Electronic structure of AlFeN films exhibiting crystallographic orientation change from c- to a-axis with Fe concentrations and annealing effect.

Wurtzite AlN film is a promising material for deep ultraviolet light-emitting diodes. However, some properties that attribute to its crystal orientation, i.e., c-axis orientation, are obstacles in realizing high efficiency devices. Constructing devices with non-c-axis oriented films is a solution to this problem; however, achieving it with conventional growth techniques is difficult. Recently, we succeeded in growing a-axis oriented wurtzite heavily Fe-doped AlN (AlFeN) films via sputtering. In this article, we report the electronic structures of AlFeN films investigated using soft X-ray spectroscopies. As-grown films were found to have conduction and valence band structures for a film with c-axis in film planes. Simultaneously, it was found that large gap states were formed via N-p and Fe-d hybridization. To remove the gap states, the films were annealed, thereby resulting in a drastic decrease of the gap states while maintaining a-axis orientation. We offer heavy Fe-doping and post annealing as a new technique to obtain non-polar AlN films.

Surface morphology and dislocation characteristics near the surface of 4H-SiC wafer using multi-directional scanning transmission electron microscopy.

To improve the reliability of silicon carbide (SiC) electronic power devices, the characteristics of various kinds of crystal defects should be precisely understood. Of particular importance is understanding the correlation between the surface morphology and the near surface dislocations. In order to analyze the dislocations near the surface of 4H-SiC wafers, a dislocation analysis protocol has been developed. This protocol consists of the following process: (1) inspection of surface defects using low energy scanning electron microscopy (LESEM), (2) identification of small and shallow etch pits using KOH low temperature etching, (3) classification of etch pits using LESEM, (4) specimen preparation of several hundred nanometer thick sample using the in-situ focused ion beam micro-sampling® technique, (5) crystallographic analysis using the selected diffraction mode of the scanning transmission electron microscope (STEM), and (6) determination of the Burgers vector using multi-directional STEM (MD-STEM). The results show a correlation between the triangular terrace shaped surface defects and an hexagonal etch pit arising from threading dislocations, linear shaped surface defects and elliptical shaped etch pits arising from basal plane dislocations. Through the observation of the sample from two orthogonal directions via the MD-STEM technique, a basal plane dislocation is found to dissociate into an extended dislocation bound by two partial dislocations. A protocol developed and presented in this paper enables one to correlate near surface defects of a 4H-SiC wafer with the root cause dislocations giving rise to those surface defects.

STEM and HRTEM studies of accumulated deposits on human tooth surface.

The aim of this study was to clarify the fine structure of accumulated deposits on the surface of teeth that are considered to affect the gloss of teeth. The study was carried out using, as specimens, human incisor teeth having gloss, which were extracted from teenage donors and those incapable of showing gloss even by brushing which were extracted from donors in their 50s. Thin longitudinal sections of tooth enamel with accumulated deposits on the surface were prepared by focused ion beam (FIB) milling, and the fine structure was analyzed using a scanning transmission electron microscope (STEM) and a high resolution transmission electron microscope (HRTEM). By FIB, thin longitudinal sections could be prepared from tooth enamel together with organic and inorganic substances accumulated on the surface without artifacts. The accumulated deposits on the surface of teeth having gloss were composed of organic substances. However, it was first revealed by STEM observation that the accumulated solid deposits on the surface of teeth having no gloss had a complicated structure wherein inorganic and organic substances coexisted. It is suggested that the organic substances contain proteins derived from saliva. The inorganic substances were spherical and needle-like hydroxyapatites (HAs). It is considered that amino acids constituting the proteins affected the nucleus formation and the crystal formation of HA. It is considered that the unevenness of the accumulated deposits existing on the surface of tooth enamel having no gloss causes the decrease in gloss of teeth due to diffuse reflection of light.

Fine structure of tooth enamel in the yellowing human teeth: SEM and HRTEM studies.

OBJECTIVE: The aim of this study was to clarify an influence of the fine structure of human tooth enamel to the yellowing teeth. MATERIALS AND METHODS: Sound maxillary first premolars of 15-50-year-old females that were extracted for the orthodontic treatment were used as the test samples. The tooth enamel sections of these teeth that prepared by ion polishing were observed by scanning electron microscopy (SEM). Furthermore, the fine structure of substance filling the inter-rod spaces was analyzed by high resolution transmission electron microscopy (HRTEM). RESULTS: In white tooth, the inter-rod spaces were observed at the width of about 0.1 µm, while in yellow tooth, the inter-rod spaces were not clearly observed by SEM. HRTEM observations revealed for the first time that the inter-rod spaces were filled with fine particles of poorly crystallized hydroxyapatite in the yellow tooth. In yellow tooth, it was considered that the color of the inner dentin was recognized due to the decrease of light scattering by filling the tooth enamel inter-rod spaces. The generation of particles in the tooth enamel inter-rod spaces was considered to be caused by the long-time progression of calcification. CONCLUSIONS: These results suggested that the change in fine structure, filling in inter-rod spaces of tooth enamel, was related to progression of calcification in the inter-rod spaces with advancing age and one of the factors of yellowness of human tooth.

Intriguing transmission electron microscopy images observed for perpendicularly oriented cylindrical microdomains of block copolymers.

Intriguing images of dislocation structures were observed by the transmission electron microscopy (TEM) technique for hexagonally packed cylindrical microdomains in a block copolymer (polystyrene-block-polyethylenebutylene-block-polystyrene triblock copolymer) film. The polystyrene (PS) cylinders were embedded in the polyethylenebutylene (PEB) matrix and oriented perpendicular to the surface of the thin section for the TEM observations. In order to understand such strange dislocation structures, we applied an image processing technique using two-dimensional Fourier transform (FT) and inverse Fourier transform (IFT) methods. It was found that these intriguing images were not ascribed to real dislocation structures but were fake ones due to the moiré effect caused by the overlapping of hexagons with a slightly mismatched orientation. Furthermore, grain boundaries in the ultrathin section can be identified by image processing using FT and IFT methods.

A metastable phase in thermal decomposition of Ca-deficient hydroxyapatite.

We investigated the microstructural changes on an atomic length scale during thermal decomposition process of Ca-deficient hydroxyapatite (Ca-def HAp) by high-resolution transmission electron microscopy (HRTEM). Ca-def HAp was prepared by hydrolysis of alpha-tricalcium phosphate. The Ca-def HAp had a whisker-like morphology 2-5 microm in length and 0.1 microm in diameter that was elongated along c-axis. Thicker planer defects parallel to the (100) plane of the HAp matrix were observed as precipitation in the sample annealed at 700 and 800 degrees C by HRTEM observation. Thickness of the precipitation was about 10 nm and the boundaries between the precipitation and HAp matrix was coincident. The periodicity in the precipitation was parallel to the (100) plane of the HAp matrix and measured to be 1.42 nm. Since the precipitation was observed only in the sample annealed at a narrow temperature range of 700-800 degrees C, it was regarded as a metastable phase formed on the thermal decomposition process. Absorption peaks in IR spectra of annealed Ca-def HAp containing the metastable phase appeared at 744 and 3538 cm(-1) due to non-stoichiometric HAp with high Ca/P molar ratio. Furthermore, the results of energy dispersive X-ray spectroscopy showed that the metastable phase had higher Ca/P molar ratio than that of the matrix and stoichiometric HAp. Therefore, the metastable phase could be identified as Ca-rich metastable phase. The presence of Ca-rich metastable phase was confirmed to be associated with the thermal decomposition process.