Jiří Kubásek

Structure, mechanical characteristics and in vitro degradation, cytotoxicity, genotoxicity and mutagenicity of novel biodegradable Zn-Mg alloys.

Zn-(0-1.6)Mg (in wt.%) alloys were prepared by hot extrusion at 300 °C. The structure, mechanical properties and in vitro biocompatibility of the alloys were investigated. The hot-extruded magnesium-based WE43 alloy was used as a control. Mechanical properties were evaluated by hardness, compressive and tensile testing. The cytotoxicity, genotoxicity (comet assay) and mutagenicity (Ames test) of the alloy extracts and ZnCl2 solutions were evaluated with the use of murine fibroblasts L929 and human osteosarcoma cell line U-2 OS. The microstructure of the Zn alloys consisted of recrystallized Zn grains of 12 μm in size and fine Mg2Zn11 particles arranged parallel to the hot extrusion direction. Mechanical tests revealed that the hardness and strength increased with increasing Mg concentration. The Zn-0.8 Mg alloys showed the best combination of tensile mechanical properties (tensile yield strength of 203 MPa, ultimate tensile strength of 301 MPa and elongation of 15%). At higher Mg concentrations the plasticity of Zn-Mg alloys was deteriorated. Cytotoxicity tests with alloy extracts and ZnCl2 solutions proved the maximum safe Zn(2+) concentrations of 120 μM and 80 μM for the U-2 OS and L929 cell lines, respectively. Ames test with extracts of alloys indicated that the extracts were not mutagenic. The comet assay demonstrated that 1-day extracts of alloys were not genotoxic for U-2 OS and L929 cell lines after 1-day incubation.

Structure, mechanical properties, corrosion behavior and cytotoxicity of biodegradable Mg–X (X = Sn, Ga, In) alloys

As-cast Mg-Sn, Mg-Ga and Mg-In alloys containing 1-7 wt.% of alloying elements were studied in this work. Structural and chemical analysis of the alloys was performed by using light and scanning electron microscopy, energy dispersive spectrometry, x-ray diffraction, x-ray photoelectron spectroscopy and glow discharge spectrometry. Mechanical properties were determined by Vickers hardness measurements and tensile testing. Corrosion behavior in a simulated physiological solution (9 g/l NaCl) was studied by immersion tests and potentiodynamic measurements. The cytotoxicity effect of the alloys on human osteosarcoma cells (U-2 OS) was determined by an indirect contact assay. Structural investigation revealed the dendritic morphology of the as-cast alloys with the presence of secondary eutectic phases in the Mg-Sn and Mg-Ga alloys. All the alloying elements showed hardening and strengthening effects on magnesium. This effect was the most pronounced in the case of Ga. All the alloying elements at low concentrations of approximately 1 wt.% were also shown to positively affect the corrosion resistance of Mg. But at higher concentrations of Ga and Sn the corrosion resistance worsened due to galvanic effects of secondary phases. Cytotoxicity tests indicated that Ga had the lowest toxicity, followed by Sn. The most severe toxicity was observed in the case of In.

Highly porous, low elastic modulus 316L stainless steel scaffold prepared by selective laser melting

Recently, porous metallic materials have been extensively studied as candidates for use in the fabrication of scaffolds and augmentations to repair trabecular bone defects, e.g. in surroundings of joint replacements. Fabricating these complex structures by using common approaches (e.g., casting and machining) is very challenging. Therefore, rapid prototyping techniques, such as selective laser melting (SLM), have been investigated for these applications. In this study, we characterized a highly porous (87 vol.%) 316L stainless steel scaffold prepared by SLM. 316L steel was chosen because it presents a biomaterial still widely used for fabrication of joint replacements and, from the practical point of view, use of the same material for fabrication of an augmentation and a joint replacement is beneficial for corrosion prevention. The results are compared to the reported properties of two representative nonporous 316L stainless steels prepared either by SLM or casting and subsequent hot forging. The microstructural and mechanical properties and the surface chemical composition and interaction with the cells were investigated. The studied material exhibited mechanical properties that were similar to those of trabecular bone (compressive modulus of elasticity ~0.15GPa, compressive yield strength ~3MPa) and cytocompatibility after one day that was similar to that of wrought 316L stainless steel, which is a commonly used biomaterial. Based on the obtained results, SLM is a suitable method for the fabrication of porous 316L stainless steel scaffolds with highly porous structures.

Microstructural, mechanical, corrosion and cytotoxicity characterization of the hot forged FeMn30(wt.%) alloy.

An interest in biodegradable metallic materials has been increasing in the last two decades. Besides magnesium based materials, iron-manganese alloys have been considered as possible candidates for fabrication of biodegradable stents and orthopedic implants. In this study, we prepared a hot forged FeMn30 (wt.%) alloy and investigated its microstructural, mechanical and corrosion characteristics as well as cytotoxicity towards mouse L 929 fibroblasts. The obtained results were compared with those of iron. The FeMn30 alloy was composed of antiferromagnetic γ-austenite and ε-martensite phases and possessed better mechanical properties than iron and even that of 316 L steel. The potentiodynamic measurements in simulated body fluids showed that alloying with manganese lowered the free corrosion potential and enhanced the corrosion rate, compared to iron. On the other hand, the corrosion rate of FeMn30 obtained by a semi-static immersion test was significantly lower than that of iron, most likely due to a higher degree of alkalization in sample surrounding. The presence of manganese in the alloy slightly enhanced toxicity towards the L 929 cells; however, the toxicity did not exceed the allowed limit and FeMn30 alloy fulfilled the requirements of the ISO 10993-5 standard.

Influence of surface pre-treatment on the cytocompatibility of a novel biodegradable ZnMg alloy.

Degradable zinc-based alloys with an appropriate corrosion rate are promising materials for the preparation of temporary orthopaedic implants. Previously, we prepared and characterised a novel Zn1.5Mg alloy. This paper is focused on the characterisation of this alloy after a surface pre-treatment, which should mimic processes occurring in vivo. The samples of the Zn1.5Mg alloy were immersed in a simulated body fluid (SBF) at 37°C for 14days in order to form a protective layer of corrosion products. Thereafter, these samples were used for the corrosion rate determination, an indirect in vitro cytotoxicity test, as well as for a direct contact test and were compared with the non-treated samples. The protective layer was characterized by SEM and its chemical composition was determined by EDS and XPS analysis. The corrosion rate was significantly decreased after the pre-incubation. The protective layer of corrosion products was rich in Ca and P. The pre-incubated samples exhibited increased cytocompatibility in the indirect test (metabolic activity of L929 cells was above 70%) and we also observed osteoblast-like cell growth directly on the samples during the contact tests. Thus, the pre-incubation in SBF leading to improved cytocompatibility could represent more appropriate model to in vivo testing.

Microstructure and mechanical properties of the micrograined hypoeutectic Zn–Mg alloy

A biodegradable Zn alloy, Zn–1.6Mg, with the potential medical applications as a promising coating material for steel components was studied in this work. The alloy was prepared by three different procedures: gravity casting, hot extrusion, and a combination of rapid solidification and hot extrusion. The samples prepared were characterized by light microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction analysis. Vickers hardness, tensile, and compressive tests were performed to determine the samples’ mechanical properties. Structural examination reveals that the average grain sizes of samples prepared by gravity casting, hot extrusion, and rapid solidification followed by hot extrusion are 35.0, 9.7, and 2.1 μm, respectively. The micrograined sample with the finest grain size exhibits the highest hardness (Hv = 122 MPa), compressive yield strength (382 MPa), tensile yield strength (332 MPa), ultimate tensile strength (370 MPa), and elongation (9%). This sample also demonstrates the lowest work hardening in tension and temporary softening in compression among the prepared samples. The mechanical behavior of the samples is discussed in relation to the structural characteristics, Hall–Petch relationship, and deformation mechanisms in fine-grained hexagonal-close-packed metals.

3D printed porous stainless steel for potential use in medicine

3D printing technologies like Selective Laser Melting (SLM) or Electron Beam Melting (EBM) produce components of very complicated shapes from various kinds of materials. In this work a highly porous (porosity of almost 90 vol. %) stainless steel component was manufactured by SLM. The material was characterized in terms of structure, surface chemistry and mechanical properties. It was observed that mechanical properties of the material were similar to those of trabecular human bone. The tests realized in this work confirmed suitability of the porous material prepared by SLM for the use in medicine, for example, for scaffolds designed to repair bone defects.

Biodegradable Metallic Materials for Temporary Medical Implants

Biodegradable Mg, Zn and Fe alloys are currently studied as prospective biomaterials for temporary medical implants like stents for repairing damaged blood vessels and devices (screws and plates) for fixing fractured bones. In the present paper, novel Mg-, Zn- and Fe-biodegradable alloys are proposed. Advantages and disadvantages of the three kinds of alloys are demonstrated regarding the mechanical performance, in vitro corrosion behavior and biocompatibility.

Structural and mechanical study on Mg–xLM (x = 0–5 wt.%, LM = Sn, Ga) alloys

Abstract Low-melting point metals, such as Sn and Ga, can improve both the mechanical and corrosion properties of pure Mg. Currently, Mg–Sn based alloys are being considered for high-temperature applications, and both Mg–Sn and Mg–Ga based alloys are also being considered as possible candidates for biodegradable materials. Although these binary systems have already been the subject of research, only limited information on their characteristics has been published. Therefore, as-cast Mg–Sn and Mg–Ga alloys containing 1, 3.5 and 5 wt.% of alloying elements were studied in the present work. Moreover, the effect of extrusion on Mg–Sn and Mg–Ga alloys containing 3.5 wt.% of the alloying element was studied. Structural and chemical analyses of the alloys were performed by using light and scanning electron microscopy, energy dispersive spectrometry and X-ray diffraction. The mechanical properties were determined by Vickers hardness measurements and tensile and compressive testing. The as-cast alloys were characterized by a dendritic morphology with the presence of secondary eutectic phases. Both Sn and Ga exhibited hardening and strengthening effects on magnesium. The extruded alloys were characterized by fine-grained microstructures with a grain size of approximately 3 and 6 μm for Mg-3.5Sn and Mg-3.5Ga alloys, respectively, and significantly improved mechanical properties compared with the as-cast state. The ultimate tensile strength reached almost 250 MPa for both extruded alloys compared with 120–150 MPa for the as-cast condition. The results indicate that Mg–Sn- and Mg–Ga-based alloys appear to be suitable candidates for both engineering and medical applications.

Corrosion Behaviour of Magnesium Lithium Alloys in NaCl Solution

This work includes the comparison between corrosion resistance of MagLi4, MgLi7.5 and MgLi15 alloys in sodium chloride (0.15M NaCl) solution at 37°C. Results showed that the corrosion resistance is strongly determined by lithium content in the alloy. The worst corrosion resistance is typical for MgLi7.5 where the dual phase structure is observed. The magnesium - lithium alloys which contain less than 5% of Li and more than 11% (one phase structures) has got better corrosion resistance than dual phase structure magnesium – lithium alloys