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Introduction
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Correspondence to: Mr. Shankha Pathak, Deputy Manager, Texmaco Rail &Engg. Ltd.
E- mail: dgpkid@yahoo.com
Pathak S et al.
Properties
Phase / Compound
Ferrite
Austenite
Pearlite
Martensite
Cementite
Uses
Color / Texture
White
White / Yellow
Black , Lamellar
Black and white ,
Acicular
White
Table 1.Color and Texture of Different Phases after Etching with 2% Nital
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Pathak S et al.
Rough preparation.
Polishing.
Etching.
Rough Preparation
If the sample is not flat, it is necessary to remove
some material on the lathe or grinding machine
first. After it, the sample should be moved forward
and backward on the paper until the whole surface
is covered with unidirectional scratches. It is then
washed with running water to remove debris
associated with the grade of paper used. It is then
ground on the next finer paper such that the
scratches produced are at right angles to those
formed by the previous paper. This helps to easily
decide when the scratches from the coarser paper
have been completely removed. This procedure is
repeated through a range of papers. When the
specimen has been ground on the final paper, it is
generally worthwhile rotating it through and
grinding again with less pressure than before. This
technique can decrease the time required for the
next stage, which is polishing.
Polishing
Due to the very small depth of field obtained from
an optical microscope, it is essential that the
surface is optically flat, acting as a perfect mirror
which is why the specimen has to be polished.
This is done using rotating wheels covered with a
J. Adv. Res. Manu. Mat. Sci. Metall. Engi. 2015; 2(1): 1- 9.
Etching
After examining the specimen in as polished
condition for the optimum surface quality, the
specimen should be etched with suitable etchants
to develop additional contrast to reveal the
microstructure.
Theory of Etching
Metallographic etching is the use of chemical
solutions known as etchants to create contrast
between the elements of the metal's microstructure
by selectively corroding some of those elements,
which show up as darker regions, used to highlight
features of metals at microscopic levels. This is
possible because differences in the composition,
structure or phase of a metal will create
electrochemical potentials that alter the relative
rates of corrosion when exposed to an etchant.
The features highlighted by etching include grain
boundaries, phase differences and inclusions.
Expose grain boundaries: The boundaries of
metallic grains can corrode very quickly when the
appropriate etchant is used, highlighting the edges
of the grains and making it possible to determine
their size and shape.
Highlight metallic phases: Different phases will
have different shading and texture after etching,
allowing for phase fraction estimation and
identification of undesirable phases.
Identify inclusions: Nonmetallic inclusions often
have characteristic shapes and colorations after
appropriate etching, which allows for quick size
measurement and number density estimation.
By studying the character, quantity and
distribution
of
these
different
features,
metallurgists are capable of predicting and
explaining physical properties and performance
failures of a given sample of metal.
Three main etching processes used
metallographic sample preparation are:
in
Chemical etching
Wet etching
Dry etching
Electrolytic etching
Heat tinting
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Pathak S et al.
Chemical Etching
This typically involves immersing the sample in
an etchant or swabbing the surface with an
etchant. The etchant selectively corrodes
microstructural features. Immersion time or
etching time is highly dependent on the system.
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. Based on the reagents used
and the techniques used, chemical etching is
divided into wet etching and dry etching.
Wet Etching
Wet etching is the use of chemical solution to
dissolve a material when immersed in it. A wet
etching process involves multiple chemical
reactions that consume the original reactants
and produce new reactants. The wet etch
process can be described by three basic steps.
(1) Diffusion of the liquid etchant to the
structure that is to be removed. (2) The reaction
between the liquid etchant and the material
being etched away. A reduction- oxidation
(redox) reaction usually occurs. This reaction
entails the oxidation of the material then
dissolving the oxidized material. (3) Diffusion
of the byproducts in the reaction from the
reacted surface. This is a simple technology
which requires only a container with a liquid
solution that will dissolve the material in
question. It will give good results if a
combination of etchant and mask material can
be found to suit our application. But
unfortunately, there are complications since
usually a suitable mask that does not dissolve
or at least etches much slower than the material
to be patterned, needs to be found out. Wet
etching works very well for etching thin films
on substrates, and can also be used to etch the
substrate itself. The problem with substrate
etching is that isotropic processes will cause
undercutting of the mask layer by the same
distance as the etch depth. Anisotropic
processes allow the etching to stop on certain
crystal planes in the substrate, but still results
in a loss of space, since these planes cannot be
vertical to the surface when etching holes or
cavities. To get rid of this limitation, dry
etching must be considered.
Dry Etching
In dry etching, plasmas or etchant gases
remove the substrate material. The reaction that
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I.
II.
III.
Electrolytic Etching
Electrolytic etching involves the use of the anodic
compartment as the specimen to be etched and the
cathodic compartment as a material that is
conductive but highly insoluble in the electrolyte
used. Typical examples of the materials that are
generally used as the cathode are platinum and
graphite. Most electrolytic etching processes use
direct current electrolysis. Since, oxidation occurs
at the anode, therefore, specimen to be etched gets
oxidized in the process.
Pathak S et al.
Heat Tinting
Heat tinting, sometimes called thermal etching, is
the process of oxidizing a sample in a furnace.
Due to difference in oxidation rates of different
parts of the sample surface, various structures are
revealed.
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Pathak S et al.
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decomposition
of
hydrogen
peroxide:
2H2O2 2H2O + O2. So, as a whole, both oxygen
and chlorine which are very good oxidizing agents
for iron are released during the course of the
reaction. H2O acts as a wetting agent.
Etching time: 5-10 sec.
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Pathak S et al.
KOH+HCIKCL+H2O
MnO2 + 4 HClMnCl2 + 2 H2O + Cl2 (Good
oxidizing agent)
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Conclusion
By studying and comparing all the micrographs, it
is evident that reagent 3 and reagent 4 revealed
high manganese austenitic steel microstructure
most prominently. However, with reagent 4, grain
Conventional
Low clarity
Very uncertain for High
Manganese austenitic
steel
Lightly etched grain
boundary
Twins may be / may not
be detected
High etching time
Less rate of corrosion
References
1. Nayak AP, Logeeswaran VJ, Islam MS.
University of California, Davis. California.
2. Vander Voort GF. ASM Handbook
Metallography and Microstructure. Volume
9:493512.
3. Grajcar A, Krukiewicz W, Koodziej S.
Corrosion behaviour of plastically deformed
high-Mn austenitic steels. JAMME Nov
2010; 43(1): 228- 35.
4. Walker P, Tarn WH. Handbook of Metal
Etchants.
5. Reiter J, Bernhard C, Presslinger H.
Austenite grain size in the continuous casting
process: Metallographic methods and
evaluation. Material Characterization Jun
2008; 59(6): 737- 46.
6. Mukhopadhyay SM. Sample preparation for
Microscopic
and
spectroscopic
characterization of solid surface and films.
Department of Mechanical and Materials
Engineering, Wright State University,
Dayton, Ohio.
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