In vitro studying corrosion behaviour of biocorrodible Mg alloys

The idea of bioabsorbable/biocorrodible stents has gained increasing attention in the last decade. Permanent coronary stents, traditionally made from 316L grade stainless steel, are routinely used for the treatment of blocked arteries. However, these stents can cause complications such as restenosis, thrombosis and the need for the patient to undergo prolonged antiplatelet therapy. Biodegradable metal stents provide an opportunity for the stent to remain in place for a period to ensure restoration of function and then degrade through a carefully controlled bio-corrosion process. Among the number of potentially suitable materials, Magnesium alloys have shown great promise as a stent material due to their non-toxicity [1] and the corrosion rates attainable in biological environments. However, a carefully controlled corrosion process is essential in order to avoid hyper hydrogen generation and the fatal consequences that follow. In addition uniform corrosion is a basic requirement to maintain the mechanical integrity and load bearing characteristics. Work being undertaken in our laboratories focuses on controlling the corrosion behaviour of magnesium in a simulated biological environment in the presence of protein. In the investigation reported here the Mg alloy has been examined using Scanning Electrochemical Microscope (SECM) to visualize the corrosion process and identify the corrosion pattern. Complementary bulk electrochemical techniques (EIS and potentiodynamic polarization) have been used to acquire kinetic and mechanistic information. Early results obtained by SECM have revealed the tendency towards pitting corrosion in the early stages which subsequently develops in to filiform corrosion.

Compositional effects on the restoration behaviour in Mg-Zn-Re alloys

Additions of rare earth elements to magnesium alloys are qualitatively reported in the literature to retard recrystallisation. However, their effect in the presence of other (non-rare earth) alloy additions has not been systematically shown nor has the effect been quantified. The microstructural restoration following the hot deformation of Mg-xZn-yRE (x = 2.5 and 5 wt.%, y = 0 and 1 wt.%, and RE = Gd and Y) alloys has been studied using double hit compression testing and microscopy. It was found that, in the absence of rare earth additions, increases in zinc level had a negligible influence on the kinetics of restoration and the microstructure developed both during extrusion and throughout double hit testing. Adding rare earth elements to Mg-Zn alloys was found to retard restoration of the microstructure and maintain finer recrystallised grains. However, in the Mg-Zn-RE alloys, increasing the zinc concentration from 2.5 wt.% to 5 wt.% accelerated the restoration process, most likely due to a depletion of rare earth elements from solid solution and modification of the particles present in the matrix.

Effect of alloying and extrusion temperature on the microstructure and mechanical properties of Mg-Zn and Mg-Zn-RE alloys

Extruded Mg-Zn-RE alloys have been shown to exhibit excellent combinations of yield strength and ductility, but it is not completely clear how adding rare earth metals to Mg-Zn alters the microstructure and affects the mechanical properties. Microstructural changes and the resulting mechanical properties from changes in composition and extrusion temperature have been investigated for Mg-. x Zn-. y RE (. x=2.5 and 5. wt.%, y=0 and 1. wt. %, and RE=Gd and Y) alloys. Adding RE to Mg-Zn increased the strength and reduced the ductility, while increasing the zinc concentration in the Mg-Zn-RE alloys had the reverse effect.

Time and spatial resolution of slip and twinning in a grain embedded within a magnesium polycrystal

Plastic yielding in magnesium alloys frequently involves the initiation of both slip and twinning events. A proper understanding of the phenomenon at the grain level requires knowledge of how these two mechanisms progress and interact over both time and space and what the local resolved stresses are. To date, simultaneous collection of such information has not been achievable. To address this shortfall, we have developed a modified Laue based in situ micro X-ray diffraction technique with an unprecedented combination of time and spatial resolution. A ten-fold reduction in data collection times is realized by the refinement of rapid polychromatic Laue "single-shot" mapping. From single Laue patterns, we extract grain depth information, detect onset of yielding and achieve 2 × 10-4 lattice strain resolution. The technique is employed to examine yielding and twinning in a magnesium grain embedded ∼200 μm below the sample surface. We examine 13 time steps and reveal the following behaviour: initial onset of basal slip, subsequent onset of twinning, development of further accommodation slip and evolution of twin shape and size; along with the corresponding values of local resolved shear stresses. © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Development of a laboratory-based transmission diffraction technique for in situ deformation studies of Mg alloys

A laboratory-based transmission X-ray diffraction technique was developed to measure elastic lattice strains parallel to the loading direction during in situ tensile deformation. High-quality transmission X-ray diffraction data were acquired in a time frame suitable for in situ loading experiments by application of a polycapillary X-ray optic with a conventional laboratory Cu X-ray source. Based on the measurement of two standard reference materials [lanthanum hexaboride (NIST SRM 660b) and silicon (NIST SRM 640c)], precise instrumental alignment and calibration of the transmission diffraction geometry were realized. These results were also confirmed by the equivalent data acquired using the standard Bragg-Brentano measurement geometry. An empirical Caglioti function was employed to describe the instrumental broadening, while an axis of rotation correction was used to measure and correct the specimen displacement from the centre of the goniometer axis. For precise Bragg peak position and hkil intensity information, a line profile fitting methodology was implemented, with Pawley refinement used to measure the sample reference lattice spacings (d o (hkil)). It is shown that the relatively large X-ray probe size available (7 × 714mm) provides a relatively straightforward approach for improving the grain statistics for the study of metal alloys, where grain sizes in excess of 114μm can become problematic for synchrotron-based measurements. This new laboratory-based capability was applied to study the lattice strain evolution during the elastic-plastic transition in extruded and rolled magnesium alloys. A strain resolution of 2 × 10-4 at relatively low 2θ angles (20-65° 2θ) was achieved for the in situ tensile deformation studies. In situ measurement of the elastic lattice strain accommodation with applied stress in the magnesium alloys indicated the activation of dislocation slip and twin deformation mechanisms. Furthermore, measurement of the relative change in the intensity of 0002 and 10 3 was used to quantify {10 2} 011 tensile twin onset and growth with applied load.

Microstructures, mechanical and corrosion properties and biocompatibility of as extruded Mg-Mn-Zn-Nd alloys for biomedical applications

Extruded Mg-1Mn-2Zn-xNd alloys (x=0.5, 1.0, 1.5 mass %) have been developed for their potential use as biomaterials. The extrusion on the alloys was performed at temperature of 623K with an extrusion ratio of 14.7 under an average extrusion speed of 4mm/s. The microstructure, mechanical property, corrosion behavior and biocompatibility of the extruded Mg-Mn-Zn-Nd alloys have been investigated in this study. The microstructure was examined using X-ray diffraction analysis and optical microscopy. The mechanical properties were determined from uniaxial tensile and compressive tests. The corrosion behavior was investigated using electrochemical measurement. The biocompatibility was evaluated using osteoblast-like SaOS2 cells. The experimental results indicate that all extruded Mg-1Mn-2Zn-xNd alloys are composed of both α phase of Mg and a compound of Mg7Zn3 with very fine microstructures, and show good ductility and much higher mechanical strength than that of cast pure Mg and natural bone. The tensile strength and elongation of the extruded alloys increase with an increase in neodymium content. Their compressive strength does not change significantly with an increase in neodymium content. The extruded alloys show good biocompatibility and much higher corrosion resistance than that of cast pure Mg. The extruded Mg-1Mn-2Zn-1.0Nd alloy shows a great potential for biomedical applications due to the combination of enhanced mechanical properties, high corrosion resistance and good biocompatibility.

Influence of grain size on hot working stresses and microstructures in Mg-3A1-1Zn

The influence of the grain size on the deformation of Mg–3Al–1Zn was examined in compression at 300 °C. At low strains the flow stress increases with increasing grain size. This is interpreted in terms of dynamic recrystallization. Empirical models of dynamic recrystallization are developed and employed to generate a microstructure map.

Observation of deformation modes in Mg-3Al-1Zn

Since magnesium alloys are the lightest metallic materials, they are very attractive for automotive and aerospace industries. The main problem of these alloys is limited ductility due to a shortage of independent slip systems. In order to improve the formability in these alloys, an understanding of the deformation modes is required. In the present work, different slip systems were investigated in rolled Mg-3Al-IZn by means of in situ tensile tests in the SEM. These permitted electron backscatter diffraction (EBSD) and electron backscatter diffraction imaging (QBSD) to be carried out during the test. The results show that non-basal slip systems are active at room temperature.

Microstructural features of rolled mg-3Al-1Zn

The microstructures of hot- and cold-rolled Mg-3Al-1Zn (AZ31) are examined using scanning electron and optical microscopy. It is shown that the microstructures following multipass hot rolling and annealing are more uniform than those formed by heavy single pass rolling and annealing. The importance of twins in producing intragranular recrystallization is evident, although the most dominant nucleation site is grain boundaries. The cold-rolled structure after a rolling reduction of 15 pct is dominated by the presence of deformation twins. Twin trace analysis suggests that approximately two thirds of the twins are a form of “c-axis compression” twin. A number of “c-axis tension” twins were also observed and additional in-situ scanning electron microscopy experiments were performed to confirm earlier observations that suggest these twins can form after deformation, during unloading.

EBSD analysis of deformation modes in Mg-3A1-1Zn

Wrought magnesium alloys exhibit poor cold formability and the accepted explanation is the shortage of independent slip systems. In order to improve the formability in these alloys, an understanding of the deformation modes is required. In the present work, activation of different slip and twinning systems are investigated in rolled Mg–3Al–1Zn using electron back scattering diffraction. Analysis was performed on deformed surfaces and on metallographically prepared cross-sections following deformation at room temperature. The results reinforce the importance of prismatic slip and c-axis compression double twinning.

In-situ investigation of twinning behaviour in Mg-3Al-1Zn

Magnesium alloys are attractive for automotive and aerospace industries, due to their low density. One problem with these alloys is their limited formability at room temperature. Twinning plays a dominant role in deformation behaviour and it can be expected that an increased understanding of twinning will help improve formability. In the present work, the behaviour of different twinning systems in as-cast Mg-3AI-IZn is investigated using in-situ tensile tests in a scanning electron microscope. Electron backscatter diffraction and back scatter electron imaging were carried out during the tests. The results show both "tension" and "compression" twinning are active at room temperature and that twinning and untwinning occur both during loading and unloading.

Influence of microstructure on strain distribution in Mg–3Al–1Zn

Inspection of pre-polished surfaces of Mg–3Al–1Zn hot-rolled plate following 5% uniaxial compression revealed a distinctive heterogeneous deformation pattern. The pattern differed depending on the face examined. The greater share of the strain was born by regions characterized by grains considerably finer than the average. These regions displayed a favourable alignment for basal slip and were probably formed by shear banding during previous rolling. It is clear that local orientation softening leads to inhomogeneous deformation despite local grain size-hardening and twin activation.

Microstructural development during hot working of Mg-3AI-1Zn

he microstructural evolution is examined during the hot compression of magnesium alloy AZ31 for both wrought and as-cast initial microstructures. The influences of strain, temperature, and strain rate on the dynamically recrystallized microstructures are assessed. Both the percentage dynamic recrysallization (DRX) and the dynamically recrystallized grain size were found to be sensitive to the initial microstructure and the applied deformation conditions. Lower Z conditions (lower strain rates and higher temperatures) yield larger dynamically recrystallized grain sizes and increased percentages of DRX, as expected. The rate with which the percentage DRX increases for the as-cast material is considerably lower than for the wrought material. Also, in the as-cast samples, the percentage DRX does not continue to increase toward complete DRX with decreasing Z. These observations may be attributed to the deformation becoming localized in the DRX fraction of the material. Also, the dynamically recrystallized grain size is generally larger in as-cast material than in wrought material, which may be attributed to DRX related to twins and the inhomogeneity of deformation. Orientation maps of the as-cast material (from electron backscattering diffraction (EBSD) data) reveal evidence of discontinuous DRX (DDRX) and DRX related to twins as predominant mechanisms, with some manifestation of continuous DRX (CDRX) and particle-stimulated nucleation (PSN).