Fabrication and basic characterization of silicon nitride ceramics as an inert matrix

Silicon nitride ceramics containing cerium as a simulating element of americium were fabricated to clarify proper sintering conditions. Basic properties of sintered specimens were evaluated for utilization to an inert matrix. Commercial powders of silicon nitride and cerium dioxide (16 or 24.6 wt%), and a powder of aluminum oxide or zirconium oxide as a sintering additive (5 wt%) for some specimens were mixed by ball milling in ethanol. Small amounts of stearic acid as a lubricant were also added. The mixed powder was uniaxially pressed into cylindrical pellets. Then, the pellets were embedded in a packing powder composed of 50 wt%-Si₃N₄ and 50 wt%-BN, and sintered at 2023 or 2073 K for 2 h in a 0.1 MPa N₂ atmosphere. Most of the sintered specimens had high densities (>95% TD). Sintered bodies consisted of columnar silicon nitride grains and grain-boundary phase. XRD analysis clarified that the grain-boundary phase contained crystalline compounds of cerium. The thermal conductivities of sintered specimens except for specimens containing aluminum oxide were about 40 W/m K at room temperature.     

Fabrication of glass-coated electrodes with nano- and micrometer size by means of dissolution with HF

Platinum nano-electrodes were fabricated at the success rate 76% by the six processes; (i) etching a Pt wire in ethanol-water mixture, (ii) sealing it with a glass sheath, (iii) grinding roughly the glass tip, (iv) polishing the tip while monitoring the capacitive ac current flowing through the glass thin film on the Pt, (v) dissolving the glass film in HF solution until a part of Pt was exposed, and (vi) heating the tip at 85 °C for stabilization. A key of the process was to make a thin glass film on the Pt tip (iv) and to expose the Pt surface chemically by (v). 50 electrodes thus fabricated had diameters ranging from 1 nm to 5 μm, estimated from the steady-state diffusion-controlled current of ferrocene in acetonitrile and ferrocenyl derivative in aqueous solution. They exhibited reproducible and stable voltammograms without hysteresis, withstanding 6 hours’ continuous use and 15 hours’ iterative processes of heat and voltammetry. Not only the halfwave potentials but also slopes of the log-plots were independent of radii of the electrodes. No kinetic effect was revealed in the steady-state voltammograms.     

Recyclable Solid Ruthenium Catalysts Supported on Metal Oxides for the Addition of Carboxylic Acids to Terminal Alkynes

Ceria‐supported ruthenium catalysts (Ru/CeO₂) were found to be quite effective for the addition of various carboxylic acids to terminal alkynes, which gave the corresponding enol esters in moderate to high yields. The major products of the reaction were E‐isomers of anti‐Markovnikov adducts. Among the ceria‐supported ruthenium catalysts examined, those prepared using ruthenium precursors with chloride ligands showed high activities. The zirconia‐supported ruthenium catalyst (Ru/ZrO₂) showed activity comparable to that of the ceria‐supported catalyst. These catalysts were recyclable without a significant loss of activity, and the leaching of ruthenium species into the liquid phase was negligible after cooling the reaction mixture, which indicates marked superiority of the present solid oxide catalysts to conventional homogeneous catalysts.     

Fast calculation method for spherical computer-generated holograms

The synthesis of spherical computer-generated holograms is investigated. To deal with the staggering calculation times required to synthesize the hologram, a fast calculation method for approximating the hologram distribution is proposed. In this method, the diffraction integral is approximated as a convolution integral, allowing computation using the fast-Fourier-transform algorithm. The principles of the fast calculation method, the error in the approximation, and results from simulations are presented.     

Highly sensitive and rapid profiling method for carotenoids and their epoxidized products using supercritical fluid chromatography coupled with electrospray ionization-triple quadrupole mass spectrometry

Epoxy carotenoids, which are products of carotenoid oxidation, are potential oxidative stress markers. However, it is difficult to profile epoxy carotenoids owing to their small amount and difficulty in their separation from hydroxy carotenoids. In this study, a high-performance analytical system based on supercritical fluid chromatography (SFC) coupled with tandem mass spectrometry (MS/MS) was developed for the simultaneous analysis of carotenoids and epoxy carotenoids. SFC is an effective separation technique for hydrophobic compounds, by which major carotenoids in human serum and their epoxidation products can be analyzed within 20 min. The use of MS/MS increased the sensitivity; the detection limit for each carotenoid was of the sub-fmol order. When the constructed method was applied to biological samples such as human serum and low-density lipoprotein (LDL), the precise detection of the target carotenoids was disturbed by several isomers. However, highly selective detection of epoxy carotenoids was performed by targeting product ions that were generated with a structure-specific neutral loss of 80Da. Furthermore, the sample volume needed for the analysis was only 0.1ml for the serum, indicating the efficiency of this system in performing small-scale analyses. Using the analytical system developed in this study, highly sensitive and selective analysis of epoxy carotenoids could be performed in a short time. These features show the usefulness of this system in application to screening analysis of carotenoid profiles that are easily modified by oxidative stress.     

Effects of Neutron Irradiation on the Mechanical Properties of Magnesium Aluminate Spinel Single Crystals and Polycrystals

The effect of fast neutron irradiation on the mechanical properties of magnesium aluminate spinel single crystals and polycrystals, such as bending strength, fracture toughness, Young's modulus, and hardness, was summarized based on the reported data. Essentially, the changes in these properties are dependent on the nature and concentration of neutron-irradiation-induced defects. Furthermore, the efficiency of damage accumulation is known to be dependent on temperature. Spinel shows superior resistance to the formation of defect aggregates, and the recombination of point defects occurs efficiently under neutron irradiation; therefore, the change in mechanical properties is not critical, up to very high neutron fluences, and the spinel maintains its structural integrity.     

360° reconstruction of a 3D object using cylindrical computer generated holography

Simulated reconstruction of a three-dimensional (3D) object in 360° from cylindrical hologram is proposed. The simulation is done using a fast calculation method, where wave propagation in spectral domain and in cylindrical coordinates is used to generate the cylindrical hologram of a 3D object. The same procedure is followed to reconstruct the object back. The reconstructions resembled the original object and could be seen from all 360°. The whole simulation process is done using open-source software.     

Three-dimensional displacement measurement for diffuse object using phase-shifting digital holography with polarization imaging camera

The amount of displacement of a diffused object can be measured using phase-shifting digital holography with a polarization imaging camera. Four digital holograms in quadrature are extracted from the polarization imaging camera and used to calculate the phase hologram. Two Fourier transforms of the phase holograms are calculated before and after the displacement of the object. A phase slope is subsequently obtained from the phase distribution of division between the two Fourier transforms. The slope of the phase distribution is proportional to the lateral displacement of the object. The sensitivity is less than one pixel size in the lateral direction of the movement. The longitudinal component of the displacement can be also measured separately from the intercept on the phase axis along the phase distribution of the division between two Fourier transforms of the phase holograms.     

Changes in immunoelectron microscopic localization of cathepsin D in muscle induced by conditioning or high-pressure treatment

Changes in the localization of cathepsin D in postmortem and pressurized rabbit muscles were investigated by immunoelectron microscopy. The anti-cathepsin D monoclonal antibody strongly labeled a large vesicle in a subsarcolemmal part of the cell , which strongly suggests that this is the primary lysosome. The liberation of the cathepsin D entrapped in the lysosomes in the muscle prepared immediately after death proceeded with the progress of the conditioning. The release of almost all cathepsin D from the lysosomes and its absorption on the myofibrils were observed in the muscle conditioned for 14 days. The accumulation of lysosomes having various volumes and shapes accompanied with the disruption of myofibrillar structure was also observed. The liberation of cathepsin D from the lysosomes can be attributed to the modification of membranes permeability of the lysosomes during conditioning. When the muscle was pressurized at 100 MPa, the modification of the round shape of the lysosome was observed. With the increase of the pressure applied to the muscle, the release of cathepsin D from the lysosome due to the disruption of membrane was accelerated, and absorption of the released cathepsin D on the myofibrils was observed. From the results obtained, it was clear that the changes in the localization of cathepsin D accompanied with the modification of lysosomes induced by the brief exposure to high pressure were drastic in comparison with that in the muscle during conditioning.     

Helium bubbles and trace of lithium in B4C control rod pellets used in JOYO experimental fast reactor

B₄C pellets used in the control rod of the experimental fast reactor ‘JOYO’ with different ¹⁰B burnups from lower than 10 × 10²⁰ captures/cm³ to 80 × 10²⁰ captures/cm³ and irradiated at less than 800 °C were examined by transmission electron microscopy (TEM). In a B₄C pellet irradiated in an irradiation capsule of ‘JOYO’ at 800 °C up to 30 × 10²⁰ captures/cm³, intragranular helium bubbles appeared in flat plate-shapes with the plane of the plate parallel to the (111) rhombohedral plane. However, in the other specimens that were taken from an actual control rod, the helium gas formed very tiny spherical intergranular bubbles with a diameter of a few nanometers . These tiny bubbles make wavy arrays roughly parallel to the (111) plane. The B₄C specimens were heated on a TEM in situ heating holder up to 1040 °C for 10 min. Clustering of tiny bubbles was observed, but did not extend to the plate-shaped bubbles. In high burnup specimens, large bubbles/cracks were rarely found along the {100} planes, which may correspond to the amorphous bands caused by the slip. While heating the specimens in TEM over 800 °C, liquid phases of lithium-bearing compoundsappeared on the surface of specimen.