A novel technique has been developed to examine site-specific, subsurface microstructures in three dimensions. A 3D data set is collected by successive cross-sectional slicing using a gallium focused ion beam (FIB) and imaging using ion-induced secondary electrons, enabling a 3D microstructure map to be generated using computer-based reconstruction techniques. In the first instance, this 3D FIB mapping technique has been applied to copper-based epitaxial metal multilayer coatings which have been deformed by nanoindentation. It is possible to produce 3D profiles of the deformed subsurface interfaces. These individual interface maps allow analysis of the deformation in terms of both the thickness of individual layers and that of the entire film. Material flow, which is seen as pile-up and residual indent zones around the indent, can thus be precisely characterised. The site at which the sectioning is to be carried out can be chosen with high spatial resolution; consequently, nanoscale mechanical properties can be linked directly with an area's microstructure.
In an attempt to examine the errors involved in this 3D mapping method the 3D FIB map of the surface of a residual indent has been compared to an atomic force microscopy (AFM) scan of the same region. The sources and significance of the errors are discussed with reference to ways in which they might be reduced.