Osmium electrocatalysts for the oxygen reduction reaction (ORR) were prepared by microwave irradiation of Os 3 (CO) 12 at different experimental conditions. The materials obtained were structurally characterized by FT-IR, micro-Raman spectroscopy and X-ray diffraction. Their chemical compositions were obtained by EDS. The electrocatalytic properties for the oxygen reduction reaction were evaluated by rotating disk electrode measurements in 0.5 mol L −1 H 2 SO 4 , in the absence and presence of aqueous methanol. The kinetic parameters, such as Tafel slope, exchange current density, and charge transfer coefficient are reported.