Authors: Hideo Awaji, Takuya Matsunaga, Seong Min Choi
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.
2242
Authors: Hideo Awaji, Seong Min Choi
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.
1632
Authors: Uraiwan Leela-adisorn, Takuya Matsunaga, Seong Min Choi, Sawao Honda, Hideo Awaji
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 2210 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.
607
Authors: Seong Min Choi, Uraiwan Leela-adisorn, Sawao Honda, Shinobu Hashimoto, Hideo Awaji
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.
115
Authors: Uraiwan Leela-adisorn, Seong Min Choi, Shinobu Hashimoto, Sawao Honda, Hideo Awaji, K. Hayakawa, Akira Yamaguchi
Abstract: Zr2Al3C5 has been successfully synthesized via solid state reaction between Al, ZrC and
carbon powder at 1600 in vacuum. This complex carbide has very strong bond between metal
atoms and carbon atoms. Thus, this material has a potential to be utilized as structural materials.
Some properties of Zr2Al3C5 powder from solid-state reaction in vacuum had been tested. It was
found that this powder was completely oxidized in air at 900 1 h, and can be hydrated in moist
air. These drawbacks might come from the high reactivity of the powder due to synthesis in vacuum.
Zr2Al3C5 powder from solid state reaction in vacuum was sintered at various temperatures from
1500 to 2000 under vacuum with pulse electric current sintering (PECS) and pressureless
sintering. Zr2Al3C5 started to sinter at 1500 and got partially dense from 1700. Physical
properties and mechanical properties of this material were investigated and discussed.
27
Authors: Seong Min Choi, Takuya Matsunaga, Sung Ho Cheon, Sawao Honda, Shinobu Hashimoto, Hideo Awaji
Abstract: To improve fracture strength and fracture toughness in ceramic materials, we focused our
attention on an intra-type structure of nanocomposites. We proposed new processing method for
fabricating intra-type nanocomposites. In this work, Al2O3/Ni nanocomposites were fabricated using
a soaking method and sintered by PECS(Pulse Electric Current Sintering) method. We also estimated
seed effects on this system. Seeded nanocomposites showed high fracture strength and higher fracture
toughness than non-seeded nanocomposites and monolithic alumina. The fracture strength of the
seeded nanocomposites was more than 800MPa in all sintering temperature range. The maximum
value of the fracture toughness was 5.5 MPa⋅m1/2 for the specimen sintered at 1350°C. The sintered
specimens with high fracture strength and high fracture toughness were annealed from 800°C to
1000°C for 0 to 10 min. The specimen annealed at 800°C for 5 min showed the highest fracture
toughness of 7.6 MPa⋅m1/2. This value is two times higher than that of the monolithic alumina.
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