Silica host matrix containing neodymium which is potentially important for the formation of nanocrystalline metal oxides was prepared by solgel method, using tetra-ethoxysilane and Nd(NO3)3 as precursor materials. The prepared samples were changed from amorphous to nanocrystallites phase at sintered temperature 550℃ (4 h), 750℃ (8 h) and 950 ℃ (12 h). The thermally treated sample microstructures were investigated using X-ray diffraction (XRD), Fourier transformation infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). While a further increase of the temperature at 750 ℃ and annealing time (8 h) resulted in the formation of cubic and hexagonal Nd2O3 nanocrystallites. At constant sintering temperature 950℃ for 12 h, the samples showed sharper and intense peaks. The sizes of Nd2O3 nanocrystallites were characterized by XRD with average size～46 nm.
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