Abstract
Quick characterization methods to determine the structure of carbon materials are sought after for a wide array of technical applications. In this study we present the combined analysis of the structure of carbide-derived carbons (CDCs) with Raman spectroscopy and wide-angle X-ray scattering (WAXS) methods. We present the optimal deconvolution method to be used for the detailed analysis of Raman spectroscopy data of CDCs and comparison to corresponding WAXS results is made. For a broad set of CDCs both WAXS and Raman spectroscopy data showed that the average graphene layer extent increases with synthesis temperature of CDC, while the coherent domain lengths obtained from Raman spectroscopy higher by an average of 4.4 nm. In addition, the presence of correlations between the parameters (D-band width and the parameter A∑D/A∑G) from Raman spectroscopy and the synthesis temperature are established. Based on the WAXS and Raman spectra data analysis the strong influence of the precursor carbide structure on the graphitization pathway is shown.
Highlights
In the Wide-Angle X-ray Scattering (WAXS) patterns of the studied carbide-derived carbons (CDCs), there is a diffuse (002) reflection located at scattering vector modulus (The scattering vector modulus, q, is defined as q = 4π sin(θ)/λ, where 2θ is the scattering angle.), q, ~18 nm−1 and a diffuse asymmetric (10) reflection at q ~30 nm−1 (Figure 1, Figure S1 in Supplementary information, SI).The patterns are typical of non-graphitic carbon, since no well-expressed reflections can be seen and, were analyzed using the algorithm derived by Ruland and Smarsly [31], which is implemented in the CarbX software [32] (Figure 1)
The 5-peak fit of the Raman spectrum first order scattering region, suggested by Sadezky et al, obtained the most coherent results, i.e., the influence of the Tsyn on the peak parameters was the clearest. Results from both wide-angle X-ray scattering (WAXS) and Raman spectroscopy methods clearly showed the influence of the precursor carbide structure and chemical composition on stage of graphitization at equivalent synthesis temperature conditions
The graphitization of C-Mo2 C and C-VC at T = 1100 ◦ C was evident from the considerable narrowing of the G-band and from the increase in average stacking size, Lc, values obtained from the WAXS data
Summary
Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affiliations. Carbon materials are vital components to a multitude of applications, from energy storage and conversion to gas separation and filtration systems. In case of chemically pure carbons the suitability of a certain carbon material for a specific application is determined by its structural properties, e.g., porosity parameters, particle size and its distribution, level of graphitization, etc. For the use of a large variety of carbons in applications with different requirements for the structure of carbon it is vital to be able to characterize novel synthesized carbons with quick, relatively cheap, and available quantitative analytical methods
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