Calcium zincate as an active material in Zn/Ni secondary battery has been successfully synthesized by microwave method. The sample was characterized by X-ray diffraction (XRD), thermogravimetric analysis, scanning electron microscope (SEM), chargedischarge test (CT) and cyclic voltammetry (CV) analysis. The results show that the chemical composition of sample is Ca(OH)2·2Zn(OH)2·2H2O with regular spherical shapes. The results from CV and CT measurement indicate that the battery has very high discharge plateau of 1.688 V as well as an initial discharge capacity 246.48 mAh.g-1, and the battery capacity does not decay much during 120 cycles, exhibiting good prospect for practical use especially at high discharge rate.