We have investigated the spatial distribution of Sm2+ inside macroporous alumina-silica (Al2O3-SiO2) glasses having three-dimensionally interconnected skeletons. The Sm2+-doped Al2O3-SiO2 glasses are prepared via an alkoxy-derived sol-gel route in the presence of poly (ethylene oxide) and SmCl3.6H(2)O. The well-defined macroporous morphology is obtained by the concurrence of the phase separation and the sol-gel transition. The reduction of Sm3+ to Sm2+ is accomplished by heat treatment under a reducing atmosphere. Two-dimensional images of the fluorescence due to the 4f-4f transition of Sm2+ with the aid of a laser scanning confocal microscope reveal the spatially uniform dispersion Of Sm2+ inside the Al2O3-SiO2 skeleton. (c) 2005 Elsevier B.V. All rights reserved.