Pd nanoparticles highly dispersed onto the surface of ordered mesoporous carbons (OMCs) were synthesized successfully by poly( sodium-p-styrenesulfonate) (PSS) assisted microwave synthesis. Here, PSS served as a bifunctional molecule both for solubilizing and dispersing OMCs into aqueous solution and for jointing Pd2+ to facilitate the subsequent uniform formation of Pd nanoparticles on their surfaces. The effects of PSS on structural and electrochemical properties of Pd/OMCs were investigated. It was found that the addition of PSS facilitated Pd nanoparticles to disperse on the carbon surface. Electrochemical properties showed that Pd catalysts prepared with addition of PSS displayed better electrochemical activity and stability for formic acid electro-oxidation than those without PSS. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.