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
To reveal the general structure of
large areas of a specimen
Equipment: binocular microscope

Magnification: 10x

MACROGRAPH: a sketch of the
etched surface of the specimen
made from a macroscopic
examination

PHOTOMACROGRAPH: a
photograph of the etched surface
made from a macroscopic
examination
To gain a representative view of
microstructure
Equipment: metallurgical
microscope
Magnification: 25x to 50x
100x to 1000x
METALLOGRAPH: a
metallurgical microscope
equipped to photograph
microstructures and produce
photomicrographs.
PHOTOMICROGRAPHS: a
photographs of microstructure

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MACROSCOPIC MICROSCOPIC
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 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.

A well-prepared metallographic specimen is:
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
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DIRECTION OF WORK
TRANSVERSE
SECTION
LONGITUDINAL
SECTION
MICROSTRUCTURE
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
DIRECTION OF WORK
TRANSVERSE
SECTION
RADIAL
LONGITUDINAL
SECTION
MICROSTRUCTURE
MICROSTRUCTURE
TANGENTIAL
LONGITUDINAL
SECTION
Figure 2: Longitudinal & transverse orientations of specimens
from a worked metal exhibit different microstructures.

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.
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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
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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TAKING SAMPLE
Sectioning/ Specimen Selection
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)

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
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.
Common Etchants
There are a number of more common etching solutions.
Several of them are listed in the following table.
The following table lists the most commonly used etchants


Etchant Composition Conc. Conditions Comments
ASTM No. 30
Ammonia
Hydrogen Peroxide
(3%)
DI Water
62.5 ml
125 ml
62.5 ml
Mix Ammonia and
water before adding
peroxide. Must be
used fresh. Swab 5-
45 seconds
For etching copper, copper
alloys and copper-silver
alloys.
Adler Etchant
Copper ammonium
chloride
Hydrochloric acid
Ferric chloride,
hydrated
DI Water
9 grams
150 ml
45 grams
75 ml
Immersion is
recommended for
several seconds
For etching 300 series
stainless steel and other
superalloys
Carpenters
Stainless
Steel Etch
FeCl3
CuCl2
Hydrochloric acid
Nitric acid
Ethanol
8.5 grams
2.4 grams
122 ml
6 ml
122 ml
Immersion etching
at 20 degrees
Celsius
For etching duplex and
300 series stainless steels.
Kalling's No. 2
CuCl2
Hydrochloric acid
Ethanol
5 grams
100 ml
100 ml
Immersion or
swabbing etch at 20
degrees Celsius
For etching duplex and
400 series stainless steels
and Ni-Cu alloys and
superalloys.
Kellers Etch
Distilled water
Nitric acid
Hydrochloric acid
Hydrofluoric acid
190 ml
5 ml
3 ml
2 ml
10-30 second
immersion. Use only
fresh etchant
Excellent for aluminum
and titanium alloys.
Etchant Composition Conc. Conditions Comments
Klemm's
Reagent
Sodium thiosulfate
solution
Potassium
metabisulfite
250 ml
Saturated
5 grams
Etch for a few
seconds to minutes
For etching alpha-beta
brass, bonze, tin, cast iron
phosphides, ferrite,
martensite, retained
austenite, zinc and steel
temper embrittlement.
Krolls
Reagent
Distilled water
Nitric acid
Hydrofluoric acid
92 ml
6 ml
2 ml

Swab specimen up
to 20 seconds
Excellent for titanium and
alloys.
Nital
Ethanol
Nitric acid
100 ml
1-10 ml
Immersion up to a
few minutes.
Most common etchant for
Fe, carbon and alloys
steels and cast iron -
Immerse sample up from
seconds to minutes; Mn-
Fe, MnNi, Mn-Cu, Mn-Co
alloys.
Marble's
Reagent
CuSO4
Hydrochloric acid
Water
10 grams
50 ml
50 ml
Immerse or swab
for
5-60 seconds.
For etching Ni, Ni-Cu and
Ni-Fe alloys and
superalloys. Add a few
drops of H2SO4 to
increase activity.
Etchant Composition Conc. Conditions Comments
Murakami's
K3Fe(CN)6
KOH
Water
10 grams
10 grams
100 ml
Pre-mix KOH and
water before adding
K3Fe(CN)6
Cr and alloys (use fresh
and immerse); iron and
steels reveals carbides; Mo
and alloys uses fresh and
immerse; Ni-Cu alloys for
alpha phases use at 75
Celcius; W and alloys use
fresh and immerse; WC-Co
and complex sintered
carbides.
Picral
Ethanol
Picric acid
100 ml
2-4 grams
Seconds to minutes
Do not let etchant
crystallize or dry
explosive
Recommended for
microstructures containing
ferrite, carbide, pearlite,
martensite and bainite.
Also useful for magnetic
alloys, cast iron, high alloy
stainless steels and
magnesium.
Vilellas
Reagent
Picric Acid
Hydrochloric acid
Ethanol
1 gram
5 ml
100 ml
Seconds to minutes
Good for ferrite-carbide
structures (tempered
martensite) in iron and
steel
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.