Iron oxide-based porous solids were prepared by a sol−gel process using Fe(III) salts in
various solvents. It was observed that the addition of propylene oxide to Fe(III) solutions
resulted in the formation of transparent red-brown monolithic gels. The resulting gels were
converted to either xerogels by atmospheric drying or aerogels by supercritical extraction
with CO2(l). Some of the dried materials were characterized by nitrogen adsorption and
desorption analysis and transmission electron microscopy (TEM). The results of those
analyses indicate that the materials have high surface areas (∼300−400 m2/g), pore sizes
with mesoporic dimensions (2−23 nm), and a microstructure made up of 5−10 nm diameter
clusters of iron(III) oxide. The dependence of both gel formation and its rate was studied by
varying the epoxide/Fe(III) ratio, the Fe(III) precursor salt, amount of water (H2O/Fe(III))
present, and the solvent employed. All of these variables were shown to affect the rate of
gel formation and provide a convenient control of this parameter. Finally, an investigation
of the mechanism of Fe2O3 gel formation was performed. Both pH and nuclear magnetic
resonance (NMR) studies suggest that the added epoxide acts as an irreversible proton
scavenger that induces the Fe(III) species to undergo hydrolysis and condensation to form
an inorganic iron oxide framework. This method can be extended to prepare other transition-
and main-group metal oxide materials.