Abstract
Solid state nuclear magnetic resonance (ssNMR) is a powerful and attractive characterization method for obtaining insights into the chemical structure and dynamics of a wide range of materials. Current interest in cellulose-based materials, as sustainable and renewable natural polymer products, requires deep investigation and analysis of the chemical structure, molecular packing, end chain motion, functional modification, and solvent–matrix interactions, which strongly dictate the final product properties and tailor their end applications. In comparison to other spectroscopic techniques, on an atomic level, ssNMR is considered more advanced, especially in the structural analysis of cellulose-based materials; however, due to a dearth in the availability of a broad range of pulse sequences, and time consuming experiments, its capabilities are underestimated. This critical review article presents the comprehensive and up-to-date work done using ssNMR, including the most advanced NMR strategies used to overcome and resolve the structural difficulties present in different types of cellulose-based materials.
Highlights
Accepted: 2 March 2022Current environmental constraints, along with the depletion of fossil fuels, necessitate the usage of greener materials in society [1,2]
We have reviewed the most advanced NMR strategies and pulse sequences used in studying cellulose-based materials and highlighted the benefits gained from the usage of every set of pulse sequences
Advanced in-situ NMR experiments can be highlighted as promising for cellulose-based materials, such as variable temperature T1, T2 relaxation and linewidth analysis used for studying polymorphism, polymeric chain dynamics, and water–matrix interactions; advanced water-edited 1D 13 C and 2D 13 C-13 C
Summary
Along with the depletion of fossil fuels, necessitate the usage of greener materials in society [1,2]. Among the techniques that have been widely used to determine the degree of crystallinity of cellulose-based materials is X-ray diffraction (XRD) [38–40]. This technique was applied to cellulose crystallites present in flax textile fibers [38]. NMR, from a low resolution out of sight technique into an indispensable one for structural and dynamic determination of a wide range of materials in different physical states [42]. The emerging orientation-dependent nuclear magnetic interactions in solid states are formed due to the restricted thermal motions and lack of rapid molecular tumbling This poor dynamical motion unveils different types of internuclear and orientation-dependent nuclear interactions, which hold detailed information on the local geometric and electronic structure [44–46]. (a)(a) cross polarization, tion, where magnetization is transferred from a high natural abundance and gyromagwhere magnetization is transferred from a high natural abundance and gyromagnetic ratio
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