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Metallography is the study of the physical structure andcomponents of metals, typically using
microscopy.
Precision metallurgical sample preparation is a key step in performing reliable metallurgical
testing.
Facilitate examination and interpretation of micro structural features.
Ex. To find out various phase present in material.
Improper preparation methods may obscure features, and even
Coarse Grinding
For a perfect observation sample, it must :
Be free from scratches, stains and others imperfections which tend to mark the
surface.
Retain non-metallic inclusions.
Reveal no evidence of chipping due to brittle intermetallic compounds and phases.
Be free from all traces of disturbed metal.
The purpose of the coarse grinding stage is to generate the initial flat surface necessary for the
subsequent grinding and polishing steps.
Course grinding can be accomplished either wet or dry using 80 to 180 grit
electrically powered disks or belts.
Care must be taken to avoid significant heating of the sample.
Grinding belt material is usually made of SiC paper.
Rotate the specimen by 90⁰ on every grade change
Polishing
Polishing involves the use of abrasives, suspended in a water solution, on a cloth-covered
electrically powered wheel.
In intermediate polishing, SiC paper of different grades are used. Again, the specimen is rotated
while switching from one grade to another. The operation is carried out on a disc with the
sandpaper stretched across it.
Following the final 600 grit fine-grinding stage, the sample must be washed and carefully dried
before proceeding to the first polishing stage.
Beginning with 25-micron suspended aluminium oxide particles (suspended in water) on a Nylon-
cloth, the final fine-grinding surface layer resulting from the previous grinding procedure should
be completely removed with a rotation rate of 150-200 rpm.
Wash the specimen and move on to finer suspended particles on separate cloth.
The final polishing stage with 1-micron suspended aluminium oxide or diamond particles should
be carried out on a separate polishing wheel at a slower speed of 100 - 150 rpm using a napped
cloth. After 1 or 2 minutes a properly polished specimen should have a mirror-like surface free of
scratches
Polishing Cloth
There are three types of polishing clothes; Woven, Non-Woven and Flocked.
Woven cloths offer ‘hard surface’ polishing properties and guarantee flat prepolishing, without
deterioration of the edges.
Non-woven cloths are used on very hard materials for high precision surface finishing such as
glass, quartz, sapphire and semi-conductors.
The Flocked cloths, guarantee a super-polished finish. The polishing duration must be as short as
possible, to avoid inclusions from being extracted.
Etching
Metallographic etching is the process of revealing micro structural details that would otherwise
not be evident on the as-polished sample.
Etching is not always required as some features are visible in the as-polished condition such as
porosity, cracks and inclusions, for eg, in grey cast iron.
Properties revealed by etching
grain size
Segregation
shape, size, and distribution of the phases
mechanical deformation
The specimen after polishing needs to be properly washed and cleaned with distilled water and
after proper drying, the etching reagent is applied by various methods.
Types of Etching:
Chemical Etching
Electrolytic etching
Heat tinting
a) Polished but unetched surface gives a clean image but no details about the microstructure of the
specimen
b) Etched surface: When the specimen has grains with same orientations, only the grain boundaries are
visible.
c) Etched surface: When the specimen has grains oriented differently, each grain reacts differently to give
varying colours.
Chemical Etching
This typically involves immersing the sample in an etchant such or swabbing the surface with an
etchant. The etchant selectively corrodes micro structural features.
Immersion time or etching time is highly dependent on the system and in most cases requires
experience.
The reactivity of a grain is dependent on the orientation of its microstructure.
Deeper etches are preferred for low magnification examinations, while shallow etches are
preferred for higher magnification etches.
Electrolytic Etching
In electrolytic (anodic) etching, electrical potential is applied to the specimen using an external
circuit
During electrolytic etching, positive metal ions leave the specimen surface and diffuse into the
electrolyte
Typical examples are platinum, graphite and stainless steels.
Heat tinting
Process of oxidizing a sample in a furnace. This induces oxidation of surface features at different
rates, to reveal various features.
Coloration of the surface takes place at different rates according to the reaction characteristics of
different elements
The observed interference colours allow the differentiation of phases and Grains
Final step
After etching process, the specimen needs to be washed again in distilled water to remove any
excess reagent present on it.
If not washed, under microscopic observation, there might be aberrations in the colour of the
sample.
Also, slow and continuous reaction for a long time may take place because of which we cannot use
the sample for proper microscopic observation.
Cleaning can also be done by placing a drop of spirit and drying it.
After washing, it can be dried using a low power blower.
Finally, the specimen is ready for observation under microscope.