Nano-sized platinum and ruthenium dispersed on the surface LiCoO2 as catalysts for borohydride hydrolysis are prepared by microwave-assisted polyol process. The catalysts are characterized by transmission electron microscopy (TEM), X-ray diffractometry (XRD) and X-ray photoelectron spectroscopy (XPS). Very uniform Pt and Ru nanoparticles with sizes of <10nm are dispersed on the surface of LiCoO2. XRD patterns show that the Pt/LiCoO2 and Ru/LiCoO2 catalysts only display the characteristic diffraction peaks of a LiCoO2 crystal structure. Results obtained from XPS analysis reveal that the Pt/LiCoO2 and Ru/LiCoO2 catalysts contain mostly Pt(0) and Ru(0), with traces of Pt(IV) and Ru(IV), respectively. The hydrogen generation rates using low noble metal loading catalysts, 1 wt.% Pt/LiCoO2 and 1 wt.% Ru/LiCoO2, are very high. The hydrogen generation rate using Ru/LiCoO2 as a catalyst is slightly higher compared with that of Pt/LiCoO2. (c) 2007 Elsevier B.V. All rights reserved.