Ga1-xInxSb (x = 0.19, 0.38, 0.63) nanoparticles embedded in a SiO2 matrix were grown on the glass substrates by radio-frequency magnetron co-sputtering. X-ray diffraction patterns strongly support the existence of nanocrystalline Gal(1-x)In(x)Sb in the SiO2 matrix. The changes in binding energies with Ga1-xInxSb nanocrystals deposition have been directly observed by X-ray photoemission spectroscopy, and these show the existence of Ga1-xInxSb nanocrystals in the SiO2 matrix. Room-temperature Raman spectra show that the Raman peaks of the Ga1-xInxSb-SiO2 composite film have a larger red-shift of about 95.3 cm(-1) (longitudinal-optical mode) and 120.1 cm(-1) (transverse-optical mode) than that of bulk GaSb, suggesting the existence of phonon confinement and tensile stress effects. Additionally, the room temperature optical transmission data exhibit a large blue-shift with respect to that of the bulk semiconductor due to the strong quantum confinement effect. (C) 2002 Elsevier Science Ltd. All rights reserved.