Abstract

The preparation of CFx by elemental fluorination of charcoal was studied using solid state 13C and 19F NMR spectroscopy. 19F−13C CP/MAS NMR experiments determine the extent of fluorination vs reaction temperature. Three types of carbon species observed over the temperature range −80 to 350 °C were assigned to graphitic carbon (C), CF, and CF2 on the basis of chemical shift. These assignments were confirmed by measurement of cross polarization and dipolar dephasing time constants, TCF and TDD, respectively. The fluorinated carbons fully cross-polarize in tenths of milliseconds, while polarization transfer among graphitic carbon is slower and is explained by a two-component model. One component, with TCF less than 1 ms, is assigned to sp2 carbons adjacent to fluorinated carbons, viz., interfacial graphitic carbon. The other component, with TCF on the order of milliseconds, is assigned to more remote carbon species, viz., bulk graphitic carbon. The concentrations of CF and CF2 found in the 19F−13C CP/MAS NMR...

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