MME 294

LECTURE-1
METALLOGRAPHY SESSIONAL

COURSE TUTOR:
SUMIT BHOWMICK
LECTURER
DEPT. OF MME, BUET
 BACKGROUND

• The properties of a metal are a direct consequence of the

microstructural features of that metal.

• These structural patterns vary both with the metals

themselves, and with their manufacturing processes.

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 BACKGROUND
• The identification of the microstructural features of a metal is
important.

• The metallurgical microscope is a major tool that is used for

the identification of these features of a material.

• Metallography is the study of the physical structure and

components of metals, typically using microscopy.

• Ceramic and polymeric materials may also be prepared using

metallographic techniques, hence the terms ceramography,
plastography and, collectively, materialography.

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 METALLOGRAPHIC SAMPLE
PREPARATION
• Need for preparation: to produce a distortion-free, polished
surface capable of revealing the true microstructure.

A typical preparation sequence and basic equipment for an

average laboratory would include:

• Selection of the sample

• Sectioning: to produce a manageable size sample
• Rough Grinding: to remove surface deposits or level irregular
surfaces.
• Mounting: to provide a safe means of holding the specimen
and protect its edges from rounding.

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 METALLOGRAPHIC SAMPLE
PREPARATION
• Fine Grinding: to systematically abrade the specimen with a
series of grits of decreasing coarseness.
• Polishing: to remove the remaining scratches and produce the
smooth lustrous surface required for microscopic examination.
• Etching: to develop the microstructure not normally visible in
the as-polished condition. Inclusions and certain types of
defect identification should be performed prior to application
of the etchant.
• Microscopy: to realize the ultimate goal of specimen
preparation to observe, analyse, and record the true
microstructure of the material. Other tests, such as micro
hardness, provide additional information as required by the
authority requesting the services.

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 SELECTION AND IDENTIFICATION
OF SPECIMEN
Only a small piece of material can be placed on the platform of a
metallurgical microscope and only a plane or flat section of it can be
observed under it.

A metallographer should always exercise careful judgement in selecting the

section to be observed.

With respect to purpose of study the metallographic examination may be

divided into three classifications
• Routine studies
• Study of failures
• Research studies

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 SELECTION AND IDENTIFICATION
OF SPECIMEN
Routine Studies:

A large body of metal may not be homogeneous either in

composition or in structure. Specimens from locations that are
most likely to reveal the maximum variations within the
material under study should be chosen. Sometimes more than
one specimen may be necessary to adequately represent the
material.

For example, for the examination of the structure of a casting,

specimens should be taken from the zones wherein maximum
segregation might be expected to occur as well from the zones
where segregation should be at a minimum.

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 SELECTION AND IDENTIFICATION
OF SPECIMEN
Study of Failures:
•For the identification of the causes of premature failures, the test
specimens should be taken as closely as possible to the fracture or to
the initiation of the failure.
• In many cases, specimens should also be taken from a sound area for
a comparison of structure and properties.

Research Studies:
•The nature of the study dictates the location of test specimens,
orientation etc.
•Sampling in such a case is usually more extensive than in routine
examinations.

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 SECTIONING OR CUTTING OF
METALLOGRAPHIC SPECIMENS
• The object of sectioning is to extract a specimen of suitable
size from the parent metal.

• Sectioning can have a drastic effect on subsequent

preparation techniques. On some occasions the damage is
so great that it is impossible to reveal the true structure by
grinding and polishing.

• Heat generated during sectioning has not been dissipated. In

cutting metallographic specimens from the main body of the
material, care must be exercised to ensure that the
structure of the metal is not changed.

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 THE COMMON TECHNIQUES FOR
SECTIONING
A sample for metallographic
examination may be cut
from a larger object with a
hacksaw.

An abrasive cut-off wheel

provides the best method of
removing a sample from an
object. This often produces
a surface ready for fine
grinding.
An Abrasive Cut-off Wheel

• Depending on the material to be cut, wheels of different compositions

may be needed. The hardness and ductility of the material influence the
choice of cut-off wheel.

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 Fault Cause Remedy
Wheel does not • Incorrect abrasive • Use alternative
cut or cutting • Wheel has become abrasive or softer
ceases after a blunted grade of wheel
short time
Wheel wears • Wheel is too soft • Use harder grade of
rapidly wheel
Wheel breaks • Excessive cutting • Reduce cutting
force pressure.
• Sample moved • Clamp sample
during cutting more securely.
• Wheel not clamped • Tighten wheel
securely more securely.

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 SECTIONS OF METALLOGRAPHIC
SAMPLES
• The specimen for microscopic examination
should be in proper orientation.
• For example, if grain flow or distortion is
important, a cross section of the part may not
show the elongated grains; only a slice parallel
to the direction of rolling would adequately
reveal elongated grains from rolling.
• The locations of surfaces examined should
always be given in reporting results and in any
illustrative micrographs.
Longitudinal Longitudinal
Section Section

Transverse Section

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 MOUNTING
• Mounting is an encapsulating process that
facilitates further processing.

The reasons for mounting can be summarised as

follows:
• the specimen is too small or of awkward shape
for ease of handling in subsequent stages of the
preparation.
• to support the outermost edge of the specimens
surface to prevent damage or rounding during
the subsequent grinding/polishing operations.
• the specimen is of delicate nature

Bulk samples usually do not require mounting

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 NECESSITY FOR POLISHING AND
ETCHING
• Metallic objects are opaque to light. These objects are, therefore,
observed under reflected light.

• If the surface of the metallic object is not perfectly flat or scratch-free

light reflected from that surface will not reach the eyes of the observer.

• A cut surface may be considered to be composed of a large number of

very small inclined surfaces. As a result such a surface will not reflect
light to the eyes of the observer.

• That is why the surface of a metallic object has to be made perfectly

flat and scratch-free for observation under a metallurgical microscope.
Such a surface is generally produced by careful grinding or polishing
with consecutively finer abrasives.

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 NECESSITY FOR POLISHING AND
ETCHING
• A perfectly flat surface, on the other hand, reflects all beams incident
on it. A polished surface, therefore, appears bright under a microscope
and thus no useful information can be obtained.
• To reveal the microstructural features of metals and alloys, the
polished surface is usually treated with an etchant.
• An etchant is a very dilute solution of an acid or alkali or salt in alcohol,
water or a suitable solvent
• The phases present in a metallic object vary in composition and energy.
When in contact with an etchant, the essential requirements for the
formation of a cell are satisfied and corrosion occurs. This etchant acts
at varying rates on different parts of the structure depending on local
variations in composition within the material being etched.
• Differential corrosion is a term used to describe this kind of varying
chemical action that creates relief on the surface being etched. This
produces contrast as some of the incident rays are directed in other
directions.

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 MECHANICAL PREPARATION
• Mechanical preparation is the most common method of preparing
metallographic samples for microscopic examination.

• Abrasive particles are used in successively finer steps to remove

material from the surface of the specimen in order to produce in it a
surface that is perfectly flat and scratch-free when viewed under a
microscope.

• According to the roughness of the ground surface the grinding

operation is classified as coarse (or rough) grinding, or as fine
grinding.

• Depending on whether the grinding operation is performed in air or

in a liquid (water, oil, etc) the process is called dry or wet grinding.

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 MECHANICAL PREPARATION
The first step towards obtaining a perfectly flat and scratch-
free surface is to rough grind the face of the specimen on a
grinding wheel.

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 MECHANICAL PREPARATION

• The samples are then ground manually by grinding on a

series of emery papers of progressively finer grade.

• Emery is a natural abrasive containing 55 – 75 per cent Al 2O3

(corundum) the balance is iron oxide (magnetite) and has
Mohs hardness of 8.0.

• The emery papers are made by attaching hard abrasive

particles onto papers by suitable glue.

• In the laboratories these papers are usually laid on a piece of

flat glass and held in wooden frames

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 MECHANICAL PREPARATION
• In some laboratory the paper containing the coarsest paper is designated as
No. 3. Subsequent papers are designated as No. 2, 1, 1/0, 2/0, 3/0 and 4/0.
• Alternatively, no. of Abrasive grains per square inch (e.g. 180, 320,…1500) are
also used.
• Each frame should be reserved for only one grade of abrasive paper, and each
should be isolated from adjacent papers of different grades, by a suitable
distance.
• When all the marks on the surface being polished are running in one direction
and all others have been removed, the operator should clean the specimen
and his hands and then proceed to the next finer paper. During grinding on the
next finer paper, the operator should hold the specimen in such a way that the
new, finer set of scratches will be approximately perpendicular to the existing
set of scratches.

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Appearance of Specimen Surface at Successive Stages of Grinding
 MECHANICAL PREPARATION

• The process is continued until grinding

on the finest paper (the 4/0 step, or
1500) is completed.

• During grinding, the specimen should

not be pressed too hard against the
abrasive paper, because the heat
generated due to friction may change A Modern Wet-grinding Deck

the original structure of the specimen.

• The specimen should be held flat

against the abrasive paper.

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 MECHANICAL PREPARATION
• At this point it should be emphasized that there are no short cuts to
the preparation of a first class specimen.

• It is quite useless to leave noticeable scratches on the surface of a

specimen and hope that these will disappear with polishing or
etching.

• Although considerable time and energy may have been spent

grinding, polishing and etching the surface of a specimen, the failure
to observe simple precautions will result in crisscross lines that will
show up under the microscope, signifying the presence of un-
removed scratches.

• Should this be the case, it will be necessary to go back and start all
over again.

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Criss-cross Lines due to Improper Grinding

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 GENERAL RULES FOR
MECHANICAL PREPARATION
• If a material is prepared for the first time the samples should be
examined after every step under the microscope. This makes it
easier to see when preparation defects occur. (alternative: mirror-
glistening scratches)
• Each set of polishing scratches must be removed completely,
before proceeding to the next finer abrasive. (Rotate 90 degrees to
next stages of polishing)
• The hands of the operator and the specimen must be cleaned
properly between each and every polishing step.
• The specimen must not tilt during grinding or polishing.
• Keep preparation times as short as possible. Unnecessarily long
preparation time waste consumables and may even damage the
sample, for example with edge rounding and relief.
• New polishing cloths or grinding discs may need to be “run in” for a
short time, or dressed or cleaned before use to give the best
results.
• Old polishing cloths should be thoroughly cleaned before polishing.

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 POLISHING
• Like grinding, polishing smoothens the surface of the specimen. The
difference between grinding and polishing consists in quality of the
surface attainable. In polishing this is always better than grinding.
• Several techniques of polishing are used, which can be divided into
chemical, mechanical or electrolytic methods.

(a) (b)

Fig. 2.14: Micrograph Showing Scratches Resulting from Insufficient

Polishing or Contamination from a Coarser Grit (b) the same
Specimen Polished Correctly

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 POLISHING
• Chemical polishing is a very simple method by which the ground surface is
immersed in an electrolyte. The electrolyte serves as a polishing media. The
specimen is moved in the electrolyte for some time. The duration depends
on the nature of the metal and the electrolyte. The chemical attack removes
the unevenness, and a smooth surface without deformations will result.

The mechanical polishing process must be regarded as a sort of very fine

machining operation, the material being removed as chips.

• Alumina (Al2O3) or diamond powders are most common abrasives in

polishing.
• In contrast to the grinding media, the polishing media are used as
suspension in water or as pastes, in some cases also as dry powders. They
are applied to a suitable polishing surface, usually a cloth, and so are not
fixed to a support as are the grinding abrasives.

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 CLEANING

• An important requirement in all metallographic work is

cleanliness.
• The impurities originally sticking to the specimen, such as oil,
grease, dust etc, and also all the residues of grinding and
polishing media from the preceding preparation stages must
be removed.
• All these remains may have harmful effects during the etching
and lead to false interpretations during examination under
the microscope.
• The remains of the cleaning medium itself (e.g. water) should
also be removed. Therefore, every cleaning procedure
includes drying.

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 CLEANING
• The simplest cleaning method is rinsing in
water with subsequent drying, but
ultrasonic cleaning is much more efficient.

• By this method impurities can be removed

from the finest cracks and voids, as found in
porous or cracked specimens or between
specimens and the mounting medium.

• In an ultrasonic cleaner the ultrasound

waves pass on into the cleaning solvent in An Ultrasonic Cleaner
the tank and guarantee an effective cleaning
of the samples which cannot at all or only
insufficiently be cleaned in the usual way.

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 ETCHING
• Mainly aqueous or alcoholic solutions of acids, bases or salts serve as
etching mediums.
• The etching conditions, i.e. the composition of the etching medium, the
temperature and the etching time can be varied.
• On the basis of more than one hundred years of experience there are
now thousands of chemical etching recipes summed up in many
manuals.
• For pure metals and single phase alloys, a potential difference exists
between grains of different orientations, between grain boundaries and
grain interiors, between impurity phases and the matrix. For multiphase
alloys, a potential difference also exists between the various phases
present. These potential differences alter the rate of attack, thus
revealing the microstructure when chemical etchants are used.

• During etching, the more electropositive (anodic) phase is attacked

while the more electronegative (cathode) phase is not attacked
appreciably.

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 ETCHING
• Before etching it must be ensured that the specimen is clean and dry.
• In general wiping the surface with moist cotton under running water is
adequate, although ultrasonic cleaning, especially if cracks or pores are
present, is preferable.
• The specimen must be dry because the presence of moisture can readily
affect the chemical behaviour of some etchants, particularly those in
alcoholic solutions such as nital and picral.
• For etching, a small amount of the proper etchant is poured into a dish.
The dry and clean specimen is then immersed, facedown, in the solution.
The surface of the specimen should be kept completely covered with the
etchant throughout the etching period
• The progress of the etching action, as it turns the shiny mirror into a
slightly cloudy mirror, should be watched carefully and closely.
• The time required to etch a specimen varies with different metals. Some
metals, such as bronzes, can be etched in a few seconds while some
stainless steels may take much longer time.

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 Type of Composition Characteristics and Uses
Etchant
Nital 2 ml HNO3 General etchant for irons and steels.
98 ml For pure iron and wrought iron the
Alcohol concn of HNO3 may be raised to 5
ml.
Also suitable for ferritic gray cast
irons and black-heart malleable
irons.
Picral 4 g Picric acid The most suitable reagent for all
96 ml Alcohol cast irons, with the exception of
alloy and completely ferritic cast
irons.
Alkaline 2 g Picric acid Its main use is to distinguish
sodium 25 g NaOH between ferrite and cementite.
picrate 100 ml. water The latter is stained black, but
ferrite is not attacked.

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 GENERAL RULES FOR ETCHING
• Time of etching should be as short as possible. An under-etched specimen can
be etched again but a over-etched samples must be polished again.

• Etchants should be free of moisture, especially if the solvent in them is alcohol.

• Etchant should be rinsed-off immediately after etching has made the surface of
the specimen slightly cloudy

• Immediately after rinsing off the etchant, the etched surface should be dried
with a powerful, dry puff of air.

• The polished, or polished and etched, surface of the specimen should never be
touched with fingers.

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