草酸配体修饰的锆取代型硅钨-氧簇合物的合成、结构和电化学性质研究  

Synthesis,Crystal Structure,and Electrochemical Properties of a Ox-Functionalized Zirconium(Ⅳ)Substituted Tungsten-Oxo Cluster

作　　者：张众 杨琳[1] 李晓慧 王梓兰 王静怡 ZHANG Zhong;YANG Lin;LI Xiaohui;WANG Zilan;WANG Jingyi(Professional Technology Innovation Center of Liaoning Province for Conversion Materials of Solar Cell,College of Chemistry and Materials Engineering,Bohai University,Jinzhou 121013,China)

机构地区：[1]渤海大学化学与材料工程学院,辽宁省全谱太阳能电池转光材料专业技术创新中心,锦州121013

出　　处：《人工晶体学报》2021年第5期884-888,共5页Journal of Synthetic Crystals

基　　金：国家自然科学基金青年科学基金(21901018);中国博士后科学基金(2019M650498);渤海大学博士启动基金(0520bs027)。

摘　　要：通过水热反应,成功合成了一个草酸配体修饰的四核锆取代的夹心型硅钨-氧簇合物H_(12)Na_(2)[Zr_(4)(μ_(3)-O)_(2)(μ2-OH)_(2)(Ox)_(2)(α-SiW_(10)O_(37))_(2)]·22H_(2) O(Ox=oxalic acid)。该夹心型硅钨-氧簇是由两个{α-SiW_(10)O_(37)}簇块通过一个{Zr_(4)(μ_(3)-O)_(2)(μ2-OH)_(2)(Ox)_(2)}簇连接构成的。通过X-射线单晶衍射、IR、TG以及元素分析对该簇合物进行表征。晶体结构分析表明:该簇合物结晶于单斜晶系,P2_(1/c)空间群,a=2.1322(6)nm,b=1.2716(4)nm,c=2.2231(7)nm,β=110.933(4)°,V=5.6299(3)nm^(3),Z=2,R 1=0.0615,w R^(2)=0.1644。电化学和电催化性质研究表明标题簇合物对NO^(-)_(2)的还原有很好的电催化效果。Under hydrothermal conditions,a new Ox-functionalized zirconium(Ⅳ)substituted tungsten-oxo cluster,H_(12)Na_(2)[Zr_(4)(μ_(3)-O)_(2)(μ2-OH)_(2)(Ox)_(2)(α-SiW_(10)O_(37))_(2)]·22H_(2) O(Ox=oxalic acid)was successfully obtained and characterized by single crystal X-ray diffraction analysis,IR,TG and elemental analysis.The title compound consists of a sandwich-type tungsten-oxo cluster unit built by two divacant{α-SiW_(10)O_(37)}fragments linked through a{Zr_(4)(μ_(3)-O)_(2)(μ2-OH)_(2)(Ox)_(2)}cluster and crystallizes in the monoclinic system,space group P 2_(1/c) with a=2.1322(6)nm,b=1.2716(4)nm,c=2.2231(7)nm,β=110.933(4)°,V=5.6299(3)nm^(3),Z=2,R 1=0.0615,w R^(2)=0.1644.The electrochemistry and electrocatalytic properties of the title compound were studied,and it exhibits excellent catalytic activities for NO^(-)_(2) reduction.

关 键 词：水热合成 草酸 钨-氧簇合物 晶体结构 电化学 电催化性质 

分 类 号：O611[理学—无机化学]