Carbon supported Palladium-Iron bimetallic nanoparticles (Pd-Fe/C) electrocatalyst is synthesized by the direct thermal decomposition method of nontoxic metallic acetate salt. During the preparation of the Pd-Fe/C electrocatalyst, the tedious wash post-treatment of electrocatalyst is effectively avoided due to non-existence of inorganic anion. The physicochemical properties of the Pd-Fe/C electrocatalyst are characterized by X-ray diffraction analysis (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). These structural analyses reveal that the Pd-Fe/C electrocatalyst possesses the high alloying degree and the small particle size. Electrochemical data indicate that the eletrocatalytic activity of the Pd-Fe/C electrocatalyst for oxygen reduction reaction (ORR) is much higher than that of Pd/C electrocatalyst, which originates from the synergistic effect between Pd atom and Fe atom. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.