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A hardwood dissolving pulp and bleached softwood Kraft pulp were subjected to continuous ultrasonic cavitation assisted TEMPO-mediated oxidation. The effects of such processing on the yield of carboxylic groups, morphological changes of the fibers as well as the effects on the final nanocellulose dispersion were studied. Ultrasonic cavitation in the TEMPO-mediated oxidation phase enhanced the yield of carboxylic groups on both pulps while having a negligible effect on materials losses due to fiber fines formation. The effect of ultrasonic cavitation was purely mechanical and acted as an additional high-shear mixer in the pre-treatment phase. As a result, the morphological changes on the fibers were enhanced, with additional swelling and fiber straightening being observed. Furthermore, the ultrasonic cavitation also influenced the properties of the nanocellulose dispersion obtained from subsequent microfluidization. The sonicated samples exhibited higher optical clarity, higher elasticity in gels while also having somewhat lower viscosities. On nanoscale, ultrasonic cavitation helped the subsequent microfluidization in releasing better individualized nanofibrils as they had smaller diameters than in non-sonicated samples. Sonication also had no effect on the crystallinity properties of the nanocellulose, the observed slight reduction was a result of intense microfluidization that was used to produce the nanocellulose dispersion. Ultrasonic cavitation in the TEMPO-oxidized pre-treatment phase was shown to be a method that can increase the throughput in lab-scale by mechanical activation of pulps and enabling shorter processing times for TEMPO-mediated oxidation. [GRAPHICS] .

Background : Biological materials have a complex, hierarchical structure, with vital structural features present at all size scales, from the nanoscale to the macroscale. A method that can connect information at multiple length scales has great potential to reveal novel information. This article presents one such method with an application to the bamboo culm wall. Moso (Phyllostachys edulis) bamboo is a commercially important bamboo species. At the cellular level, bamboo culm wall consists of vascular bundles embedded in a parenchyma cell tissue matrix. The microfibril angle (MFA) in the bamboo cell wall is related to its macroscopic longitudinal stiffness and strength and can be determined at the nanoscale with wide-angle X-ray scattering (WAXS). Combining WAXS with X-ray microtomography (XMT) allows tissue-specific study of the bamboo culm without invasive chemical treatment. Results : The scattering contribution of the fiber and parenchyma cells were separated with spatially-localized WAXS. The fiber component was dominated by a high degree of orientation corresponding to small MFAs (mean MFA 11 degrees). The parenchyma component showed significantly lower degree of orientation with a maximum at larger angles (mean MFA 65 degrees). The fiber ratio, the volume of cell wall in the fibers relative to the overall volume of cell wall, was determined by fitting the scattering intensities with these two components. The fiber ratio was also determined from the XMT data and similar fiber ratios were obtained from the two methods, one connected to the cellular level and one to the nanoscale. X-ray diffraction tomography was also done to study the differences in microfibril orientation between fibers and the parenchyma and further connect the microscale to the nanoscale. Conclusions : The spatially-localized WAXS yields biologically relevant, tissue-specific information. With the custommade bench-top set-up presented, diffraction contrast information can be obtained from pl