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
作者单位
安高军 中国石油大学重质油国家重点实验室CNPC催化重点实验室东营 257061 
柳云骐 中国石油大学重质油国家重点实验室CNPC催化重点实验室东营 257061 
柴永明 中国石油大学重质油国家重点实验室CNPC催化重点实验室东营 257061 
周同娜 中国石油大学重质油国家重点实验室CNPC催化重点实验室东营 257061 
刘晨光 中国石油大学重质油国家重点实验室CNPC催化重点实验室东营 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(in situ XRD)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。
关键词: 二硫代钨酸铵  偏钨酸铵  原位XRD  热分解机理
基金项目: 
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.
Keywords: ammonium tungsten oxide sulfide  ammonium metatungstate  in situ XRD  thermal decomposition mechanism
 
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安高军,柳云骐,柴永明,周同娜,刘晨光.二硫代钨酸铵晶体的合成、表征与热分解机理的研究[J].无机化学学报,2006,22(10):1813-1818.
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