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The mechanical properties of single fibres are highly important in the paper production process to produce and adjust properties for the favoured fields of application. The description of mechanical properties is usually characterised via linearized assumptions and is not resolved locally or spatially in three dimensions. In tensile tests or nanoindentation experiments on cellulosic fibres, only one mechanical parameter, such as elastic modulus or hardness, is usually obtained. To obtain a more detailed mechanical picture of the fibre, it is crucial to determine mechanical properties in depth. To this end, we discuss an atomic force microscopy-based approach to examine the local stiffness as a function of indentation depth via static force-distance curves. This method has been applied to linter fibres (extracted from a finished paper sheet) as well as to natural raw cotton fibres to better understand the influence of the pulp treatment process in paper production on the mechanical properties. Both types of fibres were characterised in dry and wet conditions with respect to alterations in their mechanical properties. Subsurface imaging revealed which wall in the fibre structure protects the fibre against mechanical loading. Via a combined 3D display, a spatially resolved mechanical map of the fibre interior near the surface can be established. Additionally, we labelled fibres with carbohydrate binding modules tagged with fluorescent proteins to compare the AFM results with fluorescence confocal laser scanning microscopy imaging. Nanomechanical subsurface imaging is thus a tool to better understand the mechanical behaviour of cellulosic fibres, which have a complex, hierarchical structure.

Modelling of single cellulose fibres is usually performed by assuming homogenous properties, such as strength and Young s modulus, for the whole fibre. Additionally, the inhomogeneity in size and swelling behaviour along the fibre is often disregarded. For better numerical models, a more detailed characterization of the fibre is required. Herein, we report a method based on atomic force microscopy to map these properties along the fibre. A fibre was mechanically characterized by static colloidal probe AFM measurements along the fibre axis. Thus, the contact stress and strain at each loading point can be extracted. Stress strain curves can be obtained along the fibre. Additionally, mechanical properties such as adhesion or dissipation can be mapped. The inhomogeneous swelling behaviour was recorded via confocal laser scanning microscopy along the fibre. Scanning electron microscopy measurements revealed the local macroscopic fibril orientation and provided an overview of the fibre topology. By combining these data, regions along the fibre with higher adhesion, dissipation, bending ability and strain or differences in the contact stress when increasing the relative humidity could be identified. This combined approach allows for one to obtain a detailed picture of the mechanical properties of single fibres.

Paper materials are natural composite materials and well-known to be hydrophilic unless chemical and mechanical processing treatments are undertaken. The relative humidity impacts the fiber elasticity, the fiber-fiber bonds and the failure mechanism. In this work, we present a comprehensive experimental and computational study on the mechanical and failure behaviour of the fiber and the fiber network under humidity influence. The manually extracted cellulose fiber is exposed to different levels of humidity, and then mechanically characterized using Atomic Force Microscopy, which delivers the humidity dependent longitudinal Young's modulus. The obtained relationship allows calculation of fiber elastic modulus at any humidity level. Moreover, by using Confoncal Laser Scanning Microscopy, the coefficient of hygroscopic expansion of the fibers is determined. On the other hand, we present a finite element model to simulate the deformation and the failure of the fiber network. The model includes the fiber anisotropy and the hygroscopic expansion using the experimentally determined constants. In addition, it regards the fiber-fiber bonding and damage by using a humidity dependent cohesive zone interface model. Finite element simulations on exemplary fiber network samples are performed to demonstrate the influence of different aspects including relative humidity and fiber-fiber bonding parameters on the mechanical features such as force-elongation curves, wet strength, extensiability and the local fiber-fiber debonding. In meantime, fiber network failure in a locally wetted region is revealed by tracking of individually stained fibers using in-situ imaging techniques. Both the experimental data and the cohesive finite element simulations demonstrate the pull-out of fibers and imply the significant role of the fiber-fiber debonding in the failure process of the wet paper., Comment: 21 pages,11 figures

Polymer coatings on cellulosic fibres are widely used to enhance the natural fibre properties by improving, for example, the hydrophobicity and wet strength. Here, we investigate the effects of a terpolymer P(S-co-MABP-co-PyMA) coating on cotton linters and eucalyptus fibres to improve the resistance of cellulose fibres against wetness. Coated and uncoated fibres were characterised by using scanning electron microscopy, contact angle measurements, Raman spectroscopy and atomic force microscopy with the objective of correlating macroscopic properties such as the hydrophobicity of the fleece with microscopic properties such as the coating distribution and local nanomechanics. The scanning electron and fluorescence microscopy results revealed the distribution of the coating on the paper fleeces and fibres. Contact angle measurements proved the hydrophobic character of the coated fleece, which was also confirmed by Raman spectroscopy measurements that investigated the water uptake in single fibres. The water uptake also induced a change in the local mechanical properties, as measured by atomic force microscopy. These results verify the basic functionality of the hydrophobic coating on fibres and paper fleeces but call into question the homogeneity of the coating., Comment: 24 pages, 5 figures, submitted