真空碳热还原固相合成磷酸铁锂的正交实验 - 周环波 .docVIP

收稿日期:2009-09-22 基金项目:湖北省教育厅重点项目(D者简介:周环波(1961—,男,湖北省人,博士,教授,主要研究方向为化学电源材料及电化学。 真空碳热还原固相合成磷酸铁锂的正交实验 周环波1,林 丽2,程 凡1,龚春丽1,王 丽1 (1.孝感学院化学与材料科学学院,湖北孝感432100;2.孝感学院新技术学院,湖北孝感432100 摘要:采用真空条件下的碳热还原固相方法,以Fe 2O 3、LiOH 和P 2O 5为原料、活性炭为还原剂,合成了锂离子电池正极材料LiFePO 4;选择真空度、原料配比、反应温度、恒温保持时间(反应时间和升温速率等5个影响因素,设计了一组5因素4水平(L 1645的正交实验,较系统地研究了LiFePO 4的合成工艺参数及电化学性能。研究结果表明:真空碳还原合成LiFePO 4工艺参数因素对材料电化学性能影响的大小顺序为:反应温度原料配比反应时间真空度升温速率;反应温度控制在600~650℃时所合成的LiFePO 4材料的晶体结构和电性能较好;原料LiOH 、Fe 2O 3、P 2O 5和活性炭比例为1.05∶1∶1∶1.8、反应时间为12~18h 、真空度控制10-1~10Pa 时,所得LiFePO 4材料的综合电化学性能较好。 关键词:磷酸铁锂;正交实验;碳热还原;真空中图分类号:TM 912.9 文献标识码:A 文章编号:1002-087X(201004-0367-04 Orthogonal experiments on preparation of LiFePO 4under carbothermal reduction method in vacuum condition ZHOU Huan-bo 1,LIN Li 2,CHENG Fan 1,GONG Chun-li 1,WANG Li 1 (1.College of Chemistry and Material Science,Xiaogan University,Xiaogan Hubei 432100,China; 2.College of Technology,Xiaogan University,Xiaogan Hubei 432100,China Abstracts:LiFePO 4samples were synthesized under vacuum condition using Fe 2O 3,LiOH and P 2O 5as raw material and carbon as reduction reagent. The orthogonal experiments were carried out for studying the techniques of LiFePO 4synthesis and the electrochemical performance choosing vacuum,material ratio,react temperature,and react time and heating rate as the five factors.The results indicate that the sequence of the main factors affecting the electrochemical performance of LiFePO 4were react temperature, material ratio, react time and vacuum and heating rate and the reaction temperature was the most important factor affecting the electrochemical performance of LiFePO 4.LiFePO 4samples displays better electrochemical performance when the proportion of LiOH,Fe 2O 3,P 2O 5and carbon is 1.05∶1∶1∶1.8,the reaction temperature is 600-650℃,the reaction time is 12-18h,and the vacuum pressure is 10-1-10Pa. Key words:LiFePO 4;orthogonal experiments;carbothermal reduction method;vacuum 磷酸铁锂(LiFePO 4作为锂离子电池正极材料具有良好的发展前景,该材料具有极好的热稳定性,制造的电