The X-ray, Raman and TEM Signatures of Cellulose-Derived Carbons Explained

• Published in: C (Basel) Vol. 8; no. 1; pp. 4 - 19
• Main Authors: Mubari, Petros Kasaira, Beguerie, Théotime, Monthioux, Marc, Weiss-Hortala, Elsa, Nzihou, Ange, Puech, Pascal
• Format: Journal Article
• Language: English
• Published: Basel MDPI AG 01.01.2022; MDPI
• Subjects: Carbon; Carbonization; Cellulose; crystallite size; Crystallites; disorder; Domains; Engineering Sciences; Graphene; Graphite; Heat; Heating rate; High resolution electron microscopy; Point defects; Raman; Raman spectroscopy; Scattering angle; Size distribution; Spectrum analysis; X-ray diffraction; XRD; disorder; cellulose; Raman; XRD; crystallite size; carbonization; HRTEM
• ISSN: 2311-5629; 2311-5629
• DOI: 10.3390/c8010004

Structural properties of carbonized cellulose were explored to conjugate the outcomes from various characterization techniques, namely X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy. All these techniques have evidenced the formation of graphene stacks with a size distribution. Cellulose carbonized at 1000 and 1800 °C at a heating rate of 2 °C/min showed meaningful differences in Raman spectroscopy, whereas in XRD, the differences were not well pronounced, which implies that the crystallite sizes calculated by each technique have different significations. In the XRD patterns, the origin of a specific feature at a low scattering angle commonly reported in the literature but poorly explained so far, was identified. The different approaches used in this study were congruous in explaining the observations that were made on the cellulose-derived carbon samples. The remnants of the basic structural unit (BSU) are developed during primary carbonization. Small graphene-based crystallites inherited from the BSUs, which formerly developed during primary carbonization, were found to coexist with larger ones. Even if the three techniques give information on the average size of graphenic domains, they do not see the same characteristics of the domains; hence, they are not identical, nor contradictory but complementary. The arguments developed in the work to explain which characteristics are deduced from the signal obtained by each of the three characterization techniques relate to physics phenomena; hence, they are quite general and, therefore, are valid for all kind of graphenic materials.