METHODOLOGY FOLLOWED

¾ In-situ Metallography Work (Replica Test):

Replica test is done at selected locations on the components to reproduce

accurately the microstructural features such as distribution, size, and morphology
of the carbide precipitates as well as micro-cracks.

The in-situ metallography was conducted using standard metallographic techniques

i.e. by polishing & etching (manual as well as electrolytic) followed by microscopic
examination & replication of microstructures.

1.1 POLISHIN G TECHN IQUE:

1. Collect the nature of components, its materials etc. detail on which insitu
metallography is to be done.

2. Selection of location of insitu work by metallurgist or company’s engineer as

per their requirements of tests.

3. Removing of external scale by rough grinding with the help of a stone wheel
/ abrasive wheel.

4. Do the preliminary polishing by manually using self-adhesive waterproof grit

papers in the sequence of 80, 120, 180, 220, 320, 400 and 600.

After this step, there are two options for further polishing -
5.1 Manual Polishing
Further mirror polishing is done with the help of portable hand polisher
manually using waterproof grit papers in the sequence of 1000, 1200, 1500 &
2000.

Manually polished surface are further subjected to polishing by diamond paste

of 3 microns with the help of self adhesive polishing silvet cloth and
kerosene.

5.2 Electrolytic Polishing

Electrolytic polishing is used with the help of portable electrolytic polisher
to achieve mirror polishing with prescribed voltage and current and standard
solutions. The care is taken that over-heating of electrolyte is avoided as it
causes pitting.

5. Once the mirror surface is prepared, then the surface is etched either by
using electrolyte etching or by manual etching technique with conventional
cotton swab. The etchant is selected based on laboratory experience.

6. After etching the surface, it is viewed under portable microscope at 100X /

400 magnification to ensure proper quality of microstructure. The care is
taken to preserve this microstructure for immediate replication.
1.2 REPLICA TECHN IQUE:

1. First of all, replica film is softened by Acetone.

2. Put the soft replica film on the surface where microstructure is prepared.
Care is taken to ensure no air bubble is present between film and metal
surface. Ensure that no dirt or foreign particle is rest on prepared
metallurgical surface.

3. Apply pressure on replica film to impose the microstructure on the film.

4. Apply marker ink on the opposite side of the replica film on which
microstructure is imposed. This is useful to improve the contrast of the
structure.

5. Remove the replica film from the surface and stick it on the slide.

Finally the replica is further studied on the optical / scanning electron microscope
on higher magnification depending upon the inferences required.

Microstructures are designated with respect to the microstructural degradation. This

may be only a diffusional degradation or creep damage, which would have taken
place because of high temperature exposure of the component.
Carbon steels & Cr-Mo alloy steels are subjected to diffusional degradation by
sequential formation of pearlite/ bainite followed by formation of carbides
(spherodisation). For designating the degradation level of microstructures,
following internationally accepted classification methodology is used:

Designated Level Description of microstructure

For Diffusion degradation level:

IL : Minimal tendency to break up of bainite/ pearlite.
II L : Incipient break of bainite & isolated precipitated carbides in
ferrite.
III L : Distinct break up of bainite/ pearlite. Ferrite grows darker due
to carbide precipitation
IV L : Bainite/ pearlite structure visible. Distinct grain boundary
carbides & dot like precipitates in ferrite.
For Creep degradation level:
CIL : Isolated creep cavities
C II L : Oriented creep cavities
C III L : Micro-cracks
C IV L : Macro-cracks

Creep damage is identified by the formation of voids / cavities, micro-

cracks etc. Degradation levels for creep damage are formulated for all
metallic materials in an identical manner.
Similarly, in materials such as Austenitic stainless steels carbide precipitation at
grain boundaries leads to depletion of matrix chromium resulting in loss of
corrosion resistance. Such degradation levels are classified as below:

Designated Level Description of microstructure

Normal Structure – Equi-axed austenitic grains with annealing twins.

(STEP STRUCTURE)

Mild Degradation – Chromium carbide formation at some of the grain

(DUAL STRUCTURE) boundaries.

Severe degradation – Chromium carbide formation at nearly all the grain

(DITCH STRUCTURE) boundaries resulting in formation of ditch structure.

A similar methodology can be followed for any other material.

¾ In-situ Hardness Test (HM):

In-situ hardness testing was carried out on all components operating at high stress
to determine the extent of micro-structural degradation. The locations for hardness
measurements were selected based on results of various other tests as well as on
the locations of replica test. The measurements were taken using a Portable
Hardness Tester. Before using this device, its accuracy and reproducibility was
checked using pre-calibrated standard test blocks.