Round robin on indentation fracture resistance of silicon carbide ceramics by using a powerful optical microscope

Reproducibility of indentation fracture resistance, K_IFR of silicon carbides sintered with B and C was evaluated by a round robin with ten laboratories. When the crack length was measured with an optical microscope at a low magnification of ～100×, K_IFR varied widely from 3.43 to 4.20 MPa m^1/2, whereas those obtained by a powerful microscopy with both an objective lens of 40× and a traveling stage exhibited a consistent value of 3.20±0.12 MPa m^1/2. The wide scatter of K_IFR for the former measurements was attributed mainly to the variation in misreading of the crack length. It was revealed that the high resolving power of the objective lens of 40× enabled to find exact crack tips easily, which resulted in the good matching of K_IFR between laboratories for the latter case. It was suggested that the observation of indentations with powerful optics was effective for improving the reproducibility of the IF method.     

Perpendicular oriented cylinders via directional coalescence of spheres embedded in block copolymer films induced by solvent annealing

Polystyrene-b-poly(methyl acrylate) (PS-b-PMA) block copolymer with PS volume fraction of 25.2 vol% was synthesized by atom transfer radical polymerization. Non-pretreated silicon wafers were used as the substrates to prepare perpendicular oriented PS cylinders in PMA matrix via solvent annealing which could induce the transformation of spheres to vertically oriented and hexagonally packed cylinders. The spherical microdomains were formed after the evaporation of solvents from the solutions of the block copolymer in selective solvents mixed from methanol, acetone and dichloromethane. The thickness of films could be as thick as 1000 nm, which were much thicker than usual cases and the cylinders came from the directional coalescence of the spheres, thus any pre-treatments of the substrates were not required for perpendicular orientation. The structures were characterized by small angle X-ray scattering (SAXS), transmission electron microscope (TEM), atom force microscopy (AFM) and grazing incidence small angle X-ray scattering (GISAXS).     

Thermoreversible behavior of κ-carrageenan and its apatite-forming ability in simulated body fluid

Osteoconductive materials with self-setting ability have received much attention because their properties allow developing injectable materials for bone defects. Thermosensitive hydrogel with ability of bone-like apatite formation in a body environment is a candidate of injectable bone fillers with osteoconductivity because the apatite formation on materials is an essential to show osteoconduction. The present study focused on the development of a thermosensitive hydrogel through modifications of the sulphonic groups of the polysaccharide, κ-carrageenan, with potassium chloride (KCl) and calcium chloride (CaCl₂). We found that the gelation temperature of κ-carrageenan solutions increased with increasing amounts of K⁺ ions. Apatite formation was observed on the gel after exposure to simulated body fluid for 0.5 day when the gel was prepared with a molar ratio of Ca²⁺/sulfonic groups = 1.5. These results indicate that a thermosensitive κ-carrageenan hydrogel with apatite-forming ability was obtained through the incorporation of K⁺ and Ca²⁺ ions into the solution.     

Microstructural analysis of the stir zone of Al alloy produced by friction stir spot welding

The present study applied friction spot joining (FSJ), which was recently developed as a lap joining technique of Al alloys, to two sheets of Al alloy 6061, 1 mm in thickness, and then examined the microstructural feature in the weld. The weld had the nugget-shaped stir zone around the exit hole of the probe, and the stir zone exhibited the equiaxed grain structure having finer grain size than that of the base material. The crystallographic texture analysis using electron backscattered diffraction method suggested that the material movement occurred along the rotating direction of the welding tool in the wide region including the stir zone. In the periphery of the nugget-shaped stir zone, which was characterized as the region having the finer grain size than that of the stir zone interior, any inclusions and precipitates were not found in the SEM scale. The weld was softened around the weld centre. The softening could be explained by dissolution and/or growth of the strengthening precipitates due to thermal cycle of FSJ.     

Effect of heat treatment temperature on the microstructure and actuation behavior of a Ti–Ni–Cu thin film microactuator

Ti–Ni–Cu/SiO₂ two layer diaphragm-type microactuators were fabricated by sputter deposition and micromachining. The influence of heat treatment temperature on the actuation behavior was investigated under quasi-static conditions. The interfacial structure of Ti–Ni–Cu/SiO₂ and internal structure of the Ti–Ni–Cu layer were also investigated using transmission electron microscopy. The reaction layer formed between the Ti–Ni–Cu and SiO₂ layers, and preferentially grew into the SiO₂ side. The reaction layer formed at 1023 K mainly consisted of Ti₄(Ni,Cu)₂O. The maximum height of the diaphragm decreased with increasing heat treatment temperature. The growth of the reaction layer also affected the microstructure of the Ti–Ni–Cu layer. The density of fine platelets and Ti₂Ni precipitates decreased with increasing heat treatment temperature from 873 to 923 K, and they disappeared at 973 K due to the fact that the reaction layer mainly consisted of a Ti-rich phase. The microactuator heat treated at 973 K showed the highest transformation temperature with the lowest transformation temperature hysteresis, which is attractive for high speed actuation.     

Determining surface orientations of transparent objects based on polarization degrees in visible and infrared wavelengths

Techniques for modeling an object through observation are very important in object recognition and virtual reality. A wide variety of techniques have been developed for modeling objects with opaque surfaces, whereas less attention has been paid to objects with transparent surfaces. A transparent surface has only surface reflection; it has little body reflection. We present a new method for obtaining surface orientations of transparent surfaces through analysis of the degree of polarization in surface reflection and emission in visible and far-infrared wavelengths, respectively. This parameter, the polarization degree of reflected light at the visible wavelengths, is used for determining the surface orientation at a surface point. The polarization degree at visible wavelengths provides two possible solutions, and the proposed method uses the polarization degree at far-infrared wavelengths to resolve this ambiguity.     

Enhancement of bonding strength by graded structure at interface between apatite layer and bioactive tantalum metal

Tantalum metal is a candidate for use as an implant material in high load-bearing bony defects, due to its attractive features such as high fracture toughness and high workability. This metal, however, does not have bone-bonding ability, i.e. bioactivity, and therefore the development of bioactive tantalum metal is highly desirable. It is known that the essential prerequisite for an artificial material to show bioactivity is to form a bonelike apatite layer on its surface in the body environment. The same type of apatite layer is formed in a simulated body fluid (SBF) with inorganic ion concentrations nearly equal to those of human blood plasma. The present authors previously showed that the apatite formation on tantalum metal in SBF was remarkably accelerated by treatment with 0.5 M-NaOH aqueous solution and subsequent firing at 300 °C, while untreated tantalum metal spontaneously formed the same apatite after a long soaking period. In the present study, the bonding strength of the apatite layer to the substrate was quantitatively evaluated in comparison with that to the untreated tantalum metal. Adhesive strength was measured as an estimation of bonding strength, and the surface microstructure of both the substrates was characterized in order to discuss the difference in the bonding strength in terms of surface structure. The apatite layer formed on the NaOH- and heat-treated tantalum metal shows higher adhesive strength than that formed on the untreated metal. The amorphous sodium tantalate layer formed on the tantalum metal by NaOH and heat treatments, has a smooth graded structure where its concentration gradually changes from the surface into the interior metal. Smooth graded structure with complex of apatite is constructed after soaking in SBF. The higher bonding strength of the apatite layer formed on the treated metal is attributed to its smooth graded structure.     

Electrode conditioning characteristics in vacuum under impulse voltage application in nonuniform electric field

In this paper, we quantitatively investigated the impulse conditioning mechanism under nonuniform electric field electrodes in a vacuum. A negative standard lightning impulse voltage was applied between rod and plane electrodes whose materials were Cu-Cr, stainless steel and Cu and the gap lengths were d=5 and 10 mm, respectively. Experimental results revealed the transition of the breakdown (BD) sport region on the rod electrode and the corresponding BD field strength in the conditioning process. As a result, we found that the BD spot region started at the tip of the rod electrode and moved to the wider region of the rod electrode with lower electric field as the shots of the voltage application increased before the saturation of the BD voltage. Finally, by analyzing the results with an electric field strength, we propose that "the conditioning degree" along the electrode surface distributed directly proportional to the electric field distribution under a nonuniform electric field in a vacuum, irrespective of the electrode materials