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作 者:周百斌[1] 韦永德[2] 李中华[2] 郭元茹[1]
机构地区:[1]哈尔滨师范大学化学系,黑龙江哈尔滨150080 [2]哈尔滨工业大学应用化学系,黑龙江哈尔滨150001
出 处:《中国稀土学报》2002年第z3期83-87,共5页Journal of the Chinese Society of Rare Earths
基 金:国家自然科学基金资助项目(29671009)
摘 要:用降解法合成了具有Keggin结构的钇钨硅多金属氧酸盐,以化学分析、TG曲线和ICP确定通式为K10H3[Y(SiW11O39)2]。利用IR、183W NMR等手段对配合物的结构进行了表征和研究,结果表明配合物具有Keggin结构。TG DTA分析表明配合物在400~450℃范围内仍不分解。对配合物进行了化学热扩渗稀土的实验。经ICP和XPS测试表明:微量稀土元素可以渗入到配合物的表、界面乃至体相,同时用四探针法和交流阻抗谱测试了不同温度下的电导率,扩渗后样品的电导率σ=1.935×10-2S·cm-1,比扩渗前提高约105倍,且随温度的升高,导电性增强,有望成为具有实际应用的多金属氧酸盐型固体电解质。The title compound was synthesized by means of degradation. The composition was determined by chemical analysis, TG and ICP. The studies of IR, 183W-NMR data indicate that the compound has the Keggin structure. And the results of TG DTA show that the compound is 400~450 ℃. The product, which is permeated, is analyzed with ICP and is proved to process the rare earth elements including. The spectra of IR and X ray powder diffraction patterns also show great differences between the products of before and after permeation and the disappearance of the characteristic bands of Keggin type structure. Such results indicate that the structure of complex have changed after permeation and rare earth elements have already entered the inner sphere of the compound. The XPS also gives the evidence that the rare earth elements form the weak binds with the Polyoxometalates. And accordingly, the conductivity of the complex change, too. The conductivity of the permeated sample is 1.935×10 -2 S·cm -1 , which is 105 times higher than that of K 10 H 3[Y(SiW 11 O 39 ) 2].
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