用固相和水热结合法制备LiMn0.4Fe0.6PO4/C复合材料

doi:10.3724/SP.J.1077.2014.13672

无机材料学报 ›› 2014, Vol. 29 ›› Issue (4): 443-448.DOI: 10.3724/SP.J.1077.2014.13672 CSTR: 32189.14.SP.J.1077.2014.13672

• 研究快报 • 上一篇

用固相和水热结合法制备LiMn_0.4Fe_0.6PO₄/C复合材料

李荐^1,2,3, 姚书恒¹, 周宏明^1,2,3, 耿文俊¹

(1. 中南大学材料科学与工程学院, 长沙410083; 2. 湖南省正源储能材料与器件研究所, 长沙410083; 3. 中南大学有色金属材料科学与工程教育部重点实验室, 长沙410083)

收稿日期:2013-12-19 修回日期:2014-01-08 出版日期:2014-04-20 网络出版日期:2014-03-24
作者简介:李荐. E-mail: ziliao2000@126.com
基金资助:
Hunan Science and Technology Project(2013GK3002); Changsha Science and Technology Project (K1202039-11)

Preparation of LiMn_0.4Fe_0.6PO₄/C Composite by A New Route Combining Solid-state Reaction with Hydrothermal Synthesis

LI Jian^{1, 2, 3}, YAO Shu-Heng¹, ZHOU Hong-Ming^{1, 2, 3}, GENG Wen-Jun¹

(1. School of Materials Science and Engineering, Central South University, Changsha 410083, China; 2. Hunan Zhengyuan Institute for Energy Storage Materials and Devices, Changsha 410083, China; 3. Key Laboratory of Nonferrous Metal Materials Science and Engineering of Ministry of Education, Central South University, Changsha 410083, China)

Received:2013-12-19 Revised:2014-01-08 Published:2014-04-20 Online:2014-03-24
About author:LI Jian(1969–), male, PhD. E-mail: ziliao2000@126.com
Supported by:
Hunan Science and Technology Project(2013GK3002); Changsha Science and Technology Project (K1202039-11)

摘要/Abstract

摘要： 以Li₂CO₃、FeC₂O₄•2H₂O、MnCO₃和 NH₄H₂PO₄为原料, 按5:6:4:10的摩尔比混合, 采用固相反应和水热法结合的新方法制备得到LiMn_0.4Fe_0.6PO₄。通过XRD、SEM、TEM以及循环伏安(CV)和充放电测试对材料进行结构、形貌以及电化学性能表征。结果表明, 此方法合成的产物具有单一的橄榄石晶体结构, 颗粒尺寸约为120 nm, 且表面均匀包覆一层无定形碳。电化学测试结果表明, 样品的循环伏安曲线中有两对氧化还原峰, 分别对应Fe³⁺/Fe²⁺(3.5 V)和Mn³⁺/Mn²⁺(4.0 V)。LiMn_0.4Fe_0.6PO₄/C在0.1C下的初始放电比容量为160 mAh/g, 0.5C下的初始放电比容量为143 mAh/g, 且具有较好的循环性能。

关键词: 锂离子电池, 固相反应, 水热合成, 电化学性能, 电子显微技术

Abstract: The olivine type LiMn_0.4Fe_0.6PO₄ was synthesized via a new route that combining solid-state reaction with hydrothermal synthesis from Li₂CO₃, FeC₂O₄·2H₂O, MnCO₃ and NH₄H₂PO₄ (molar ratio of 5:6:4:10). The structure, particle size and surface morphology of these cathode active materials were investigated by XRD, SEM and TEM techniques. The electrochemical properties of LiMn_0.4Fe_0.6PO₄/C as cathode in lithium-ion cells were tested via cyclic voltammetry and galvanostatic charge-discharge measurements. Phase-pure particles of size ~120 nm are prepared with a conductive, thin web of carbon surrounding them. Cyclic voltammetry shows the active voltage range of the material which consists of two pairs of redox peaks: 3.5 V corresponding to Fe³⁺/Fe²⁺ reaction and 4.0 V corresponding to Mn³⁺/Mn²⁺ reaction. An initial discharge capacity of 160 mAh/g at 0.1C, 143 mAh/g and a stable cycling property at 0.5C are obtained for the LiMn_0.4Fe_0.6PO₄/C composite.

Key words: Li-ion battery, solid-state reaction, hydrothermal synthesis, electrochemical property, electron microscopy

中图分类号:

TQ174

李荐, 姚书恒, 周宏明, 耿文俊. 用固相和水热结合法制备LiMn_0.4Fe_0.6PO₄/C复合材料[J]. 无机材料学报, 2014, 29(4): 443-448.

LI Jian, YAO Shu-Heng, ZHOU Hong-Ming, GENG Wen-Jun. Preparation of LiMn_0.4Fe_0.6PO₄/C Composite by A New Route Combining Solid-state Reaction with Hydrothermal Synthesis[J]. Journal of Inorganic Materials, 2014, 29(4): 443-448.

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用固相和水热结合法制备LiMn_0.4Fe_0.6PO₄/C复合材料

Preparation of LiMn_0.4Fe_0.6PO₄/C Composite by A New Route Combining Solid-state Reaction with Hydrothermal Synthesis

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