Electrocatalysts were fabricated for a polymer electrolyte membrane fuel cell using a sputter deposition technique. A pure Ni target was deposited onto a carbon nanotube impregnated on carbon paper. The sample was then heat treated in ammonia based environment. In examining the ORR polarization curve and cyclic voltammetry, as the heat treatment temperature changed, the sample showed the highest mass activity at 850 degrees C. This level of mass activity was 3 times higher than that of samples treated at other temperatures at the same voltage (0.9 V). The optimal heat treatment temperature for maximum mass activity was dependent on the formation of ligands between Ni and CNT which were linked by nitrogen. Even though the catalytic activity is not comparable to that of Pt/C catalysts yet, sputtered Ni based electrocatalysts may potentially serve as the non-precious metal electrocatalysts. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.