Papers by Author: Hideo Awaji

Abstract: In order to improve fracture toughness of ceramics, an intrinsically small frontal process zone (FPZ) size must be expanded. An intra-type nano-structure, where nano-particles are embedded within matrix grains, yields dislocations around the dispersed particles due to residual stresses. These dislocations become sessile dislocations at room temperature, operate as origins of small stress concentration in the matrix, and create nano-cracks in the FPZ. To produce the intra-type nano-structure, we developed a soaking method. This method makes it possible to produce nano-sized metallic particles dispersed within ceramic powders. In this research, alumina-nickel nanocomposite powder was obtained using the soaking method. The powder mixed with α-alumina as a seed was sintered using a pulse electric current sintering technique. The sintered nanocomposites are then annealed to disperse dislocations around the nanoparticles into alumina grains. Results showed that the maximum fracture toughness was 7.6 MPam1/2, which was two times higher than that of alumina.

Abstract: Aluminum titanate ceramics (Al2TiO5) is a synthetic ceramic material of potential interest for many structural applications. A critical feature, which greatly limits the mechanical properties of polycrystalline Al2TiO5, is considerable intergranular microcracking, which occurs due to the high thermal anisotropy of individual grains. In this study, the temperature dependencies of mechanical properties were discussed along with the microstructure observation. Both of fracture strength and fracture toughness increased considerably with increasing the temperature. These phenomena were explained on the basis of the stress redistribution and unique microscopic feature on the fracture surface of aluminum titanate ceramics. The experimental results also revealed that the repeated heat treatments resulted in the change of fracture strength and fracture toughness due to the stress redistribution in the Al2TiO5 matrix.

Abstract: A novel estimation for the critical size of the frontal process zone of ceramics is proposed using a single-edge V-notched beam (SEVNB) technique. A three-point flexure test is carried out on aluminum titanate ceramics containing a sharp V-shaped notch with different depth. An exact solution of the critical local stress is analyzed at a critical distance from the notch tip. The critical frontal process zone size is determined as the distance between the notch tip and the point where the critical local stress equals the flexural strength of specimens without notches, based on the local fracture criterion and the Griffith-Irwin criterion. The critical size of the frontal process zone, the fracture toughness and the flexural strength were also estimated for several materials, such as, alumina, porous alumina, and alumina-based nanocomposites. The relationship between these mechanical properties indicated that there was an almost linear relationship between the fracture toughness and the resultant of strength and square root of the critical frontal process zone size, and that both of them must be increased to improve the fracture toughness of ceramics.

Abstract: Intra-type nanocomposites, in which nanosized second-phase particles are embedded within matrix grains, generate dislocations around the dispersed nanoparticles. The intra-type nanostructure induces a thermal expansion mismatch between the matrix and the dispersed particles, which will yield nanoscale stress distribution around the particles and generate lattice defects, such as dislocations. The dislocations of ceramics can be generated at elevated temperatures, become sessile dislocations at room temperature, and serve as nanocrack nuclei in highly stresses fields, e.g. at a main crack tip. The frontal process zone size ahead of a crack tip is expanded due to creation of nanocracks and hence the fracture toughness is improved. Annealing after sintered nanocomposites is important in controlling the dislocation activities. Appropriate annealing will disperse dislocations into the matrix grains. However, dislocations are sensitive to temperature, and higher temperature or longer annealing time result in dislocation disappearance and cause the reduction of the strength and fracture toughness of nanocomposites. In this study, commercially available γ-alumina agglomerated powder with high porosity was used to create the intra-type nanostructure. Nickel nitrate solution was infiltrated into nanopores of the γ-alumina agglomerates in vacuum. The alumina/nickel composite powder following reduction in hydrogen atmosphere was sintered using a pulse electric current sintering method. The volume fraction of nickel was about 3 vol %. After appropriate annealing, the highest fracture toughness was obtained to be 7.6 MPam1/2, which is two times higher than that of monolithic alumina.

Abstract: Porous Ni
ZrO2 has been widely used as anode in SOFC. However, it has been reported that there was reduction in cell performance at high temperature since Ni grains in the porous Ni
ZrO2 sintered during cell operation. In this study, NiO
ZrO2 composite powders in which NiO powder were covered with ZrO2 particles were prepared with controlled microstructure of porous Ni
ZrO2 which can prevent sintering of Ni grains during cell operation. NiO
ZrO2 composite powders (HNZ) were prepared using NiO powder of high specific surface area and ZrO2 sol of average particle size of 50 nm by ball milling (sol-coating method). SEM and EPMA analysis of prepared NiO
ZrO2 composite powders showed that NiO particles were covered with ZrO2 particles. The crystallite phases, crystallite sizes, BET specific surface area of NiO
ZrO2 composite powders and porosities of fabricated porous Ni
ZrO2 were characterized. SEM and EPMA analysis showed that ZrO2 was distributed around Ni of a few μm range in the porous Ni
ZrO2 (HNZ) fabricated by the sol-coating method. Mechanical properties of porous Ni
ZrO2 (HNZ) are required to be improved.

Abstract: Nickel dispersed alumina matrix nanocomposites were fabricated using a novel soaking method. Secondary particles were introduced into the nano-pores of a porous matrix grains by a soaking method, such that γ-alumina powder was soaked in nickel nitrate solution under vacuum. During pre-calcination, nickel oxide particles were created inside of the nano-pores of γ-alumina. The alumina powders were then reduced under hydrogen atmosphere to obtain nano-sized metallic nickel embedded in γ-alumina grains. The alumina-nickel composite powders were sintered by pulse electric current sintering (PECS) technique with α-alumina seeds. The maximum strength of the alumina-nickel nanocomposites was 984 MPa after sintering at 1,450 °C with α-alumina seeds, where the specimen size was 2
2
10 mm3. The maximum fracture toughness was 5.5 MPa·m1/2 after sintering at 1,350 °C with seeds measured by the single edge V-notched beam (SEVNB) method.

Abstract: Based on the FGM concept, laminated alumina tube with a tailored porosity gradient along the radial direction has been successfully fabricated by the lamination method in the centrifugal molding technique. Experiments were performed with colloidally processed alumina powder and pore-former agent. The powder mixture was made into slurry in water media and the tubes were cast using a stainless steel mold. The porosity profile was designed with the presence of PMMA particles as pore-former agent and the nature of porosity was investigated by microstructure observations. The bimodal pore structure of the tubes was constructed from large spherical pores about 10 μm formed by burning-out the pore-former agent and small sub-micron pores caused by the lower sintering temperature. The fracture behavior of porous tubes with tailored porosity gradient was investigated using the O-ring compression testing. The failure behavior was divided into two types depending on the pore-former agent. The air permeability and fracture behavior were independent of the lamination process. The influence of the porosity gradient on the fracture strength was investigated and the results showed there was a reduction in fracture strength with increase in the laminate number, and the minimum strength was found in continuous graded tubes.

Abstract: Thermal shock is a mechanism often leading to failure of ceramic materials that may occur during rapid heating or cooling. These tests were performed in order to compare the thermal shock resistance of ceramic materials by cooling with that of the heating method and hence to evaluate parameters such as thermal shock strength (R1c) and thermal shock fracture toughness (R2c). During the present study, thermal shock resistance of alumina and mullite ceramics was estimated experimentally and theoretically using the thermal shock parameters. The critical thermal stress at the onset of thermal shock fracture was calculated using fracture time, which is measured by an acoustic emission. Results show that thermal shock parameters of alumina specimens decreased with increasing temperature of fracture point. This effect can be attributed to the temperature dependence of the thermal properties. The experimental values of thermal shock parameters evaluated by IRH and WFC techniques were in good agreement at the temperature of fracture point. The thermal shock parameters enabled the definition of a unified thermal shock resistance of ceramics, which is independent of the nature of the testing techniques.

Abstract: Although porous ceramics are materials with high potential for helping conserve the environment, the characteristics of pore-related mechanical properties have not yet been examined sufficiently. The R-curve behavior of porous ceramics was estimated using the crack stabilizer technique developed by Nojima et al. Also, the critical frontal process zone (CFPZ) size for porous ceramics was estimated from the strength and fracture toughness of the materials used. The results revealed that the R-curve behavior was almost flat in porous ceramics, in contrast with a steeply rising R-curve behavior for porous silicon carbide observed previously, and that the CFPZ size of porous ceramics was larger than that of dense ceramics. A schematic explanation for the crack extension in porous materials was presented to discuss the R-curve behavior of porous ceramics.

Abstract: Intra-type structure of ceramic matrix composites (CMCs) can improve the mechanical properties of ceramic materials. In this work, we used γ-alumina as a matrix including nano-pore for fabricating alumina/silicon carbide composites using pressure-less sintering and pulse electric current sintering (PECS) techniques. We added α-alumina as a seed in order to improve densification of this commercially available γ-alumina. The mixture was sintered from 1250 to 1450
by pressure-less sintering and PECS techniques. Densification of the specimen sintered by pressure-less sintering is very difficult and bulk density of the specimen sintered at 1450
showed lower than 3.0 g/cc. In the case of the PECS technique, the density was improved to 3.8 g/cc in seed added specimen sintered at 1450
. Maximum Vickers hardness and maximum fracture strength were obtained 17 GPa and 500 MPa for the seed added specimens sintered at 1450
, respectively.