AbstractPoly(p-phenylene/pyrrole) (PPP-PPY) films were electrochemically synthesised on transparent indium-tin-oxide-covered glass (ITO) electrodes. The presence of two monomers, p-phenylene and pyrrole, in the polymerisation medium facilitated the synthesis process, yielding electroactive, uniform and stable films. In order to obtain materials with improved quality, PPP, PPY and PPP-PPY films were prepared in a mild, dry atmosphere. The morphological, electrochemical and optical properties were compared for different films obtained by varying the number of cycles with and without controlling humidity.