Phase relations in heat treated sodium borosilicate glasses

Sodium borosilicate glasses are processed to porous glasses as well as to Vycor™ type glasses via phase separation and selective leaching. Both materials consist mainly of SiO2. Thermal treatment inducing phase separation is crucial for microstructure development. Sodium borosilicate glasses with molar compositions of 8Na2O.21B2O3.71SiO2 and 8Na2O.28B2O3.64 SiO2 were melted, rapidly cooled and investigated by thermal analysis and scanning electron microscopy. The glasses were thermally treated for 120 h at 630 to 730°C, and then leached, first for 72 h in 0·1 M HCl at 60°C, and subsequently for 4 h in 0·5 M NaOH at 30°C. X-ray fluorescence was applied to characterise the chemical compositions. Microstructure development was first analysed by differential thermal analysis and dilatometry, and the pore structure was characterised by Hg porosimetry and N2 adsorption. Heat treated glasses were then analysed by low voltage scanning electron microscopy, combined in one case with chemical analysis by energy dispersive x-ray analysis. The results are discussed with respect to phase relations. After long term heat treatment, at least three phases exist in two independent metastable two-phase equilibria on different size and time scales.