The preparation of LiNi0.8Co0.2O2 was discussed by the multiply sintering method for solid reaction, in which the sintered material was smashed, ground and pelletted between two successive sintering steps. The optimum technological condition was obtained through orthogonal experiments by L9（34） and DTA analysis. The result indicates that the factors of effecting the electrochemical properties of synthesized LiNi0.8Co0.2O2 are molar ratio of Li/Ni/Co, oxygen pressure, homothermal time, the final sintering temperature in turn according to its importance. The oxygen pressure is reviewed independently and the technological condition is further optimized. With the same method, rare earth element Ce was studied as substitute element of Co and the cathode material of LiNi0.95Ce0.05O2 with excellent electrochemical properties was prepared. The electrochemical testing results of LiNi0.8Co0.2O2 and LiNi0.95Ce0.05O2 experimental batteries show that discharge capacities of them reach 165 and 148 mAh·g-1 respectively and the persistence is more than 9 h at 3.7 V.
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