溶胶凝胶法结合电喷技术制备锂离子电池正极材料
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摘要
本论文主要是设计具有不同电场分布的实验装置,来进行对比软件仿真。通过电场模拟结果,结合实验结论总结得出电场分布对静电纺丝的影响。同时利用溶胶-凝胶结合电喷技术合成不同形貌的纳米结构纤维并对其进行了详细的表征,特别是作为锂离子电池的正极材料,通过对纤维电性质的研究,以提高纤维作为锂离子电池正极材料的电化学性能。
1.绪论部分
介绍了制备纤维的电喷技术,包括其发展历史、基本原理和基本过程,重点介绍有关电喷技术的理论研究,为电喷技术的应用提供理论指导。接下来介绍了电喷纳米纤维的应用,电喷技术的发展为纳米纤维的应用开拓了广阔的空间。第二部分内容介绍了溶胶-凝胶化学的发展以及这种方法的特点和基本原理以及溶胶-凝胶过程中每一步的影响因素。最后介绍了溶胶-凝胶结合电喷技术在制备纳米纤维方面的应用和发展。
2.静电纺丝系统的静电场仿真
通过电场模拟的方法探究电场分布对静电纺丝的影响,设计两种具有不同电场分布的静电纺丝实验装置,一种是常规针头形式,一种是加入辅助板的针头形式。用有限元(FEM)研究了多喷头系统喷丝管不同间距对喷丝口处最大电场强度的影响,并与单喷头系统进行了比较。研究表明,由于其它喷丝管的引入,多喷头系统喷丝口处的局部电场明显减弱；在一定范围内,随着喷丝管间距的增大,电场强度并没有明显的变化趋势。实验结果显示,相同条件下多喷头系统的纺丝效果优于单喷头系统；多喷头系统喷丝管间距与纺出的纤维状态有一定的联系。
3.Li1+xV3O8多级结构的合成、表征及电化学性质的研究
运用电喷技术结合烧结合成由纳米棒生长在Li1+xV3O8电喷纤维上构成的多级结构。所得产物通过场发射扫描(FE-SEM),透射电镜(TEM),XRD以及拉曼光谱等进行了表征。通过对多级结构的形成机制进行调查,发现多级结构的形貌主要由电喷纤维的尺寸以及烧结条件所决定。Li1+xV3O8多级结构的电化学性通过循环伏安以及充放电实验进行调查,结果显示Li1+xV3O8多级结构具有较高的放电容量,材料也同时表现出极好的循环稳定性。
4.金属离子掺杂LiFePO4纳米纤维的合成及电化学性质的表征
用电喷技术结合溶胶-凝胶化学制备镁、硼掺杂的LiFePO4(?)内米结构纤维,并对其进行了详细的表征,Mg的掺杂有效提高了材料的导电性,从而提高了其充放电容量,而B掺杂有效改善了纤维的微结构,提高了纤维在电化学循环过程中微结构的稳定性,从而有利于电化学循环稳定性的提高。镁、硼掺杂的LiFePO4(?)内米结构纤维将会有效改善锂离子电池电极材料的性能,是一种极有发展前景的正极材料。
5.溶胶-凝胶法结合共轴电喷制备BaFe12O19/Fe203中空复合纤维
通过溶胶-凝胶结合共轴电喷制备BaFe12O19/Fe203(?)中空复合纤维。在实验中有机添加剂被用来调控溶胶的性质。在接下来的烧结过程中,溶胶的性质对电喷后干凝胶纤维的烧结行为有重要的影响,这导致了具有不同形貌的BaFe12o19/Fe203复合纤维的形成,特别是中空复合纤维的形成。同时烧结过程中烧结速率对于BaFe12O19/Fe203纤维的形貌也有一定的影响。
6.三碘苯三酸金属有机配合物单晶的合成研究
在第六章中,利用新颖的配体三碘苯三酸与镧系金属离子Sm自组装反应制备了一个金属-有机化合物,对其进行了结构解析,并研究了热稳定性和荧光性能,发现该化合物具有较强的热稳定性,并具有一定的荧光性能。
Experimental devices with different electric field distribution were designed for software simulation. The effect of electric field distribution on the electrospinning was investigated by the electric field simulation combined with the experimental results. The nanostructured fibers with different morphologies were prepared by the electrospingning combined with the sol-gel method and characterized by a variety of means. The fibers were used as a kind of new cathode materials for micro-batteries and their electrochemical properties were detailedly investigated in order to increase electrochemical performance. The contents include the preparation of the fibers and the control of fiber morphology, the investigation of electrochemical performance as the cathode materials for lithium ion batteries.
In the chapter one of this thesis, the electrospinning was introduced briefly. The contents include historical development, basic principles and processes. It focuses on the theory of the electrospinning, which provides theoretical guidance for the application of the electrospinning technology. In the below content, the application of the fibers was presented and the development of the electrospinning technology opens up a broad space for the applications of the nanofibers. In the sencond, the sol-gel process was introduced briefly. The contents include the phylogeny, character and principle of the sol-gel process. A great deal of attention had been paid for the influence of the processing parameters on every step. At last, the application and development of sol-gel combined with the electrospinning in the preparation of nanofibers were introduced.
We design multi-nozzle electrospinning equipments which have different electric field distribution, one is conventional needle equipment and another is auxiliary-plate needle equipment. The impact of the spacing of multi-nozzle on the maximum electric field strength at the tip of the nozzles in multi-nozzle arrangement was investigated via finite element method (FEM), and the results were compared with single-nozzle system. It can be seen that the maximum electric field of multi-nozzle arrangement has been significantly weakened due to the influence of another needle in the arrangement, and the field varied very little as a function of needle spacing for the range used in this study. Experimental results showed that the multi-nozzle electrospinning head performed much better than single-nozzle system, and the spacing of multi-nozzle had some relationship with the diameter and discrete distribution of the spun fiber.
In the third chapter, Hierarchical structures of Li1+xV3O8nanorods growing on electrospun fibers were successfully synthesized by electrospinning and calcinations. The products were characterized by field-emission scanning election microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectra. The formation mechanism of the hierarchical structures was investigated, showing that the morphology of the hierarchical structures was mainly determined by the calcined conditions. Electrochemical properties of the Li1+xV3O8hierarchical structures were investigated by cyclic voltammetry and charge-discharge experiments, and the results demonstrated that the Li1+xV3O8hierarchical structures exhibited a high discharge capacity and excellent cycling stability.
The Mg, B-doped LiFePO4nanostructured fibers were prepared by the electrospinning with the sol-gel method. The doping of Mg effectively increased the conductivity of the material, thereby improving its charge-discharge capacities. On the other hand, the doping of B effectively improved the micro-structure of the fibers, thus contributing to the improved stability of the electrochemical cycle. Mg, B-dopedLiFePO4nanostructure fiber will effectively improve the performance of the lithium-ion battery electrode materials, is a very promising cathode material.
Hollow BaFe12O19/Fe2O3composite fibers were prepared by co-electrospinning related sol-gel method. The organic additives were added into the BaFe12O19sols to adjust the properties of the sols. During the calcined process, the properties of sols obviously affected the desiccation and sinter of xerogel fibers, which resulted in hollow BaFe12O19/Fe2O3composite fibers. The heating rate had also an important influence on the morphologies of BaFe12O19/Fe2O3fibers, the decrease of surface tension of the sol and appropriate heating rate were favorable for the hollow structure.
In the chapter6, a metal-organic compounds were prepared through a self assembled reaction between a novel ligand (three iodine benzene acid) and the lanthanide metal ion Sm. We analysized their structures, and found the compounds have stronger thermal stability, and better fluorescence properties.
1.绪论部分
介绍了制备纤维的电喷技术,包括其发展历史、基本原理和基本过程,重点介绍有关电喷技术的理论研究,为电喷技术的应用提供理论指导。接下来介绍了电喷纳米纤维的应用,电喷技术的发展为纳米纤维的应用开拓了广阔的空间。第二部分内容介绍了溶胶-凝胶化学的发展以及这种方法的特点和基本原理以及溶胶-凝胶过程中每一步的影响因素。最后介绍了溶胶-凝胶结合电喷技术在制备纳米纤维方面的应用和发展。
2.静电纺丝系统的静电场仿真
通过电场模拟的方法探究电场分布对静电纺丝的影响,设计两种具有不同电场分布的静电纺丝实验装置,一种是常规针头形式,一种是加入辅助板的针头形式。用有限元(FEM)研究了多喷头系统喷丝管不同间距对喷丝口处最大电场强度的影响,并与单喷头系统进行了比较。研究表明,由于其它喷丝管的引入,多喷头系统喷丝口处的局部电场明显减弱；在一定范围内,随着喷丝管间距的增大,电场强度并没有明显的变化趋势。实验结果显示,相同条件下多喷头系统的纺丝效果优于单喷头系统；多喷头系统喷丝管间距与纺出的纤维状态有一定的联系。
3.Li1+xV3O8多级结构的合成、表征及电化学性质的研究
运用电喷技术结合烧结合成由纳米棒生长在Li1+xV3O8电喷纤维上构成的多级结构。所得产物通过场发射扫描(FE-SEM),透射电镜(TEM),XRD以及拉曼光谱等进行了表征。通过对多级结构的形成机制进行调查,发现多级结构的形貌主要由电喷纤维的尺寸以及烧结条件所决定。Li1+xV3O8多级结构的电化学性通过循环伏安以及充放电实验进行调查,结果显示Li1+xV3O8多级结构具有较高的放电容量,材料也同时表现出极好的循环稳定性。
4.金属离子掺杂LiFePO4纳米纤维的合成及电化学性质的表征
用电喷技术结合溶胶-凝胶化学制备镁、硼掺杂的LiFePO4(?)内米结构纤维,并对其进行了详细的表征,Mg的掺杂有效提高了材料的导电性,从而提高了其充放电容量,而B掺杂有效改善了纤维的微结构,提高了纤维在电化学循环过程中微结构的稳定性,从而有利于电化学循环稳定性的提高。镁、硼掺杂的LiFePO4(?)内米结构纤维将会有效改善锂离子电池电极材料的性能,是一种极有发展前景的正极材料。
5.溶胶-凝胶法结合共轴电喷制备BaFe12O19/Fe203中空复合纤维
通过溶胶-凝胶结合共轴电喷制备BaFe12O19/Fe203(?)中空复合纤维。在实验中有机添加剂被用来调控溶胶的性质。在接下来的烧结过程中,溶胶的性质对电喷后干凝胶纤维的烧结行为有重要的影响,这导致了具有不同形貌的BaFe12o19/Fe203复合纤维的形成,特别是中空复合纤维的形成。同时烧结过程中烧结速率对于BaFe12O19/Fe203纤维的形貌也有一定的影响。
6.三碘苯三酸金属有机配合物单晶的合成研究
在第六章中,利用新颖的配体三碘苯三酸与镧系金属离子Sm自组装反应制备了一个金属-有机化合物,对其进行了结构解析,并研究了热稳定性和荧光性能,发现该化合物具有较强的热稳定性,并具有一定的荧光性能。
Experimental devices with different electric field distribution were designed for software simulation. The effect of electric field distribution on the electrospinning was investigated by the electric field simulation combined with the experimental results. The nanostructured fibers with different morphologies were prepared by the electrospingning combined with the sol-gel method and characterized by a variety of means. The fibers were used as a kind of new cathode materials for micro-batteries and their electrochemical properties were detailedly investigated in order to increase electrochemical performance. The contents include the preparation of the fibers and the control of fiber morphology, the investigation of electrochemical performance as the cathode materials for lithium ion batteries.
In the chapter one of this thesis, the electrospinning was introduced briefly. The contents include historical development, basic principles and processes. It focuses on the theory of the electrospinning, which provides theoretical guidance for the application of the electrospinning technology. In the below content, the application of the fibers was presented and the development of the electrospinning technology opens up a broad space for the applications of the nanofibers. In the sencond, the sol-gel process was introduced briefly. The contents include the phylogeny, character and principle of the sol-gel process. A great deal of attention had been paid for the influence of the processing parameters on every step. At last, the application and development of sol-gel combined with the electrospinning in the preparation of nanofibers were introduced.
We design multi-nozzle electrospinning equipments which have different electric field distribution, one is conventional needle equipment and another is auxiliary-plate needle equipment. The impact of the spacing of multi-nozzle on the maximum electric field strength at the tip of the nozzles in multi-nozzle arrangement was investigated via finite element method (FEM), and the results were compared with single-nozzle system. It can be seen that the maximum electric field of multi-nozzle arrangement has been significantly weakened due to the influence of another needle in the arrangement, and the field varied very little as a function of needle spacing for the range used in this study. Experimental results showed that the multi-nozzle electrospinning head performed much better than single-nozzle system, and the spacing of multi-nozzle had some relationship with the diameter and discrete distribution of the spun fiber.
In the third chapter, Hierarchical structures of Li1+xV3O8nanorods growing on electrospun fibers were successfully synthesized by electrospinning and calcinations. The products were characterized by field-emission scanning election microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectra. The formation mechanism of the hierarchical structures was investigated, showing that the morphology of the hierarchical structures was mainly determined by the calcined conditions. Electrochemical properties of the Li1+xV3O8hierarchical structures were investigated by cyclic voltammetry and charge-discharge experiments, and the results demonstrated that the Li1+xV3O8hierarchical structures exhibited a high discharge capacity and excellent cycling stability.
The Mg, B-doped LiFePO4nanostructured fibers were prepared by the electrospinning with the sol-gel method. The doping of Mg effectively increased the conductivity of the material, thereby improving its charge-discharge capacities. On the other hand, the doping of B effectively improved the micro-structure of the fibers, thus contributing to the improved stability of the electrochemical cycle. Mg, B-dopedLiFePO4nanostructure fiber will effectively improve the performance of the lithium-ion battery electrode materials, is a very promising cathode material.
Hollow BaFe12O19/Fe2O3composite fibers were prepared by co-electrospinning related sol-gel method. The organic additives were added into the BaFe12O19sols to adjust the properties of the sols. During the calcined process, the properties of sols obviously affected the desiccation and sinter of xerogel fibers, which resulted in hollow BaFe12O19/Fe2O3composite fibers. The heating rate had also an important influence on the morphologies of BaFe12O19/Fe2O3fibers, the decrease of surface tension of the sol and appropriate heating rate were favorable for the hollow structure.
In the chapter6, a metal-organic compounds were prepared through a self assembled reaction between a novel ligand (three iodine benzene acid) and the lanthanide metal ion Sm. We analysized their structures, and found the compounds have stronger thermal stability, and better fluorescence properties.
引文
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