Electroconductive polychloroprene (CR)-polyaniline (Pani) composites were prepared by swelling the vulcanized rubber material in aniline followed by immersing the specimen in an aqueous solution of HCl containing ammonium persulfate as the oxidant, The results obtained from surface and volume conductivity, scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS) analysis suggest that the Pani component is preferentially located in the surface layer. These composites display better electrical and mechanical performance than those obtained by mixing both polymer components in the bulk state.