Amorphous nickel hydroxide powders doped with rare earth La3+ and Al3+ were synthesized by the combined chemical precipitation and rapid freezing method. The microstructure of the samples was characterized by XRD and Raman spectra. The electrochemical performance of the prepared samples was analyzed by electrochemical impedance spectroscopy and charge-discharge tests. The results showed that this amorphous nickel hydroxide codoped with La3+ and Al3+ had more structural defects than those of the undoped amorphous nickel hydroxide and La3+ singly doped amorphous nickel hydroxide. These abundant structural defects with La3+ and Al3+ codoped amorphous nickel hydroxide decreased the electrochemical impedance spectroscopy and improved the electrochemical reversibility of the amorphous nickel hydroxide electrode.