Structural characterization of Rh/pumice SMAD catalysts

The structure of Rh/pumice catalysts prepared by the SMAD (Solvated Metal Atoms Dispersion) technique at different metal loadings has been investigated by EXAFS (Extended X-ray Absorption Fine Structure Spectroscopy) XPS (X-ray Photoelectron Spectroscopy), SAXS (Small-Angle X-ray Scattering), WAXS (Wide-Angle X-ray Scattering) and TEM (Transmission Electron Microscopy). According to EXAFS and XPS, a fraction of the Ph atoms is oxidised, but a noticeable part is also present as Rh-0. The Rh oxidation is attributed to the interaction of the Rh atoms with the hydroxyls of the support; after the formation of the oxide, the nucleation of metallic rhodium becomes possible. The WAXS data do not show evidence of rhodium fcc crystallites; the metal-bearing particles are probably amorphous and/or very small, as results from the SAXS and TEM data analysis. The disagreement between the latter two techniques, resulting in a small-angle determination of the average size of the particles that is about half that of TEM in the catalyst with the higher Rh loading, is acknowledged and discussed. Preliminary catalytic tests are described, demonstrating the suitability of using a low surface area support for the preparation of SMAD catalysts.