高等学校化学学报

高等学校化学学报 ›› 2004, Vol. 25 ›› Issue (6): 1005.

• 研究论文 • 上一篇    下一篇

ZrW1.7ⅥW0.3ⅤO7H0.3(OH)2·2H2O的合成与表征

赵怀周1,2, 赵新华1, 韩布兴2   

  1. 1. 北京师范大学化学系, 北京 100875;
    2. 中国科学院化学研究所, 北京 100080
  • 收稿日期:2003-06-24 出版日期:2004-06-24 发布日期:2004-06-24
  • 通讯作者: 赵新华(1949年出生),男,硕士,教授,博士生导师,从事无机固体化学研究.E-mail:xinhuaz@bnu.edu.cn; 韩布兴(1957年出生),男,博士,研究员,博士生导师,从事物理化学研究.E-mail:hanbx@infoc3.icas.ac.cn E-mail:xinhuaz@bnu.edu.cn;hanbx@infoc3.icas.ac.cn
  • 基金资助:

    国家自然科学基金(批准号:29871006,20133030)和北京市无机化学重点学科项目资助.

Synthesis and Characterization of ZrW1.7ⅥW0.3Ⅴ O7H0.3（OH）2·2H2O

ZHAO Huai-Zhou1,2, ZHAO Xin-Hua1, HAN Bu-Xing2   

  1. 1. Department of Chemistry, Beijing Normal University, Beijing 100875, China;
    2. Center for Molecular Science, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100080, China
  • Received:2003-06-24 Online:2004-06-24 Published:2004-06-24

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摘要： 分别利用微乳液水热法和酸蒸气水热法合成了杂多蓝化合物ZrW1.7ⅥW0.3ⅤO7H0.3(OH)2·2H2O.XRD测定结果表明,该化合物与ZrMo2O7(OH)2·2H2O具有相同晶体结构类型.使用Rietveld方法对产物进行了结构精修,并计算出了键参数和键价.运用EPR技术测定了该化合物中W的价态,并利用XPS能谱测定了W/W的比例.利用价键和规则,指出ZrW1.7ⅥW0.3ⅤO7H0.3(OH)2·2H2O中的W—O3—H0.15存在羟基化现象,并对杂多蓝化合物的红外吸收光谱进行了指认.

关键词: 杂多蓝, ZrW1.7ⅥW0.3ⅤO7H0.3(OH)2·, 2H2O, 电子顺磁共振

Abstract: A new sort of heteropoly blue compound,ZrW1.7ⅥW0.3ⅤO7H0.3(OH)2·2H2O,was synthesized by the acidic-steam hydrothermal process and the microemulsion hydrothermal process. XRD pattern proves that the heteropoly blue compound has the same type of crystal structure as that of ZrMo2O7（OH）2· 2H2O. The rietveld refinement method was used to refine the crystal structure of the heteropoly blue compound. The bond parameters were calculated and the bond valences of atoms were obtained. The EPR result affirmed the subsistence of W Ⅴ ion in the new compound,and the molar ratio of W Ⅴ/W Ⅵ was determined by XPS. Combining with bond valences of atoms and IR spectra analysis,random hydroxylation of W—O3—H0.15 exits in the molecule and the FTIR absorption spectra were assigned.

Key words: Heteropoly blue, ZrW1.7ⅥW0.3ⅤO7H0.3(OH)2·2H2O, EPR

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