Nanophase LiCoO 2 was synthesized by solid state reaction with low heating temperature, i.e. the reactants Co(Ac) 2·4H 2O and LiOH·H 2O in the appropriate molar ratio(1∶1) were mixed and ground in agate mortar, then calcined. The samples obtained were characterized by XRD and IR methods. The phenomena during synthesizing are discussed by TG/TDA analysis, and the optimum temperature of heating was chosen. The BET and ICP results suggest that the sample has a large specific surface(54.29 m 2/g), a low quantity of impurity, thus it may be a good battery material. The nanophase LiCoO 2 samples produced have good cyclic performance and a higher working voltage plateau(3.9 V). Nanophase LiCoO 2 was synthesized by solid state reaction with low heating temperature, ie the reactants Co (Ac) 2 · 4H 2O and LiOH · H 2O in the appropriate molar ratio (1: 1) were mixed and ground in agate mortar, then calcined The samples were obtained by XRD and IR methods. The phenomena during synthesisizing discussed by TG / TDA analysis, and the optimum temperature of heating was chosen. The BET and ICP results suggest that the sample has a large specific surface (54.29 m 2 / g), a low quantity of impurity, thus it may be a good battery material. The nanophase LiCoO 2 samples have good cyclic performance and a higher working voltage plateau (3.9 V).