Experiment No.
1
Aim: To study and perform the various steps in metallographic specimen preparation, including
cutting, mounting, polishing, and etching.
Apparatus/Equipment/Materials: Abrasive cut-off wheel machine, polishing machine, Mounting
Press, chemicals.
Introduction:
Metallography is the science of preparing, interpreting, and analyzing microstructures of materials. It
Is the art and science of preparing microstructure metals and alloys using microscopy. It is better to
understand the behavior and performance. The method is used to evaluate metallic materials in various
industries, including the aerospace industry, the automotive industry, and parts of the construction
industry. It is also used for process control, including the studies of parts that have failed during service
or partly finished products, as well as the examination of defects that appear in finished. It is an
important branch of Metallurgical Engineering.
Awell-prepared metallographic specimen is:
a) Representative sample:
b) Sectioned, ground, and polished to minimize disturbed or flowed surface metal caused by
mechanical deformation and thus to allow the true microstructure to be revealed by etching.
c) Free from polishing scratches and pits, and liquid staining
d) Flat enough to permit examination by optical microscope or SEM.
Procedure:
Various steps involved in the specimen preparation and the significance of each step:
Many steps in the preparation of metallographic specimens described here are also applicable in other
types of metallographic studies, such as electron microscopes, microhardness testing, quantitative
measurement of constituents of structures, and the five major operations.
Preparation of metallographic specimens generally requires five major operations:
a) Cutting
b) Mounting (which is necessary when the sample cannot be held properly due to its shape and/or
size, while polishing)
c) Grinding
d) Etching
1. Sectioning
Separate test pieces or coupons attached to castings or forgings should be designed so that a minimum
of sectioning is required for producing metallographic specimens. Sectioning becomes necessary when
studying parts that have failed in service where specimens have to be taken from a large block of
material. Therefore, metallographic studies of such samples often involve more than one sectioning
operation.
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vany netallographic studies require more than one specimen. For example, a study of deformation in
Wrought metals usually requires two sections - one perpendicular to, and the other parallel to,
axis of the direction of deformation, Failed narts may be best studied by the major
selecting a specimen that
intersects the origin of the failure if the origin can be identified on the surface. Depending on the type
of failure, it may be necessary to take several specimens from the area of failure
and adjacent areas.
2. Mounting of Specimens
Ine primary purpose of mounting is to make it convincement to handle specimens of arbitrary shape
and/or small sizes during various steps of metallographic sample preparation and examination. A
Secondary purpose of is to protect and preserve extreme edges or surface defects during metallographic
preparation. Specimens may also require mounting to accommodate various types of automatic
devices used in metallographic laboratories or to facilitate placement on the microscope stage.
An
additional benefit of mounting is the identification of the sample (name, alloy number, or laboratory
code number) without damaging the
specimen.
Compression mounting: It is the most common mounting method, which involves molding around the
metallographic specimen by heat and pressure using molding materials such as Bakelite, Diallyl
Phthalate resins, and acrylic resins. Bakelite and Diallyl phthalate are thermosetting, and acrylic resins
are thermoplastic.
Not all materials or specimens can be mounted in thermosetting or thermoplastic mounting. The
heating cycle may cause changes in the microstructure or the pressure.
Grinding
Grinding is accomplished by abrading the specimen surface through a sequence of operations using
progressively finer abrasive grits. Grit sizes ranging from 60 mesh to 150 mesh are usually accepted
as coarse abrasives, and grit sizes ranging from 180 size to 600 mesh is regarded as fine abrasives and
commence with the coarse grit size for making initial flat surfaces. Grinding should commence with
the coarse grit size, and the effect of abrasive sizes in the range of 80 to 150 mesh. Grinding should
be done sequentially starting from the coarser one to finer one. A satisfactory grinding sequence might
involve grit sizes of 180, 240, 400 and 600 mesh. The purpose of grinding is to remove the oxide layer
or damaged layer or uneven surfaces that might have formed during last sectioning operation.
However, the depth of cold worked metal is roughly inversely proportional to the hardness of the
specimen and may be 10to 50 times the depth of penetration of the abrasive particle.
Toensure the complete elimination of the previous grinding scratches found by visual inspection, the
direction of grinding must be changed by 90° from the one stage of grinding to the next stage. In
addition, microscopic examination of the various ground surfaces during the grinding sequence may
be worthwhile in evaluating the effect of grinding. Each ground surface should have scratches that are
clean-cut and uniform in size, with no evidence of previous grinding scratches. Cleaning before going
to next stage grinding is always helpful.
Grinding Mediums
Grinding media are silicon carbide (SiC), aluminum oxide (Al203), emery (AlL03-FesO4), and
diamond particles. All except diamond are generally bonded to paper or cloth backing material of
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Various weights in the form of sheets, disks. and belts of various sizes. The abrasives may be used
also
in the powder form by charging the grinding surfaces with loose abrasive particles.
Automatic grinding, as the name implies, is done without hand assistance. All automatic grinding
devices use lap surfaces on which paper-based disks are placed or abrasive powder is charged. The lap
1S elthera rotating or a vibrating disk, where the use of the latter is described as vibratory grinding.
3. Grinding
Grinding is a most important operation in specimen preparation. During grinding, the operator has the
opportunity of minimizing mechanical surface damage, that can be removed by subsequent polishing
operations. Even if sectioning is done in a careless manner resulting into a severely damaged surface,
the damage can be eliminated by prolonged grinding. However, prolonged grinding should be avoided
since it might lead to excess heating or surface
damage.
Figure 1.1: SEM micrograph of 600 grit SiCabrasive paper (original mag. 150x)
Grinding is accomplished by abrading the specimen surface through a sequence of operations using
progressively finer abrasive grits. Grit sizes ranging from 60 mesh to 150 mesh are usualy regarded
as coarse abrasives, and grit sizes ranging from 180 mesh to 600 meshas fine abrasives. Grinding
should commence with the coarse grit size to make an initial flat surface and remove the effects of
sectioning. Hack-sawed, band-sawed, or rough surfaces usually require abrasive grit sizes in the 80 to
150 mesh range. Grinding should be done sequentially, starting from the
4. Polishing
Polishing is the final step in producing a surface that is flat, scratch-free, and mirror-like in appearance.
Such a surface is necessary for subsequent accurate metallographic interpretation, both qualitative and
quantitative. The polishing technique used should not introduce extraneous structure, such as disturbed
metal, pitting, dragging out of inclusions, and staining. may cause delicate specimens to collapse or
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available mold sizes.
deform. The size of the selected specimen may be too large to be accepted by the
These difficulties are usually overconme by cold mounting.
1203 slurry. The
involving the use of cloth-covered laps and suitable polishing abrasives, basically A
held by a hand, held
laps have either a rotating or a vibrating motion, and the specimens are
relatively
mechanically, or nerely confined within the polishing area. Polishing should be done in a
dust-free area, preferably removed from the area for sectioning, mounting, and rough grinding. Any
contamination of a polishing lap by abrasive particles carried over from preceding operations or by
ust, dirt or other foreign matter in the air cannot be tolerated. Carryover as a result of improper
Cleaning between final polishing steps is another prime source of contamination. It is just as important
for the operator to wash his/her hands meticulously as it is for him/her to remove alltraces of polishing
abrasive from the specimen before proceeding to the next finer polishing operation.
Electrolytic Polishing
Even with the most careful mechanical polishing, some disturbed metal, even very small the amount,
will remain after preparation of a metallographic specimen. This is no problem if the specimen is to
be etched for structural investigation because etching is usually suficient to remove the slight layer
of disturbed metal. However, if the specimen is to be examined in the as polished condition, or if no
surface disturbance can be tolerated, then either electrolytic polishing or chemical polishing is
preferred. The basic principle involved in this technique is anodic dissolution of surface of the sample
which results in a leveling and brightening of its surface. Electro polishing does not disturb any metal
on the specimen surface, and therefore, ideally suited for the metallographic preparation of soft metals,
most single-phase alloys, and alloys that works harden readily. The disadvantages of electro polishing
include preferential attack in multiphase alloys caused by differences in electrical potential between
phases. Proper choice of electrolyte and operating conditions will minimize these disadvantages.
5. Etching
Metallographic etching is used to reveal particular structural characteristics of a metal. This is essential
since these structuralcharacteristics are not visible in the polished mirror-like surface in the metal. It
can be used for phase identification, for dislocation density calculation (etch pitting), and for
orientation studies. The principle of etching multiphase alloys is based on the preferential attack
(different rates of electrochemical dissolution of phases in the etchant) or preferential staining of one
or more phases because of differences in chemical composition and differences in grain-orientation.
Before being etched, a specimen should be inspected for polishing defects, such as scratches, pits,
relief polish, comet tails, pulled-out inclusions, and voids.
Chemical Etching
Chemical etching is accomplished by immersing the specimen in (or swabbing it with) a suitable
etchant until the required structure is revealed. Etching is done in Petri dishes or in other suitable
containers with loose covers to prevent excessive evaporation of the solvent, particularly alcohol
solutions. Glass containers can be used for all etchants except hydrofluoric acid solutions, where the
container should be made of polyethylene or other suitable material. By the use of tongs or another
convenient handling device, the surface of the specimen is immersed in the etchant with some agitation
to ensure that the fresh etchant is in contact with the specimen at all times. Most metals lose their
bright appcarance during etching, indicating that etching occurs. With practice, one can ascertain the
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procedure calls for
completion of etching by the degree of the dullness of the surface. If the etching
saturated with the etchant, or the
Swabbing, the surface of the specimen can be scrubbed with cotton
specimen can be immersed and swabbed while in the solution. When
etching is complete, the specimen
stream of warm air (hand dryer).
1S rinsed in running water and then in alcohol, followed by drying in a
the optical-microscope to study its
Alter etching, the specimen surface is observed under not affected by the etching.
microstructure. Care should be taken while etching so that the hand is
