This master’s thesis deals with design and preparation of a new biodegradable magnesium alloy based on Mg-Ca-Zn. Based on information from literature, the Mg-3Zn-2Ca alloy was designed. The base material was produced by gravity casting and the evaluation in the as-cast and heat treated state was performed. For preparation of the experimental material, following methods were designed: squeeze casting, hot rolling and the ECAP. During preparation by hot rolling, no optimal conditions were found and significant cracks occurred in both as-cast and heat treated material. In the case of experimental material, prepared by the ECAP method with back-pressure, better combination of stress-strain properties was observed. Also the squeeze casting method showed improvement; especially the amount of casting defects was eliminated. The evaluation of microstructure and mechanical properties was performed by the light and scanning electron microscopy, RTG phase analysis and the tensile and compression tests.

This doctoral thesis deals with the fatigue behaviour of AZ31 and AZ61 magnesium alloy casted by advanced methods of casting squeeze casting. Based on the regression functions and measured fatigue data were determined fatigue characteristics of these alloys. The work also extends into the area of fatigue cracks in the AZ31 alloy. Were measured fatigue crack propagation rate on modified cylindrical specimens. The paper also outlines the possibilities for describing the fatigue behaviour of AZ61 alloy in extremely low-cycle fatigue.

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Today, there is an essential need for lightweight, energy-efficient, environmentally benign engineering systems, and this is the driving force behind the development of a wide range of structural and functional materials for energy generation, energy storage, propulsion, and transportation. These challenges have motivated the use of magnesium alloys for lightweight structural systems. Magnesium has a density of 1.74 g/cm3, which is almost 30% less than that of aluminium, one quarter of steel, and almost identicalto polymers. The ease of recycling magnesium alloys as compared to polymers makes them environmentally attractive, but their poor mechanical performance is the primary reason for the limited adoption of these alloys for structural applications. The Mg-Al-Zn alloy AZ91D exhibits an excellent combination of strength, die-castability, and corrosion resistance. However, its mechanical performance with regard to creep strength, for example, at evaluated temperatures is poor. Moreover, very little is known about the correlation between its mechanical properties and microstructural features. This thesis aims to provide new knowledge regarding the role played by microstructure in the mechanical performance of the magnesium alloy. The properties/performance of the material in relation to process parameters became of great interest during the investigation. An exhaustive characterisation of the grain size, secondary dendrite arm spacing (SDAS) distribution, and fraction of Mg17Al12 was performed using optical and electron backscatter diffraction (EBSD). These microstructural parameters were correlated to the offset yield point (Rp0.2), fracture strength, and elongation to failure of the material. It was proposed that the intermetallic phase, Mg17Al12, plays an important role in determining the mechanical and physical properties of the alloy in a temperature range of room temperature to 190°C by forming a rigid network of intermetallic. The presence of this network was confirmed by studying the thermal expansion behaviour of samples of the alloy containing different amounts of Mg17Al12. A physically based constitutive model with a wide validity range was successfully adapted to describe the flow stress behaviour of AZ91D with various microstructures. The temperature-dependent variables of the model correlated quite well with the underlying physics of the material. The model was validated through comparison with dislocation densities obtained using EBSD. The influence of high-pressure die-cast parameters on the distortion and residual stress of the cast components was studied, as were distortion and residual stress in components after shot peening and painting. Interestingly, it was found that intensification pressure has a major effect on distortion and residual stresses, and that the temperature of the fixed half of the die had a slight influence on the component's distortion and residual stress. / Numera finns det ett väsentligt behov av lätta, energieffektiva och miljövänliga tekniksystem. Detta behov är drivkraften för utveckling av ett brett utbud av material för energigenerering, energilagring, framdrivning och transport. Dessa utmaningar motiverade användningen av magnesiumlegeringar för lättviktskonstruktioner. Magnesium har en densitet på 1,74 g/cm3, vilket är ca 30% lägre än för aluminium, en fjärdedel av densiteten för stål och nästan i nivå med många polymerer. Då magnesiumlegeringar dessutom är lätta att återvinna, jämfört med polymerer, gör det dem miljömässigt attraktiva. Låga mekaniska egenskaper är den främsta orsaken till begränsad användning av dessa legeringar för lastbärande tillämpningar. Mg-Al-Zn-legeringen AZ91D uppvisar en utmärkt kombination av styrka, gjutbarhet och korrosionsbeständighet. Dess mekaniska egenskaper vid förhöjd temperatur, som tex kryphållfasthet, är låga. Dessutom är korrelationen mellan mikrostruktur och mekaniska egenskaper oklar. Denna avhandling syftade till att ge ny kunskap om mikrostrukturens roll för magnesiumlegeringars mekaniska egenskaper. Slutligen var materialets egenskaper i förhållande till processparametrar vid tillverkningen av stort intresse. En omfattande karaktärisering av kornstorleks-, sekundära dendritarmavstånds (SDAS)-fördelning och fraktion av Mg17Al12 utfördes med hjälp av optisk mikroskopering och diffraktion av bakåtspridda elektroner (EBSD). Mikrostrukturen korrelerades till sträckgränsen (Rp0.2), brottstyrkan och brottförlängningen. Det föreslogs att den intermetalliska fasen, Mg17Al12, spelar en viktig roll vid bestämning av legeringens mekaniska och fysikaliska egenskaper vid temperaturintervall från rumstemperatur upp till 190°C genom att bilda ett styvt nätverk av intermetaller. Uppkomsten av ett sådant nätverk stöddes genom en studie av den termiska expansionen av legeringen för olika fraktioner av Mg17Al12. En fysikalisk konstitutiv modell med ett brett giltighetsområde användes framgångsrikt för att beskriva det plastiska flytbeteendet hos AZ91D för olika mikrostrukturer. De temperaturberoende variablerna i modellen korrelerade ganska väl med materialets underliggande fysik. Modellen validerades genom att jämföra dislokationstätheten som predikterades av modellen och den med EBSD uppmätta dislokationstätheten. Påverkan av pressgjutningsparametrar på geometrisk tolerans och restspänning hos de gjutna komponenterna studerades. Vidare studerades geometrisk tolerans och restspänning av komponenter efter pening och målning. Intressant nog hade eftermatningsfasen en stor effekt på geometrisk tolerans och restspänningar. Dessutom hade temperaturen på den fasta formhalvan av verktyget även ett visst inflytande på komponentens geometriska tolerans och restspänning.

Magnesium alloys have emerged as a promising material for light-weighting due to their potential for higher weight saving compared with advanced high-strength steel, aluminium alloys and glass fibre reinforced polymer composites based on equal stiffness or strength. Even though magnesium alloys offer low density, high strength to weight ratio and excellent machinability their poor creep resistance and low yield strength at elevated temperatures (~150oC) restricts their use in automotive powertrain applications. Possible ways of improving the creep resistance include development of creep resistant alloys and/or reinforcing the alloy with ceramic particulates, fibres/whiskers. Several magnesium alloys such as – Mg-Zr based alloys, Mg-Al-RE alloys (RE: rare earth), Mg-Al-Ca alloys, Mg-Al-Sr alloys, Mg-Al-Sr-Ca alloys, Mg-Al-Si alloys offer improvement in creep resistance to different extent. However, these alloys are relatively expensive than the widely used Mg-Al-Zn alloys. Some of these alloys are unsuitable for die casting application due to cracking or die filling problems for example, in Ca and Sr containing alloys their content must be controlled to avoid castability problems. Discontinuous reinforcement of magnesium alloys opens up wide variety of casting techniques for production. Most of the components do not require high performance capability all throughout the component. Squeeze casting technique can be used to economically produce selectively reinforced composites having complex near-net-shape components. By selectively reinforcing only the regions of stress concentration, material property can be optimised at the same time lowering both the cost of manufacturing and machining. In the present study, wear behaviour of Saffil short fibre reinforced AZ91D Mg alloy composite prepared by squeeze casting is explored. The Mg-Saffil composite had a two dimensional planar random fibre orientation which was inherent to the fabrication process of porous fibre preform. In the as-polished specimen fibres protrude out of the Mg matrix due to differential polishing. The Mg-Saffil composites were subject to unidirectional sliding wear against steel counterface under nominally dry condition in ambient atmosphere at low velocities, to simulate the piston reversal at the top dead centre of an engine wherein lubrication starvation results in wear of engine cylinder. The fibres protruding out of the magnesium matrix prevent the softer Mg matrix coming in contact with the counterface material. The worn surface was examined by means of scanning electron microscopy and the physical and chemical changes caused by the wear processes were characterised using different spectroscopic techniques. The effect of fibre distribution and fibre orientation on wear of the composite was studied. Depending on the radius of curvature of the counterface, inhomogeneities in the fibre distribution up to a certain length scale were permissible without deteriorating the wear resistance of the composite. The normal fibre orientation proved deleterious to the wear of the counterface. But wear of the composite was independent of the fibre orientation of the wear surface. In contrast to unreinforced AZ91 Mg alloy which undergoes extensive wear, the steel counterface was machined by the hard alumina fibres protruding out of the matrix. With progressive sliding a discontinuous patch of transferred material formed on the worn surface. Eventually, an oxidised iron-rich transfer layer formed on the worn surface due to compaction of the transferred material and wear debris under the combined action of applied normal load and frictional force. The coefficient of friction plateaus following an initial rapid increase with the increase in the areal coverage of the transfer layer. The abrupt increase in friction coincides with the change in contact at the sliding interface from protruding alumina fibres/steel counterface to mostly between the transferred layer and steel counterface. The increase in friction due to the iron-rich transfer layer formed on the worn surface induced bending stresses in the fibre. A correlation between the incipient fibre fracture and build-up of the transfer layer was observed. Wear of the composite was governed by the dawn of the fibre fracture event, which in turn leads to three-body wear. Diamond-like carbon coatings are well-known for their low friction, high hardness and elastic modulus, chemical inertness and optical transparency. They have found widespread use due to their superior tribological characteristics as protective coatings for magnetic storage media (hard-disk drives), in micro-electromechanical devices (MEMS), biomedical applications (joint implants, artificial heart valves), optical windows (anti-reflection coating) and razor blades. The physical and mechanical properties of these coatings can be tailored by controlling the sp3 /sp2 ratio and modification via alloying with metals such as W, Ti, Cr, Al; or non-metallic elements such as B, N, F, Si. A tungsten doped hydrogenated diamond-like carbon coated steel counterface was used to rule out or minimise any chemical and physical interaction between the composite and the counterface. The composite exhibited a higher wear resistance when slid against a DLC coated steel counterface due to ease of interfacial sliding between the carbon-rich transfer layer and the DLC coated counterface. The transition from ultra-mild to mild wear was not altogether suppressed but delayed to higher loads, prolonging the ultra-mild wear regime. As a result of reduced friction the point of maximum shear stress recedes from the surface, which manifests as subsurface cracks. The dominant wear mechanism of Mg-Saffil composite sliding against the DLC coated counterface was delamination wear.

Dans ce projet, le matériau est l'alliage de magnésium AZ31-O en tôle. L'épaisseur de tôles est de 1,2 mm. Les essais de traction à chaud sont réalisés afin d'étudier la ductilité de l'alliage de magnésium AZ31-O, la température et l'influence la vitesse de déformation sont incluses dans tous les tests. Le résultat d'analyse montre que la ductilité est renforcée avec une température croissante et une vitesse de déformation décroissante, le phénomène d'adoucissement est évident à la température élevée. La propriété anisotrope n'est pas considérée dans ce projet. Les essais Nakazima à chaud avec le poinçon d'hémisphère sont réalisés pour étudier la formabilité de l'alliage de magnésium AZ31-O. Enfin, la FLD (Forming Limit Diagram) est identifiée et les comparaisons montrent que la formabilité est préférable à une température plus élevée. En outre, les prédictions des limites de formage sont effectuées dans le modèle M-K. La comparaison montre clairement avec la prédiction théorique ne convient pas avec l'expérience. Les simulations des éléments finis sont effectuées pour un emboutissage par poinçon hémisphérique et un emboutissage en croix. Tout d'abord, les simulations d'emboutissage de poinçon hémisphérique sont réalisés sur FORGE® et sur ABAQUS®. Les résultats des simulations de FORGE et de ABAQUS sont comparés afin d'étudier la différence de divers codes de simulation des éléments finis. Deuxièmement, le comportement de d'endommagent est étudié dans FORGE par modèle d'endommagement Lemaitre. Enfin, la simulation d'emboutissage en croix qui est un benchmark de la conférence 2011 NUMISHEET est réalisée avec FORGE. La charge de poinçon, l'épaisseur et la distribution de température sont obtenues et comparées pour chaque simulation. En outre, ces résultats de la simulation de benchmark (FORGE) sont également comparés à d'autres logiciels de simulation en conférence. Les résultats des analyses détaillées sont présentés dans cette thèse. / In this project, the material is AZ31-O magnesium alloy sheet. The sheet thickness is 1.2mm. Warm tensile tests are performed to study ductility of AZ31-O magnesium alloy, the temperature and strain rate influence are included in all tests. The analysis result shows the ductility is enhanced with temperature increasing and strain rate decreasing, and the softening phenomenon is obvious at high temperature. The anisotropic property is not considered in this project. Warm Nakazima tests with hemisphere punch are performed to study formability of AZ31-O magnesium alloy. Finally, the FLD (Forming Limit Diagram) is identified and the comparisons distinctly show that the formability is better at higher temperature. Moreover, the forming limits predictions are performed in M-K model. The comparison clearly shows the theoretical prediction do not fit well with experiment. Finite element simulations are performed for a hemisphere punch deep drawing and a cross-shaped deep drawing. Firstly, the hemisphere punch deep drawing simulations are performed in FORGE® and ABAQUS®. The simulation result from FORGE and ABAQUS are compared in order to study the difference of various finite element simulation codes. Secondly, the damage behavior is studied in FORGE by Lemaitre damage model. Finally, the cross-shaped deep drawing simulation which is a benchmark of NUMISHEET 2011 conference is performed with FORGE. The punch load, thickness and temperature distribution are obtained and compared for each simulation. Furthermore, this benchmark simulation results (FORGE) are also compared with other various simulation software in conference. The detailed analysis results are presented in this thesis.

The proposed dissertation thesis deals with the characterization of HVOF and APS-thermally sprayed coatings prepared on the AZ31 and AZ91 magnesium substrates. The theoretical part of the thesis describes in-detail Mg substrates used in the experimental part of the thesis. There are also characterized materials and coatings based on NiCrAlY and FeCrNiMoSiC metals, WC-CoCr cermets, and YSZ ceramic materials. At the end of the theoretical part, the literary research summarizing the characterization and analysis performed on thermally sprayed coatings on Mg alloys. Based on the theoretical knowledge, the characterization of Mg substrates and deposited coatings was performed in terms of the surface morphology, microstructure, and the chemical composition using the light microscopy (LM) and scanning electron microscopy with energy-dispersive spectroscopy (SEM+EDS). The phase composition of the coatings was analyzed using the X-ray diffraction (XRD). The diffractions corresponding to the sprayed coatings were compared with the feedstock powders, i.e. materials used for the spraying of the coatings. The characterization of the prepared coatings in terms of the mechanical and tribological properties was performed. The hardness and microhardness of the coatings as well as the coefficient of friction, and the wear rate were measured. The last chapter of the experimental part deals with the evaluation of the electrochemical corrosion properties by the potentiodynamic measurements in a 3.5% NaCl solution. In the case of exposed samples, the evaluation of the surface and coating/substrate interface was performed using LM and SEM with EDS. The mechanism of the corrosion attack and degradation was determined from the acquired knowledge and base on the results of the short-term measurements. Based on the measured results, it can be stated that the deposited coatings were successfully applied on the surface of both Mg alloys. All the coatings increase the surface hardness of the Mg alloys and significantly improve their tribological properties. However, except for FeCrNiMoSiC coatings, the corrosion properties of Mg alloys deteriorate due to the fact that the corrosion environment can pass through the coating to the less noble Mg substrate and the corrosion microcells are created.

Im Rahmen der vorliegenden Arbeit sind die Struktur und die Wasserstoffsorptionseigenschaften neuer nanokristalliner, hydridbildender magnesiumbasierter Legierungen, die mittels Rascherstarrung (Melt-Spinning Verfahren) hergestellt wurden, untersucht worden. Der Schwerpunkt der Arbeit bestand in der Erforschung der Vorgänge während der Aktivierung und der zyklischen Hydrierung/Dehydrierung der rascherstarrten Mg-Legierungen. Zusätzlich wurde das Gefüge, das sich nach der Kristallisation, Aktivierung bzw. Hydrierung einstellt, seine Erhaltung und Auswirkung auf das H2-Speicherverhalten (Struktur-Eigenschafts-Beziehungen) untersucht. Die für die Verbesserung der Kinetik des H2-Speicherverhaltens angestrebte Nanostruktur konnte nach der Hydrierung der rascherstarrten Legierungen erreicht werden. Die REM-, TEM- sowie EFTEM (EELS)-Untersuchungen zeigten, dass ein Y-Zusatz zu Mg-basierten Legierungen zu einer sehr feinen (ca. 50 nm) und homogenen Verteilung von Y-Hydriden im Gefüge der rascherstarrten Bänder führt. Mg2Ni-Hydride bilden dagegen größere Körner im Größenbereich von 2-3 µm. Bei den Cu-haltigen Legierungen wurde eine Koexistenz von Mg2NiH4 und MgCu2 in direkter Nachbarschaft nachgewiesen. Detaillierte Untersuchungen der Wasserstoffabsorption haben gezeigt, dass die Chemisorption während des linearen Anfangsbereiches des Hydrierungsverlaufes geschwindigkeitsbestimmend ist. Nach dem linearen Hydrierungsverlauf ist die Hydrierungskinetik von der Wasserstoffdiffusion durch eine geschlossene Hydridschicht beeinflusst. Mit dem breiten Spektrum der Untersuchungen (REM, EELS, TEM, HP-TGA, DSC, in situ-Synchrotron-XRD) als auch durch gezielte Variation der Zusammensetzungen wurden neue und grundlegende Erkenntnisse zum H2-Speicherverhalten der rascherstarrten Mg-basierten Legierungssysteme gewonnen. Besondere Beachtung verdient die Mg90Ni8Y1,6SE0,4-Legierung. Durch die Möglichkeit einer einfachen Herstellung, ihre schnelle Reaktionskinetik, ihren hohen Wasserstoffgehalt (bis zu 5,6 Gew.%) und ihre gute Zyklenstabilität eignet sich diese Legierung zur sicheren, volumeneffizienten sowie leichtgewichtigen Speicherung von Wasserstoff. Damit kann Wasserstoff gespeichert, transportiert und als CO2-freier Sekundärenergieträger in stationären und mobilen Anwendungen eingesetzt werden.