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Waugh结构(NH4)6[NiMo9O32]·8H2O杂多酸盐的合成、表征及电化学性质研究
引用本文:刘伟,袁华,王立霞,杨慧芳,谢德银.Waugh结构(NH4)6[NiMo9O32]·8H2O杂多酸盐的合成、表征及电化学性质研究[J].沧州师专学报,2008,24(1):27-29.
作者姓名:刘伟  袁华  王立霞  杨慧芳  谢德银
作者单位:沧州师专化学与环境科学系 河北沧州061001
基金项目:河北省教育学会科研基金
摘    要:以(NH4)6Mo7O24.4H2 O,NiSO4和(NH4)2S2O8为原料合成了(NH4)6NiMo9O32]·8H2O杂多酸盐,并利用化学分析、差热热重、红外光谱、紫外光谱、循环伏安等方法对其进行了元素分析、结构及性质的研究。样品的红外光谱分析显示:在1000-400cm^-1处由两组突出的峰组成,显示出Waugh结构单元的特征谱带;紫外可见光谱分析显示:紫外区吸收峰位置为207nm处,可见区吸收峰位置为563.2nm;差热-热重分析显示:该化合物在1067.9-1103.5K分解,说明具有较高热稳定性;循环伏安曲线显示:该电极反应为半可逆过程,是以扩散控制的表面氧化还原过程,且伴随质子化。

关 键 词:Waugh结构  九钼镍杂多酸铵  合成  表征
文章编号:1008-4762(2008)01-0027-03
修稿时间:2006年10月21

Synthesis and Characterization of Ammonium 9-molybdate Nickel Heteropoly Salt with Waugh Sructure.
LIU Wei,YUAN Hua,WANG Li-xia,YANG Hui-fang,XIE De-yin.Synthesis and Characterization of Ammonium 9-molybdate Nickel Heteropoly Salt with Waugh Sructure.[J].Journal of Cangzhou Teachers‘College,2008,24(1):27-29.
Authors:LIU Wei  YUAN Hua  WANG Li-xia  YANG Hui-fang  XIE De-yin
Institution:(Department of Chemistry ,Cangzhou Teachers College, Hebei Cangzhou 061001 China )
Abstract:Ammonium 9-molybdate nickel heteropoly salt with Waugh structure was synthesized by the reaction of nickel sulfate and ammonium heptamolybdate by oxidation of ammonium peroxydisulfate at acetic acid pH4-6.The title compound was characterized by IR,UV-Vis,TG-DT thermal analysis and CV.The fomula was determined by chemical analysis to be(NH4)6NiMo9O32].8H2O.It can be seen from IR spectrum that there are characteristic band of Waugh-type heteropolyacidic salt in the range of 1000-400cm-1.From UV spectrum,in Ultraviolet region there is a band at 207nm assigned to electronic transition from double bonds of oxygen to Mo atom and there is a bond at 563.2nm in visible range.We can see from the TG-DTA curves that ammonium 9-molybdate nickel heteropoly salt can be decomposed at 1067.9-1103.5K..It indicated from the cyclic voltammetry(CV) curve there was a good linear relationship between ip and v1/2,suggesting the electrode reaction being controlled by diffusion oxido-reduction process.The voltage of cathodic and anodic peak was becoming progressively more positive with decreasing pH,the variation presumably related to variation in protonation.of the cluster.
Keywords:ammonium 9-molybdate nickel heteropoly salt synthesis  characterization Waugh structure  cyclic voltammetry(CV)  IR  UV-Vis  TG-DTA
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