Y(NO 3 ) 3 and NH 3 ·H 2 O were used as a raw materials, and nano-Y 2 O 3 powder was successfully synthesized by a precipitation method. Employing TEOS as a raw material, SiO 2 powder was successfully prepared by a alkoxide-hydrolysis method, and a Y 2 O 3 /SiO 2 composite powder was obtained by coating. The Y 2 O 3 , SiO 2 , and Y 2 O 3 /SiO 2 powders were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared spectrophotometer (FT-IR); the Y 2 O 3 and Y 2 O 3 /SiO 2 powders were further examined by photoluminescence (PL) spectra. The results indicated that the Y 2 O 3 powder had a body-centered cubic structure with an average size of 35 nm, while the SiO 2 powder was amorphous, with an average size of 145 nm and a narrow size distribution. The PL spectra of the Y 2 O 3 and Y 2 O 3 /SiO 2 powders showed that their wavelength of emission spectra were 585 nm, while their wavelength of excitation spectra were in the range of 240-260 nm. The optical properties of the Y 2 O 3 /SiO 2 powder were identical to the Y 2 O 3 powder.