We report the synthesis of ultra-low-density three-dimensional macroassemblies of graphene sheets that exhibit high electrical conductivities and large internal surface areas. These materials are prepared as monolithic solids from suspensions of single-layer graphene oxide in which organic sol-gel chemistry is used to cross-link the individual sheets. The resulting gels are supercritically dried and then thermally reduced to yield graphene aerogels with densities approaching 10 mg/cm(3). In contrast to methods that utilize physical cross-links between GO, this approach provides covalent carbon bonding between the graphene sheets. These graphene aerogels exhibit an improvement in bulk electrical conductivity of more than 2 orders of magnitude (∼1 × 10(2) S/m) compared to graphene assemblies with physical cross-links alone (∼5 × 10(-1) S/m). The graphene aerogels also possess large surface areas (584 m(2)/g) and pore volumes (2.96 cm(3)/g), making these materials viable candidates for use in energy storage, catalysis, and sensing applications.

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.

Alumina aerogels were prepared through the addition of propylene oxide to aqueous or ethanolic solutions of hydrated aluminum salts, AlCl 3 •6H 2 O or Al(NO 3) 3 •9H 2 O, followed by drying with supercritical CO 2. This technique affords low-density (60-130 kg/m 3), high surface area (600-700 m 2 /g) alumina aerogel monoliths without the use of alkoxide precursors. The dried alumina aerogels were characterized using elemental analysis, highresolution transmission electron microscopy, powder X-ray diffraction, solid state NMR, acoustic measurements and nitrogen adsorption/desorption analysis. Powder X-ray diffraction and TEM analysis indicated that the aerogel prepared from hydrated AlCl 3 in water or ethanol possessed microstructures containing highly reticulated networks of pseudoboehmite fibers, 2-5 nm in diameter and of varying lengths, while the aerogels prepared from hydrated Al(NO 3) 3 in ethanol were amorphous with microstructures comprised of interconnected spherical particles with diameters in the 5-15 nm range. The difference in microstructure resulted in each type of aerogel displaying distinct physical and mechanical properties. In particular, the alumina aerogels with the weblike microstructure were far more mechanically robust than those with the colloidal network, based on acoustic measurements. Both types of alumina aerogels can be transformed to γ-Al 2 O 3 through calcination at 800 o C without a significant loss in surface area or monolithicity.

We describe the fabrication of ultralow-density carbon nanotube (CNT) foams that simultaneously exhibit high electrical conductivities and robust mechanical properties. Our approach utilizes carbon nanoparticles as a binder to crosslink randomly oriented bundles of single-walled CNTs. The resulting CNT foams are the stiffest low-density nanoporous solids reported and exhibit elastic behavior up to strains as large as ∼80%. The use of the carbon binder also allows bulk electrical conductivity to be maintained at low densities.

The plastic deformation of nanoporous Au under compressive stress was studied by depth-sensing nanoindentation combined with scanning electron microscope characterization. The nanoporous Au investigated in the current study exhibits a relative density of 42%, and a spongelike morphology of interconnecting ligaments on a length scale of ϳ100 nm. The material is polycrystalline with a grain size on the order of 10-60 nm. Microstructural characterization of residual indentation impressions reveals a localized densification via ductile (plastic) deformation under compressive stress and demonstrates the ductile behavior of Au ligaments. A mean hardness of 145͑±11͒ MPa and a Young's modulus of 11.1͑±0.9͒ GPa was obtained from the analysis of the load-displacement curves. The hardness of investigated np-Au is ϳ10 times higher than the hardness predicted by scaling laws of open-cell foams thus potentially opening a door to a class of high yield strengthlow-density materials.