Résumé : Thin sulfonated polystyrene films were prepared by high pressure PECVD of styrene and trifluoromethane sulfonic acid using a DBD. Argon or helium was used as carrier gas. The chemical composition of the pp-sulfonated polystyrene was investigated by XPS, SSIMS, and FTIR. XPS shows that the content in sulfonated groups of the films deposited in the discharge can be tuned by varying the temperature of the acid monomer or by improving the HF voltage. Therefore, the films obtained are rich in ionizable groups (more than Nafion). TOF-SSIMS and FTIR spectra allow to confirm the presence of sulfonic groups (observed on S2p XPS spectra) grafted in the polystyrene matrix. Plasma polymerized sulfonated polystyrene films, of potential interest as fuel cell membranes, are synthesized at high pressure in a DBD from styrene and trifluoromethane sulfonic acid. They are characterized by XPS, SSIMS and FTIR. The process shows a high retention of the sulfonic character of sulphur. The concentration of sulfonated groups in the membranes can be tuned by the plasma parameters. © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.