ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray...ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray diffraction, infrared spectrum, scanning electron microscope and differential scanning calorimetric. And the mechanical properties of the nano-ceramics were studied. The results show that the bulks are still in amorphous state at 900 ℃ and the t-ZrO2 forms at about 950 ℃ with a faint spinel-like phase which changes into mullite on further heating. ZrO2 and mullite become major phases at 1 100 ℃ and an amount of m-ZrO2 occur at the same time. The sample heated at 950 ℃ for 2 h and then at 1 100 ℃ for 1 h shows very dense and homogenous microstructure with ball-like grains in size of 20-50 nm. With the increase of crystallization temperature up to 1 350 ℃, the grains grow quickly and some grow into lath-shaped grains with major diameter of 5 μm. After two-step treatment the highest micro-hardness, flexural strength and fracture toughness of the samples are 13.72 GPa, 520 MPa and 5.13 MPa·m1/2, respectively.展开更多
Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary...Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200 ℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.展开更多
Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studi...Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI（OH）3 sols are produced by using 0.1 mol/L Al（NO3）3·9H2O and 0.16 mol/L （NH4）2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%（volume fraction） surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.展开更多
基金Project(2003AA332040) supported by the National High Technology Research and Development Program of China
文摘ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray diffraction, infrared spectrum, scanning electron microscope and differential scanning calorimetric. And the mechanical properties of the nano-ceramics were studied. The results show that the bulks are still in amorphous state at 900 ℃ and the t-ZrO2 forms at about 950 ℃ with a faint spinel-like phase which changes into mullite on further heating. ZrO2 and mullite become major phases at 1 100 ℃ and an amount of m-ZrO2 occur at the same time. The sample heated at 950 ℃ for 2 h and then at 1 100 ℃ for 1 h shows very dense and homogenous microstructure with ball-like grains in size of 20-50 nm. With the increase of crystallization temperature up to 1 350 ℃, the grains grow quickly and some grow into lath-shaped grains with major diameter of 5 μm. After two-step treatment the highest micro-hardness, flexural strength and fracture toughness of the samples are 13.72 GPa, 520 MPa and 5.13 MPa·m1/2, respectively.
基金Project (5JJ30103) supported by the Natural Science Foundation of Hunan Province, China
文摘Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200 ℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.
文摘Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI（OH）3 sols are produced by using 0.1 mol/L Al（NO3）3·9H2O and 0.16 mol/L （NH4）2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%（volume fraction） surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.
