Papers by Author: Tatsuki Ohji

Abstract: Based on the proposed inorganic reactions a series of high performance hexagonal boron nitride-containing composites (BNCC), include SiC-BN, Si3N4-SiC-BN, SiAlON-BN, AlN-BN, Al2O3-BN, AlON-BN and mullite-BN, have been prepared via reactive hot pressing or pressureless reactive sintering. Various boron-bearing components such as B, B4C, AlB2, SiB4, SiB6, B2O3 or H3BO3, 9Al2O3×2B2O3 (9A2B) and 2Al2O3×B2O3 (2AB) are used as the boron source. On the other hand, nitrogen gas or solid state nitirgen-bearing metal nitrides such as Si3N4 and AlN can be used as the nitrogen source. The in situ synthesized composites demonstrated homogeneous and isotropical microstructures with very fine (nano-sized) BN platelets or their agglomerates distributed in the matrixes. These composites showed high strength, low elasticity and improved strain tolerance. In this article the reaction design, thermodynamics, reaction mechanisms, reactive hot pressing or pressureless reactive sintering, microstructures and mechanical properties will be discussed.

Abstract: Porous Si3N4 ceramics with different pore morphology have been fabricated, utilizing either organic whiskers or starch as the fugitive agents, through slip-casting and die-pressing technique, respectively. The obtained porous ceramics have rod shaped or equiaxial pore morphology, originated from there two kinds of pore forming agents. The mechanical properties were investigated. The strength decreased considerably when small amount of whiskers were added, however, further increase in the whisker content only cause a moderate decrease of the strength. Gas permeability were measured for the samples with high whisker content of 60 vol% (corresponding to porosity of about 45% in the sintered bodies), and was compared with the counterpart contained the same porosity in which pores were equiaxial. The flexural strength of the samples with these two types of fugitive particles was almost the same, but the permeability of samples with rod-shaped pores were much higher than that with equiaxial pores, which can be understood in terms of a short pass model.

Abstract: Silicon nitride ceramics with and without β-Si3N4 seed addition were prepared via tape casting nonaqueous ceramic slurries, laminating the green ceramic tapes, and gas pressure sintering the green bodies in nitrogen atmosphere. Lu2O3 and SiO2 were used as sintering additives. The results showed that the rod-like β-Si3N4 seed was helpful to enhance β-Si3N4 grain growth unidirectionally. The elongated grains grown from seeds were preferentially oriented parallel to the casting direction, resulting in anisotropic microstructure. When a stress was applied with along the grain alignment, the bending strength of the tape-cast Si3N4 with 3 wt% β-Si3N4 seed addition measured at 1500oC was 738 MPa, which was almost the same as the room temperature bending strength 739 MPa, and the fracture energy can be improved from 301 J/m2 at room temperature to 781 J/m2 at 1500oC. The large fracture energy and bending strength at 1500oC were attributable primarily to the unidirectional alignment fibrous grains and a high melting point grain boundary phase.

Abstract: In this work, cordierite whiskers were successfully coated on cordierite honeycomb support by in-situ method. Whisker coating was performed on walls of the pore channels of cordierite support from aqueous slurry. Sintering was carried out at 1300 °C for 4 hours. XRD measurements revealed a complete formation of cordierite phase, no traces of other phases were identified. A well adherence of coating on the support was identified from the microstructure. SEM analysis also revealed the formation of three-dimensional network of cordierite whiskers with open pores between them on the cordierite support.

Abstract: Lu2O3 and SiO2 were used as sintering additives and rod-like β-Si3N4 seeds were added to enhance β-Si3N4 grain unidirectional growth. Silicon nitride ceramics were prepared by tape casting and gas pressure sintering
at 1950oC in 10 atm nitrogen atmosphere for 6 h. Compare to the no-seeded Si3N4, the seeded and tape-cast Si3N4 ceramics have obvious anisotropic microstructure and anisotropic properties. When a stress applied along with the grain alignment direction, the bending strength of the seeded and tape-cast Si3N4 at 1500oC was 738 MPa, which was almost the same as its room temperature bending strength. However, the bending strength of the seeded and tape-cast at room temperature was 556 MPa (perpendicular direction); and their thermal conductivity were 67 W/m·K (perpendicular direction) and 83 W/m·K (parallel direction), respectively. The anisotropic properties of the seeded and tape-cast Si3N4 were attributable to the elongated Si3N4 grain alignment.

Abstract: The corrosion behaviors of Ln2Si2O7 (Ln=Yb and Lu) and ASiO4 (A=Ti, Zr and Hf) EBC's were examined at 1500oC in water vapor environment. These oxides were coated on silicon nitride specimens by oxidation-bonded reaction sintering technique. Among Ln2Si2O7 system, though the thermal expansion coefficient of Yb2Si2O7 phase is closer to silicon nitride than that of Lu2Si2O7 phase, the corrosion resistance of silicon nitride with Lu2Si2O7 EBC was higher than that of Yb2Si2O7 EBC sample. In these EBC materials, boundary silica phase was easily corroded by water vapor. Among ASiO4 system, though the corrosion rate of HfSiO4 bulk was larger than that of ZrSiO4 and TiSiO4 phases, the oxidation of the silicon nitride substrate for HfSiO4 coated sample was smaller than that of other two. Many cracks were in ASiO4 EBC layer during the corrosion test. The introduced crack length in HfSiO4 EBC layer is shorter than in ZrSiO4 EBC layer due to the thermal expansion mismatch between EBC materials and the silicon nitride substrate.

Abstract: High strength particulate ceramic composites are in general reinforced by strong dispersoids, such as strong ceramic particles (SiC, TiB2, ZrO2, et al) and strong metallic particles (Mo, W, et al). In this work high strength ceramic composites with in-situ synthesized hexagonal boron nitride (h-BN) have been prepared and characterized. As an example, we manufactured mullite-BN composites by reactive hot pressing (RHP) using aluminum borates (9Al2O3·2B2O3 and 2Al2O3·B2O3) and silicon nitride as starting materials. The obtained material RHPed at 1800°C showed a strength of 540 MPa, which was 1.64 times higher than that of the monolithic mullite ceramics. TEM observation revealed that the composite had an isotropic microstructure with a fine mullite matrix grain size of less than 1 μm and a nano-sized h-BN platelets of about 200 nm in length and 60∼80 nm in thickness. The high strength was suggested to be from the reduced matrix grain size and the small toughening effect by the h-BN platelets. In addition, this kind of ceramic composite demonstrates low Young’s modulus that is beneficial to the thermal/mechanical shock resistance, and excellent machinability.

Abstract: Silicon nitride ceramics was prepared by tape casting nonaqueous ceramic slurries, laminating the green ceramic tapes, and gas pressure sintering in nitrogen atmosphere. Lu2O3 and SiO2 were used as the sintering additives, and 3 wt.% β-Si3N4 seed was added to enhance β-Si3N4 grain growth unidirectionally. The seeded and tape-cast Si3N4 showed very good high temperature bending strength at 1500oC, when the stress applied along with the grain alignment direction. This was attributable to the formation of a high melting point grain boundary phase and the fibrous Si3N4 grains alignment. After exposure in air at 1500oC for up to 100 h, the oxidation products formed on the Si3N4 surface consist of Lu2Si2O7 and SiO2. The bending strength of the oxidized and tape-cast Si3N4 was degradation, the strength decrease was associated with the formation of new defects on the surface and the interface between the oxide layer and the Si3N4 bulk.

Abstract: Various coating methods of EBC layer for silicon nitride were discussed. High density EBC layer was successfully coated by different techniques such as sputtering, sol-gel and reaction sintering methods. Water vapor corrosion and recession mechanisms of Lu2Si2O7 which is a potential material for EBC were discussed. The problems in the development of EBC revealed by corrosion tests were summarized. The most important problem addressed here was the corrosion of silica at grain boundary. Due to corrosion of silica at the boundary, formation of porous surface is inevitable, then the silicon nitride substrate gets easily oxidized and/or corroded by water vapor. To resolve this issue, we propose a new EBC material without boundary silica and the corrosion mechanism of this improved EBC material is discussed.