Using solgel method Nd2O3−SiO2 binary oxide systems were prepared. The binary oxide transformed from the amorphous phase to nanocrystalline phase upon heat treatment in air. Characterization of the Nd2O3-SiO2 was carried out by using X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. The effect of the sintering temperature and time on the evolution of the binary oxide system was discussed. It is found that sintering time plays a pivotal role to obtain Nd 2 O 3 -SiO2 nanocomposite. At temperature of 900• C, the sample was sintered for 12 h and monoclinic Nd 2 O 3 nanocrystallites, with average crystallite size ≈ 12 nm, were obtained.