Dissertations / Theses on the topic 'In Situ X Ray Nano Tomography'
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1
Harrup, Gutierrez Anthony Albert. "Evolution des dommages lors du traitement thermomécanique de plaques épaisses d'aluminium aérospatial." Electronic Thesis or Diss., Université Grenoble Alpes, 2024. http://www.theses.fr/2024GRALI019.
Abstract:
Les alliages d'aluminium avancés utilisés dans l'industrie aérospatiale nécessitent des propriétés de haute performance telles que la ténacité à la fracture, la résistance à la fatigue et la résistance à la corrosion. L'AA2050 est un alliage d'aluminium largement utilisé pour les composants de structure interne aérospatiale en raison de ses hautes propriétés mécaniques combinées à sa faible densité. Durant le processus de fabrication, les alliages d'aluminium subissent diverses étapes thermomécaniques, telles que le laminage à chaud. En particulier, le laminage à chaud permet de fermer la porosité de ségrégation qui peut se former lors de la coulée. Explorer de nouvelles fenêtres de processus pour ce procédé peut conduire à des conditions extrêmes où le comportement des pores n'est pas bien connu. L'objectif principal de ce travail est de comprendre comment les pores peuvent germer et croître sous des déformations à chaud en traction représentatives de ces conditions de laminage à chaud extrêmes.Dans ce travail, nous avons étudié la germination et la croissance des pores sous différentes conditions thermomécaniques dans l'AA2050 pour imiter les dommages lors du laminage à chaud de plaques épaisses. La partie centrale de cette étude a consisté à utiliser la tomographie aux rayons X multi-échelles réalisée au European Synchrotron Radiation Facility (ESRF). La méthodologie consistait à effectuer une nano-tomographie synchrotron aux rayons X in situ lors de tests de traction micrométriques à haute température et une micro-tomographie synchrotron aux rayons X ex situ de Tests de Traction Secondaires. Des analyses SEM et EBSD ont également été effectuées sur des échantillons de traction micrométriques post-mortem.Avec la nano-tomographie aux rayons X, nous avons observé la germination et l'évolution des pores à trois températures différentes (400°C, 440°C et 480°C). Les pores ont été segmentés et mesurés en termes de volume et de morphologie, ainsi que les intermétalliques et les précipités les entourant. Avec cela, une classification des pores en fonction de leur lieu de germination est proposée.En utilisant des algorithmes de Corrélation de Volume Numérique (DVC), nous avons suivi l'évolution de centaines de pores individuels pour déterminer leur croissance en lien avec la déformation locale à l'intérieur des échantillons. En couplant l'évolution des pores et les données de contrainte locale avec des simulations de Méthode des Éléments Finis de tests de traction à haute température, nous avons déterminé le champ de contrainte local et comparé nos résultats expérimentaux avec cinq modèles existants d'évolution des vides. Les prédictions des modèles sont discutées.Pour relier le comportement du matériau et l'évolution de la porosité à une échelle plus grande, nous avons mené des Tests de Traction Secondaires ex situ. En utilisant le logiciel DVC PT4D, nous avons extrait le champ de déformation des images 3D obtenues, corroborant le comportement du matériau à différentes températures. Cette étude améliore non seulement notre compréhension du comportement de l'AA2050 dans des conditions extrêmes, mais fournit également des informations précieuses sur la formation de défauts dans les processus thermomécaniques avancésAdvanced aluminium alloys used in the aerospace industry require high performance properties such as fracture toughness, fatigue resistance, and corrosion resistance. AA2050 is an aluminium alloy widely used for aerospace internal structure components because of its high mechanical properties combined with its low density. During the manufacturing process of aluminium alloys undergo various thermomechanical steps, such as hot rolling. In particular, hot-rolling enables to close the segregation porosity that may form during casting. Exploring new process windows for this process may lead to extreme conditions where pore behaviour is not well known. The main objective of this work is to understand how pores may nucleate and grow under hot tensile deformations representative of these extreme hot rolling conditions.In this work, we studied pore nucleation and growth under different thermo-mechanical conditions in AA2050 to mimic damage during hot rolling of thick plates. The central part of this study involved multi-scale X-ray tomography performed at the European Synchrotron Radiation Facility (ESRF). The methodology consisted in performing in situ synchrotron X-ray nano-tomography during high-temperature micrometric tensile tests and ex situ synchrotron X-ray micro-tomography of Secondary Tensile Tests. SEM and EBSD analysis were also performed on post-mortem micrometric tensile specimens.With X-ray nano-tomography, we observed the nucleation and evolution of pores at three different temperatures (400°C, 440°C, and 480°C). The pores were segmented and measured in terms of volume and morphology, along with the intermetallics and precipitates surrounding them. With this, a classification of the pores depending on their nucleation location is proposed.Using Digital Volume Correlation (DVC) algorithms, we tracked the evolution of hundreds of individual pores, learning about their growth behaviour and measuring local strain within the specimens. By coupling pore evolution and local strain data with Finite Element Method simulations of high-temperature tensile tests, we determined the local stress field and compared our experimental results with five existing void evolution models. Model predictions are discussed.To link material behaviour and porosity evolution on a larger scale, we conducted ex situ Secondary Tensile Tests. Using the DVC software PT4D, we extracted the strain field from the obtained 3D images, corroborating the material's behaviour at different temperatures. This study not only enhances our understanding of AA2050's behaviour under extreme conditions but also provides valuable insights into defect formation in advanced thermo-mechanical processes
2
Acito, Vito. "In situ X-ray computed tomography for soft contact mechanics." Electronic Thesis or Diss., Ecully, Ecole centrale de Lyon, 2023. http://www.theses.fr/2023ECDL0054.
Abstract:
L'aire de contact réelle AR entre deux solides en contact est une quantité fondamentale qui contrôle le comportement de frottement d'une interface de contact. Bien que la plupart des techniques expérimentales visant à mesurer cette quantité soient basées sur le contraste optique entre les régions en contact et hors contact, ces méthodes sont limitées par la transparence optique requise par au moins l'un des deux corps en contact. En outre, ces techniques ne permettent d'accéder qu'à l'interface de contact sans fournir d'informations sur d'autres quantités physiques importantes telles que la déformation globale ou les phénomènes hors contact à la surface. À partir de quelques travaux pionniers, nous proposons la tomographie à rayons X (XRCT) in-situ comme méthode alternative pour surmonter ces limites et accéder à la morphologie complète du contact en 3D avec des paires de contacts potentiellement non transparentes. Dans toutes les études précédentes, les analyses ont été effectuées sur des surfaces complexes sans se concentrer sur des examens préliminaires des limites de la XRCT (comme l'estimation des erreurs dans la mesure de AR). Dans ce cadre, nous avons proposé l'utilisation d'un système modèle composé d'une sphère lisse en élastomère (PDMS) et d'une plaque rigide lisse (en PMMA) pour simplifier le problème et souligner les avantages et les inconvénients de cette méthode expérimentale. Nous nous sommes d'abord concentré sur la mesure in-situ de l'évolution de AR au cours d'un essai de compression et de cisaillement réalisé sur notre système modèle. Les résultats ont été comparés à ceux d'un dispositif opto-mécanique 2D déjà maîtrisé. Enfin, à partir de la reconstruction en 3D in-operando du contact modéle indenté cisaillé, nous avons pu extraire les champ de déplacement, déformation et contraintes dans le contact par corrélation numérique des volumes (DVC) en utilisant comme marqueurs des particules préalablement dispersés dans le PDMS. Tous ces résultats ont été mis en regard des prédictions théoriques de modèles de la littératureThe real contact area AR between two solids in contact is a fundamental quantity that controls the frictional behavior of a contact interface. Although most experimental techniques aimed at measuring this quantity are based on the optical contrast between in-contact and out-of-contact regions, these methods are limited by the optical transparency required for least one of the two contacting bodies. Furthermore, these techniques only provide access to the contact interface without providing information on other important physical quantities such as the global deformation or the out-of-contact phenomena at the surface. Building on some pioneering work, we propose in-situ X-ray tomography (XRCT) as an alternative method to overcome these limitations and access the full 3D contact morphology with potentially non-transparent contact pairs. In all previous studies, analyzes were performed on complex surfaces without focusing on preliminary examinations of the limitations of XRCT (such as estimating errors in measuring AR). In this context, we proposed the use of a model system composed of a smooth elastomer sphere (PDMS) and a smooth rigid plate (PMMA) to simplify the problem and highlight the advantages and disadvantages of this experimental method. We first focused on measuring in-situ the evolution of AR during a compression and shear test carried out on our model system. The results were compared to those of a 2D opto-mechanical device already mastered. Finally, from the in-operando 3D reconstruction of the indented and sheared contact , we were able to extract the displacement, deformation and stress fields in the contact by digital correlation of volumes (DVC) using as markers particles previously dispersed in PDMS. All these results were compared to theoretical predictions from models in the literature
3
Ando, Edward. "Experimental investigation of microstructural changes in deforming granular media using x-ray tomography." Thesis, Grenoble, 2013. http://www.theses.fr/2013GRENI097/document.
Abstract:
Cette thèse présente un travail expérimental dans le domaine de la mécanique des milieux granulaires.Ce travail introduit une nouveauté fondamentale: durant la déformation d’échantillonsde sable en compression triaxiale classique, leur micro-structure est enregistrée par tomographieà rayons-x en environ 15 étapes de déformation différentes.Afin que tous les grains d’un échantillon soient individuellement visibles dans les imagesde tomographie, les échantillons sont considérablement réduits pour qu’ils mesurent 11 mm endiamètre et 22 mm en hauteur. Cela permet d’identifier et d’individualiser tous les plus decinquante mille grains d’un échantillon.Dans ce travail expérimental, une série d’essais triaxiaux a été réalisée sur trois sables naturels(le sable d’Hostun, le sable d’Ottawa et des Caicos ooids, tous à partir des états initiauxrelativement denses), à deux valeurs de pression de confinement différents (100 et 300 kPa).Dans les images 3D résultantes de la reconstruction des acquisitions tomographiques réaliséesau cours de chaque essai, les grains sont identifiés dans chaque état en utilisant un algorithmede type watershed (ligne de partage des eaux) classique. À partir de ces données discrétisées,des techniques ont été mises au point pour caractériser les contacts grain-à-grain mais aussipour mesurer la cinématique de tous les grains identifiés entre les états pour lesquels des imagestridimensionnelles existent. La cinématique des grains est mesurée avec deux outils spécialementdéveloppés: “ID-Track” suit les grains et donne leurs déplacements; cette information est ensuitenécessaire pour une technique hybride de corrélation d’images discrète pour mesurer la rotationde chaque grain.Des mesures à l’échelle du grain sont présentées en détail pour un essai, et sont ensuitecomparées à des essais dans des conditions différentes. L’objectif est de mettre en évidence lesmicro-mécanismes responsables des différents comportements macroscopiques observés pour cesmatériaux. Cette comparaison met en évidence certains micro-mécanismes importants tels que,par exemple, la déformation d’un échantillon. Celle-ci est concentrée dans une bande de cisaillementbien développée qui correspond à une bande de grains avec des rotations intenses. Dans unéchantillon de grains arrondis, cette bande – définie par des grains – est très nette. Par contre,avec des grains anguleux, les rotations des grains dans la bande “polluent” les grains voisins;leur forme facilite l’engrenage entre grains, qui limite aussi les grosses rotations individuelles desgrains. Cette différence de mécanisme de déformation est utilisée pour expliquer la différencedans la contrainte résiduelle observée à macro-échelle. Des signes de déformation localisée sontsystématiquement observés en train de se produire avant le pic de déformation des échantillons etdes systèmes complexes de chaînes de rotations de grains (qui correspondent aussi à une mesurelocale de déformation calculée avec les déplacements des grains) sont remarquées autour du picde la réponse macroscopique de chaque échantillonThis doctoral thesis presents an experimental investigation into the mechanics of granular media.The novelty that this work brings is that the specimens of sand tested in this work are systematicallyand non-destructively imaged using x-ray tomography. Sample size is considerably reducedfrom standard (specimens measure approximately 22 mm height by 11 mm diameter), allowingentire specimens to be scanned at a sufficiently high resolution to identify all the grains (morethan fifty thousand) in each specimen.A campaign of triaxial compression tests has been run on a series of three different naturalsands with different grain shapes (Hostun sand, Ottawa sand and Caicos ooids – all prepared atrelatively dense initial states), and tested at 100 or 300 kPa cell pressure. In each test around 15x-ray scans are performed. In the 3D images resulting from the reconstruction of the x-ray scansperformed, grains are identified each state using a standard watershed algorithm. Starting fromthese discretised data, techniques are developed in order characterise grain-to-grain contacts,as well as to measure the kinematics of all the identified grains between imaged states. Grainkinematics are measured with two specifically-developed tools: “ID-Track” to track grains yieldingtheir displacements, and a discrete image correlation technique to measure grain rotations.Grain-scale measurements are reported in detail for one test, and are then compared to testsin different conditions, in order to highlight the micro-mechanisms responsible for the observedmacroscopic behaviour. This comparison highlights some important micro-scale mechanisms suchas the increasing rotational frustration of more angular grains when the sample’s deformation isconcentrated in a fully developed shear band; this is used to explain to some extent the highervalue of their residual stress for these materials. Signs of localised deformation are seen to occurwell before the peak in many samples, and complex patterns of rotating grains (which match alocal, grain-based measurement of strain) are noticed around the peak of each sample’s response
4
Ren, Wenyuan. "In-situ X-ray computed tomography characterisation and mesoscale image based fracture modelling of concrete." Thesis, University of Manchester, 2015. https://www.research.manchester.ac.uk/portal/en/theses/insitu-xray-computed-tomography-characterisation-and-mesoscale-image-based-fracture-modelling-of-concrete(3307ca0b-b492-4bfc-91f7-61c092b21707).html.
Abstract:
This study develops a 3D meso-scale fracture characterisation and modelling framework for better understanding of the failure mechanisms in concrete, by combining in-situ micro-scale X-ray computed tomography (XCT) experiments and XCT image-based finite element (FE) simulations. Firstly, sophisticated in-situ XCT experiments are conducted on concrete cubes under Brazilian-like, uniaxial and cyclic compression. Proper procedures for XCT image reconstruction and multi-phasic segmentation are identified. The fracture evolution at different loading stages is characterised and visualised as well as the detailed distributions of aggregates and voids. The Young's moduli of aggregate and cement are obtained by micro-indentation tests and used in XCT-image based asymptotic homogenisation simulations to calculate effective elastic constants of concrete cubes. The XCT technique proves very powerful in characterising and visualising the complicated 3D fracture evolution in concrete. The material properties and the segmented 3D images from the experiments are then used for FE fracture simulations with realistic aggregates, cement and voids. Image-based mesh generation algorithms are developed for 2D in a MATLAB code and identified for 3D in Simpleware. Cohesive interface elements are embedded within cement and aggregate-cement interfaces to simulate the complex nonlinear fracture. Extensive simulations of 40mm and 20mm cubes under compression and tension are carried out. Good agreements are achieved between the load-displacement curves and final crack patterns from the simulations and those from the compressive in-situ XCT tests. The XCT image-based modelling proves very promising in elucidating fundamental mechanisms of complicated crack initiation and propagation in concrete.
5
Lalechos, Antonios V. "Evaluation of X-ray CT tomography as a means for investigating in-situ electrical contact interfaces." Thesis, University of Southampton, 2010. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.536365.
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Qsymah, Ansam. "In-situ X-ray computed tomography tests and numerical modelling of ultra high performance fibre reinforced concrete." Thesis, University of Manchester, 2016. https://www.research.manchester.ac.uk/portal/en/theses/insitu-xray-computed-tomography-tests-and-numerical-modelling-of-ultra-high-performance-fibre-reinforced-concrete(7c27ef36-afc8-4ea7-8c72-7d92eba924f9).html.
Abstract:
Ultra high performance fibre reinforced concrete (UHPFRC) is a relatively new fibre reinforced cementitious composite and has become very popular in construction applications. Extensive experimental studies have been conducted, demonstrating its superior properties such as much higher strength, ductility and durability than conventional fibre reinforced concrete (FRC) and high performance concrete. However, the material's damage and fracture mechanisms at meso/micro scales are not well understood, limiting its wider applications considerably. This study aims at an in-depth understanding of the damage and fracture mechanisms of UHPFRC, combining microscale in-situ X-ray computed tomography (µXCT) experiments and mesoscale image-based numerical modelling. Firstly, in-situ µXCT tests of small-sized UHPFRC specimens under wedge splitting loading were carried out, probably for the first time in the world, using an in-house designed loading rig. With a voxel resolution of 16.9µm, the complicated fracture mechanisms are clearly visualised and characterised using both 2D images and 3D volumes at progressive loading stages, such as initiating of micro-cracks, arresting of cracks by fibres, bending and pulling out of fibres and spalling of mortar at the exit points of inclined fibres. Secondly, based on the statistics of pores in the µXCT images obtained for a 20mm cube specimen, an efficient two-scale analytical-numerical homogenisation method was developed to predict the effective elastic properties of the UHPFRC. The large number of small pores were first homogenised at microscale with sand and cement paste, using elastic moduli from micro-indentation tests. 3D mesoscale finite element models were built at the second scale by direct conversion of the µXCT images, with fibres and large pores were faithfully represented. The effects of the volume fraction and the orientation of steel fibres on the elastic modulus were investigated, indicating that this method can be used to optimise the material micro-structure. Thirdly, 3D mesoscale finite element models were built for the specimen used in the in-situ µXCT wedge splitting test, with embedded fibre elements directly converted from the µXCT images. The fracture behaviour in the mortar was simulated by the damage plasticity model available in ABAQUS. Finally, 2D mesoscale finite element models were developed to simulate the fracture behaviour of UHPFRC using cohesive interface elements to simulate cracks in the mortar, and randomly distributed two-noded 1D fibres and connector elements to simulate the pull-out behaviour of fibres. This approach offers a link between the fibres pull-out behaviour and the response of the whole composite at the macroscale, thus it can be used to conduct parametric studies to optimise the material properties.
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Wheatland, Jonathan Antony Thomas. "Characterising the multi-scale properties of flocculated sediment by X-ray and focused ion beam nano-tomography." Thesis, Queen Mary, University of London, 2017. http://qmro.qmul.ac.uk/xmlui/handle/123456789/25984.
Abstract:
The hydrodynamic behaviour of fine suspended aqueous sediments, and stability of the bedforms they create once settled, are governed by the physical properties (e.g., size, shape, porosity and density) of the flocculated particles in suspension (flocs). Consequently, accurate prediction of the transport and fate of sediments and of the nutrients and pollutants they carry depends on our ability to characterise aqueous flocs. Current research primarily focuses on characterising flocs based on their external gross-scale (>1 μm) properties (e.g., gross morphology, size and settling velocity) using in situ techniques such as photography and videography. Whilst these techniques provide valuable information regarding the outward behaviour of flocculated sediment (i.e. transport and settling), difficulties associated with extracting 3D geometries from 2D projections raises concerns regarding their accuracy and key parameters such as density can only be estimated. In addition, they neglect to inform on the internal micro- and nano-scale structure of flocs, responsible for much of their behaviour and development. Transmission electron microscope (TEM) and environmental electron microscope may be used to obtain nano-scale information in, essentially, 2D but there is a large scale gap between this information and the macro-scale of optical techniques. To address this issue this study uses 3D tomographic imaging over a range of spatial scales. Whilst commonly used in materials science and the life sciences, correlative tomography has yet to be applied in the environmental sciences. Threading together 3D Xray micro-computed tomography (X-ray μCT) and focused ion beam nano-tomography (FIBnt) with 2D TEM makes material characterisation from the centimetre to nanometre-scale possible. Here, this correlative imaging strategy is combined with a non-destructive stabilisation procedure and applied to the investigation of flocculated estuarine sediment, enabling the multi length-scale properties of flocs to be accurately described for the first time. This work has demonstrated that delicate aqueous flocs can be successfully stabilised via a resin embedding process and contrasted for both electron microscopy and X-ray tomography imaging. The 3D information obtained can be correlated across all length-scales from nm to mm revealing new information about the structure and morphology of flocs. A new system of characterising floc structure can be defined based on the association of particles and their stability in the structure rather than simply their size. This new model refutes the postulate that floc structures are fractal in nature.
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Costin, Marius. "Multiresolution Image Reconstruction in X-ray Micro- and Nano- Computed Tomography : Application in Materials Non-Destructive Testing." Lyon, INSA, 2010. http://theses.insa-lyon.fr/publication/2010ISAL0034/these.pdf.
Abstract:
Dans le cadre d'une large coopération internationale, le projet Saphir a comme but principal la production sure, intégrée et contrôlée de produits nano-structurés multifonctionnels. Dans ce contexte, notre contribution consiste à développer une méthode d'imagerie tridimensionnelle pour inspecter et caractériser les échantillons et les pièces fournis par les partenaires du projet. La tomographie par rayonnement X a été choisie car elle constitue une technique adaptée au contrôle non-destructif. Mais pour des échantillons très complexes présentant des détails sur plusieurs ordres de grandeur, les scanners commerciaux ne répondent pas à tous les besoins et une méthode adaptée a du être développée. Cette thèse établit une base théorique et expérimentale pour une méthode originale capable de produire des images multi-résolution et que nous avons nommé ASDIR (Approximate Single Detail Image Reconstruction). Dans une configuration de type « zoom-in », deux jeux de données sont acquis et fusionnés. La reconstruction de ces données combinées est basée sur l'algorithme standard de rétroprojection filtrée (FBP), mais notre méthode est une extension qui implémente une accélération par l'utilisation de la théorie des ondelettes. Deux versions préliminaires sont également présentées : elles produisent des résultats moins satisfaisants et ont servi de base pour la version finale. Une période importante a été consacrée aux expériences ainsi qu'à l'étude et la compréhension des phénomènes physiques intervenant en CT. Des corrections pour les plus importantes sources d'artefacts ont été mises en oeuvre et leur efficacité a été démontré e grâce à la qualité des images obtenues. Nous avons validé notre approche sur des données simulées et expérimentales. Nous avons généré des données simulées avec des fantômes que nous avons spécialement conçus pour évaluer différentes caractéristiques de la méthode et des échantillons. Les données expérimentales ont été acquises avec deux dispositifs différents, un microtomographe et un nanotomographe, et sur des échantillons de tailles différentes. Une étude de métrologie a été menée sur les images produites et des informations sur la porosité des échantillons ont pu être extraitesIn a large international cooperation, the Saphir project aims at producing in a safe, integrated and controlled way, multifunctional nanostructured products. Within this framework, our contribution is the development of a method for three dimensional inspection and characterization of samples and parts produced by the partners. As a starting point, the X-ray computed tomography (CT) was chosen as the most appropriate non-destructive technique. But because the samples are very complex, with features over more orders of magnitude, the available commercial devices could not solve all the requirements and an adapted method for the image reconstruction needed to be developed. This thesis puts a theoretical and an experimental basis for an original method that we abbreviated ASDIR (Approximate Single Detail Image Reconstruction), capable of producing multiresolution images. In a zoom in CT setup, two sets of projections are acquired and combined. The reconstruction is based on the standard filtered backprojection (FBP) algorithm, but we extended it by implementing an acceleration technique that uses a wavelet processing of the data. Two preliminary variants are also presented, which turned out to produce unsatisfactory results, but they were the basis for the final version. We validated our approach on both simulated and experimental data. We generated numerical data with phantoms that we designed specially to assess different features of the method and of the samples. The experimental data was acquired with two different devices, a micro-tomograph and a nano-tomograph, with samples of different sizes. The images that we produced were subject to a basic analysis and we are confident that more information can be extracted from a detailed study
9
Cai, Biao. "In situ synchrotron tomographic quantification of semi-solid properties of aluminum-copper alloys." Thesis, University of Manchester, 2015. https://www.research.manchester.ac.uk/portal/en/theses/in-situ-synchrotron-tomographic-quantification-of-semisolid-properties-of-aluminumcopper-alloys(60c222d0-7e70-4a1e-9ed4-75b8f559d5de).html.
Abstract:
Semi-solid deformation mechanisms are important in a range of manufacturing and natural phenomena, which range from squeeze casting to magma flows. In this thesis, using high speed synchrotron X-ray tomography and a bespoke precision thermo-mechanical rig, a four dimensional (3D plus time) quantitative investigation was performed to study the mechanical / rheological behavior of semi-solid Al-Cu alloys. Various deformation techniques, namely, isothermal semi-solid compression, extrusion and indentation were used. The time-resolved dynamic 3D images were analyzed with the help of novel image quantification techniques including digital volume correlation and image-based simulations of fluid flow. The quantified dynamics at a microstructural scale was then linked with macroscopic mechanical properties. The qualitative and quantitative analyses revealed a range of important semi-solid micromechanical mechanisms including the occurrence and effects of dilatancy, associated liquid flow through the equiaxed microstructure, intra-dendritic deformation, and strain localization during semi-solid deformation, not only shedding new insights into the mechanisms of deformation-induced solidification defect formation (solute segregation, porosity and hot tearing) of semi-solid alloys at both a macroscopic and microscopic level, but also providing benchmark cases for semi-solid deformation models and theories. The experimental methodology, techniques and analysis procedures developed in this thesis are generic in nature and can be applied to a wide range of research fields.
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Weber, Loriane. "Iterative tomographic X-Ray phase reconstruction." Thesis, Lyon, 2016. http://www.theses.fr/2016LYSEI085/document.
Abstract:
L’imagerie par contraste de phase suscite un intérêt croissant dans le domaine biomédical, puisqu’il offre un contraste amélioré par rapport à l’imagerie d’atténuation conventionnelle. En effet, le décalage en phase induit par les tissus mous, dans la gamme d’énergie utilisée en imagerie, est environ mille fois plus important que leur atténuation. Le contraste de phase peut être obtenu, entre autres, en laissant un faisceau de rayons X cohérent se propager librement après avoir traversé un échantillon. Dans ce cas, les signaux obtenus peuvent être modélisés par la diffraction de Fresnel. Le défi de l’imagerie de phase quantitative est de retrouver l’atténuation et l’information de phase de l’objet observé, à partir des motifs diffractés enregistrés à une ou plusieurs distances. Ces deux quantités d’atténuation et de phase, sont entremêlées de manière non-linéaire dans le signal acquis. Dans ces travaux, nous considérons les développements et les applications de la micro- et nanotomographie de phase. D’abord, nous nous sommes intéressés à la reconstruction quantitative de biomatériaux à partir d’une acquisition multi-distance. L’estimation de la phase a été effectuée via une approche mixte, basée sur la linéarisation du modèle de contraste. Elle a été suivie d’une étape de reconstruction tomographique. Nous avons automatisé le processus de reconstruction de phase, permettant ainsi l’analyse d’un grand nombre d’échantillons. Cette méthode a été utilisée pour étudier l’influence de différentes cellules osseuses sur la croissance de l’os. Ensuite, des échantillons d’os humains ont été observés en nanotomographie de phase. Nous avons montré le potentiel d’une telle technique sur l’observation et l’analyse du réseau lacuno-canaliculaire de l’os. Nous avons appliqué des outils existants pour caractériser de manière plus approfondie la minéralisation et les l’orientation des fibres de collagènes de certains échantillons. L’estimation de phase, est, néanmoins, un problème inverse mal posé. Il n’existe pas de méthode de reconstruction générale. Les méthodes existantes sont soit sensibles au bruit basse fréquence, soit exigent des conditions strictes sur l’objet observé. Ainsi, nous considérons le problème inverse joint, qui combine l’estimation de phase et la reconstruction tomographique en une seule étape. Nous avons proposé des algorithmes itératifs innovants qui couplent ces deux étapes dans une seule boucle régularisée. Nous avons considéré un modèle de contraste linéarisé, couplé à un algorithme algébrique de reconstruction tomographique. Ces algorithmes sont testés sur des données simuléesPhase contrast imaging has been of growing interest in the biomedical field, since it provides an enhanced contrast compared to attenuation-based imaging. Actually, the phase shift of the incoming X-ray beam induced by an object can be up to three orders of magnitude higher than its attenuation, particularly for soft tissues in the imaging energy range. Phase contrast can be, among others existing techniques, achieved by letting a coherent X-ray beam freely propagate after the sample. In this case, the obtained and recorded signals can be modeled as Fresnel diffraction patterns. The challenge of quantitative phase imaging is to retrieve, from these diffraction patterns, both the attenuation and the phase information of the imaged object, quantities that are non-linearly entangled in the recorded signal. In this work we consider developments and applications of X-ray phase micro and nano-CT. First, we investigated the reconstruction of seeded bone scaffolds using sed multiple distance phase acquisitions. Phase retrieval is here performed using the mixed approach, based on a linearization of the contrast model, and followed by filtered-back projection. We implemented an automatic version of the phase reconstruction process, to allow for the reconstruction of large sets of samples. The method was applied to bone scaffold data in order to study the influence of different bone cells cultures on bone formation. Then, human bone samples were imaged using phase nano-CT, and the potential of phase nano-imaging to analyze the morphology of the lacuno-canalicular network is shown. We applied existing tools to further characterize the mineralization and the collagen orientation of these samples. Phase retrieval, however, is an ill-posed inverse problem. A general reconstruction method does not exist. Existing methods are either sensitive to low frequency noise, or put stringent requirements on the imaged object. Therefore, we considered the joint inverse problem of combining both phase retrieval and tomographic reconstruction. We proposed an innovative algorithm for this problem, which combines phase retrieval and tomographic reconstruction into a single iterative regularized loop, where a linear phase contrast model is coupled with an algebraic tomographic reconstruction algorithm. This algorithm is applied to numerical simulated data
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Lauraux, Florian. "Etudes nano-mécaniques in situ de nanostructures métalliques utilisant le rayonnement synchrotron." Electronic Thesis or Diss., Aix-Marseille, 2020. http://www.theses.fr/2020AIXM0441.
Abstract:
Dans cette thèse, le comportement nano-mécanique d’ilots d'Au sub-micrométriques est étudié par nano-indentation in-situ en utilisant le microscope à force atomique SFINX en combinaison avec la microdiffraction de Laue et l’imagerie par diffraction cohérente des rayons X en condition de Bragg (BCDI). Ces études de couplage des rayons X à la nano-indentation ont été menés sur des lignes synchrotron, les lignes ID01 et BM32 à l'ESRF (Grenoble). De nouvelles méthodes ont été développées dans le cadre de cette thèse : une nouvelle technique de mesure de la force appliquée in situ qui repose sur le mesure de la déflexion de la poutre AFM en silicium par microdiffraction de Laue fournissant une résolution de force de 90 nN. Une technique d'imagerie par diffraction cohérente des rayons X en condition de Bragg à plusieurs longueurs d'ondes (Multi Wavelength BCDI) qui permet un BCDI in situ réel pendant les tests nano-mécaniques. Les tests mécaniques couplés à la micro diffraction de Laue ont permis de déterminer la densité de dislocation dans un cristal d'or en fonction de la force appliquée mettant en évidence un recuit mécanique par la baisse de la densité des dislocations géométriquement nécessaires (GND). La technique de MW-BCDI a été utilisée lors de l'indentation in situ d'un mono cristal d'Au et a permis de visualiser en 3D l'évolution des dislocations. Elle a aussi montré la disparition des dislocations après un déchargement complet, laissant derrière elle un cristal d'or sans défaut. Ces expériences de couplage in situ permettent d'apporter de nouveaux éléments de réponse concernant la nucléation des premiers défauts dans des nano-structures métalliques CFCThe nano-mecanic behavior of Au sub-micronic islands has been studied by in situ nano-indentation using the atomic force microscope SFINX coupled with the Laue X ray microdiffraction and the Bragg coherent diffraction imaging (BCDI°techniques. These coupled studies have been led on synchrotron beamlines, ID01 and BM32 at the ESRF (France Grenoble). New methods have been developped during this PHD work : a mesure of the in situ applied force by measuring the deflexion of the AFM Si cantilever by Laue microdiffraction with a resolution of 90 nm. A brand new multi-wavelength BCDI approach allowing real in situ nano-mecanical tests coupled with X ray diffraction. The mecanical tests coupled with Laue microdiffraction led to the determination of defaults density in a Au nanocristal function of the applied force, which demonstrated a mecanical annealing by the drop of the GNDs. The mw-BCDI has also be coupled with nanoindentation tests on a Au nano-cristal, which allowed us to visualize in 3D the evolution and the nucleation of dislocations. It also showed the disapearing of the dislocations after a full unloading, leaving the nano-cristal with no defaults. These in situ coupled experiments will shed some new light about the nucleation of the first defaults in metalic FCC nanostructures
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AGASHE, NIKHIL R. "IN-SITU SMALL ANGLE X-RAY SCATTERING STUDIES OF CONTINUOUS NANO-PARTICLE SYNTHESIS IN PREMIXED AND DIFFUSION FLAMES." University of Cincinnati / OhioLINK, 2004. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1092055991.
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Jonsson, Åsa, and Grim Skarsgård. "Synchrotron tomography of pressboard during in-situ compression loading : Construction of compression rig, image acquisition procedure and methods for image processing." Thesis, Uppsala universitet, Tillämpad mekanik, 2015. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-257276.
Abstract:
Pressboard, a high density cellulose-based material used for insulation in high voltage power transformers, exhibits stress relaxation during compressive loading. Investigating the micro-mechanical mechanisms responsible for the relaxation can lead to modifications of the production process to control the behaviour of the material. This investigation can be done using Synchrotron X-ray micro Computed Tomography which provides sufficient temporal and spatial resolutions to capture the stress relaxation process. In the present thesis, a compression rig for in-situ mechanical loading during X-ray micro Computed Tomography was designed and constructed. Local tomography scans with sub-micrometre resolution were obtained at the TOMCAT beamline at the Swiss Light Source, Paul Scherrer Institut, Switzerland. Several fibre segmentation techniques are analysed, together with Optical Flow and Digital Volume Correlation (DVC), methods used for estimating displacement, strain and velocity vector fields. Suitability of the tested methods is evaluated, and it is found that segmentation of individual fibres in a cellulose material of such a high density is probably not possible using currently available segmentation techniques. The movements during relaxation are measurable at the used resolution, and can be estimated using Optical Flow. Further work into correction of image shift due to rig movement between scans, as well as image artefact reduction should allow for measurement and comparisons of displacement during relaxation as well as DVC-computed strain measurements during compression, recreating earlier results.
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Sencu, Razvan. "Multiscale stochastic fracture mechanics of composites informed by in-situ X-ray CT tests." Thesis, University of Manchester, 2017. https://www.research.manchester.ac.uk/portal/en/theses/multiscale-stochastic-fracture-mechanics-of-composites-informed-by-insitu-xray-ct-tests(85a0be40-9e7a-4df3-a366-69ac6ce02e35).html.
Abstract:
This thesis presents the development of a new multiscale stochastic fracture mechanics modelling framework informed by in-situ X-ray Computed Tomography (X-ray CT) tests, which can be used to enhance the quality of new designs and prognosis practices for fibre reinforced composites. To reduce the empiricism and conservatism of existing methods, this PhD research systematically has tackled several challenging tasks including: (i) extension of the cohesive interface crack model to multi-phase composites in both 2D and 3D, (ii) development of a new in-house loading rig to support in-situ X-ray CT tests, (iii) reconstruction of low phase-contrast X-ray CT datasets of carbon fibre composites, (iv) integration of X-ray CT image-based models into detailed crack propagation FE modelling and (v) validation of a partially informed multiscale stochastic modelling method by direct comparison with in-situ X-ray CT tensile test results.
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Li, Zhen [Verfasser], Andreas [Gutachter] Magerl, and Jürgen [Gutachter] Ristein. "In-Situ X-ray Study of Nano SiO_x with Germanium Doping in Czochralski Silicon / Zhen Li ; Gutachter: Andreas Magerl, Jürgen Ristein." Erlangen : Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), 2017. http://d-nb.info/1144619238/34.
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Kalasová, Dominika. "Rentgenová počítačová nano tomografie polymerních strukturovaných bio materiálu." Doctoral thesis, Vysoké učení technické v Brně. CEITEC VUT, 2019. http://www.nusl.cz/ntk/nusl-409089.
Abstract:
Tato práce se zaměřuje na pokročilou zobrazovací technologii, rentgenovou počítačovou tomografii (CT). Tato nedestruktivní technika je využívána pro výzkum různých biomateiálů ve tkáňovém inženýrství a materiálové vědě obecně (skafoldy, polymery, keramické materiály, kompozity aj.). Vizualizace a kvantifikace ve 3D jsou výhodné v rámci multidisciplinárního přístupu, který je často v těchto odvětvích uplatňován. Záměr této práce lze rozdělit do dvou oblastí. Prvním tématem je optimalizace měřicí procedury různých měkkých materiálů pomocí CT s laboratorními rentgenovými zdroji. To zahrnuje převážně zobrazování ve fázovém kontrastu, konkrétně metodu volného šíření záření (VŠZ). Tato práce teoreticky popisuje VŠZ a demonstruje tento jev na řadě experimentů. Následné nezbytné zpracování dat získaných VŠZ je implementováno a vyhodnoceno na základě míry zlepšení obrazových dat. Druhé téma ukazuje konkrétní aplikace CT v materiálovém inženýrství. Několik studií s různými CT zařízeními ukazuje příklady možných aplikací a obrazového zpracování. Příklady korelace CT dat s jinými doplňkovými technikami ukazují, jak může být CT aplikována v multioborovém přístupu ke komplexnímu řešení vědeckých problémů.
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Yu, Boliang. "3D analysis of bone ultra structure from phase nano-CT imaging." Thesis, Lyon, 2019. http://www.theses.fr/2019LYSEI016/document.
Abstract:
L'objectif de cette thèse était de quantifier le réseau lacuno-canaliculaire du tissu osseux à partir d’images 3D acquises en nano CT synchrotron de phase. Ceci a nécessité d’optimiser les processus d’acquisition et de reconstruction de phase, ainsi que de développer des méthodes efficaces de traitement d'images pour la segmentation et l’analyse 3D. Dans un premier temps, nous avons étudié et évalué différents algorithmes de reconstruction de phase. Nous avons étendu la méthode de Paganin pour plusieurs distances de propagation et l’avons évaluée et comparée à d’autres méthodes, théoriquement puis sur nos données expérimentales Nous avons développé une chaine d’analyse, incluant la segmentation des images et prenant en compte les gros volumes de données à traiter. Pour la segmentation des lacunes, nous avons choisi des méthodes telles que le filtre médian, le seuillage par hystérésis et l'analyse par composantes connexes. La segmentation des canalicules repose sur une méthode de croissance de région après rehaussement des structures tubulaires. Nous avons calculé des paramètres de porosité, des descripteurs morphologiques des lacunes ainsi que des nombres de canalicules par lacune. Par ailleurs, nous avons introduit des notions de paramètres locaux calculés dans le voisinage des lacunes. Nous avons obtenu des résultats sur des images acquises à différentes tailles de voxel (120nm, 50nm, 30nm) et avons également pu étudier l’impact de la taille de voxel sur les résultats. Finalement ces méthodes ont été utilisées pour analyser un ensemble de 27 échantillons acquis à 100 nm dans le cadre du projet ANR MULTIPS. Nous avons pu réaliser une analyse statistique pour étudier les différences liées au sexe et à l'âge. Nos travaux apportent de nouvelles données quantitatives sur le tissu osseux qui devraient contribuer à la recherche sur les mécanismes de fragilité osseuse en relation avec des maladies comme l’ostéoporoseOsteoporosis is a bone fragility disease resulting in abnormalities in bone mass and density. In order to prevent osteoporotic fractures, it is important to have a better understanding of the processes involved in fracture at various scales. As the most abundant bone cells, osteocytes may act as orchestrators of bone remodeling which regulate the activities of both osteoclasts and osteoblasts. The osteocyte system is deeply embedded inside the bone matrix and also called lacuno-canalicular network (LCN). Although several imaging techniques have recently been proposed, the 3D observation and analysis of the LCN at high spatial resolution is still challenging. The aim of this work was to investigate and analyze the LCN in human cortical bone in three dimensions with an isotropic spatial resolution using magnified X-ray phase nano-CT. We performed image acquisition at different voxel sizes of 120 nm, 100 nm, 50 nm and 30 nm in the beamlines ID16A and ID16B of the European Synchrotron Radiation Facility (ESRF - European Synchrotron Radiation Facility - Grenoble). Our first study concerned phase retrieval, which is the first step of data processing and consists in solving a non-linear inverse problem. We proposed an extension of Paganin’s method suited to multi-distance acquisitions, which has been used to retrieve phase maps in our experiments. The method was compared theoretically and experimentally to the contrast transfer function (CTF) approach for homogeneous object. The analysis of the 3D reconstructed images requires first to segment the LCN, including both the segmentation of lacunae and of canaliculi. We developed a workflow based on median filter, hysteresis thresholding and morphology filters to segment lacunae. Concerning the segmentation of canaliculi, we made use of the vesselness enhancement to improve the visibility of line structures, the variational region growing to extract canaliculi and connected components analysis to remove residual noise. For the quantitative assessment of the LCN, we calculated morphological descriptors based on an automatic and efficient 3D analysis method developed in our group. For the lacunae, we calculated some parameters like the number of lacunae, the bone volume, the total volume of all lacunae, the lacunar volume density, the average lacunae volume, the average lacunae surface, the average length, width and depth of lacunae. For the canaliculi, we first computed the total volume of all the canaliculi and canalicular volume density. Moreover, we counted the number of canaliculi at different distances from the surface of each lacuna by an automatic method, which could be used to evaluate the ramification of canaliculi. We reported the statistical results obtained on the different groups and at different spatial resolutions, providing unique information about the organization of the LCN in human bone in three dimensions
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Liu, Yuanyuan. "Inkjet printed drops and three-dimensional ceramic structures." Thesis, University of Manchester, 2017. https://www.research.manchester.ac.uk/portal/en/theses/inkjet-printed-drops-and-threedimensional-ceramic-structures(36785d3d-cca6-4903-8e5b-043fd2198e0f).html.
Abstract:
Inkjet printing is a versatile manufacturing method with applications beyond its traditional application in graphics and text printing, particularly in structural and functional materials. This thesis aims to enhance the understanding of DOD inkjet printing processes by investigating the behaviour of solvent mixtures and nanoparticle suspensions to identify the key parameters affecting drop ejection, drying and stacking processes. Drop ejection and flight were investigated with two modes of inkjet printheads, using a range of fluids formulated from solvent mixtures and characterised by the dimensionless Z number. The printable range was found to be 1.17 smaller or equal to Z smaller or equal to 36.76 for a 10 pl (21.5 micro metre diameter) shear-mode Dimatix printhead. However, with an 80 micro metre diameter squeeze-mode MicroFab printhead, the range was found to be narrower with 4.02 smaller or equal to Z smaller or equal to 16.2. However, both printheads were found to show a printable range of Weber number with 0.4 <We <20. Weber number is determined by the drop velocity and hence the actuating pulse. When designing inks for future printing work, not only the fluid properties, but also the pulse voltages need to be considered. The drop stacking and solidification processes of drops containing nano ZrO2 particles were investigated to enhance the understanding of drop drying and drop/drop interactions. In-situ synchrotron X-ray radiography provides a promising method to track the time-evolved solid segregation within printed drops during drying. Both the initial contact angle and substrate temperature during printing strongly influence the drying process and the final dried deposit shape. The drops were first pinned and then there was a slight sliding of the three-phase contact line. Drops were deformed by the stacking of overprinted drops when printed on Kapton tapes and silicon wafer surfaces, but not on glass slides due to the small contact angle of water on glass slides. Crack-like defects were found at the edge of the final dried stacking structures. The coffee stain effects within a single inkjet printed droplet and the 3D structures before and after sintering were investigated to find out the influence of ink properties, printing parameters and substrate temperature on inkjet printed structures. It was found coffee staining was more obvious at high substrate temperatures. When adding 25 vol% ethylene glycol (EG) or 5 wt% polyethylene glycol (PEG), the coffee stain effect is reduced or eliminated under room temperature drying. X-ray tomography has been demonstrated as a valuable tool for the characterization of 3D printed objects and defects that form during their manufacture. Defects were characterised as microvoids or large-scale crack-like defects. The majority of the microvoids revealed are associated with mechanisms and processes within a single drop, e.g. segregation during dryings such as the formation of coffee stains or coffee rings. The size or distribution of microvoids can be controlled by changing the ink formulation, with higher PEG content inks showing lower concentrations of microvoids.
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Stockmar, Marco Kurt Verfasser], Franz [Akademischer Betreuer] Pfeiffer, Pierre [Akademischer Betreuer] Thibault, and Reinhard [Akademischer Betreuer] [Kienberger. "Ptychographic phase retrieval for the near-field regime with applications in x-ray nano-tomography / Marco Kurt Stockmar. Betreuer: Franz Pfeiffer. Gutachter: Pierre Thibault ; Reinhard Kienberger ; Franz Pfeiffer." München : Universitätsbibliothek der TU München, 2015. http://d-nb.info/1095766244/34.
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Chen, Yang. "Damage mechanisms in SiC/SiC composite tubes : three-dimensional analysis coupling tomography imaging and numerical simulation." Thesis, Paris Est, 2017. http://www.theses.fr/2017PESC1056/document.
Abstract:
Du fait de leurs propriétés physiques et chimiques exceptionnelles à haute température par rapport aux métaux, les composites de carbure de silicium (SiC) sont étudiés comme éventuel matériau de gainage du combustible nucléaire dans les réacteurs de fusion ou fission avancée futurs, ainsi que, depuis plus récemment, dans les réacteurs à eau légère existants. Les tubes composites SiC/SiC tressés en 2D, fabriqués par procédé d'infiltration chimique en phase vapeur (CVI), présentent un comportement mécanique anisotrope, faiblement déformable (~ 1%). La maîtrise des relations entre la microstructure, l’endommagement et le comportement macroscopique est essentielle pour optimiser précisément le dimensionnement structurel de ce matériau pour les applications envisagées. Un paramètre de fabrication important est l'angle de tressage, angle entre les torons de fibres et l'axe du tube. L'objectif de ce travail est de fournir une compréhension détaillée de la relation endommagement-microstructure, en particulier des effets de l'angle de tressage sur les mécanismes d’endommagement. Dans ce but, une étude combinant observations expérimentales à macro et micro-échelle et simulations numériques est menée. Les tubes composites sont d’abord étudiés par des essais de traction in situ sous tomographie par rayons X. Les expériences ont été réalisées sur la ligne PSICHE du synchrotron SOLEIL sous faisceau rose polychromatique. Les images tridimensionnelles sont analysées par la technique de corrélation d’image volumique (DVC), complétée par une série d'algorithmes de traitement d'image originaux, développés spécifiquement pour analyser les microstructures 3D, mesurer les déformations à travers l'épaisseur du tube, détecter et caractériser quantitativement le réseau de microfissures créées par le chargement mécanique. De plus, les microstructures réelles, décrites par les images de haute résolution issues des tests in situ, sont utilisées dans les simulations numériques multi-échelle. Les champs de contrainte à l’échelle microstructurale sont calculés en régime élastique par une technique utilisant la transformée de Fourier rapide (FFT). Ils permettent de mieux comprendre l'initiation des fissures et d’interpréter les observations expérimentales par une comparaison directe. Ces approches expérimentales et numériques sont appliquées à trois tubes présentant différents angles de tressage (30 °, 45 ° et 60 °). L’influence de l'angle de tressage sur l'initiation et l'évolution de l’endommagement à cœur des composites est ainsi mise en évidenceBecause of their outstanding physical and chemical properties at high temperature, in comparison with metals, silicon carbide (SiC) composite materials are studied as possible nuclear fuel cladding materials either for future advanced fission/fusion reactors, or more recently, for the currently existing light water reactors. 2D-braided SiC/SiC composite tubes, manufactured by chemical vapor infiltration (CVI), exhibit an anisotropic, hardly deformable (~1%) mechanical behavior. Understanding the relations between the microstructure, the damage mechanisms and the macroscopic behavior is essential to optimize the structural design of this material for the considered applications. One important manufacturing parameter is the braiding angle, i.e. the angle between the fiber tows and the tube axis. The objective of this work is to provide a comprehensive understanding of the damage-microstructure relations, in particular of the effects of the braiding angle on the damage mechanisms. For this purpose, an investigation combining experimental observations at macro and micro-scale and numerical simulations is developed. The composite tubes are first studied through in situ tensile testing under X-ray computed tomography. Experiments were carried out on the PSICHE beamline at synchrotron SOLEIL using a pink polychromatic beam. The recorded 3D images are processed using the digital volume correlation (DVC) technique, extended by a series of advanced image processing algorithms specifically developed in order to analyze the 3D microstructures, to measure the deformations through the tube thickness, and to detect and quantitatively characterize the network of micro-cracks created by the mechanical loading. In addition, numerical simulations are performed on the real microstructures as observed in the high-resolution images recorded during the in situ tests. Stress fields are calculated at the microstructural scale in the elastic regime using a numerical tool based on the Fast Fourier Transform (FFT). They help to better understand crack initiation and interpret the experimental observations within one-to-one comparisons. Both the experimental and numerical approaches are applied to three tubes with different braiding angles (30°, 45° and 60°). The effect of the braiding angle on the initiation and evolution of damage in the bulk of the composite materials can thus be highlighted
21
Engelberg, Dirk Lars. "Grain boundary engineering for intergranular stress corrosion resistance in austenitic stainless steel." Thesis, University of Manchester, 2006. http://www.manchester.ac.uk/escholar/uk-ac-man-scw:207805.
Abstract:
Austenitic stainless steels are frequently used for engineering applications in aggressive environments. Typical sources of component failures are associated with localized attack at grain boundaries, such as intergranular corrosion and stress corrosion cracking. To prevent premature failures, structural integrity assessments are carried out, with the aim of predicting the maximum likelihood of cracking that may develop. For accurate predictions it is of great importance to know the interaction of parameters involved in life-determining processes. This PhD thesis investigates the effect of microstructure and stress on intergranular stress corrosion cracking in Type 302 / Type 304 austenitic stainless steels. High-resolution X-ray tomography has been successfully applied to examine, for the first time in 3-dimensions, in-situ, the interaction between microstructure and crack propagation. The development and subsequent failure of crack bridging ligaments has been observed and correlated with regions of ductile tearing persistent on the fracture surface. These ductile regions were consistent with the morphology of low-energy, twin-type grain boundaries, and are believed to possess the capability of shielding the crack tip. Following this observation, a new grain bridging model has been developed, in order to quantify the effect of static stress and crack bridging on the maximum likely crack length. The model was compared and evaluated with in the literature available percolation-like models. Intergranular stress corrosion tests in tetrathionate solutions have been designed and carried out to validate the new model. The assessment comprised,(i) a thorough examination of the microstructure and analysis parameters employed,(ii) the determination of the degree of sensitisation with subsequent crack path investigations,(iii) the identification of a suitable test system with associated grain boundary susceptibility criteria,(iv) the application of Grain Boundary Engineering (GBE) for microstructure control,(v) statistical crack length assessments of calibrated IGSCC test specimens. The results of these tests showed that the new model successfully predicts the magnitude of stress and the effect of grain boundary engineering on the maximum crack lengths.
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Wilke, Robin Niklas [Verfasser], Tim [Akademischer Betreuer] Salditt, and Claus [Akademischer Betreuer] Ropers. "Coherent X-Ray Diffractive Imaging on the Single-Cell-Level of Microbial Samples: : Ptychography, Tomography, Nano-Diffraction and Waveguide-Imaging / Robin Niklas Wilke. Gutachter: Tim Salditt ; Claus Ropers. Betreuer: Tim Salditt." Göttingen : Niedersächsische Staats- und Universitätsbibliothek Göttingen, 2014. http://d-nb.info/1064148360/34.
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Lemarié, Quentin. "Développement et caractérisation in situ d'électrodes positives pour batteries Lithium/soufre." Thesis, Lyon, 2020. http://www.theses.fr/2020LYSEI041.
Abstract:
La technologie Li-ion, bien que dominant le marché actuel des batteries, souffre du prix élevé et de la toxicité de certains de ses matériaux et peine à atteindre les objectifs de performances notamment fixés pour leur utilisation dans les véhicules électriques et hybrides. Face à ces limitations, la technologie lithium/soufre (Li/S) se pose en candidat prometteur pour remplacer à moyen terme la technologie Li-ion. Basée sur un matériau actif abondant et peu cher, le soufre, elle permettrait d’atteindre des densités d’énergie pratiques deux à trois fois supérieures à celles des batteries Li-ion actuelles. Cependant, les réactions électrochimiques du système Li/S impliquent une dissolution/déposition de la matière active, engendrant d’importantes variations morphologiques et la perte de matière active à l’électrode positive qui ont un impact majeur sur la capacité et la tenue au cyclage des batteries Li/S. Ainsi, une bonne compréhension de ces mécanismes de dégradation est nécessaire afin de développer de nouveaux matériaux d’électrode innovants et permettant une optimisation des performances du système Li/S. À ce titre, l’objectif premier de cette thèse était d’appliquer des techniques de caractérisation in situ novatrices permettant de relier les propriétés mécaniques et les variations morphologiques des différents matériaux d’électrode utilisés à leur comportement électrochimique. Pour ce faire, trois techniques ont été employées : l’émission acoustique, la tomographie RX et la dilatométrie. Les conclusions tirées des observations effectuées à l’aide de ces outils de caractérisation ont permis d’axer la conception d’électrodes sur l’utilisation d’un liant innovant de type polyélectrolyte. Au cours de ces travaux, nous avons notamment pu démontrer une relation entre l’activité acoustique mesurée au cours des premiers cycles de charge/décharge de différentes formulations d’électrode à leurs propriétés mécaniques. Ensuite, le couplage de la tomographie et de la diffraction RX synchrotron in situ a permis de mettre en évidence de nouveaux phénomènes liés à la dissolution et la déposition du soufre lors du 1er cycle. Enfin, la combinaison de l’étude de la variation d’épaisseur des électrodes par dilatométrie, du suivi de l’activité acoustique et d’observations tomographiques a permis d’attester des propriétés mécaniques améliorées du liant polyélectrolyte. Additionnées à ses propriétés de régulation de la diffusion des espèces soufrées, ces conclusions renforcent l’intérêt certain de ce type de liants pour les électrodes positives des batteries Li/SEven though the Li-ion technology is dominating nowadays battery market, it is suffering from the high cost and toxicity of some of its materials as well as struggling to reach the performance goals set by always more demanding hybrid and electric vehicles. Facing the need for a new battery generation, the lithium/sulfur (Li/S) technology stands as a promising candidate for a medium term industrialization and commercialization. Based on an abundant and low-cost active material, elemental sulfur, it enables practical energy densities two to three times higher than current Li-ion batteries. However, the intermediate electrochemical reactions of this system imply many dissolutions/depositions of the active material, causing important morphological variations at the positive electrode which have a major impact on the capacity and cycling performance of the batteries. Hence a better comprehension of those degradation mechanisms is required in order to develop new and innovating electrode materials enabling an optimization of the performance of the system. Therefore, the first goal of the thesis was to employ innovative in situ characterization techniques in order to develop tools allowing to link the properties of the different electrode materials to the performance of the batteries. To do so, three techniques were used: acoustic emission, X-ray tomography and dilatometry. Then, the conclusions drawn from the observations made from the characterization tools enabled us to focus the conception of the electrodes on using a new binder based on a polyelectrolyte material. In this work, we were in particular able to demonstrate a relationship between the measured acoustic activity during the first charge/discharge cycles of different electrode formulations to their mechanical properties. Then, coupling in situ X-ray tomography and diffraction enabled us to shed light on new phenomena linked to the dissolution and deposition of sulfur during the 1st cycle. Finally, the combination of the study of thickness variation via dilatometry, of the monitoring of the acoustic activity and of tomographic observations was the key to prove the better mechanical properties of the polyelectrolyte binder. Together with its properties of regulation of the sulfur species, our conclusions strengthen the certain interest in the family of materials as a binder of positive electrodes for Li/S batteries
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Messager, Alexandre. "Étude de l'amorçage et de la propagation de fissures de fatigue internes courtes en régime gigacyclique dans un alliage d'aluminium de fonderie." Thesis, Paris, HESAM, 2020. http://www.theses.fr/2020HESAE032.
Abstract:
Le procédé de fonderie permet de produire en grande série des pièces à géométrie complexe à faible coût. Cependant, les défauts inhérents à ce procédé de fabrication (soufflures, retassures, etc.) sont des sites privilégiés d’amorçage de fissures de fatigue. La position d'un défaut par rapport à la surface de la pièce influe sur sa nocivité et sur la résistance en fatigue du composant. Les connaissances actuelles sur les mécanismes d'amorçage et de propagation de fissures de fatigue internes sont bien moins développées que celles sur les fissures amorcées à partir de défauts de surface. L’objectif de ce travail est donc de caractériser les mécanismes et cinétiques d’amorçage et de propagation de fissures de fatigue internes courtes dans l’alliage d'aluminium moulé A357-T6. Pour cela, un dispositif expérimental permettant d’observer l’amorçage et la propagation de fissures de fatigue internes par tomographie synchrotron in-situ et thermographie infrarouge a été développé. Les données de tomographie ont permis de quantifier les cinétiques de propagation de fissures internes. Les étendues des facteurs d’intensité des contraintes ont été calculées par éléments finis le long des fronts de fissure en supposant le matériau homogène. Par ailleurs, La microstructure des éprouvettes a été caractérisée par tomographie à contraste de diffraction (DCT) ce qui a permis de réaliser des calculs sur agrégats polycristallins afin de mieux comprendre les interactions entre fissures et microstructure. Enfin, grâce à des simulations thermomécaniques par éléments finis, les élévations de température en surface des éprouvettes, mesurées par thermographie infrarouge, ont pu être corrélées aux évolutions 3D des fronts de fissure observées par tomographieCasting allows the mass production of parts with complex geometry at a low cost. However, defectsinherent to the manufacturing process (pores, shrinkages, etc.) are natural stress concentrators and act as amajor cause of fatigue crack initiation. The defect position from the part surface influences its harmfulnessand the fatigue strength of the component. Initiation and propagation mechanisms of internal fatiguecracks are currently less studied than those emanating from surface defects. The purpose of this work is tocharacterize short internal fatigue crack initiation and propagation mechanisms and kinetics in the A357-T6 cast aluminium alloy. An experimental testing device allowing the observation of internal fatigue crackinitiation and propagation by in-situ synchrotron tomography and infrared thermography was developed.The propagation kinetics of internal cracks were quantif ied through tomographic data processing. Stressintensity factor ranges were calculated by f inite element analysis along the crack fronts assuminghomogeneous material. In addition, the microstructure of the specimens was characterized by diffractioncontrast tomography (DCT) which allowed polycrystalline aggregates simulation in order to betterunderstand the interactions between cracks and microstructure. Finally, thanks to f inite elementthermomechanical simulations, the surface temperature increases of the specimens, measured by infraredthermography, were correlated to the 3D evolution of the crack fronts observed by tomography
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Pushkareva, Marina. "Study of Void Growth in Commercially Pure Titanium." Thesis, Université d'Ottawa / University of Ottawa, 2017. http://hdl.handle.net/10393/35667.
Abstract:
The ductile fracture process, which consists of the nucleation, growth and coalescence of microvoids, was extensively studied for materials deforming homogeneously. For materials with a non-homogeneous deformation behavior, such as those having hexagonal closed packed (HCP) crystal structure, experimental and numerical data is lacking. Therefore, the fracture properties of materials with such HCP structure, like titanium (used in aerospace and biomedical applications), zirconium (nuclear industry) and magnesium (manufacturing industry) are not well understood. The main research objective of this Ph.D. thesis is to better understand the mechanisms governing fracture in commercially pure (CP) titanium. In particular, the effect of grain orientation on void growth is investigated. The fracture process of CP titanium was visualized in model materials containing artificial holes. These model materials were fabricated using a femtosecond laser coupled with a diffusion bonding technique to obtain voids in the interior of titanium samples. Diffusion bonding was carried out either above or below the phase transformation temperature resulting in different microstructures. Changes in void dimensions during in-situ straining were recorded in three dimensions using x-ray computed tomography. Void growth obtained experimentally was compared with the Rice and Tracey model which predicted well the average void growth. However, a large scatter in void growth was observed experimentally and was explained in terms of differences in grain orientation which was confirmed by crystal plasticity simulations. It was also shown that grain orientation has a stronger effect on void growth than intervoid spacing and material strength. Intervoid spacing, however, appears to control whether the intervoid ligament failure is ductile or brittle. While this study showed a good agreement between experiments and simulations on average, there is no direct void growth comparison for particular grain orientations. In a follow-up study, an experimental approach was developed to directly relate the growth of a void to its underlying grain orientation. This is achieved by first annealing CP titanium samples below the α-β phase transformation temperature, then performing electron backscatter diffraction iii (EBSD) and finally diffusion bonding the samples together. Samples were then tested in x-ray tomography. This study showed the importance of the local state of strain on void growth. Crystal plasticity simulations that take into account the particular grain orientation and the local state of strain were found to predict well experimental void growth. Crystal plasticity simulations confirmed that the orientation of the voidcontaining grain is more important than the orientation of surrounding grains and more important than the volume fraction of voids, in order to determine void growth. This thesis on the growth and coalescence of voids is important to validate and improve the predictions of ductile fracture models and to design new materials with improved fracture properties.
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Hallouard, François. "Formulation de nano-particules iodées comme agents de contraste a longue rémanence vasculaire pour tomodensitométrie." Thesis, Lyon 1, 2012. http://www.theses.fr/2012LYO10307.
Abstract:
L’objectif de cette thèse est de réaliser un agent de contraste vasculaire pour tomodensitométrie utilisable en préclinique. En collaboration avec le laboratoire de biogalénique de Strasbourg, ce travail a permis d’obtenir des nano-émulsions iodées produites par diffusion spontanée de surfactif et des nanoparticules iodées produites par ”émulsion - diffusion de solvant”, comme agent de contraste vasculaire. Ces émulsions et particules polymériques présentent en effet, un temps de rémanence vasculaire de plusieurs heures, un pouvoir contrastant suffisant pour un usage en tomodensitométrie (compris entre 170 et 400 HU), la possibilité de les administrer par intraveineuse et une stabilité de plusieurs mois. Les nano-émulsions, notamment celles produites à partir de Lipiodol®, sont les plus prometteuses comme agents de contraste vasculaire de par leur forte radiopacité (475 ± 30 HU) et leur rémanence vasculaire (T1/2 of 4.1 ± 1.10 h). Les nanoparticules iodées à base de PCL présentent un pouvoir contrastant inférieur (168 ± 13 HU) mais elles sont connus pour leur capacité à modifier la libération du principe actif encapsulé. De ce fait même si les agents de contraste de nature lipidique ou ceux inorganiques sont plus performant, elles restent intéressantes pour une visualisation rapide de la distribution du principe actif dans l’organisme. Cette thèse par ailleurs, apporte plusieurs éléments pour la compréhension de la formulation des nano-émulsions obtenues par diffusion spontanée de surfactif et celle des nanoparticules produites par ”émulsion - diffusion de solvant”. Concernant les nano-émulsions, l’influence de l’iodation des huiles et du surfactif a été étudiée autant sur le plan pharmacotechnique que ceux toxicologique et pharmacocinétique. Concernant les nanoparticules à base de PCL, nous avons montré que l’impact du type d’huile et de l’iodation, des polymères PCL et PCL-mPEG et de diverses méthodes de concentration sur la formulationThe aim of this thesis is to formulate a blood pool contrast agent for preclinical X-ray imaging application. In collaboration with the galenic laboratory of Strasbourg, this work has allowed to obtain iodinated nano-emulsions produced by spontaneous diffusion of surfactant and nano-particles produced by iodine ”emulsion - solvent diffusion” as blood pool contrast agent. These emulsions and polymer particles present indeed a vascular persistence of several hours, a sufficient contrast to be use in computed tomography (between 170 and 400 HU), the ability to be administered intravenous and stability of several months. Nano-emulsions, including those produced from Lipiodol®, are the most promising as blood pool contrast media by their high radiopacity (475 ± 30 HU) and vascular persistence (T1/2 of 4.1 ± 1.10 h). Iodinated nano-particles of PCL have a lower X-ray attenuation (168 ± 13 HU), but they are known for their control release of the encapsulated substances. Therefore even if inorganic or lipidic contrast agents show a better contrast, they remain attractive for rapid visualization of the co-encapsulated substance distribution in the body. This thesis also introduced several features for understanding the formulation of nano-emulsions obtained by spontaneous diffusion of surfactant and the nano-particles produced by ”emulsion - solvent diffusion.”
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Guillou, Raphaëlle. "Étude in-situ des propriétés mécaniques de films minces d'or nanostructurés déposés sur substrats flexibles lors d'essais de traction biaxiale contrôlée sous rayonnement synchrotron." Thesis, Poitiers, 2015. http://www.theses.fr/2015POIT2271/document.
Abstract:
Ce travail de thèse propose d'étudier les effets de taille et de microstructure sur les propriétés mécaniques de films minces d'or nanostructurés déposés sur des substrats flexibles lors d'essais de traction bi-axiale. Les couches minces d'or sont déposées sur du polyimide par pulvérisation ionique, technique qui permet de contrôler la taille des grains selon la direction de croissance dans les films minces en contrôlant l'épaisseur de ces derniers. Nous avons ensuite réalisé des expériences de déformation in-situ sur ces couches minces grâce à la machine de traction bi-axiale installée sur la ligne de lumière DiffAbs du synchrotron SOLEIL, source de rayons X intense qui permet de mesurer par diffraction les déformations dans les films minces polycristallins. La première étape de ce travail a été d'effectuer des expériences de traction bi-axiale pour des chargements dits « pas à pas » en imposant différents ratios de force sur deux séries de couches minces d’or d'épaisseurs différentes afin d'étudier la limite d'élasticité en fonction du chemin de chargement choisi et de tracer une surface de charge pour les deux séries d'échantillons d'or étudiés. La deuxième étape de ce travail a consisté à valider un mode de chargement dit « continu » en comparant les propriétés mécaniques d'une même série d'échantillons d'or obtenus avec ces deux types de chargements : « pas à pas » et « continu ». Une fois validé, nous avons réalisé des expériences de traction bi-axiale sur différentes séries d'échantillons d'or possédant différentes tailles grains et architecture afin de mettre en évidence un effet de taille sur les propriétés mécaniques de films minces nanométriquesThe main purpose of this thesis is to study the size and microstructure effects on the mechanical response of gold nanostructured thin films deposited on flexible substrates during biaxial tensile tests. Gold thin films are deposited onto polyimide substrates by sequenced ion sputtering technique in order to control the grain size in the growth direction. We have carried out in situ deformation experiments using the biaxial tensile device installed on the diffractometer of the DiffAbs beamline at synchrotron SOLEIL (Saint-Aubin, France), an intense X-rays source which allows to determine applied strains in polycrystalline thin films thanks to x-ray diffraction measurements. In a first step, we performed tensile biaxial tests for different load ratio using “step by step” procedure on two series of gold thin films showing different thicknesses in order to study the mechanical response analyzing the yield surface that can be extracted with the biaxial device. In a second step, we validated a continuous loading procedure which allows gaining a factor of 10 in the time frame. Validation is made by comparing the mechanical properties of two series of gold thin films investigated using “step by step” loading and “continuous” loading. After validation of the continuous loading procedure, tensile biaxial tests have been performed on different series of gold thin films with different grain size and architecture in order to put in highlight a size effect on the mechanical behavior of nanolayered thin films
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Kožiol, Martin. "Návrh vhodného etalonu délky pro nano-CT měřicí přístroj." Master's thesis, Vysoké učení technické v Brně. Fakulta strojního inženýrství, 2020. http://www.nusl.cz/ntk/nusl-417542.
Abstract:
The diploma thesis deals with the design of three length standards, which will serve to ensure metrological traceability between Rigaku nano3DX, SIOS NMM-1, Zeiss UPMC Carat 850 and other devices located at ÚVSSR BUT and CEITEC Brno. The first part of the thesis focuses on the theoretical acquaintance with concepts closely related to the issue of ensuring metrological traceability. In addition, this section deals with computed tomography and the description of individual devices. The second part of the thesis is devoted to design, production process and testing of individual standards. The last part describes the ensuring the calibration of the smallest standard, the so-called Nano standard and the calculation of the uncertainty of measuring its calibrated length. At the end of the thesis, the outputs of these activities are evaluated.
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Arif, Muhamad Fatikul. "Mécanismes d’endommagement du polyamide-66 renforcé par des fibres de verre courtes, soumis à un chargement monotone et en fatigue : Influence de l’humidité relative et de la microstructure induite par le moulage par injection." Thesis, Paris, ENSAM, 2014. http://www.theses.fr/2014ENAM0008/document.
Abstract:
Le présent travail s'appuie sur une approche expérimentale étendue visant l'identification des mécanismes d'endommagement en chargement quasi-statique et en fatigue du PA66/GF30, en prenant notamment en compte l'influence de la teneur en eau et de la microstructure induite par le moulage par injection. Les essais et les observations in situ au MEB mettent en exergue le rôle déterminant de l'humidité relative sur l'initiation, le niveau et la chronologie de l'endommagement. Une analyse par micro-tomographie aux rayons X sur des échantillons ayant subi un chargement de fatigue montre que l'endommagement augmente continuellement et progressivement au cours de la fatigue, et plus significativement dans la deuxième moitié de sa durée de vie. Les résultats obtenus en quasi-statique et en fatigue révèlent des mécanismes d'endommagement similaires, notamment une décohésion des interfaces fibre/matrice. Une chronologie générale de l'endommagement est établie. Celui-ci s'initie en extrémités de fibres ou plus globalement là où les fibres sont relativement proches les unes des autres. Il s'ensuit des décohésions interfaciales se propageant le long des fibres. A une contrainte en flexion plus élevée, des microfissures de la matrice peuvent apparaître et se propager par coalescence, ce qui aboutira à la rupture. Ces résultats expérimentaux permettent d'alimenter une modélisation multi-échelles de l'endommagement à fort contenu physique. Celle-ci contribuera alors à une prédiction pertinente de l'endommagement dans les thermoplastiques renforcés pour application automobileThe current work focuses on extensive experimental approaches to identify quasi-static and fatigue damage behavior of PA66/GF30 considering various effects such as relative humidity and injection process induced microstructure. By using in situ SEM tests, it was observed that relative humidity conditions strongly impact the damage mechanisms in terms of their initiation, level and chronology. The X-ray micro-tomography analysis on fatigue loaded samples demonstrated that the damage continuously increases during fatigue loading, but the evolution occurs more significantly in the second half of the fatigue life. From the results of damage investigation under quasi-static and fatigue loading, it was established that both loading types exhibit the same damage mechanisms, with fiber/matrix interfacial debonding as the principal damage mechanisms. General damage chronologies were proposed as the damage initiates at fiber ends and more generally at locations where fibers are relatively close to each other due to the generation of local stress concentrations. Afterwards, interfacial decohesions further propagate along the fiber/matrix interface. At high relative flexural stress, matrix microcracks can develop and propagate, leading to the damage accumulation and then the final failure. The experimental findings are important to provide a physically based damage mechanisms scenarios that can be integrated into multiscale damage models. These models will contribute towards reliable predictions of damage in reinforced thermoplastics for lightweight automotive applications
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Wang, Long. "Etude de l’influence de la microstructure sur les mécanismes d’endommagement dans des alliages Al-Si de fonderie par des analyses in-situ 2D et 3D." Thesis, Ecole centrale de Lille, 2015. http://www.theses.fr/2015ECLI0004/document.
Abstract:
Un protocole expérimental a été développé dans cette thèse pour étudier l'influence de la microstructure héritée du procédé de fonderie dit Procédé à Modèle Perdu sur le comportement en fatigue oligocyclique des alliages Al-Si à température ambiante. Dans un premier temps, la microstructure des alliages étudiés a été caractérisée à la fois en 2D et en 3D. Les éprouvettes les plus appropriées et les plus représentatives et les régions d’intérêt où le suivi in-situ est réalisé (ROIs) ont été sélectionnées par une caractérisation préliminaire en tomographie aux rayons X. Cette caractérisation 3D est également nécessaire pour comprendre les mécanismes d’endommagement après rupture de l’éprouvette. Les observations in-situ réalisées en surface en utilisant un microscope longue distance (Questar) et en volume avec la tomographie aux rayons X permettent de suivre l’amorçage et la propagation des fissures et ainsi d'identifier la relation entre les mécanismes d’endommagement et les microstructures moulées. Les champs de déplacement et de déformation en 2D/3D mesurés à l'aide de la Corrélation d'Images Numériques et la Corrélation d’Images Volumiques permettent d'analyser la relation entre les champs mesurés et les mécanismes d'endommagement. L'analyse post-mortem et la simulation éléments finis ont permis de compléter l’analyse des mécanismes d’endommagement. Les grands pores favorisent l'amorçage de fissures car ils augmentent fortement le niveau de contrainte locale. Les inclusions dures (phase Si, intermétalliques au fer et phases au cuivre) jouent un rôle important dans l’amorçage et la propagation des fissures en raison des localisations de déformation sur ces inclusionsAn experimental protocol was developed in this thesis in order to study the influence of casting microstructure on the fatigue behavior in Lost Foam Casting Al-Si alloys in tension and in Low Cycle Fatigue at room temperature. First of all, the microstructures of studied alloys were thoroughly characterized both in 2D and in 3D. The most suitable and representative specimens and Region of Interest (ROIs) where the in-situ monitoring was performed were selected through a preliminary characterization using X-ray tomography, which is also necessary to understand damage mechanisms after failure. In-situ observations performed on surface using Questar long distance microscope and in volume using X-ray tomography allow following cracks initiations and their propagations and thus allow identifying the relation between damage mechanisms and casting microstructure. 2D/3D displacement and strain fields measured using Digital Image Correlation and Digital Volume Correlation allows analyzing the relation between measured fields and damage mechanisms. Postmortem analysis and FEM simulation gave more information for the damage mechanisms. Large pores favor crack initiation as they strongly increase local stress level. Hard inclusions (Si phase, iron intermetallics and copper containing phases) also play an important role in crack initiation and propagation due to strain localizations at these inclusions
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Spartacus, Gabriel. "Evolution des nano-oxydes et de la microstructure au cours du procédé de fabrication d'aciers renforcés par dispersion d'oxydes." Thesis, Université Grenoble Alpes, 2020. http://www.theses.fr/2020GRALI085.
Abstract:
Les aciers renforcés par dispersion d’oxydes (ODS pour Oxide Dispersion Strengthened) sont des matériaux candidats pour leur utilisation comme gainage du combustible pour des centrales nucléaires de génération IV. Dans ces aciers, une dispersion de nano-oxydes Y-Ti-O à l’origine de l’essentiel des propriétés mécaniques de l’alliage, est incorporée dans une matrice par métallurgie des poudres. Pendant ce procédé, une poudre d’acier Fe-Cr est broyée avec une poudre d’Y2O3 et une poudre de TiH2, afin de mettre en solution l’Y, le Ti et l’O, autrement immiscible dans la matrice. Le broyage induit aussi une microstructure de très petits grains avec une forte densité de dislocations. La poudre obtenue est ensuite consolidée par filage à chaud ou compaction isostatique à chaud à une température de 1100℃. Cette étape induit la précipitation des nano-oxydes, finement dispersés dans la matrice, en forte densité numérique et extrêmement stables à haute température. La microstructure évolue aussi pendant le recuit, de façon concomitante à l’évolution des nano-oxydes, qui agissent comme points d’ancrage pour les joints de grains et les dislocations. Ceci mène à un phénomène de croissance anormale des grains (croissance importante de certains grains seulement), et à une répartition de taille de grains bimodale après consolidation. L’objectif de cette thèse est de caractériser la cinétique et les évolutions de chimie des nano-oxydes, ainsi que les évolutions de la microstructure granulaire, pendant le procédé de fabrication, qui sont encore mal compris. Ces résultats sont cruciaux pour la maitrise du procédé de fabrication des aciers ODS, et représentent un jeu de données unique pour le développement de simulations de précipitation.Ainsi, des échantillons de poudres après broyage ont été compactés à froid, afin de les densifier sans induire la précipitation des nano-oxydes. Ces échantillons ont été ensuite caractérisés au cours du traitement thermique de consolidation. La cinétique de précipitation a été mesurée sur plusieurs nuances d’aciers ODS par diffusion de rayons-X aux petits angles (SAXS pour Small Angle X-ray Scattering) in-situ pendant le traitement thermique jusqu’à 1100℃. Pour caractériser les évolutions de chimie et de structure des nano-oxydes, des mesures de SAXS anomales au seuil de l’Y (in-situ), au seuil du Ti (ex-situ), de diffusion de neutrons aux petits angles et de sonde atomique tomographique ont été réalisées. Finalement, l’évolution de la microstructure granulaire a été caractérisée par diffraction des rayons-X in-situ.Ces caractérisations ont été réalisées sur des aciers ODS ferritiques et ferritiques / martensitiques, ainsi que sur des aciers ODS comportant des variations sur les propriétés des renforts. En particulier, la présence d’amas de très petite taille contenant de l’Y, de l’O et du Ti dans une moindre mesure a été constatée dès la condition post-broyage. Ces amas, évoluent en chimie et en structure jusqu’à devenir des nano-oxydes stables, Y2Ti2O7 pyrochlore et Y2TiO5 orthorhombique, dans des proportions variables suivant les nuances. De plus, une augmentation de la vitesse de croissance et de coalescence a été observée lors du changement de phase de la matrice des ODS ferritiques / martensitiques. La comparaison entre les résultats de cinétique de précipitation et de microstructure granulaire a permis la compréhension des températures de croissance anormale des grains, suivant la nuance considérée. Finalement, les comparaisons des simulations de précipitation avec les résultats expérimentaux ont permis d’obtenir de nouveaux éléments de compréhension des mécanismes de précipitationsOxide Dispersion Strengthened (ODS) steels with a Fe-Cr matrix are of great interest in the development of generation IV fission nuclear power plants as a fuel cladding material. These materials, elaborated by powder metallurgy, include a high density of Y-Ti-O oxide precipitates of a few nm, providing the main contribution to the ODS steels strength. During the fabrication process, powders of Fe-Cr steel, Y2O3 and TiH2 are milled together to obtain a super-saturated solution of Y, Ti and O, otherwise insoluble in Fe. The obtained powder is subsequently processed by Hot Extrusion or Hot Isostatic Pressing around 1100℃. This induces the precipitation of Y-Ti-O and leads to a fully dense steel with finely dispersed nano-oxides in high density, extremely stable even at very high temperature. Moreover, the complex microstructure induced by the milling stage, including high density of dislocations and very small grain size, also evolve during the heating, in an intricate ways with the evolution of the nano-oxides that act as strong pinning points for both grain boundaries and dislocations. This features leads to abnormal grain growth (significant growth of some grains, while others remain stable) and therefore a bimodal grain size after consolidation.The aim of this thesis is to characterize both kinetics and chemical evolution of the nano-oxides during the fabrication process of these steels, as well as the grain microstructure evolution, which are still misunderstood. Such experimental characterization would be invaluable to further control the fabrication process and improve available model of the ODS precipitation kinetics. For this purpose, cold pressed specimens from as-milled powder were prepared (in order to achieve dense specimens without precipitation) and observed by means of various in-situ or ex-situ techniques. In particular, in-situ Small Angle X-ray Scattering measurements were performed during the heating until 1100℃ to measure the precipitation kinetics of several ODS grades. The chemistry and structure of nano-oxides were assessed thanks to anomalous SAXS at Y (performed in-situ) and Ti (ex-situ) edges, ex-situ small angle neutron scattering and atom probe tomography. Then, the grain microstructure was monitored by in-situ X-ray diffraction.These characterizations allow to describe the whole kinetics of purely ferritic ODS, ferritic / martensitic ODS and ODS strengthened with variation of the strengthening powders. In particular, this study highlights a non-homogeneous as-milled stage with clusters containing Y, O and Ti in lesser extent. These clusters evolve in chemistry and structure until reaching a stable structure and stoichiometry, revealed to be Y2Ti2O7 pyrochlore and Y2TiO5 orthorhombic depending on the ODS steel grade. Moreover, a kinetic modification induced by the in temperature phase transformation of the matrix in the ferritic / martensitic ODS (increasing the growth and coarsening rate) was observed. Correlation between nano-oxide and the grain microstructure evolutions were performed and help in the comprehension of the abnormal grain growth temperature and final grain morphology, from one ODS grade to another. Finally, comparisons of the precipitation simulations with experimental data allow to get more insights on the nano-oxides properties
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Vanpeene, Victor. "Étude par tomographie RX d'anodes à base de silicium pour batteries Li-ion." Thesis, Lyon, 2019. http://www.theses.fr/2019LYSEI023/document.
Abstract:
De par sa capacité spécifique théorique dix fois plus élevée que celle du graphite actuellement utilisé comme matériau actif d'anode pour les batteries Li-ion, le silicium peut jouer un rôle important dans l'augmentation de la densité d'énergie de ces systèmes. La réaction d'alliage mise en place lors de sa lithiation se traduit cependant par une forte expansion volumique du silicium (~300 % contre seulement ~10 % pour le graphite), conduisant à la dégradation structurale de l'électrode, affectant notablement sa tenue au cyclage. Comprendre en détail ces phénomènes de dégradation et développer des stratégies pour limiter leur impact sur le fonctionnement de l'électrode présentent un intérêt indéniable pour la communauté scientifique du domaine. L'objectif de ces travaux de thèse était en premier lieu de développer une technique de caractérisation adaptée à l'observation de ces phénomènes de dégradation et d'en tirer les informations nécessaires pour optimiser la formulation des anodes à base de silicium. Dans ce contexte, nous avons utilisé la tomographie aux rayons X qui présente l'avantage d'être une technique analytique non-destructive permettant le suivi in situ et en 3D des variations morphologiques s'opérant au sein de l'électrode lors de son fonctionnement. Cette technique a pu être adaptée à l'étude de cas du silicium en ajustant les volumes d'électrodes analysés, la résolution spatiale et la résolution temporelle aux phénomènes à observer. Des procédures de traitement d'images adéquates ont été appliquées afin d'extraire de ces analyses tomographiques un maximum d'informations qualitatives et quantitatives pertinentes sur leur variation morphologique. De plus, cette technique a pu être couplée à la diffraction des rayons X afin de compléter la compréhension de ces phénomènes. Nous avons ainsi montré que l'utilisation d'un collecteur de courant 3D structurant en papier carbone permet d'atténuer les déformations morphologiques d'une anode de Si et d'augmenter leur réversibilité en comparaison avec un collecteur de courant conventionnel de géométrie plane en cuivre. Nous avons aussi montré que l'utilisation de nanoplaquettes de graphène comme additif conducteur en remplacement du noir de carbone permet de former un réseau conducteur plus à même de supporter les variations volumiques importantes du silicium. Enfin, la tomographie RX a permis d'étudier de façon dynamique et quantitative la fissuration et la délamination d'une électrode de Si déposée sur un collecteur de cuivre. Nous avons ainsi mis en évidence l'impact notable d'un procédé de "maturation" de l'électrode pour minimiser ces phénomènes délétères de fissuration-délamination de l'électrodeBecause of its theoretical specific capacity ten times higher than that of graphite currently used as active anode material for Li-ion batteries, silicon can play an important role in increasing the energy density of these systems. However, the alloying reaction set up during its lithiation results in a high volume expansion of silicon (~300% compared with only ~10% for graphite) leading to the structural degradation of the electrode, which is significantly affecting its cycling behavior. Understanding in detail these phenomena of degradation and developing strategies to limit their impact on the functioning of the electrode are of undeniable interest for the scientific community of the field. The objective of this thesis work was first to develop a characterization technique adapted to the observation of these degradation phenomena and to draw the necessary information to optimize the formulation of silicon-based anodes. In this context, we have used X-ray tomography which has the advantage of being a non-destructive analytical technique allowing in situ and 3D monitoring of the morphological variations occurring within the electrode during its operation. This technique has been adapted to the case study of silicon by adjusting the analyzed electrode volumes, the spatial resolution and the temporal resolution to the phenomena to be observed. Appropriate image processing procedures were applied to extract from these tomographic analyzes as much qualitative and quantitative information as possible on their morphological variation. In addition, this technique could be coupled to X-ray diffraction to complete the understanding of these phenomena. We have shown that the use of a carbon paper structuring 3D current collector makes it possible to attenuate the morphological deformations of an Si anode and to increase their reversibility in comparison with a conventional copper current collector of plane geometry. We have also shown that the use of graphene nanoplatelets as a conductive additive to replace carbon black can form a conductive network more able to withstand the large volume variations of silicon. Finally, the X-ray tomography allowed studying dynamically and quantitatively the cracking and delamination of an Si electrode deposited on a copper collector. We have thus demonstrated the significant impact of a process of "maturation" of the electrode to minimize these deleterious phenomena of cracking-delamination of the electrode
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Sorel, Julien. "Tomographie électronique analytique : Automatisation du traitement de données et application aux nano-dispositifs 3D en micro-électronique." Thesis, Lyon, 2020. http://www.theses.fr/2020LYSEI078.
Abstract:
Ce travail porte sur l’automatisation du traitement des données de tomographie électronique analytique appliquée aux nano-dispositifs électroniques. La technique utilisée est la spectroscopie de dispersion en énergie des rayons-X en mode balayage en microscopie électronique en transmission (STEM-EDX : Scanning Transmission Electron Microscopy, Energy Dispersive X-ray spectroscopy). Si la tomographie électronique STEM-EDX a bénéficié d’avancées technologiques récentes, comme de nouvelles sources électroniques ‘X’-FEG (Field Emission Gun) et des détecteurs X sensibles, les SDD (Silicon Drift Detectors), elle reste chronophage avec une statistique de comptage souvent faible pour éviter des durées prohibitives et une dégradation de l’échantillon par irradiation électronique. L’empilement des projections STEM-EDX, acquises sous différents angles d’inclinaison, est par ailleurs très volumineux et les logiciels commerciaux actuels ne peuvent pas le traiter automatiquement et de manière optimale. Pour améliorer cette situation, nous avons développé un programme utilisant la librairie Hyperspy en langage python, dédiée au traitement de données multi-dimensionnelles. L’analyse statistique multivariée permet d’optimiser et d’automatiser le débruitage des données, la calibration des spectres et la séparation des raies d’émission X superposées pour l’obtention de reconstructions tridimensionnelles quantitatives. Une technique de reconstruction avancée, l’acquisition comprimée, a aussi été mise en œuvre, diminuant le nombre de projections sans réduire l’information 3D finale. La méthode développée a été utilisée pour l’analyse chimique 3D de quatre nanostructures issues de la microélectronique : des transistors FET multi-grilles, HEMT et GAA, et un film mince GeTe. Les échantillons ont été taillés en pointe par FIB (Focused Ion Beam: Faisceau d’ions focalisés), et les données obtenues sur un microscope Titan Themis muni d’un système à 4 détecteurs SDD. L’évaluation du programme atteste qu’il permet d’obtenir des résultats précis et fiables sur les architectures 3D étudiées. Des pistes d’améliorations sont discutées en perspective d’un futur logiciel dédié au traitement de données en tomographie électronique analytiqueThe aim of this thesis is to automate the process of hyperspectral analysis for analytical electron tomography applied to nanodevices. The work presented here is focused on datasets obtained by energy-dispersive X-ray spectroscopy in a scanning transmission electron microscope (STEM-EDX). STEM-EDX tomography has benefited greatly from recent developments in electron sources such as the ‘X’-FEG (Field Emission Gun), and multiple X-ray detector systems such as the Super-X, incorporating four SSD (Silicon Drift Detectors) detectors. The technique remains however very time-consuming, and low X-ray count rates are necessary to minimize the total acquisition time and avoid beam damage during the experiment. In addition, tomographic stacks of STEM-EDX datacubes, acquired at different tilt angles, are too large to be analyzed by commercial software packages in an optimal way. In order to automate this process, we developed a code based on Hyperspy, a Python library for multidimensional data analysis. Multivariate statistical analysis techniques were employed to optimize and automate the denoising, the energy calibration and the separation of overlapping X-ray lines, with the aim to achieve quantitative, chemically sensitive volumes. Moreover, a compressed sensing based algorithm was employed to achieve high fidelity reconstructions with undersampled tomographic datasets. The code developed during this thesis was used for the 3D chemical analysis of four microelectronic nanostructures: FinFET, HEMT and GAA transistors, and a GeTe thin film for memory device applications. The samples were prepared in a needle shape using a focused ion beam, and the data acquisitions were performed using a Titan Themis microscope equipped with a super-X EDX detector system. It is shown that the code yields 3D morphological and chemical information with high accuracy and fidelity. Ways to improve the current methodology are discussed, with future efforts aiming at developing a package dedicated to analytical electron tomography
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Devillard, Julie. "Lien entre microstructure et résistance à la compression du gypse moussé." Thesis, Lyon, 2020. http://www.theses.fr/2020LYSEI043.
Abstract:
La présente étude porte sur la caractérisation microstructurale et mécanique du gypse moussé, matériau de cœur des plaques de plâtre allégées, présentant une forte porosité (75%) multi-échelle. L'objectif de ce travail est de déterminer l'influence de la microstructure du gypse moussé sur la dureté mesurée en indentation sphérique et d'analyser les mécanismes d'endommagement pour différentes microstructures. Des essais d’indentation sphérique ont été conduits sur des échantillons présentant des variations des différentes caractéristiques microstructurales du gypse moussé. Ces essais montrent que la masse a une influence du premier ordre sur la dureté et que la dispersion des mesures de dureté en indentation sphérique peut être reliée à l’hétérogénéité de la macroporosité. Des essais d'indentation in situ ont également été effectués, avec un suivi en tomographie aux rayons X et une analyse par corrélation d’images volumiques, afin d’étudier avec précision les mécanismes d'endommagement. Deux modes d'endommagement différents ont été déterminés selon les densités considérées (fraction de macropores variable). Les résultats de ces essais ont été utilisés pour alimenter un modèle analytique, basé sur un critère énergétique qui relie la force d'indentation à la zone endommagée sous l’indenteur. Cela permet de prédire la courbe force-déplacement d'indentation propre à une microstructure avec comme seule donnée d'entrée un scan de la microstructure initiale. Une modélisation numérique a également été effectuée grâce à la méthode des éléments finis avec la prise en compte de la microstructure réelle, à deux échelles. L’utilisation de différents modèles de comportement, basés sur des critères de plasticité, a permis de prévoir les régions impactées par la densificationThis study focuses on the microstructural and mechanical characterization of foamed gypsum, the core material of lightweight gypsum boards, with a high (75%) multi-scale porosity. The objective of this work is to determine the influence of the microstructure of foamed gypsum on the hardness measured in spherical indentation and to analyze the damage mechanisms for different microstructures. Spherical indentation tests were conducted on samples showing variations in microstructural features of foamed gypsum. The results of these tests show that density has a first-order influence on hardness and that the dispersion of hardness measurements in spherical indentation can be related to heterogeneity in macroporosity. In situ indentation tests were also carried out, with X-ray tomography and digital volume correlation (DVC) analysis, in order to accurately study the damage mechanisms. Two different modes of damage were determined according to the densities considered (variable macropore fraction). The results of these tests were used to feed an analytical model, based on an energy criterion that links the indentation force to the damaged area under the indenter. This provides the prediction of the indentation force-displacement curve specific to a microstructure with a scan of the initial microstructure as the only input data. Numerical modelling was also carried out using the finite element method with consideration of the actual microstructure, at two scales. The densified areas were properly predicted by different behaviour models based on plasticity criteria
35
Ornek, Cem. "Performance characterisation of duplex stainless steel in nuclear waste storage environment." Thesis, University of Manchester, 2016. https://www.research.manchester.ac.uk/portal/en/theses/performance-characterisation-of-duplex-stainless-steel-in-nuclear-waste-storage-environment(4db73e9b-c87c-40a6-9778-0b823b1c499f).html.
Abstract:
The majority of UK’s intermediate level radioactive waste is currently stored in 316L and 304L austenitic stainless steel containers in interim storage facilities for permanent disposal until a geological disposal facility has become available. The structural integrity of stainless steel canisters is required to persevere against environmental degradation for up to 500 years to assure a safe storage and disposal scheme. Hitherto existing severe localised corrosion observances on real waste storage containers after 10 years of exposure to an ambient atmosphere in an in-land warehouse in Culham at Oxfordshire, however, questioned the likelihood occurrence of stress corrosion cracking that may harm the canister’s functionality during long-term storage. The more corrosion resistant duplex stainless steel grade 2205, therefore, has been started to be manufactured as a replacement for the austenitic grades. Over decades, the threshold stress corrosion cracking temperature of austenitic stainless steels has been believed to be 50-60°C, but lab- and field-based research has shown that 304L and 316L may suffer from atmospheric stress corrosion cracking at ambient temperatures. Such an issue has not been reported to occur for the 2205 duplex steel, and its atmospheric stress corrosion cracking behaviour at low temperatures (40-50°C) has been sparsely studied which requires detailed investigations in this respect. Low temperature atmospheric stress corrosion cracking investigations on 2205 duplex stainless steel formed the framework of this PhD thesis with respect to the waste storage context. Long-term surface magnesium chloride deposition exposures at 50°C and 30% relative humidity for up to 15 months exhibited the occurrence of stress corrosion cracks, showing stress corrosion susceptibility of 2205 duplex stainless steel at 50°C.The amount of cold work increased the cracking susceptibility, with bending deformation being the most critical type of deformation mode among tensile and rolling type of cold work. The orientation of the microstructure deformation direction, i.e. whether the deformation occurred in transverse or rolling direction, played vital role in corrosion and cracking behaviour, as such that bending in transverse direction showed almost 3-times larger corrosion and stress corrosion cracking propensity. Welding simulation treatments by ageing processes at 750°C and 475°C exhibited substantial influences on the corrosion properties. It was shown that sensitisation ageing at 750°C can render the material enhanced susceptible to stress corrosion cracking at even low chloride deposition densities of ≤145 µm/cm². However, it could be shown that short-term heat treatments at 475°C can decrease corrosion and stress corrosion cracking susceptibility which may be used to improve the materials performance. Mechanistic understanding of stress corrosion cracking phenomena in light of a comprehensive microstructure characterisation was the main focus of this thesis.
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"Corrosion and Corrosion-Fatigue Behavior of 7075 Aluminum Alloys Studied By In Situ X-Ray Tomography." Doctoral diss., 2017. http://hdl.handle.net/2286/R.I.46294.
Abstract:
abstract: 7XXX Aluminum alloys have high strength to weight ratio and low cost. They are used in many critical structural applications including automotive and aerospace components. These applications frequently subject the alloys to static and cyclic loading in service. Additionally, the alloys are often subjected to aggressive corrosive environments such as saltwater spray. These chemical and mechanical exposures have been known to cause premature failure in critical applications. Hence, the microstructural behavior of the alloys under combined chemical attack and mechanical loading must be characterized further. Most studies to date have analyzed the microstructure of the 7XXX alloys using two dimensional (2D) techniques. While 2D studies yield valuable insights about the properties of the alloys, they do not provide sufficiently accurate results because the microstructure is three dimensional and hence its response to external stimuli is also three dimensional (3D). Relevant features of the alloys include the grains, subgrains, intermetallic inclusion particles, and intermetallic precipitate particles. The effects of microstructural features on corrosion pitting and corrosion fatigue of aluminum alloys has primarily been studied using 2D techniques such as scanning electron microscopy (SEM) surface analysis along with post-mortem SEM fracture surface analysis to estimate the corrosion pit size and fatigue crack initiation site. These studies often limited the corrosion-fatigue testing to samples in air or specialized solutions, because samples tested in NaCl solution typically have fracture surfaces covered in corrosion product. Recent technological advancements allow observation of the microstructure, corrosion and crack behavior of aluminum alloys in solution in three dimensions over time (4D). In situ synchrotron X-Ray microtomography was used to analyze the corrosion and cracking behavior of the alloy in four dimensions to elucidate crack initiation at corrosion pits for samples of multiple aging conditions and impurity concentrations. Additionally, chemical reactions between the 3.5 wt% NaCl solution and the crack surfaces were quantified by observing the evolution of hydrogen bubbles from the crack. The effects of the impurity particles and age-hardening particles on the corrosion and fatigue properties were examined in 4D.Dissertation/Thesis
Doctoral Dissertation Materials Science and Engineering 2017
37
"Deformation Behavior of adidas BOOST(TM) Foams Using In Situ X-ray Tomography and Correlative Microscopy." Doctoral diss., 2020. http://hdl.handle.net/2286/R.I.62793.
Abstract:
abstract: Energy return in footwear is associated with the damping behavior of midsole foams, which stems from the combination of cellular structure and polymeric material behavior. Recently, traditional ethyl vinyl acetate (EVA) foams have been replaced by BOOST(TM) foams, thereby reducing the energetic cost of running. These are bead foams made from expanded thermoplastic polyurethane (eTPU), which have a multi-scale structure consisting of fused porous beads, at the meso-scale, and thousands of small closed cells within the beads at the micro-scale. Existing predictive models coarsely describe the macroscopic behavior but do not take into account strain localizations and microstructural heterogeneities. Thus, enhancement in material performance and optimization requires a comprehensive understanding of the foam’s cellular structure at all length scales and its influence on mechanical response.
This dissertation focused on characterization and deformation behavior of eTPU bead foams with a unique graded cell structure at the micro and meso-scale. The evolution of the foam structure during compression was studied using a combination of in situ lab scale and synchrotron x-ray tomography using a four-dimensional (4D, deformation + time) approach. A digital volume correlation (DVC) method was developed to elucidate the role of cell structure on local deformation mechanisms. The overall mechanical response was also studied ex situ to probe the effect of cell size distribution on the force-deflection behavior. The radial variation in porosity and ligament thickness profoundly influenced the global mechanical behavior. The correlation of changes in void size and shape helped in identifying potentially weak regions in the microstructure. Strain maps showed the initiation of failure in cell structure and it was found to be influenced by the heterogeneities around the immediate neighbors in a cluster of voids. Poisson’s ratio evaluated from DVC was related to the microstructure of the bead foams. The 4D approach taken here provided an in depth and mechanistic understanding of the material behavior, both at the bead and plate levels, that will be invaluable in designing the next generation of high-performance footwear.Dissertation/Thesis
Doctoral Dissertation Materials Science and Engineering 2020
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(8780756), Imad A. Hanhan. "Investigating damage in discontinuous fiber composites through coupled in-situ X-ray tomography experiments and simulations." Thesis, 2020.
Abstract:
Composite materials have become widely used in engineering applications, in order to reduce the overall weight of structures while retaining their required strength. Due to their light weight, relatively high stiffness properties, and formability into complex shapes, discontinuous fiber composites are advantageous for producing small and medium size components. However, qualifying their mechanical properties can be expensive, and therefore there is a need to improve predictive capabilities to help reduce the overall cost of large scale testing. To address this challenge, a composite material consisting of discontinuous glass fibers in a polypropylene matrix is studied at the microstructural level through coupled experiments and simulations, in order to uncover the mechanisms that cause microvoids to initiate and progress, as well as certain fiber breakage events to occur, during macroscopic tension. Specifically, this work coupled in-situ X-ray micro computed tomography (μ-CT) experiments with a finite element simulation of the exact microstructure to enable a 3D study that tracked damage initiation and propagation, and computed the local stresses and strains in the microstructure. In order to have a comprehensive 3D understanding of the evolution of the microstructure, high fidelity characterization procedures were developed and applied to the μ-CT images in order to understand the exact morphology of the microstructure. To aid in this process, ModLayer - an interactive image processing tool - was created as a MATLAB executable, and the 3D microstructural feature detection techniques were compared to traditional destructive optical microscopy techniques. For damage initiation, this work showed how high hydrostatic stresses in the matrix can be used as a metric to explain and predict the exact locations of microvoid nucleation within the composite’s microstructure. From a damage propagation standpoint, matrix cracking - a mechanism that has been notably difficult to predict because of its apparent stochastic nature - was studied during damage propagation. The analysis revealed the role of shear stress in fiber mediated flat matrix cracking, and the role of hydrostatic stress in fiber-avoidance conoidal matrix cracking. Overall, a sub-fiber simulation and an in-situ experimental analysis provided the microstructural physical phenomena that govern certain damage initiation and progression mechanisms, further enabling the strength and failure predictions of short fiber thermoplastic composites.
39
"Characterization of Thermo-Mechanical Damage in Tin and Sintered Nano-Silver Solders." Doctoral diss., 2018. http://hdl.handle.net/2286/R.I.49323.
Abstract:
abstract: Increasing density of microelectronic packages, results in an increase in thermal and mechanical stresses within the various layers of the package. To accommodate the high-performance demands, the materials used in the electronic package would also require improvement. Specifically, the damage that often occurs in solders that function as die-attachment and thermal interfaces need to be addressed. This work evaluates and characterizes thermo-mechanical damage in two material systems – Electroplated Tin and Sintered Nano-Silver solder.
Tin plated electrical contacts are prone to formation of single crystalline tin whiskers which can cause short circuiting. A mechanistic model of their formation, evolution and microstructural influence is still not fully understood. In this work, growth of mechanically induced tin whiskers/hillocks is studied using in situ Nano-indentation and Electron Backscatter Diffraction (EBSD). Electroplated tin was indented and monitored in vacuum to study growth of hillocks without the influence of atmosphere. Thermal aging was done to study the effect of intermetallic compounds. Grain orientation of the hillocks and the plastically deformed region surrounding the indent was studied using Focused Ion Beam (FIB) lift-out technique. In addition, micropillars were milled on the surface of electroplated Sn using FIB to evaluate the yield strength and its relation to Sn grain size.
High operating temperature power electronics use wide band-gap semiconductor devices (Silicon Carbide/Gallium Nitride). The operating temperature of these devices can exceed 250oC, preventing use of traditional Sn-solders as Thermal Interface materials (TIM). At high temperature, the thermomechanical stresses can severely degrade the reliability and life of the device. In this light, new non-destructive approach is needed to understand the damage mechanism when subjected to reliability tests such as thermal cycling. In this work, sintered nano-Silver was identified as a promising high temperature TIM. Sintered nano-Silver samples were fabricated and their shear strength was evaluated. Thermal cycling tests were conducted and damage evolution was characterized using a lab scale 3D X-ray system to periodically assess changes in the microstructure such as cracks, voids, and porosity in the TIM layer. The evolution of microstructure and the effect of cycling temperature during thermal cycling are discussed.Dissertation/Thesis
Doctoral Dissertation Materials Science and Engineering 2018
40
Wilke, Robin Niklas. "Coherent X-Ray Diffractive Imaging on the Single-Cell-Level of Microbial Samples:." Doctoral thesis, 2014. http://hdl.handle.net/11858/00-1735-0000-0023-996A-0.
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"Structure-Property Relationships in Aluminum-Copper alloys using Transmission X-Ray Microscopy (TXM) and Micromechanical Testing." Doctoral diss., 2017. http://hdl.handle.net/2286/R.I.46186.
Abstract:
abstract: Aluminum alloys are ubiquitously used in almost all structural applications due to their high strength-to-weight ratio. Their superior mechanical performance can be attributed to complex dispersions of nanoscale intermetallic particles that precipitate out from the alloy’s solid solution and offer resistance to deformation. Although they have been extensively investigated in the last century, the traditional approaches employed in the past haven’t rendered an authoritative microstructural understanding in such materials. The effect of the precipitates’ inherent complex morphology and their three-dimensional (3D) spatial distribution on evolution and deformation behavior have often been precluded. In this study, for the first time, synchrotron-based hard X-ray nano-tomography has been implemented in Al-Cu alloys to measure growth kinetics of different nanoscale phases in 3D and reveal mechanistic insights behind some of the observed novel phase transformation reactions occurring at high temperatures. The experimental results were reconciled with coarsening models from the LSW theory to an unprecedented extent, thereby establishing a new paradigm for thermodynamic analysis of precipitate assemblies. By using a unique correlative approach, a non-destructive means of estimating precipitation-strengthening in such alloys has been introduced. Limitations of using existing mechanical strengthening models in such alloys have been discussed and a means to quantify individual contributions from different strengthening mechanisms has been established.
The current rapid pace of technological progress necessitates the demand for more resilient and high-performance alloys. To achieve this, a thorough understanding of the relationships between material properties and its structure is indispensable. To establish this correlation and achieve desired properties from structural alloys, microstructural response to mechanical stimuli needs to be understood in three-dimensions (3D). To that effect, in situ tests were conducted at the synchrotron (Advanced Photon Source) using Transmission X-Ray Microscopy as well as in a scanning electron microscope (SEM) to study real-time damage evolution in such alloys. Findings of precipitate size-dependent transition in deformation behavior from these tests have inspired a novel resilient aluminum alloy design.Dissertation/Thesis
Doctoral Dissertation Materials Science and Engineering 2017