Ak. Singh et Cg. Pantano, SURFACE-CHEMISTRY AND STRUCTURE OF SILICON OXYCARBIDE GELS AND GLASSES, JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, 8(1-3), 1997, pp. 371-376
In this study, the surface chemistry and structure of methyl-substitut
ed silica gels and porous oxycarbide glasses were investigated. FTIR w
as used to measure the relative concentration of Si-CH3 and Si-OH as a
function of the degree of methyl-substitution and the pyrolysis tempe
rature. The gels and glasses were further heated, dehydrated or hydrat
ed, in situ, within the FTIR spectrometer. In the temperature range of
800-850 degrees C, high surface area oxycarbide glasses were created
with no detectable surface hydroxyl groups. Oxycarbide glasses synthes
ized in argon at 700 degrees C displayed a weak band for surface hydro
xyl groups and reversible physisorption of water, while those synthesi
zed at 850/900 degrees C showed a complete absence of surface hydroxyl
groups and the formation of vicinal silanols upon chemisorption of wa
ter. Isolated silanols were observed upon heat treatment in vacuum. Fo
rmation of aromatic carbon species was found to correlate with the dec
omposition of the methyl groups. The oxycarbide surface is quite stabl
e to densification (presumably due to elemental carbon on the pore sur
faces). In the absence of oxygen, porous silicon oxycarbide glass powd
ers maintain surface areas >200 m(2)/g at 1200 degrees C. However, oxi
dizing species in the atmosphere deplete the aromatic carbon species,
and the glasses lose surface area.