Carbon-supported Pd-Co alloy electrocatalysts were synthesized and characterized for the purpose of the fuel cell cathode oxygen reduction reaction (ORR). An impregnation method was employed for the synthesis, in which sodium borohydride was used as a reducing agent. The synthesized catalysts were characterized in terms of structural morphology and catalytic activity by XRD, XPS and electrochemical measurements. Surface cyclic voltammetry was used to confirm the formation of the Pd-Co alloy. In order to improve activity and stability, the catalysts were heat-treated in the temperature range of 300 degrees C to 700 degrees C. The optimal heat-treatment temperature was found to be 300 degrees C, where the average particle size of 8.9 nm, and the highest ORR catalytic activity, were obtained. The catalyzed ORR kinetics were also studied using the rotating disk electrode (RDE) method. The kinetic parameters were then obtained. Electrocatalytic ORR activity was also examined in an acidic solution containing methanol. The results showed that the synthesized Pd-Co/C catalyst has methanol tolerant capabilities. Crown Copyright (c) 2006 Published by Elsevier Ltd. All rights reserved.