J.A. del Valle

Corrosion behaviour of AZ31 magnesium alloy with different grain sizes in simulated biological fluids

The corrosion behaviour of AZ31 magnesium alloy with different grain sizes immersed in simulated body fluids was compared in chloride solution (8 gl(-1)) and in phosphate-buffer solution (PBS). The influence of immersion time was also analyzed. Electrochemical techniques such as open circuit potential, polarization curves, transient currents and electrochemical impedance spectroscopy, complemented with scanning electron microscopy and energy dispersive spectroscopy, were used. Immediately after the immersion in the corrosive media the corrosion resistance was similar for both grain sizes of the AZ31 alloy and higher in NaCl solutions than in PBS. However, this corrosion behaviour was reversed after longer periods of immersion due to the stabilizing of the corrosion products of MgO by P-containing compounds. These P-compounds contribute to a higher level of protection by hindering the aggressive action of chloride ions. The best corrosion behaviour of the AZ31 alloy was obtained for the finest grain alloy associated with the highest transfer resistance value, after long periods of immersion in PBS.

Texture evolution during large-strain hot rolling of the Mg AZ61 alloy

Abstract Grain refinement in a Mg-based AZ61 alloy of initially coarse, recrystallized microstructure was successfully achieved by thermomechanical processing (TMP) consisting of two to three hot-rolling steps with large reductions per pass. Reductions as large as 85% (equivalent to a true strain of ≈1) were achieved without surface cracking. The underlying microscopic mechanisms operative during the TMP that allowed this hcp material to accommodate such large strains per pass were investigated by macro- and microtexture analysis. A significant decrease in the intensity of the initial basal texture was observed after the first pass. This was attributed to rotational dynamic recrystallization, a mechanism by which new recrystallized grains develop, with orientations favourable for basal slip. Upon subsequent passes, basal slip becomes the main deformation mechanism. Simultaneously, grain refinement takes place by continuous dynamic recrystallization. The fine-grained microstructure thus developed showed improved superplastic behaviour in comparison with that of similar alloys processed by more elaborate methods.

Corrosion inhibition of powder metallurgy Mg by fluoride treatments

Pure Mg has been proposed as a potential degradable biomaterial to avoid both the disadvantages of non-degradable internal fixation implants and the use of alloying elements that may be toxic. However, it shows excessively high corrosion rate and insufficient yield strength. The effects of reinforcing Mg by a powder metallurgy (PM) route and the application of biocompatible corrosion inhibitors (immersion in 0.1 and 1M KF solution treatments, 0.1M FST and 1M FST, respectively) were analyzed in order to improve Mg mechanical and corrosion resistance, respectively. Open circuit potential measurements, polarization techniques (PT), scanning electrochemical microscopy (SECM) and electrochemical impedance spectroscopy (EIS) were performed to evaluate its corrosion behavior. SECM showed that the local current of attacked areas decreased during the F(-) treatments. The corrosion inhibitory action of 0.1M FST and 1M FST in phosphate buffered solution was assessed by PT and EIS. Under the experimental conditions assayed, 0.1M FST revealed better performance. X-ray photoelectron spectroscopy, energy dispersive X-ray and X-ray diffraction analyses of Mg(PM) with 0.1M FST showed the presence of KMgF(3) crystals on the surface while a MgF(2) film was detected for 1M FST. After fluoride inhibition treatments, promising results were observed for Mg(PM) as degradable metallic biomaterial due to its higher yield strength and lower initial corrosion rate than untreated Mg, as well as a progressive loss of the protective characteristics of the F(-)-containing film which ensures the gradual degradation process.

Superplastic Behavior of a Fine Grained AZ61 Alloy Processed by Large Strain Hot Rolling

CICYT grant MAT2000-1313 is appreciated. MTP acknowledges a Ramon y Cajal 2001 contract, awarded by the Spanish Ministry of Science and Technology. JAV is thankful to CONICET

Influence of grain size fluctuations on ductility of superplastic magnesium alloys processed by severe plastic deformation

Abstract The influence of fluctuations in the grain size along the gauge length on ductility is analysed in the superplastic regime. It is demonstrated that these fluctuations produce a similar effect to that produced by variations in the initial uniformity of the sample, leading to premature necking. To reach superplastic elongations of 400%, fluctuations in grain size of <0·5% between two zones of the gauge length are required. As an example, the superplastic behaviour of an AZ61 alloy, processed by severe plastic deformation (SPD), with a heterogeneous microstructure is analysed when the grain boundary sliding mechanism controls deformation. It is found that neck formation is related to bands of fine grains that are formed during SPD processing by the mechanism of recrystallisation by rotation. Under these circumstances, grain refinement is rendered unsuccessful. The present investigation emphasises the importance of the microstructure homogeneity in developing grain refinement processing routes.

Influence of thermomechanical processing on superplastic forming of Mg-Al alloys

Abstract The aim of this paper is to study the influence of the initial microstructure of several Mg–Al alloys on their superplastic formability and on their post-forming microstructure and mechanical properties. Various thermomechanical processing routes, such as annealing, conventional rolling, severe rolling and cross rolling, were used in order to fabricate AZ31 and AZ61 alloys with different grain sizes. These materials were then blow formed into a hat shaped die. It was found that the processing route has only a small effect in the formability of Mg–Al alloys or on the post-forming microstructures and properties due to rapid dynamic grain growth taking place at the forming temperatures. Nevertheless, good formability is achieved as a result of the simultaneous operation of grain boundary sliding and crystallographic slip during forming.

Friction Stir Processing of the Magnesium Alloy AZ61: Grain Size Refinement and Mechanical Properties

The effect of friction stir processing (FSP), on the microstructure and mechanical properties of a magnesium alloy AZ61 has been analyzed. This is a widely used wrought magnesium alloy provided in the form of rolled and annealed sheets with a grain size of 45 μm. The FSP was performed with an adequate cooling device in order to increase the heat extraction and reduce the processing temperature. The final microstructure showed a noticeable grain size refinement down to values close to 1.8 μm and an important change in texture. The change in texture favors basal slip during tensile testing leading to an increase of ductility and a decrease in yield stress. The stability of the grain size and the creep behavior at high temperatures were investigated. The optimum conditions for superplastic forming were determined; however, the presence of a large amount of cavities precludes the achievement of high superplastic elongations. Additionally, these results are compared with those obtained by severe hot rolling.

Fine and Ultra-Fine Grained AZ61 and AZ91 Magnesium Alloys Obtained by Friction Stir Processing

Friction Stir Processing (FSP) has attracted much interest as a tool for refining grain size and achieving high angle boundary misorientation in magnesium alloys. These characteristics have a great influence in key engineered properties such as strength and ductility, which could be markedly improved by means of this technique. The main objective of this work is to study the microstructural modifications produced when FSP is applied to homogenized cast AZ91 and wrought AZ61 magnesium alloys. Several attempts were made for achieving a homogenous microstructure without defects and enhancing the refinement of the grain size in the stir zone. It was revealed that is of great importance to break the initial microstructure, of coarse grains unfavourably oriented for deformation, in order to facilitate the process, particularly in the case of cast AZ91 alloy. It is highlighted that, after breaking up the initial microstructure, is possible to process the material, in subsequent passes, Furthermore, the use of different backing materials as heat sink and a previous heating treatment of the sample were evaluated. Changing the backing plate can improve more the reduction of the grain size during a second pass. Using a copper plate instead of a steel one can promote a refinement up to 700 nm in AZ91 and 1 μm in AZ61. A coolant agent can be used for inhibiting the grain growth causing a little more reduction of the grain size.

Microstructural Evolution During Hot Rolling of an AZ31 Mg Alloy

The microstructural evolution of a AZ31 Mg alloy during hot rolling has been investigated using optical microscopy and texture (macro and micro) analysis as the main characterization tools. In particular, the differences between the microstructure obtained by unidirectional rolling (UR) and cross rolling (CR) are studied. Significant twinning activity is observed in both cases. Additionally, after cross rolling, a rather heterogeneous microstructure develops, with scattered regions populated by very fine grains. The strong basal fiber texture of the as-received material remains present after both hot rolling schemes. The imposibility to obtain accurate EBSD measurements within the twinned regions suggests that significant localized deformation takes place in those areas. Thus, due to the increase in the local strain energy, these regions become preferential sites for nucleation of recrystallization.

Effect of Annealing Treatments on Strain Rate Sensitivity and Anisotropy in a Magnesium Alloy Processed by Severe Rolling

The effect of annealing treatments on the evolution of the strain rate sensitivity with strain of AZ61 magnesium alloy processed by severe rolling was investigated and related to previous results on normal plastic anisotropy (r-value). The various annealing treatments produce two effects on the microstructure: grain coarsening and slight weakening of the texture. In addition, these treatments produce a noticeable decrease in strain rate sensitivity and an increase of work hardening rate that is related to the decrease of the anisotropy. It is concluded that these effects are related to an enhanced contribution of basal slip as a consequence of the microstructural changes induced by the annealing treatments.