Gd(NO 3 ) 3 Á6H 2 O and TEOS were used as precursors and obtained powdered form of Gd 2 O 3 :SiO 2 nanocomposite. The as-prepared sample was annealed at 773 K and 1173 K and characterized by XRD, TEM, UV-Vis spectra, and PL. The average nanocrystallite size was found of the order of~27 nm using well-known Debye-Scherer's equation. From the UV-Vis spectra, it was shown that the position of absorption peak has been shifted toward the higher wavelength side with temperature. In the PL spectra, the broad emission band has been observed at 583 nm along with weak bands at 516, 526, and 556 nm.