11 results
Search Results
Now showing 1 - 10 of 11
- ItemCalciothermic Synthesis of Very Fine, Hydrogenated Ti and Ti–Nb Powder for Biomedical Applications(Weinheim : Wiley-VCH Verl., 2020) Lindemann, Inge; Gebel, Bernhard; Pilz, Stefan; Uhlemann, Margitta; Gebert, AnnettDue to their excellent biocompatibility, titanium and titanium–niobium alloys are especially interesting for biomedical applications. With regard to favorable near-net shape production, Ti powder synthesis is the key hurdle. Extensive research has been in progress for alternative synthesis methods since decades. Herein, an efficient alternative method to the conventional powder production process to prepare spherical powders with very small sizes (<45 μm) for high-strength materials is shown. Very fine, hydrogenated Ti and Ti–Nb alloy powders are stable in air and are synthesized by calciothermic reduction in hydrogen. The herein presented reduction using CaH2 starts directly from the oxides instead of chlorides. Correlations of size and morphology of the as-synthesized TiH2 and (Ti,Nb)H2 powders with the precursors (TiO2, Nb2O5, and CaH2) are illustrated and are used to tailor the desired powders.
- ItemExperimental and numerical characterization of imperfect additively manufactured lattices based on triply periodic minimal surfaces(Amsterdam [u.a.] : Elsevier Science, 2023) Günther, Fabian; Pilz, Stefan; Hirsch, Franz; Wagner, Markus; Kästner, Markus; Gebert, Annett; Zimmermann, MartinaLattices based on triply periodic minimal surfaces (TPMS) are attracting increasing interest in seminal industries such as bone tissue engineering due to their excellent structure-property relationships. However, the potential can only be exploited if their structural integrity is ensured. This requires a fundamental understanding of the impact of imperfections that arise during additive manufacturing. Therefore, in the present study, the structure-property relationships of eight TPMS lattices, including their imperfections, are investigated experimentally and numerically. In particular, the focus is on biomimetic network TPMS lattices of the type Schoen I-WP and Gyroid, which are fabricated by laser powder bed fusion from the biocompatible alloy Ti-42Nb. The experimental studies include computed tomography measurements and compression tests. The results highlight the importance of process-related imperfections on the mechanical performance of TPMS lattices. In the numerical work, firstly the as-built morphology is artificially reconstructed before finite element analyses are performed. Here, the reconstruction procedure previously developed by the same authors is used and validated on a larger experimental matrix before more advanced calculations are conducted. Specifically, the reconstruction reduces the numerical overestimation of stiffness from up to 341% to a maximum of 26% and that of yield strength from 66% to 12%. Given a high simulation accuracy and flexibility, the presented procedure can become a key factor in the future design process of TPMS lattices.
- 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.
- ItemApproach to Estimate the Phase Formation and the Mechanical Properties of Alloys Processed by Laser Powder Bed Fusion via Casting(Basel : MDPI, 2022) Kühn, Uta; Sander, Jan; Gabrysiak, Katharina Nicole; Giebeler, Lars; Kosiba, Konrad; Pilz, Stefan; Neufeld, Kai; Boehm, Anne Veronika; Hufenbach, Julia KristinA high-performance tool steel with the nominal composition Fe85Cr4Mo8V2C1 (wt%) was processed by three different manufacturing techniques with rising cooling rates: conventional gravity casting, centrifugal casting and an additive manufacturing process, using laser powder bed fusion (LPBF). The resulting material of all processing routes reveals a microstructure, which is composed of martensite, austenite and carbides. However, comparing the size, the morphology and the weight fraction of the present phases, a significant difference of the gravity cast samples is evident, whereas the centrifugal cast material and the LPBF samples show certain commonalities leading finally to similar mechanical properties. This provides the opportunity to roughly estimate the mechanical properties of the material fabricated by LPBF. The major benefit arises from the required small material quantity and the low resources for the preparation of samples by centrifugal casting in comparison to the additive manufacturing process. Concluding, the present findings demonstrate the high attractiveness of centrifugal casting for the effective material screening and hence development of novel alloys adapted to LPBF-processing.
- ItemDesigning the microstructural constituents of an additively manufactured near β Ti alloy for an enhanced mechanical and corrosion response(Amsterdam [u.a.] : Elsevier Science, 2022) Hariharan, Avinash; Goldberg, Phil; Gustmann, Tobias; Maawad, Emad; Pilz, Stefan; Schell, Frederic; Kunze, Tim; Zwahr, Christoph; Gebert, AnnettAdditive manufacturing of near β-type Ti-13Nb-13Zr alloys using the laser powder bed fusion process (LPBF) opens up new avenues to tailor the microstructure and subsequent macro-scale properties that aids in developing new generation patient-specific, load-bearing orthopedic implants. In this work, we investigate a wide range of LPBF parameter space to optimize the volumetric energy density, surface characteristics and melt track widths to achieve a stable process and part density of greater than 99 %. Further, optimized sample states were achieved via thermal post-processing using standard capability aging, super-transus (900 °C) and sub-transus (660 °C) heat treatment strategies with varying quenching mediums (air, water and ice). The applied heat treatment strategies induce various fractions of α, martensite (α', α'') in combination with the β phase and strongly correlated with the observed enhanced mechanical properties and a relatively low elastic modulus. In summary, our work highlights a practical strategy for optimizing the mechanical and corrosion properties of a LPBF produced near β-type Ti-13Nb-13Zr alloy via careful evaluation of processing and post-processing steps and the interrelation to the corresponding microstructures. Corrosion studies revealed excellent corrosion resistances of the heat-treated LPBF samples comparable to wrought Ti-13Nb-13Zr alloys.
- ItemStructure-property relationships of imperfect additively manufactured lattices based on triply periodic minimal surfaces(Amsterdam [u.a.] : Elsevier Science, 2022) Günther, Fabian; Hirsch, Franz; Pilz, Stefan; Wagner, Markus; Gebert, Annett; Kästner, Markus; Zimmermann, MartinaLattices based on triply periodic minimal surfaces (TPMS) have recently attracted increasing interest, but their additive manufacturing (AM) is fraught with imperfections that compromise their structural integrity. Initial research has addressed the influence of process-induced imperfections in lattices, but so far numerical work for TPMS lattices is insufficient. Therefore, in the present study, the structure–property relationships of TPMS lattices, including their imperfections, are investigated experimentally and numerically. The main focus is on a biomimetic Schoen I-WP network lattice made of laser powder bed fusion (LPBF) processed Ti-42Nb designed for bone tissue engineering (BTE). The lattice is scanned by computed tomography (CT) and its as-built morphology is examined before a modeling procedure for artificial reconstruction is developed. The structure–property relationships are analyzed by experimental and numerical compression tests. An anisotropic elastoplastic material model is parameterized for finite element analyses (FEA). The numerical results indicates that the reconstruction of the as-built morphology decisively improves the prediction accuracy compared to the ideal design. This work highlights the central importance of process-related imperfections for the structure–property relationships of TPMS lattices and proposes a modeling procedure to capture their implications.
- ItemInvestigating the Static Recrystallization Behavior of 22MnB5 Manganese–Boron Steel through Stress Relaxation Analysis(Basel : MDPI, 2023) Birnbaum, Peter; Pilz, Stefan; Neufeld, Kai; Kunke, AndreasA constitutive model was developed to characterize the static recrystallization (SRX) and evolution of the grain size of the industrially relevant press-hardening steel, 22MnB5, subsequent to the hot forming of sheet metal. Isothermal stress relaxation tests were conducted using the BAEHR 805 A/D thermomechanical simulator, encompassing a temperature range of 950 to 1050 °C, prestrain levels ranging from 0.01 to 0.1, and strain rates spanning from 0.01 to 0.8 s−1. The results obtained from the isothermal stress relaxation tests facilitated the formulation of an Avrami equation-based model, which aptly describes the kinetics of SRX in relation to the temperature, prestrain, and strain rate. Notably, an increase in temperature led to accelerated recrystallization kinetics, signifying temperature-dependent behavior. When the temperature increased from 950 to 1050 °C, the recrystallization time was reduced to approximately one-third. Additionally, the prestrain exhibited a positive influence on the acceleration of SRX kinetics. A quintupling of the prestrain from 0.01 to 0.05 resulted in a reduction of the static recrystallization duration to approximately one-fifth. Among the parameters studied, the strain rate had the least impact on the SRX kinetics, as doubling the strain rate from 0.01 to 0.8 only resulted in a halving of the recrystallization duration. Moreover, an analysis of the microstructural evolution in response to the forming parameters was undertaken. While the grain-size investigation post-isothermal stress relaxation tests provided results in line with the SRX kinetics calculations, the observed effects were comparatively subdued. Furthermore, a comprehensive examination was conducted using electron backscatter diffraction (EBSD) analysis, aiming to explore the effects of specific stress relaxation states on the morphology of martensite. The findings reveal fully recrystallized globulitic microstructures, characterized by relatively minor differences among them.
- ItemNovel low modulus beta-type Ti–Nb alloys by gallium and copper minor additions for antibacterial implant applications(Rio de Janeiro : Elsevier, 2022) Alberta, Ludovico Andrea; Vishnu, Jithin; Hariharan, Avinash; Pilz, Stefan; Gebert, Annett; Calin, MarianaThis study aims to develop novel low-modulus, corrosion-resistant Ti-based alloys with enhanced antimicrobial properties for bone-related implant applications. Novel β-type (Ti–45Nb)-based alloys with minor additions of the antibacterial elements Ga and/or Cu (up to 4 wt.%) were produced by a two-step casting process followed by homogenization treatment. Three nominal compositions (Ti–45Nb)96-4 Ga, (Ti–45Nb)96–4Cu and (Ti–45Nb)96-2 Ga–2Cu (wt.%) were prepared based on alloy design approach using [Mo]eq and electron per atom (e/a) ratio. The influence of Ga and/or Cu addition on the phase constitution, mechanical response and corrosion characteristics in simulated body fluids (PBS, 37.5 °C) has been investigated. X-ray diffraction studies displayed a single β phase structure for all alloys, with an observed lattice contraction evidenced by the reduction of lattice parameters during Rietveld analysis. Homogenous equiaxed microstructures with grain sizes ranging from 55 μm up to 323 μm were observed for (Ti–45Nb)96-4 Ga, (Ti–45Nb)96-2 Ga–2Cu and (Ti–45Nb)96–4Cu alloys. The alloys displayed excellent plasticity with no cracking, or fracturing during compression tests. Their tensile strength, Young's modulus, maximum tensile strain and elastic energy were measured in the ranges of 544–681 MPa, 73–78 GPa, 17–28% and 2.5–3.7 MJ/m3, in the order (Ti–45Nb)96-4 Ga > (Ti–45Nb)96-2 Ga–2Cu > (Ti–45Nb)96–4Cu. In addition, it has been observed that micro-alloying Ti–Nb alloy with Ga and/or Cu posed no deleterious effect on the corrosion resistance in simulated body fluid conditions. The improvement in strength of the developed alloys has been discussed based on grain boundary and solid-solution strengthening, whereas the improved plasticity is attributed to work hardening.
- ItemElectrodeposition of Sr-substituted hydroxyapatite on low modulus beta-type Ti-45Nb and effect on in vitro Sr release and cell response(Amsterdam : Elsevier, 2019) Schmidt, Romy; Gebert, Annett; Schumacher, Matthias; Hoffmann, Volker; Voss, Andrea; Pilz, Stefan; Uhlemann, Margitta; Lode, Anja; Gelinsky, MichaelBeta-type Ti-based alloys are promising new materials for bone implants owing to their excellent mechanical biofunctionality and biocompatibility. For treatment of fractures in case of systemic diseases like osteoporosis the generation of implant surfaces which actively support the problematic bone healing is a most important aspect. This work aimed at developing suitable approaches for electrodeposition of Sr-substituted hydroxyapatite (Srx-HAp) coatings onto Ti-45Nb. Potentiodynamic polarization measurements in electrolytes with 1.67 mmol/L Ca(NO3)2, which was substituted by 0, 10, 50 and 100% Sr(NO3)2, and 1 mmol/L NH4H2PO4 at 333 K revealed the basic reaction steps for OH– and PO4 3− formation needed for the chemical precipitation of Srx-HAp. Studies under potentiostatic control confirmed that partial or complete substitution of Ca2+- by Sr2+-ions in solution has a significant effect on the complex reaction process. High Sr2+-ion contents yield intermediate phases and a subsequent growth of more refined Srx-HAp coatings. Upon galvanostatic pulse-deposition higher reaction rates are controlled and in all electrolytes very fine needle-like crystalline coatings are obtained. With XRD the incorporation of Sr-species in the hexagonal HAp lattice is evidenced. Coatings formed in electrolytes with 10 and 50% Sr-nitrate were chemically analyzed with EDX mapping and GD-OES depth profiling. Only a fraction of the Sr-ions in solution is incorporated into the Srx-HAp coatings. Therein, the Sr-distribution is laterally homogeneous but non-homogeneous along the cross-section. Increasing Sr-content retards the coating thickness growth. Most promising coatings formed in the electrolyte with 10% Sr-nitrate were employed for Ca, P and Sr release analysis in Tris-Buffered Saline (150 mM NaCl, pH 7.6) at 310 K. At a sample surface: solution volume ratio of 1:200, after 24 h the amount of released Sr-ions was about 30–35% of that determined in the deposited Srx-HAp coating. In vitro studies with human bone marrow stromal cells (hBMSC) revealed that the released Sr-ions led to a significantly enhanced cell proliferation and osteogenic differentiation and that the Sr-HAp surface supported cell adhesion indicating its excellent cytocompatibility. © 2019 The Authors
- ItemEffect of Selective Laser Melting on Microstructure, Mechanical, and Corrosion Properties of Biodegradable FeMnCS for Implant Applications(Weinheim : Wiley-VCH Verl., 2020) Hufenbach, Julia; Sander, Jan; Kochta, Fabian; Pilz, Stefan; Voss, Andrea; Kühn, Uta; Gebert, AnnettSelective laser melting (SLM) of biodegradable metallic materials offers a great potential for manufacturing customized implants. Herein, SLM processing of a novel Fe–30Mn–1C–0.02S twinning-induced plasticity (TWIP) alloy and the resulting structural, mechanical, and corrosion properties are presented. The occurring rapid solidification results in a fine-grained austenitic microstructure with mainly homogeneous element distribution, which is investigated by scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDX) and electron backscatter diffraction (EBSD) as well as X-ray diffraction (XRD). By processing the alloy via SLM, significantly higher strengths under tensile and compressive load in comparison with those for the as-cast counterpart and a 316L reference steel are achieved. Electrochemical corrosion tests in a simulated body fluid (SBF) indicate a moderate corrosion activity, and a beneficial uniform degradation is shown in immersion tests in SBF. Regarding the envisaged application for vascular implants, SLM-processed stent prototypes out of the novel alloy are presented and a first functionality test is shown. © 2020 The Authors. Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim