Modulation of the crystallinity of hydrogenated nitrogen-rich graphitic carbon nitrides

Denis Foy (1) , Gérard Demazeau (1) , Pierre Florian (2) , Dominique Massiot (2) , Christine Labrugère (1) , Graziella Goglio (1)

1 ICMCB - Institut de Chimie de la Matière Condensée de Bordeaux
2 CEMHTI - Conditions Extrêmes et Matériaux : Haute Température et Irradiation

An hydrogenated nitrogen-rich graphitic carbon nitride, structurally related to the theoretical graphitic phase of C3N4, has been synthesized in a bulk well-crystallized form. This new material was prepared by thermal decomposition of thiosemicarbazide up to 600 °C at ambient pressure under nitrogen flow. Its composition was determined by elemental combustion analysis. Powder X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy and C13 MAS NMR characterizations were performed. This material can be schematically described with a two-dimensional framework and a composition close to C3N4.17H1.12. In this nitrogen-rich material, C3N3 voids are fully occupied by water molecules which are strongly trapped into the material. A loss of crystallinity associated with a modification of the thermal behavior is observed when the amount of trapped molecules decreases in the graphitic material, order being damaged both between and in the graphitic planes.

Mots clés: Carbon nitride; Graphitic materials; X-ray diffraction (XRD); Nuclear magnetic resonance (NMR); X-ray photoelectron spectroscopy (XPS); Thermogravimetric analysis (TGA); Triazine; Heptazine

Domaines: Matériaux

Denis Foy, Gérard Demazeau, Pierre Florian, Dominique Massiot, Christine Labrugère, et al.. Modulation of the crystallinity of hydrogenated nitrogen-rich graphitic carbon nitrides. Journal of Solid State Chemistry, 2009, 182 (1), pp.165-171. ⟨10.1016/j.jssc.2008.10.018⟩. ⟨hal-00351466⟩