引用本文:
程继贵, 熊二涛, 蒋阳, 夏永红, 吴玉程. WS2超细粉体的固相法合成[J]. 应用化学,
2006, 23(7): 786-789.
Citation: CHENG Ji-Gui, XIONG Er-Tao, JIANG Yang, XIA Yong-Hong, WU Yu-Cheng. Preparation and Characterization of Tungsten Disulfide Ultra-fine Powders by Solid State Reaction Method[J]. Chinese Journal of Applied Chemistry, 2006, 23(7): 786-789.

Citation: CHENG Ji-Gui, XIONG Er-Tao, JIANG Yang, XIA Yong-Hong, WU Yu-Cheng. Preparation and Characterization of Tungsten Disulfide Ultra-fine Powders by Solid State Reaction Method[J]. Chinese Journal of Applied Chemistry, 2006, 23(7): 786-789.

WS2超细粉体的固相法合成
摘要:
以W粉和S粉为原料,混合压片后,在保护气氛中加热反应合成WS2粉体,考察了反应温度、过硫系数等对反应的影响。同时研究了W-S混合粉末高能球磨处理对合成反应和产物性能的影响。X射线衍射分析(XRD)结果表明,在适当的反应温度(650℃)和过硫系数(2.0)下,通过固相法可合成出具有六方结构的WS2粉体。透射电镜观测表明,以经过高能球磨的W-S混合粉为原料,控制反应温度650℃,过硫系数1.5,所制得的WS2粉末粒度细小均匀,尺寸在0.1~0.4 μm,与激光粒度仪测得粒径相一致。实验结果表明,高能球磨处理可以细化原料粒度,提高反应物粉体的活性,有利于WS2的形成。对固相法制备WS2的反应机理进行了初步探讨。
English
Preparation and Characterization of Tungsten Disulfide Ultra-fine Powders by Solid State Reaction Method
Abstract:
Ultra-fine WS2 powders were synthesized via an improved solid reaction method from mixed tungsten and sulfur powders with different excessive sulfur coefficients(ESC),followed by the reactions in N2 or Ar atmosphere at different temperatures.Phase composition,morphology and particle size of the resulting powders were characterized by X-ray diffraction(XRD),transmission electron microscopy(TEM) and laser diffraction method.Effects of the reaction temperature and the excessive sulfur coefficient(ESC) on the phase composition and the morphology of the resulting powders were also investigated.Furthermore,W-S powders were mixed by high energy ball milling to investigate the effects of raw materials on the performance of the synthesized WS2 powders.XRD results show that pure and hexagonal tungsten disulfides are obtained at a temperature of 650℃ and an ESC of 2.0 for the ordinary blended W-S powder mixes, but only an ESC of 1.5 is needed for the high energy ball milled W-S powder mixes at the same reaction temperature.The WS2 powder synthesized have an ultrafine particle size of 0.1~0.4 μm with a granular particle shape.It was also shown that the atmosphere has an important influence on the synthesis reaction.
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