NMR Characterization of Graphene Oxide-Doped Carbon Aerogel in a Liquid Environment

In this study, we report the findings of a morphological analysis of a resorcinol-formaldehyde (RF)-based carbon aerogel (CA) and its graphene oxide (GO)-doped version (CA-GO), prepared for possible applications as an electrode material. Beyond some electron microscopic and N₂ sorption investigations, we mostly used NMR cryoporometry and relaxometry to characterize the gels in a wet state, as they are usually applied. The precursor RF polymer aerogel was prepared both with and without GO and was subsequently carbonized into carbon aerogel. Modifying the polymer aerogel using GO resulted in a larger variety of C-O bonds in both polymer aerogels. However, the most important changes occurred in the morphology of the carbon aerogels. NMR relaxometry revealed the highly hydrophilic nature of the pore wall of the RF polymer aerogels, as demonstrated by their uniform wetting behavior. The carbonization resulted in a mostly hydrophobic pore wall decorated by some oxygen-containing spots and a macroporous system. Doping with GO after pyrolysis resulted in spherical pores in the CA and cylindrical pores in the CA-GO, which is potentially a more promising material for electrochemical use than CA.