Effect of thiourea on nickel deposition at glassy carbon and nickel-deposited glass carbon electrodes was investigated with cyclic voltammograms and impetance-potential curves. It was found that the nucleation processes occurred at the glassy carbon electrode. However, this characteristics disappeared at the nicked-deposited glassy carbon electrode. It was suggested that the presence of thiourea hindered the nucleation processes, yet accelerated grain growth.Curves of impetance-potential could sensitively detect effect of thiourea on nickel depositon and reflect changes in rate-determining step with potential.