Increasing use of aluminum alloys in the automotive industry increases the importance of the production of sheet aluminum. To provide cost effective sheet aluminum to the industry, twin-roll casting (TRC) is becoming more important compared to DC casting. Demand for usage of different aluminum alloys in sheet form introduces some difficulties that should be considered during their applications. The main problem encountered during the welding of aluminum alloys is hot cracking. The aim of this study is to understand the difference in hot cracking susceptibility of two twin roll cast (TRC) aluminum-magnesium alloys (5754 and 5049 alloys) during welding. Varestraint test method was used to evaluate the effect of welding parameters, strain levels, filler alloys and mid-plane segregation on hot cracking susceptibilities. Hot cracking susceptibility of both 5049(Al-2wt%Mg) and 5754(Al-3wt%Mg) alloys increased with increasing strain level. Also, it was observed that hot cracking susceptibility was higher for the alloy having higher magnesium content. Thermal analysis results verified that hot cracking susceptibility indeed can be related to the v solidification range. As is suggested in the solidification range approach, the results of the present study confirm that the extent of solidification and liquation cracking depend on the magnitude of solidification range and the strain imposed during welding. Hot cracking susceptibility of 5754(Al-3wt%Mg) alloy has shown slightly decreasing behavior with addition of 5356 filler alloy. On the other hand, addition of 5183 filler alloy has increased solidification cracking susceptibility of two base alloys. The fracture surfaces of liquation and solidification cracks were investigated by scanning electron microscope with EDS. Liquation crack surfaces of the 5754(Al-3wt%Mg) alloy were found to have high Mg and Si content. For the 5754(Al-3wt%Mg) alloy, a quench test was designed to observe the effect of mid-plane segregation zone. It was observed that there was a eutectic reaction resulting in formation of liquid phase below solidus temperature of 5754(Al-3wt%Mg) alloy. Moreover, internal cracks have formed at the mid-plane segregation zone after Varestraint test. Results show that 5049(Al-2wt%Mg) alloy should be chosen compared to 5754(Al-3wt%Mg) alloy for welding. Moreover, low line energy should be applied and filler alloys with high magnesium content should be used during welding to decrease hot cracking tendency of welds.

Because of its low density and high strength, magnesium (Mg) and its alloys are being sought after in the automotive industry for structural applications. Although many road-going cars today contain cast Mg parts, in the fabrication of chassis structural members the wrought alloys are required. One of the challenges of fabrication with wrought Mg is welding and joining the formed sheets. Because of the commonly observed difficulties in fusion welding of Mg such as hot cracking and severe Heat Affected Zone (HAZ), this work aimed to establish the feasibility of the solid-state process Magnetic Pulse Welding in producing lap welds of Mg sheet. Mg AZ31 alloy sheets have been lap-welded with Magnetic Pulse Welding (MPW), an Impact Welding technique, using H-shaped symmetric coils connected to a Pulsar MPW-25 capacitor bank. MPW uses the interaction between two opposing magnetic fields to create a high speed oblique collision between the metal surfaces. The oblique impact sweeps away the contaminated surface layers and forces intimate contact between clean materials to produce a solid-state weld. Various combinations of similar and dissimilar metals can be welded using MPW. Other advantages of MPW are high speed, high strength, and the possibility of being mounted on a robotic arm. The present research focuses on the feasibility and mechanical performance of an MPW weld of 0.6 mm AZ31 Mg alloy sheets made in a lap joint configuration. Tensile shear tests were carried out on the joints produced. Load bearing capacity showed linear increase with capacitor bank discharge energy up to a certain value above which a parabolic increase was seen. Strength was estimated to be at least as high as base metal strength by measuring the fracture surface area of selected samples. The fracture surface of samples welded at higher discharge energy showed two regions. In the beginning of the bond a platelet-featured fracture brittle in appearance and a ductile, micro-voiding fracture in the latter part. The joint cross section morphology consisted of a flattened area that had two symmetric bond zones 1 mm wide each separated by an unbonded centre zone ~3mm wide. Reasons for the morphology were presented as a sequence of events based on the transient nature of the oblique collision angle. The interface microstructure was studied by optical and electron microscopy. Examination of the bonds has revealed sound and defect free interfaces. No microcracking, porosity, resolidification, or secondary phase formation was observed. Metallographic examination of the unbonded centre zone revealed anisotropic deformation and a lack of cleaning from the interface. This zone is formed as a result of normal impact in the initial stage of collision. The bond zone interface of the joint was characterized by a smooth interface consisting of refined grains. In samples welded at higher energy interfacial waves developed in the latter half of the bond zone. Transmission electron microscopy (TEM) of the bond zone revealed a continuous interface having an 8-25 μm thick interlayer that coincided with the waves and had a dislocation cell structure and distinct boundaries with adjacent material. Equiaxed 300 nm dynamic recrystallized (DRX) grains were found adjacent to the interlayer as well as other slightly larger elongated grains. The interlayer is thought to be formed in plasticized state at elevated temperature through severe shear strain heating. The interlayer corresponds to a ductile fracture surface and, along with the interfacial waves, is responsible for the joint’s high strength.

Additive friction stir deposition (AFSD) of AZ31B magnesium alloy was conducted to examine evolution of grain structure, phases, and crystallographic texture. AFSD was carried out using a hollow tool made from tool steel at a constant rotational velocity of 400 rpm on the AZ31B base plate. Bar stock of AZ31B was utilized as a feed material. The linear velocity of the tool was varied in the range of 4.2-6.3 mm/s. The feed rate of the material had to be maintained at a half value compared to the corresponding linear velocity for the successful deposition. The layer thickness and length of the deposits were kept constant at 1 mm and 50 mm respectively. The tool torque and actuator force values were recorded during the process and for calculation of the average input energy for each processing condition. Temperature during the AFSD experiments was monitored using a type k thermocouple located 4 mm beneath the deposition surface at the center of the deposition track. The average input energy values showed a decreasing trend with increasing tool linear velocity. The temperature values during deposition were ∼0.7 times the liquidus of the alloy. The deposited material then was examined by laser microscope and profilometer, X-ray diffraction, scanning electron microscopy, electron back scatter diffraction (EBSC), contact angle measurement and micro hardness tests. The AFSD AZ31B samples showed reduction in areal surface roughness with an increase in the tool linear velocity. The X-ray spectra revealed increase in the intensity of prismatic planes of α-Mg phase with increase in tool linear velocity. AFSD of AZ31B Mg alloy resulted in shifting of the grain size from a broader and courser distribution within the feed material to a tighter distribution. Moreover, EBSD observations confirmed the refinement in grain size distribution as well as the presence of predominantly prismatic texture for the AFSD samples when compared to the feed material. There was a marginal improvement in the hardness for the AFSD samples compared to the feed material. However, there was no significant change in the contact angle measurements in simulated body fluid for the AFSD samples compared to the feed material. The current work demonstrated ability of AFSD technique for the additive fabrication of magnesium-based alloys and provided a methodology for examining various process attributes influencing the processing-structure-property relationship.

As ligas de magnésio atraíram a atenção novamente nos últimos anos por causa de suas propriedades de baixa densidade, resistência à tração e rigidez específica. Por outro lado, a maior limitação para o uso de ligas trabalhadas é a baixa conformabilidade em temperatura ambiente devido à estrutura hexagonal compacta (HCP) das ligas. O presente trabalho de pesquisa teve como objetivo estudar o encruamento, recristalização e crescimento de grãos durante a laminação de liga magnésio AZ31B em alta e baixa temperatura, analisando a evolução da microestrutura, da textura e a variação das propriedades sensíveis à microestrutura. A liga AZ31B é sensível à taxa de deformação em alta temperatura, entretanto, a anisotropia é negativamente afetada na laminação a frio, portanto, apresenta uma melhor laminação na faixa de temperaturas de 200 a 300ºC, devido ao refinamento de grãos, causado pela recuperação e recristalização dinâmica. O estudo foi realizado em amostras de uma chapa de liga de magnésio AZ31B recristalizada (2 mm de espessura). Amostras foram deformadas por laminação em temperaturas diferentes (25, 100, 200, 250 e 300ºC) e com diferentes taxas de deformação. A caracterização microestrutural foi realizada com auxílio de várias técnicas complementares de análise microestrutural, tais como microscopia óptica, microscopia eletrônica de varredura, análise de raios-X por dispersão de energia, difração de raios X e microdureza Vickers. A deformabilidade e a ocorrência de recristalização dinâmica e crescimento de grãos mostraram forte dependência com as condições de laminação. Na laminação a frio, o refinamento de grão foi mais efetivo com baixas taxas de deformação (1,6 s-1) do que na laminação a quente. Entretanto, a intensa textura basal foi enfraquecida em temperaturas próximas a 300ºC e com taxas de deformação próximas a 3,5 s-1. A ductilidade das ligas pode ser melhorada em altas temperaturas de deformação, pelo refinamento dos grãos que produz a diminuição da fração volumétrica das regiões macladas e pelo aumento do número de sistemas de deslizamento, além do enfraquecimento da intensa textura basal, característica das ligas de magnésio. / Magnesium alloys have attracted the attention again in recent years because of their low density, their specific tensile strength and rigidity. However, the greatest limitation for the usage of wrought magnesium alloys is their poor formability at room temperature due to the hexagonal closed packed (HCP) crystal structure. The present research focused on study the work-hardening, recrystallization and grain growth during rolling of AZ31B magnesium alloy at low and high rolling temperature. It was made through the analysis of microstructure and texture evolution and variations of microstructure-sensitive properties. The AZ31 magnesium alloy is sensitive to strain rate at high temperature, meanwhile, the anisotropy is adversely impacted in cold rolling sheets. Thus, AZ31B magnesium alloy exhibits better workability in 200-300°C temperature range due to the grain refinement caused by dynamic recovery and dynamic recrystallization. This research was carried out on samples of recrystallized sheet (2 mm in thickness). Samples were deformed by rolling at different temperatures (25, 100, 200, 250 and 300°C), using different strain rates. Microstructural characterization was done by using several complementary techniques of microstructural analysis, such as optical microscopy, scanning electron microscopy, X-ray analysis by energy dispersive, X-ray diffraction and Vickers microhardness tests. A competition between dynamic recrystallization and grain growth depends on rolling conditions. Low strain rate (1,6 s-1) at cold rolling improved more effective in refining grains than warm rolling. Meanwhile, the intense basal texture was weakened at 300°C with a high strain rate of 3,5 s-1. The ductility of magnesium alloys can be greatly improved at high temperature, with a fine grain structure that causes the reduced volume fraction of twins, and an increase the number of slip systems, weakening the intense basal texture, rather characteristic for magnesium alloys.

The design of new engineering materials resistant to both wear damage and corrosion degradation becomes increasingly demanding in complex service conditions. Unfortunately, there is typically a tradeoff between wear and corrosion resistance, even for important passive metals such as Al alloys. This is because the presence of precipitates hardens the material but at the same time lead to unfavorable galvanic coupling between the precipitates and the matrix, resulting in accelerated corrosion. This work showed that Al (or Mg) supersaturated solid solution formed using non-equilibrium methods exhibited enhanced corrosion resistance without compromising strength. For Al, alloying with Mn up to ~ 20.at.% simultaneously increased the wear resistance of Al as well as the protectiveness of the passive layer, thus improving the overall tribocorrosion resistance. For Mg, alloying with Y (4.67 wt.%), Zr (0.45 wt%), and Nd (1.79 wt%) in solid solution led to ~ 8 fold increment in corrosion resistance in physiological environment. Magnetron-sputtered aluminum (Al) and aluminum–manganese (Al-Mn) films with structures ranging from nanocrystalline to amorphous were obtained by tuning the Mn% up to 20.5 at.%. Corrosion behavior of the films was investigated in 0.6 M and 0.01 M NaCl aqueous solutions by potentiodynamic polarization (PD) and electrochemical impedance spectroscopy (EIS). Pitting corrosion was found to be strongly affected by alloy composition. The amorphous Al–20.5 at.% Mn exhibited the best pitting resistance during short term exposure. However, over longer immersion in 0.01 M NaCl up to 108 hrs, nanocrystalline Al–5.2 at.% Mn showed the highest corrosion resistance. The dual-phase Al-11.5 at % Mn alloy was found to have higher nominal corrosion rate compared to its nanocrystalline or amorphous counterparts. The effects of Mn alloying on the tribocorrosion behavior of magnetron-sputtered Al-Mn thin films with 5.2 at.% and 20.5 at.% Mn were investigated in 0.6 M NaCl aqueous solution. Tribocorrosion resistance of Al-Mn was found to be strongly affected by the alloying composition and applied potential. Higher Mn content increased H/E ratio and promoted the formation of denser and more compact passive film, hence improving tribocorrosion resistance of Al. In particular, alloying with 20.5 at.% Mn led to an increase of the corrosion resistance by ~ 10 times and the hardness ~ 8 times compared to pure Al. The total material loss during tribocorrosion was found to increase with applied potential. When the applied potential was increased from cathodic to anodic, simultaneous contribution of the mechanical and the electrochemical wear leads to accelerated material loss. A galvanic cell model was used to investigate the depassivation-repassivation kinetics during tribocorrosion. It was found that alloying with 5.2 at.% Mn led to more than 10-fold reduction in the current density required to re-passivate similar worn areas compared to pure Al. The origin of wear-corrosion synergy was discussed based on these observations. Magnesium alloys such as WE43 are considered for biomedical applications including cardiovascular stents and bone implants due to their biocompatibility, good cell adhesion, and mechanical properties close to that of bones. Unfortunately, their high degradation rate and subsequent loss of structural integrity in physiological environments hinders such applications. To improve the corrosion resistance of WE43 magnesium alloy, its microstructure was optimized to prevent micro-galvanic coupling between Mg matrix and precipitates. Chemically homogeneous WE43 with nanoscale surface roughness was obtained by magnetron sputtering with high effective quench rate. The effect of chemical heterogeneity on the corrosion resistance of biodegradable WE43 magnesium alloy was studied by performing corrosion tests in blood bank buffered saline using samples from two metallurgical states, cast and deposited. The microstructure of all samples was investigated by grazing incidence X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The deposited samples, prepared by magnetron sputtering using targets with the same global composition as cast WE43, exhibited chemically homogeneous microstructure without the formation of secondary phases typically observed in the cast alloy. The corrosion behavior was studied by PD and EIS tests. It was found that the deposited alloy showed enhanced corrosion resistance, ~8-fold reduction in corrosion rate compared to the cast alloy, owing to the elimination of micro-galvanic coupling between the Mg matrix and the precipitates. In-situ monitoring of hydrogen bubble evolution during corrosion indicated significantly reduced cathodic reaction kinetics in the deposited alloy. Post-corrosion surface and cross-sectional SEM studies showed that the high corrosion rate in the cast alloy was associated with the formation of severely cracked corrosion products preferably around Zr- and Y-containing precipitates.

Magnesium is the lightest metal that can be used for structural applications. For the reasons of weight saving, there has been an increasing demand for magnesium from the automotive industry. However, poor formability at room temperature, due to a limited number of slip systems available owing to its hexagonal close packed crystal structure, imposes severe limitations on the application of Mg and its alloys in the wrought form. One possibility for improving formability is to form the components superplastically. For this, it is necessary to refine the grain structure. A fine-grained material is also stronger than its coarse grain counterpart because of grain size strengthening. Moreover, fine-grained magnesium alloys have better ductility as well as a low ductile to brittle transition temperature, thus their formability at room temperature could be improved. In addition to grain refinement, the issues pertaining to poor formability or limited ductility of Mg alloys can be addressed by controlling the crystallographic texture. Recently, it has been shown that warm equal channel angular extrusion (ECAE) of magnesium led to reduction in average grain size and shear texture formation, by virtue of which subsequent room temperature rolling was possible. Based on the literature, it was also certain that, in order to make magnesium alloys amenable for processing, grain refinement needs to be carried out and the role of shear texture needs to be explored. Since processing at higher temperature would lead to relatively coarser grain size, large strain deformation at lower temperatures is desirable. The present thesis is an attempt to address these issues. The thesis has been divided in to eight chapters. The chapters 1 and 2 are dedicated to introduction and literature review on the subject that provides the foundation and motivation to the present work. Subsequent chapters deal with the research methodology, experimental and simulation results, discussion, summary and conclusion. In the present investigation, two single phase alloys were chosen, the commercially pure magnesium and the magnesium alloy AM30. These materials were subjected to suitable processing techniques, detailed posteriori. A systematic analysis of microstructure and texture for each of the as-processed materials was performed by electron backscattered diffraction (EBSD) using a field emission gun scanning electron microscope (FEG-SEM). Bulk texture measurement by X-ray diffraction, neutron diffraction and local texture measurement by synchrotron X-rays were also carried out. In addition, dislocation density was measured using X-Ray diffraction line profile analysis (XRDLPA). The experimental textures were validated by using Visco-Plastic Self Consistent (VPSC) simulation. The details of experimental as well simulation techniques used in the present investigation is described in chapter 3. To understand the philosophy of large strain deformation by shear in magnesium and its alloy, free end torsion tests could provide a guide line. Based on the understanding developed from these tests, further processing strategy could be planned. Therefore, a rigorous study of deformation behaviour under torsion was carried out. In chapter 4, the results of free end torsion tests carried out at different temperatures, 250⁰C, 200⁰C and 150⁰C and strain rates, 0.01 rad.s-1, 0.1 rad.s-1, 1 rad.s-1 are presented for both the alloys. In addition to the analysis of stress-strain behaviour, a thorough microstructural characterization including texture analyses pertaining to deformation and dynamic recrystallization was performed. Both pure Mg and the AM30 alloy exhibit similar ductility under the same deformation condition, while the strength of AM30 was more. The strain hardening rate decreased with temperature and increased with strain rate for both the materials. However, the strain hardening rate was always higher in case of the alloy AM30. Large amount of dynamic recrystallization (DRX) was observed for both the alloys. The initial texture had an influence on the deformation behaviour under torsion and the resulting final texture. The initial non-axisymmetric texture of pure Mg samples led to nonaxisymmetric deformation producing ear and faces along the axial direction, and the final texture was also non-axisymmetric. An examination of the texture heterogeneity was carried out in one of the pure Mg torsion tested samples by subjecting it to EBSD examination at different locations of the surface along the axial direction. The strain induced on the ear portion was maximum, and in the face was lower. This has been attributed to the orientation of basal planes in the two regions. The axisymmetric initial texture in case of the alloy AM30 led to the formation of axisymmetric texture with no change in the shape of the material. Owing to this simplicity, the occurrence of dynamic recrystallization (DRX) was studied in more detail for this alloy. The mechanism of texture development due to deformation as well as dynamic recrystallization could be tracked at every stage of deformation. A typical shear texture was observed with respect to the strain in each case. Very low fraction of twins was observed for all the cases indicating slip dominated deformation, which was validated by VPSC simulation. It was found that with the increase in strain during torsion, the fraction of dynamically recrystallized grains increased. The recrystallization mechanism was classified as “continuous dynamic recovery and recrystallization” (CDRR) and is characterized by a rotation of the deformed grains by ~30⁰ along c-axis. After developing an understanding of large strain deformation behaviour of pure Mg and the alloy AM30 through torsion tests, the possibility of low temperature severe plastic deformation for both the materials by equal channel angular extrusion (ECAE) was explored. The outcome of this investigation has been presented in chapter 5. At first, ECAE of pure magnesium was conducted at 250⁰C up to 4 passes and then the temperature was reduced by 50⁰C in each subsequent pass. In this way, ECAE could be carried out successfully up to 8th pass with the last pass at room temperature. A grain size ~250 nm and characteristic ECAE texture with the fibres B and C2 were achieved. The AM30 alloy subjected to similar processing schedule as pure Mg, however, could be deformed only up to 6th pass (TECAE=150⁰C) without fracture. An average grain size ~ 420 nm and a texture similar to ECAE processed pure Mg was observed for this alloy. The difference in the deformation behaviour of the two alloys has been explained on the basis of the anisotropy in the stacking fault energy (SFE) in the case of pure Mg. Neutron diffraction was carried out to confirm and validate the microtexture results obtained from the EBSD data, while the local texture measurement by synchrotron radiation was carried out at different locations of the ECAE samples to give a proper account of the heterogeneity in texture. The effect of grain refinement was examined, deconvoluting the effect of shear in improving the strength and ductility using another severe plastic deformation technique, namely multi axial forging (MAF). In this process, the material was plastically deformed by a combination of uniaxial compression and plane strain compression subsequently along all the three axes. The details of this investigation has been presented in chapter 6. By this method, the alloy AM30 could be deformed without fracture up to a minimum temperature of 150⁰C leading to ultra-fine grain size (~400 nm) with very weak texture. A room temperature ductility ~55% was observed for this material. Finally, a comparison of room temperature mechanical properties of the alloy AM30 was carried out for the ECAE and MAF processed conditions having similar grain size in order to observe the effect of texture formed during both the processes. A similar strength and ductility for both the cases was attributed to the orientation obtained from both the ECAE and MAF, which is away from the ideal end orientation for tensile tests. The final outcomes of the thesis has been summarized in chapter 7.

Magnesium and its alloys are interesting materials due to their many physical properties. They have considerable potential, especially in medical applications, where they can serve as a material for the production of orthopedic and cardiovascular implants. The disadvantage of these materials is their sensitivity to corrosion. As a result, it is necessary to know the corrosive properties of magnesium and its alloys in contact with substances that occur in the human body. Hyaluronan is a polysaccharide that is naturally present in the human body and can interact with implants. This master's thesis deals with the influence of low molecular weight (80–130 kDa) and high molecular weight (1 500–1 750 kDa) hyaluronan on the corrosion properties of magnesium alloy AZ31 in the environment of two simulated physiological solutions (0,9 % NaCl and synovial fluid). Potentiodynamic polarization (PD) and electrical impedance spectroscopy (EIS) were used for electrochemical tests. Surface analysis was performed using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) to reveal the chemical composition of the corrosion products and the surface morphology after corrosion.

This master´s thesis is focused on classification of corrosion resistivity magnesium alloy type AZ91 in environment of salt vapour testing in corrosion chambers. For tests were used samples of magnesium alloy manufactured by three different methods of casting: cast-iron mold, die vacuum casting, die casting without vacuum and method of die casting with additional pressure (squeeze casting). In this work was accomplished metallographic evaluation of corrosion attack and detailed analysis of corrosion products. Conclusions of exposits tests are assembled of analysis of influence of corrosion environment on structure of alloy. On the basis of these conclusions of corrosion tests were evaluated influences of corrosion speed [mm/year] on time [hours] for individual states of magnesium alloy.

This work is focused on the study of the relationship between microstructure, texture and deformation mechanisms in aluminum-free magnesium (Mg) alloys. Extruded alloys containing zirconium, zinc, manganese and neodymium (ZK10, MN11, ZN11) in a form of rectangular profiles were deformed at room temperature. Uniaxial tensile and compression tests were performed in the extrusion (ED), transversal (TD) and normal direction (ND). The concurrent acoustic emission (AE) measurement was used in order to study the collective dislocation dynamic and the nucleation of twins. The deformation texture was studied by X-ray diffraction on samples deformed in compression up to different stress levels. Keywords: Mg alloys, deformation tests, acoustic emission, texture

Title: Microstructure and mechanical properties of lightweight structural AZ31 alloy prepared by twin-roll casting method Author: Mariia Zimina Abstract: Microstructure of AZ31 twin-roll cast magnesium alloy was studied using light optical, electron and atomic force microscopy. The effect of annealing temperature on the microstructure was tested. Mechanical properties of a thin magnesium strip were investigated by means of microhardness tests and tensile tests at a relatively low strain rate 10-3 s-1 . Results show that the ductility of the twin roll cast strip increases with increasing deformation temperature, however, a remarkable decrease was observed at about 200 řC. This effect appears also in a conventionally cast ingot of a master alloy and is caused by a change of a deformation mode occurring at this temperature. Moreover, the effect of severe plastic deformation on the microstructure and mechanical properties was studied. Equal channel angular pressing was applied on magnesium strip samples and lead to a significant grain refinement accompanied by an unfavorable strengthening of the initial basal texture, which is effectively suppressed by a subsequent annealing. A constrained groove pressing was for the first time successfully applied on AZ31 twin-roll cast strip leading to an increase of...