Recently, a new dual plasma-process to produce non noble metal catalysts for the oxygen reduction in proton exchange membrane fuel cells has been developed and catalytically active cobalt-polypyrrole-films have been produced. This paper shows a modification to this process, so that iron-polypyrrole is formed. The magnetron power as well as the process gases were varied. The structure of the compounds was then analyzed by energy-dispersive X-ray spectroscopy, X-ray diffraction, near edge X-ray absorption fine structure and extended X-ray absorption fine structure. It is shown that the oxidation of the compounds is suppressed when hydrogen or nitrogen is added to the process. Furthermore, cyclic voltammetry and rotating ring-disk electrode measurements were done to determine the electrochemical properties of the films. Only films produced in hydrogen or nitrogen containing gases show catalytic activity and it can be seen that the four-electron reduction mechanism is dominant.