Using converting the air in muffle sufficiently, LiNio.7Coo.3O2 lithium-ion battery anode materials were synthesized by solid state reaction in air condition. The relationship between material structure and electrochemicat properties were characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM) and charge-discharge studies. The experiment cells were charged at constant current (C/3) to 4.2 V, after a rest period of 2 min, cells were discharged to 2.7 V at the same constant current (C/3). The specific charge and discharge capacity of the first circle are 181 mAh/g and 157 mAh/g, respectively. And its coulombic efficiency is 86.7%. After the fifteen cycle, the specific discharge capacity gets stably, and the coulombic efficiency of each cycle is over 98%, the specific discharge capacity retains 122 mAh/g in the fortieth cycle.