The Characterization of a Biodegradable Mg Alloy after Powder Bed Fusion with Laser Beam/Metal Processing for Custom Shaped Implants.

A new Mg-Zn-Zr-Ca alloy in a powder state, intended to be used for custom shaped implants, was obtained via a mechanical alloying method from pure elemental powder. Further, the obtained powder alloy was processed by a PBF-LB/M (powder bed fusion with laser beam/of metal) procedure to obtain additive manufactured samples for small biodegradable implants. A series of microstructural, mechanical and corrosion analyses were performed. The SEM (scanning electron microscopy) analysis of the powder alloy revealed a good dimensional homogeneity, with a uniform colour, no agglutination and almost rounded particles, suitable for the powder bed fusion procedure. Further, the PBF-LB/M samples revealed a robust and unbreakable morphology, with a suitable porosity (that can reproduce that of cortical bone) and without an undesirable balling effect. The tested Young's modulus of the PBF-LB/M samples, which was 42 GPa, is close to that of cortical bone, 30 GPa. The corrosion tests that were performed in PBS (Phosphate-buffered saline) solution, with three different pH values, show that the corrosion parameters have a satisfactory evolution comparative to the commercial ZK 60 alloy.

Biodegradable Magnesium Alloys for Personalised Temporary Implants.

The objective of this experimental work was to examine and characterise the route for obtaining demonstrative temporary biodegradable personalised implants from the Mg alloy Mg-10Zn-0.5Zr-0.8Ca (wt.%). This studied Mg alloy was obtained in its powder state using the mechanical alloying method, with shape and size characteristics suitable for ensuing 3D additive manufacturing using the SLM (selective laser melting) procedure. The SLM procedure was applied to various processing parameters. All obtained samples were characterised microstructurally (using XRD-X-ray diffraction, and SEM-scanning electron microscopy); mechanically, by applying a compression test; and, finally, from a corrosion resistance viewpoint. Using the optimal test processing parameters, a few demonstrative temporary implants of small dimensions were made via the SLM method. Our conclusion is that mechanical alloying combined with SLM processing has good potential to manage 3D additive manufacturing for personalised temporary biodegradable implants of magnesium alloys. The compression tests show results closer to those of human bones compared to other potential metallic alloys. The applied corrosion test shows result comparable with that of the commercial magnesium alloy ZK60.

Microstructural Considerations of a Multi-Pass Rolled Ti-Nb-Ta-Zr Alloy.

The microstructural characteristic evolution was investigated during thermomechanical processing of Ti-29Nb-9Ta-10Zr (wt %) alloy, which consisted of, in a first stage, in a Multi-Pass Rolling with increasing thickness reduction of 20%, 40%, 60%, 80%, and 90%; in step two, the multi-pass rolled sample with the highest thickness reduction (90%) was subjected to a series of three variants of static short recrystallization and then to a final similar aging. The objective was to evaluate the microstructural features evolution during thermomechanical processing (phase's nature, morphology, dimensions, and crystallographic characteristics) and to find the optimal heat treatment variant for refinement of the alloy granulation until ultrafine/nanometric level for a promising combination of mechanical properties. The microstructural features were investigated by X-ray diffraction and SEM techniques through which the presence of two phases was recorded: the ß-Ti phase and the α″-Ti martensitic phase. The corresponding cell parameters, dimensions of the coherent crystallite and the micro-deformations at the crystalline network level for both recorded phases were determined. The majority ß-Ti phase underwent a strong refinement during the Multi-Pass Rolling process until ultrafine/nano grain dimension (about 9.8 nm), with subsequent slow growing during recrystallization and aging treatments, hindered by the presence of sub-micron α″-Ti phase dispersed inside ß-Ti grains. An analysis concerning the possible deformation mechanisms was performed.

{332}<113> and {112}<111> Twin Variant Activation during Cold-Rolling of a Ti-Nb-Zr-Ta-Sn-Fe Alloy

Deformation twinning is a phenomenon that causes local shear strain concentrations, with the material either experiencing elongation (and thus a tensile stress) or contraction (compressive stress) along the stress directions. Thus, in order to gauge the performance of the alloy better, it is imperative to predict the activation of twinning systems successfully. The present study investigates the effects of deformation by cold-rolling on the {332}<113> and {112}<111> twin variant activation in a Ti-30Nb-12Zr-5Ta-2Sn-1.25Fe (wt.%) (TNZTSF) alloy. The Ti-30Nb-12Zr-5Ta-2Sn-1.25Fe (wt.%) alloy was synthesized in a cold crucible induction levitation furnace, under an argon-controlled atmosphere, using high-purity elemental components. The TNZTSF alloy was cold-deformed by rolling, in one single step, with a total deformation degree (thickness reduction) of ε ≈ 1% (CR 1), ε ≈ 3% (CR 3), and ε ≈ 15% (CR 15). The microstructural investigations were carried out with the SEM-EBSD technique in order to determine the grain morphology, grain-size distribution, crystallographic orientation, accumulated strain-stress fields and Schmid Factor (SF) analysis, all necessary to identify the active twin variants. The EBSD data were processed using an MTEX Toolbox ver. 5.7.0 software package. The results indicated that the TNZTSF alloy's initial microstructure consists of a homogeneous ß-Ti single phase that exhibits equiaxed polyhedral grains and an average grain-size close to 71 µm. It was shown that even starting with a 1% total deformation degree, the microstructure shows the presence of the {332}<113> twinning ((233)[3¯11] active twin variant; Schmit factor SF = −0.487); at a 3% total deformation degree, one can notice the presence of primary and secondary twin variants within the same grain belonging to the same {332}<113> twinning system ((323¯)[13¯1¯] primary twin variant­SF = −0.460; (233¯)[3¯11¯] secondary twin variant­SF = −0.451), while, at a 15% total deformation degree, besides the {332}<113> twinning system, one can notice the activation of the {112}<111> twinning system ((11¯2)[1¯11] active twin variant­SF = −0.440). This study shows the {332}<113> and {112}<111> twinning variant activation during cold-deformation by rolling in the case of a Ti-30Nb-12Zr-5Ta-2Sn-1.25Fe (wt.%) (TNZTSF) alloy.

Laser Powder Bed Fusion Applied to a New Biodegradable Mg-Zn-Zr-Ca Alloy.

The aim of the present paper is to apply the laser powder bed fusion process to a new biodegradable Mg-Zn-Zr-Ca alloy powder prepared via a mechanical alloying method from powder pure components. This additive manufacturing method is expected to allow for the obtaining of high biomechanical and biochemical performance. Various processing parameters for laser powder bed fusion are tested, with a special focus on laser energy density-E [J/mm3]-which is calculated for all experiment variants, and which represents an important processing parameter, dependent upon all the rest. The goal of all the trials is to find the most efficient schema for the production of small biodegradable parts for the medical domain, meaning the selection of optimal processing parameters. An important observation is that the most robust and homogeneous samples without cracks are obtained for lower values of the E, around 100 J/mm3. Thus, the most performant samples are analyzed by scanning electron microscopy, X-ray diffraction and by compression mechanical test.

Microstructure Evolution during Hot Deformation of UNS S32750 Super-Duplex Stainless Steel Alloy.

The present paper analyzes UNS S32750 Super-Duplex Stainless Steel hot deformation behavior during processing by upsetting. The objective of this paper is to determine the optimum range of deformation temperatures, considering that both austenite and ferrite have different deformation behaviors due to their different morphology, physical, and mechanical properties. Because the capability of plastic deformation accommodation of ferrite is reduced when compared to austenite, side cracks and fissures can form during the hot deformation process. Consequently, it is important to find the optimum conditions of deformation of this type of stainless steel to establish the best processing parameters without deteriorating the material. The experimental program involved the application of hot deformation by the upsetting method on a series of samples between 1000 °C and 1275 °C, with a total degree of deformation of 30%. The resultant samples were examined by SEM-EBSD to establish and analyze the evolution of the phases present in the structure from several points of view: nature, distribution, morphology (size and shape), and their structural homogeneity. The GROD (Grain Reference Orientation Deviation) distribution map was also determined while taking into account the possible precipitation of the secondary austenite phase (γ2-phase) and the analysis of the dynamic recrystallization process according to the applied deformation temperature. The main conclusion was that UNS S32750 SDSS steel can be safely deformed by upsetting between 1050-1275 °C, with an experimented total degree of deformation of 30%.

Tailoring a Low Young Modulus for a Beta Titanium Alloy by Combining Severe Plastic Deformation with Solution Treatment.

The present paper analyzed the microstructural characteristics and the mechanical properties of a Ti-Nb-Zr-Fe-O alloy of ß-Ti type obtained by combining severe plastic deformation (SPD), for which the total reduction was of εtot = 90%, with two variants of super-transus solution treatment (ST). The objective was to obtain a low Young's modulus with sufficient high strength in purpose to use the alloy as a biomaterial for orthopedic implants. The microstructure analysis was conducted through X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM) investigations. The analyzed mechanical properties reveal promising values for yield strength (YS) and ultimate tensile strength (UTS) of about 770 and 1100 MPa, respectively, with a low value of Young's modulus of about 48-49 GPa. The conclusion is that satisfactory mechanical properties for this type of alloy can be obtained if considering a proper combination of SPD + ST parameters and a suitable content of ß-stabilizing alloying elements, especially the Zr/Nb ratio.

Influence of ageing treatment temperature and duration on σ-phase precipitation and mechanical properties of UNS S32750 SDSS alloy.

Introduction: Super-Duplex Stainless Steeles (SDSS) proved an excellent potential for its use in many chemical and offshore applications due to their both high mechanical properties and a high corrosion resistance in chloride ion solutions. Objectives: This study evaluates the influence of ageing treatment temperature and duration on σ-phase precipitation and mechanical properties of UNS S32750 SDSS alloy. Methods: The influence of ageing treatment on microstructural features was analysed by SEM-EBSD (Scanning Electron Microscopy - Electron Backscatter Diffraction) technique, while on mechanical properties by tensile and impact testing techniques. Results: The obtained results show that for the short duration ageing treatments the σ-phase nucleates, within the δ-phase matrix, at the δ/γ grains boundary by the δ → σ precipitation, while for long duration ageing treatments the σ-phase nucleates, within the δ-phase matrix, at the δ/δ grains boundary, or in other favourable nucleation sites, due to the eutectoid decomposition δ → σ + γ2. Experimental data showed that at low temperatures, i.e. 780 °C, in order to induce the precipitation of σ-phase, the minimum incubation time is situated close to 20 min, and that increasing treatment temperature decreases the minimum incubation time, with at 850 °C and 920 °C the σ-phase being firstly detected at 5 min. The σ-phase precipitation shows the highest precipitation kinetics at 850 °C, when the maximum weight-fraction is obtained for each treatment duration when compared with ageing treatments performed at 780 °C and 920 °C. Conclusion: All presented data brings valuable insight into the σ-phase precipitation phenomena and its influence on UNS S32750 SDSS alloy's exhibited mechanical properties and, also, can provide researchers and industrial steel processors a guide regarding the selection of optimal ageing treatment parameters to avoid/minimise the embrittlement induced by the precipitation of deleterious σ-phase.