In order to research the effects of pH values on the electrochemical performance of Zn-doped nano-scale Ni(OH)₂, the nano-scale Ni(OH)₂ doped with Zn was prepared by precipitate transformation method at different pH, and characterized by XRD and TEM. The electrochemical performance was investigated by voltammetry (CV) and constant current technology. The measurement results indicate that the material prepared under pH=10 is a kind of α-type nano-scale Ni(OH)₂, and with the increase of pH, the material becomes the mixture of α-Ni(OH)₂ and β-Ni(OH)₂, and the agglomeration of particles becomes obvious. pH exerts a great influence on the electrochemical performance of materials. With the increase of pH, the diffusion coefficient of materials becomes bigger. Compared with the material prepared at pH=10, the material prepared at pH=12 shows better discharge performance, its discharge specific capacity of 02C and 3C were enhanced by 20％ and 27％ respectively.