This thesis dealt with thermal stability of magnesium alloy AZ91 prepared by severe plastic deformation, which leeds to fine grained structure. This structure is characterised by its inherent instability and this thesis tries to find out the value of critical temperature and rate of this instability, which manifests as grain coarsening.

The aim of this master’s thesis is electrochemical characteristics evaluation of magnesium alloys. The theoretical part describes the properties of magnesium and its alloys and their corrosion characteristics. In the experimental part are presented results of corrosion resistance measurement of two types of wrought magnesium alloys. It was AZ31 and AZ61 magnesium alloys, which were measured in Hank’s solutions with addition of ions Ca2+ and Mg2+ (SBF+) and without addition of the ions (SBF). The solution temperature during the measurement was 37 ± 1 °C. The experiments were used electrochemical impedance spectroscopy (EIS) and potentiodynamic tests using linear polarization (LP). EIS measurements were done in times of 5 minutes, 1, 2, 4, 8, 12, 24, 48, 72, 96 and 168 hours. Potentiodynamic tests were only short-term and they started after 5 minutes of stabilization. Both methods were used for measuring the electrochemical characteristics of polished and ground surface of the samples. The most important measurement results were polarization resistance, corrosion potential and corrosion current density. The electrochemical measurements are used to estimate the chemical composition influence and alloy’s structure of the corrosion resistance.

Two magnesium alloys (Mg-4Y-4Gd-2Ca and Mg-2Y-2Gd-1Ca) with high ignition tem- perature were successfully processed by extrusion. Mg-2Y-2Gd-1Ca alloy was addition- ally processed by equal channel angular pressing (ECAP) to achieve ultrafine-grained microstructure. The effect of extrusion parameters on fraction of recrystallized grains, grain size, and texture was revealed by EBSD analysis. The presence of Mg2Ca, REH2 and Mg5RE secondary phases was proven by SEM and TEM. Microstructural condition including distribution and morphology of secondary phase par- ticles directly affected the mechanical properties. Yield tensile stress exceeding 200 MPa was achieved in each condition. Large non-recrystallized grains with strong {10̄10} tex- ture resulted in a significant anisotropy in mechanical properties. Processing by ECAP led to a homogeneous microstructure with a mean grain size below 1 µm. ECAP condition showed superior mechanical properties with a low anisotropy. The developed and analysed microstructural condition resulted in favourable mechanical properties. The studied alloys are therefore promising for the application in aerospace industry. 1

In this present work, the dynamics of deformation mechanisms activated in binary magnesium-gadolinium alloys with respect to amount of Gd were investigated with in-situ experimental methods. Cast alloys are characterized by random texture. Compression test were done at room temperature with simultaneous record of acoustic emission response. The acoustic emission signal was subsequently analysed using advanced clustering method providing information about the dominant deformation mechanisms. High speed camera was used to study the dynamics of twinning, including estimation of the velocity of twin propagation with respect to Gd concentration. The deformation tests were repeated in a chamber of scanning electron microscope (in-situ SEM) with concurrent following the microstructure development using secondary electrons and electron back-scattered diffraction (EBSD) in different stages of the deformation. Main goal of this measurements was to identify active slip systems and the progress of twin volume fraction during deformation. Keywords: magnesium alloy, deformation tests, acoustic emission, high-speed camera, electron microscopy, twinning

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Indiana University-Purdue University Indianapolis (IUPUI) / In recent years, magnesium alloys, due to their high strength and biocompatibility, have attracted significant interest in medical applications, such as cardiovascular stents, orthopedic implants, and devices. To overcome the high corrosion rate of magnesium alloys, coatings have been developed on the alloy surface. Most coating methods, such as anodic oxidation, polymer coating and chemical conversion coating, cannot produce satisfactory coating to be used in human body environment. Recent studies demonstrate that micro-arc oxidation (MAO) technique can produce hard, dense, wear-resistant and well-adherent oxide coatings for light metals such as aluminum, magnesium, and titanium. Though there are many previous studies, the understanding of processing conditions on coating performance remains elusive. Moreover, previous tests were done in simulated body fluid. No test has been done in a cell culture medium, which is much closer to human body environment than simulated body fluid. In this study, the effect of MAO processing time (1 minute, 5 minutes, 15 minutes, and 20 minutes) on the electrochemical behaviors of the coating in both conventional simulated body fluid and a cell culture medium has been investigated. Additionally a new electrolyte (12 g/L Na2SiO3, 4 g/L NaF and 4 ml/L C3H8O3) has been used in the MAO coating process. Electrochemical behaviors were measured by performing potentiodynamic polarization and electrochemical impedance spectroscopy tests. In addition to the tests in simulated body fluid, the MAO-coated and uncoated samples were immersed in a cell culture medium to investigate the corrosion behaviors and compare the difference in these two kinds of media. The results show that in the immersion tests in conventional simulated body fluid, the 20-minute MAO coated sample has the best resistance to corrosion due to the largest coating thickness. In contrast, in the cell culture medium, all MAO coated samples demonstrate a similar high corrosion resistance behavior, independent of MAO processing time. This is probably due to the organic passive layers formed on the coating surfaces. Additionally, a preliminary finite element model has been developed to simulate the immersion test of magnesium alloy in simulated body fluid. Comparison between the predicted corrosion current density and experimental data is discussed.

The effect of individual additions of calcium oxide (CaO), Gd, Nd and Y was investigated on the microstructure, mechanical properties and corrosion resistance of the as-cast ZK40 alloy. The microstructural features were analised using optical, scanning and transmission electron microscopy, X-ray diffraction and Scanning Kelvin Atomic Probe Force Microscopy. The compressive and tensile behaviours of the as-cast alloys at room temperature were investigated. Electrochemical Impedance Spectroscopy, hydrogen evolution and weight loss under immersion in 0.5 wt.% NaCl solution were used to evaluate the corrosion behaviour. The results of the mechanical and corrosion tests were correlated with the microstructures. The 2 wt.% Gd addition enhanced the ductility, while the Nd addition resulted in deterioration in mechanical properties. The addition of 2 wt.% Gd and 1 wt.% Y resulted in the improvement of the ductility. The addition of CaO did not affect the mechanical properties while the 2 wt.% Nd deteriorate it. The 1 wt.% Y addition enhanced the ductility. The CaO addition did not caused enhancement in mechanical properties. The corrosion behaviour was enhanced with the addition of CaO and Gd. The modification of ZK40 with Gd opens up new perspectives in the development of Mg-Zn based alloys. / O efeito da adição individual de óxido de cálcio (CaO), Gd, Nd e Y foi investigado na microestrutura, propriedades mecânicas e resistência à corrosão de ligas ZK40 fundidas. As características microestruturais foram analisadas via microscopia óptica, microscopia eletrônica de varredura, microscopia eletrônica de transmissão, difração de Raios-X e \"Scanning Kelvin Atomic Probe Force Microscopy\". O comportamento à compressão e à tração das ligas à temperatura ambiente foi investigado. Espectroscopia eletroquímica de impedância, evolução de hidrogênio e ensaios de imersão em solução de 0.5% em peso de NaCl foram utilizados para avaliar a resistência à corrosão. Os resultados dos ensaios mecânicos e corrosão foram relacionados com a microestrutura. A adição de 2% em peso de Gd melhorou a ductilidade, ao passo que a adição de Nd resultou na piora das propriedades mecânicas. A adição de 2% em peso de Gd e 1% em peso de Y resultou na melhora da ductilidade. A adição de 1% em peso de Y causou uma melhora na ductilidade e a adição de CaO não teve impacto benéfico nas propriedades mecânicas. A resistência à corrosão foi melhorada com a adição de CaO e Gd. A modificação da liga ZK40 com a adição de Gd abre novas perspectivas no desenvolvimento de ligas Mg-Zn.

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Title: Physical properties of ultrafine-grained magnesium based alloys prepared by various severe plastic deformation techniques Author: Jitka Stráská Department / Institute: Department of Physics of Materials Supervisor of the doctoral thesis: Doc. RNDr. Miloš Janeček, CSc. Abstract: The objective of the doctoral thesis is the complex investigation of ultrafine-grained magnesium alloy AZ31 prepared by two different severe plastic deformation techniques, in particular the hot extrusion followed by equal-channel angular pressing (EX-ECAP) and high pressure torsion (HPT). These severe plastic deformation methods, and as well as many others, are described in detail in the introductory theoretical section. Experimental results are summarized in the following experimental part of the thesis. Mechanical properties, lattice defect structure and especially microstructure were investigated using various experimental techniques. Thermal stability of ultrafine-grained microstructure of AZ31 after EX-ECAP was investigated and the activation energies for grain growth in different temperature ranges were calculated using kinetic equation for grain growth and Arrhenius equation. Results from the dislocation density measurements proved temperature ranges of the recovery and the following grain growth. Results from the...