ano-scale α-phase nickel hydroxide electrode materials were fabricated by multi-ion substitution. XRD test indicates that the crystal is α-style and TEM shows that the particles are between 20 and 30 nanometers in size with an irregular shape. Optimum technological parameters are obtained through orthogonal test of the substitution quantities of A13+ ions , Zn2+ ions, categories of anions , surfactants and reaction temperature. By using the optimized technological parameters, electrode materials with electrochemical capacity of 316 mA·h/g are prepared.