Highly porous carbon xerogels (CXGs) were synthesized to be used as support for PtRu nanoparticles. Metal particles were deposited on CXGs by means of the sulfite complex method for the first time. Catalysts so-obtained were submitted to thermal treatment in H 2 , at different temperatures, in order to increase the particle size and thus the intrinsic activity. Physico-chemical characterizations included N 2 physisorption, X-Ray diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy. Highly dispersed alloyed PtRu particles were obtained, with crystal sizes ranging from 1.6 to 2.0 nm. PtRu-catalysts were tested in half-cell for the methanol oxidation reaction (MOR). The resulting thermal treatment was effective in increasing both particle size and catalytic activity toward MOR.