Sodium borosilicate gels of compositions similar to that of Vycor(R) glass like 80SiO(2).15B(2)O(3).5Na(2)O (wt%) were prepared from hydrolysis and polycondensation of metal alkoxides under the HCl catalysis. Variation of specific surface area and porosity with temperature indicated that closed pores were opened below 400℃, and collapsed above 450℃ after the porosity reached a maximum value around 450℃. The structural evolution was examined due to IR spectra and a phase separation in the gels was observed. The solubility of the gels into 1N-HCl was studied as a function of the treatment temperature.