Pt catalyst supported on Vulcan XC-72R containing 5 wt% NiO (Pt/NiO-C) showed larger electrochemical active surface area and higher electrochemical activity for methanol oxidation than Pt catalyst supported on Vulcan XC-72R using polyol method without NiO addition. Prepared Pt/NiO-C electrocatalyst was heat-treated at four temperatures (200, 400, 600, and 800 degrees C) in flowing N(2). X-ray diffraction and tempera tu re-programmed desorption results indicated that NiO was reduced to Ni in inert N(2) during heat-treatments at temperatures above or equal to 400 degrees C, while oxygen from NiO reacted with carbon support due to the catalytic effect of Pt. The reduced Ni formed an alloy with Pt, which, according to the X-ray photoelectron spectroscopy data, resulted in a shift to a lower binding energy of Pt 4f electrons. The Pt/NiO-C electrocatalyst heat-treated at 400 degrees C showed the best activity in methanol oxidation due to the change in Pt electronic structure by Ni and the minimal aggregation of Pt particles. (C) 2009 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.