DSpace :: Browsing by Author "Gebert, Annett"

Browsing by Author "Gebert, Annett"

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A comparative study of the influence of the deposition technique (electrodeposition versus sputtering) on the properties of nanostructured Fe70Pd30 films
(Abington : Taylor & Francis, 2020) Cialone, Matteo; Fernandez-Barcia, Monica; Celegato, Federica; Coisson, Marco; Barrera, Gabriele; Uhlemann, Margitta; Gebert, Annett; Sort, Jordi; Pellicer, Eva; Rizzi, Paola; Tiberto, Paola
Sputtering and electrodeposition are among the most widespread techniques for metallic thin film deposition. Since these techniques operate under different principles, the resulting films typically show different microstructures even when the chemical composition is kept fixed. In this work, films of Fe70Pd30 were produced in a thickness range between 30 and 600 nm, using both electrodeposition and sputtering. The electrodeposited films were deposited under potentiostatic regime from an ammonia sulfosalicylic acid-based aqueous solution. Meanwhile, the sputtered films were deposited from a composite target in radio frequency regime. Both approaches were proven to yield high quality and homogenous films. However, their crystallographic structure was different. Although all films were polycrystalline and Fe and Pd formed a solid solution with a body-centered cubic structure, a palladium hydride phase was additionally detected in the electrodeposited films. The occurrence of this phase induced internal stress in the films, thereby influencing their magnetic properties. In particular, the thickest electrodeposited Fe70Pd30 films showed out-of-plane magnetic anisotropy, whereas the magnetization easy axis lied in the film plane for all the sputtered films. The domain pattern of the electrodeposited films was investigated by magnetic force microscopy. Finally, nanoindentation studies highlighted the high quality of both the sputtered and electrodeposited films, the former exhibiting higher reduced Young’s modulus and Berkovich hardness values.
Acid Treatments of Ti-Based Metallic Glasses for Improving Corrosion Resistance in Implant Applications
(Basel : MDPI, 2024) Fernández-Navas, Nora; Shtefan, Viktoriia; Hantusch, Martin; Gebert, Annett
Ti-based bulk metallic glasses are promising materials for metallic bone implants, mainly due to their mechanical biofunctionality. A major drawback is their limited corrosion resistance, with high sensitivity to pitting. Thus, effective surface treatments for these alloys must be developed. This work investigates the electrochemical treatment feasibility of nitric acid (HNO3) solution for two bulk glass-forming alloys. The surface states obtained at different anodic potentials are characterized with electron microscopy and Auger electron spectroscopy. The corrosion behavior of the treated glassy alloys is analyzed via comparison to non-treated states in phosphate-buffered saline solution (PBS) at 37 °C. For the glassy Ti47Zr7.5Cu38Fe2.5Sn2Si1Ag2 alloy, the pre-treatment causes pseudo-dealloying, with a transformation from naturally passivated surfaces to Ti- and Zr-oxide nanoporous layers and Cu-species removal from the near-surface regions. This results in effective suppression of chloride-induced pitting in PBS. The glassy Ti40Zr10Cu34Pd14Sn2 alloy shows lower free corrosion activity in HNO3 and PBS due to Pd stabilizing its strong passivity. However, this alloy undergoes pitting under anodic conditions. Surface pre-treatment results in Cu depletion but causes enrichment of Pd species and non-homogeneous surface oxidation. Therefore, for this glassy alloy, pitting cannot be completely inhibited in PBS. Concluding, anodic treatments in HNO3 are more suitable for Pd-free glassy Ti-based alloys.
Anelastic-like nature of the rejuvenation of metallic glasses by cryogenic thermal cycling
(Amsterdam [u.a.] : Elsevier Science, 2022) Costa, Miguel B.; Londoño, Juan J.; Blatter, Andreas; Hariharan, Avinash; Gebert, Annett; Carpenter, Michael A.; Greer, A. Lindsay
Cryogenic thermal cycling (CTC) is an effective treatment for improving the room-temperature plasticity and toughness in metallic glasses. Despite considerable attention to characterizing the effects of CTC, they remain poorly understood. A prominent example is that, contrary to expectation, the stored energy in a metallic glass first rises, and then decreases, as CTC progresses. In this work, CTC is applied to bulk metallic glasses based on Pd, Pt, Ti, or Zr. The effects on calorimetric and mechanical properties are evaluated. Critically, CTC-induced effects, at whatever stage, are found to decay over about one week at room temperature after CTC, returning the properties to those of the as-cast glass. A model is proposed for CTC-induced effects, treating them as analogous to the accumulation of anelastic strain. The implications for analysis of existing data, and for future research on CTC effects, are highlighted.
Calciothermic 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, Annett
Due 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.
Catechol 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, Martin
The 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.
Controlling 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, Annett
The 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.
Corrosion Fatigue Studies on a Bulk Glassy Zr-Based Alloy under Three-Point Bending
(Lausanne : Frontiers Media, 2017-1-9) Grell, Daniel; Wilkin, Yannic; Gostin, Petre F.; Gebert, Annett; Kerscher, Eberhard
Corrosion fatigue (CF) tests were carried out on bulk glassy Zr52.5Cu17.9Al10Ni14.6Ti5 (Vitreloy 105) samples under load-controlled three-point bending conditions with a load ratio of R = 0.1 in 0.01 M Na2SO4 + 0.01 M NaCl electrolyte. During cyclic testing, the bar-shaped specimens were polarized in situ at constant potentials and the current was monitored. Three different anodic potentials within the interval between the pitting potential EP and the repassivation potential ER and three different load amplitudes were applied. In some cases, in situ microscopic observations revealed the formation of black corrosion products in the vicinity of the crack tip during anodic polarization. Fractographic analysis revealed a clear distinction between two modes of crack growth characterized by smooth dissolution induced regions on the one hand and slim fast fracture areas on the other hand. Both alternating features contributed to a broad-striated CF fracture surface. Moreover, further fatigue tests were carried out under free corrosion conditions yielding additional information on crack initiation and crack propagation period by means of the open circuit potential (OCP) changes. Thereby, a slight increase in OCP was detected after rupture of the passive layer due to bare metal exposed to the electrolyte. The electrochemical response increased continuously according to stable crack propagation until fracture occurred. Finally, the fracture surfaces of the CF samples were investigated by energy dispersive X-ray with the objective of analyzing the elemental distribution after anodic dissolution. Interestingly, anodic polarization at a near repassivation potential of −50 mV vs. saturated calomel electrode (SCE), which commands a constant electric potential of E = 0.241 V vs. standard hydrogen electrode (SHE), led to favorable effects on the fatigue lifetime. In conclusion, all results are conflated to a CF model for bulk glassy Vitreloy 105 under anodic polarization in chloride-containing electrolyte and compared to the previously proposed stress corrosion mechanisms under similar conditions. © 2017 Grell, Wilkin, Gostin, Gebert and Kerscher.
Designing Gallium-Containing Hydroxyapatite Coatings on Low Modulus Beta Ti-45Nb Alloy
(Basel : MDPI, 2023) Vishnu, Jithin; Voss, Andrea; Hoffmann, Volker; Alberta, Ludovico Andrea; Akman, Adnan; Shankar, Balakrishnan; Gebert, Annett; Calin, Mariana
Low-modulus β-type Ti-45Nb alloy is a promising implant material due to its good mechanical biocompatibility, non-toxicity, and outstanding corrosion resistance. Its excellent chemical stability brings new challenges to chemical surface modification treatments, which are indispensable for both osteogenesis and antibacterial performance. Coatings containing metal ions as anti-microbial agents can be an effective way to reduce implant-associated infections caused by bacterial biofilm. Gallium ion (Ga3+) has the potential to reduce bacterial viability and biofilm formation on implant surfaces. In this study, a novel two-step process has been proposed for Ga3+ incorporation in hydroxyapatite (HAP) to develop bioactive and antibacterial surfaces on Ti-45Nb alloy. For the generation of bioactive surface states, HAP electrodeposition was conducted, followed by wet chemical immersion treatments in gallium nitrate (1 mM). Different buffers such as phosphate, sodium bicarbonate, ammonium acetate, and citrate were added to the solution to maintain a pH value in the range of 6.5–6.9. Coating morphology and HAP phases were retained after treatment with gallium nitrate, and Ga3+ ion presence on the surface up to 1 wt.% was confirmed. Combining Ga and HAP shows great promise to enable the local delivery of Ga3+ ions and consequent antibacterial protection during bone regeneration, without using growth factors or antibiotics.
Designing 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, Annett
Additive 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.
Effect 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, Annett
Metastable 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.
Effect 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, Annett
Selective 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
Electrodeposition 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, Michael
Beta-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
Experimental 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, Martina
Lattices 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.
Fabrication 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, Tim
Complex 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.
Functionalization of Ti-40Nb implant material with strontium by reactive sputtering
(London : BioMed Central, 2017-10-10) Göttlicher, Markus; Rohnke, Marcus; Moryson, Yannik; Thomas, Jürgen; Sann, Joachim; Lode, Anja; Schumacher, Matthias; Schmidt, Romy; Pilz, Stefan; Gebert, Annett; Gemming, Thomas; Janek, Jürgen
Background: Surface functionalization of orthopedic implants with pharmaceutically active agents is a modern approach to enhance osseointegration in systemically altered bone. A local release of strontium, a verified bone building therapeutic agent, at the fracture site would diminish side effects, which could occur otherwise by oral administration. Strontium surface functionalization of specially designed titanium-niobium (Ti-40Nb) implant alloy would provide an advanced implant system that is mechanically adapted to altered bone with the ability to stimulate bone formation. Methods: Strontium-containing coatings were prepared by reactive sputtering of strontium chloride (SrCl2) in a self-constructed capacitively coupled radio frequency (RF) plasma reactor. Film morphology, structure and composition were investigated by scanning electron microscopy (SEM), time of flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). High-resolution transmission electron microscopy (HR-TEM) was used for the investigation of thickness and growth direction of the product layer. TEM lamellae were prepared using the focused ion beam (FIB) technique. Bioactivity of the surface coatings was tested by cultivation of primary human osteoblasts and subsequent analysis of cell morphology, viability, proliferation and differentiation. The results are correlated with the amount of strontium that is released from the coating in biomedical buffer solution, quantified by inductively coupled plasma mass spectrometry (ICP-MS). Results: Dense coatings, consisting of SrOxCly, of more than 100 nm thickness and columnar structure, were prepared. TEM images of cross sections clearly show an incoherent but well-structured interface between coating and substrate without any cracks. Sr2+ is released from the SrOxCly coating into physiological solution as proven by ICP-MS analysis. Cell culture studies showed excellent biocompatibility of the functionalized alloy. Conclusions: Ti-40Nb alloy, a potential orthopedic implant material for osteoporosis patients, could be successfully plasma coated with a dense SrOxCly film. The material performed well in in vitro tests. Nevertheless, the Sr2+ release must be optimized in future work to meet the requirements of an effective drug delivery system.
Novel 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, Mariana
This 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.
Polyelectrolyte complex based interfacial drug delivery system with controlled loading and improved release performance for bone therapeutics
(Basel : MDPI, 2016) Vehlow, David; Schmidt, Romy; Gebert, Annett; Siebert, Maximilian; Lips, Katrin Susanne; Müller, Martin
An improved interfacial drug delivery system (DDS) based on polyelectrolyte complex (PEC) coatings with controlled drug loading and improved release performance was elaborated. The cationic homopolypeptide poly(l-lysine) (PLL) was complexed with a mixture of two cellulose sulfates (CS) of low and high degree of substitution, so that the CS and PLL solution have around equal molar charged units. As drugs the antibiotic rifampicin (RIF) and the bisphosphonate risedronate (RIS) were integrated. As an important advantage over previous PEC systems this one can be centrifuged, the supernatant discarded, the dense pellet phase (coacervate) separated, and again redispersed in fresh water phase. This behavior has three benefits: (i) Access to the loading capacity of the drug, since the concentration of the free drug can be measured by spectroscopy; (ii) lower initial burst and higher residual amount of drug due to removal of unbound drug and (iii) complete adhesive stability due to the removal of polyelectrolytes (PEL) excess component. It was found that the pH value and ionic strength strongly affected drug content and release of RIS and RIF. At the clinically relevant implant material (Ti40Nb) similar PEC adhesive and drug release properties compared to the model substrate were found. Unloaded PEC coatings at Ti40Nb showed a similar number and morphology of above cultivated human mesenchymal stem cells (hMSC) compared to uncoated Ti40Nb and resulted in considerable production of bone mineral. RIS loaded PEC coatings showed similar effects after 24 h but resulted in reduced number and unhealthy appearance of hMSC after 48 h due to cell toxicity of RIS.
Production of porous β-Type Ti–40Nb alloy for biomedical applications: Comparison of selective laser melting and hot pressing
(Basel : MDPI, 2013) Zhuravleva, Ksenia; Bönisch, Matthias; Prashanth, Konda Gokuldoss; Hempel, Ute; Helth, Arne; Gemming, Thomas; Calin, Mariana; Scudino, Sergio; Schultz, Ludwig; Eckert, Jürgen; Gebert, Annett
We used selective laser melting (SLM) and hot pressing of mechanically-alloyed β-type Ti–40Nb powder to fabricate macroporous bulk specimens (solid cylinders). The total porosity, compressive strength, and compressive elastic modulus of the SLM-fabricated material were determined as 17% ± 1%, 968 ± 8 MPa, and 33 ± 2 GPa, respectively. The alloy’s elastic modulus is comparable to that of healthy cancellous bone. The comparable results for the hot-pressed material were 3% ± 2%, 1400 ± 19 MPa, and 77 ± 3 GPa. This difference in mechanical properties results from different porosity and phase composition of the two alloys. Both SLM-fabricated and hot-pressed cylinders demonstrated good in vitro biocompatibility. The presented results suggest that the SLM-fabricated alloy may be preferable to the hot-pressed alloy for biomedical applications, such as the manufacture of load-bearing metallic components for total joint replacements.
Strontium substitution of gelatin modified calcium hydrogen phosphates as porous hard tissue substitutes
(New York, NY [u.a.] : Wiley, 2020) Kruppke, Benjamin; Heinemann, Christiane; Gebert, Annett; Rohnke, Marcus; Weiß, Manuel; Henß, Anja; Wiesmann, Hans-Peter; Hanke, Thomas
Aiming at the generation of a high strontium-containing degradable bone substitute, the exchange of calcium with strontium in gelatin-modified brushite was investigated. The ion substitution showed two mineral groups, the high-calcium containing minerals with a maximum measured molar Ca/Sr ratio of 80%/20% (mass ratio 63%/37%) and the high-strontium containing ones with a maximum measured molar Ca/Sr ratio of 21%/79% (mass ratio 10%/90%). In contrast to the high-strontium mineral phases, a high mass loss was observed for the calcium-based minerals during incubation in cell culture medium (alpha-MEM), but also an increase in strength owing to dissolution and re-precipitation. This resulted for the former in a decrease of cation concentration (Ca + Sr) in the medium, while the pH value decreased and the phosphate ion concentration rose significantly. The latter group of materials, the high-strontium containing ones, showed only a moderate change in mass and a decrease in strength, but the Ca + Sr concentration remained permanently above the initial calcium concentration in the medium. This might be advantageous for a future planned application by supporting bone regeneration on the cellular level. © 2020 The Authors. Journal of Biomedical Materials Research Part A published by Wiley Periodicals LLC.
Structure-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, Martina
Lattices 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.

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