Amorphous nickel hydroxide powders codoped with Ce and Fe were synthesized by the combined chemical precipitation and rapid freezing method. The microstructure and chemical composition of the samples was characterized by XRD,SAED and EDS. The electrochemical performance of the prepared samples was analyzed by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and charge-discharge tests. The results showed that this amorphous nickel hydroxide codoped with Ce and Fe had more structural defects than those of Fe singly doped amorphous nickel hydroxide. These abundant structural defects with Ce and Fe codoped amorphous nickel hydroxide increased the thermal stability, decreased the charge transfer resistance, inhibited oxygen evolution reaction effectively and improved the electrochemical reversibility of the amorphous nickel hydroxide electrode.