10 Metallography

Metallography is the branch of science dealing with the study of the constitution and structure of
metals and alloys, its control through processing, and its influence on properties and behaviour. The
original implementation of this science was limited by the resolution of the reflected light microscope
used to study specimens. This limitation has been overcome by the development of transmission
and scanning electron microscopies (TEM and SEM). The analysis of X-rays generated by the
interaction of electron beams with atoms at or near the surface, with wavelength or energy-dispersive
spectroscopy (WDS, EDS) with SEM, electron microprobe analysis (EMPA) or TEM has added
quantitative determination of local compositions, e.g., of intermediate phases, to the deductions based
upon observations. Introduction of metrological and stereological methods, and the development of
computer-aided image analysers, permits measurement of microstructural features. Crystallographic
data can be obtained using classic X-ray diffraction methods using a diffractometer, or diffraction
analysis can be performed with the TEM using selected area or convergent-beam electron diffraction
(SAD and CBD) techniques, and more recently with the SEM with the orientation-imaging (EBSD)
procedure. There is a wide variety of very sophisticated electron or ion devices that can be utilised
to characterise surfaces and interfaces, but these devices are generally restricted in availability due
to their high cost.
Conventional light-optical techniques are still the most widely used and are capable of providing
the information needed to solve most problems. Examination by light optical microscopy (LOM)
should always be performed before use of electron metallographic instruments. LOM image contrast
mechanisms are different from electron microscopy (EM) imaging modes. Natural colour can not
be seen with EM devices. Microstructures are easier to study at low magnification with the LOM
than with the SEM. The LOM examination may indicate the need for SEM or TEM analysis and
determine the locations for such work. Interpretation of LOM examination results is enhanced and
reinforced by the use of electron metallographic techniques. The SEM has become ubiquitous in the
metallographic laboratory.
Important Safety Note: The metallographic laboratory can involve a number of serious hazards,
that can lead potentially to fatalities. For example, many of the reagents used in the preparation of
metallographic etchants are highly corrosive (hydrofluoric acid severely attacks the bone) and/or
extremely toxic. These reagents are frequently inflammable and in some cases are explosive (e.g.,
picric acid). It is especially important to understand that, often, the etchant can possess hazards
that are greater and/or different from those of the reagents from which it was prepared (e.g., some
perchloric acid based solutions pose a much greater explosion risk than others). Some etchants (e.g.,
those containing hydrofluoric acid) can be extremely hazardous even when dilute. All etchants have
a limited shelf life and some require special storage precautions. In some cases (e.g., glyceregia),
etchants cannot be stored safely and must be made up freshly at each use. Identifying a safe and legal
method of disposal of used or discarded etchants requires consideration of all of their ingredients.
Given the risks involved, metallographic specimen preparation requires both suitable operating
conditions/safety equipment and appropriate training for the metallographer. This chapter points out
some of the hazards associated with specific etchants, but is not intended as a substitute for either
a detailed laboratory safety manual or reading of the regulations in force in the metallographer’s
location. A discussion of etchant safety may be found in Petzow1 and various other references given
in the present section.

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