Papers by Author: Toyohiko Yano

Abstract: In this study, SiC/SiO₂ core-shell nanowires (SiCNWs) were fabricated by thermal evaporation method without any catalyst, using pre-oxidized silicon powder and methane (CH₄) gas as precursors. The reaction temperature was 1340°C in an inert atmosphere. The SiCNWs produced by this process had a single crystal β-SiC core ranging from 20 to 80 nm in diameter and low-crystalline SiO₂ shell about 10-20 nm thick, and up to 1 mm long. The exhaust gas from the production system was analyzed by gas chromatography and the growth activity of SiCNWs was captured by digital camera during a soaking period. From the results, CO gas was detected only when SiCNWs were growing and was not found when methane gas was stopped. It was clarified that CO gas was produced as a by-product during the formation of SiCNWs. The formation mechanism of SiCNWs synthesized by thermal evaporation method was suggested to be oxide-assisted growth mechanism.

Abstract: C-and BN-interphases on SiC fibers for unidirectional SiC_f/SiC composites were formed by EPD process, and their microstructure and mechanical properties were investigated. Whereas the C-SiC_f/SiC composites showed a pseudo-ductile fracture behavior with large amount of fiber pullout, the BN-SiC_f/SiC composites fractured in a brittle manner without fiber pullout in spite of sufficient thickness of BN interphase. It is inferred from the results of EDS that sintering additives would react with h-BN-interphase, and the interphase did not act effectively for toughening the SiC_f/SiC composites.

Abstract: The CNT/B₄C composite with Al₂O₃ additive was fabricated by hot-pressing following extrusion molding of a CNT/B₄C paste, and mechanical properties of the obtained composite were investigated. Many CNTs in the composite aligned along the extrusion direction from SEM observation. 3-points bending strength of the composite was slightly lower than that of the monolithic B₄C. Elastic modulus and Vickers hardness of the composite drastically decreased with CNT addition. Fracture toughness of the composite was higher than that of the monolithic B₄C.

Abstract: Hafnium carbide powder was synthesized by sol-gel polycondensation of hafnium chloride with citric acid. The starting materials were dissolved in water and mixed homogeneously on a hot plate until a precomposite gel was formed. Pyrolysis of the obtained gel resulted in formation of monoclinic hafnia and amorphous carbon, which after subsequent heat treatment transformed into hafnium carbide. Materials were analyzed by means of X-ray diffraction and electron microscopy investigations. The results showed that the obtained carbide powder was composed of nearly equiaxed particles of narrow size distribution. The obtained hafnium carbide powder was densified via spark plasma sintering (SPS) at 1950 oC using molybdenun silicide as sintering additive. Microstructure and mechanical properties of the obtained hafnium carbide ceramics were investigated.

Abstract: Effects of simultaneous addition of SiO2 and gadrinium oxide on densification of SiC ceramics were examined, and relation between microstructure and their mechanical properties were discussed. Total 11wt% of Gd2O3 and SiO2 were mixed with fine -SiC powder. The weight of Gd2O3 in (Gd2O3 + SiO2) were set as 0, 20, 40, 60, 80 and 100%. The mixture was hot-pressed at 1950oC under 40 MPa applied pressure for 1 h. In the case of 40Gd2O3 and 80Gd2O3 compositions, the effect of sintering temperature from 1900 to 2000oC was also examined. The bulk density increased with increasing Gd2O3 content at the sintering temperature of 1950oC. Bending strength of the sintered bodies also improved with increasing Gd2O3 content generally, but at 40Gd2O3 composition, the maximum over ~800 MPa was observed. Young’s modulous, Vickers hardness and fracture toughness also increased with increasing Gd2O3 content. The distribution of grain boundary phase was not homogeneous. Evaporation of additives, mainly SiO2, caused non-homogeneous distribution of grain boundary phase between outside and inside of sintered bodies. High temperature bending strength of 80Gd2O3 specimen was superior than that of 40Gd2O3 specimen.

Abstract: Alpha- or beta-Si3N4 powder with larger grain size was uses as starting material, and the effect of heat-treatment on thermal conductivity of Si3N4 ceramics using MgO, Y2O3 and SiO2 as sintering additives was investigated in terms of their microstructure and the amount of grain boundary phase. Most of the components derived from sintering additives existed as glassy phase in sintered Si3N4. After heat-treatment at 1950oC for 8 h, the amount of glassy phase significantly decreased, and then small amount of glassy phase existed in Si3N4 ceramics was crystallized as Y2O3 and Y2Si3N4O3. In the case of Si3N4 ceramics using SN-7 powder, thermal conductivity of heat-treated Si3N4 was around twice of the value of sintered Si3N4, and the thermal conductivity was increased from 41.4 to 87.2 W/m•K due to not only the reduction of grain boundary phase but also the grain growth. In the case of Si3N4 using SN-F1 powder, thermal conductivity of Si3N4 ceramics was also significantly increased from 36.0 to 73.2 W/m•K after heat-treatment. In this case, the reduction of grain boundary phase mainly affected the thermal conductivity of Si3N4 ceramics because the grain size of heat-treated Si3N4 was nearly the same as that of sintered Si3N4. The reduction of grain boundary phase from Si3N4 was effective for the improvement of their thermal conductivity in addition to grain growth of Si3N4.

Abstract: For the transmutation of the very long half-lived isotopes which are separated from the spent nuclear fuels, it is necessary to find proper inert matrices these are stable under heavy neutron irradiation at high temperature. Silicon nitride ceramics is a candidate since it is very tolerant for heavy neutron irradiation and keeps relatively high thermal conductivity. For these reasons, we try to sinter Si3N4 ceramics containing large amounts of CeO2 as a simulant for Am2O3, a typical transuranium element. The low-temperature pressureless-sintering behavior of the ceramics and chemical and thermal properties of the obtained sintered bodies are reported.

Abstract: The layers of ZrO2-Al2O3 were coated on the surface of SiC fibers (Tyranno SA fiber) by dip-coating process. The citric acid-ethylene glycol solution containing Al and Zr ions was polymerized at 150oC to obtain a polymerized complex precursor. The 2D-woven SiC Tyranno SA fibers were dipped into this precursor few times. Heat treatment for coated fiber was conducted at 800-1200oC for 1 h in air. Thin film of mixed zirconium/aluminum oxides on SiC fibers were successfully elaborated using the sol-gel process. The coated zirconium/aluminum oxides layer of SiC Tyranno SA fiber was about 200-1000 nm. The coated fibers were stable in an oxidizing environment even at high temperatures.

Abstract: Silicon nitride (Si3N4) ceramics have been interested for electrical substrate applications, because the ceramics can be made highly mechanical strength, fracture toughness, electrical resistivity and high thermal conductivity. Generally, relatively large amount of additives are required to obtain dense Si3N4 ceramics. During sintering, additives react with SiO2 including surface oxide of Si3N4 raw powder to form a liquid phase. Most of liquid phase changed into glassy phase during cooling down. In this study, Si3N4 ceramics were fabricated by gas pressure sintering. Yttrium oxide (Y2O3), silica (SiO2), and magnesia (MgO) were used for liquid-phase-enhanced sintering process. Dense materials were sintered by this process, but their thermal conductivities were not so high (30-40 W/m·K). Therefore, post-sintering heat-treatment process was performed to reduce the excess amount of glassy phase. An additive system (3 mass% SiO2 with 3 mass% MgO and 1-5 mass% Y2O3) was selected as the sintering aid. These ceramics could be sintered to almost full density at relatively low temperature as 1650oC for 2 h under 0.1 MPa-N2 without packing powder. The resulting materials have high bending strength, about 1 GPa, when 5mass% of Y2O3 was added. Based on the creation of low temperature pressureless sintering without packing powder, a novel two-step sintering (once firing) was proposed. The two-step sintering conducted by sintered at 1650oC under 0.1 MPa-N2 for 2 h for densification in the first step. Followed by heated up to and kept at 1950oC for 8 h under 1.0 MPa-N2 in the second step. The Si3N4 ceramics could be fabricated with relatively high thermal conductivity of 90 W/m·K. Mass loss, microstructure, mechanical properties, oxygen content and chemical composition were discussed.

Abstract: Monazite(LaPO4)-coated alumina-fiber/alumina-YAG (Y3Al5O12) matrix composites were fabricated by in-situ coating of monazite followed by hot-pressing, and the effects of coating and sintering condition on mechanical properties of the composite were examined. Alumina powder and YAG powder (weight ratio, 95:5) were used as raw materials for green sheets, which was fabricated by tape casting technique. Monazite was synthesized by the in-situ reaction of La(NO3) solution with H3PO4 on the surface of fibers. After slurry infiltration into the coated fiber bundles, the fiber cloths were laminated with the green sheets alternately, then they were heat-treated, finally sintered by hot-pressing at various temperatures. The mechanical properties of the composites were changed by the fabrication conditions. Non-brittleness of the composites reduced with the increase of sintering temperature. The composites sintered at 1200oC showed the highest Weibull modulus and pseudo-ductility.