Ka. Pischow et al., ION-BEAM ETCHING TECHNIQUE IN THE PREPARATION OF SAMPLES FOR CROSS-SECTIONAL MICROSCOPY STUDIES OF THIN-FILMS AND HARD COATINGS, Surface & coatings technology, 67(1-2), 1994, pp. 95-104
The scanning tunneling microscope has proved to be an effective tool i
n the structure characterization of interfaces and interlayers in thin
films and coatings. However, since it lacks the deep profiling capabi
lities sufficient to penetrate hard coatings, an ion beam etching meth
od has been developed for cross-sectional sample preparation. The samp
le preparation method is developed keeping in mind the image formation
of a scanning tunneling microscope which is based on the topographica
l differences of the inspected surface. Thus the sample preparation pr
ocess includes three main parts. Firstly, a mechanical grinding and po
lishing step, secondly, an ion beam polishing step for producing a smo
oth surface and, thirdly, an ion beam etching step for producing a top
ography related to the bulk microstructure of the sample. Examples of
results obtained with TiN hard coatings are given, including X-ray sca
nning force microscopy pictures of a tribofilm grown on a TiN-coated c
ast iron sample during a high temperature wear test; the usefulness of
the developed technique is discussed. The results achieved are compar
ed with the structural information obtained by X-ray transmission elec
tron microscopy analysis from the same samples.