Abstract: The precursors of non-stoichiometric spinel Li _1.05 Co _0.05 Ni _0.05 Mn _1.9 O _3.9 F _0.1 were prepared by coprecipitation, supersonic irradiation coprecipitation,the Pechini method and high temperature solid phase reaction separately according to adulteration of anion-cation combination, then the precursors were treated by three-step heat-treatment , i. e. pre-annealing at 650℃, annealing at 780℃ and backfiring at 550℃. The content of manganese and the average chemical valence in spinel were determined by volumetric analysis, and the as-prepared powders were characterized with granularity distribution, X-ray diffraction (XRD), scanning electron microscopy (SEM) and electrochemical performance test. The results showed that the content of manganese and the average chemical valence fitted well with the theoretical value.In contrast with the products prepared by coprecipitation,the Pechini method and high temperature solid phase reaction, the product synthesized by supersonic irradiation coprecipitation had the narrowest granularity distribution,and the smallest volumetric surface area (0.96 m²•g^-1).The intensity value of XRD was the highest, so was its crystallinity, and its lattice constant was 0.821 nm and grain size was 57.78 nm according to the Scherrer equation. The powders prepared by supersonic irradiation coprecipitation had higher capacity and static cycle life by capacity test than that of the three others which was only reduced by 9.3% after 30 cycles.