Calcium zincate as an active material in Zn/Ni secondary battery has been successfully synthesized by solid-phase synthesis method without strong alkali. The chemical composition of Ca(OH)(2)center dot 2Zn(OH)(2)center dot 2H(2)O was confirmed by X-ray powder diffraction pattern and weight loss in thermogravimetric analysis. Well defined monoclinic crystals of calcium zincate synthesized at 348 K was exhibited by scanning electron microscope. The results of cyclic voltammetry of powder microelectrocle and experimental Zn/Ni battery charge-discharge test showed that the material of Ca(OH)(2)center dot 2Zn(OH)(2)center dot 2H(2)O had excellent electrochemical performances: a good cycleability, a high discharging platform of 1.686V and a practical specific capacity of 195.8 mAh g(-1). Nevertheless, this method of preparing calcium zincate is simple and more suitable for mass production. (C) 2008 Elsevier B.V. All rights reserved.