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The comparative study of LiNi0.8Co0.2O2 and LiNi0.75Al0.25O2 was carried out by X-ray diffraction (XRD) and electrochemical methods. The results show that Co and Al doping suppress the phase transition during charge-discharge. The experiments indicate that LiNi0.75Al0.25O2 has the better cycle-ability and over-charge resistance comparing with LiNi0.8Co0.2O2. The interfacial behavior was studied by use of electrochemical impedance spectroscopy (EIS). The results show that LiNi0.75Al0.25O2 has a slightly larger polarization character than LiNi0.8Co0.2O2.