In this paper, ZnCo 2 O 4 was deposited on nickel substrate by electrophoretic deposition (EPD) method as electrocatalyst for the oxygen evolution reaction. The effect of electrophoresis variables including the deposition time, the applied voltages was discussed. XRD, SEM, and electrochemical measurement techniques were used to characterize the deposit and ZnCo 2 O 4 /Ni electrode. Compared with the ZnCo 2 O 4 electrode prepared by nitrate decomposition method, the electrophoretic ZnCo 2 O 4 electrodes exhibit better electrocatalytic properties and higher mechanical stability. And the electrode prepared at 10V for 5min has the best electrocatalytic properties with the overpotential of only 0.203V at current density of 100mAcm −2 .