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Electrolyte Polishing & Etching

Directly polished surfaces can be inspected using EBSD, but in many cases, if the sample is
conductive, the pattern quality is improved by electrolytic polishing.

Electrolytic preparation uses an electrolytic reaction cell containing a liquid electrolyte with two
electrodes: an anode and cathode. The sample to be polished / etched forms the anode. Current is
applied which forces the metal of the anode to dissolve, to wander and deposit itself on the cathode
as a coating. The electrodes are connected to an external power supply and voltage applied to cause
reaction within the cell.

For EBSD of metallic samples only electrolytic polishing is usually adequate, electrolytic etching is
usually not necessary.
Prepared samples using electrolytic polishing

ENLARGE (http://www.ebsd.com/images/articles/29/samples1.jpg)
Shown above is the characteristic curve for an electrolytic cell. This curve is dependent on the
electrolyte used and will vary for different electrolytes. Control of the voltage and current density at
the anode, plus electrolyte composition, temperature and agitation are all critical in achieving the
desired polishing/etching characteristics. Establishing adequate control of these parameters can be
difficult and further, many of the electrolytes are hazardous or even explosive. In the case of the latter,
temperature control is critical. Do not attempt electrolytic polishing or etching without the necessary
experience and safety measures in place.

Factors controlling etching/polishing characteristics include:

Electrolyte composition
Electrolyte temperature
Electrolyte stirring
Area to be polished/etched (current density)
Voltage

Advantages: Disadvantages:

Polishing and etching are possible Conductive specimens only

Fast preparation process Not all alloys can be polished
Is reproducible when the process is automated Preferential attack or pitting can occur
No mechanical deformation and smeared surfaces No edge retention
Can produce excellent surfaces for EBSD Limited polishing area
Limited scratch/material removal
Hazardous Electrolytes
Temperature control vital
Etching

Directly polished surfaces can be inspected using EBSD, but in many cases the pattern quality is
improved by etching. Additionally, etching delineates the grain structure, which is of obvious benefit.
However, etching may attack a second phase preferentially, or attack grain boundaries excessively.
Caution should be exercised when choosing and using etchants. Inspect the sample surface using a
light microscope before and after etching to assess the effect. Materials that are difficult to polish may
benefit from repeated etching and re-polishing. This method can expose an undamaged surface
suitable for EBSD when conventional polishing and etching fails to achieve an adequate surface.
Using special acid or alkali resistant cloths, it is also possible to add dilute etchants to the polishing
cloth during polishing. This can be effective, but can be difficult to control. Some experience is
required. Any etchant that is used must dissolve the specimen surface in an even manner, and not
leave behind any oxide or reaction product layers. Such layers can completely suppress diffraction.
Many etchants listed in metallographic text books are 'contrast etches' which rely on the formation of
different thickness oxide layers to generate colors visible using a light microscope. Therefore such
etchants are generally not suitable for EBSD.

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Explore a 3rd dimension of the sample. 3D EBSD provides a new view of microstructure by complete
description of all grains, grain boundaries, morphological & crystallographic relationships between
grains and phases, and microtextures…

Read More (/ebsd-analysis/types-of-ebsd-experiment/3d-ebsd)

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