Preparation of Li4Ti5O12 submicrospheres and their application as anode materials of rechargeable lithium-ion batteries

We report on the preparation of spinel Li4Ti5O12 submicrospheres and their application as anode materials of rechargeable lithium-ion batteries. The spinel Li4Ti5O12 submicrospheres are synthesized with three steps of the hydrolysis of TiCl4 to form rutile TiO2, the hydrothermal treatment of rutile TiO2 with LiOH to prepare an intermediate phase of LiTi2O4+δ, and the calcinations of LiTi2O4+δ to obtain spinel Li4Ti5O12. The as-prepared products are investigated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The diameters of Li4Ti5O12 submicrospheres with novel hierarchical microstructures are about 200–300 nm with the assembly of 20–30 nm nanoparticles. The electrochemical properties of Li4Ti5O12 submicrospheres are measured by galvanostatical discharge/charge test and cyclic voltammetry (CV). The as-prepared Li4Ti5O12 display excellent discharge/charge rate and cycling capability. A high discharge capacity of 174.3 mAh/g is obtained in the first discharge at 1 C rate. Meanwhile, there is only tiny capacity fading with nearly 100% columbic efficiency in the sequential 5–50 cycles. Moreover, lithium-ion diffusion coefficient in Li4Ti5O12 is calculated to be 1.03 × 10-7 cm2/s. The present results indicate that the as-prepared Li4Ti5O12 submicrospheres are promising anode candidates of rechargeable Li-ion batteries for high-power applications.