高性能锂离子电池电极材料及薄膜电极的研究
摘要
在当今信息、流通便捷的社会里，可充电锂离子电池是手提式娱乐、计算、通讯工具的重要电源。小型化和动力电池是锂离子电池的两个重要研究方向。本论文主要是研究薄膜电极，为制备微型电池开展基础研究工作，并研究开发适合做动力电池的LiMn_2O_4正极材料和石墨负极材料。
论文第一章一方面介绍了锂离子电池的工作原理和各种电极材料，另一方面介绍了静电喷雾沉积法制备薄膜技术(ESD)，解释了ESD的工作原理并且展示了这项技术在多个研究领域中的应用。论文第二章简要介绍了实验手段，包括钮扣式锂离子电池的制作工艺和本论文涉及到的主要研究手段。
实现电池小型化要求有薄膜电极，ESD技术已被证明是一项很好的制膜技术，它设备简单，非真空沉积，膜的形貌易于控制。本研究中它被用来制备锂离子电池正极和负极薄膜。论文第三章的研究主要是关于LiCoPO_4正极膜的制备和表征。LiCoPO_4由于其电压高的特点(4.8V)，代表了新一代正极材料；但其缺点是锂离子在其内部的扩散缓慢。它的可利用容量很低，循环性很差，尤其在使用常规的LiPF_6(EC-DEC)电解液体系条件下。当原始组成中存在着过量的锂时(Li_(1+x)CoPO_4，x=0～1)，本论文研究发现热处理后可以得到LiCoPO_4-Li_3PO_4-Co_3O_4三元复合成分，其中Li_3PO_4和Co_3O_4被均匀地分布到LiCoPO_4基质内。我们得到了明显的在4.8V和4.9V的充放电平台，较高的容量密度和良好的循环性能。由于电池的双平台特征总是在低电阻时出现，且伴随着较高的容量，因此双平台特征的出现被推断为受锂离子扩散动力学控制的。Co_3O_4的存在可以提高电极的电子导电性从而增加容量，Li_3PO_4可以起到保护层作用，阻挡电解液(LiPF_6(EC-DEC，1：1 v／v))在活性物质表面的反应，从而提高电池的循环性能。通过在LiCoPO_4电极里混入乙炔黑导电剂或在电极表面覆盖一层导电剂均可不同程度的提高电池的循环性能。
论文第四章研究了海绵状多孔膜的一些特性。海绵状多孔膜是ESD技术可以制备的一项独特的形貌，作者调查了沉积参数对多孔结构的影响，包括：衬底温度、前驱液输送速率、电场强度和沉积时间。除了常用的卡比醇溶剂体系，乙二醇和丙二醇液在合适的衬底温度下也可以作为溶剂用来制备多孔膜。增加前驱液输送速率
Rechargeable Li-ion cells are key components of the portable entertainment, computing and telecommunication equipment required by today's information-rich and mobile society. Miniaturization and development towards large power sources are two important directions for the lithium ion battery research. In this thesis, the author mainly conducted the research on thin-film electrodes fabricated by Electrostatic Spray Deposition (ESD) technique, which can be used in fabricating microbatteries. Besides, electrodes materials LiMn_2O_4 and graphite was improved in their electrochemical performance to fit for the use in high power sources.
In Chapter 1 the working principle of lithium ion battery and various electrode materials were introduced. Also, a film preparation technique i.e. Electrostatic Spray Deposition was introduced. The author explained the working principle of ESD and showed the applications of this technique. In Chapter 2. the process of coin-type cells assembly and some related experimental methods used in this thesis were introduced.
The realization of thin-film lithium-ion batteries requires the successful fabrication of thin-film components of cathode, anode and electrolyte. Electrostatic spray deposition (ESD) technique has proved to be a versatile film formation method, owing to its simplicity, non-vacuum deposition condition, and easy film-morphology control. In this thesis study, it was used to prepare cathode and anode films for lithium ion batteries. In Chapter 3 we prepared LiCoPO_4 electrode films. LiCoPO_4 represents a new class of high-energy cathode material for its higher working voltage at 4.8V, but the lithium-ion diffusion is very slow in it. Its achievable capacity is comparatively low and drops very rapidly after a limited number of cycles, especially in the commonly used LiPF_6 (EC-DEC) electrolyte systems. With an excess of lithium in the initial nominal compositions Li_(1+x)CoPO_4 (x=0～1), a LiCoPO_4-Li_3PO_4-Co_3O_4 ternary composite can be obtained after heat treatment. Li_3PO_4 and Co_3O_4 were introduced and homogeneously distributed in the LiCoPO_4 matrix. We have obtained distinct two-step feature of the voltage plateaus at 4.8V and 4.9V, high specific
论文第一章一方面介绍了锂离子电池的工作原理和各种电极材料，另一方面介绍了静电喷雾沉积法制备薄膜技术(ESD)，解释了ESD的工作原理并且展示了这项技术在多个研究领域中的应用。论文第二章简要介绍了实验手段，包括钮扣式锂离子电池的制作工艺和本论文涉及到的主要研究手段。
实现电池小型化要求有薄膜电极，ESD技术已被证明是一项很好的制膜技术，它设备简单，非真空沉积，膜的形貌易于控制。本研究中它被用来制备锂离子电池正极和负极薄膜。论文第三章的研究主要是关于LiCoPO_4正极膜的制备和表征。LiCoPO_4由于其电压高的特点(4.8V)，代表了新一代正极材料；但其缺点是锂离子在其内部的扩散缓慢。它的可利用容量很低，循环性很差，尤其在使用常规的LiPF_6(EC-DEC)电解液体系条件下。当原始组成中存在着过量的锂时(Li_(1+x)CoPO_4，x=0～1)，本论文研究发现热处理后可以得到LiCoPO_4-Li_3PO_4-Co_3O_4三元复合成分，其中Li_3PO_4和Co_3O_4被均匀地分布到LiCoPO_4基质内。我们得到了明显的在4.8V和4.9V的充放电平台，较高的容量密度和良好的循环性能。由于电池的双平台特征总是在低电阻时出现，且伴随着较高的容量，因此双平台特征的出现被推断为受锂离子扩散动力学控制的。Co_3O_4的存在可以提高电极的电子导电性从而增加容量，Li_3PO_4可以起到保护层作用，阻挡电解液(LiPF_6(EC-DEC，1：1 v／v))在活性物质表面的反应，从而提高电池的循环性能。通过在LiCoPO_4电极里混入乙炔黑导电剂或在电极表面覆盖一层导电剂均可不同程度的提高电池的循环性能。
论文第四章研究了海绵状多孔膜的一些特性。海绵状多孔膜是ESD技术可以制备的一项独特的形貌，作者调查了沉积参数对多孔结构的影响，包括：衬底温度、前驱液输送速率、电场强度和沉积时间。除了常用的卡比醇溶剂体系，乙二醇和丙二醇液在合适的衬底温度下也可以作为溶剂用来制备多孔膜。增加前驱液输送速率
Rechargeable Li-ion cells are key components of the portable entertainment, computing and telecommunication equipment required by today's information-rich and mobile society. Miniaturization and development towards large power sources are two important directions for the lithium ion battery research. In this thesis, the author mainly conducted the research on thin-film electrodes fabricated by Electrostatic Spray Deposition (ESD) technique, which can be used in fabricating microbatteries. Besides, electrodes materials LiMn_2O_4 and graphite was improved in their electrochemical performance to fit for the use in high power sources.
In Chapter 1 the working principle of lithium ion battery and various electrode materials were introduced. Also, a film preparation technique i.e. Electrostatic Spray Deposition was introduced. The author explained the working principle of ESD and showed the applications of this technique. In Chapter 2. the process of coin-type cells assembly and some related experimental methods used in this thesis were introduced.
The realization of thin-film lithium-ion batteries requires the successful fabrication of thin-film components of cathode, anode and electrolyte. Electrostatic spray deposition (ESD) technique has proved to be a versatile film formation method, owing to its simplicity, non-vacuum deposition condition, and easy film-morphology control. In this thesis study, it was used to prepare cathode and anode films for lithium ion batteries. In Chapter 3 we prepared LiCoPO_4 electrode films. LiCoPO_4 represents a new class of high-energy cathode material for its higher working voltage at 4.8V, but the lithium-ion diffusion is very slow in it. Its achievable capacity is comparatively low and drops very rapidly after a limited number of cycles, especially in the commonly used LiPF_6 (EC-DEC) electrolyte systems. With an excess of lithium in the initial nominal compositions Li_(1+x)CoPO_4 (x=0～1), a LiCoPO_4-Li_3PO_4-Co_3O_4 ternary composite can be obtained after heat treatment. Li_3PO_4 and Co_3O_4 were introduced and homogeneously distributed in the LiCoPO_4 matrix. We have obtained distinct two-step feature of the voltage plateaus at 4.8V and 4.9V, high specific
引文
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