Interactions of single and multi-layer graphene oxides with water, methane, organic solvents and HCl studied by 1H NMR

Contemporary characterisation techniques for graphenes are often performed for samples in a dried state or vacuum, which can lead to significant structural changes and difficulty in assessing the actual physical or physicochemical characteristics of graphenes in a colloid state. The interfacial phenomena between water or mixtures (of water with benzene, methane, or HCl) bound to single-layer graphene oxide (SLGO) and multi-layer graphene oxide (MLGO) in different dispersion media (CDCl3, CCl4, CDCl3/DMSO, air) were studied using low-temperature (200-280 K) 1H NMR spectroscopy. Use of the NMR cryoporometry method allows determination of the textural characteristics of SLGO and MLGO depending on their hydration degree. It was found that SLGO in diluted suspensions is more agglomerated after freezing-thawing. This effect could be assigned to cryogelation of carbon sheets leading to a decrease in the specific surface area (from 1841 to 533 m2/g) representing the area of sheets that are accessible for water that is unfrozen at subzero temperatures. The results obtained show that the cryoporometry method is appropriate for the investigation of the texture of both wetted and suspended graphene oxides.