Investigation into the hot workability of the as-extruded WE43 magnesium alloy using processing map.

The research concerned the characterization of the hot-working behavior of the as-extruded WE43 magnesium alloy potentially for biomedical applications and the construction of processing maps to guide the choice of forming process parameters. Isothermal uniaxial compression tests were performed over a temperature range of 350-480°C and strain rate range of 0.001-10s(-1). Flow stresses obtained were used to construct processing maps. Domains in processing maps corresponding to relevant deformation mechanisms, i.e., dynamic recrystallization (DRX), dynamic recovery (DRV) and flow instability, were identified, according to power dissipation efficiency and flow instability parameter values. Microstructures of compression-tested specimens were examined to validate these deformation mechanisms. Two mechanisms of DRX nucleation, i.e., particle-stimulated nucleation (PSN) and grain boundary bulging, were found to be operative at the low-temperature and high-temperature DRX domains, respectively. Flow instability was related to adiabatic shear bands and abnormal grain growth. An optimum condition for the hot working of this alloy was determined to be at a temperature of 475°C and a strain rate of 0.1s(-1).

Multipass cold drawing of magnesium alloy minitubes for biodegradable vascular stents.

Magnesium alloys possess highly limited room-temperature formabilities. This presents a technological barrier to the fabrication of minitubes for biodegradable vascular stents. The research was aimed at developing precision forming technology to fabricate ZM21 magnesium alloy minitubes with a refined microstructure. A multipass cold drawing process with a moving mandrel was successfully developed to convert seamless hollow billets through five passes of cold drawing and an interpass annealing treatment into minitubes with an outside diameter of 2.9 mm and a wall thickness of 0.217 mm, ready for laser cutting into vascular stents. It was found that a cumulative reduction in cross-section area as much as 32% could be applied to the material without causing fracture. However, a further reduction in cross-section area required annealing at 300°C for 1h to change a twinned microstructure into a recrystallized grain structure and to regain formability. The interpass annealing treatment after the fourth pass led to a reduction in drawing force by 22%, in comparison with the drawing force at the fourth pass of drawing. The variations in the outside diameter and wall thickness of the minitubes could be kept within 5 and 12 µm, respectively. Further research is directed toward improvements in dimensional precisions.

Porous TiO2 surface formed on nickel-titanium alloy by plasma electrolytic oxidation: a prospective polymer-free reservoir for drug eluting stent applications.

In this study, a porous oxide layer was formed on the surface of nickel-titanium alloy (NiTi) by plasma electrolytic oxidation (PEO) with the aim to produce a polymer-free drug carrier for drug eluting stent (DES) applications. The oxidation was performed galvanostatically in concentrated phosphoric acid electrolyte at low temperature. It was found that the response of NiTi substrate during the PEO process was different from that of bulk Ti, since the presence of large amount of Ni delayed the initial formation of a compact oxide layer that is essential for the PEO to take place. Under optimized PEO conditions, the resultant surface showed porosity, pore density and oxide layer thickness of 14.11%, 2.40 × 105 pores/mm² and 0.8 µm, respectively. It was additionally noted that surface roughness after PEO did not significantly increase as compared with that of original NiTi substrate and the EDS analyses revealed a decrease in Ni/Ti ratio on the surface after PEO. The cross-section morphology showed no discontinuity between the PEO layer and the NiTi substrate. Furthermore, wettability and surface free energy of the NiTi substrate increased significantly after PEO treatment. The PEO process could be successfully translated to NiTi stent configuration proving for the first time its feasibility for such a medical device and offering potential for development of alternative, polymer-free drug carriers for NiTi DES.

Characterization of Porous TiO2 Surfaces Formed on 316L Stainless Steel by Plasma Electrolytic Oxidation for Stent Applications.

In this study, a porous oxide layer was formed on the surface of 316L stainless steel (SS) by combining Ti magnetron sputtering and plasma electrolytic oxidation (PEO) with the aim to produce a polymer-free drug carrier for drug eluting stent (DES) applications. The oxidation was performed galvanostatically in Na3PO4 electrolyte. The surface porosity, average pore size and roughness varied with PEO treatment duration, and under optimum conditions, the surface showed a porosity of 7.43%, an average pore size of 0.44 µm and a roughness (Ra) of 0.34 µm. The EDS analyses revealed that the porous layer consisted of Ti, O and P. The cross-sectional morphology evidenced a double-layer structure, with a porous titania surface and an un-oxidized dense Ti film towards the interface with 316L SS. After the PEO treatment, wettability and surface free energy increased significantly. The results of the present study confirm the feasibility of forming a porous TiO2 layer on stainless steel by combining sputtering technology and PEO. Further, the resultant porous oxide layer has the potential to be used as a drug carrier for DES, thus avoiding the complications associated with the polymer based carriers.

In vitro degradation behavior and bioactivity of magnesium-Bioglass(®) composites for orthopedic applications.

To improve the bioactivity and degradation behavior of biodegradable magnesium, biodegradable metal matrix composites with the ZK30 magnesium alloy as the matrix and bioactive glass (BG, 45S5) as the reinforcement were prepared. The microstructures of the ZK30-BG composites showed homogeneous dispersion of BG particles throughout the matrix. XRD and EDX analyses confirmed the retention of the morphological characteristics and composition of BG particles in the composites. Immersion tests in the minimum essential medium with Earle's balanced salts at 37°C showed that the composites with 5 and 10% BG had lower rates of degradation and hydrogen evolution than the matrix alloy. In addition, the tests confirmed that the composites possessed an enhanced ability to induce calcium and phosphate ion deposition on sample surfaces during degradation, suggesting accelerated surface mineralization that would lead to improved bioactivity when compared with the matrix alloy. In vitro cytotoxicity tests showed that the ionic products of the composites formed during degradation possessed a superior ability to support the survival, proliferation, and osteoblastic differentiation of bone marrow stromal cells to those of the ZK30 alloy. The ZK30-BG composites with enhanced bioactivity and reduced degradation rate could be promising biodegradable materials for orthopedic implants.

Drug release from PLGA microspheres attached to solids using supercritical CO2.

Functionalization of a porous orthopedic implant with dexamethasone, a widely used anti-inflammatory drug, encapsulated within a biodegradable polymer for controlled release could help reduce or eliminate the inflammation response by the local tissue. In this research, we investigated the possibility of using supercritical carbon dioxide (CO2) for attaching dexamethasone-loaded PLGA (polylactic-co-glycolic acid) microspheres to porous CoCrMo alloy for continuous delivery of dexamethasone. Supercritical CO2 has been shown to be effective for attachment of PLGA microspheres to glass plates and porous CoCrMo alloy. Attached microspheres showed similar dexamethasone release profiles but different magnitude of burst release. Microspheres attached to the porous alloy samples using supercritical CO2 at 10 bar and 40 °C for 30 min showed a release profile similar to that of the nonattached microspheres. The microsphere morphology and the release profiles of microspheres attached to the glass plates and to the porous alloy samples suggest that dexamethasone burst release is enhanced by PLGA swelling at higher CO2 pressures and better dispersion of microspheres. This study shows that microspheres can be incorporated into porous solids using supercritical CO2, allowing for a wide variety of drug-biodegradable polymer formulations prepared using the proven emulsion/solvent evaporation method to be tested.

Magnesium-based composites with improved in vitro surface biocompatibility.

In this study, bioactive glass (BG, 45S5) particles were added to a biodegradable magnesium alloy (ZK30) through a semi-solid high-pressure casting process in order to improve the surface biocompatibility of the biomaterial and potentially its bioactivity. The observation of the as-cast microstructures of ZK30-BG composites indicated homogeneous dispersion of BG particles in the matrix. SEM, EDX and EPMA showed the retention of the morphological characteristics and composition of BG particles in the as-cast composite materials. In vitro tests in a cell culture medium confirmed that the composites indeed possessed an enhanced ability to induce the deposition of a bone-like apatite layer on the surface, indicating an improved surface biocompatibility as compared with the matrix alloy.

In vitro antibacterial activity of porous TiO2-Ag composite layers against methicillin-resistant Staphylococcus aureus.

The aim of this study was the synthesis of a porous TiO(2)-Ag composite coating and assessment of its in vitro bactericidal activity against methicillin-resistant Staphylococcus aureus. The coating was produced by plasma electrolytic oxidation of Ti-6Al-7Nb medical alloy in a calcium acetate/calcium glycerophosphate electrolyte bearing Ag nanoparticles. Following oxidation, the surface of the titanium substrate was converted into the corresponding oxide (TiO(2)) bearing Ca and P species from the electrolyte. In addition, Ag was detected associated with particles present in the oxide layers. The coatings revealed a porous interconnected structure with pores up to 3 microm in size, a threefold increase in roughness and improved wettability relative to the non-oxidized specimens. The composite TiO(2)-Ag coating showed complete killing of methicillin-resistant S. aureus within 24h in all culture conditions, whereas a 1000-fold increase in bacterial numbers was recorded with the ground titanium specimens and the samples oxidized in the absence of Ag nanoparticles.