The Pd-Co/C alloy catalysts with an atomic ratio of 3 1 were deposited at various pH values and reduced at different temperatures for oxygen reduction reaction (ORR) The structure-activity relationship of the prepared catalysts has been elucidated The pH values and reduction temperatures during the preparation process affect the deposition and reduction rates of Pd and Co ions significantly, and thus the degrees of alloying, surface species, and ORR activities of the Pd-Co/C catalysts are also influenced Due to the enhancement of Co surface segregation and the formation of Co oxide on the surface, a deterioration of ORR activity for the catalysts reduced at high temperatures and high pH values is observed The catalysts deposited at pH value of 9 and reduced at a very low temperature of 390 K have well-formed Pd-Co alloy structure, Pd-rich surface, and excellent ORR activity (C) 2009 Professor T Nejat Veziroglu. Published by Elsevier Ltd All rights reserved