Sm. Manocha et al., Thermal evolution of hybrid organic-inorganic gels derived from reaction of 1,4 butanediol with tetraethoxysilane, J SOL-GEL S, 16(3), 1999, pp. 221-226
Transparent monolithic discs of organic-inorganic hybrid gels have been pre
pared by hydrolysis-condensation reactions of tetraethyl orthosilicate with
1,4 butanediol. The gels and glasses have been characterized by infrared s
pectroscopy and Si-29 MAS NMR. The characterization of the gels by infrared
spectroscopy showed the incorporation of carbonaceous groups in the polyme
ric structure and Si-C bonding in the glasses. Pyrolysis of the gels has be
en studied using thermal analysis. It showed that the pyrolysis of the gels
occurs in two temperature domains. The first is below 400 degrees C due to
condensation reactions and second is in the temperature range 450-550 degr
ees C due to decomposition of carbonaceous groups and crosslinking. Pyrolys
is of the gels at 1000 degrees C resulted in X-ray amorphous, hard black gl
asses similar to oxycarbide glasses obtained by pyrolysis of siloxanes. On
further heat treatment to 1400-1600 degrees C, development of cristobalite
structure and crystalline silicon carbide is observed in the otherwise amor
phous black mass. The pyrolysed materials have been found to exhibit good r
esistance towards oxidation at 1000 degrees C.