Estimation of the in-situ elastic constants of wood pulp fibers in freely dried paper via AFM experiments

Atomic force microscopy-based nanoindentation (AFM-NI) enables characterization of the basic mechanical properties of wood pulp fibers in conditions representative of the state inside a paper sheet. Determination of the mechanical properties under different loads is critical for the success of increasingly advanced computational models to understand, predict and improve the behavior of paper and paperboard. Here, AFM-NI was used to indent fibers transverse to and along the longitudinal axis of the fiber. Indentation moduli and hardness were obtained for relative humidity from 25 % to 75 %. The hardness and the indentation modulus exhibit moisture dependency, decreasing by 75 % and 50 %, respectively, over the range tested. The determined indentation moduli were combined with previous work to estimate the longitudinal and transverse elastic modulus of the fiber wall. Due to the relatively low indentation moduli, the elastic constants are also low compared to values obtained via single fiber testing

Design of Friction, Morphology, Wetting, and Protein Affinity by Cellulose Blend Thin Film Composition

Cellulose derivate phase separation in thin films was applied to generate patterned films with distinct surface morphology. Patterned polymer thin films are utilized in electronics, optics, and biotechnology but films based on bio-polymers are scarce. Film formation, roughness, wetting, and patterning are often investigated when it comes to characterization of the films. Frictional properties, on the other hand, have not been studied extensively. We extend the fundamental understanding of spin coated complex cellulose blend films via revealing their surface friction using Friction Force Microscopy (FFM). Two cellulose derivatives were transformed into two-phase blend films with one phase comprising trimethyl silyl cellulose (TMSC) regenerated to cellulose with hydroxyl groups exposed to the film surface. Adjusting the volume fraction of the spin coating solution resulted in variation of the surface fraction with the other, hydroxypropylcellulose stearate (HPCE) phase. The film morphology confirmed lateral and vertical separation and was translated into effective surface fraction. Phase separation as well as regeneration contributed to the surface morphology resulting in roughness variation of the blend films from 1.1 to 19.8 nm depending on the film composition. Friction analysis was successfully established, and then revealed that the friction coefficient of the films could be tuned and the blend films exhibited lowered friction force coefficient compared to the single-component films. Protein affinity of the films was investigated with bovine serum albumin (BSA) and depended mainly on the surface free energy (SFE) while no direct correlation with roughness or friction was found. BSA adsorption on film formed with 1:1 spinning solution volume ratio was an outlier and exhibited unexpected minimum in adsorption

How the Test Setup Can Affect Single Fiber Tensile Testing

ABSTRACTTensile testing is the most common method to investigate natural fibers. The fibers’ mechanical behavior can be considered non-linear and is influenced by viscoelasticity, plasticity, and environmental conditions. Very often such fibers are tested by gluing them with an adhesive onto a sample holder. Such a system consisting of a polymeric sample holder, adhesive, and natural fiber is complex and there is a risk that the mechanical response measured is a mix of the different contributions of those components. In this work, the key components for tensile testing of natural fibers ‒ sample holder and adhesive ‒ are investigated, to determine their influence on the measurement results. In order to isolate the influence of the measurement setup, the natural fiber is replaced with a platinum wire, which is purely linear-elastic. Hence all non-linear contributions from sample holder or adhesive can be identified. The main influence factor on the results was the glue used for fixating the fiber on the sample holder. Epoxy resin was found to be best suited. Taking these findings into account, a series of tensile tests was performed on cellulose-based natural fibers for demonstration but is applicable to any natural fiber

Design of Friction, Morphology, Wetting, and Protein Affinity by Cellulose Blend Thin Film Composition

Cellulose derivate phase separation in thin films was applied to generate patterned films with distinct surface morphology. Patterned polymer thin films are utilized in electronics, optics, and biotechnology but films based on bio-polymers are scarce. Film formation, roughness, wetting, and patterning are often investigated when it comes to characterization of the films. Frictional properties, on the other hand, have not been studied extensively. We extend the fundamental understanding of spin coated complex cellulose blend films via revealing their surface friction using Friction Force Microscopy (FFM). Two cellulose derivatives were transformed into two-phase blend films with one phase comprising trimethyl silyl cellulose (TMSC) regenerated to cellulose with hydroxyl groups exposed to the film surface. Adjusting the volume fraction of the spin coating solution resulted in variation of the surface fraction with the other, hydroxypropylcellulose stearate (FIPCE) phase. The film morphology confirmed lateral and vertical separation and was translated into effective surface fraction. Phase separation as well as regeneration contributed to the surface morphology resulting in roughness variation of the blend films from 1.1 to 19.8nm depending on the film composition. Friction analysis was successfully established, and then revealed that the friction coefficient of the films could be tuned and the blend films exhibited lowered friction force coefficient compared to the single-component films. Protein affinity of the films was investigated with bovine serum albumin (BSA) and depended mainly on the surface free energy (SFE) while no direct correlation with roughness or friction was found. BSA adsorption on film formed with 1:1 spinning solution volume ratio was an outlier and exhibited unexpected minimum in adsorption

Comprehensive investigation of the viscoelastic properties of PMMA by nanoindentation

Instrumented nanoindentation (NI) was used to examine the viscoelastic properties of poly(methyl methacrylate) (PMMA) as an amorphous polymer model. An evaluation combining adhesive contact and empiric spring–dashpot models has been applied to obtain the instantaneous elastic modulus E0 and the infinitely elastic modulus E∞ from nanoindentation creep curves. The value of E0 has been compared to moduli obtained with atomic force microscopy-based nanoindentation (AFM-NI) and compression tests. Furthermore, the elastic modulus has been evaluated by the method introduced by Oliver and Pharr (O&P) for the NI and AFM-NI results. Comparison of the elastic modulus E0 from the creep measurements of NI and AFM-NI to compression tests reveals good agreement of the results. However, only the O&P based AFM-NI results yield to lower values

Distributed Bragg Reflectors: Morphology of Cellulose Acetate and Polystyrene Multilayers

The optical quality and photonic properties of all-polymer distributed Bragg reflectors are related to the morphology of the layers and the optical responses of the materials. We introduce the X-ray reflectivity method to determine the thickness, the interface- and surface-roughness of cellulose acetate and polystyrene layers which are two polymers often used in the domain of spin casted multilayer systems. Atomic force microscopy and spectroscopic ellipsometry were used as complementary techniques for investigating the surface roughness and the film thickness. The shrinkage and the change of interface roughness of the polymers were investigated up to temperatures of 200 degrees C. Up to 170 degrees C the interface roughness stays constant at about 1 nm while it increases up to 2 nm at 200 degrees C. The thickness of the polystyrene layer remains constant up to 170 degrees C, well above its glass transition temperature T-g. For cellulose acetate a monothonic decrease is observed with increasing temperature. It could be shown, that the change in the optical response of a thermally treated distributed Bragg reflector is related to the change of the layer thickness of cellulose acetate. Spectra of (PS CA)(20)PS distributed Bragg reflectors (DBR) are in a good agreement with calculated spectra with parameters optained from of the X-ray reflectivity measurements

Assessing Fire-Damage in Historical Papers and Alleviating Damage with Soft Cellulose Nanofibers

Funding Information: The authors thank Prof. Dr. Banik for helpful discussions. Dr. Bacher and Dr. Schiehser are acknowledged for practical support (NMR and GPC). Special thanks to P. Reindl for the AFM measurements. L.V. would like to thank Klassik Stiftung Weimar and the doctoral school ABC&M for financial support. The financial support of the Austrian Biorefinery Center Tulln (ABCT), the Austrian Federal Ministry for Digital and Economic Affairs, and the National Foundation for Research Technology and Development is gratefully acknowledged. The authors are grateful to Borregaard (Norway) and SAPPI (Belgium) for donating CNF. Publisher Copyright: © 2022 The Authors. Small published by Wiley-VCH GmbHThe conservation of historical paper objects with high cultural value is an important societal task. Papers that have been severely damaged by fire, heat, and extinguishing water, are a particularly challenging case, because of the complexity and severity of damage patterns. In-depth analysis of fire-damaged papers, by means of examples from the catastrophic fire in a 17th-century German library, shows the changes, which proceeded from the margin to the center, to go beyond surface charring and formation of hydrophobic carbon-rich layers. The charred paper exhibits structural changes in the nano- and micro-range, with increased porosity and water sorption. In less charred areas, cellulose is affected by both chain cleavage and cross-linking. Based on these results and conclusions with regard to adhesion of auxiliaries, a stabilization method is developed, which coats the damaged paper with a thin layer of cellulose nanofibers. It enables the reliable preservation of the paper and—most importantly—retrieval ofthe contained historical information: the nanofibers form a flexible, transparent film on the surface and adhere strongly to the damaged matrix, greatly reducing its fragility, giving it stability, and enabling digitization and further handling.Peer reviewe

Gas Permeation, Mechanical Behavior and Cytocompatibility of Ultrathin Pure and Doped Diamond-Like Carbon and Silicon Oxide Films

Protective ultra-thin barrier films gather increasing economic interest for controlling permeation and diffusion from the biological surrounding in implanted sensor and electronic devices in future medicine. Thus, the aim of this work was a benchmarking of the mechanical oxygen permeation barrier, cytocompatibility, and microbiological properties of inorganic ~25 nm thin films, deposited by vacuum deposition techniques on 50 µm thin polyetheretherketone (PEEK) foils. Plasma-activated chemical vapor deposition (direct deposition from an ion source) was applied to deposit pure and nitrogen doped diamond-like carbon films, while physical vapor deposition (magnetron sputtering in pulsed DC mode) was used for the formation of silicon as well as titanium doped diamond-like carbon films. Silicon oxide films were deposited by radio frequency magnetron sputtering. The results indicate a strong influence of nanoporosity on the oxygen transmission rate for all coating types, while the low content of microporosity (particulates, etc.) is shown to be of lesser importance. Due to the low thickness of the foil substrates, being easily bent, the toughness as a measure of tendency to film fracture together with the elasticity index of the thin films influence the oxygen barrier. All investigated coatings are non-pyrogenic, cause no cytotoxic effects and do not influence bacterial growth