基于铁粉还原的LiFePO4/C合成路径及其电化学性能研究

doi:10.15541/jim20150583

无机材料学报 ›› 2016, Vol. 31 ›› Issue (8): 802-806.DOI: 10.15541/jim20150583

基于铁粉还原的LiFePO₄/C合成路径及其电化学性能研究

孟方礼¹, 章冬云¹, 常程康¹, 徐家跃¹, KAMZIN A S²

(1. 上海应用技术大学材料科学与工程学院, 上海 201418; 2. Ioffe Physical Technical Institute, Russian Academy of Sciences, St. Petersburg 194021, Russia)

收稿日期:2015-11-30 修回日期:2016-02-25 出版日期:2016-08-20 网络出版日期:2016-07-20
作者简介:孟方礼 (1991–), 男, 硕士研究生. E-mail: mfl828@126.com
基金资助:
国家自然科学基金(21203120);上海市科委能力建设项目(14520503100);上海市科委春笋计划(201310-JD-B2-009);上海市教委科研创新项目(15ZZ095)

Synthesis and Electrochemical Performance of LiFePO₄/C Cathode Materials Using Fe Powder

MENG Fang-Li¹, ZHANG Dong-Yun¹, CHANG Cheng-Kang¹, XU Jia-Yue¹, KAMZIN A S²

(1. School of Materials Science and Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2. Ioffe Physical Technical Institute, Russian Academy of Sciences, St. Petersburg 194021, Russia)

Received:2015-11-30 Revised:2016-02-25 Published:2016-08-20 Online:2016-07-20
About author:MENG Fang-Li. E-mail: mfl828@126.com
Supported by:
National Natural Science Foundation of China(21203120), Shanghai Committee of Science and Technology (14520503100, 201310-JD-B2-009);Shanghai Municipal Education Commission(15ZZ095)

摘要/Abstract

摘要：

使用还原铁粉作为铁源, 通过超细球磨与喷雾干燥、高温煅烧技术制备了球形微纳米LiFePO₄/C复合材料。使用DSC/TG以及XRD对LiFePO₄/C复合材料的形成过程进行了分析; 使用SEM、穆斯堡谱仪等手段对复合材料进行分析; 使用电化学工作站、容量测试仪对其充放电行为进行分析。研究发现, 使用该合成技术路线, 在500~700℃下能够合成LiFePO₄/C复合材料。获得的LiFePO₄/C复合材料具有规则的球形外貌, 平均尺寸4~5 μm。该微米颗粒由200 nm左右细小颗粒组成, 颗粒间具有纳米尺寸微孔。穆斯堡谱仪测试结果表明, 复合材料中Fe处于+2价的价态。复合材料在1C倍率下表现出稳定的充放电行为, 平均比容量在156 mAh/g, 300次循环后, 容量保持率为92.8%。该技术制备的LiFePO₄/C复合材料具有潜在的应用价值。

关键词: 磷酸铁锂, 超细球磨, 穆斯堡谱, 比容量, 循环性能

Abstract:

Using Fe source as starting material, the composite LiFePO₄/C material was obtained through a combined method of nano grinding, spray drying and high temperature calcinating. The as-prepared samples were verified by TG/DSC and XRD and characterized by SEM and Mossbauer spectrum. The electrochemical performances were studied by CV and cyclic tests. The results show that the LiFePO₄/C composite is successfully synthesized by calcinating the precursor at 500-700℃. The obtained LiFePO₄/C materials are spherical porous agglomerates with mean size of 4-5 μm, which are composed of 200 nm particles. According to Mössbauer data, all the iron ions are in +2 valence state. The spherical nano LiFePO₄/C composite shows great electrochemical performance as potential cathode material for lithium ion batteries, with a specific capacity of 156 mAh/g at 1C rate and capacity retention of 92.8% after 300 charge/discharge cycles.

Key words: LiFePO4, nano grinding, Mossbauer spectrum, specific capacity, cyclic performance

中图分类号:

TQ73

孟方礼, 章冬云, 常程康, 徐家跃, KAMZIN A S. 基于铁粉还原的LiFePO₄/C合成路径及其电化学性能研究[J]. 无机材料学报, 2016, 31(8): 802-806.

MENG Fang-Li, ZHANG Dong-Yun, CHANG Cheng-Kang, XU Jia-Yue, KAMZIN A S. Synthesis and Electrochemical Performance of LiFePO₄/C Cathode Materials Using Fe Powder[J]. Journal of Inorganic Materials, 2016, 31(8): 802-806.

图/表 5

图1 前驱体的(a)XRD图谱以及(b)TG-DSC 曲线

Fig. 1 XRD pattern (a) and TG-DSC curves (b) of the as-sprayed precursor

图2 不同煅烧温度下获得材料LiFePO4/C的XRD图谱

Fig. 2 XRD patterns of LiFePO4/C composites calcined at different temperatures

图3 前驱体(a, c)和煅烧获得的LiFePO4/C(b, d)的SEM照片

Fig. 3 SEM images of precursor (a, c) and as-calcined LiFePO4/C composite (b, d)

图4 前驱体(a)和煅烧获得的LiFePO4/C复合材料(b)的穆斯堡谱图

Fig. 4 Mössbauer spectra of precursor (a) and as-calcined LiFePO4/C powder (b)

图5 球形微纳米LiFePO4/C复合材料的(a) CV曲线, (b)不同倍率下首次充放电行为和(c)循环特性

Fig. 5 (a) CV curve, (b) first runs at different rates and (c) cyclic performances of LiFePO4/C composite

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基于铁粉还原的LiFePO₄/C合成路径及其电化学性能研究

Synthesis and Electrochemical Performance of LiFePO₄/C Cathode Materials Using Fe Powder

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