In situ nanoindentation in a transmission electron microscope

This dissertation presents the development of the novel mechanical testing technique of in situ nanoindentation in a transmission electron microscope (TEM). This technique makes it possible to simultaneously observe and quantify the mechanical behavior of nano-scale volumes of solids.; Chapter 2 details the unique specimen preparation techniques employed to meet the geometrical constraints of the in situ experiments. These techniques include bulk silicon micromachining and the use of a focused ion beam. In section 2.4 a method of voltage-controlled mechanical testing is derived theoretically and proven experimentally. This method enables the quantification of the mechanical behavior during in situ nanoindentation experiments.; Three classes of material systems were studied with this new technique: (1) bulk single crystal, (2) a soft thin film on a harder substrate and (3) a hard thin film on a softer substrate. Section 3.2 provides the first direct evidence of dislocation nucleation in single crystal silicon at room temperature. In contrast to the observation of phase transformations during conventional indentation experiments, the unique geometry employed for the in situ experiments resulted in dislocation plasticity. In section 3.3 results from in situ nanoindentation of Al films on Si substrates are presented. These results include the correlation of the microstructural deformation behavior with load vs. displacement data. It is shown that a sharp change in the force-displacement response at the elastic-to-plastic transition signifies the nucleation of dislocations. Additionally, the softening of sub-micron grains with size is observed. Section 3.4 discussed the influence of the substrate on the indentation response of two thin film/substrate systems where the films were harder than the substrate. Amorphous diamond on Si and epitaxial TiN on MgO (001) systems were studied. It was found that the deformation in the harder films was controlled by the deformation in the softer substrates.; The direct observations of each material system during indentation provided unique insight into the interpretation of ex situ nanoindentation tests, as well as to the intrinsic mechanical behavior of nano-scale volumes of solids. These results represent the first real time observations of the discrete microstructural events that occur during nanoindentation.