Nanocomposite PANi/TiO2 has been synthesized in HNO3 1 N on stainless steel (SS) electrode using cyclic voltammetry (CV) technique. The presence of nano- TiO2 modified the synthesis CV curves, especially the characteristic redox reaction of formed P ANi. Peak potential Ep, peak current Jp and total electric quantity Q were strongly affected. Electrochemical impedance of the nanocomposite PANi/TiO2 film was increased in comparison with intrinsic PANi film, mostly due to an increasing of the charge transfer resistance Ret-Nano-TiO2 has been incorporated into PANi chain, and affected some physicochemical properties of the PANi film.