Using the sol-gel technique a SiO2-PMMA hybrid matrix was synthesized by the simultaneous hydrolysis of tetraethyl orthosilicate (TEOS) and the polymerization of methyl methacrylate (MMA). The hybrid material was doped with terbium ions for it's luminescent properties for applications in thin film devices, sensors and as an active laser media. The optical properties of the material were characterized by UV–vis and photoluminescence spectroscopy. Surface morphology of the material properties were observed using atomic force microscopy and the material's composition was studied using Raman spectroscopy. Distribution of the dopant inside matrix was analyzed by confocal microscopy. Measurements indicate that a homogeneous, non-porous composite was obtained with the terbium ions retaining their luminescent properties with good optical transmission across all the visible spectra.