By employing honeycomb GO with large surface area as the starting materials and using elemental fluorine, we developed a novel, straightforward topotactic route toward highly fluorinated graphene in really large quantities at low temperature. The value of F/C molar ratio approaches to 1.02. Few-layer fluorinated graphene sheets are obtained, among which the yield of monolayered FG sheet is about 10% and the number of layers is mainly in the range of 2-5. Variations in morphology and chemical structure of fluorinated graphene were explored, and some physical properties were reported.

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Pristine and oxidized multiwalled carbon nanotubes (MWCNTs) were separately prepared and directly fluorinated with F2 through two different routes: heating-fluorination and isothermal-fluorination. The amount of fluorine atoms (hereinafter referred to as “F-content”) bonding to the fluorinated samples was largely dependent on the modifing route and chemical bonding of MWCNTs. The F-content of heating-fluorinated pristine and oxidized MWCNTs was 3.2% and 9.2% respectively, which were about 8 times and 18 times that of the corresponding isothermal-fluorinated MWCNTs. According to structural analysis of samples before and after fluorination, it was found that thermal elimination of oxygen-related groups bonding to MWCNTs contributed to the formation of strongly covalent C–F bonds during heating-fluorination. It was considered that the oxygen-related groups provided reactive sites for the fluorination. The fluorination reaction took place at an sp3 carbon linking with the oxygen-related groups and did not increase the density of defect on MWCNTs. A radical-mediated mechanism is accepted for this reaction. Thus, MWCNTs could be first oxidized to increase the number of oxygen-related groups and then heating-fluorinated by F2 directly to get highly fluorinated MWCNTs with stable C–F bonds.

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