light (all
metals, many ceramics and polymers), only the surface is subject to observation, and the light
microscope must be used in a reflective mode. Contrasts in the image produced result from
differences in reflectivity of the various regions of the microstructure.

Careful and meticulous surface preparations are necessary to reveal the important details of the
microstructure. The specimen surface must first be ground and polished to a smooth and mirror
like finish. This is accomplished by using successively finer abrasive papers and powders. The
microstructure is revealed by a surface treatment using an appropriate chemical reagent in a
procedure termed etching. The etching reagents depend on the material used and after etching
the specimen must be washed with alcohol and ether to remove the grease. The atoms at the
grain boundaries are chemically more active, and consequently dissolve more readily than those
within the grains forming small grooves. These grooves become discernible when viewed under
a microscope because they reflect light at an angle different from that of the grains themselves.

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When the microstructure of a two phase alloy is to be examined, an etchant is chosen that
produces a different texture for each phase so that the different phases may be distinguished
from each other.

The maximum possible magnification with an electron microscope is approximately 2000

diameters.

Electron Microscopy:

Transmission Electron Microscopy (TEM):

The image seen with a TEM is formed by an electron beam that passes through the specimen.
Details of the internal microstructural features are accessible to observation; contrasts in the
image are produced by differences in beam scattering or diffraction produced between various
elements of the microstructure or defect.

In the TEM, electrons are focused on an extremely thin foil of the material; the beam of
electrons interacts with imperfections in the material, causing differences in the fraction of
electrons that are transmitted. The transmitted beam is projected onto a fluorescent screen or a
photographic film so that the image may be viewed.

Magnifications approaching 1000000x are possible with TEM. The TEM is used to observe
dislocations.

Scanning Electron Microscopy (SEM):

The surface to be examined is scanned with an electron beam, and the reflected beam of
electrons is collected, then displayed at the same scanning rate on a cathode ray tube. The image
that appears on the screen, which may be photographed, represents the surface features of the
specimen. The surface may or may not be polished and etched, but it must be electrically
conductive; a very thin metallic coating must be applied to non conductive materials.
Magnifications ranging from 10 to in excess of 50 000 diameters and also very great depths of
field are possible.

GRAIN SIZE DETERMINATION:

The grain size of metals are usually expressed as the American Society for Testing and Materials
(ASTM) grain size number. The ASTM has prepared 10 standards comparison charts, all
having different average grain sizes. To each is assigned a grain size number ,n, ranging from 1
to 10, the larger the number, the smaller the grains. The designation is based on the equation,
N = 2n-1
where N is the number of grains in an area of 1 sq. in at 100x magnification. A specimen must
be properly prepared to reveal the grain structure, which is photographed at a magnification of
100x.Thus a steel with N=6 has , on average, 32 grains in an area of 1 sq. in. at 100x. Grain
size is expressed as the grain size number of the chart that most nearly matches the grains in the
micrograph.

Grain size may also be determined using an intercept method described below.
Straight lines all of the same length are drawn through several photomicrographs that
show the grain structure. The grains intersected by each line segment are counted; the line
length is then divided by an average of the number of grains intersected, taken over all the line
segments. The average grain diameter is found by dividing this result by the linear
magnification of the micrographs.
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SPECIMEN PREPARATION FOR OPTICAL MICROSCOPY

The examination of materials by optical microscopy is essential in order to understand the
relationship between properties and microstructure. Metallography is the study of metals by
optical examination. This is most commonly done using a conventional light microscope.
However useful information can be gained by examination with the naked eye of the surface of
metal objects or of polished and etched sections. Structures which are coarse enough to be
discernible be the naked eye are termed macrostructures. Those which require magnification to
be visible are termed microstructures.
Fig 1: Optical Microscope
Fitted with 35mm Camera
and Digital Camera

MICROSTRUCTURES.
The preparation of a specimen to reveal its microstructure involves.
Sawing the section to be examined
Mounting in resins (if sample is too small)
Coarse grinding
Grinding on progressively finer emery paper
Polishing using alumina powder or diamond paste on rotating wheel
Etching in dilute acid (2% Nital for steel)
Washing in Alcohol and drying
Typical magnifications used are between 50x and 1000x

ROUGH PREPARATION.
The specimen is ground on progressively finer SiC waterproof papers from 120 to 1000 grit, to
produce a reasonably flat surface, it is lubricated with water to keep it cool and to remove the
grinding products. If the sample is not flat, it might be necessary to remove some material on
the lathe or grinding machine first. The sample should be moved forward and backward on the
paper until the whole surface is covered with unidirectional scratches. It is then washed with
running water to remove debris associated with the grade of paper used. It is then ground on the
next finer paper such that the scratches produced are at right angles to those formed by the
previous paper. This enables you to easily decide when the scratches from the coarser paper
have been completely removed. This procedure is repeated through the range of papers
available.

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When the specimen has been ground on the final paper, it is generally worthwhile rotating it
through and grinding again with less pressure than before. This technique can decrease the time
required for the next stage, which is polishing. Before polishing, the specimen and your hands
must be washed and dried to remove any SiC particles.

POLISHING
Due to the very small depth of field obtained from an optical microscope it is essential that the
surface is flat, in fact it needs to be optically flat, acting as a perfect mirror. The specimen
therefore has to be polished. This is done using rotating wheels covered with a cloth
impregnated with a very fine abrasive compound. The common compounds used are diamond
and alumina.
Fig 2 : An Automatic
Polishing Machine with Two
Rotating Discs

DIAMOND POLISHING.
The Diamond paste is available in various sizes 25 m, 15 m, 6 m, 1 m, m and if
required, polishing may be started with 25 m. When the surface is of acceptable quality,
polishing is continued with diamond paste of lower sizes. Separate wheels must be used for the
different sizes. Check the appropriateness of diamond paste for the polishing process for a
particular material. Other Grinding paste are available.

In most cases two polishing should be sufficient i.e. the 6m and the 1m . Two separate
wheels are used, the first with 6m diamond paste and the second 1 m diamond paste. Both
are lubricated with an organic liquid and water must not come into contact with these polishing
wheels. The 6 m diamond wheel is used first. The specimen is pressed down onto the
lubricated rotating wheel. It is important not to hold the specimen in one orientation for an
extended time as it will cause dragging of some microstructural components. For example,
small spherical particles can develop tail rather like a comet. To avoid this, the specimen is
oscillated about its vertical axis continuously. After 20-30 seconds the specimen is removed and
rotated through 900 in the hand, placed back on the wheel and then again oscillated. This
process is continued until the fine scratches from the final paper have been removed.

The specimen and your hands, particularly finger nails, should be thoroughly washed to remove
all traces of lubricant and the 6 m diamond. The specimen should be rinsed in alcohol and
dried. The above technique is repeated using the 1 m diamond wheel. After polishing on this
wheel, the surface should be optically flat, you should be able to use it as a mirror. With many
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specimens the 1 m diamond finish will be adequate. On occasions where it is not possible, the
specimen is further polished on an alumina wheel lubricated with water or diamond wheel with
finer abrasives.

EXAMINATION.

Fig 3: Microstructure of part of a laser Fig 4 : Microstructure of a laser weld bead in

weld bead in brass (Original mag X100) mild steel sheet

Specimens should always be examined in the as polished condition to assess the quality of
polishing and to observe any features showing contrast. After examination and noting any
features, the specimen should be etched to develop additional contrast to reveal the
microstructure.

For mild steels, high Carbon steel in part (a) and b (3), the specimen must be etched for about
10-15 seconds in Nital. For high carbon steel in part b (1) and b (2), the specimen must be
etched for about 5 seconds. Analyse the specimen under the microscope and etch for a few
more seconds if required.
(For other alloys, different etching reagents may be required)

MOUNTING.
With very small or irregularly shaped specimens it is generally more convenient to mount them
in a resin. Bakelite is commonly used. Also, more than one specimen from a single component
can be mounted and therefore polished at the same time. Never mount dissimilar metals in the
same mount.

A further advantage of mounting is that the edges of the specimen will be reasonably well
polished and not bevelled by the preparation process. In certain instances the very edge of the
specimen is most important. In these circumstances the specimen would be electroplated with
nickel before mounting. Any slight degradation will then take place on the nickel coating and
not the specimen.

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Metallurgy Lab. Materials Science-MECH 2006Y
Fig 5: A Hot Mounting Press

ASSIGNMENT.

(If in doubt please contact the technician or your lecturer)

Please be careful while using the equipment in the lab. Switch off all equipment and tidy the
room before you leave.
Lecturer : Mr. S. Venkannah Tel: Ext 1712 email : sv@uom.ac.mu
Chief Tech: Mr Choo Ping Kwan (Metallurgy Lab.)
Technician : Messrs. Banji Soni & Seetohul (Metallurgy Lab.)

Make sure that you note all your observations and readings as you will be using the same
specimens for all the tests. Each group will be provided with two different steel specimens
depending on availability most probably a mild steel (up to 0.3 %C) and a tool steel (approx.
0.87 % C) specimen.

(a) You will be required to prepare the specimens for macrostructural and microstructural
analysis and sketch the grain structure. Perform (note the results) some micro hardness tests at
various locations on the specimen.

(b) The properties of materials depend on the type, size, distribution and amount of the different
phases present. By the proper heat treatment process, the properties of some materials can
be changed. With reference to steel, briefly explain what you understand by (i) Hardening,
(ii) Tempering (iii) Annealing and (iv) Normalising.

1. You will be required to harden the 2 specimens. Use the Iron-Iron Carbide Phase
Equilibrium Diagram, determine the hardening temperature for each specimen. Contact the
Technician and heat the specimen in the furnace. Allow the specimen/s to soak in the
furnace for some time and then quickly remove the specimen/s and quench it/them in oil or
water.
Repeat step (a) for the microstructural analysis and hardness tests.

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Metallurgy Lab. Materials Science-MECH 2006Y
2. In many cases some materials are too hard for any practical applications. The specimens
can be tempered to relieve some hardness at the expense of hardness and tensile strength.
Using the Iron-Iron Carbide Phase Equilibrium Diagram, select a tempering temperature
and perform a tempering.
Repeat step (a) for the microstructural analysis and hardness tests.

3. The original microstructure and properties of the specimens can be restored by annealing.
With reference to the Iron-Iron Carbide Phase Equilibrium Diagram determine the
annealing temperature for each specimen. Contact the Technician and heat the specimen in
the furnace to the required temperature. Allow the specimen/s to soak at that temperature
for some time. Then cool the specimen very slowly to room temperature.
Repeat step (a) for the microstructural analysis and hardness tests.

Comment on the different results obtained.

Iron-Iron Carbide Phase Equilibrium Diagram (Reproduced from Engineering Metallurgy

Pt. I by Higgins.
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WELDING METALLURGY:
Welding is a joining process that produces coalescence of materials by heating them to the
welding temperature with or without the application the application of pressure or by the
application of pressure alone, and with or without the use of filler metal. The weldability is
defined as the capacity of materials to be welded under the imposed fabrication conditions into
a specific, suitably designed structure and to perform satisfactorily in the intended service.

Although the composition plays a dominant part in determining the weldability of a metal, other
factors, including design, section size, service conditions, etc., influence the economical joining
of metals by welding. The plain carbon steels containing less than 0.3% carbon have excellent
weldability and are the most important source of material for welded construction. High carbon
steels require special techniques, such as preheating and post heating, to prevent cracking and
formation of martensite upon air cooling.

Inherent to the fusion welding process there is the formation of a molten pool directly below
the heat source which contains impurities. The weld shape is influenced by both the resultant
heat and fluid flow. A significant turbulence, hence good mixing, takes place in the molten
pool. The heat input determines the volume of the molten metal and therefore dilution, weld
metal composition, and the thermal condition. The molten metal volume is small compared to
the size of the base metal and its composition is very similar to that of the base metal. There
are very large temperature gradients across the weld. Since the heat source moves, weld
solidification is considered a dynamic process comprising of very localized melting and
freezing.

Weld metal solidification behaviour controls the size and shape of the grains, the extent of
segregation, the distribution of inclusions, the extent of defects such as hot cracking and
porosity, and the properties of weld metal.
Fusion welds consist of three major zones, namely
(a) the fusion zone, (b) the unmelted heat affected
zone (HAZ), and (c) the unaffected base metal. In
alloys there is a fourth region surrounding the weld
pool known as the solid-liquid transition zone
where the metal is partially melted. The heat
affected zone is adjacent to the fusion zone and is
not melted during the welding process. This
region will achieve high temperatures but below
the melting point of the parent metal. As a result
of the high temperatures and different rate of heat
transfer from the fusion zone, microstructural and
properties changes are inevitable. Under certain
conditions the HAZ may consist of a coarse
grained region and a fine grained region.

The figure shows the different regions surrounding

the fusion weld of steel and the typical peak
temperatures achieved in each region.

Figure [Varney]: Diagram showing the peak

temperatures achieved in the different zones in
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fusion welding

The development of weld pool geometry is influenced by the amount of heat transfer from the
heat source to the workpiece, the welding speed, the nature of fluid flow in the weld pool and
the rate at which heat can be removed at the liquid solid interface.

Solidification structure within a weld is mostly dependent on the solidification conditions,

which in turn depend on the welding parameters.

Welding Defects:
Welding defects can be broadly classified in three groups;
1. Dimensional defects
2. Structural defects
3. Property deficiency

Dimensional defects include warpage, incorrect weld size and profile. The second group include defects
such as porosity, non metallic inclusions, incomplete fusion of parent metal, lack of penetration, surface
defects, cracking etc. The resulting weld may have inadequate mechanical properties and corrosion
resistance in comparison to the parent metal which are known as property deficiencies.

Some of the defects that may occur

in a weld are compared with a
desirable weld in the figure on the
left .

At low carbon levels (less than

0.15%C), the steels are non
hardening and weldability is
excellent. Higher carbon steels on
the other hand has poor weldability
because of the likelihood of
formation of martensitic structure
upon weld cooling.

Figure [Davies]: Desirable features and imperfections in a weld

High arc welding speeds were found to introduce defects such as humping, undercutting, lack of side
wall or interpass fusion, poor bead shape, arc instability or porosity. Humping was found to be related to
internal pressure differences which depend on the surface tension. The undercutting is related to wetting
which is affected by the surface tension. The type of flux used, presence of oxide layer on the base
metal, and also presence of oxygen may lead to undercutting and humping.

CRACKING:
Welds may be subjected to hot or cold cracking. Hot cracks develop in a weldment during solidification
whereas cold cracks may occur during or after cooling to room temperature, sometimes with a time
delay.
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Cold cracking may a result of the following factors;

1. Thermal stress (contraction and expansion)
2. Hydrogen (from hydrogen containing welding consumables)
3. A susceptible microstructure

Different manifestations of hot cracking during welding are:

1. Solidification cracking
2. Liquation cracking in the heat affected zone
3. A combination of the above
4. Elevated-temperature (sub-solidus) cracking during heat treatment of welds.

Microcracking may be due to the impingement of martensite plates on one another or on austenite grain
boundaries. Microcracking cannot occur in mild steel since the plate martensite only occurs in high
carbon steel. The formation of microcracks is not dependent on the severity of quench. Microcracks
density increased with austeizing temperature and smaller grain size caused a reduction in the microcrack
density. Microcracking may lead to gross cracking.

Quench cracking is associated with stresses created during the quenching and the strength and toughness
of the structures. Quench cracking normally occurs in martensite because of its high brittleness. The
quench cracking depend on the carbon content which affect the temperature of formation of martensite,
Mf and Ms. The coefficient of expansion of martensite and austenite are different which means that the
amount of expansion is larger if the martensite forms at a lower temperature.

ASSIGNMENT.

(If in doubt please contact the technician or your lecturer)

Please be careful while using the equipment in the lab. Switch off all equipment and tidy the
room before you leave.
Lecturer : Mr. S. Venkannah Tel: Ext 1712, email : sv@uom.ac.mu
Chief Tech: Mr Choo Ping Kwan (Metallurgy Lab.)
Technician : Messrs. Banji Soni & Seetohul (Metallurgy Lab.)

You are provided with coupons of mild steel and you are required to weld two such coupons
together using appropriate welding parameters by each of the following processes;
1. oxy acetylene welding
2. manual metal arc welding
3. Metal Inert Gas welding
4. Tungsten Inert Gas welding

Perform a macrostructural analysis of the weld bead and note your observations. Then
prepare a metallographic as described above and compare the weld bead size and
microstructure. Measure the microhardness of the fusion zone, HAZ and the base metal in
each case.

Observe any defects that may have been formed during welding.

You are required to perform an annealing with the remaining section of each weld after having
prepared the metallographic sample for weld analysis. Repeat the procedure as above and
compare the microstructure obtained with each other and with the corresponding original
weld.

Comment on your results.

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REFERENCE:

Material Science and Engineering- An introduction by W. D. Callister

Engineering Metallurgy- Part I by R. A. Higgins
Materials Science and Engg. By V. Raghavan
Manufacturing Engineering and Technology by S. Kalpakjian
Clark D. S. & Varney W. R., Physical Metallurgy for Engineers
Davies A. C., The Science and Practice of Welding, Volume 2.
David S. A, and Liu C. T., High Power Laser and Arc Welding of Thorium-Doped Iridium
Alloys, Welding Journal, May 1982, pp157s-163s.
Bradstreet B. J., Effect of Surface Tension and Metal Flow on Weld Bead Formation,
Welding Journal, Jul 1968, p314s-322s.
Brooks C.R., Principles of Heat Treatment of Plain Carbon and Low Alloy Steels, 1st Ed., 1999,
ASM international.
American Welding Society, Standard Welding Terms and Definitions, ANSI/AWS A3.0, American
Welding Society, Miami, FL.

All pictures (except diagrams as referenced) obtained from the

Metallurgy Lab of the University of Mauritius

Prepared by S. Venkannah AUG 2006