Sample Preparation

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Sample Preparation
Camera integration time
Background removal
Microscope conditions
Sample tilt
Resolution and accuracy
Summary

Undertaking EBSD experiments

Sample preparation

EBSD is very sensitive to crystalline perfection and sample preparation may be needed to remove any surface damage. A well prepared sample is a prerequisite to obtaining a good diffraction pattern. Surfaces must be sufficiently smooth to avoid forming shadows on the diffraction pattern from other parts of the sample. Suitable techniques for use with EBSD include:

For metals and insulators, mounting in conductive resin, mechanical grinding, diamond polishing and final polishing with colloidal silica.
For metals, mounting in conductive resin, mechanical grinding, diamond polishing and electropolishing.
Brittle materials such as ceramics and geological materials can often be fractured to reveal surfaces immediately suitable for EBSD.
Ion milling for materials which are not amenable to conventional metallography such as zirconium and zircalloy.
Dual focussed ion beam – electron beam microscopes fitted with EBSD can perform in-situ specimen preparation for EBSD.
Plasma etching for microelectronic devices.

Charging in non-conductive samples can be eliminated, as for X-ray microanalysis, by the deposition of a conducting layer. The deposited layer must be very thin – for example 2 to 3 nm of carbon or gold/palladium– otherwise a diffraction pattern will not be obtained. It may be necessary to increase the electron accelerating voltage to penetrate the conducting layer. Charging can be reduced when the sample is tilted for EBSD experiments and can also be reduced by analysing the sample in an environmental or low vacuum SEM.

Further information about sample preparation is given in a separate tutorial.