SHARMIWATI

METALLOGRAPHY

Metallography is
o the microscopic examination of the microstructure (grain
structure) of metals
 the most important tool in metallurgy, provides invaluable
information on the processing history and properties of
metals
 used as a quality control tool, in failure analysis and for alloy
development
 It may involve techniques and tools such as visual
inspection, low-powered magnification, optical microscopes,
electron microscopes and X-ray crystallography.

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 MACROSCOPIC vs MICROSCOPIC
ANALYSIS
MACROSCOPIC MICROSCOPIC
 To reveal the general structure of  To gain a representative view of
large areas of a specimen microstructure
 Equipment: binocular microscope  Equipment: metallurgical
microscope
 Magnification: 10x  Magnification: 25x to 50x
100x to 1000x
 MACROGRAPH: a sketch of the  METALLOGRAPH: a metallurgical
etched surface of the specimen microscope equipped to
made from a macroscopic photograph microstructures and
examination produce photomicrographs.
 PHOTOMICROGRAPHS: a
photographs of microstructure
 PHOTOMACROGRAPH: a
photograph of the etched surface
made from a macroscopic
examination

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 PREPARATION PROCESS OF
METALLOGRAPHIC TEST PIECE

 Metallographic tests: the most appropriate tests

for determining the constitution of steels
 Metallographic tests include these following:
 taking samples/sectioning
 smoothing
 polishing
 etching
 cleaning-drying

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A well-prepared metallographic specimen is:

 A good representative of the sample.

 Sectioned, ground and polished so as to minimize
disturbed or flowed surface metal caused by mechanical
deformation, and thus to allow the true microstructure to
be revealed by etching.
 Free from polishing scratches and pits and liquid
staining.
 Polished so that inclusions are preserved intact.
 Flat enough to permit examination at high magnification.
 TAKING SAMPLE
Samples may be taken for the following purposes:
 to obtain a sample representative of a material. In the
case of laminated materials, a sample must be taken of
the sample in the non-laminated section, and then
another, in the direction of the lamination.
 to observe defects suspected to exist in a particular
area.
 to study the causes of breakage in a part, in which case,
the sample must be taken from the area affected by the
breakage. An additional, healthy sample should also be
taken from a different area of the same part, in order to
study the differences.

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 TAKING SAMPLE
Orientation of Specimen-Square/Rectangular Bar

DIRECTION OF WORK

MICROSTRUCTURE

LONGITUDINAL
SECTION

TRANSVERSE
SECTION MICROSTRUCTURE

Figure 1: Longitudinal & transverse orientations of specimens

from a worked metal exhibit different microstructures.

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 TAKING SAMPLE
Orientation of Specimen-Round Bar
MICROSTRUCTURE
DIRECTION OF WORK

TANGENTIAL
LONGITUDINAL
SECTION

RADIAL
LONGITUDINAL
TRANSVERSE SECTION
SECTION

MICROSTRUCTURE
Figure 2: Longitudinal & transverse orientations of specimens
from a worked metal exhibit different microstructures.

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 TAKING SAMPLE
Sectioning/ Specimen Selection
 Sectioning is defined as the removal of a partial sized,
representative specimen from a larger sample.
 This is the main step that has to be taken when preparing
a specimen for a physical or microscopic analysis.
 When performing this operation the use of incorrect
preparation techniques may lead to false microstructure. 
 The damage to a specimen during sectioning depends upon
the material being sectioned, the nature of the cutting
device used, the cutting speed rate, and the amount and
type of coolant used.

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 TAKING SAMPLE
Sectioning/ Specimen Selection
 The sample should be cut by means of a saw or abrasive disc.
In both cases, but especially so in the latter, refrigeration
must be intense, in order to keep the presence of heat from
modifying the original constitution of the part.
One good rule of thumb for making certain that the
temperature is never excessive is to operate in such a way
that during cutting or later smoothing or polishing, the part
never becomes too hot to touch.
 As regards the size of the sample, generally, the most
adequate would be from 20-25mm wide by 50mm long, and
10-12mm thick

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 Mounting

 After the metal is cut into a small

piece, it is placed in the mounting
machine.
 With the aid of a thermosetting
resin powder, the specimen is
mounted by the heat and pressure
applied to the powder.
 This causes the specimen to be
surrounded by a plastic like
material, in a cylindrical shape.

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The mounting operation accomplishes
three important functions:
 it protects the specimen edge and maintains the
integrity of a materials surface features
 fills voids in porous materials
 improves handling of irregular shaped samples, especially
for automated specimen preparation.
 GRINDING/SMOOTHING
 Initial smoothing to flatten the sample is done by
means of a disc sander.
 The pressure of the sample on the sander must be
slight in order to avoid distortion and excessive
scratching of the metal.
 This operation means going over the sample with
different grain sandpapers (400/600/800/1,000).
 Grinding uses sandpaper of different grades to remove
oxides

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 POLISHING
 Polishing is the final step in production a surface that is flat,
scratch free, and mirror finish on the specimen for
examination of a metal's microstructure under a microscope.
 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.
 The specimen is polished using DISC POLISHER.
 The surface must be free from pits (small, sharp
depressions) & subsurface deformation effects that lead to
artifacts when the specimen is etched.
 PITS are caused by the polishing operation that remove tiny
nonmetallic particles from the metal surface.

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 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.
 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)
 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..

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 Etching is usually performed by subjecting the polished
surface to the chemical action of some appropriate reagent.
 The specimen to be etched is treated by immersion in the
appropriate reagent.
 It is impossible to lay down general rules for the time of
etching. Usually the desired effect will be produced between
ten seconds and two minutes.
 The specimen after etching should be washed in a stream of
running water and subsequently in alcohol or acetone.
 The surface should be dried untouched by holding in a current
of warm air, such as supplied the laboratory shop air supply.
 When selecting etching times, it is more desirable to
under-etch than to over-etch.
 If a specimen, after a first attempt is found to be
insufficiently etched, the etching process can usually be
repeated without further preparation of the surface.
 A specimen that is over-etched can only be corrected by
repolishing and then re-etching for a shorter time.
 The Metallurgical Microscope
 A horizontal beam of light is deflected by a plane glass
reflector, upward and through a microscope objective onto
the surface of the specimen.
 A certain amount of incident light will be reflected from the
specimen surface back through the objective lens system and
then through a second lens system, the microscope eyepiece.
 The total visual magnification obtained by the combination of
a given eyepiece and objective is equal to the product of the
magnifications of the two systems.
 These magnifications are usually marked clearly on the
appropriate parts.
 When examining a metallographic specimen, the
objective of lowest magnifying power should first be
used.
 Subsequently, greater detail of particular areas can be
obtained by using progressively higher magnifications.
 The different objectives are mounted on a rotating
head, so that their focal planes are very nearly at the
same level.
 Thus, after focusing at the lowest magnification, only
small adjustments should be necessary at higher
magnifications.