热处理温度对多元醇合成Li2MnSiO4/C电化学性能的影响

doi:10.3724/SP.J.1077.2009.09472

摘要/Abstract

摘要： 采用多元醇法合成Li₂MnSiO₄/C复合材料:将Si(OC₂H₅)₄、LiAc·2H₂O、Mn(Ac)₂·4H₂O在乙二醇中196℃回流16h，沉淀物过滤、干燥以后与蔗糖混合并在500、600和700℃分别加热10h,自然冷却到室温.利用X射线衍射、元素分析、场发射扫描电镜、高分辨透射电镜等手段对合成样品进行表征.Rietveld精修表明，合成样品中存在两种Li₂MnSiO₄相，空间群分别为Pmn21和P121/n1，还有Li₂SiO₃杂相.FESEM观察显示当热处理温度从500℃升高至700℃时，样品的颗粒粒径从5~20nm提高到20~40nm.Li₂MnSiO₄/C复合材料中的碳分布是均匀的.HRTEM分析表明在Li₂MnSiO₄颗粒上包覆有一层无定型的碳薄膜.电化学性能测试表明，在600℃保温10h得到的样品具有最佳的电化学性能，首次放电容量达到132.4mAh/g，10次循环后容量保持率为80%.

关键词: 硅酸锰锂, 正极材料, 多元醇法, 热处理温度, 电化学性能

Abstract: The Li₂MnSiO₄/C composite was synthesized through a polyol process following by heattreatment at intermediate temperatures. The precursors were precipitated from Si(OC₂H₅)₄, LiAc·2H₂O and Mn(Ac)₂·4H₂O in ethylene glycol by refluxing at 196℃ for 16h, the dried powders were milled, pressed and heat-treated at 500℃, 600℃ and 700℃ for 10h. The obtained samples were characterized by X-ray diffraction, automatic elemental analyzer, field emission scanning electron microscope (FESEM), energy dispersive spectroscope (EDS), and high resolution transmission electron microscope (HRTEM). As a result of the Rietveld refinement, two possible Li₂MnSiO₄ forms crystallizing in Pmn21 and P121/n1 space groups, respectively, are considered as the major phases, and Li2SiO3 is identified as the impurity phase. According to the FESEM observation, the mean particle size increases from 5-20nm to 20-40nm as the heattreatment temperature increasing from 500℃ to 700℃. Carbon is homogenously distributed on the prepared Li₂MnSiO₄/C composites. The HRTEM examination confirms that the Li₂MnSiO₄ particles are surrounded by a very thin amorphous carbon layer. The electrochemical experiments reveal that the Li₂MnSiO₄/C composite heat-treated at 600℃ for 10h has the higher electrochemical performance with an initial discharge capacity of 132.4mAh/g and a capacity retention ratio of 80% at the tenth cycle.

Key words: lithium manganese silicate, cathode material, polyol process, electrochemical performance

中图分类号:

TM912

刘文刚,许云华,杨蓉,HOJAMBERDIEV Mirabbos,周志斌. 热处理温度对多元醇合成Li₂MnSiO₄/C电化学性能的影响[J]. 无机材料学报, DOI: 10.3724/SP.J.1077.2009.09472.

LIU Wen-Gang,XU Yun-Hua,YANG Rong,HOJAMBERDIEV Mirabbos,ZHOU Zhi-Bin. Effect of Heattreatment Temperature on the Electrochemical Performances of the Li₂MnSiO₄/C Composite Prepared through Polyol Process[J]. Journal of Inorganic Materials, DOI: 10.3724/SP.J.1077.2009.09472.

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热处理温度对多元醇合成Li₂MnSiO₄/C电化学性能的影响

Effect of Heattreatment Temperature on the Electrochemical Performances of the Li₂MnSiO₄/C Composite Prepared through Polyol Process

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