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四钼簇合物具有非线性光学性质,本文对它的光谱,电氧化还原性质,X光电子能谱进行研究.并用半经验的量子化学方法对它的电子结构作了理论上的解释. 实验部分光谱测定标题簇合物的合成和晶体结构测定见文献[1].采用PE-783红外光谱仪,KBr压片法测定红外光谱.用UV-365型紫外可见光谱仪,测定固体反射光谱。循环伏安测定用DH-1型多功能恒电位仪,3086型x-y记录仪.电解池由三电极组成,工作电极和辅助电极均采用光滑铂片,参考电极为222型饱和甘汞电极,通过盐桥和鲁金毛细管与研究电极连接.测试样品的浓度为10~(-4)～10~(-3)mol·L~(-1)样品溶解在含有0.1mol·L~(-1)的高氯酸正丁基铵的DMF溶液中,测试始终以干燥净化的氮气通入电解池中,扫描电压范围为-1.6～+1.4V.室温下在+1.4V开始扫描,测得循环伏安曲线绘于图1.
Tetra-molybdenum cluster has non-linear optical properties. In this paper, its spectra, electrooxidative reduction properties and X-ray photoelectron spectroscopy are studied. Its electronic structure is theoretically explained by semi-empirical quantum chemistry method. The experimental part Spectroscopic determination of the title cluster synthesis and crystal structure determination in the literature [1]. PE-783 infrared spectrometer, KBr tablet method for the determination of infrared spectroscopy. UV-365 UV-visible spectrometer to measure the solid reflection spectrum. Cyclic voltammetry with DH-1-type multi-function potentiostat, 3086 xy recorder.The electrolytic cell consists of three electrodes, the working electrode and the auxiliary electrode are made of smooth platinum, the reference electrode is 222 saturated calomel electrode, through the Salt bridge and Lujin capillary were connected with the research electrode.The samples were dissolved in the solution containing 0.1 mol·L -1 of 10 ~ (-4) ~ 10 ~ (-3) mol·L ~ (-1) Of ammonium perchlorate in DMF and the test was always conducted with dry, purified nitrogen into the cell at a scan voltage ranging from -1.6 to +1.4 V. Scanning was started at + 1.4V at room temperature and cyclic voltammetry Ancurves are plotted in Figure 1.