Amorphous nickel hydroxide codoped with Fe 3+ and CO 3 2− was synthesized by micro-emulsion precipitation method combined with rapid freezing technique. The microstructure and composition of the sample were characterized by X-ray diffraction and IR analysis. The electrochemical performance of the sample was analyzed by cyclic voltammetry, electrochemical impedance spectroscopy, and chargedischarge tests. The results showed that the Fe 3+ and CO 3 2− codoping enhances the amorphous feature of the prepared nickel hydroxide. Moreover, the Fe 3+ and CO 3 2− codoping could increase the specific capacity and improve the electrochemical reversibility of the amorphous nickel hydroxide electrode.