The Fe-Mn-Si shape memory alloys are considered promising materials for the biodegradable bone implant application since their functional properties can be optimized to combine bioresorbability with biomechanical and biochemical compatibility with bone tissue. The present study focuses on the fatigue and corrosion fatigue behavior of the thermomechanically treated Fe-30Mn-5Si (wt %) alloy compared to the conventionally quenched alloy because this important functionality aspect has not been previously studied. Hot-rolled and water-cooled, cold-rolled and annealed, and conventionally quenched alloy samples were characterized by X-ray diffraction, transmission electron microscopy, tensile fatigue testing in air atmosphere, and bending corrosion fatigue testing in Hanks’ solution. It is shown that hot rolling at 800 °C results in the longest fatigue life of the alloy both in air and in Hanks’ solution. This advantage results from the formation of a dynamically recrystallized γ-phase grain structure with a well-developed dislocation substructure. Another important finding is the experimental verification of Young’s modulus anomalous temperature dependence for the studied alloy system, its minimum at a human body temperature, and corresponding improvement of the biomechanical compatibility. The idea was realized by lowering Ms temperature down to the body temperature after hot rolling at 800 °C.
11 November 2020 in Journal of Manufacturing Science and Engineering
Improving the post-processing of metallic porous tissue scaffolds is an essential step to create a new generation of superelastic implants for the replacement of damaged bone tissue. In this study, the dynamic chemical etching technique is applied to improve the permeability and to optimize the porous structure of Ti-Nb-Zr scaffolds fabricated by the powder metallurgy-based space holder technique. The etched scaffolds are characterised in terms of their porous structure geometry, permeability, and mechanical properties. It is shown that an increase in porosity from 49% to 54% during the etching is mainly due to an increase in the number of 100 to 800 µm-diameter pores; from 30 to 50% of them measuring from 100 to 300 µm in size. These changes in the porous structure lead to a significant increase of its permeability, i.e. from (0.1-15)×10−11 m2 before etching to (44-91)×10−11 m2, after etching; these permeability ranges corresponding to those of bone tissues. Furthermore, the etched scaffolds show systematically higher yield compressive stresses as compared to the as-sintered scaffolds of equivalent porosities. Finally, the highly-permeable etched Ti-Nb-Zr scaffolds with a porosity varying from 40 to 60% exhibit an apparent Youngs modulus ranging from 8.6 to 1.9 GPa, and an ultimate compressive strength, from 650 to 190 MPa, which can be considered as a promising balance of properties for the potential use of these scaffolds as bone implants.
Titanium alloys are well recognized as appropriate materials for biomedical implants. These devices are designed to operate in quite aggressive human body media, so it is important to study the corrosion and electrochemical behavior of the novel materials alongside the underlying chemical and structural features. In the present study, the prospective Ti‒Zr-based superelastic alloys (Ti-18Zr-14Nb, Ti-18Zr-15Nb, Ti-18Zr-13Nb-1Ta, atom %) were analyzed in terms of their phase composition, functional mechanical properties, the composition and structure of surface oxide films, and the corresponding corrosion and electrochemical behavior in Hanks’ simulated biological solution. The electrochemical parameters of the Ti-18Zr-14Nb material in bulk and foam states were also compared. The results show a significant difference in the functional performance of the studied materials, with different composition and structure states. In particular, the positive effect of the thermomechanical treatment regime, leading to the formation of a favorable microstructure on the corrosion resistance, has been revealed. In general, the Ti-18Zr-15Nb alloy exhibits the optimum combination of functional characteristics in Hanks’ solution, while the Ti-18Zr-13Nb-1Ta alloy shows the highest resistance to the corrosion environment. The Ti-18Zr-14Nb-based foam material exhibits slightly lower passivation kinetics as compared to its bulk equivalent.
In this study, a superelastic Ti-18Zr-15Nb (at. %) alloy was subjected to thermomechanical treatment, including cold rotary forging, intermediate annealing, cold drawing, post-deformation annealing, and additional low-temperature aging. As a result of intermediate annealing, two structures of β-phase were obtained: a fine-grained structure (d ≈ 3 µm) and a coarse-grained structure (d ≈ 11 µm). Cold drawing promotes grain elongation in the drawing direction; in a fine-grained state, grains form with a size of 4 × 2 µm, and in a coarse-grained state, they grow with a size of 16 × 6 µm. Post-deformation annealing (PDA) at 550 °C for 30 min leads to grain sizes of 5 µm and 3 µm, respectively. After PDA at 550 °C (30 min) in the fine-grained state, the wire exhibits high tensile strength (UTS = 624 MPa), highest elongation to failure (δ ≥ 8%), and maximum difference between the dislocation and transformation yield stresses, as well as the highest superelastic recovery strain (εrSE ≥ 3.3%) and total elastic + superelastic recovery strain (εrel+SE ≥ 5.4%). Additional low-temperature aging at 300 °C for 30–180 min leads to ω-phase formation, alloy hardening, embrittlement, and a significant decrease in superelastic recovery strain.
Biomedical Ti-22Nb-6Zr, Ti-18Zr-15Nb, and Ti-41Zr-12Nb (at.%) shape memory alloys were subjected to cold rolling (CR) and subsequent post-deformation annealing (PDA). The evolutions of phase and structure states, crystallographic texture, and crystallographic limit of recovery strain were studied using EBSD, TEM, and XRD analyses. The study found that CR (e = 1.5) and PDA at 800 °C for 30 min results in fine- and coarse-grained structures. Severe CR (e = 3.0) and PDA at 550 °C for 5 min results in a recrystallized, equiaxed, predominantly ultrafine-grained structure of the β-phase with a small amount of low-angle boundaries. Increasing the degree of CR from moderate (e = 0.3) to severe (e = 3.0) results in a favorable strong {111}ββ recrystallization texture. Alloys with low Zr content are more susceptible to this type of crystallographic texture formation during TMT, primarily due to a higher Nb content. The Ti-41Zr-12Nb alloy shows the highest crystallographic limit of recovery strain (εrmax ≈ 6%). The limit decreases to ≈5% (for Ti-18Zr-15Nb) and ≈3% (for Ti-22Nb-6Zr) when transitioning from high- to low-Zr alloys. The transition of Ti-Zr-Nb alloys from coarse-grained to ultrafine-grained structures of the β-phase and a decrease in grain size do not affect the crystallographic limit of recovery strain in the studied grain size ranges.