The effect of higher non-precious metal loading in oxygen reduction catalysts for use in proton exchange membrane fuel cell catalysts was investigated using the rotating ring disk electrode and rotating disk electrode methods. Metal loadings of 6, 10, and 15 weight percent were deposited on a support where acetonitrile decomposition in an inert atmosphere formed a carbon-nitride material that was active for the electroreduction of oxygen in an acidic medium. Activity results indicate that higher metal loading in the carbon growth media affects the activity of oxygen reduction catalysts formed during carbon growth. These iron phases and oxidation states of the growth media was further characterized during in-situ pyrolytic carbon growth using X-ray absorption techniques. It was found that the iron phase of the impregnated support mostly consisted of mixed oxides, which were reduced to metallic iron and iron carbide upon the introduction of acetonitrile that caused carbon growth.US Department of Energy Basic Energy SciencesA one-year embargo was granted for this item