The effect of severe plastic deformation on the structure, mechanical properties, corrosion resistance, and biocompatibility of the WE43 (Mg-Y-Nd-Zr) alloy earmarked for applications as bioresorbable material has been studied. The alloy was deformed by rotary swaging (RS), equal channel angular pressing (ECAP), and multiaxial deformation (MAD). The microstructure examination by transmission electron microscopy showed that all SPD modes lead to the formation of ultrafine-grained structure with a structural element size of 0.5-1 µm and the Mg 12 Nd phase particles 0.3 µm in size. The microstructure refinement by all three treatments resulted in strengthening of the alloy. ECAP and MAD also raised ductility to up to 12-17%, while RS increased the ultimate tensile strength to up to 415 MPa. The study of the corrosion properties showed that SPD does not affect the electrochemical corrosion of the alloy. Its biocompatibility in vitro was estimated after incubation of the samples with red blood cells (hemolysis study), white blood cells (cell viability assay), and mesenchymal stromal cells (cell proliferation analysis). The biodegradation rate in fetal bovine serum was also evaluated. ECAP and MAD were found to cause some deceleration of biodegradation by slowing down the gas formation in the biological fluid and, compared to MSC, to improve the biocompatibility of the WE43 alloy.
In this work, the effect of an ultrafine-grained (UFG) structure obtained by multiaxial deformation (MAD) on the mechanical properties, fatigue strength, biodegradation, and biocompatibility in vivo of the magnesium alloy WE43 was studied. The grain refinement down to 0.93 ± 0.29 µm and the formation of Mg41Nd5 phase particles with an average size of 0.34 ± 0.21 µm were shown to raise the ultimate tensile strength to 300 MPa. Besides, MAD improved the ductility of the alloy, boosting the total elongation from 9% to 17.2%. An additional positive effect of MAD was an increase in the fatigue strength of the alloy from 90 to 165 MPa. The formation of the UFG structure also reduced the biodegradation rate of the alloy under both in vitro and in vivo conditions. The relative mass loss after six weeks of experiment was 83% and 19% in vitro and 46% and 7% in vivo for the initial and the deformed alloy, respectively. Accumulation of hydrogen and the formation of necrotic masses were observed after implantation of alloy specimens in both conditions. Despite these detrimental phenomena, the desired replacement of the implant and the surrounding cavity with new connective tissue was observed in the areas of implantation.
The effect of equal channel angular pressing (ECAP) on the microstructure, texture, mechanical properties, and corrosion resistance of the alloys Mg-6.0%Ag and Mg-10.0%Gd was studied. It was shown that ECAP leads to grain refinement of the alloys down to the average grain size of 2–3 μm and 1–2 μm, respectively. In addition, in both alloys the precipitation of fine particles of phases Mg54Ag17 and Mg5Gd with sizes of ~500–600 and ~400–500 nm and a volume fraction of ~9% and ~8.6%, respectively, was observed. In the case of the alloy Mg-6.0%Ag, despite a significant grain refinement, a drop in the strength characteristics and a nearly twofold increase in ductility (up to ~30%) was found. This behavior is associated with the formation of a sharp inclined basal texture. For alloy Mg-10.0%Gd, both ductility and strength were enhanced, which can be associated with the combined effect of significant grain refinement and an increased probability of prismatic and basal glide. ECAP was also shown to cause a substantial rise of the biodegradation rate of both alloys and an increase in pitting corrosion. The latter effect is attributed to an increase in the dislocation density induced by ECAP and the occurrence of micro-galvanic corrosion at the matrix/particle interfaces.
The effect of equal-channel angular pressing (ECAP) on the microstructure, texture, mechanical properties, corrosion resistance and cytotoxicity of two magnesium-silver alloys, Mg-2.0%Ag and Mg-4.0%Ag, was studied. Their average grain size was found to be reduced to 3.2 ± 1.4 μm and 2.8 ± 1.3 μm, respectively. Despite the substantial grain refinement, a drop in the strength characteristics of the alloys was observed, which can be attributed to the formation of inclined basal texture. On a positive side, an increase in tensile ductility to ~34% for Mg-2.0%Ag and ~27% for Mg-4.0%Ag was observed. This effect can be associated with the activity of basal and prismatic slip induced by ECAP. One of the ECAP regimes tested gave rise to a drop in the corrosion resistance of both alloys. An interesting observation was a cytotoxic effect both alloys had on tumor cells in vitro. This effect was accompanied with the release of lactate dehydrogenase, an increase in oxidative stress, coupled with the induction of NO-ions and an increase in the content of such markers of apoptosis as Annexin V and Caspase 3/7. Differences in the chemical composition and the processing history-dependent microstructure of the alloys did not have any significant effect on the magnitude of their antiproliferative effect.
Widespread use of Mg-Zn-Ca alloys in clinical orthopedic practice requires improvement of their mechanical properties—in particular, ductility—and enhancement of their bioactivity for accelerated osteoreconstruction. The alloy was studied in two structural states: after homogenization and after equal-channel angular pressing. Immersion and potentiodynamic polarization tests showed that the corrosion rate of the alloy was not increased by deformation. The mass loss in vivo was also statistically insignificant. Furthermore, it was found that deformation did not compromise the biocompatibility of the alloy and did not have any significant effect on cell adhesion and proliferation. However, an extract of the alloy promoted the alkaline phosphatase activity of human mesenchymal stromal cells, which indicates osteogenic stimulation of cells. The osteoinduction of the deformed alloy significantly exceeded that of the homogenized one. Based on the results of this work, it can be concluded that the alloy Mg-1%Zn-0.3%Ca modified by equal-channel angular pressing is a promising candidate for the manufacture of biodegradable orthopedic implants since it stimulates osteogenic differentiation and has greater ductility, which provides it with a competitive advantage in comparison with the homogenized state.