Effect of sterilization process on surface characteristics and biocompatibility of pure Mg and MgCa alloys.

The aim of this work was to investigate the effect of various sterilization methods on surface characteristics and biocompatibility of MgCa alloy, with pure Mg as a comparison, including steam autoclave sterilization (SA), ethylene oxide steam sterilization (EO), glutaraldehyde sterilization (GD), dry heat sterilization (DH) and Co60 γ ray radiation sterilization (R) technologies. The surface characterizations were performed by environmental scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, grazing incidence X-ray diffraction, water contact angle and surface free energy measurement, whereas the cytotoxicity and hemocompatibility were evaluated by cellular adhesive experiment, platelet adhesion and hemolysis test. The results showed that the five sterilization processes caused more changes on the surface of MgCa alloy than that on the surface of pure Mg. The GD sterilization caused the most obvious changes on the surface of the pure Mg, and the SA sterilization made the largest alteration on the MgCa alloy surface. The GD and DH sterilization processes could cause increases on surface free energy for both pure Mg and MgCa alloys, while the other three sterilization processes reduced the surface free energy. The DH and GD sterilization processes caused the least alteration on the cell adhesion on pure Mg surface, whereas the EO sterilization performed the greatest impact on the cell adhesion on the Mg-Ca alloy surface. The hemolysis percentage of pure Mg and MgCa alloys were reduced by SA sterilization, meanwhile the other four sterilization processes increased their hemolysis percentages significantly, especially for the EO sterilization.

Mechanical property, biocorrosion and in vitro biocompatibility evaluations of Mg-Li-(Al)-(RE) alloys for future cardiovascular stent application.

Mg-Li-based alloys were investigated for future cardiovascular stent application as they possess excellent ductility. However, Mg-Li binary alloys exhibited reduced mechanical strengths due to the presence of lithium. To improve the mechanical strengths of Mg-Li binary alloys, aluminum and rare earth (RE) elements were added to form Mg-Li-Al ternary and Mg-Li-Al-RE quarternary alloys. In the present study, six Mg-Li-(Al)-(RE) alloys were fabricated. Their microstructures, mechanical properties and biocorrosion behavior were evaluated by using optical microscopy, X-ray diffraction, scanning electronic microscopy, tensile tests, immersion tests and electrochemical measurements. Microstructure characterization indicated that grain sizes were moderately refined by the addition of rare earth elements. Tensile testing showed that enhanced mechanical strengths were obtained, while electrochemical and immersion tests showed reduced corrosion resistance caused by intermetallic compounds distributed throughout the magnesium matrix in the rare-earth-containing Mg-Li alloys. Cytotoxicity assays, hemolysis tests as well as platelet adhesion tests were performed to evaluate in vitro biocompatibilities of the Mg-Li-based alloys. The results of cytotoxicity assays clearly showed that the Mg-3.5Li-2Al-2RE, Mg-3.5Li-4Al-2RE and Mg-8.5Li-2Al-2RE alloys suppressed vascular smooth muscle cell proliferation after 5day incubation, while the Mg-3.5Li, Mg-8.5Li and Mg-8.5Li-1Al alloys were proven to be tolerated. In the case of human umbilical vein endothelial cells, the Mg-Li-based alloys showed no significantly reduced cell viabilities except for the Mg-8.5Li-2Al-2RE alloy, with no obvious differences in cell viability between different culture periods. With the exception of Mg-8.5Li-2Al-2RE, all of the other Mg-Li-(Al)-(RE) alloys exhibited acceptable hemolysis ratios, and no sign of thrombogenicity was found. These in vitro experimental results indicate the potential of Mg-Li-(Al)-(RE) alloys as biomaterials for future cardiovascular stent application and the worthiness of investigating their biodegradation behaviors in vivo.

Corrosion resistance and surface biocompatibility of a microarc oxidation coating on a Mg-Ca alloy.

The Mg-Ca alloy system has been proposed as a potential new kind of degradable biomaterial with possible application within bone. Here microarc oxidation (MAO) coatings were fabricated on top of a Mg-Ca alloy using different applied voltages and the effect of applied voltage on the surface morphology and phase constitution, hydrogen evolution, pH variation in the immersion solution and in vitro biocompatibility of the MAO coating on the Mg-Ca alloy were extensively studied. It was found that the thickness and pore size of the MAO coating increased with the increasing applied voltage, whereas some micro-pores could be seen inside the 400 V treated MAO coating. The 360 V treated MAO coating gave the best long-term corrosion resistance during a 50 days immersion test. All the MAO coatings could promote MG63 cell adhesion, proliferation and differentiation in comparison with the uncoated Mg-Ca alloy sample, due to significantly reduced Mg ion release and pH value variations in the culture medium. After 5 days culture well-spread and elongated MG63 cells could be seen on the surface of the 360 V and 400 V MAO coatings, in contrast to no cells on the uncoated Mg-Ca alloy sample. In summary, MAO showed beneficial effects on the corrosion resistance of, and thus improved cell adhesion to, the Mg-Ca alloy, and should be a good surface modification method for other biomedical magnesium alloys.

Corrosion fatigue behaviors of two biomedical Mg alloys - AZ91D and WE43 - In simulated body fluid.

Magnesium alloys have been recently developed as biodegradable implant materials, yet there has been no study concerning their corrosion fatigue properties under cyclic loading. In this study the die-cast AZ91D (A for aluminum 9%, Z for zinc 1% and D for a fourth phase) and extruded WE43 (W for yttrium 4%, E for rare earth mischmetal 3%) alloys were chosen to evaluate their fatigue and corrosion fatigue behaviors in simulated body fluid (SBF). The die-cast AZ91D alloy indicated a fatigue limit of 50MPa at 107 cycles in air compared to 20MPa at 106 cycles tested in SBF at 37°C. A fatigue limit of 110MPa at 107 cycles in air was observed for extruded WE43 alloy compared to 40MPa at 107 cycles tested in SBF at 37°C. The fatigue cracks initiated from the micropores when tested in air and from corrosion pits when tested in SBF, respectively. The overload zone of the extruded WE43 alloy exhibited a ductile fracture mode with deep dimples, in comparison to a brittle fracture mode for the die-cast AZ91D. The corrosion rate of the two experimental alloys increased under cyclic loading compared to that in the static immersion test.

Microstructure, biocorrosion and cytotoxicity evaluations of rapid solidified Mg-3Ca alloy ribbons as a biodegradable material.

Rapidly solidified (RS) Mg­3Ca alloy ribbons were prepared by the melt-spinning technique at different wheel rotating speeds (15 m s(-1), 30 m s(-1) and 45 m s(-1) with the as-cast Mg­3Ca alloy ingot as a raw material. The RS45 Mg­3Ca alloy ribbon showed a much more fine grain size feature (approximately 200­500 nm) in comparison to the coarse grain size (50­100 µm)of the original as-cast Mg­3Ca alloy ingot. The corrosion electrochemical tests in simulated body fluid indicated that the corrosion rate of the as-cast Mg­3Ca alloy was strongly reduced by the RS procedure and tended to be further decreased with increasing wheel rotating speeds(1.43 mm yr(-1) for RS15, 0.94 mm yr(-1) for RS30 and 0.36 mm yr(-1) for RS45). The RS Mg­3Ca alloy ribbons showed more uniform corrosion morphology compared with the as-cast Mg­3Ca alloy after polarization. The cytotoxicity evaluation revealed that the three experimental as-spun Mg­3Ca alloy ribbon extracts did not induce toxicity to the L-929 cells,whereas the as-cast Mg­3Ca alloy ingot extract did. The L-929 cells showed more improved adhesion on the surfaces of the three as-spun Mg­3Ca alloy ribbons than that of the as-cast Mg­3Ca alloy ingot.

[Osteoclastic resorption of trabeculae in osteoporotic femoral head: a scanning electron microscopic study].

Osteoclastic resorption was studied by scanning electron microscopy on the trabeculae of femoral heads collected from 7 cases of aged women at an average age of 72.4 years, who underwent endoprosthetic replacement for intracapsular fracture of femoral neck. Femoral head trabeculae from 3 young adults killed in traffic accident served as control. The trabeculae of the femoral head formed round or roundish arch structure. The columnar trabeculae of the femoral head in the aged women showed overt osteoclastic resorption, manifesting thinning, tapering and perforation. The icicle-like trabeculae then became rounded, lost height and eventually turned into a small tubercle. As a result, the inter-trabecular space enlarged markedly. Under high magnification, on the trabeculae could be discerned oval, narrow oval or spindle-shaped Howship lacunae, which were various in size, depth and content, but all revealed punch-out edge. Around the lacunae the collagen fibril lamella normally covering the quiscient bone surface became resorbed sooner or later. During bone resorption, the inorganic component of the bone matrix were first dissolved and resorbed leaving behind rough and irregular collagen fibrils; nevertheless, the collagen might be degraded and resorbed first with residual inorganic crystals and irregular bone nodules. Then emerged in the Howship lacunae and surrounding area newly formed collagen fibrils and bone tissue, signifying reversal and new bone formation phases following the the bone resorption phase. In the aged women, however, this phenomenon was rather infrequently encountered, thereby leaving the bone turnover always in a negative balance state.

Arch structure of trabeculae of the upper femoral end and its biomechanical significance in hip fractures.

We studied ultrastructurally the cancellous bone tissues of the upper femoral ends, collected from 12 patients undergoing endoprosthesis replacement for fractures of the femoral neck and from 7 fresh cadavers. The bone tissues were composed of meshwork of trabeculae, that constituted tier upon tier of anisotropic arch structures of different diameters and sizes. The arch structures of the cancellous bone tissues in the femoral heads assumed round or roundish configurations, whereas those of the femoral head-neck junctions revealed oval outlines and those of the femoral necks showed narrow oval profiles. The fine structures of the trabeculae in the femoral head could be divided into superficial zone, central zone, and transitional zone. Under weight-bearing, the central zone suited to sustain the load, while the superficial zone could produce elastic deformation lest fracture of the trabecaulae should ensue. The long axes of the oval arch structures of the femoral head-neck junction and the narrow oval arch structures of the femoral neck coincided with those of the femoral neck, thereby facilitating weight-bearing under physiological conditions. However, external violence in the form of either adduction or abduction force would act in a horizontal direction on the long axes of the oval and narrow oval arches so as to produce subcapital or transverse fracture of the femur in the aged.