The precursors of Li4Ti5O12 were prepared from tetrabutyl titanate and lithium acetate by sol-gel process. The Li4Ti5O12 samples were synthesized by calcining the gel precursors at 400～900℃ in air for 6～20h. Its reaction mechanism was investigated by infrared speetroseopy(IR), thermogravimetry(TG) and X-ray diffraetion(XRD). The effects of sinter-temperature, calcination-time and thermal-treatment for the products were discussed. The samples were characterized by X-ray diffraetion(XRD), scanning electron mieroseopy(SEM). The results showed that the single-phase products were obtained by calcining the gel precursors at 800℃ in air for 20h, the sintertemperature was lower than that of solid-state method, the particles were narrowly distributed, well crystallized with a size range from 0.3μm to 0.5μm.