PREPARATION OF SPECIMEN FOR MICROSCOPIC EXAMINATION

 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

Cutting and Slicing of sample:

 It is important to study something that is representative of the whole specimen.
 Cutting of that representative part must also be done very carefully.
 Operations such as shearing produce severe cold work, which can alter the microstructure of a
sample
 Abrasive cutting (sectioning) offers the best solution to eliminate these undesirable features; the
resultant surface is smooth, and the sectioning task is quickly accomplished.
 Low-speed cut-off wheels are utilized in cases where the heat created by standard abrasive cutters
must be avoided. Ample coolant and proper speed control are essential in all sectioning
operations..
Mounting:
 When the specimen to be tested is inexpensive and easily available, a suitable size specimen may
be cut and polished for examination.
 Mounting of specimens is usually necessary to allow them to be handled easily. It also minimises
the amount of damage likely to be caused to the specimen itself.
 Properties of mounting material
 Should not influence the specimen as a result of chemical reaction
 Should not impart any mechanical stresses
 Should adhere well to the specimen
 Specimens can be hot mounted (at around 200 °C) using a mounting press,either in a
thermosetting plastic (e.g. phenolic resin), or a thermo-softening plastic (e.g. acrylic resin).
 If hot mounting will alter the structure of the specimen a cold-setting resin can be used, e.g. epoxy,
acrylic or polyester resin.
 A mounted specimen usually has a thickness of about half its diameter, to prevent rocking during
grinding and polishing.
 The edges of the mounted specimen should be rounded to minimise the damage to grinding and
polishing discs.

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.