Cobalt- or iron-based electrocatalysts have been examined for their electrocatalytic activity toward the reduction of oxygen. These materials were obtained from organic aerogels prepared with melamine, formaldehyde, and iron or cobalt salt, followed by carbonization. The activity of the electrocatalysts for the oxygen reduction reaction (ORR) was investigated using cyclic voltammeter (CV) and the rotating disk electrode (RDE) technique in 0.5 M H2SO4 solution at room temperature. The fuel cell performance of single cells with the electrocatalysts was examined under actual DMFC conditions. Iron or cobalt supported on N-doped carbon aerogels electrocatalysts showed good electrocatalytic activity for the oxygen reduction in acidic solutions. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.