以TiCl4为原料,通过中和水解法合成嵌锂活性较高的无定形水合TiO2,然后将其与LiOH·H2O在水介质中湿法合成Li4Ti5O12前驱体。研究热处理温度对样品的物相组成、颗粒形貌及电化学性能的影响。运用热重差热分析(TG-DTA)、X线衍射(XRD)、扫描电子显微镜(SEM)和恒流充放电测试等方法表征和测试Li4Ti5O12样品的物理性能和电化学性能。研究结果表明:湿化学法制备的Li4Ti5O12在750℃和800℃下热处理后都具有良好的尖晶石型结构;样品在750℃热处理6 h后,颗粒分散,形貌较为规整,具有最佳的电化学性能;在1.0~2.5V的电压范围,0.1C倍率下首次放电比容量可达175.0 mA·h/g;0.5C倍率下放电容量可达167.5 mA·h/g,经过60次循环后容量为163.0 mA·h/g,容量保持率为97.3%。
Li4Ti5O12 precursor was synthesized by a wet chemical method in aqueous media using amorphous hydrated TiO2, which was prepared by hydrolysis method from TiCl4 aqueous solution. The effects of calcining temperature on the phase composition, morphology and electrochemical property of the products were investigated. The physical and electrochemical performances of Li4TisOl2 were characterized by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscope (SEM) and constant current discharge-charge measurement. The results indicate that the Li4TisO12 products synthesized by the wet chemical method followed by heat treatment at 750 ℃ and 800 ℃ have a good spinel structure. The sample calcined at 750 ℃ for 6 h has a uniform particle size distribution, regular morphology, and shows the best electrochemical performance. The tests show that the as-prepared LigZi5O12 delivers the initial discharge specific capacity of 175.0 mA.h/g at 0.1C current rate in the voltage range of 1.0-2.5 V, and its discharge capacity reduces to 167.5 mA-h/g at 0.5C. The capacity decays to 163.0 mA.h/g after 60 cycles, and remains 97.3% of its initial specific capacity at 0.5C rate.