Résumé : Multilayer carbonaceous nanomaterial has been synthesized using a two-step process: carbon nanodiscs/nanocones were fluorinated using either the direct reaction with pure F 2 gas or the thermal decomposition of solid fluorinating agent (TbF 4). Then the fluorinated parts were removed by treatment at 600 °C in air. When the fluorine atoms are homogenously dispersed, using fluorination by TbF 4, thinning due to thermal defluorination results in multilayer materials with 7-10 nm of thickness and 400-500 nm of width. Such resulting materials and the fluorinated precursors have been characterized by solid state NMR, TGA, XRD, SEM, TEM, AFM and Raman spectroscopy. © 2012 Elsevier Ltd. All rights reserved.