Catalytic layers of platinum-ruthenium of preliminarily specified compositions are manufactured with the aid of ion exchange and subsequent chemical and electrochemical reduction in polymeric Nafion films applied onto carbonaceous materials and inside a standard Nafion 117 membrane. The procedure used for conducting the ion-exchange procedure ensures a high process rate and a short time required to conduct it, which makes it possible to obtain large roughness factors at relatively small contents of platinum metals (0.1–0.2 mg cm−2). The electrochemical activity of catalyzed membrane samples for methanol oxidation in aqueous and sulfuric acid solutions is close to the activity of standard E-TEK platinum-ruthenium catalysts.