Poly[Ni(salen)] films were electropolymerized on multiwalled carbon nanotubes (MWCNTs) in tetrabutylammonium perchlorate/acetonitrile by cyclic voltammetry method. And the employed scan rates were 5, 10, 20 and 40 mV s . The excellent electrochemical performance of poly[Ni(salen)] electropolymerized at 20 mV s −1 is ascribed to the better conductivity and superior diffusion ability according to the kinetics.