高硅氧发光玻璃是一种极具发展潜力的新型发光材料，制备过程中分相是影响其发光性能的重要因素。为了研究分相过程的影响因素和内部变化的基本原理，借助红外吸收光谱和紫外可见吸收光谱研究了高硅氧发光玻璃制备中分相前后钠硼硅酸盐玻璃样品的微结构变化与相应的光谱特性，理论上分析了变化产生的原因。结果表明，分相后玻璃原有的网络结构遭到破坏，非桥氧含量增加，同时三配位硼含量降低，四配位硼含量增加。四配位硼由于钠离子的作用会对三配位硼有吸引作用，使硼氧网络无法形成架状结构，与硅氧网络结构差异很大，最终形成分相。

High silica luminescent glasses are one of new luminescence materials with the most potential development. And phase separation is one of the most important influencing factors on their fluorescence properties. To research the influence factors and internal basic principle during phase separation, infrared spectrum and UV-visible spectrum are used for the studies on the change of microstructure and the corresponding spectra when the samples of sodium borosilicate glasses are heat-treated. Experimental results show that after the process of phase separation, the original network structures of the glass samples are broken, non-bridging oxygen content increases and meanwhile three-coordinated boron′s content decreases with four-coordinated boron′s content increasing. The three-coordinated boron is attracted by four-coordinated boron because of the effects of Na+. So the differences between Si net work and B net work become more and more obvious, at last the phase separation is induced.