Two advanced, automated crystal orientation mapping techniques suited for nanocrystalline materials—precession electron diffraction (PED) in transmission electron microscopy (TEM) and on-axis transmission Kikuchi diffraction (TKD) in scanning electron microscopy (SEM)—are evaluated by comparing the orientation maps obtained from the identical location on a 30 nm-thick nanocrystalline tungsten (W) thin film. A side-by-side comparison of the orientation maps directly showed that the large-scale orientation features are almost identical. However, there are differences in the fine details, which arise from the fundamentally different nature of the spot pattern and Kikuchi line pattern in terms of the excitation volume and the angular resolution. While TEM-PED is more reliable to characterize grains oriented along low-index zone axes, the high angular resolution of SEM-TKD allows the detection of small misorientation between grains and thus yields better quantification and statistical analysis of grain orientation. Given that both TEM-PED and SEM-TKD orientation mapping techniques are complementary tools for nanocrystalline materials, one can be favorably selected depending on the requirements of the analysis, as they have competitive performance in terms of angular resolution and texture quantification.

In situ nanomechanical testing in (scanning) transmission electron microscopy provides unique opportunities for studying fundamental deformation processes in materials. New insights have been gained by combining advanced imaging techniques with novel preparation methods and controlled loading scenarios. For instance, by applying in situ high-resolution imaging during tensile deformation of metallic nanostructures, the interplay of dislocation slip and surface diffusion has been identified as the key enabler of superplasticity. Evidence for dislocation pinning by hydrogen defect complexes has been provided by in situ imaging under cyclic pillar compression in a tunable gas environment. And, for the very first time, individual dislocations have been moved around in situ in two-dimensional materials by combining micromanipulation and imaging in a scanning electron microscope.

Surface evolution was studied for strained SrRuO3 films with a nominal 75 nm thickness deposited at various substrate temperatures (650–850 °C). Epitaxial growth of the films was achieved on single TiO2-terminated SrTiO3 (001) substrates by using ion-beam sputtering. The surface morphology of the deposited films was investigated by scanning tunneling microscopy in ambient conditions, and their microstructure was characterized by transmission electron microscopy. The self-organized step-terrace structure was observed for the films deposited at lower than 800 °C, suggesting that the epitaxial growth proceeded by step-flow growth. In particular, each film showed characteristic surface evolutions pertinent to the misfit strain relaxation stage, mostly influenced by the moving segment of misfit dislocations threading up to the surface: surface undulations for the film at the initial stage of relaxation (deposited at 650 °C), circular growth spirals during the relaxation stage (700 °C), and well-ordered step-terrace structure after almost full development of misfit dislocations (750 and 800 °C).

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Mechanisms of misfit strain relaxation in epitaxially grown Bi4-xLaxTi3O12 (BLT) thin films deposited on SrTiO3 (STO) and LaAlO3 (LAO) substrates have been investigated by means of transmission electron microscopy (TEM). The misfit strain of 20 nm thick BLT films grown on STO substrate was relaxed by forming misfit dislocations at the interface. However, cracks were observed in 100 nm thick BLT films grown on the same STO. It was confirmed that cracks were formed because of high misfit strain accumulated with increasing the thickness of BLT, that was not sufficiently relaxed by misfit dislocations. In the case of the BLT film grown on LAO substrate, the magnitude of lattice misfit between BLT and LAO was very small (~1/10) in comparison with the case of the BLT grown on STO. The relatively small misfit strain formed in layered structure of the BLT films on LAO, therefore, was easily relaxed by distorting the film, rather than forming misfit dislocations or cracks, resulting in misorientation regions in the BLT film.

Effects of grain orientation on the electrical polarization and leakage current characteristics of Bi3.25La0.75Ti3O12 (BLT) thin films have been investigated with respect to c-axis off-alignment. The BLT thin films from epitaxially aligned along c-axis to (117) and (014) off-aligned orientations have been successfully grown by using both different electrode materials (Pt and SrRuO3) and heat-treatments. In order to evaluate the crystallinity and the film texture of various off-aligned BLT thin films, X-ray diffraction (XRD) and transmission electron microscopy (TEM) were carried out. The BLT thin films deposited on SrRuO3/SrTiO3 (100) substrate was grown epitaxial c-axis alignment. That is, the c-axis of the film was completely parallel to the substrate normal, resulting in a cube on cube epitaxial relationship with the underlying SrRuO3 film. The corresponding P-E curve showed nearly paraelectric property. The polycrystalline (117) and (014) oriented BLT thin films revealed that remnant polarization increased remarkably due to the anisotropy of spontaneous polarization of BLT. The surface roughness of BLT thin films was increased to result in degraded leakage current characteristic. According to the present results, it can be concluded that the grain orientation of BLT thin films is a crucial factor controlling the polarization properties and leakage current characteristics.

The microstructural characteristics of ion-beam-sputtered conductive SrRuO3 films, such as interfacial reactions, which govern growth behavior, defects, and thermal stability, were investigated using transmission electron microscopy. On a Si substrate, two binary constituents of SrRuO3, i.e., SrO and RuO2 were shown to have quite different reaction behaviors. The reduction of the RuO2 constituent to elemental Ru by Si led to an unstable contact of SrRuO3 on the Si substrate. Possible reaction thermodynamics are suggested, which are based on the formation energies of the corresponding reactions. In the case of films grown in an oxygen-deficient atmosphere, stacking faults were observed. The stacking faults originated from twinning on the {111}pc plane to accommodate the oxygen deficiency in the growth atmosphere by changing the arrangement of RuO6 octahedra from corner to one of face sharing.

Interfacial reactions between SrRuO3 films and Si substrate were investigated by using field emission-transmission electron microscopy (FE-TEM). The compositional and structural variations across the interface were analyzed by using energy dispersive X-ray spectroscopy (EDS) and diffraction with an electron probe in 0.5 nm in diameter. Two constituent binary oxides of SrRuO3, i.e. SrO and RuO2, were found to react differently on Si surface: 1) SrO in stable contact with Si, and 2) RuO2 in unstable contact. The reduction of SrRuO3 to elemental Ru by Si is believed to be most favorable candidate for the reaction leading to the unstable contact of SrRuO3 on Si.