高硅氧发光玻璃是一种极具研究潜力的新型发光材料，制备过程中其分相温度是影响最终光致发光性质的重要因素。在不同分相温度下制备了多孔玻璃，并在相同吸附条件下制备了Eu2+/Dy3+共掺的高硅氧发光玻璃，测试了各多孔玻璃的比表面积参数和相应高硅氧发光玻璃的发射光谱。多孔玻璃比表面积参数测试结果表明，随着分相温度升高，多孔玻璃的比表面积先减小后增大。发射光谱测试结果表明，随着分相温度升高，烧结制备的高硅氧发光玻璃的发射特征峰峰值位置相同，发光强度先减小后增大。其中分相温度为620 ℃的多孔玻璃具有最大的比表面积，所制备的高硅氧发光玻璃具有最大的发光强度。

High silica glass is a potential luminescence material in the future, whose photoluminescence properties are seriously influenced by phase separation temperature in the procedure. Porous glass with different phase separation temperatures and Eu2+/Dy3+ co-doped high silica luminescence glass with the same adsorption conditions are prepared. The specific surface area parameters of porous glass and the emission spectra of corresponding high silica luminescence glass are measured. The specific surface area measurement results indicate that the specific surface area of porous glass decrease firstly and then increase when the phase separation temperature is rising. The emission spectra of high silica luminescence glass indicate that the positions of characteristic peaks of high silica luminescence glass remain unchanged, while the emission intensity decreases firstly and then increases when the phase separation temperature is rising. Porous glass with phase separation temperature 620 ℃ has relative maximal specific surface area and corresponding high silica luminescence glass has the maximal emission intensity.