Compressive behaviour of nanocrystallilne Mg-5%Al alloys

Magnesium alloys are attracting increasing research interests due to their low density, high specific strength and good mechineability and availability as compared to other structural materials. However, the deformation and failure mechanisms of nanocrystalline Mg alloys have not been well understood. In this work, the deformation behavior of nanocrystalline Mg-5% Al alloys was investigated using compression test, with a focus on the effects of grain size. The average grain size of the Mg-Al alloy was changed from 13 µm to 50 nm via mechanical milling. The results showed that grain size had a significant influence on the yield stress and ductility of the Mg alloys, and the materials exhibited increased strain rate sensitivity with decrease of grain size. The deformation mechanisms were also strongly dependent with the grain sizes.

Deformation behaviours of coarse-grained and nanocrystalline Mg-5wt% Al alloys

Magnesium alloys have been of growing interest to various engineering applications, such as the automobile, aerospace, communication and computer industries due to their low density, high specific strength, good machineability and availability as compared with other structural materials. However, most Mg alloys suffer from poor plasticity due to their Hexagonal Close Packed structure. Grain refinement has been proved to be an effective method to enhance the strength and alter the ductility of the materials. Several methods have been proposed to produce materials with nanocrystalline grain structures. So far, most of the research work on nanocrystalline materials has been carried out on Face-Centered Cubic and Body-Centered Cubic metals. However, there has been little investigation of nanocrystalline Mg alloys. In this study, bulk coarse-grained and nanocrystalline Mg alloys were fabricated by a mechanical alloying method. The mixed powder of Mg chips and Al powder was mechanically milled under argon atmosphere for different durations of 0 hours (MA0), 10 hours (MA10), 20 hours (MA20), 30 hours (MA30) and 40 hours (MA40), followed by compaction and sintering. Then the sintered billets were hot-extruded into metallic rods with a 7 mm diameter. The obtained Mg alloys have a nominal composition of Mg–5wt% Al, with grain sizes ranging from 13 μm down to 50 nm, depending on the milling durations. The microstructure characterization and evolution after deformation were carried out by means of Optical microscopy, X-Ray Diffraction, Scanning Electron Microscopy, Transmission Electron Microscopy, Scanning Probe Microscopy and Neutron Diffraction techniques. Nanoindentaion, compression and micro-compression tests on micro-pillars were used to study the size effects on the mechanical behaviour of the Mg alloys. Two kinds of size effects on the mechanical behaviours and deformation mechanisms were investigated: grain size effect and sample size effect. The nanoindentation tests were composed of constant strain rate, constant loading rate and indentation creep tests. The normally reported indentation size effect in single crystal and coarse-grained crystals was observed in both the coarse-grained and nanocrystalline Mg alloys. Since the indentation size effect is correlated to the Geometrically Necessary Dislocations under the indenter to accommodate the plastic deformation, the good agreement between the experimental results and the Indentation Size Effect model indicated that, in the current nanocrystalline MA20 and MA30, the dislocation plasticity was still the dominant deformation mechanism. Significant hardness enhancement with decreasing grain size, down to 58 nm, was found in the nanocrystalline Mg alloys. Further reduction of grain size would lead to a drop in the hardness values. The failure of grain refinement strengthening with the relatively high strain rate sensitivity of nanocrystalline Mg alloys suggested a change in the deformation mechanism. Indentation creep tests showed that the stress exponent was dependent on the loading rate during the loading section of the indentation, which was related to the dislocation structures before the creep starts. The influence of grain size on the mechanical behaviour and strength of extruded coarse-grained and nanocrystalline Mg alloys were investigated using uniaxial compression tests. The macroscopic response of the Mg alloys transited from strain hardening to strain softening behaviour, with grain size reduced from 13 ìm to 50 nm. The strain hardening was related to the twinning induced hardening and dislocation hardening effect, while the strain softening was attributed to the localized deformation in the nanocrystalline grains. The tension–compression yield asymmetry was noticed in the nanocrystalline region, demonstrating the twinning effect in the ultra-fine-grained and nanocrystalline region. The relationship k tensions < k compression failed in the nanocrystalline Mg alloys; this was attributed to the twofold effect of grain size on twinning. The nanocrystalline Mg alloys were found to exhibit increased strain rate sensitivity with decreasing grain size, with strain rate ranging from 0.0001/s to 0.01/s. Strain rate sensitivity of coarse-grained MA0 was increased by more than 10 times in MA40. The Hall-Petch relationship broke down at a critical grain size in the nanocrystalline region. The breakdown of the Hall-Petch relationship and the increased strain rate sensitivity were due to the localized dislocation activities (generalization and annihilation at grain boundaries) and the more significant contribution from grain boundary mediated mechanisms. In the micro-compression tests, the sample size effects on the mechanical behaviours were studied on MA0, MA20 and MA40 micro-pillars. In contrast to the bulk samples under compression, the stress-strain curves of MA0 and MA20 micro-pillars were characterized with a number of discrete strain burst events separated by nearly elastic strain segments. Unlike MA0 and MA20, the stress-strain curves of MA40 micro-pillars were smooth, without obvious strain bursts. The deformation mechanisms of the MA0 and MA20 micro-pillars under micro-compression tests were considered to be initially dominated by deformation twinning, followed by dislocation mechanisms. For MA40 pillars, the deformation mechanisms were believed to be localized dislocation activities and grain boundary related mechanisms. The strain hardening behaviours of the micro-pillars suggested that the grain boundaries in the nanocrystalline micro-pillars would reduce the source (nucleation sources for twins/dislocations) starvation hardening effect. The power law relationship of the yield strength on pillar dimensions in MA0, MA20 supported the fact that the twinning mechanism was correlated to the pre-existing defects, which can promote the nucleation of the twins. Then, we provided a latitudinal comparison of the results and conclusions derived from the different techniques used for testing the coarse-grained and nanocrystalline Mg alloy; this helps to better understand the deformation mechanisms of the Mg alloys as a whole. At the end, we summarized the thesis and highlighted the conclusions, contributions, innovations and outcomes of the research. Finally, it outlined recommendations for future work.

Compressive behaviour of nanocrystalline Mg-5Al alloys

Magnesium alloys are attracting increasing research interests due to their low density, high specific strength, good machinability and availability as compared to other structural materials. However, the deformation and failure mechanisms of nanocrystalline (nc) Mg alloys have not been well understood. In this work, the deformation behaviour of nc Mg-5Al alloys was investigated using compression test, with focus on the effects of grain size. The average grain size of the Mg- Al alloy was changed from 13 to 50 nm via mechanical milling. The results showed that grain size had a significant influence on the yield stress and ductility of the Mg alloys, and the materials exhibited increased strain rate sensitivity with a decrease in grain size. The deformation mechanisms were also strongly dependent on the grain sizes.

Biodegradable Mg and Mg based alloys for biomedical implants

Mg and its alloys become natural biomaterials as the elemental Mg is found in the human body in abundance and their mechanical properties being akin to the natural bone as well as due to their inherent bioabsorbable/bioresorbable property. This paper discusses the development of new Mg alloys and their corrosion characteristics in detail. The latest advancements in coating of Mg alloys to control their degradation rate are also reviewed along with the future challenges that need to be addressed.

Structure and mechanical properties of Mg-Zn-RE system alloys

The lightest density of Mg has stimulated renewed interest in Mg based alloys for applications in the automotive, aerospace and communications industries. However, Mg in the pure form has relatively low strength, limited ductility and is susceptible to corrosion. Great efforts have been made to improve the mechanical properties of Mg alloys. Alloying Mg with other elements is one of the most important methods. An important class of Mg alloys is the Mg-Zn-RE system (RE = rare earth elements). In recent few decades, a series of new Mg-Zn-RE system alloys have been obtained, and detailed the structure and mechanical properties of the alloys. In this paper, the structure and mechanical properties of the Mg-Zn-RE alloys have been summarized. It showed that these alloys have high strength and they are prospected to be widely used in the future.

Microstructures and tensile properties of Mg-8Gd-0.6Zr-xNd-yY (x+y=3, mass%) alloys

Mg-8Gd-0.6Zr-xNd-yY (mass%) alloys which containing different Nd:Y mass ratio of 3:0, 2:1, 1:2 and 0:3 with a constant x + y = 3 were prepared by metal mould casting method, and the microstructure, aging behaviour and tensile properties have been investigated. The fibrous eutectic areas along the boundaries enlarge clearly in the as-cast alloys containing Y element, and the fine grain boundaries and dispersed precipitation are observed in the aged alloys. The Mg-8Gd-0.6Zr-2Nd-Y alloy exhibits notably age-hardening behaviour and the highest mechanical property. The ultimate tensile strength and yield strength of Mg-8Gd-0.6Zr-2Nd-Y alloy in the peak aged hardness are 293 and 221 MPa at room temperature, 248 and 191 MPa at 230 degrees C. The improvement of age-hardening response and tensile properties is mainly attributed to the quadrate-like stable Mg5RE precipitate, which forms readily and orderly in aged Mg-8Gd-0.6Zr-2Nd-Y alloy.

Grain refinement studies on Mg and Mg-Al based alloys

Demand on magnesium and its alloys is increased significantly in the automotive industry because of their great potential in reducing the weight of components, thus resulting in improvement in fuel efficiency of the vehicle. To date, most of Mg products have been fabricated by casting, especially, by die-casting because of its high productivity, suitable strength, acceptable quality & dimensional accuracy and the components produced through sand, gravity and low pressure die casting are small extent. In fact, higher solidification rate is possible only in high pressure die casting, which results in finer grain size. However, achieving high cooling rate in gravity casting using sand and permanent moulds is a difficult task, which ends with a coarser grain nature and exhibit poor mechanical properties, which is an important aspect of the performance in industrial applications. Grain refinement is technologically attractive because it generally does not adversely affect ductility and toughness, contrary to most other strengthening methods. Therefore formation of fine grain structure in these castings is crucial, in order to improve the mechanical properties of these cast components. Therefore, the present investigation is “GRAIN REFINEMENT STUDIES ON Mg AND Mg-Al BASED ALLOYS”. The primary objective of this present investigation is to study the effect of various grain refining inoculants (Al-4B, Al- 5TiB2 master alloys, Al4C3, Charcoal particles) on Pure Mg and Mg-Al alloys such as AZ31, AZ91 and study their grain refining mechanisms. The second objective of this work is to study the effect of superheating process on the grain size of AZ31, AZ91 Mg alloys with and without inoculants addition. In addition, to study the effect of grain refinement on the mechanical properties of Mg and Mg-Al alloys. The thesis is well organized with seven chapters and the details of the studies are given below in detail.

Effect of magnesium addition on the vacancy-Mg binding free enthalpy in Al-Cr alloys

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Investigation on mechanical behaviour of AM60 magnesium alloys

Purpose: In this work, tension, impact, bend and fatigue tests were conducted in an AM60 magnesium alloy. The effects of environmental temperature and loading rates on impact and tension behavior of the alloy were also investigated. Design/methodology/approach: The tests were conducted using an Instron universal testing machine. The loading speed was changed from 1 mm/min to 300 mm/min to gain a better understanding of the effect of strain rate. To understand the failure behavior of this alloy at different environmental temperatures, Charpy impact test was conducted in a range of temperatures (-40~35°C). Plane strain fracture toughness (KIC) was evaluated using compact tension (CT) specimen. To gain a better understanding of the failure mechanisms, all fracture surfaces were observed using scanning electron microscopy (SEM). In addition, fatigue behavior of this alloy was estimated using tension test under tension-tension condition at 30 Hz. The stress amplitude was selected in the range of 20~50 MPa to obtain the S-N curve. Findings: The tensile test indicated that the mechanical properties were not sensitive to the strain rates applied (3.3x10-4~0.1) and the plastic deformation was dominated by twining mediated slip. The impact energy is not sensitive to the environmental temperature. The plane strain fracture toughness and fatigue limit were evaluated and the average values were 7.6 MPa.m1/2 and 25 MPa, respectively. Practical implications: Tested materials AM60 Mg alloy can be applied among others in automotive industry aerospace, communication and computer industry. Originality/value: Many investigations have been conducted to develop new Mg alloys with improved stiffness and ductility. On the other hand, relatively less attention has been paid to the failure mechanisms of Mg alloys, such as brittle fracture and fatigue, subjected to different environmental or loading conditions. In this work, tension, impact, bend and fatigue tests were conducted in an AM60 magnesium alloy.

Grain boundary sliding during diffusion and dislocation creep in a Mg-0.7 pct Al alloy

Early studies on grain boundary sliding (GBS) in Mg alloys have suggested frequently that the contribution of GBS to creep is high even under conditions corresponding to dislocation creep. The role of creep strain and grain size in influencing the experimental measurements has not been clearly identified. Grain boundary sliding measurements were conducted in detail over experimental conditions corresponding to diffusion creep as well as dislocation creep in a single-phase Mg-0.7 wt pet Al alloy. The results indicated clearly that the GBS contribution to creep was Very high during,, diffusion creep at low stresses (similar to 75 pct) and substantially reduced during dislocation creep at high stresses (similar to 15 pct). These measurements were consistent with the observation of significant intragranular slip band activity observed in most grains at high stresses and very little slip band activity at low stresses. The experimental measurements and analysis indicated also that the GBS contribution to creep was high during the initial stages of creep and decreased to a steady-state value at large strains.

Influence of Cu and Cr on the matrix decomposition of quenched Al-Zn-Mg alloy

The Inoue procedure is used to study the influence of Cr and Cu elements, jointly or individually, on the matrix decomposition of quenched Al-Zn-Mg alloys. The addition of copper and copper with chromium does not significantly change the limits of the temperatures of formation of Guinier-Preston zone and the range of the matrix decomposition. The control of the vacancy concentration in the alloys by different heat treatments and the addition of certain elements such as copper and chromium seems to play an important role in the nucleation rate and the kinetics of phase transformations.

Slow Strain Rate Testing and Stress Corrosion Cracking of Ultra-Fine Grained and Conventional Al-Mg Alloy

Stress corrosion cracking susceptibility was investigated for an ultra-fine grained (UFG) AI-7.5Mg alloy and a conventional 5083 H111 alloy in natural seawater using slow strain rate testing (SSRT) at very slow strain rates between 1E(-5) s(-1), 1E(-6) s(-1) and 1E(-7) s(-1). The UFG Al-7.5Mg alloy was produced by cryomilling, while the 5083 H111 alloy is considered as a wrought manufactured product. The response of tensile properties to strain rate was analyzed and compared. Negative strain rate sensitivity was observed for both materials in terms of the elongation to failure. However, the UFG alloy displayed strain rate sensitivity in relation to strength while the conventional alloy was relatively strain rate insensitive. The mechanical behavior of the conventional 5083 alloy was attributed to dynamic strain aging (DSA) and delayed pit propagation while the performance of the UFG alloy was related to a diffusion-mediated stress relaxation mechanism that successfully delayed crack initiation events, counteracted by exfoliation and pitting which enhanced crack initiation. (C) 2014 Elsevier B.V. All rights reserved.

On the Controversy About the Presence of Grain Boundary Sliding in Mg AZ31

Highly-textured, rolled AZ31 sheet material shows a significant drop in the plastic anisotropy (r-value; r=εw/εt) in tension between 25°C and 200°C. This behavior was initially explained as a result of the increased activity of non-basal slip with increased temperature. Other authors suggested, however, that the mechanism resp onsible for this phenomenon was the activation of grain boundary sliding (GBS). Here, in-situ ten sile tests have been carried out in an SEM at various temperatures in order to obtain further evi dence of the role of GBS during moderate to high temperature deformation of Mg alloys, which remains highly controversial.

Continuum models of the mechanical behavior of rolled and die-cast magnesium alloys

En los últimos años ha habido una fuerte tendencia a disminuir las emisiones de CO2 y su negativo impacto medioambiental. En la industria del transporte, reducir el peso de los vehículos aparece como la mejor opción para alcanzar este objetivo. Las aleaciones de Mg constituyen un material con gran potencial para el ahorro de peso. Durante la última década se han realizado muchos esfuerzos encaminados a entender los mecanismos de deformación que gobiernan la plasticidad de estos materiales y así, las aleaciones de Mg de colada inyectadas a alta presión y forjadas son todavía objeto de intensas campañas de investigación. Es ahora necesario desarrollar modelos que contemplen la complejidad inherente de los procesos de deformación de éstos. Esta tesis doctoral constituye un intento de entender mejor la relación entre la microestructura y el comportamiento mecánico de aleaciones de Mg, y dará como resultado modelos de policristales capaces de predecir propiedades macro- y microscópicas. La deformación plástica de las aleaciones de Mg está gobernada por una combinación de mecanismos de deformación característicos de la estructura cristalina hexagonal, que incluye el deslizamiento cristalográfico en planos basales, prismáticos y piramidales, así como el maclado. Las aleaciones de Mg de forja presentan texturas fuertes y por tanto los mecanismos de deformación activos dependen de la orientación de la carga aplicada. En este trabajo se ha desarrollado un modelo de plasticidad cristalina por elementos finitos con el objetivo de entender el comportamiento macro- y micromecánico de la aleación de Mg laminada AZ31 (Mg-3wt.%Al-1wt.%Zn). Este modelo, que incorpora el maclado y tiene en cuenta el endurecimiento por deformación debido a las interacciones dislocación-dislocación, dislocación-macla y macla-macla, predice exitosamente las actividades de los distintos mecanismos de deformación y la evolución de la textura con la deformación. Además, se ha llevado a cabo un estudio que combina difracción de electrones retrodispersados en tres dimensiones y modelización para investigar el efecto de los límites de grano en la propagación del maclado en el mismo material. Ambos, experimentos y simulaciones, confirman que el ángulo de desorientación tiene una influencia decisiva en la propagación del maclado. Se ha observado que los efectos no-Schmid, esto es, eventos de deformación plástica que no cumplen la ley de Schmid con respecto a la carga aplicada, no tienen lugar en la vecindad de los límites de baja desorientación y se hacen más frecuentes a medida que la desorientación aumenta. Esta investigación también prueba que la morfología de las maclas está altamente influenciada por su factor de Schmid. Es conocido que los procesos de colada suelen dar lugar a la formación de microestructuras con una microporosidad elevada, lo cuál afecta negativamente a sus propiedades mecánicas. La aplicación de presión hidrostática después de la colada puede reducir la porosidad y mejorar las propiedades aunque es poco conocido su efecto en el tamaño y morfología de los poros. En este trabajo se ha utilizado un enfoque mixto experimentalcomputacional, basado en tomografía de rayos X, análisis de imagen y análisis por elementos finitos, para la determinación de la distribución tridimensional (3D) de la porosidad y de la evolución de ésta con la presión hidrostática en la aleación de Mg AZ91 (Mg- 9wt.%Al-1wt.%Zn) colada por inyección a alta presión. La distribución real de los poros en 3D obtenida por tomografía se utilizó como input para las simulaciones por elementos finitos. Los resultados revelan que la aplicación de presión tiene una influencia significativa tanto en el cambio de volumen como en el cambio de forma de los poros que han sido cuantificados con precisión. Se ha observado que la reducción del tamaño de éstos está íntimamente ligada con su volumen inicial. En conclusión, el modelo de plasticidad cristalina propuesto en este trabajo describe con éxito los mecanismos intrínsecos de la deformación de las aleaciones de Mg a escalas meso- y microscópica. Más especificamente, es capaz de capturar las activadades del deslizamiento cristalográfico y maclado, sus interacciones, así como los efectos en la porosidad derivados de los procesos de colada. ---ABSTRACT--- The last few years have seen a growing effort to reduce CO2 emissions and their negative environmental impact. In the transport industry more specifically, vehicle weight reduction appears as the most straightforward option to achieve this objective. To this end, Mg alloys constitute a significant weight saving material alternative. Many efforts have been devoted over the last decade to understand the main mechanisms governing the plasticity of these materials and, despite being already widely used, high pressure die-casting and wrought Mg alloys are still the subject of intense research campaigns. Developing models that can contemplate the complexity inherent to the deformation of Mg alloys is now timely. This PhD thesis constitutes an attempt to better understand the relationship between the microstructure and the mechanical behavior of Mg alloys, as it will result in the design of polycrystalline models that successfully predict macro- and microscopic properties. Plastic deformation of Mg alloys is driven by a combination of deformation mechanisms specific to their hexagonal crystal structure, namely, basal, prismatic and pyramidal dislocation slip as well as twinning. Wrought Mg alloys present strong textures and thus specific deformation mechanisms are preferentially activated depending on the orientation of the applied load. In this work a crystal plasticity finite element model has been developed in order to understand the macro- and micromechanical behavior of a rolled Mg AZ31 alloy (Mg-3wt.%Al-1wt.%Zn). The model includes twinning and accounts for slip-slip, slip-twin and twin-twin hardening interactions. Upon calibration and validation against experiments, the model successfully predicts the activity of the various deformation mechanisms and the evolution of the texture at different deformation stages. Furthermore, a combined three-dimensional electron backscatter diffraction and modeling approach has been adopted to investigate the effect of grain boundaries on twin propagation in the same material. Both experiments and simulations confirm that the misorientation angle has a critical influence on twin propagation. Non-Schmid effects, i.e. plastic deformation events that do not comply with the Schmid law with respect to the applied stress, are absent in the vicinity of low misorientation boundaries and become more abundant as misorientation angle increases. This research also proves that twin morphology is highly influenced by the Schmid factor. Finally, casting processes usually lead to the formation of significant amounts of gas and shrinkage microporosity, which adversely affect the mechanical properties. The application of hydrostatic pressure after casting can reduce the porosity and improve the properties but little is known about the effects on the casting’s pores size and morphology. In this work, an experimental-computational approach based on X-ray computed tomography, image analysis and finite element analysis is utilized for the determination of the 3D porosity distribution and its evolution with hydrostatic pressure in a high pressure diecast Mg AZ91 alloy (Mg-9wt.%Al-1wt.%Zn). The real 3D pore distribution obtained by tomography is used as input for the finite element simulations using an isotropic hardening law. The model is calibrated and validated against experimental stress-strain curves. The results reveal that the pressure treatment has a significant influence both on the volume and shape changes of individuals pores, which have been precisely quantified, and which are found to be related to the initial pore volume. In conclusion, the crystal plasticity model proposed in this work successfully describes the intrinsic deformation mechanisms of Mg alloys both at the mesoscale and the microscale. More specifically, it can capture slip and twin activities, their interactions, as well as the potential porosity effects arising from casting processes.

An inverse optimization strategy to determine single crystal mechanical behavior from polycrystal tests: Application to AZ31 Mg alloy

An inverse optimization strategy was developed to determine the single crystal properties from experimental results of the mechanical behavior of polycrystals. The polycrystal behavior was obtained by means of the finite element simulation of a representative volume element of the microstructure in which the dominant slip and twinning systems were included in the constitutive equation of each grain. The inverse problem was solved by means of the Levenberg-Marquardt method, which provided an excellent fit to the experimental results. The iterative optimization process followed a hierarchical scheme in which simple representative volume elements were initially used, followed by more realistic ones to reach the final optimum solution, leading to important reductions in computer time. The new strategy was applied to identify the initial and saturation critical resolved shear stresses and the hardening modulus of the active slip systems and extension twinning in a textured AZ31 Mg alloy. The results were in general agreement with the data in the literature but also showed some differences. They were partially explained because of the higher accuracy of the new optimization strategy but it was also shown that the number of independent experimental stress-strain curves used as input is critical to reach an accurate solution to the inverse optimization problem. It was concluded that at least three independent stress-strain curves are necessary to determine the single crystal behavior from polycrystal tests in the case of highly textured Mg alloys.