Highly efficient Pt/TiO2 photocatalyst has been prepared using plasma-enhanced impregnation method. Impregnated 0.5 wt% Pt/TiO2 was treated by plasma followed with thermal calcinations and hydrogen reduction. The catalyst characterizations show that Pt is highly dispersed with a size of 3-5 nm. UV-Vis reflection spectrum suggests it a high photosensitivity in near UV region. Such plasma prepared catalyst exhibits a much higher activity and better metal stability for hydrogen generation from methanol/water mixture, compared to the catalyst prepared conventionally. This highly efficient photocatalyst should have extensive applications in photocatalytic processes. (C) 2004 Elsevier B.V. All rights reserved.