从铅阳极泥中制备纳米三氧化二锑粉体的研究

以铅电解精炼过程中的副产物———铅阳极为原料,通过加入碳粉,使铅阳极泥中的高价锑还原成三氧化二锑;在低压下,用直接蒸发冷凝的方法制备了纳米三氧化二锑。此方法无需对铅阳极泥中所含其它成份进行分离,生产成本低。经XRD分析,产品为立方晶型三氧化二锑。SEM分析表明,产品为球形;粒度分布测定表明:平均粒度为66 nm,标准差(GSD)为1.67,粒度分布均匀;化学分析表明,产品中所含三氧化二锑大于97.5%。

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.

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 of ultrafine WC-10Co composite powders by reduction and carbonization

A solid state synthesis of ultrafine/nanocrystalline WC-10Co composite powders was reported from WO3 , Co3O4 and carbon powders after reduction and carburization at relatively low temperatures in a short time under pure H2 atmosphere. The effects of ball milling time and reaction temperature on the preparation of ultrafine/nanocrystalline WC-Co composite powders were studied using X-ray diffraction and scanning electron microscope (SEM). The results show that fine mixed oxide powders (WO3 , Co3O4 and carbon powders) can be obtained by long time ball milling. Increasing the reaction temperature can decrease the formation of Co3W3C and graphite phases and increase the WC crystallite size. Long-time ball milling and high reaction temperature are favorable to obtain fine and pure composite powders consisting of nanocrystalline WC from WO3 , Co3O4 and carbon powders.

SC-IrO_2 NR-carbon hybrid:A catalyst with high electrochemical stability for oxygen reduction

The enhanced electrochemical stability of the synthesized hybrid catalyst has been demonstrated by the introduction of the synergistic effect between carbon powder additive and the prepared catalyst.Single crystal IrO 2 nanorod (SC-IrO 2 NR) catalyst was prepared by a sol-gel method.The structure and performance of the catalyst sample were characterized by X-ray diffraction spectroscopy (XRD),scanning electron microscope (SEM),transmission electron microscope (TEM),rotating disk electrode (RDE) and cyclic voltammetry (CV) measurements.XRD patterns and TEM images indicate that the catalyst sample has a rutile IrO 2 single crystal nanorod structure.The onset potential for oxygen reduction reaction (ORR) of the SC-IrO 2 NR-carbon hybrid catalyst specimen is 0.75 V (vs.RHE) in RDE measurement.CV and RDE test results show that the SC-IrO 2 NR-carbon hybrid catalyst has a better electrochemical stability in comparison with the commercial Pt/C catalyst,with attenuation ratios of 17.67% and 44.60% for the SC-IrO 2 NR-carbon hybrid catalyst and the commercial Pt/C catalyst after 1500 cycles,respectively.Therefore,in terms of stability,the SC-IrO 2 NR-carbon hybrid catalyst has a promising potential in the application of the proton exchange membrane fuel cell.