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.
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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