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- 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.
- ItemFabrication of four-level hierarchical topographies through the combination of LIPSS and direct laser interference pattering on near-beta titanium alloy(New York, NY [u.a.] : Elsevier, 2022) Schell, Frederic; Alamri, Sabri; Hariharan, Avinash; Gebert, Annett; Lasagni, Andrés Fabián; Kunze, TimComplex repetitive periodic surface patterns were produced on a near-beta Ti-13Nb-13Zr alloy, using two-beam Direct Laser Interference Patterning (DLIP) employing a picosecond-pulsed laser source with wavelengths of 355 nm, 532 nm and 1064 nm. Different types of Laser-induced periodic surface structures (LIPSS) are produced, including low and high spatial frequency LIPSS, which are observed frequently on top of the line-like DLIP microstructures, as well as quasi-periodic microstructures with periods greater than the laser wavelength. The feature size of the fabricated LIPSS features could be tuned as function of the utilized laser process parameters.
- 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.
- ItemSurface Modified β-Ti-18Mo-6Nb-5Ta (wt%) Alloy for Bone Implant Applications: Composite Characterization and Cytocompatibility Assessment(Basel : MDPI, 2023) Escobar, Michael; Careta, Oriol; Fernández Navas, Nora; Bartkowska, Aleksandra; Alberta, Ludovico Andrea; Fornell, Jordina; Solsona, Pau; Gemming, Thomas; Gebert, Annett; Ibáñez, Elena; Blanquer, Andreu; Nogués, Carme; Sort, Jordi; Pellicer, EvaCommercially available titanium alloys such as Ti-6Al-4V are established in clinical use as load-bearing bone implant materials. However, concerns about the toxic effects of vanadium and aluminum have prompted the development of Al- and V-free β-Ti alloys. Herein, a new alloy composed of non-toxic elements, namely Ti-18Mo-6Nb-5Ta (wt%), has been fabricated by arc melting. The resulting single β-phase alloy shows improved mechanical properties (Young’s modulus and hardness) and similar corrosion behavior in simulated body fluid when compared with commercial Ti-6Al-4V. To increase the cell proliferation capability of the new biomaterial, the surface of Ti-18Mo-6Nb-5Ta was modified by electrodepositing calcium phosphate (CaP) ceramic layers. Coatings with a Ca/P ratio of 1.47 were obtained at pulse current densities, −jc, of 1.8–8.2 mA/cm2, followed by 48 h of NaOH post-treatment. The thickness of the coatings has been measured by scanning electron microscopy from an ion beam cut, resulting in an average thickness of about 5 μm. Finally, cytocompatibility and cell adhesion have been evaluated using the osteosarcoma cell line Saos-2, demonstrating good biocompatibility and enhanced cell proliferation on the CaP-modified Ti-18Mo-6Nb-5Ta material compared with the bare alloy, even outperforming their CaP-modified Ti-6-Al-4V counterparts.
- ItemCatechol Containing Polyelectrolyte Complex Nanoparticles as Local Drug Delivery System for Bortezomib at Bone Substitute Materials(Basel : MDPI, 2020) Vehlow, David; Wong, Jeremy P.H.; Urban, Birgit; Weißpflog, Janek; Gebert, Annett; Schumacher, Matthias; Gelinsky, Michael; Stamm, Manfred; Müller, MartinThe proteasome inhibitor bortezomib (BZM) is one of the most potent anti-cancer drugs in the therapy of multiple myeloma. In this study, an adhesive drug delivery system (DDS) for BZM was developed. Therefore, we extended the present DDS concept of polyelectrolyte complex (PEC) nanoparticle (NP) based on electrostatic interactions between charged drug and polyelectrolyte (PEL) to a DDS concept involving covalent bonding between PEL and uncharged drugs. For this purpose, 3,4-dihydroxyphenyl acetic acid (DOPAC) was polymerized via an oxidatively induced coupling reaction. This novel chemo-reactive polyanion PDOPAC is able to temporarily bind boronic acid groups of BZM via its catechol groups, through esterification. PDOPAC was admixed to poly(l-glutamic acid) (PLG) and poly(l-lysine) (PLL) forming a redispersible PEC NP system after centrifugation, which is advantageous for further colloid and BZM loading processing. It was found that the loading capacity (LC) strongly depends on the PDOPAC and catechol content in the PEC NP. Furthermore, the type of loading and the net charge of the PEC NP affect LC and the residual content (RC) after release. Release experiments of PDOPAC/PEC coatings were performed at medically relevant bone substitute materials (calcium phosphate cement and titanium niobium alloy) whereby the DDS worked independently of the surface properties. Additionally, in contrast to electrostatically based drug loading the release behavior of covalently bound, uncharged BZM is independent of the ionic strength (salt content) in the release medium.
- 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.
- ItemEffect of minor gallium addition on corrosion, passivity, and antibacterial behaviour of novel β-type Ti–Nb alloys(Sao Paulo : ABM, 2023) Akman, Adnan; Alberta, Ludovico Andrea; Giraldo-Osorno, Paula Milena; Turner, Adam Benedict; Hantusch, Martin; Palmquist, Anders; Trobos, Margarita; Calin, Mariana; Gebert, AnnettMetastable Ti–Nb alloys are promising bone-implant materials due to improved mechanical biofunctionality and biocompatibility. To overcome increasing bacterial infection risk, alloying with antibacterial elements is a promising strategy. This study investigates the effect of minor gallium (Ga) additions (4, 8 wt% Ga) to as-cast and solution-treated β-type Ti–45Nb-based alloy (96(Ti–45Nb)-4Ga, 92(Ti–45Nb)-8Ga (wt.%)) on corrosion and passive film properties, as well as cytocompatibility and antibacterial activity. The electrochemical properties were evaluated by potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and Mott-Schottky analyses in phosphate-buffered saline (PBS). X-ray photoelectron spectroscopy (XPS) was performed to analyze the chemical composition of passive films. Early adhesion and viability of macrophages and Staphylococcus aureus were assessed by nucleocounting and colony-forming unit counting, respectively. The results showed that high corrosion resistance and passive film properties of Ti–45Nb are retained and even slightly improved with Ga. EIS results revealed that Ga addition improves the passive film resistance. XPS measurements of 92(Ti–45Nb)-8Ga show that the passive film contains Ti-, Nb- and Ga-based oxides, implying the formation of mixed (Ti–Nb-Ga) oxides. In addition, marginal Ga ion release rate was detected under free corrosion conditions. Therefore, it can be assumed that Ga species may contribute to passive film formation on Ga-containing alloys. The 92(Ti–45Nb)-8Ga elicited an antibacterial effect against S. aureus compared to cp-Ti at 4 h. Moreover, Ga-containing alloys showed good cytocompatibility with THP-1 macrophages at 24 h. In conclusion, it was demonstrated that Ga additions to Ti–45Nb are beneficial to corrosion resistance and showed promising initial host and bacterial interactions.
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