片状LiFePO4/C正极材料制备及其电化学性能研究

doi:10.11949/j.issn.0438-1157.20181395

摘要/Abstract

摘要：

在温和的反应条件下，使用十二烷基苯磺酸钠(SDBS)成功合成了片状二水磷酸铁，并将其与氢氧化锂、柠檬酸球磨混合，采用碳热还原法制备了具有纳米厚度的片状LiFePO₄/C电极材料。研究了SDBS对磷酸铁形貌以及LiFePO₄/C电极材料电化学性能的影响。利用X-射线衍射、扫描电子显微镜和充放电测试等技术手段，对合成样品的物相、形貌和电化学性能进行了分析测试。电化学测试表明，在25℃，2.0～4.2 V电压范围条件下，使用片状二水磷酸铁为前驱体制备的LiFePO₄/C样品，在0.1 C下放电比容量高达166.4 mA·h·g^-1，且首次库仑效率达到99.6%，在1 C下循环500次容量保持率为99%，表现出了优异的电化学性能。

关键词: 合成, 二维片状, 表面活性剂, 二水磷酸铁, 磷酸铁锂, 电化学

Abstract:

Under mild reaction conditions, flaky iron phosphate dihydrate was successfully synthesized using sodium dodecyl benzene sulfonate (SDBS), and mixed with lithium hydroxide and citric acid by ball milling, and prepared by carbothermal reduction method. The effects of SDBS on FePO₄·2H₂O morphology and the electrochemical properties of LiFePO₄/C were studied. The phase, morphology and electrochemical properties of the synthesized samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and charge-discharge test. The LiFePO₄/C plate-like electrode material achieves excellent electrochemical performance under 2.0—4.2 V at 25℃. It delivers a specific discharge capacity of 166.4 mA·h·g^–1 at 0.1 C with initial Coulombic efficiency up to 99.6% and exhibits a capacity retention of 99% after 500 cycles at 1 C.

Key words: synthesis, two-dimensional plate, surfactants, ferric phosphate, lithium iron phosphate, electrochemistry

中图分类号:

TQ 150

高强, 吕洪, 熊凡, 陈飞, 杨则恒, 张卫新. 片状LiFePO₄/C正极材料制备及其电化学性能研究[J]. 化工学报, 2019, 70(4): 1628-1634.

Qiang GAO, Hong LYU, Fan XIONG, Fei CHEN, Zeheng YANG, Weixin ZHANG. Preparation of LiFePO₄/C plate cathode materials and their electrochemical properties[J]. CIESC Journal, 2019, 70(4): 1628-1634.

图/表 9

图1 FP-a和FP-b样品的XRD谱图

Fig.1 XRD patterns of FP-a and FP-b

图2 LFP-a和LFP-b样品的XRD谱图

Fig.2 XRD patterns of LFP-a and LFP-b

图3 FePO4·2H2O样品的扫描电镜图

Fig.3 FESEM images of FePO4·2H2O

图4 LiFePO4/C样品的扫描电镜图

Fig.4 FESEM images of LiFePO4/C

图5 LFP-b样品的透射电镜图和高分辨透射电镜图

Fig.5 TEM and HRTEM images of LFP-b

图6 LiFePO4/C样品在不同倍率下的充放电曲线

Fig.6 Charge-discharge curves of as-prepared LiFePO4/C at different rates

图7 LiFePO4/C样品倍率循环性能图和循环性能图

Fig.7 Rate cyclability and cycle performance of LiFePO4/C

图8 LiFePO4/C样品的循环伏安曲线

Fig.8 Cycling voltammetry (CV) curves of LFP-a and LFP-b

图9 LFP-a和LFP-b样品的交流阻抗曲线

Fig.9 Electrochemical impedance spectroscopy (EIS) of samples LFP-a and LFP-b

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片状LiFePO₄/C正极材料制备及其电化学性能研究

Preparation of LiFePO₄/C plate cathode materials and their electrochemical properties

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