This study represented a novel conducting poly (p-nitroaniline-co-p-aminophenol) (P(p-NAn-co-p-APh)) material, obtained by electrocopolymerization of para-nitroaniline (p-NAn) and para-aminophenol (p-APh) in aqueous sulfuric acid solution. Copolymerization was carried out using cyclic voltammetry technique on gold electrode with different monomer feed concentrations. The obtained polymer and copolymer films had been characterized by scanning electron microscopy (SEM), in situ conductivity measurements, in situ UV-Vis, and FT-IR spectroscopy. Initial cyclic voltammograms of p-NAn, p-APh and p-NAn p-APh showed that the peak potentials were located at different values. The in situ conductivity of the copolymers measured between -0.20 V< E-SCE < 0.70 V increased with decreasing the [p-NAn]/[p-APh] concentration ratio. In situ UV-Vis. spectra of the obtained samples revealed strong absorption bands at different applied potentials and wavelengths. The structure and morphology characterizations of homo and copolymer films were studied by FT-IR spectroscopy and SEM analysis. Fundamental differences between the morphology of the homo- and copolymers were observed. The mechanism of the electrochemical copolymerization reaction was discussed as well. (c) 2015 The Electrochemical Society. All rights reserved.