LiCo1−y M y O2 (M=Ni or Fe) oxides with large specific areas and nanoscale grain sizes were prepared by an improved amorphous citric precursor method (IACP) at low temperature. Their electrocatalytic performances were characterized by the polarization curves of gas diffusion electrodes employing the oxides. The measurements of polarization curves indicate that most of the samples, especially LiCo0.6Ni0.4O2 and LiCo0.8Fe0.2O2, showed excellent bifunctional electrocatalytic activities. The activities of the oxides for oxygen evolution could be improved by acid-delithiation.