Les aciers inoxydables à haute teneur en molybdène présentent une excellente résistance à la corrosion et ont été récemment utilisés dans des applications marines. L'acier inoxydable de type 254 SMO contient du molybdène (6% Mo) et des quantités plus élevées en éléments d'alliages que les aciers inoxydables plus classiques tels que 304, 316 et 316L. Alors que Anees Uddin Malik et al. montrent que l’acier 254 SMO est moins sensible à la corrosion par piqûre en eau de mer du golfe persique, Abdulsalam et al. démontrent que bien que cet acier présente une bonne résistance à la corrosion, il reste encore sensible à une corrosion caverneuse (surtout en milieu à 16% en masse d’ion chlorure ou à plus de 30°C).La première partie de ce travail traite du comportement électrochimique de l’acier inoxydable 254 SMO immergé dans l’eau de mer naturelle en laboratoire. Ainsi deux sites de la Guyane ont été choisis pour effectuer des prélèvements d’eau. Des analyses physicochimiques de ces eaux sont réalisées et montrent que l’eau du site du Port Larivot contient une quantité en ions chlorures plus importante que celle de l’eau du site du Mahury. Une colonisation par des bactéries et crustacés (balanes) a été mise en évidence, à l’aide du microscope électronique à balayage environnemental. Les mesures électrochimiques, notamment la voltammétrie cyclique a montré l’existence d’une zone de passivation et l’augmentation du courant de passivation par un facteur de 10 en présence d’un biofilm pour l’acier inoxydable immergé en eau du Mahury durant 22 jours. La deuxième partie propose une étude approfondie du comportement de l’interface complexe métal/couche passive/biofilm. Trois différents coupons d’aciers inoxydables (brut, poli et grenaillé) ont été déposés sur site (in-situ) dans un premier temps. Dans une seconde étape, nous avons réalisé des expérimentations mixtes (incubation in-situ et croissance en laboratoire). L’évolution du potentiel d’abandon de ces aciers est très proche pour l’acier brut et l’acier poli. En revanche, celui de l’acier grenaillé, de par la présence des grains d’alumine à sa surface, affiche un comportement différent. Une étude comparative des deux expérimentations montre des différences concernant les paramètres électriques de l’interface complexe métal/couche passive/biofilm. / Stainless steels with high content in molybdenum present an excellent corrosion resistance and were recently used in marine applications. The stainless steel 254 SMO contains molybdenum (6 %) and higher amounts of alloying elements than conventional stainless steels such as 304, 316 and 316L. While Anees Uddin Malik et al. show that 254 SMO steel is less likely to be susceptible to pitting corrosion in Arabian Gulf sea water, Abdulsalam et al. demonstrate that although this steel has good resistance to corrosion, it remains still susceptible to crevice corrosion (especially in environment with 16 chloride percent weight or more than 30 ° C).The first part of this work deals with the electrochemical behaviour of stainless steel 254 SMO immersed in natural seawater at laboratory. Two sites in French Guyane were chosen to take samples of seawater. Physicochemical analyses of these waters are made and show than the in Port Larivot site seawater contains a higher quantity of chloride ion than to Mahury seawater. Colonization by bacteria and crustaceans (barnacles) was highlighted, using the environmental scanning electron microscope. The electrochemical measurements, including cyclic voltammetry showed the existence of a passivation region and increasing the passivation current by a factor of 10 in the presence of biofilm on stainless steel immersed in Mahury seawater during 22 days.The second part offers a detailed study of the behaviour of the interface metal/passive film/biofilm. Three different coupons of stainless steel (crude, polished and blasted) were deposited on the site (in-situ) in the first time. In a second step, we performed experiments mixed (in-situ incubation and growth in the laboratory). The evolution of the free potential of these steels is very close for crude steel and polished steel. Conversely, the blasted steel, by the presence of alumina grains on its surface, shows a different behaviour. A comparative study of those two experiments shows differences in the electrical parameters of the interface metal/passive film/biofilm.

This thesis work has been conducted in the Handheld Laboratory at Husqvarna AB with the purpose of finding the parameters responsible for the performance of the catalytic converters used in the test rig. The catalytic converters are used in the test rig during the long term testing of the chain saws to reduce the hydrocarbon content from the exhaust before it enters into the environment.   To perform this research two approaches were carried out. One with Design of Experiment (DOE) and another using Scanning Electron Microscope (SEM) analysis. In Design of Experiments parameters that are suspected to be influencing the performance of the catalytic converter were refined. Using these parameters a test plan is made with the help of statistical analysis application Minitab and the tests were carried out in the test rig. Using SEM the effects of aging and its effect on microstructure and chemical composition on the catalyst surface was analyzed. The results from the DoE shows that the exhaust flow, collector diameter and distance to the muffler are responsible for the collection of exhaust. Distance to the muffler and collector length are the factors affecting the conversion of the exhaust. In addition to that exhaust flow is also responsible for the duration of heating coil running time.        The results from the SEM analysis shows that the operating temperature is high due to which there is thermal degradation of catalyst and there is also deactivation due to fouling. Another finding is that the flow on to the catalyst is not uniformly distributed

The theme of this diploma thesis is the design of a scanning electron microscope with a focused ion beam. Specifically, the thesis is focused on the design of the microscope covers and the adjacent workplace of the operator for Tescan Orsay Holding a.s.. Design is solved as the first proposal aimed at future innovation of the design of the entire product line.

The thesis is focused on the medium dynamics simulation in the environmental scanning electron microscope. Specifically, it researches (examines) the conical aperture location effect in the differential pumped chamber and the width of the pumping channel in this chamber. The theoretical part deals with the environmental scanning microscope generally and other tools used in this thesis, e.g. ANSYS Fluen software, fluid turbulence, medium free path of molecules and electrons scattering. In the practical part, the work is focused on data processing from the ANSYS Fluent program and on their evaluation.

First part of this thesis is a theoretical essay which deals with the basics of scanning electron microscopy, with structure and function of a scanning electron microscope, its’ special case of an various pressure scanning electron microscope, electron interaction with surrounding environment and with a scintillation detector. The applied part of the thesis is focused on evaluation of material contrast on Cu-W specimen. Material contrast is evaluated for different pressures of water vapors in the microscope specimen chamber and for different detection conditions.

The aim of my Master's thesis is the design of a scanning electron microscope. The designed concept presents an innovative approach to the problems and respects all technical, ergonomic and aesthetical demands made on it. The main creative part of design process starting from the concept development and ending up with the final solution is preceded by a background research study including a historical, technical and design analysis of the electron microscope. The conclusion of my Master's thesis analyses the final design, its character and its contribution in broader context.

Cette thèse s’ajoute aux différents travaux de recherche qui traitent des alliages d’aluminium fortement utilisés dans l’industrie aéronautique et contribue fortement à comprendre le comportement élastoplastique en chargement cyclique à contrainte imposée du 2017A. L’apport essentiel de ce travail est l’étude de l’anisotropie propre du matériau utilisé à travers le suivi de l’évolution des différents paramètres caractérisant la plasticité cyclique de notre matériau. En effet, nous avons caractérisé cette anisotropie en comparant le comportement du matériau en traction-compression avec celui de la torsion alternée selon l’évolution cyclique de la réponse contrainte-déformation, l’évolution de l’état stabilisé, l’évolution des variables d’écrouissages cinématique et isotrope ainsi que l’anisotropie selon le comportement en fatigue et endommagement. Pour mieux affiner la partie expérimentale de ce travail, des investigations microstructurales des faciès de rupture de toutes les éprouvettes utilisées ont été effectuées afin de mieux comprendre les mécanismes d’endommagement cyclique dans notre matériau. Dans la partie numérique de cette thèse, nous avons réalisé des simulations numériques en utilisant la dernière version du modèle multimécanismes qui tient compte de l’anisotropie du matériau. Les résultats de ces simulations, réalisées en considérant les mêmes conditions de nos essais expérimentaux, confirment les capacités de cette nouvelle version à estimer le comportement élastoplastique d’un matériau anisotrope. / The present work is devoted to study the anisotropic behavior of an extruded aluminum alloy under cyclic loading in axial and shear directions. In the first part, we have studied its elastoplastic behavior through the evolution of stress–strain loops, isotropic and kinematic hardening and we have associated this behavior with the evolution of its elastic adaptation (shakedown). We have studied the behavior of the material in fatigue damage using the evolution of stiffness. Microstructural investigations were performed on fractured surfaces using scanning electron microscope (SEM) in orderto understand the evolution of fatigue damage during cyclic loading. In the second part, we have simulated all the tests performed in the experimental part using the new version of multimechanisms model. The obtained results show that this version is able to take into account the anisotropic behavior of the materials under stress controlled tests.

Advanced High Strength Steel (AHSS) has become a popular steel grade among automakers to produce vehicle bodies. With improvements in strength and elongation, AHSS has evolved to its 2nd generation, including high manganese steel. Even though it has outstanding strength, the 2nd generation of AHSS faces some production problems due to its high alloying elements. With continual improvement, the 3rd generation of AHSS is currently in production. In this generation, the steel types still have a competitive strength and elongation like the 2nd generation of AHSS while having lower alloying element contents and production costs. One of the types of 3rd generation AHSS is medium manganese steel. Research related to the 2nd and 3rd generation of AHSS mainly focuses on their mechanical properties and microstructures. As there is a strong correlation between mechanical properties and inclusion characteristics, further investigation of the evolution of inclusions is still required. In this study, high-temperature experiments were conducted to investigate the effects of metal chemistry on the inclusion evolution in liquid steel. The concentrations of manganese, aluminum, and nitrogen were varied systematically. Two and three-dimensional analysis techniques were applied to study the number, composition, and size distribution of inclusions. Electrolysis extraction was used to identify the oxide, sulfide, and nitride inclusions, whereas an automated SEM with an ASPEX feature was used to detect a larger number of inclusions for better representation of the steel matrix. This work has established inclusion classification rules to distinguish nitride inclusions from oxide inclusions. To the best of the authors’ knowledge, this is the first discussion of this type of inclusion classification in the open literature. Based on the automated SEM (ASPEX Feature) analysis, the type of detected inclusions in medium and high manganese steels were Al2O3(pure), Al2O3-MnS, AlN(pure), AlN-MnS, AlON, AlON-MnS, and MnS inclusions. As the manganese content in the steel increased from 2% to 20%, the total amount of inclusions, especially AlN-contained inclusions, was raised. This phenomenon occurred due to the increase in nitrogen solubility with increased manganese content in the steel. The thermodynamic calculation also predicted that AlN inclusions would form when the steel was cooled or during the solidification. Moreover, AlN and MnS inclusions were observed to co-precipitate together. Similar to manganese, the increase in the aluminum content (Al = 0.5-6%) increased the total amount of inclusions in the steel, and the dominant inclusion type is AlN. AlN and Al2O3 inclusions can be heterogenous nucleation sites for MnS inclusions. Furthermore, Al2O3 inclusions also became heterogeneous nucleation sites for AlN inclusions. The experimental set-up was further modified to investigate the effect of nitrogen on the formation of inclusions in the medium manganese steels. The nitrogen was introduced by purging or injecting N2 gas into the steel system. Similar to the effect of manganese and aluminum, the increase in the nitrogen content also increased the total amount of inclusions. Once the nitrogen content in the steel exceeded the critical limit for the formation of AlN inclusions, AlN inclusions can be stable in the liquid steel. Moreover, regardless of the nitrogen content in the steel, AlN-MnS inclusions were formed in the slow-cooled steels. In terms of morphology, AlN inclusions can be formed of plate-like, needle, angular, agglomerate, or irregular shapes. Furthermore, a brief investigation on the addition of calcium and nitrogen to the medium manganese steels found that calcium led to the formation of other complex inclusions, such as CAx and CAS-Other inclusions. In the medium manganese steel composition in the present study, the number of CAS-Other inclusions was dominated by (Ca,Mn)S-Oxide inclusions after the addition of Ca. However, with time and after introducing N2 gas into the steel, the number of (Ca,Mn)S-Nitride inclusions also increased. The formation of (Ca,Mn)S-Nitride inclusions resulted from the co-precipitation of CaS, MnS, and AlN. The current work provides a better understanding of the formation mechanism of inclusions in medium manganese steels and high manganese steels. It presents complete information on the characteristics of inclusions, such as the number density, type, and morphology of inclusions. This knowledge can help steelmakers improve the steelmaking process to control the formation of inclusions, which can be problematic for the manufacture and performance of medium manganese steels and high manganese steels. / Dissertation / Doctor of Philosophy (PhD)

Bifilms is the oxide layer created between two surfaces in the melt of light metals that form an oxide layer. These become planar inclusions in the final casting and are problematic for the mechanical properties such as cracks and crack initiations. Bifilms are too thin to be viewed properly in two dimension cross-section method as they will only appear as thin lines. Because of this, it is relevant to test if it is possible to use electrolytic extraction (EE) as a alternative method to investigate bifilms. Both the deeply etched surface and the inclusions on a filter from the extraction are looked at in the scanning electron microscope (SEM) to get an understanding of the size and shape of the inclusions. With this, a greater understanding of these types of defects can be achieved. After both the filtered inclusions and the surface are examined in SEM with images and Energy-dispersive X-ray spectroscopy (EDS), the images are measured in the software ImageJ. The measurements and analysis show that it is probably bifilms and that they can be relatively large, and not so circular. However, the measurements with the filter have shown high levels of oxygen and carbon. Some levels of chlorine, nitrogen and iron have also been found. But if the surface is compared to the metal surface, it can be concluded that it is likely that bifilms have been found. There are sufficient levels of aluminum and oxygen present. Images in SEM also show the appearance of film-like inclusions. If the method of electrolytic extraction is to be improved to investigate bifilms,optimizations such as filters of other compositions are recommended. / Bifilms är det oxidskikt som skapas mellan två ytor i smältan hos lätta metaller som bildar ett oxidskikt. Dessa blir sedan plana inneslutningar i den slutliga gjutningen och är problematiskt för de mekaniska egenskaperna i form av sprickor och sprickinitieringar. Bifilms är för tunna för att de ska kunna ses korrekt i en tvärsnittsmetod, eftersom de bara kommer att visas som tunna linjer. På grund av detta är det relevant att testa om det är möjligt att använda elektrolytisk extraktion (EE) som en alternativ metod. Både den djupt etsade ytan och inneslutningarna på ett filter från extraktionen tittas på i svepelektronmikroskop för att få en förståelse för inneslutningarnas storlek och form. I och med det kan en högre förståelse uppnås för dessa typer av defekter. Efter att både de filtrerade inneslutningarna och ytan granskats i SEM med bilder och Energy-dispersive X-ray spectroscopy (EDS), mäts bilderna i en mjukvara, ImageJ. De mätningarna och analyserna visar att det antagligen hittats bifilms och att de kan vara förhållandevis stora, samt inte så cirkulära. Däremot har mätningarna med filtret visat höga halter av syre och kol. Även vissa halter av klor, kväve och järn har hittats. Men om ytan jämförs med metallytan så kan en slutsats dras om att det är troligt att bifilms har hittats. Där finns tillräckliga halter av aluminium och syre. Även bilder i SEM påvisar filmliknande inneslutningar till sitt utseende. Om metoden med elektrolytisk extraktion ska förbättras för att undersöka bifilms behövs optimeringar, som till exempel filterav en annan sammansättning.

Thesis deals with theoretical knowledge about scanning electron microscopy and environmental scanning electron microscopy. It describes principle of operation, signals generated by interaction between primary electron beam and specimen and means of detection of secondary electron signal in environmental conditions using scintillation detector. Furthermore, thesis focuses on optimization of detection od secondary electrons by adjusting electrode system of scintillation detector. Computer program Simion is used for modelling signal electron trajectories for proper adjustments. Simulation were starting-point for adjusting the design of the detector. Detection efficiency of adjusted detector was determined by evaluating signal magnitude from captured images, secondary electron detection capability from voltage contrast and quality of the captured images from signal/noise ratio.