SAMPLE PREPARATION FOR

METALLOGRAPHIC EXAMINATION
BY LIGHT OPTICAL MICROSCOPY

Sample Preparation

Sample Preparation
The preparation starts by
cutting a small representative
piece of the metal to be studied.
Mounting. Small samples can
be difficult to hold safely during
grinding
and
polishing
operations, and their shape may
not be suitable for observation
on a flat surface. They are
therefore mounted inside a
polymer block or mount.

SECTIONING
Many metallographic specimens are used for process control. Separate test
pieces or coupons attached to castings or forging should be designed so that a
minimum of sectioning is required for producing metallographic specimens.
Important uses of metallography other then process control include examination
of defects that appear in finished or partly finished products and studies of parts
that have failed in service. Investigations for these purposes usually require that
the specimen be broken from a large mass of material, and often involve more
than one sectioning operation.
Many metallographic 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, the major axis of direction of
deformation. Failed parts may best be studied by 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 that area of the failure and from adjacent areas.

ABRASIVE WHEEL CUTTING

By far the most widely used sectioning devices in metallographic laboratories are
abrasive cutoff machines. They range from small, thin-sectioning machines
employing abrasive or diamond-rimmed wheels approximately 4 in. in diameter and a
few mils thick to large floor-model machines employing abrasive or diamond-rimmed
wheels up to 12 in. in diameter and 1/16 in. thick. An advanced design of automatic
cutoff machine for laboratory use employs abrasive wheels 6 to 12 in. in diameter.
Abrasive-wheel cutting may produce deformation damage to a depth as great as 0.04
in. Deformation damage can be minimized by using thin cutoff wheels. A hard wheel
is usually best for cutting soft stocks, whereas a soft wheel is preferred for cutting
hard materials. A good general purpose cutoff wheel is a medium-hard silicon
carbide abrasive wheel.
All abrasive-wheel sectioning should be done wet. An ample flow of water or water
soluble oil coolant should be directed onto cut.
Some laboratory cutoff machines provide for submerged wet cutting. Wet cutting will
produce a smooth surface finish and will guard against excessive surface damage
caused by overheating.

Mounting

MOUNTING OF SPECIMENS
PURPOSE OF MOUNTING
The primary purpose of mounting specimens is for convenience in handling
specimens of difficult shapes or sizes during the subsequent steps of
preparation and examination.
A secondary purpose is to protect and preserve extreme edges or surface
defects during preparation.
Specimens also may require mounting to accommodate various types of
automatic devices used in laboratories or to facilitate placement on the
microscope stage.
An added benefit of mounting is the ease with which a mounted specimen
can be identified by name, alloy number, or laboratory code number for storage
by scribing the surface of the mount without damage to the specimen.

MOUNT SIZE AND SHAPE

As the size of the specimen increases, so does the difficulty of keeping the
specimen surface area flat during grinding and polishing. A saving in the
time required for the preparation of one large metallographic specimen may
be realized by sectioning the specimen into two or more smaller specimens.
A specimen having an area of approximately 1/4 sq in. is perhaps the most
suitable; the maximum area should be limited to about 4 sq in. if possible.
Thickness of the mount should be sufficient to enable the operator to hold
the mount firmly during grinding and polishing and thereby to prevent a
rocking motion and to maintain a flat surface. Circular mounts are commonly
1 to 2 in. in diameter and are the most easily handled. The length-to-width
ratio of rectangular mounts should be limited to approximately 2 to 1 to
facilitate handling.

MOUNTING METHODS
The method of mounting should in no way be injurious to the microstructure of
the specimen. Mechanical deformation and the heat are the most likely sources of
injurious effects. The mounting medium and the the specimen should be
compatible with respect to hardness and abrasion resistance. A great difference in
hardness or abrasion resistance between mounting media and specimen promotes
differential polishing characteristics, relief, and poor edge preservation. The
mounting medium should be chemically resistant to the polishing and etching
solutions required for the development of the microstructure of the specimen.

Mounting Methods :
Clamp Mounting
Compression Mounting
Cold Mounting
Conductive Mounting

CLAMP MOUNTING
Clamps are used most often for mounting thin sheets of metal when preparing
metallographic cross sections. Several specimens can be clamped
conveniently in sandwich form. The two clamp plates are frequently made
from 1/4 in. thick steel; in general, the hardness of the clamp should be
approximate or exceed the hardness of the specimen. The clamp plates are
cut longer and wider than specimens to be clamped. Then two holes are
drilled and tapped in the face of one clamp plate outboard of the specimen
area; corresponding holes are drilled in the other clamp plate. Machine bolts
are inserted through these latter holes and into the tapped holes; the clamp
plates with the specimen or specimens are drawn tightly up means of these
bolts. Sometimes, a third bolt positioned near the top of the clamp midway
between the ends is useful for maintaining a uniform vertical separation
between the clamp plates.

CLAMP MOUNTING

(Contd)

Clamp mounting affords a means of rapid mounting, and of very good edge
preservation by virtue of the intimate contact between specimens. On the
other hand, hairline separations between specimens occur frequently and
entrap abrasive particles or liquid solutions during preparation. Sometimes,
the particle and liquids can be removed by soaking the mount in alcohol an
then thoroughly drying it. If this cannot be done, the liquid eventually seeps
out and stains the polished surface, and often obscures the true
microstructure after etching. One solution to this difficulty is the insertion of
one thickness of transparent plastic wrapping film at each interface. (The
plastic must be one that is inert to alcohol and etchants). Under clamping
pressure, the plastic flows readily and seals all hair-line separations. Since
the film is only a fraction of a mil thick, specimen edges are preserved by
adjoining specimens or clmap edges. Alternatively, soft, thin sheets of metal
of the same type as that be examined can be used instead of the plastic film,
or the mount can be vacuum impregnated.

Mounting
Hot-mounting the sample is surrounded by
an organic polymeric powder which melts
under the influence of heat (about 200 C).
Pressure is also applied by a piston,
ensuring a high quality mould free of
porosity and with intimate contact between
the sample and the polymer.

COMPRESSION MOUNTING
Compression mounting, the most common mounting method, involves molding
around the specimen by heat and pressure such molding materials as Bakelite
diallyl phthalate resins, and acrylic resins. Bakelite and diallylic resins are
thermosetting, and acrylic
resins are thermoplastic. Both thermosetting and thermoplastic materials require
heat and pressure during the molding cycle, but after curing, mounts made of
thermosetting materials may be ejected from the mold at maximum temperature.
Thermoplastic
materials remain molten at the maximum molding temperature and must cool
under pressure before ejection.
Mounting presses equipped with molding tools and a heater are necessary for
compression mounting. Readily available molding tools for mounts having
diameters of 1, 1 1/4 and 1 1/2 in. consist of a hollow cylinder of hardened steel, a
base plug, and a plunger.
A specimen to be mounted is placed on the base plug, which is inserted in one
end of the cylinder. The cylinder is nearly filled with molding material in powder
form, and the plunger is inserted into open end of the cylinder. A cylindrical
heater is placed around the mold assembly, which has been positioned between
the platens of the mounting press. After the prescribed pressure has been

COMPRESSION MOUNTING

(Contd)

exerted and maintained on the plunger to compress the molding material until it
and the mold assembly have been heated to the proper temperature, the finished
mount may be ejected from the mould by forcing the plunger entirely through the
mold cylinder.
Not all materials or specimens can be mounted in thermosetting or thermoplastic
mounting mediums. The heating cycle may cause changes in the microstructure,
or the pressure may cause delicate specimens to collapse or deform. The size of
selected specimen may be to large to be accepted by the available mold sizes.
These difficulties are usually overcome by cold mounting.

Fully automatic mounting press

Mounting press with manual operation

Mounting
Cold mounting can be done using two
components resins (epoxies) which are liquid to
start with but which set solid shortly after mixing.
it requires very simple equipment consisting of a
cylindrical ring which serves as a mould and a flat
piece which serves as the base of the mould. the
sample is placed on the flat piece within the mould
and the mixture poured in and allowed to set. Cold
mounting takes few hours to complete.

COLD MOUNTING
Cold mounting requires no pressure and little heat, and is a means of mounting
large numbers of specimens more rapidly than by compression mounting.
Materials for cold mounting are classified as polyesters, epoxies and acrylics.
Polyesters are transparent and usually water clear;epoxies are almost transparent
and straw color; acrylics are opaque. Cold mounting materials of all three
classifications are two component systems that consist of resin and a hardener;
both the resin and the hardener can be liquid, both can be solids, or one can be
liquid and the other a solid. Mixing of the resin and the hardener produces
exothermic polymerization, and therefore this operation is critical in producing a
satisfactory cure and limiting the temperature to a permissible level. The
temperature rise may reduced at the expense of longer curing time.
Cold mounting is a casting method, because each of the three classifications of
cold mounting materials is liquid after the resin and). The casting molds can be of
any size or shape desired. For round molds, either Bakelite ring forms, or ring
sections cut from plastic or metal tubes or pipes are suitable. The mold material
may become part of the mount in the form of an outer shell, or mold release
agents may be used to permit the mount the mount to be ejected from the mold.
Rectangular molds are formed readily by wrapping heavy-duty aluminum foil
around wood blocks of the desired size. The aluminum foil can be removed from
the mount by peeling it away, grinding it off, or using a mold release agent.

COLD MOUNTING

(Contd)

Molds of any size or shape can be prepared from silicone rubber materials. The
flexibility of silicone rubber molds allows cured cold mounts to be removed easily.
Epoxy resins are the most widely used cold mounting materials. They are hard
and adhere tenaciously to most metallurgical, mineral and ceramic specimen.
They also exhibit lower volume shrinkage then either polyesters or acrylics and
are very useful for impregnating porous structures or cracks by vacuum method.
Epoxy resin mounts May be cured in a low-temperature or placed in a low
temperature oven for fast curing, depending on the mixture ratio of resin to
hardener.
Polyester resins have greater volume shrinkage the epoxies. They provide waterclear or slightly colored transparent mounts, which strip readily from glass
casting surfaces and metal molds.
Acrylic materials are fast curing, and the mixing and casting process for the
acrylics is quick and simple. The fast curing rate results from the relatively high
rate heat evolution during exothermic polymerization, but some control of the
exothermal temperature rise can be accomplished by varying the sizes of the
specimen and the mount. Stripping acrylic mounts from metal or glass molds
is not difficult.

Schematic illustration of a metallography sample embedded

in a plastic mount. The top face is ground and polished.

CONDUCTIVE MOUNTING
For specimens requiring metallographic preparation by electrolytic techniques,
an electrically conductive mount affords a convenient means of completing the
electrical circuit through the specimen; merely an electrical contact with the
mount, rather than with specimen, is required. Most conductive mounting
materials are mixtures of a metal, usually copper or iron powder, and
thermosetting or thermoplastic molding materials. During compression
mounting the metal powder particles are compacted sufficiently to provide
electrical continuity throughout the mount. An equally convenient method is to
attach a copper wire to the back of the specimen.

GRINDING
Grinding is a most important operation in specimen preparation. During grinding the
operator has the opportunity of minimizing mechanical surface damage that must be
removed by subsequent polishing operations. Even if sectioning is done in a careless
manner, resulting is severe surface damage, the damage can be eliminated by
prolonged grinding. However, prolonged polishing will do little toward eliminating
severe surface damage introduced by grinding.
Grinding is accomplished by abrading the specimen surface through a sequence of
operations using progressively finer abrasive grit. Grit sizes from 40 mesh through
150 mesh are usually regarded as coarse abrasives and grit sizes from 180 mesh
through 600 mesh as fine abrasives.
Grinding should commence with coarse grit size that will establish an initial flat
surface and remove the effects of sectioning within a few minutes. An abrasive grit
size 150 or 180 mesh is coarse enough to use on specimen surfaces sectioned by an
abrasive cutoff wheels. Hacksawed, band sawed surfaces usually require abrasive grit
sizes in the range 80 to 150 mesh. The abrasive used for each succeeding grinding
operation should be one or two grit size smaller than that used in the preceding
operation. A satisfactory grinding sequence might involve grit sizes of 180, 240, 400
and 600 mesh.

GRINDING (Contd)
As in abrasive-wheel sectioning, all grinding should be done wet, provided water has
no adverse effects on any constituents of the microstructure. Wet grinding minimizes
loading of the abrasive with metal removed from the specimen being prepared. Water
flushes away most of the surface removal products before they become embedded
between adjacent abrasive particles. Thus the sharp edges of the abrasive particle
remain exposed to the surface of the specimen throughout the operation. If the sharp
edges are unexposed the result is smearing of the abraded surface rather then
removal of surface metal. The operator must determine, by examining the specimen
throughout the sequence of grinding steps, that the abrasive is actually cutting and
not merely smearing or burnishing. Burnishing results primarily from using an
abrasive beyond its effective limit. Use of worn-out abrasives and dulled cutting
edges is detrimental to good preparation.
Another advantage of the wet grinding is the cooling effect of the water. Considerable
frictional heat can develop at the surface of a specimen during grinding and can
cause alterations of the true microstructure - for example, tempering of martensite in
steel - that cannot be removed during polishing. Wet grinding provides effective
control of overheating. The abraded surface of a specimen may become embedded
with loose abrasive particles during grinding. These particles may persist in the
surface and appear to be nonmetallic inclusions in the polished specimen. The
flushing action of the water removes many of loose particles that might otherwise
become embedded. Some laboratories have found that dressing the abrasive material
with a solid wax lubricant recommended for grinding and other machining operations
can minimize the embedding of abrasive particles.

GRINDING (Contd)
The purpose of grinding is to lessen the depth of deformed metal to the point where
the last vestiges of damage can be removed by series of polishing steps. The scratch
depth and the depth of cold worked metal underneath the scratches decrease with
decreasing particle size of abrasive. However the depth of cold worked metal is
roughly inversely proportional to the hardness of the specimen and may be 10 to 50
times the depth of penetration of the abrasive particle. It is imperative that each
grinding steps completely remove the deformed metal produced by the previous step.
The operator usually can assume this is accomplished if he or she grinds more than
twice as long as the time required to remove the scratches incurred by the previous
step. To ensure the complete elimination of the previous grinding scratches found by
visual inspection, the direction of grinding must be changed 45 to 90 degrees between
successive grit sizes. 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.
Success in grinding depends in part on the pressure applied to the specimen. A very
light pressure removes insufficient metal. Somewhat heavier pressure produce
polishing, while still heavier pressure brings about the desired grinding action. Very
heavy pressure results in nonuniform scratch size, deep gouges, and embedded
abrasive particles. Generally, a medium to moderately heavy pressure applied firmly
gives the best results.

GRINDING (Contd)
Most grinding of metallographic specimen is performed by manually holding the
specimen with its surface against a grinding material. To establish and maintain a
flat surface over the entire area being ground, the operator must apply equal
pressure on both sides of the specimen and avoid any rocking motion that will
produce a convex surface. If grinding operation is interrupted - the operator must
re-establish contact with grinding material carefully in order to resume grinding in
the plane already established.
Specimens should be cleaned after each grinding steps to avoid any carryover of
abrasive particles to the next step. Water solutions containing detergents are
excellent cleaners and ultrasonic cleaning is an effective technique. Cleanness of
the operator's hands is as important as cleanness of specimen. Contamination of
the grinding equipment by flying abrasive particles must be avoided.
The grinding abrasives commonly used in the preparation of specimens are
silicon carbide (SiC), aluminum oxide (Al2O3), emery (Al2O3 - Fe3O4), diamond
particles, etc. Usually are generally bonded to paper or cloth backing material of
various weights in the form of sheets, disks and belts of various sizes. Limited
use is made of grinding wheels consisting of abrasives embedded in a bonding
material. The abrasive may be used also in powder form by charging the grinding
surfaces with loose abrasive particles.

Polishing
The polishers consist of rotating discs covered with soft
cloth impregnated with a pre-prepared slurry of hard
powdery alumina particles (Al2O3, the size ranges from
0.5 to 0.03 m).
Begin with the coarse slurry and continue polishing until
the grinding scratches have been removed. It is of vital
importance that the sample is thoroughly cleaned using
soapy water, followed by alcohol, and dried before moving
onto the final stage. Any contamination of the final
polishing disc will make it impossible to achieve a
satisfactory polish.
Examining the specimen in the microscope after polishing
should reveal mirror like surface.

POLISHING
Polishing is the final step in production 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, comet tails and staining.
Before final polishing is started, the surface condition should be at least as good
that obtained by grinding with a 400-grit (25 microns) abrasive.

POLISHING CLOTHS
The requirements of any good polishing cloth include the ability to hold an abrasive,
long life, absence of any foreign material that may cause scratches, and absence of
any processing chemicals that may react with the specimen.
A cloth without nap or with a very low nap is preferred for the preliminary or rough
polishing operation. The absence of nap ensures maximum contact with the
polishing abrasive, and results in fast cutting with minimum of relief. The cloths
most frequently used are canvas, low-nap, cotton, nylon, silk and Pelon. These
cloths are stretched tight on the laps and fastened securely, usually by a
band-type clamp. Some cloths are available with a contact adhesive on the back,
which greatly simplifies installation on the wheel. After installation, the cloths are
charged with the appropriate abrasive (usually in sizes from 15 microns down to 1
microns) and carrier. Rough polishing is usually done with the laps rotating at 500 to
600 rpm. Cloths with a medium or high nap are ordinarily used on slow rotating laps
(less than 300 rpm) for intermediate and final polishing. Felt or billiard cloths (100%
virgin wool), used with 0.3 micron aluminum oxide or other comparable abrasive, are
excellent for intermediate polishing of soft metals (most nonferrous alloys and low
carbon steels) and final polishing of hard materials (such as hardened alloy steels).
One of the most popular cloths for final polishing of most metals is composed of
densely packed, vertically aligned, synthetic fibers bonded to a suitable backing. For
some metals or for particular types of polishing, other cloths, such as velvets,
satins, cashmeres or cottons, may be required. The ability to select the proper
combination of cloth, abrasive, carrier, polishing speed (rotational speed of the
polishing wheel), and pressure applied can be acquired only by experience.

POLISHING ABRASIVES
Polishing usually involves the use one or more of five types of abrasive: aluminum
oxide (Al2O3), magnesium oxide (MgO), chromic oxide (Cr2O3), iron oxide (Fe2O3),
and diamond compound. With the exception of diamond compound these abrasives
are normally used in a distilled water suspension, but if the metal to be polished is
not compatible with water, other suspensions, such as ethylene glycol, alcohol,
kerosene or glycerin, may be required. The diamond compounds should be
extended only with the carrier recommended by the manufacturer.
Aluminum oxide (alumina) is the polishing abrasive most widely used for general
metallographic polishing. The alpha grade aluminum oxide is used in a range of
particle sizes from 15 microns to 0.3 micron. For some hard materials the 0.3 micron
size is sufficient for a final polish. The gamma grade of aluminum oxide is available
in a 0.05 micron particle size for final polishing.
Diamond polishing compounds are becoming increasingly popular for preparing
metallographic specimen. Diamond is the only substance hard enough and with
good enough cutting qualities to be used for mechanical polishing of materials such
as boron carbide and sintered tungsten. Specimens that have both hard and soft
constituents, such as graphite in cast iron and silicon in aluminum, can be polished
without causing relief, with diamond compounds on an appropriate lap. These
polishing compounds are available either in water soluble and oil soluble carriers or
in the form of dry diamond powder in particle size down to 0.25 microns.

(a)

(b)

(c)

(d)

( a ), ( b ) bench type abrasive cutters

( c ), ( d ) floor type abrasive cutters

Grinding
Grinding is done using rotating discs covered with silicon carbide paper
and water.
There are a number of grades of paper, with 180, 240, 400, 1200, grains of
silicon carbide per square inch. 180 grade therefore represents the coarsest
particles and this is the grade to begin the grinding operation. Always use
light pressure applied at the centre of the sample.
Continue grinding until all the blemishes have been removed, the sample
surface is flat, and all the scratches are in a single orientation.

Wash the sample in water and move to the next grade, orienting the
scratches from the previous grade normal to the rotation direction. This
makes it easy to see when the coarser scratches have all been removed.
After the final grinding operation on 1200 paper, wash the sample in water
followed by alcohol and dry it before moving to the polishers.

Variable speed single

wheel polisher
Manual roll grinder

Variable speed double

wheel polisher

(a)

(b)

(c)

Schematic illustration of
a method for grinding
metallography
specimens.
( a) Coarse scratches
left by previous grit size.
( b) First set of fine
scratches left by the
current grit size.
(c) Second set of fine
scratches left by the
current grit size.
Note: Arrows show the
direction of polishing
motion.
Each time a new grit
size is used, apply a
polishing direction at a
90 o angle to the
previous polishing
direction.

Etching
The purpose of etching is two-fold.
1.Grinding and polishing operations produce a
highly deformed, thin layer on the surface which
is removed chemically during etching.
2. attacks the surface with preference for those sites
with the highest energy, leading to surface relief
which allows different crystal orientations, grain
boundaries, precipitates, phases and defects to be
distinguished in reflected light microscopy as
demonstrated in Figure

Etching
Etching should always be done in stages, beginning with light attack, an
examination in the microscope and further etching only if required.
If you overetch a sample on the first step then the polishing procedure will
have to be repeated.
The table below gives the etchants for alloys that will be examined in this
experiment.

Sample

Etchant

Al alloys

Kellers (2 ml HF +3 ml HCL + 5 ml NO3+ 190 ml water)

Cu-Zn alloy (brass)

10 ml HNO3+90 ml water

Steel and cast irons

Nital (2% HNO3 + 98% ethanol)

ETCHING
Although certain information may be obtained from as-polished specimens, the
microstructure is usually visible only after etching. Only features which exhibit a
significant difference in reflectivity (10% or greater) can be viewed without etching.
This is true of microstructural features with strong color differences or with large
differences in hardness causing relief formation. Cracks, pores, pits, and
nonmetallic inclusions may be observed in the as-polished condition. In most
cases, a polished specimen will not exhibit its microstructure because incident
light is uniformly reflected. Since small differences in reflectivity cannot be
recognized by the human eye, some means of producing image contrast must be
employed. Although this has become known as "etching" in metallography, it does
not always refer to selective chemical dissolution of various structural features.
There are numerous ways of achieving contrast. These methods may classified as
optical, electrochemical (chemical), or physical, depending on whether the
process alters the surface or leaves if intact.
Chemical Etching :
Chemical etching is based on the application of certain illumination methods, all of
which use the Kohler illumination principle. This principle also underlies common
bright-filed illumination. These illumination modes are dark field, polarized light,
phase contrast and interference contrast. They are available in many commercially
produced microscopes, and in most cases, the mode may be put into operation
with few simple manipulations. There is distinct advantage in employing optical
etching rather than those technique which alter the specimen surface. Chemical
and physical etching require considerable time and effort and there is always a
danger of producing artifacts which lead to misinterpretations.

Metallographic Etching Processes

There main etching processes used in metallographic sample preparation are:
1. Chemical etching
2. Electrolytic etching
3. Heat tinting
1. Chemical Etching
This typically involves immersing the sample in an etchant such or swabbing
the surface with an etchant. The etchant selectively corrodes microstructural
features. Immersion time or etching time is highly dependent on the system
and in most cases requires experience. The selection of the optimum etchant is
also very important in sample production.
Deeper etches are preferred for low magnification examinations, while shallow
etches are preferred for higher magnification etches.

2. Electrolytic Etching
Electrolytic etching and electropolishing are in effect the same process, except
that electrolytic etching uses lower voltages and current densities. Most
electrolytic etching processes use direct current electrolysis. The process uses
the specimen as the anode, with the cathode being a highly insoluble, but
conductive material. Typical examples are platinum, graphite and stainless steels.

3. Heat Tinting
Heat tinting, sometimes called thermal etching is the process of oxidizing a
sample in a furnace. This induces oxidation of surface features at different rates,
to reveal various features.