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- ItemDesign of biomimetic collagen matrices by reagent-free electron beam induced crosslinking: Structure-property relationships and cellular response(Amsterdam [u.a.] : Elsevier Science, 2019) Riedel, Stefanie; Hietschold, Philine; Krömmelbein, Catharina; Kunschmann, Tom; Konieczny, Robert; Knolle, Wolfgang; Mierke, Claudia T.; Zink, Mareike; Mayr, Stefan G.Novel strategies to mimic mammalian extracellular matrix (ECM) in vitro are desirable to study cell behavior, diseases and new agents in drug delivery. Even though collagen represents the major constituent of mammalian ECM, artificial collagen hydrogels with characteristic tissue properties such as network size and stiffness are difficult to design without application of chemicals which might be even cytotoxic. In our study we investigate how high energy electron induced crosslinking can be utilized to precisely tune collagen properties for ECM model systems. Constituting a minimally invasive approach, collagen residues remain intact in the course of high energy electron treatment. Quantification of the 3D pore size of the collagen network as a function of irradiation dose shows an increase in density leading to decreased pore size. Rheological measurements indicate elevated storage and loss moduli correlating with an increase in crosslinking density. In addition, cell tests show well maintained viability of NIH 3T3 cells for irradiated collagen gels indicating excellent cellular acceptance. With this, our investigations demonstrate that electron beam crosslinked collagen matrices have a high potential as precisely tunable ECM-mimetic systems with excellent cytocompatibility.
- ItemInfluence of annealing on microstructure and mechanical properties of ultrafine-grained Ti45Nb(Amsterdam [u.a.] : Elsevier Science, 2019) Völker, B.; Maier-Kiener, V.; Werbach, K.; Müller, T.; Pilz, S.; Calin, M.; Eckert, J.; Hohenwarter, A.Beta-Ti alloys have been intensively investigated in the last years because of their favorable low Young's moduli, biocompatibility and bio-inertness, making these alloys interesting candidates for implant materials. Due to their low mechanical strength, efforts are currently devoted to increasing it. A promising way to improve the strength is to tailor the microstructure using severe plastic deformation (SPD). In this investigation high pressure torsion was used to refine the microstructure of a Ti-45wt.%Nb alloy inducing a grain size of ~50 nm. The main focus of the subsequent investigations was devoted to the thermal stability of the microstructure. Isochronal heat-treatments performed for 30 min in a temperature range up to 500 °C caused an increase of hardness with a peak value at 300 °C before the hardness decreased at higher temperatures. Simultaneously, a distinct temperature-dependent variation of the Young's modulus was also measured. Tensile tests revealed an increase in strength after annealing compared to the SPD-state. Microstructural investigations showed that annealing causes the formation of α-Ti. The findings suggest that the combination of severe plastic deformation with subsequent heat treatment provides a feasible way to improve the mechanical properties of SPD-deformed β-Ti alloys making them suitable for higher strength applications.
- ItemA novel approach to fabricate load-bearing Ti6Al4V-Barium titanate piezoelectric bone scaffolds by coupling electron beam melting and field-assisted sintering(Amsterdam [u.a.] : Elsevier Science, 2022) Riaz, Abdullah; Polley, Christian; Lund, Henrik; Springer, Armin; Seitz, HermannA critical-size bone defect in load-bearing areas is a challenging clinical problem in orthopaedic surgery. Titanium alloy (Ti6Al4V) scaffolds have advantages because of their biomechanical stability but lack electrical activity, which hinders their further use. This work is focused on the fabrication of Ti6Al4V-Barium Titanate (BaTiO3) bulk composite scaffolds to combine the biomechanical stability of Ti6Al4V with electrical activity through BaTiO3. For the first time, a hollow cylindrical Ti6Al4V is additively manufactured by electron beam melting and combined with piezoelectric BaTiO3 powder for joint processing in field-assisted sintering. Scanning electron microscope images on the interface of the Ti6Al4V-BaTiO3 composite scaffold showed that after sintering, the Ti6Al4V lattice structure bounded with BaTiO3 matrix without its major deformation. The Ti6Al4V-BaTiO3 scaffold had average piezoelectric constants of (0.63 ± 0.12) pC/N directly after sintering due to partial dipole alignment of the BaTiO3 tetragonal phase, which increased to (4.92 ± 0.75) pC/N after a successful corona poling. Moreover, the nanoindentation values of Ti6Al4V exhibited an average hardness and Young's modulus of (5.9 ± 0.9) GPa and (130 ± 14) GPa, and BaTiO3 showed (4.0 ± 0.6) GPa and (106 ± 10) GPa, respectively. It reveals that the Ti6Al4V is the harder and stiffer part in the Ti6Al4V-BaTiO3 composite scaffold. Such a scaffold has the potential to treat critical-size bone defects in load-bearing areas and guide tissue regeneration by physical stimulation.
- ItemMachine learning for additive manufacturing: Predicting materials characteristics and their uncertainty(Amsterdam [u.a.] : Elsevier Science, 2023) Chernyavsky, Dmitry; Kononenko, Denys Y.; Han, Jun Hee; Kim, Hwi Jun; van den Brink, Jeroen; Kosiba, KonradAdditive manufacturing (AM) is known for versatile fabrication of complex parts, while also allowing the synthesis of materials with desired microstructures and resulting properties. These benefits come at a cost: process control to manufacture parts within given specifications is very challenging due to the relevance of a large number of processing parameters. Efficient predictive machine learning (ML) models trained on small datasets, can minimize this cost. They also allow to assess the quality of the dataset inclusive of uncertainty. This is important in order for additively manufactured parts to meet property specifications not only on average, but also within a given variance or uncertainty. Here, we demonstrate this strategy by developing a heteroscedastic Gaussian process (HGP) model, from a dataset based on laser powder bed fusion of a glass-forming alloy at varying processing parameters. Using amorphicity as the microstructural descriptor, we train the model on our Zr52.5Cu17.9Ni14.6Al10Ti5 (at.%) alloy dataset. The HGP model not only accurately predicts the mean value of amorphicity, but also provides the respective uncertainty. The quantification of the aleatoric and epistemic uncertainty contributions allows to assess intrinsic inaccuracies of the dataset, as well as identify underlying physical phenomena. This HGP model approach enables to systematically improve ML-driven AM processes.
- ItemThermal annealing to influence the vapor sensing behavior of co-continuous poly(lactic acid)/polystyrene/multiwalled carbon nanotube composites(Amsterdam [u.a.] : Elsevier Science, 2020) Li, Yilong; Pionteck, Jürgen; Pötschke, Petra; Voit, BrigitteWith the main purpose of being used as vapor leakage detector, the volatile organic compound (VOC) vapor sensing properties of conductive polymer blend composites were studied. Poly(lactic acid)/polystyrene/multi-walled carbon nanotube (PLA/PS/MWCNT) based conductive polymer composites (CPCs) in which the polymer components exhibit different interactions with the vapors, were prepared by melt mixing. CPCs with a blend composition of 50/50 wt% resulted in the finest co-continuous structure and selective MWCNT localization in PLA. Therefore, these composites were selected for sensor tests. Thermal annealing was applied aiming to maintain the blend structure but improving the sensing reversibility of CPC sensors towards high vapor concentrations. Different sensing protocols were applied using acetone (good solvent for PS and PLA) and cyclohexane (good solvent for PS but poor solvent for PLA) vapors. Increasing acetone vapor concentration resulted in increased relative resistance change (Rrel) of CPCs. Saturated cyclohexane vapor resulted in lower response than nearly saturated acetone vapor. The thermal annealing at 150 °C did not change the blend morphology but increased the PLA crystallinity, making the CPC sensors more resistant to vapor stimulation, resulting in lower Rrel but better reversibility after vapor exposure.
- ItemLaser powder bed fusion of a superelastic Cu-Al-Mn shape memory alloy(Amsterdam [u.a.] : Elsevier Science, 2021) Babacan, N.; Pauly, S.; Gustmann, T.Dense and crack-free specimens of the shape memory alloy Cu71.6Al17Mn11.4 (at.%) were produced via laser powder bed fusion across a wide range of process parameters. The microstructure, viz. grain size, can be directly tailored within the process and with it the transformation temperatures (TTs) shifted to higher values by raising the energy input. The microstructure, and the superelastic behavior of additively manufactured samples were assessed by a detailed comparison with induction melted material. The precipitation of the α phase, which inhibit the martensitic transformation, were not observed in the additively manufactured samples owing to the high intrinsic cooling rates during the fabrication process. Fine columnar grains with a strong [001]-texture along the building direction lead to an enhanced yield strength compared to the coarse-grained cast samples. A maximum recoverable strain of 2.86% was observed after 5% compressive loading. The first results of our approach imply that laser powder bed fusion is a promising technique to directly produce individually designed Cu-Al-Mn shape memory parts with a pronounced superelasticity at room temperature.
- ItemTransparent model concrete with tunable rheology for investigating flow and particle-migration during transport in pipes(Amsterdam [u.a.] : Elsevier Science, 2020) Auernhammer, Günter K.; Fataei, Shirin; Haustein, Martin A.; Patel, Himanshu P.; Schwarze, Rüdiger; Secrieru, Egor; Mechtcherine, ViktorThe article describes the adaption and properties of a model concrete for detailed flow studies. To adapt the yield stress and plastic viscosity of the model concrete to the corresponding rheological properties of real concrete, the model concrete is made of a mixture of glass beads and a non-Newtonian fluid. The refractive index of the non-Newtonian fluid is adjusted to the refractive index of the glass beads by the addition of a further constituent. The rheological properties of the model concrete are characterised by measurements in concrete rheometers. Finally, the first exemplary results from experiments with the model concrete are presented, which give incipient impressions of the complex internal dynamics in flowing concrete.
- ItemControlled synthesis of mussel-inspired Ag nanoparticle coatings with demonstrated in vitro and in vivo antibacterial properties(Amsterdam [u.a.] : Elsevier Science, 2021) Wang, Xiaowei; Xu, Kehui; Cui, Wendi; Yang, Xi; Maitz, Manfred F.; Li, Wei; Li, Xiangyang; Chen, JialongThe in-situ formation of silver nanoparticles (AgNPs) via dopamine-reduction of Ag+ has been widely utilized for titanium implants to introduce antibacterial properties. In previous studies, the preparation of AgNPs has focused on controlling the feeding concentrations, while the pH of the reaction solution was ignored. Herein, we systematically determined the influence of various pH (4, 7, 10) and Ag+ concentrations (0.01, 0.1 mg/mL) on the AgNPs formation, followed by the evaluation of the antibacterial properties in vitro and in vivo. The results revealed that an alkaline environment was favourable for AgNP formation and resulted in more particles. Although the AgNPs bearing Ti had lower biocompatibilities, it was significantly improved after 7 days of mineralization in simulated body fluid. The outstanding antibacterial property of the AgNPs was well maintained after one day and seven days of implantation. Moreover, 3D micro-CT modelling showed that the pH 10/0.1 group exhibited remarkable osteogenesis, which may be due to their strong antibacterial properties and ability to promote mineralization. Therefore, we have demonstrated that the solution pH was as important as the feeding Ag+ concentration in determining AgNP formation, and it has paved the way for developing various AgNP-loaded surfaces that could meet different antibacterial needs.
- ItemOrganic vapor sensing behavior of polycarbonate/polystyrene/multi-walled carbon nanotube blend composites with different microstructures(Amsterdam [u.a.] : Elsevier Science, 2019) Li, Yilong; Pionteck, Jürgen; Pötschke, Petra; Voit, BrigitteWith the focus on the use as leakage detectors, the vapor sensing behavior of conductive polymer composites (CPCs) based on polycarbonate/polystyrene/multi-walled carbon nanotube (PC/PS/MWCNT) blends with different blend ratios was studied as well as their morphological and electrical properties. In the melt mixed blend composites, the MWCNTs are preferentially localized in PC. At the PC/PS ratio of 70/30 wt%, the composites showed a sea-island structure, while for blends containing 40 wt% or 50 wt% PS co-continuous structures were developed resulting in a reduction in the MWCNT percolation threshold. The saturated vapors of the selected solvents have good interactions to PS but different interactions to PC. At 0.75 wt% MWCNT, sea-island CPCs showed high relative resistance change (Rrel) but poor reversibility towards moderate vapors like ethyl acetate and toluene, while CPCs with co-continuous structure exhibited lower Rrel and better reversibility. All CPCs showed poor reversibility towards vapor of the good solvent dichloromethane due to strong interactions between polymers and vapor. In the vapor of the poor solvent cyclohexane, CPCs with higher PS content showed increased Rrel. After extraction of the PS component by cyclohexane, the sensing response was decreased and the Rrel of the co-continuous blend even reached negative values.
- ItemControlling the Young’s modulus of a ß-type Ti-Nb alloy via strong texturing by LPBF(Amsterdam [u.a.] : Elsevier Science, 2022) Pilz, Stefan; Gustmann, Tobias; Günther, Fabian; Zimmermann, Martina; Kühn, Uta; Gebert, AnnettThe ß-type Ti-42Nb alloy was processed by laser powder bed fusion (LPBF) with an infrared top hat laser configuration aiming to control the Young’s modulus by creating an adapted crystallographic texture. Utilizing a top hat laser, a microstructure with a strong 〈0 0 1〉 texture parallel to the building direction and highly elongated grains was generated. This microstructure results in a strong anisotropy of the Young’s modulus that was modeled based on the single crystal elastic tensor and the experimental texture data. Tensile tests along selected loading directions were conducted to study the mechanical anisotropy and showed a good correlation with the modeled data. A Young’s modulus as low as 44 GPa was measured parallel to the building direction, which corresponds to a significant reduction of over 30% compared to the Young’s modulus of the Gaussian reference samples (67–69 GPa). At the same time a high 0.2% yield strength of 674 MPa was retained. The results reveal the high potential of LPBF processing utilizing a top hat laser configuration to fabricate patient-specific implants with an adapted low Young’s modulus along the main loading direction and a tailored mechanical biofunctionality.
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