Homogeneous mixed-metal oxides of the general formula (Si/E/Pb)O-x, where E is either Se or Te, can be prepared using typical sol-gel processing techniques. Reduction of the in situ Se or Te ions by hydrogen affords crystalline nanoparticles of PbSe or PbTe widely dispersed throughout the silica xerogel matrix. The materials prepared contain PbSe or PbTe nanoparticles with average diameters of 8.9 nm and 7.6 nm, respectively. Precursor gels and nanocomposite materials have been characterized using powder X-ray diffraction and transmission electron microscopy. These results demonstrate a convenient method for the production of practical quantities of nanostructured lead chalcogenides in a ceramic matrix. (C) 2010 Elsevier B.V. All rights reserved.