Seong Min Choi

Sintering and Characterization of Zr2Al3C5 Monolith

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.

Annealing Effects on Toughened Intra-Type Nanocomposites

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.

Nanocomposites – Toughened Ceramics

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.

Alumina-Based Nanocomposites Fabricated by a Novel Soaking Method

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.

Effect of α-Alumina as a Seed in Alumina/Silicon Carbide Composites

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.

Fabrication of Toughened Alumina Nanocomposites Using γ-Alumina Powder

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.