Dehydroxylation of gels is important for the preparation of high quali
ty glasses and for the application of the porous gel materials at high
temperatures. In this report, the effect of changing the microstructu
re of silica aerogels on the thermal dehydroxylation of the gels in va
cuum is presented. Surface area, density and IR spectra of the aerogel
s were determined after heat treatment to 1100 degrees C in vacuum. Th
e two different microstructures have been obtained by aging one set of
gels in a water/ethanol solution to promote coarsening of the wet gel
prior to supercritical drying. Network coarsening causes a larger por
e size and less concave neck curvature of this type of aerogels. Coars
ening of the network was shown to facilitate dehydroxylation of the ae
rogels.