Quantitative Characterization by Transmission Electron Microscopy and Its Application to Interfacial Phenomena in Crystalline Materials.

This paper reviews quantitative characterization via transmission electron microscopy (TEM) and its application to interfacial phenomena based on the results obtained through the studies. Several signals generated by the interaction between the specimen and the electron beam with a probe size of less than 1 nm are utilized for a quantitative analysis, which yields considerable chemical and physical information. This review describes several phenomena near the interfaces, e.g., clear solid-vapor interface (surface) segregation of yttria in the zirconia nanoparticles by an energy-dispersive X-ray spectroscopy analysis, the evaluation of the local magnetic moment at the grain boundary in terms of electron energy loss spectroscopy equipped with TEM, and grain boundary character dependence of the magnetism. The direct measurement of the stress to the dislocation transferred across the grain boundary and the microstructure evolution focused on the grain boundary formation caused by plastic deformation are discussed as examples of material dynamics associated with the grain boundary. Finally, the outlook for future investigations of interface studies, including the recent progress, is also discussed.

Direct Characterization of the Relation between the Mechanical Response and Microstructure Evolution in Aluminum by Transmission Electron Microscopy In Situ Straining.

Transmission electron microscopy in situ straining experiments of Al single crystals with different initial lattice defect densities have been performed. The as-focused ion beam (FIB)-processed pillar sample contained a high density of prismatic dislocation loops with the <111> Burgers vector, while the post-annealed specimen had an almost defect-free microstructure. In both specimens, plastic deformation occurred with repetitive stress drops (∆σ). The stress drops were accompanied by certain dislocation motions, suggesting the dislocation avalanche phenomenon. ∆σ for the as-FIB Al pillar sample was smaller than that for the post-annealed Al sample. This can be considered to be because of the interaction of gliding dislocations with immobile prismatic dislocation loops introduced by the FIB. The reloading process after stress reduction was dominated by elastic behavior because the slope of the load-displacement curve for reloading was close to the Young's modulus of Al. Microplasticity was observed during the load-recovery process, suggesting that microyielding and a dislocation avalanche repeatedly occurred, leading to intermittent plasticity as an elementary step of macroplastic deformation.

Transmission electron microscopy/electron energy loss spectroscopy measurements and ab initio calculation of local magnetic moments at nickel grain boundaries.

We have determined local magnetic moments at nickel grain boundaries using a transmission electron microscopy/electron energy loss spectroscopy method assuming that the magnetic moment of Ni atoms is a linear function of the L3/L2 (white-line ratio) in the energy loss spectrum. The average magnetic moment measured in the grain interior was 0.55 µB, which agrees well with the calculated magnetic moment of pure nickel (0.62 µB). The local magnetic moments at the grain boundaries increased up to approximately 1.0 µB as the mis-orientation angle increased, and showed a maximum around 50°. The respective enhancement of local magnetic moments at the Σ5 (0.63 µB) and random (0.90 µB) grain boundaries in pure nickel was approximately 14 and 64% of the grain interior. In contrast, the average local magnetic moment at the (111) Σ3 grain boundary was found to be 0.55 µB and almost the same as that of the grain interior. These results are in good agreement with available ab initio calculations.

First-principles study of electronic structures and stability of body-centered cubic Ti-Mo alloys by special quasirandom structures.

The electronic structures and structural properties of body-centered cubic Ti-Mo alloys were studied by first-principles calculations. The special quasirandom structures (SQS) model was adopted to emulate the solid solution state of the alloys. The valence band electronic structures of Ti-Mo and Ti-Mo-Fe alloys were measured by hard x-ray photoelectron spectroscopy. The structural parameters and valence band photoelectron spectra were calculated using first-principles calculations. The results obtained with the SQS models showed better agreement with the experimental results than those obtained using the conventional ordered structure models. This indicates that the SQS model is effective for predicting the various properties of solid solution alloys by means of first-principles calculations.

Identification of crack path of inter- and transgranular fractures in sintered silicon nitride by in situ TEM.

Inter- and/or transgranular crack paths in sintered silicon nitride (Si3N4) during fracture were investigated by in situ straining experiments in a transmission electron microscope at room temperature, using a high-precision micro-indenter. By this technique, cracks introduced in an in situ manner were observed to propagate in the grain interior and along grain boundaries. High-resolution electron microscopy (HREM) observation revealed that the crack propagation takes place at an interface between Si3N4 grains and an intergranular glassy film (IGF) in the case of intergranular fractures. According to the results by previous molecular dynamics simulations, a number of dangling bonds are present at the Si3N4/IGF interface, which should result in the observed fracture behavior at the interface. On the other hand, the crack path introduced during transgranular fracture of Si3N4 grains was found to be sharp and straight. The observed crack propagated towards [1120] inside the Si3N4 grain with the crack surface parallel to the (1100) plane. The HREM observations of crack walls revealed them to be atomically flat. The atomic termination of the crack walls was identified in combination with image simulations based on atomic models of the cleaved crack walls.