Résumé : Cobalt and platinum-cobalt bimetallic alloy nanoparticles of uniform size distribution where prepared and supported on MCF-17 to produce a controlled and well-characterized model catalyst which was studied under reaction conditions during CO2 hydrogenation. Near edge X-ray absorption fine structure (NEXAFS) spectroscopy was used to elucidate the oxidation state of the catalyst under reaction conditions while the effect of reducing H2 gas on the composition and structure of the bimetallic PtCo nanoparticles was measured using ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and environmental transmission electron microscopy (ETEM). NEXAFS indicates that Pt aids the reduction of Co to its metallic state under relevant reaction conditions, while AP-XPS and ETEM indicate that Pt is enriched at the surface by exchange with subsurface layers which become Pt deficient-in agreement with the "Pt-like" selectivity seen during catalytic testing of these materials. © 2011 Springer Science+Business Media, LLC.