LiNi0.9Co0.1O2 cathode material is prepared from LiOH center dot H2O and Ni0.9Co0.1(OH)(2) by co-precipitation and subsequent two-stage heat treatment in flowing oxygen based on the results of thermogravimetric. The structural and electrochemical properties of the samples are characterized by means of inductively coupled plasma-atomic emission spectrometer (ICP-AES), X-ray diffraction (XRD), scanning electron microscope (SEM), cyclic voltammogram (CV) and charge-discharge studies. All the samples sintered at different temperatures have a typical layered structure with space group R3-m and good electrochemical performances. The sintering temperature has a remarkable effect on the electrochemical performance of the samples. The sample sintered at 730 degrees C shows the largest initial discharge capacity 191.1 mAh g(-1) (50 mA g(-1), 3.0-4.3 V) and the best cycling performance. The initial discharge capacity rises to above 200 mAh g(-1) with the voltage range 3.0-4.5 V.