QUANTITATIVE MICROSCOPY 4 3 7

treated tool steels, the sample can be fractured and rated using the Shepherd
fracture grain size method.
In low-carbon steels, such as sheet metal, the ferrite grain size is measured
because the parent austenite grains cannot be revealed. The ferrite grain size is
smaller than the parent austenite grains. Only in rare cases can both the ferrite and
austenite grains be revealed in such steels. The morphology of ferrite grains can
vary widely, which will influence the validity of the grain size measurement.
The rating of grain size in austenitic material is difficult when annealing twins
are present. Annealing twins are ignored in such measurements of grain size even
though twin boundaries influence properties and behavior in the same manner as
grain boundaries. In structure-property correlations on such material, it has been
shown that the total interfacial area correlates better with properties than the
grain-boundary interfacial area alone.
In measuring grain size, several procedures can be employed:

Comparison with standard charts

Fracture grain size
Planimetric (Jeffries) method
Intercept (Heyn) method
Snyder-Graff intercept method
Grain size distribution methods

General reviews on grain size measurement are found in Refs. 39 to 42.

Delineation of grain boundaries Methods to reveal austenite grain structures in
steels can employ direct observation, e.g., hot-stage microscopy or electronemission microscopy. Most methods, however, use indirect methods such as those
outlined previously in this chapter. Each of these methods has limited applicability and inherent advantages and disadvantages.
The thermal-etching method of heating a polished sample to the desired
temperature in a vacuum is similar to hot-stage microscopy except that the sample
is observed after it is cooled to room temperature. Thermal grooving occurs at the
grain boundaries because of surface tension effects. A vacuum furnace can be
used, or the polished sample can be encapsulated in an evacuated glass or quartz
tube and heated in an ordinary furnace. Poor grain-boundary contrast is obtained
at temperatures just above the upper critical temperature of the steel. Dark-field
illumination is useful in the examination of such samples. Thermal etching is
applicable to nearly any steel sample and is sometimes referred to as "the method
of last resort."
Another variant of thermal etching involves etching of austenite grain boundaries either in a molten salt bath or in molten glass. Salt baths consisting of equal
parts NaCl, BaCl2 and CaCl2 have been used. After about 10 min at heat in the
bath, the sample is removed and oil-quenched. The adhering salt is removed, and
the sample is repolished and etched in picral. This method is widely applicable but
tends to produce a finer grain size at the surface than in the interior [37], a
common problem with all these surface techniques.