An improved sol-gel method was employed to prepare Eu3+ ions doped SiO2-Y2O3 nanocomposites.Systematic study was carried out on the effect of post-annealing treatment on photoluminescence(PL) properties of the samples under various europium ions doping concentrations.X-ray diffraction(XRD) patterns indicated that the samples showed an amorphous matrix structure,and the scanning electron microscopy(SEM) pictures showed that the samples presented a nano size(from 21 to 42 nm) granular-stack structure after high-temperature annealing treatment(from 600 to 900 °C,respectively) for 3 h.Raman spectra demonstrated that Y3+ and Eu3+ ions were incorporated into the composites through the sol-gel and post-annealing process.Under the excitation of 394 nm(7F0→5L6) light,red emission was observed around 613 nm(5D0→7F2).Without annealing treatment,the optimized doping amount of Eu ions was about 6.5 mol.%,which was much higher than that single doped in SiO2 glass matrix with Eu ions concentration of 3%,and it raised to 9.0% when the samples were annealed at high-temperature(900 °C) annealing. An improved sol-gel method was employed to prepare Eu3 + ions doped SiO2-Y2O3 nanocomposites. Systematic studies was carried out on the effect of post-annealing treatment on photoluminescence (PL) properties of the samples under various europium ions doping concentrations. X-ray diffraction (XRD) patterns indicated that the samples showed an amorphous matrix structure, and the scanning electron microscopy (SEM) pictures showed that the samples presented a nano size (from 21 to 42 nm) granular-stack structure after high-temperature annealing treatment ( from 600 to 900 ° C, respectively) for 3 h. Raman spectra of that Y3 + and Eu3 + ions were incorporated into the composites through the sol-gel and post-annealing process. Undertaken by the excitation of 394 nm (7F0 → 5L6) light, red emission was observed around 613 nm (5D0 → 7F2) .Without annealing treatment, the optimized doping amount of Eu ions was about 6.5 mol.%, which was much higher than that single doped in SiO2 glass matrix with Eu ions concentrati on of 3%, and it raised to 9.0% when the samples were annealed at high-temperature (900 ° C).