Production of graphene nanosheets by supercritical CO2 process coupled with micro-jet exfoliation

A facile and cost-effective method which combines supercritical CO₂ and micro-jet exfoliation has been developed for producing graphene nanosheets with high-quality. CO₂ molecules can intercalate into the interlayer of graphite because of their high diffusivity and small molecule size in supercritical operation. The tensile stress induced by graphite interfacial reflection of compressive waves exert on the graphite flakes, which lead to further exfoliation of graphite. Scanning electron microscope (SEM), transmission electron microscope (TEM), atomic force microscopy (AFM), Raman spectrum and X-ray diffraction (XRD) are used to identify morphology and quality of the exfoliated graphene nanosheets, which reveal that the graphite was successfully exfoliated into graphene and more than 88% of graphene nanosheets are less than three layers. The yield of graphene nanosheets is about 28 wt% under optimum conditions, which can be greatly improved by repeated exfoliation of the graphene sediment. The pure graphene film has a high conductivity of 2.1 × 10⁵ S/m.