Use of Fourier Series in X-ray Diffraction (XRD) Analysis and Fourier-Transform Infrared Spectroscopy (FTIR) for Estimation of Crystallinity in Cellulose from Different Sources

• Published in: Polymers 2022-11, Vol.14 (23), p.5199
• Main Authors: Montoya-Escobar, Nicolás, Ospina-Acero, Daniel, Velásquez-Cock, Jorge Andrés, Gómez-Hoyos, Catalina, Serpa Guerra, Angélica, Gañan Rojo, Piedad Felisinda, Vélez Acosta, Lina Maria, Escobar, Juan Pablo, Correa-Hincapié, Natalia, Triana-Chávez, Omar, Zuluaga Gallego, Robin, Stefani, Pablo M
• Format: Article
• Language: English
• Subjects: Cellulose; Crystallinity; Crystallization; Deconvolution; Fourier series; Fourier transforms; Homogenization; Infrared analysis; Infrared spectroscopy; Methods; NMR; Nuclear magnetic resonance; Software; Spectrum analysis; X-ray diffraction
• ISSN: 2073-4360; 2073-4360
• DOI: 10.3390/polym14235199

Cellulose crystallinity can be described according to the crystal size and the crystallinity index (CI). In this research, using Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) methods, we studied the crystallinity of three different types of cellulose: banana rachis (BR), commercial cellulose (CS), and bacterial cellulose (BC). For each type of cellulose, we analyzed three different crystallization grades. These variations were obtained using three milling conditions: 6.5 h, 10 min, and unmilled (films). We developed a code in MATLAB software to perform deconvolution of the XRD data to estimate CI and full width at half-maximum (FWHM). For deconvolution, crystalline peaks were represented with Voigt functions, and a Fourier series fitted to the amorphous profile was used as the amorphous contribution, which allowed the contribution of the amorphous profile to be more effectively modeled. Comparisons based on the FTIR spectra and XRD results showed there were no compositional differences between the amorphous samples. However, changes associated with crystallinity were observed when the milling time was 10 min. The obtained CI (%) values show agreement with values reported in the literature and confirm the effectiveness of the method used in this work in predicting the crystallization aspects of cellulose samples.