To understand the textural properties of carbon replicas obtained from the charring of styryl-based LDH hybrid assemblies, the calcination process was carefully studied within a temperature domain between 500 and 700 °C. Supported by several characterizations such as nitrogen gas adsorption, X-ray diffraction recorded in situ, Raman and ESR, the drastic change in the porosity (micro- and meso-porosity) should be explained by the thermal process combined to the acid-leaching procedure responsible for the opening of the porosity and more specifically by the intimate mixing between the organic and inorganic components. Indeed, a temperature of 600 °C is found to ensure the carbonisation of the organic part, as well as supplying small inorganic particles. Their departure during the acid-leaching is believed to create the well defined mesoporosity, and higher temperatures of treatment induce a crystallisation of the particles, and ill defined mesopores for the relative carbon replica. The carbon replica is found to be reactive against fluorine gas, with a nominal uptake dependant of the temperature and of up to 1.0 F per carbon atom. The fluorination is highly deleterious for the texture with a drastic decrease in the specific surface area. The higher the temperature of fluorination, the lower is the corresponding BET surface area. The mechanism of fluorination is studied by ESR and 19F solid state NMR. Against lithium ion the fluorinated carbon replicas exhibit an intricate electrochemical behavior, and an unexpected reversible process is observed at 2.5 V vs Li for the carbon replica fluorinated at 300 °C.
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