Synthesis of (Ca, Mg)-α′-Sialon-AlN-BN powders from boron-rich blast furnace slag by microwave carbothermal reduction-nitridation

(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.

Fabrication of β-Sialon/ZrN/ZrON composites using fly ash and zircon

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.

Influence of processing parameters on the phase composition of ZrN-Si_3N_4 synthesized from zircon

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.

Effects of synthesis temperature and raw materials composition on preparation of β-Sialon based composites from fly ash

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.

Preparation and Microstructure of Bauxite-Based Sialon by Reduction Nitridation

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).