Résumé : Room temperature graphite fluorides consisting of raw material and samples post-treated in pure fluorine atmosphere in the temperature range 100-500 °C have been studied by solid-state NMR. Several NMR approaches have been used, both high and low-field 19F, 19F MAS and 13C MAS with 19F to 13C cross polarization. The modifications, in the graphitic lattice, of the catalytic iodine fluorides products have been examined. A transformation of the C-F bond character from semi-ionic to covalent has been found to occur at a post-treatment temperature close to 400 °C. It is shown that covalency increases with temperature.