The present study highlights the reactivity of carbon nanofibers (CNFs) with fluorine gas. Highly
purified and graphitized CNFs were treated under a stream of fluorine gas for 16 h at temperatures
ranging from 380 to 480 °C. Different fluorination temperature zones have been revealed by direct
physicochemical analysis such as XRD, Raman spectroscopy, EPR, and solid-state NMR (13C and 19F).
The comparison between various parameters such as covalence of C−F bond, T
1 spin−lattice nuclear
relaxation time, density, and environment of the dangling bonds, among others, allows the fluorination
mechanism to be determined, i.e., the formation of (C2F)
n
type graphite fluoride as the precursor of
richer (CF)
n
compound. This is supported by TEM characterization as the fluorination proceeds from the
external parts of the carbon nanofibers and then propagates through the core without a major structural
change of the fluorinated parts. A low exfoliation of the sheets is necessary for extended fluorination
and conversion into (CF)
n
; this occurs for fluorination temperatures higher than 472 °C, with concomitant
disappearance of the graphitic structure.
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