Raman spectra were acquired in situ during tensile straining of mechanically isolated fibers of spruce latewood. Stress-strain curves were evaluated along with band positions and intensities to monitor molecular changes due to deformation. Strong correlations (r = 0.99) were found between the shift of the band at 1097 cm(-1) corresponding to the stretching of the cellulose ring structure and the applied stress and strain. High overall shifts (-6.5 cm(-1)) and shift rates (-6.1 cm(-1)/GPa) were observed. After the fiber failed, the band was found on its original position again, proving the elastic nature of the deformation. Additionally, a decrease in the band height ratio of the 1127 and 1097 cm(-1) bands was observed to go hand in hand with the straining of the fiber. This is assumed to reflect a widening of the torsion angle of the glycosidic C-O-C bonding. Thus, the 1097 cm(-1) band shift and the band height ratio enable one to follow the stretching of the cellulose at a molecular level, while the lignin bands are shown to be unaffected. Observed changes in the OH region are shown and interpreted as a weakening of the hydrogen-bonding network during straining. Future experiments on different native wood fibers with variable chemical composition and cellulose orientation and on chemically and enzymatically modified fibers will help to deepen the micromechanical understanding of plant cell walls and the associated macromolecules.
The formation mechanisms of complex BaSO(4) fiber bundles and cones in the presence of polyacrylate sodium salt via a bioinspired approach at ambient temperature in an aqueous environment are reported. These complex organic-inorganic hybrid structures assemble after heterogeneous nucleation of amorphous precursor particle aggregates on polar surfaces, and the crystallization area can be patterned. In contrast to earlier reports, three different mechanisms based on the oriented attachment of nanoparticles were revealed for the formation of typical fibrous superstructures depending on the supersaturation or on the number of precursor particles. (A) High supersaturation (S > 2): large amorphous aggregates stick to a polar surface, form fiber bundles after mesoscopic transformation and oriented attachment, and then form a narrow tip through polymer interaction. (B) Low supersaturation (S = 1.02-2): only a few fibers nucleate heterogeneously from a single nucleation spot, and amorphous particles stick to existing fibers, which results in the formation of a fiber bundle. (C) Vanishing supersaturation (S = 1-1.02): nucleation of a fiber bundle from a single nucleation spot with self-limiting repetitive growth as a result of the limited amount of building material. These growth processes are supported by time-resolved optical microscopy in solution, TEM, SEM, and DLS.
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