Universität Stuttgart
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Item Open Access Alumina and zirconia-reinforced polyamide PA-12 composites for biomedical additive manufacturing(2021) Nakonieczny, Damian S.; Kern, Frank; Dufner, Lukas; Antonowicz, Magdalena; Matus, KrzysztofThis work aimed to prepare a composite with a polyamide (PA) matrix and surface-modified ZrO2 or Al2O3 to be used as ceramic fillers (CFs). Those composites contained 30 wt.% ceramic powder to 70 wt.% polymer. Possible applications for this type of composite include bioengineering applications especially in the fields of dental prosthetics and orthopaedics. The ceramic fillers were subjected to chemical surface modification with Piranha Solution and suspension in 10 M sodium hydroxide and Si3N4 to achieve the highest possible surface development and to introduce additional functional groups. This was to improve the bonding between the CFs and the polymer matrix. Both CFs were examined for particle size distribution (PSD), functional groups (FTIR), chemical composition (XPS), phase composition (XRD), and morphology and chemical composition (SEM/EDS). Filaments were created from the powders prepared in this way and were then used for 3D FDM printing. Samples were subjected to mechanical tests (tensility, hardness) and soaking tests in a high-pressure autoclave in artificial saliva for 14, 21, and 29 days.Item Open Access Mechanical properties and electrical discharge machinability of alumina-10 vol% zirconia-28 vol% titanium nitride composites(2020) Gommeringer, Andrea; Kern, FrankElectrical discharge machinable ceramics provide an alternative machining route independent on the material hardness which enables manufacturing of customized ceramic components. In this study a composite material based on an alumina/zirconia matrix and an electrically conductive titanium nitride dispersion was manufactured by hot pressing and characterized with respect to microstructure, mechanical properties and ED-machinability by die sinking. The composites show a combination of high strength of 700 MPa, hardness of 17-18 GPa and moderate fracture resistance of 4.5-5 MPa√m. With 40 kS/m the electrical conductivity is sufficiently high to ensure ED-machinability.Item Open Access Plasma spraying of a microwave absorber coating for an RF dummy load(2021) Killinger, Andreas; Gantenbein, Gerd; Illy, Stefan; Ruess, Tobias; Weggen, Jörg; Martinez-Garcia, VenancioThe European fusion reactor research facility, called International Thermonuclear Experimental Reactor (ITER), is one of the most challenging projects that involves design and testing of hundreds of separately designed reactor elements and peripheric modules. One of the core elements involved in plasma heating are gyrotrons. They are used as a microwave source in electron-cyclotron resonance heating systems (ECRH) for variable injection of RF power into the plasma ring. In this work, the development and application of an alumina-titania 60/40 mixed oxide ceramic absorber coating on a copper cylinder is described. The cylinder is part of a dummy load used in gyrotron testing and its purpose is to absorb microwave radiation generated by gyrotrons during testing phase. The coating is applied by means of atmospheric plasma spraying (APS). The absorber coating is deposited on the inner diameter of a one-meter cylindrical tube. To ensure homogeneous radiation absorption when the incoming microwave beam is repeatedly scattered along the inner tube surface, the coating shows a varying thickness as a function of the tube length. By this it is ensured that the thermal power is distributed homogeneously on the entire inner tube surface. This paper describes a modeling approach of the coating thickness distribution, the manufacturing concept for the internal plasma spray coating and the coating characterization with regard to coating microstructure and microwave absorption characteristics.Item Open Access In vitro evaluation of biologically derived hydroxyapatite coatings manufactured by high velocity suspension spraying(2021) Blum, M.; Sayed, M.; Mahmoud, E. M.; Killinger, A.; Gadow, R.; Naga, S. M.This investigation aims to study a novel biologically derived coating applied on Ti alloy substrates. Obtained from a low-cost fish bone resource, a nanocrystalline hydroxyapatite has been synthesized and converted to an organic suspension. Coating was then manufactured by a high-velocity suspension flame spray process. The microstructure, phase composition, coating thickness, and roughness of hydroxyapatite (HA)-coated samples were studied. The results indicated the presence of both hydroxyapatite and β-tricalcium phosphate phases and the final coating layer was uniform and dense. In vitro bioactivity and biodegradability of the HA/Ti composite samples were estimated by immersion in simulated body fluid. Remarkable reductions in Ca2+ and PO43- ion concentrations were observed as well as low weight loss percentage and a slight variation in the pH value, indicating the generation of an apatite layer on the surface of all studied samples. Scanning electron microscopy, energy-dispersive x-ray analysis, and inductively coupled plasma–optical emission spectrometry confirm these results. Thus biological derived HA coatings are a promising candidate to enhance bioactivity and biodegradability of bone implants. To demonstrate feasibility on commercial medical components, a medical screw was coated and evaluated.Item Open Access PA-12-zirconia-alumina-cenospheres 3D printed composites : accelerated ageing and role of the sterilisation process for physicochemical properties(2022) Nakonieczny, Damian S.; Antonowicz, Magdalena; SimhaMartynkova, Gražyna; Kern, Frank; Pazourková, Lenka; Erfurt, Karol; Hüpsch, MichałThe aim of this study was to conduct artificial ageing tests on polymer-ceramic composites prepared from polyamide PA-12 polymer matrix for medical applications and three different variants of ceramic fillers: zirconia, alumina and cenospheres. Before ageing, the samples were subjected to ethyl oxide sterilization. The composite variants were prepared for 3D printing using the fused deposition modeling method. The control group consisted of unsterilized samples. Samples were subjected to artificial ageing in a high-pressure autoclave. Ageing conditions were calculated from the modified Hammerlich Arrhenius kinetic equation. Ageing was carried out in artificial saliva. After ageing the composites were subjected to mechanical (tensile strength, hardness, surface roughness) testing, chemical and structural (MS, FTIR) analysis, electron microscopy observations (SEM/EDS) and absorbability measurements.Item Open Access Cu-doped calcium phosphate supraparticles for bone tissue regeneration(2024) Höppel, Anika; Bahr, Olivia; Ebert, Regina; Wittmer, Annette; Seidenstuecker, Michael; Carolina Lanzino, M.; Gbureck, Uwe; Dembski, SofiaCalcium phosphate (CaP) minerals have shown great promise as bone replacement materials due to their similarity to the mineral phase of natural bone. In addition to biocompatibility and osseointegration, the prevention of infection is crucial, especially due to the high concern of antibiotic resistance. In this context, a controlled drug release as well as biodegradation are important features which depend on the porosity of CaP. An increase in porosity can be achieved by using nanoparticles (NPs), which can be processed to supraparticles, combining the properties of nano- and micromaterials. In this study, Cu-doped CaP supraparticles were prepared to improve the bone substitute properties while providing antibacterial effects. In this context, a modified sol-gel process was used for the synthesis of CaP NPs, where a Ca/P molar ratio of 1.10 resulted in the formation of crystalline β-tricalcium phosphate (β-TCP) after calcination at 1000 °C. In the next step, CaP NPs with Cu 2+ (0.5-15.0 wt%) were processed into supraparticles by a spray drying method. Cu release experiments of the different Cu-doped CaP supraparticles demonstrated a long-term sustained release over 14 days. The antibacterial properties of the supraparticles were determined against Gram-positive ( Bacillus subtilis and Staphylococcus aureus ) and Gram-negative ( Escherichia coli ) bacteria, where complete antibacterial inhibition was achieved using a Cu concentration of 5.0 wt%. In addition, cell viability assays of the different CaP supraparticles with human telomerase-immortalized mesenchymal stromal cells (hMSC-TERT) exhibited high biocompatibility with particle concentrations of 0.01 mg mL -1 over 72 hours.Item Open Access Modelling and experimental validation of the flame temperature profile in atmospheric plasma coating processes on the substrate(2024) Martínez-García, Jose; Martínez-García, Venancio; Killinger, AndreasThis work presents a characterisation model for the temperature distribution at different substrate depths during the atmospheric plasma spray (APS) coating process. The torch heat flow in this model is simulated as forced convection defined by a surface, a temperature profile, and a convection coefficient. The simulation model considers three plasma temperature profiles of the Al2O3 coating on a 5 mm thickness flat aluminium substrate. The simple and low-cost experimental procedure, based on a thermocouple, measures the plasma plume temperature distribution of the APS coating system, and their results are used to obtain the parameter values of each of the three proposed plasma temperature profiles. The experimental method for in situ non-contact temperature measurements inside the substrate is based on an infrared pyrometry technique and validates the simulation results. The Gaussian temperature profile shows excellent accuracy with the measured temperatures. The Gaussian approach could be a powerful tool for predicting residual stress through a coupled one-way thermal-mechanical analysis of the APS process.Item Open Access Adjustment of micro- and macroporosity of ß-TCP scaffolds using solid-stabilized foams as bone replacement(2023) Dufner, Lukas; Oßwald, Bettina; Eberspaecher, Jan; Riedel, Bianca; Kling, Chiara; Kern, Frank; Seidenstuecker, MichaelTo enable rapid osteointegration in bioceramic implants and to give them osteoinductive properties, scaffolds with defined micro- and macroporosity are required. Pores or pore networks promote the integration of cells into the implant, facilitating the supply of nutrients and the removal of metabolic products. In this paper, scaffolds are created from ß-tricalciumphosphate (ß-TCP) and in a novel way, where both the micro- and macroporosity are adjusted simultaneously by the addition of pore-forming polymer particles. The particles used are 10-40 wt%, spherical polymer particles of polymethylmethacrylate (PMMA) (Ø = 5 m) and alternatively polymethylsilsesquioxane (PMSQ) (Ø = 2 m), added in the course of ß-TCP slurry preparation. The arrangement of hydrophobic polymer particles at the interface of air bubbles was incorporated during slurry preparation and foaming of the slurry. The foam structures remain after sintering and lead to the formation of macro-porosity in the scaffolds. Furthermore, decomposition of the polymer particles during thermal debindering results in the formation of an additional network of interconnecting micropores in the stabilizing structures. It is possible to adjust the porosity easily and quickly in a range of 1.2-140 m with a relatively low organic fraction. The structures thus prepared showed no cytotoxicity nor negative effects on the biocompatibility.Item Open Access Cenospheres-reinforced PA-12 composite : preparation, physicochemical properties, and soaking tests(2022) Nakonieczny, Damian S.; Antonowicz, Magdalena; Heim, Thomas; Swinarew, Andrzej S.; Nuckowski, Paweł; Matus, Krzysztof; Lemanowicz, MarcinThe main aim of this research was the preparation of a polymer–ceramic composite with PA-12 as the polymer matrix and modified aluminosilicate cenospheres (CSs) as the ceramic filler. The CSs were subjected to an early purification and cleaning process, which was also taken as a second objective. The CSs were surface modified by a two-step process: (1) etching in Piranha solution and (2) silanization in 3-aminopropyltriethoxysilane. The composite was made for 3D printing by FDM. Raw and modified CSs and a composite with PA-12 were subjected to the following tests: surface development including pores (BET), real density (HP), chemical composition and morphology (SEM/EDS, FTIR), grain analysis (PSD), phase composition (XRD), hardness (HV), and static tensile tests. The composites were subjected to soaking under simulated body fluid (SBF) conditions in artificial saliva for 14, 21, and 29 days. Compared to pure PA-12, PA-12_CS had generally better mechanical properties and was more resistant to SBF at elevated temperatures and soaking times. These results showed this material has potential for use in biomedical applications. These results also showed the necessity of developing a kinetic aging model for aging in different liquids to verify the true value of this material.Item Open Access Additive manufacturing of β-tricalcium phosphate components via Fused Deposition of Ceramics (FDC)(2020) Eßlinger, Steffen; Grebhardt, Axel; Jäger, Jonas; Kern, Frank; Killinger, Andreas; Bonten, Christian; Gadow, RainerDas Paper beschreibt die Compoundierung bioaktiver Keramik (Beta-Tricalciumphosphat) in einer organischen Matrix, die anschließende Extrusion zu Filamenten, die für den FDM-3D-Druck geeignet sind, sowie die Formgebund zu Scaffolds mittels additiver Fertigung. Weiterhin werden fertigungsprozessbegleitende Untersuchungen zur Entbinderung und Sinterung durchgeführt.