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 tetraethyl orthosilicate, trimethyl borate, and sodium methylate under the HCl catalysis. Variation of the gelation time is examined as a function of the mixing ratio of the starting materials and the catalyst. The thermal behavior of the gels has been discussed on the basis of their TG and DTA traces.