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二硫代钨酸铵晶体的合成、表征与热分解机理的研究

Synthesis, Characterization and Thermal Decomposition Mechanism of Ammonium Tungsten Oxide Sulfide Crystal

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【作者】 安高军柳云骐柴永明周同娜刘晨光

【Author】 AN Gao-Jun LIU Yun-Qi* CHAI Yong-Ming ZHOU Tong-Na LIU Chen-Guang (State Key Laboratory of Heavy Oil Processing, Key Laboratory of Catalysis, CNPC, China University of Petroleum, Dongying, Shandong 257061)

【机构】 中国石油大学 重质油国家重点实验室CNPC催化重点实验室中国石油大学重质油国家重点实验室东营257061

【摘要】 本工作用偏钨酸铵和硫化铵为原料,在水溶液中合成二硫代钨酸铵晶体[(NH4)2WO2S2]。用紫外-可见光谱(UV-Vis)的方法研究了二硫代钨酸铵晶体的形成机理。采用元素分析、X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、激光拉曼光谱(LRS)等对化合物进行了表征。结果表明采用该方法制备出的二硫代钨酸铵晶体,晶型良好。热重-差热分析(TG-DTA)、原位X射线衍射(insituXRD)和FTIR等结果表明二硫代钨酸铵晶体在氢气气氛下的热分解主要发生在160 ̄450℃之间,分两步进行,首先分解为{WOS2},随后转化为二硫化钨。

【Abstract】 Ammonium tungsten oxide sulfide [(NH4)2WO2S2] crystal was synthesized in aqueous solution using ammonium metatungstate (AMT) and ammonium sulfide as raw materials. The formation mechanism of (NH4)2WO2S2 was studied by Ultraviolet-visible (UV-Vis) spectroscopy. The as-synthesized compound was characterized by Elemental analysis, X-ray power diffraction (XRD), Fourier transform infrared (FTIR) and Laser Raman spectroscopy (LRS). The results show that the as-synthesized (NH4)2WO2S2 is with good crystallinity. In addition, thermogravimetric analysis (TG), differential thermal analysis (DTA), in situ XRD and FTIR results reveal that (NH4)2WO2S2 undergoes thermal decomposition in the range of 160~450 ℃ in hydrogen by two steps, where (NH4)2WO2S2 is converted to {WOS2} firstly between 160 ℃ and 300 ℃ and then transformed to WS2 eventually.

【基金】 国家重点基础研究发展规划(973计划)(No.2004CB217807);中国石油重点基础研究项目(No.04A50502)
  • 【文献出处】 无机化学学报 ,Chinese Journal of Inorganic Chemistry , 编辑部邮箱 ,2006年10期
  • 【分类号】O614.3
  • 【被引频次】2
  • 【下载频次】377
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