AbstractNumerous materials (supports and catalysts) based on alumina have been prepared using the sol‐gel process and carbon dioxide supercritical drying. In this work two types of solids, i.e. xerogels and aerogels, were systematically compared and a way of introducing platinum metal with a content of 5% percent by weight was examined. The structural data, the surface area, Pt dispersion and catalytic activity for the decomposition of the propellant were measured for the various samples. The (Al2O3)0.88(SiO2)0.12 samples prepared show very interesting porosity values, especially for the aerogel. For this reason, they were chosen as supports for the synthesis of 5 wt% platinum on alumina catalysts. The results presented in this work allowed us to obtain an overall view of the influence of the preparation mode on the properties of platinum on alumina supported catalysts. The dispersion of the metal phase is directly dependent on the specific surface of the support. A significant value for the surface area implies a large amount of centers for interaction with the metal precursor and, consequently, the appearance of more centres of simultaneous germination. Although aerogels obtained by carbon dioxide supercritical drying always show superior properties compared with xerogels, for catalytic decompositions the xerogels still remain superior. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005)