固相反应合成掺铜磷酸锌锂及其结晶度的研究  

Study on synthesis and crystallization degree of Cu^(2+)-doped lithium zinc phosphate by solid state reaction

作　　者：廖森[1] 陈霞[1] 吴文伟[1] 王天顺[1] 

机构地区：[1]广西大学化学化工学院,广西南宁530004

出　　处：《无机盐工业》2007年第12期13-15,22,共4页Inorganic Chemicals Industry

基　　金：教育部科研重点项目(205120);广西科学基金(桂科基0575006);广西测试基金(2006年)

摘　　要：以硫酸锌和磷酸铵为原料,以硫酸铜为掺杂剂,以PEG-400为表面活性剂,经低热固相反应制得掺铜磷酸锌铵。接着以PEG-400为表面活性剂,用掺铜磷酸锌铵与碳酸锂经室温固相反应得到前驱体,然后在700℃下煅烧前驱体得到锂电池电极材料掺铜磷酸锌锂纳米晶。用产物XRD图谱数据计算得到的结晶度作为考察指标,应用均匀设计试验法及数据挖掘技术,在数据挖掘成果的指导下进行了试验,试验结果表明产物的结晶度随着掺杂铜离子的增加而急剧下降。用最优工艺条件合成得到的产物为50 nm的掺铜磷酸锌锂,结晶度为96.30%,与数据挖掘得到的最佳结果相吻合。试验结果表明应用固相合成法制备掺杂磷酸锌锂及把结晶度作为一种指标去控制合成结果是可行的。Cu^2＋-doped ammonium zinc phosphate was prepared by low-heat solid state reaction with zinc sulphate and ammonium phosphate as raw materials,copper sulphate as doping agent and PEG-400 as surfactant.Then use Cu^2＋-doped ammonium zinc phosphate to react with lithium carbonate at room temperature in the solid state with PEG-400 as surfactant to prepare precursor.The nano-sized crystal of Cu^2＋-doped lithium zinc phosphate-electrode material of lithium-ion battery was prepared finally by sintering the precursor at the temperature of 700 ℃.Crystallization degree of the products calculated with XRD data was used as a testing index,and by the application of uniform experimental design as well as data mining technology,experiments have been made under the direction of data mining results.The experimental results indicated that crystallization degree of the products reduced sharply with the increase of Cu^2＋-doped.The product synthesized with the optimal technical conditions was Cu^2＋-doped LiZnPO4 with size of 50 nm,and the crystallization degree of product was 96.30% that inosculate with the optimization result of data mining.Test results showed that it′s feasible to prepare Cu^2＋-doped LiZnPO4 by solid state reaction and to control the synthesis results with crystallization degree as a testing index.

关 键 词：磷酸锌锂 固相反应 均匀设计 数据挖掘技术 

分 类 号：TQ126.35[化学工程—无机化工]