微波辅助固相法合成锂离子电池正极复合材料Li2FeSiO4/C

doi:10.3724/SP.J.1077.2012.11763

无机材料学报 ›› 2012, Vol. 27 ›› Issue (10): 1023-1029.DOI: 10.3724/SP.J.1077.2012.11763 CSTR: 32189.14.SP.J.1077.2012.11763

微波辅助固相法合成锂离子电池正极复合材料Li₂FeSiO₄/C

曹雁冰^1,2, 段建国¹, 胡国荣¹, 姜锋², 彭忠东¹, 杜柯¹

(中南大学1. 冶金科学与工程学院; 2. 材料科学与工程学院, 长沙 410083)

收稿日期:2011-12-09 修回日期:2012-02-04 出版日期:2012-10-20 网络出版日期:2012-09-17
基金资助:
中央高校基本科研业务费项目(2010Q22D0101, 2012QNZT018); 国家科技支撑计划项目(2007BAE12B01)

Synthesis of Li2FeSiO4/C Composite as Cathode Materials for Lithium Ion Battery by Microwave Assisted Solid Reaction Method

CAO Yan-Bing^1,2, DUAN Jian-Guo¹, HU Guo-Rong¹, JIANG Feng², PENG Zhong-Dong¹, DU Ke¹

(1. School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China; 2. School of Materials Science and Engineering, Central South University, Changsha 410083, China)

Received:2011-12-09 Revised:2012-02-04 Published:2012-10-20 Online:2012-09-17
Supported by:
Fundamental Research Funds for the Central Universities of China (2010Q22D0101, 2012QNZT018); National Key Technology Research and Development Program of China (2007BAE12B01)

摘要/Abstract

摘要： 以Na₂SiO₃·9H₂O和FeCl₂·4H₂O为原料, 采用低热固相反应获得了分散均匀的β-FeOOH/SiO₂前驱体; 再以Li₂CO₃为锂源、聚乙烯醇和超导电炭黑为复合碳源, 通过微波辅助固相法合成了Li₂FeSiO₄/C材料. 通过X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和恒电流充放电测试等方法对材料的结构、微观形貌及电化学性能进行表征. 650℃下微波处理12 min可获得结晶好、晶粒细小均匀的Li₂FeSiO₄/C材料; 在选用的微波合成体系下, 超导碳和聚乙烯醇热分解的无定形碳不仅利于合成反应的顺利进行, 而且提高了Li₂FeSiO₄的整体导电性能. 制备的复合正极材料在60 ℃下0.05C倍率首次放电容量为129.6 mAh/g, 0.5C倍率下为107.5 mAh/g, 0.5C下15次循环后保持为104.8 mAh/g, 具有较好的放电比容量和良好的循环稳定性能. 结果表明, 微波辅助固相合成工艺是制备Li₂FeSiO₄/C复合材料的一种很有前景的方法.

关键词: 正极材料, Li₂FeSiO₄, 微波辅助固相合成, 碳包覆

Abstract: The homogeneous distribution of FeOOH/SiO₂ precursor material was prepared from FeCl₂•4H₂O and Na₂SiO₃•9H₂O by low-heating solid-state reaction. Then Li₂FeSiO₄/C composites were prepared by microwave assisted solid reaction method, with prepared precursor FeOOH/SiO₂and Li₂CO₃as the starting materials, PVA and super-P carbon as carbon sources. The prepared samples were characterized by X-ray diffractometry, SEM, TEM, and galvanostatic charge-discharge test. Highly pure Li₂FeSiO₄/C material with uniform and fine particle size was obtained at 650℃ in 12 min. Under the selective microwave synthesis system, super-P carbon powder and pyrolyzed amorphous carbon not only effectively provided the high temperature to induce the complete reaction but also formed the conductive network to enhance the electronic conductivity. The optimum Li₂FeSiO₄/C composite displayed discharge capacity of 129.6 mAh/g at 0.05C rate and 107.5 mAh/g at 0.5C rate at 60℃. After 15 cycles the discharge capacity maintained 104.8 mAh/g at 0.5C, indicating good electrochemical capacity and cycling stability. Consequently, the results show that microwave assisted solid synthesis process is a promising method for preparing Li₂FeSiO₄/C composite.

Key words: cathode materials, Li₂FeSiO₄, microwave assisted solid synthesis, carbon coating

中图分类号:

TM912

曹雁冰, 段建国, 胡国荣, 姜锋, 彭忠东, 杜柯. 微波辅助固相法合成锂离子电池正极复合材料Li₂FeSiO₄/C[J]. 无机材料学报, 2012, 27(10): 1023-1029.

CAO Yan-Bing, DUAN Jian-Guo, HU Guo-Rong, JIANG Feng, PENG Zhong-Dong, DU Ke. Synthesis of Li2FeSiO4/C Composite as Cathode Materials for Lithium Ion Battery by Microwave Assisted Solid Reaction Method[J]. Journal of Inorganic Materials, 2012, 27(10): 1023-1029.

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微波辅助固相法合成锂离子电池正极复合材料Li₂FeSiO₄/C

Synthesis of Li2FeSiO4/C Composite as Cathode Materials for Lithium Ion Battery by Microwave Assisted Solid Reaction Method

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