(Ca, Mg)-α′-Sialon-AlN-BN powders were synthesized by the carbothermal reduction and nitridation (CRN) method using boron-rich slag, one of the intermediate products from pyrometallurgy separation of pageit, as the ...(Ca, Mg)-α′-Sialon-AlN-BN powders were synthesized by the carbothermal reduction and nitridation (CRN) method using boron-rich slag, one of the intermediate products from pyrometallurgy separation of pageit, as the staring material. The influences of synthesis temperature and holding time on the phase composition and microstructure during the microwave CRN were studied by XRD, SEM and EDS. The comparison between two heating techniques, conventional and microwave heating, on the synthesized powder was presented as well. The experimental results revealed that the phase compositions and microstructures of the synthesized products were greatly affected by the synthesis temperature and holding time. With an increase in the synthesis temperature or holding time, the relative amount of α′-Sialon increased and α′-Sialon became the main crystalline phase at 1400 °C for 6 h. The synthesized products also contained AlN, BN and a small amount of β-SiC. Elongated α′-Sialon grains, short rod AlN grains, aggregate nanoscale BN grains were observed in the synthesized powders. The reaction temperature of microwave heating method was reduced by 80 °C, the reaction time was shortened by 2 h, and more elongated α′-Sialon grains with large aspect ratio were observed.展开更多
Currently,the carbothermal reduction-nitridation(CRN)process is the predominant method for preparing aluminum nitride(AlN)powder.Although AlN powder prepared by CRN process exhibits high purity and excellent sintering...Currently,the carbothermal reduction-nitridation(CRN)process is the predominant method for preparing aluminum nitride(AlN)powder.Although AlN powder prepared by CRN process exhibits high purity and excellent sintering activity,it also presents challenges such as the necessity for high reaction temperatures and difficulties in achieving uniform mixing of its raw materials.This study presents a comprehensive investigation into preparation process of AlN nanopowders using a combination of hydrothermal synthesis and CRN.In the hydrothermal reaction,a homogeneous composite precursor consisting of carbon and boehmite(γ-AlOOH)is synthesized at 200℃using aluminum nitrate as the aluminum source,sucrose as the carbon source,and urea as the precipitant.During the hydrothermal process,the precursor develops a core-shell structure,with boehmite tightly coated with carbon(γ-AlOOH@C)due to electrostatic attraction.Compared with conventional precursor,the hydrothermal hybrid offers many advantages,such as ultrafine particles,uniform particle size distribution,good dispersion,high reactivity,and environmental friendliness.The carbon shell enhances thermodynamic stability of γ-Al_(2)O_(3) compared to the corundum phase(α-Al_(2)O_(3))by preventing the loss of the surface area in alumina.This stability enables γ-Al_(2)O_(3) to maintain high reactivity during CRN process,which initiates at 1300℃,and concludes at 1400℃.The underlying mechanisms are substantiated through experiments and thermodynamic calculations.This research provides a robust theoretical and experimental foundation for the hydrothermal combined carbothermal preparation of non-oxide ceramic nanopowders.展开更多
β-Sialon/ZrN/ZrON composites were successfully fabricated by an in-situ carbothermal reduction？nitridation process with fly ash, zircon and active carbon as raw materials. The effects of raw materials composition an...β-Sialon/ZrN/ZrON composites were successfully fabricated by an in-situ carbothermal reduction？nitridation process with fly ash, zircon and active carbon as raw materials. The effects of raw materials composition and holding time on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by means of XRD and SEM. It was found that increasing carbon content in a sample and holding time could promote the formation of β-Sialon, ZrN and ZrON. The proper processing parameters to synthesize β-Sialon/ZrN/ZrON composites were mass ratio of zircon to fly ash to active carbon of 49：100：100, synthesis temperature of 1550 °C and holding time of 15 h. The average grain size ofβ-Sialon and ZrN（ZrON） synthesized at 1550 °C for 15 h reached about 2 and 1μm, respectively. The fabrication process ofβ-Sialon/ZrN/ZrON composites included the formation ofβ-Sialon and ZrO2 as well as the conversion of ZrO2 to ZrN and ZrON.展开更多
The optimum parameters were determined for synthesizing ZrN-Si3N4 composite powder from zircon by carbothermal reduction-nitridation （CTRN） process. The samples were prepared by mixing the carbon black of an average...The optimum parameters were determined for synthesizing ZrN-Si3N4 composite powder from zircon by carbothermal reduction-nitridation （CTRN） process. The samples were prepared by mixing the carbon black of an average particle size less than 30 μm and the zircon of 40 μm with C/ZrSiO4 mass ratios of 0.2, 0.3, 0.4, and 0.5. The prepared samples were subjected to the CTRN process at temperatures of 1673, 1723, 1753, and 1773 K for 6, 9, and 12 h. The CTRN process was conducted in an atmosphere-controlled tubular furnace in a nitrogen gas flow of 1.0 L/rain. All the products were examined by X-ray powder diffraction to determine the transformation. The results showed that the proper transformation of ZrN-Si3N4 occurred at 1773 K for 12 h with a C/ZrSiO4 mass ratio of 0.4.展开更多
β-Sialon based composites were successfully prepared from fly ash and carbon black under nitrogen atmosphere by carbothermal reduction-nitridation process. Effects of heating temperature and raw materials composition...β-Sialon based composites were successfully prepared from fly ash and carbon black under nitrogen atmosphere by carbothermal reduction-nitridation process. Effects of heating temperature and raw materials composition on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by X-ray diffraction and scanning electronic microscopy. The results show that increasing heating temperature or mass ratio of carbon black to fly ash can promote the formation of β-Sialon. The β-Sialon based composites can be synthesized at 1723 K for 6 h while heating the sample with mass ratio of carbon black to fly ash of 0.56. The as-received β-Sialon in the composites exists as granular with an average particle size of 2-3 μm. The preparation process of β-Sialon based composites includes the formation of O′-Sialon, X-Sialon and β-Sialon as well as the conversion processes of O′-Sialon and X-Sialon to β-Sialon.展开更多
The phase composition and microstructure of Sialon prepared from Chinese bauxite have been studied. The use of Si powder is more effective than that of activated carbon for reduction-nitridation. For bauxite specimens...The phase composition and microstructure of Sialon prepared from Chinese bauxite have been studied. The use of Si powder is more effective than that of activated carbon for reduction-nitridation. For bauxite specimens with 40～50% Si addition, more than 90% of Sialon may be obtained when nitrided at 1450～1500℃; the main crystalline phase is O′-Sialon (Z=0.2).展开更多
基金Project (2006AA06Z368) supported by High-tech Research and Development Programs of ChinaProject (N100402007) supported by the Fundamental Research Funds for the Central Universities in China
文摘(Ca, Mg)-α′-Sialon-AlN-BN powders were synthesized by the carbothermal reduction and nitridation (CRN) method using boron-rich slag, one of the intermediate products from pyrometallurgy separation of pageit, as the staring material. The influences of synthesis temperature and holding time on the phase composition and microstructure during the microwave CRN were studied by XRD, SEM and EDS. The comparison between two heating techniques, conventional and microwave heating, on the synthesized powder was presented as well. The experimental results revealed that the phase compositions and microstructures of the synthesized products were greatly affected by the synthesis temperature and holding time. With an increase in the synthesis temperature or holding time, the relative amount of α′-Sialon increased and α′-Sialon became the main crystalline phase at 1400 °C for 6 h. The synthesized products also contained AlN, BN and a small amount of β-SiC. Elongated α′-Sialon grains, short rod AlN grains, aggregate nanoscale BN grains were observed in the synthesized powders. The reaction temperature of microwave heating method was reduced by 80 °C, the reaction time was shortened by 2 h, and more elongated α′-Sialon grains with large aspect ratio were observed.
基金National Key Research and Development Program of China(2022YFB3708500,2023YFB3611000)Fujian Science&Technology Innovation Laboratory for Optoelectronic Information of China(2020ZZ109)。
文摘Currently,the carbothermal reduction-nitridation(CRN)process is the predominant method for preparing aluminum nitride(AlN)powder.Although AlN powder prepared by CRN process exhibits high purity and excellent sintering activity,it also presents challenges such as the necessity for high reaction temperatures and difficulties in achieving uniform mixing of its raw materials.This study presents a comprehensive investigation into preparation process of AlN nanopowders using a combination of hydrothermal synthesis and CRN.In the hydrothermal reaction,a homogeneous composite precursor consisting of carbon and boehmite(γ-AlOOH)is synthesized at 200℃using aluminum nitrate as the aluminum source,sucrose as the carbon source,and urea as the precipitant.During the hydrothermal process,the precursor develops a core-shell structure,with boehmite tightly coated with carbon(γ-AlOOH@C)due to electrostatic attraction.Compared with conventional precursor,the hydrothermal hybrid offers many advantages,such as ultrafine particles,uniform particle size distribution,good dispersion,high reactivity,and environmental friendliness.The carbon shell enhances thermodynamic stability of γ-Al_(2)O_(3) compared to the corundum phase(α-Al_(2)O_(3))by preventing the loss of the surface area in alumina.This stability enables γ-Al_(2)O_(3) to maintain high reactivity during CRN process,which initiates at 1300℃,and concludes at 1400℃.The underlying mechanisms are substantiated through experiments and thermodynamic calculations.This research provides a robust theoretical and experimental foundation for the hydrothermal combined carbothermal preparation of non-oxide ceramic nanopowders.
基金Project(2013AA030902)supported by the National High-tech Research and Development Program of ChinaProjects(51074038,51274057)supported by the National Natural Science Foundation of China+2 种基金Projects(N120402006,N100302002)supported by the Fundamental Research Funds for the Central Universities,ChinaProject(L2012079)supported by the Educational Commission of Liaoning Province of ChinaProject(110215)supported by the Training Program on National College Students Innovation Experiment
文摘β-Sialon/ZrN/ZrON composites were successfully fabricated by an in-situ carbothermal reduction？nitridation process with fly ash, zircon and active carbon as raw materials. The effects of raw materials composition and holding time on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by means of XRD and SEM. It was found that increasing carbon content in a sample and holding time could promote the formation of β-Sialon, ZrN and ZrON. The proper processing parameters to synthesize β-Sialon/ZrN/ZrON composites were mass ratio of zircon to fly ash to active carbon of 49：100：100, synthesis temperature of 1550 °C and holding time of 15 h. The average grain size ofβ-Sialon and ZrN（ZrON） synthesized at 1550 °C for 15 h reached about 2 and 1μm, respectively. The fabrication process ofβ-Sialon/ZrN/ZrON composites included the formation ofβ-Sialon and ZrO2 as well as the conversion of ZrO2 to ZrN and ZrON.
基金supported by the National Natural Science Foundation of China (No. 50274021)
文摘The optimum parameters were determined for synthesizing ZrN-Si3N4 composite powder from zircon by carbothermal reduction-nitridation （CTRN） process. The samples were prepared by mixing the carbon black of an average particle size less than 30 μm and the zircon of 40 μm with C/ZrSiO4 mass ratios of 0.2, 0.3, 0.4, and 0.5. The prepared samples were subjected to the CTRN process at temperatures of 1673, 1723, 1753, and 1773 K for 6, 9, and 12 h. The CTRN process was conducted in an atmosphere-controlled tubular furnace in a nitrogen gas flow of 1.0 L/rain. All the products were examined by X-ray powder diffraction to determine the transformation. The results showed that the proper transformation of ZrN-Si3N4 occurred at 1773 K for 12 h with a C/ZrSiO4 mass ratio of 0.4.
基金Project (51074038) supported by the National Natural Science Foundation of ChinaProject (N100302002) supported by the Fundamental Research Funds for the Central Universities, China
文摘β-Sialon based composites were successfully prepared from fly ash and carbon black under nitrogen atmosphere by carbothermal reduction-nitridation process. Effects of heating temperature and raw materials composition on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by X-ray diffraction and scanning electronic microscopy. The results show that increasing heating temperature or mass ratio of carbon black to fly ash can promote the formation of β-Sialon. The β-Sialon based composites can be synthesized at 1723 K for 6 h while heating the sample with mass ratio of carbon black to fly ash of 0.56. The as-received β-Sialon in the composites exists as granular with an average particle size of 2-3 μm. The preparation process of β-Sialon based composites includes the formation of O′-Sialon, X-Sialon and β-Sialon as well as the conversion processes of O′-Sialon and X-Sialon to β-Sialon.
文摘The phase composition and microstructure of Sialon prepared from Chinese bauxite have been studied. The use of Si powder is more effective than that of activated carbon for reduction-nitridation. For bauxite specimens with 40～50% Si addition, more than 90% of Sialon may be obtained when nitrided at 1450～1500℃; the main crystalline phase is O′-Sialon (Z=0.2).
