The synthesis of iron(III) oxide aerogel monoliths was performed by adding any one of
several different 1,2- and 1,3-epoxides to ethanolic Fe(III) salt solutions at room temperature.
While all of the epoxides examined resulted in gel formation, robust low-density (∼30−40
kg/m3; 99% porous), high-surface-area (∼250−300 m2/g), aerogel monoliths were prepared
by the addition of 1,3-epoxide derivatives to solutions of FeCl3·6H2O, followed by drying
with supercritical CO2. Both types of iron(III) oxide aerogels (those made with 1,2- and 1,3-epoxides respectively) were characterized using elemental analysis, X-ray diffraction, thermal
analysis, acoustic measurements, transmission electron microscopy, scanning electron
microscopy, and N2 adsorption desorption analysis. Elemental analyses and powder X-ray
diffraction indicated that the strong aerogel monoliths made with the 1,3-epoxides are made
up predominately of polycrystalline β-FeOOH, akaganeite, and those made with the 1,2-epoxides are amorphous. To our knowledge, this is first known report of synthesis and
characterization of akaganeite aerogel materials. Transmission electron microscopy analysis
indicates that aerogels derived using 1,3-epoxides have a microstructure made up of a highly
reticulated network of fibers with diameters from ∼5 to 35 nm and lengths several times
that, whereas those resulting from the use of 1,2-epoxides consist of interconnected spherical
particles, whose diameters are 5−15 nm. The difference in microstructure results in each
type of aerogel displaying very distinct physical and mechanical properties. In particular,
the stiffness of the β-FeOOH aerogels is remarkable for a transition metal oxide aerogel.
Monolithic cylinders of β-FeOOH aerogel can be sintered at 515 °C, transforming to α-Fe2O3
without shattering.