介孔磷酸钛正极材料的合成、结构和电化学性能研究
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摘要
聚阴离子型正极材料因具有稳定的框架结构和易于调变的电位平台等优点,因而具有良好的电化学性能,有可能被推动成为第三代锂离子电池正极材料。但是,由于这类材料电导率低,材料的大电流充放电性能差,限制了它在实际中的应用。为了改善这类材料的大电流充放电性能,对材料进行了包碳、掺杂等处理,来提高其电子电导率。本论文也是基于要改善这类材料的离子传输性能,采用一种不同于传统的新方法,即把介孔结构引入到材料中,通过改善该材料的微观结构来克服其电导率低的缺点,最终实现其大电流放电性能的目的。
我们采用溶胶凝胶模板结合煅烧的方法合成出了具有介孔结构的磷酸钛正极材料。材料的制备是一个复杂的过程,受到诸多因素的影响,本实验组曾对材料制备过程中的前驱体制备阶段的一些因素(诸如:磷源、温度、湿度、溶剂的蒸发速度及溶胶放置陈化的时间等)进行了研究,研究发现,溶剂蒸发过快或溶胶陈化时间太短都不利于介孔结构的形成,尤其是长程有序介孔结构的形成;三氯化磷是一种较好的磷源;温度或湿度太高不利于介孔结构的形成。
为了制备长程有序介孔结构,本论文对上述方法进行了优化,并成功制得一系列介孔磷酸钛材料,同时并对模板剂、溶剂,及前驱体煅烧处理阶段中除模板剂时间、煅烧温度、煅烧时间和煅烧方式等因素对介孔结构的影响进行了研究,结果发现,用疏水基链长较长的P123模板剂合成得到的介孔材料具有较好的长程有序性,并且比表面积和孔容都较大,介孔结构呈平面六方排列;而用亲水基链长较长的F108模板剂合成得到的介孔材料孔径分布比较集中,孔道的孔壁变厚,介孔结构呈立方相排列;用强亲水性的乙醇做溶剂时,对形成长程有序的介孔结构有利;长时间除模板剂处理或长时间的煅烧都会使介孔材料的比表面积和孔容变小;煅烧温度是煅烧处理阶段中的主要影响因素,适当的煅烧处理有利于介孔结构的优化,但过高的煅烧温度(如:800℃)则使材料介孔结构坍塌,而且材料完全晶体化;相比一步焙烧法而言,两步焙烧法煅烧得到的介孔材料具有较大的比表面积和孔容。
在对具有不同介孔结构的磷酸钛材料电化学性能的研究中,实验结果显示,与没有孔结构的磷酸钛材料相比,具有介孔结构的磷酸钛材料具有较好的循环性能,尤其是大电流下的充放电性能。此外,与长程有序性差的或孔径小的介孔磷酸钛材料相比,长程有序性好的或孔径较大的介孔磷酸钛材料具有相对较好的大电流循环性能和大电流充放电性能。
Poly-anion compounds have advantages of steady framework and easily adjustable potential plat, and thus give good cyclic performance. Because of this, they may become a third era lithium ion battery cathode materials. However, the low electrical conductivity is bad for the poly-anion compounds electrochemical performace at the high current density. In order to improve their performance, carbon coating and metal doping are two conventional methods. We have investigated some materials with mesoporous structure for improving their ionic transport behaviour. Mesoporous structure has distinct effects on the electrode materials' performance, and then overcome the drawback of the low electrical conductivity of the materials. The sol-gel template combinded with the calcination method was used in our study. During this preparation process, there are many factors, such as a suitable phosphorus source, temperature, humidity, solvent vaporizing speed and aging time of the sol, have some influence on mesoporous structure synthesis. It was found that both solvent-vaporing speed and too short sol-aging time wouldn't build ordered mesoporous structure, and PCl_3 is a better phosphorus source, and it was unadvisable to use too high temperature and too high humidity.
In order to get ordered mesostructure, a modified sol-gel template method was established to synthesize mesoporous materials. We successfully synthesized a series of different mesoporous titanium phosphate materials, and at the same time, other effects were also considered, such as template, solvent, template removing time, calcination temperature and calcination method during the synthesis. In our study, it is confirmed that P123 with larger hydropobic PO units were used as template resulting in a highly ordered hexagonal mesoporous titanium phosphate materials, and these materials were in possession of a larger surface area and a larger pore volume. And on the other hand, F108 with a larger hydrophilic EO chain is good for synthesizing titanium phosphate with a narrower pore size and a cubic mesostructure. Ethanol as solvent can get long-range ordering of the mesopore. The longer time was spent on removing template or calcination, and the smaller surface area and pore volume of mesoporous titanium phosphate materials were made. Compared with one step calcination, two steps calcination made mesoporous titanium phospahte with a larger surface area and pore volume. In addition, it was proved that calcination temperature is a key factor during the calcination process, and calcination can optimize titanium phosphate mesostructure, and however, too high calcination temperature, for example 800℃, results in collapse of materials mesostructure, and at the same time amorphous titanium phosphate slowly changed into cystalline titanium phosphate.
In our study on titanium phosphate electrochemical performance, it was showed that mesoporous titanium phosphate, compared with no porous titanium phospahte, gave a better performance especially at the high current density. Mesoporous titanium phosphate, which had either highly ordered mesostructure or larger pore size, can deliver higher capacity especially at the hugh current density.
我们采用溶胶凝胶模板结合煅烧的方法合成出了具有介孔结构的磷酸钛正极材料。材料的制备是一个复杂的过程,受到诸多因素的影响,本实验组曾对材料制备过程中的前驱体制备阶段的一些因素(诸如:磷源、温度、湿度、溶剂的蒸发速度及溶胶放置陈化的时间等)进行了研究,研究发现,溶剂蒸发过快或溶胶陈化时间太短都不利于介孔结构的形成,尤其是长程有序介孔结构的形成;三氯化磷是一种较好的磷源;温度或湿度太高不利于介孔结构的形成。
为了制备长程有序介孔结构,本论文对上述方法进行了优化,并成功制得一系列介孔磷酸钛材料,同时并对模板剂、溶剂,及前驱体煅烧处理阶段中除模板剂时间、煅烧温度、煅烧时间和煅烧方式等因素对介孔结构的影响进行了研究,结果发现,用疏水基链长较长的P123模板剂合成得到的介孔材料具有较好的长程有序性,并且比表面积和孔容都较大,介孔结构呈平面六方排列;而用亲水基链长较长的F108模板剂合成得到的介孔材料孔径分布比较集中,孔道的孔壁变厚,介孔结构呈立方相排列;用强亲水性的乙醇做溶剂时,对形成长程有序的介孔结构有利;长时间除模板剂处理或长时间的煅烧都会使介孔材料的比表面积和孔容变小;煅烧温度是煅烧处理阶段中的主要影响因素,适当的煅烧处理有利于介孔结构的优化,但过高的煅烧温度(如:800℃)则使材料介孔结构坍塌,而且材料完全晶体化;相比一步焙烧法而言,两步焙烧法煅烧得到的介孔材料具有较大的比表面积和孔容。
在对具有不同介孔结构的磷酸钛材料电化学性能的研究中,实验结果显示,与没有孔结构的磷酸钛材料相比,具有介孔结构的磷酸钛材料具有较好的循环性能,尤其是大电流下的充放电性能。此外,与长程有序性差的或孔径小的介孔磷酸钛材料相比,长程有序性好的或孔径较大的介孔磷酸钛材料具有相对较好的大电流循环性能和大电流充放电性能。
Poly-anion compounds have advantages of steady framework and easily adjustable potential plat, and thus give good cyclic performance. Because of this, they may become a third era lithium ion battery cathode materials. However, the low electrical conductivity is bad for the poly-anion compounds electrochemical performace at the high current density. In order to improve their performance, carbon coating and metal doping are two conventional methods. We have investigated some materials with mesoporous structure for improving their ionic transport behaviour. Mesoporous structure has distinct effects on the electrode materials' performance, and then overcome the drawback of the low electrical conductivity of the materials. The sol-gel template combinded with the calcination method was used in our study. During this preparation process, there are many factors, such as a suitable phosphorus source, temperature, humidity, solvent vaporizing speed and aging time of the sol, have some influence on mesoporous structure synthesis. It was found that both solvent-vaporing speed and too short sol-aging time wouldn't build ordered mesoporous structure, and PCl_3 is a better phosphorus source, and it was unadvisable to use too high temperature and too high humidity.
In order to get ordered mesostructure, a modified sol-gel template method was established to synthesize mesoporous materials. We successfully synthesized a series of different mesoporous titanium phosphate materials, and at the same time, other effects were also considered, such as template, solvent, template removing time, calcination temperature and calcination method during the synthesis. In our study, it is confirmed that P123 with larger hydropobic PO units were used as template resulting in a highly ordered hexagonal mesoporous titanium phosphate materials, and these materials were in possession of a larger surface area and a larger pore volume. And on the other hand, F108 with a larger hydrophilic EO chain is good for synthesizing titanium phosphate with a narrower pore size and a cubic mesostructure. Ethanol as solvent can get long-range ordering of the mesopore. The longer time was spent on removing template or calcination, and the smaller surface area and pore volume of mesoporous titanium phosphate materials were made. Compared with one step calcination, two steps calcination made mesoporous titanium phospahte with a larger surface area and pore volume. In addition, it was proved that calcination temperature is a key factor during the calcination process, and calcination can optimize titanium phosphate mesostructure, and however, too high calcination temperature, for example 800℃, results in collapse of materials mesostructure, and at the same time amorphous titanium phosphate slowly changed into cystalline titanium phosphate.
In our study on titanium phosphate electrochemical performance, it was showed that mesoporous titanium phosphate, compared with no porous titanium phospahte, gave a better performance especially at the high current density. Mesoporous titanium phosphate, which had either highly ordered mesostructure or larger pore size, can deliver higher capacity especially at the hugh current density.
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