Characterization of TEMPO-oxidized cellulose nanofibers in aqueous suspension by small-angle X-ray scattering

Cellulose nanofibers, extracted from wood pulps using the (2,2,6,6-tetramethylpiperidine-1-yl)oxyl (TEMPO)-mediated oxidation method, are low-cost, sustainable and high-performance materials with potential usage in many applications. The structural information of these cellulose nanofibers in aqueous suspension was characterized by synchrotron small-angle X-ray scattering (SAXS). A simplified ribbon model having a near rectangular cross section was found to give the best fit to the SAXS results. The analytical expression of the ribbon model also led to a higher calculation efficiency compared with the more conventional parallelepiped model. The extracted structural information included the cross-section size and size distribution of the cellulose nanofibers. For example, for nanofibers prepared from the dried pulp of the maritime pine, the size-weighted averages of thickness and width were 3.2 and 12.7 nm, respectively, and the corresponding standard deviations were 2.2 and 5.5 nm, respectively. The scattering results of the size-weighted average of the nanofiber width are also consistent with those determined directly from transmission electron microscopy.