We report the preparation and catalytic properties of highly ordered mesoporous Fe-Ga-SBA-15 materials via direct hydrothermal synthesis. Gallium and iron ions were introduced directly into the synthesis gel typical for the preparation of SBA-15. The resulting materials had hexagonally ordered mesopores of about 6 nm and surface areas >1000 m(2)/g. In Fe-SBA-15, the iron species were mainly tetrahedrally coordinated in the amorphous silica walls. In the presence of Ga (Fe-Ga-SBA-15), Fe species were located at the silica surface as isolated species, as determined by Raman and diffuse-reflectance UV-Vis spectroscopy measurements. The Fe species in Fe-Ga-SBA-15 displayed similar properties as the FeZSM-5 zeolites toward nitrous oxide decomposition and were active in the oxidation of benzene to phenol by nitrous oxide. Ga-SBA-15 and Fe-SBA-15, on the other hand, showed no catalytic activity. Compared with Fe-Al-SBA-15, Fe-Ga-SBA-15 displayed greater selectivity to the desired phenol product. (C) 2008 Elsevier Inc. All rights reserved.