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- ItemDry-jet wet spinning of thermally stable lignin-textile grade polyacrylonitrile fibers regenerated from chloride-based ionic liquids compounds(Basel : MDPI, 2020) Al Aiti, Muhannad; Das, Amit; Kanerva, Mikko; Järventausta, Maija; Johansson, Petri; Scheffler, Christina; Göbel, Michael; Jehnichen, Dieter; Brünig, Harald; Wulff, Lucas; Boye, Susanne; Arnhold, Kerstin; Kuusipalo, Jurkka; Heinrich, GertIn this paper, we report on the use of amorphous lignin, a waste by-product of the paper industry, for the production of high performance carbon fibers (CF) as precursor with improved thermal stability and thermo-mechanical properties. The precursor was prepared by blending of lignin with polyacrylonitrile (PAN), which was previously dissolved in an ionic liquid. The fibers thus produced offered very high thermal stability as compared with the fiber consisting of pure PAN. The molecular compatibility, miscibility, and thermal stability of the system were studied by means of shear rheological measurements. The achieved mechanical properties were found to be related to the temperature-dependent relaxation time (consistence parameter) of the spinning dope and the diffusion kinetics of the ionic liquids from the fibers into the coagulation bath. Furthermore, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dynamic mechanical tests (DMA) were utilized to understand in-depth the thermal and the stabilization kinetics of the developed fibers and the impact of lignin on the stabilization process of the fibers. Low molecular weight lignin increased the thermally induced physical shrinkage, suggesting disturbing effects on the semi-crystalline domains of the PAN matrix, and suppressed the chemically induced shrinkage of the fibers. The knowledge gained throughout the present paper allows summarizing a novel avenue to develop lignin-based CF designed with adjusted thermal stability.
- ItemA Polymer for Application as a Matrix Phase in a Concept of In Situ Curable Bioresorbable Bioactive Load-Bearing Continuous Fiber Reinforced Composite Fracture Fixation Plates(Basel : MDPI, 2021) Plyusnin, Artem; He, Jingwei; Elschner, Cindy; Nakamura, Miho; Kulkova, Julia; Spickenheuer, Axel; Scheffler, Christina; Lassila, Lippo V. J.; Moritz, NikoThe use of bioresorbable fracture fixation plates made of aliphatic polyesters have good potential due to good biocompatibility, reduced risk of stress-shielding, and eliminated need for plate removal. However, polyesters are ductile, and their handling properties are limited. We suggested an alternative, PLAMA (PolyLActide functionalized with diMethAcrylate), for the use as the matrix phase for the novel concept of the in situ curable bioresorbable load-bearing composite plate to reduce the limitations of conventional polyesters. The purpose was to obtain a preliminary understanding of the chemical and physical properties and the biological safety of PLAMA from the prospective of the novel concept. Modifications with different molecular masses (PLAMA-500 and PLAMA-1000) were synthesized. The efficiency of curing was assessed by the degree of convergence (DC). The mechanical properties were obtained by tensile test and thermomechanical analysis. The bioresorbability was investigated by immersion in simulated body fluid. The biocompatibility was studied in cell morphology and viability tests. PLAMA-500 showed better DC and mechanical properties, and slower bioresorbability than PLAMA-1000. Both did not prevent proliferation and normal morphological development of cells. We concluded that PLAMA-500 has potential for the use as the matrix material for bioresorbable load-bearing composite fracture fixation plates.
- ItemDynamic Single-Fiber Pull-Out of Polypropylene Fibers Produced with Different Mechanical and Surface Properties for Concrete Reinforcement(Basel : MDPI, 2021) Wölfel, Enrico; Brünig, Harald; Curosu, Iurie; Mechtcherine, Viktor; Scheffler, ChristinaIn strain-hardening cement-based composites (SHCC), polypropylene (PP) fibers are often used to provide ductility through micro crack-bridging, in particular when subjected to high loading rates. For the purposeful material design of SHCC, fundamental research is required to understand the failure mechanisms depending on the mechanical properties of the fibers and the fiber–matrix interaction. Hence, PP fibers with diameters between 10 and 30 µm, differing tensile strength levels and Young’s moduli, but also circular and trilobal cross-sections were produced using melt-spinning equipment. The structural changes induced by the drawing parameters during the spinning process and surface modification by sizing were assessed in single-fiber tensile experiments and differential scanning calorimetry (DSC) of the fiber material. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and contact angle measurements were applied to determine the topographical and wetting properties of the fiber surface. The fiber–matrix interaction under quasi-static and dynamic loading was studied in single-fiber pull-out experiments (SFPO). The main findings of microscale characterization showed that increased fiber tensile strength in combination with enhanced mechanical interlocking caused by high surface roughness led to improved energy absorption under dynamic loading. Further enhancement could be observed in the change from a circular to a trilobal fiber cross-section.
- ItemElectrolytic Surface Treatment for Improved Adhesion between Carbon Fibre and Polycarbonate(Basel : MDPI, 2018) Kamps, Jan Henk; Henderson, Luke C.; Scheffler, Christina; Van der Heijden, Ruud; Simon, Frank; Bonizzi, Teena; Verghese, NikhilTo achieve good mechanical properties of carbon fibre-reinforced polycarbonate composites, the fibre-matrix adhesion must be dialled to an optimum level. The electrolytic surface treatment of carbon fibres during their production is one of the possible means of adapting the surface characteristics of the fibres. The production of a range of tailored fibres with varying surface treatments (adjusting the current, potential, and conductivity) was followed by contact angle, inverse gas chromatography and X-ray photoelectron spectroscopy measurements, which revealed a significant increase in polarity and hydroxyl, carboxyl, and nitrile groups on the fibre surface. Accordingly, an increase in the fibre-matrix interaction indicated by a higher interfacial shear strength was observed with the single fibre pull-out force-displacement curves. The statistical analysis identified the correlation between the process settings, fibre surface characteristics, and the performance of the fibres during single fibre pull-out testing.
- ItemSurface Treatment of Carbon Fibers by Oxy-Fluorination(Basel : MDPI, 2019) Kruppke, Iris; Scheffler, Christina; Simon, Frank; Hund, Rolf-Dieter; Cherif, ChokriIn this paper, the oxy-fluorination process and the influence of different concentrations of fluorine and oxygen in the gas phase on the physicochemical properties of polyacrylonitrile(PAN)-based carbon fibers are described. The properties of the treated carbon structures are determined by zeta potential and tensiometry measurements. In addition, changes in surface composition and morphology are investigated by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Adhesion properties are characterized by the single fiber pull-out (SFPO) test. Furthermore, changes in intrinsic properties are described by means of tensile and density measurements. After a primary desizing effect by oxy-fluorination, an increased number of oxygen-containing surface functional groups could be detected, which led to more debonding work in SFPOs with an epoxy-based matrix. It was also shown that the polar surface energy grows with rising fluorine concentration in the reaction gas mixture. In addition, a minor increase of ~10% in the maximum strength of PAN-based carbon fibers is detected by single fiber tensile measurements after oxy-fluorination with a fluorine content of 5% in the reaction mixture.
- ItemPolydopamine-Coated Paraffin Microcapsules as a Multifunctional Filler Enhancing Thermal and Mechanical Performance of a Flexible Epoxy Resin(Basel : MDPI, 2020) Fredi, Giulia; Zimmerer, Cordelia; Scheffler, Christina; Pegoretti, AlessandroThis work focuses on flexible epoxy (EP) composites containing various amounts of neat and polydopamine (PDA)-coated paraffin microcapsules as a phase change material (PCM), which have potential applications as adhesives or flexible interfaces with thermal management capability for electronics or other high-value-added fields. After PDA modification, the surface of PDA-coated capsules (MC-PDA) becomes rough with a globular appearance, and the PDA layer enhances the adhesion with the surrounding epoxy matrix, as shown by scanning electron microscopy. PDA deposition parameters have been successfully tuned to obtain a PDA layer with a thickness of 53 ± 8 nm, and the total PDA mass in MC-PDA is only 2.2 wt %, considerably lower than previous results. This accounts for the fact that the phase change enthalpy of MC-PDA is only marginally lower than that of neat microcapsules (MC), being 221.1 J/g and 227.7 J/g, respectively. Differential scanning calorimetry shows that the phase change enthalpy of the prepared composites increases with the capsule content (up to 87.8 J/g) and that the enthalpy of the composites containing MC-PDA is comparable to that of the composites with MC. Dynamic mechanical analysis evidences a decreasing step in the storage modulus of all composites at the glass transition of the EP phase, but no additional signals are detected at the PCM melting. PCM addition positively contributes to the storage modulus both at room temperature and above Tg of the EP phase, and this effect is more evident for composites containing MC-PDA. As the capsule content increases, the mechanical properties of the host EP matrix also increase in terms of elastic modulus (up to +195%), tensile strength (up to +42%), Shore D hardness (up to +36%), and creep compliance (down to −54% at 60 min). These effects are more evident for composites containing MC-PDA due to the enhanced interfacial adhesion.
- ItemPolymeric Coatings for AR-Glass Fibers in Cement-Based Matrices: Effect of Nanoclay on the Fiber-Matrix Interaction(Basel : MDPI, 2021) Bompadre, Francesca; Scheffler, Christina; Utech, Toni; Donnini, JacopoPolymeric coatings are widely used to enhance the load bearing capacity and chemical durability of alkali-resistant glass (AR-glass) textile in cement-based composites. The contact zone between coated yarns and concrete matrix plays a major role to enable the stress transfer and has still to be improved for the full exploitation of the mechanical behavior of the composite. As a new approach, this paper studies how the addition of nanoclay particles in the polymer coating formulation can increase the chemical bond between organic coating and inorganic matrix. This includes the description of the water-based coating preparation by dispersing sodium montmorillonites, whereby the resulting coating nanostructure is characterized by X-ray diffraction and energy dispersive X-ray spectroscopy. Single glass fibers were treated by dip-coating. Atomic force microscopy was used to determine the surface roughness, and the effect on the fiber tensile properties was studied. Moreover, the morphological and chemical characteristics of the coatings were compared with the results obtained from single fiber pull-out (SFPO) tests. It was shown that the incorporation of nanoclays leads to increased interfacial shear strength arising from the ability of nanoclay particles to nucleate hydration products in the fiber-matrix contact zone.
- ItemSpinning of Endless Bioactive Silicate Glass Fibres for Fibre Reinforcement Applications(Basel : MDPI, 2021) Eichhorn, Julia; Elschner, Cindy; Groß, Martin; Reichenbächer, Rudi; Herrera Martín, Aarón X.; Prates Soares, Ana; Fischer, Heilwig; Kulkova, Julia; Moritz, Niko; Hupa, Leena; Stommel, Markus; Scheffler, Christina; Kilo, MartinBioactive glasses have been used for many years in the human body as bone substitute. Since bioactive glasses are not readily available in the form of endless thin fibres with diameters below 20 µm, their use is limited to mainly non-load-bearing applications in the form of particles or granules. In this study, the spinnability of four bioactive silicate glasses was evaluated in terms of crystallisation behaviour, characteristic processing temperatures and viscosity determined by thermal analysis. The glass melts were drawn into fibres and their mechanical strength was measured by single fibre tensile tests before and after the surface treatment with different silanes. The degradation of the bioactive glasses was observed in simulated body fluid and pure water by recording the changes of the pH value and the ion concentration by inductively coupled plasma optical emission spectrometry; further, the glass degradation process was monitored by scanning electron microscopy. Additionally, first in vitro experiments using murine pre-osteoblast cell line MC3T3E1 were carried out in order to evaluate the interaction with the glass fibre surface. The results achieved in this work show up the potential of the manufacturing of endless bioactive glass fibres with appropriate mechanical strength to be applied as reinforcing fibres in new innovative medical implants.