In this study, supercritical carbon dioxide (scCO(2)) deposition was used to prepare vulcan-supported Pt (Pt/Vulcan) electrocatalysts for proton exchange membrane fuel cells (PEMFCs), and the effects of process variables on the properties of the electrocatalysts were investigated. The two different methods used to reduce the organometallic precursor were thermal reduction in nitrogen at atmospheric pressure and thermal reduction in scCO(2). In the former method, the maximum Pt loading achieved was 9%, and this was governed by the adsorption isotherm of the Pt precursor between the scCO(2) phase and the Vulcan phase. By using the latter method, higher Pt loadings of 15% and 35% could be achieved. The Pt/Vulcan catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and cyclic voltammetry (CV). The average particle sizes for Pt/Vulcan 9%, 15%, and 35% catalysts were 1.2, 1.3, and 2nm, respectively. Electrochemical surface areas obtained from CV data were found to vary with the Pt loading.