Die Dunkelfeld off-axis Elektronenholographie (DFH) im Transmissionselektronenmikroskop ist eine nanoskalige Interferometriemethode, die es erlaubt, eine ausgewählte Beugungswelle eines Kristalls aufzuzeichnen und anschließend als zweidimensionale Amplituden- und Phasenverteilung zu rekonstruieren. Da sich aus dem Gradientenfeld der Phasenverteilung geometrische Verzerrungen des Kristallgitters bestimmen lassen, ermöglicht die DFH, Deformationsfelder in Kristallen zu vermessen. Damit eröffnen sich der Halbleiterindustrie vielversprechende Analysemöglichkeiten von lokalen mechanischen Verspannungen in Halbleiterkristallen insbesondere im Kanalbereich von Transistoren. Dabei verspricht die DFH eine höhere Ortsauflösung als rasternde, auf Elektronenbeugung mit möglichst fein fokussierten Elektronensonden basierende Methoden wie Nanobeugung. Jedoch steht die DFH als Analysemethode für mechanische Verspannungen bisher noch nicht standardmäßig zur Verfügung. Forschungs- und Entwicklungsbedarf besteht insbesondere hinsichtlich der Anpassung der Methodik auf kompliziertere Halbleiterstrukturen. Am Beispiel des Elementargitters wird demonstriert, wie einerseits die Gitterverzerrung die Phase der Beugungswelle moduliert, und wie andererseits aus dem Gradient der Phase diese Deformation wieder rekonstruiert werden kann. Zusätzlich wird die Modulation der Beugungswelle mit Hilfe eines erst kürzlich veröffentlichten analytischen Modells für den Zweistrahlfall erläutert. Spezielle Anpassungen der DFH im TEM erlauben, die geometrische Phase entweder mit 3...5 nm Lateralauflösung bei 200 nm breitem Gesichtsfeld oder mit 8...10 nm Lateralauflösung bei 800 nm breitem Gesichtsfeld aufzuzeichnen. Da die Deformationskarte durch numerische Ableitung der geometrischen Phase bestimmt wird, hängt die Signalauflösung der Deformationsmessung direkt von der Signalqualität in der rekonstruierten geometrischen Phase ab. Da die Ableitung das Rauschen verstärkt, werden verschiedene Strategien zur Rauschminderung und Signalverbesserung untersucht, u.a. werden Methoden zur Rauschfilterung eines DF-Hologramms oder zur Glättung der Deformationskarte vorgestellt. Durch Rekonstruktion einer gemittelten geometrischen Phase aus einer Dunkelfeldhologrammserie lassen sich Deformationen E mit einer Messabweichung von lediglich Delta_E=+/-0,05% bestimmen. Bei Aufzeichnung und Rekonstruktion der geometrischen Phase treten eine Reihe von Artefakten auf, die durch Fresnelsche Beugungssäume, defekte Detektorpixel sowie Verzeichnungen durch Projektivlinsen und Detektoroptik hervorgerufen werden. Da sie die Bestimmung der Deformationskarte erschweren, werden geeignete Methoden zur Vermeidung oder Korrektur vorgestellt. Die Präparation von TEM-Lamellen mit fokussiertem Ionenstrahl (FIB) verursacht Schädigungen der Probenoberfläche. Durch Vergleiche von DFH-Messungen mit Finite-Elemente-Simulationen wird gezeigt, dass die auf Oberflächenrelaxation zurückzuführenden Abweichungen vom simulierten Deformationszustand bei 120...160 nm Lamellendicke bis zu 10% betragen können. Präparationsbedingte lokale Dickenvariationen (Curtaining) können zu ähnlich großen Abweichungen führen. Anwendbarkeit und Funktionalität der DFH werden an modernen Halbleiterstrukturen untersucht. Die Vermessung einer verspannten SiGe-Schicht auf Si-Substrat zeigt eine sehr gute Übereinstimmung mit einem analytischen Modell. Die Abweichung beträgt ca. 10% und kann durch Oberflächenrelaxation an der SiGe/Si-Grenzfläche erklärt werden. Mittels SiGe an Source und Drain verspannte Transistoren dienen als Testobjekte für einen Vergleich von DFH und Nanobeugung. Beide Methoden liefern identische Ergebnisse. Der Vorteil der DFH besteht jedoch darin, das Deformationsfeld vollständig in Form einer zweidimensionalen Karte abzubilden, anstatt wie die Nanobeugung lediglich einzelne Profilschnitte zu messen. Die Deformationsmessung an SOI-Strukturen wird durch die leicht unterschiedliche Kristallorientierung (Miscut) zwischen SOI und Si-Substrat, das als Referenzbereich dient, erschwert. Die Deformationswerte im SOI zeigen ein Offset von 0,2% Dehnung gegenüber dem Si-Substrat. Der Miscut zwischen SOI und Si-Substrat kann zu 0,3°bestimmt werden. Für Transistoren mit tensiler Deckschicht gelingt es, Dehnungen von +0,3% in perfekter Übereinstimmung mit FE-Simulationen zu messen. Bei Transistoren, bei denen gleichzeitig eine kompressive Deckschicht und SiGe an Source und Drain eingesetzt werden, gelingt es mittels DFH, Stauchungen von -(0,1+/-0,05)% im Transistorkanal 5 nm unterhalb des Gateoxids nachzuweisen. / Dark-field off-axis electron holography (DFH) in a transmission electron microscope is based on the interference of a diffracted wave emanating from adjacent strained and unstrained sample areas to form a dark-field hologram, from which the phase of the diffracted wave can be reconstructed. Since the gradient of the phase parallel to the diffraction vector yields the lattice strain in this direction, a two-dimensional strain map can be derived. Therefore, DFH is considered to be a promising technique for strain metrology by semiconductor industry, especially for local strain measurements in the transistor channel. In particular, DFH offers better lateral resolution than scanning TEM-techniques based on electron diffraction with small focused electron probe like nano-beam diffraction. However, DFH is not yet available as a standard technique for strain metrology. Research is still needed to apply the method to complex devices. Using the example of a strained cosine lattice the phase modulation due to lattice distortions is discussed. In addition, modulation of the diffracted wave is approximated in two-beam diffraction condition. Adjustments of DFH in the TEM provide strain measurements with 3...5 nm lateral resolution at 200 nm field of view or 8...10 nm lateral resolution at 800 nm field of view. During recording and reconstruction of dark-field holograms several artifacts appear, for instance Fresnel diffraction, defective detector pixels, distortions of projective lenses or detector optics. Since they limit strain evaluation, suitable methods to either avoid or correct these artifacts are discussed. Sample preparation with focused ion beam (FIB) causes surface damage. Comparing DFH results with finite-element simulations reveals a deviation of 10% between simulation and experiment at 120...160 nm sample thickness due to surface relaxation. FIB-induced thickness variations (curtaining) lead to comparable deviations. Applicability of DFH for strain metrology is analyzed on several modern device structures. Strain measurements of SiGe-layers on Si-substrate correspond quite well with an analytic model. A residual deviation of 10% can be explained by surface relaxation close to the SiGe/Si-interface. Transistors strained by SiGe-source/drain serve as test objects for a comparison of DFH with nano-beam diffraction. Though both techniques reveal identical results, DFH is able to map the complete two-dimensional strain field, whereas nano-beam diffraction can only provide single line-scans. Strain mapping in silicon-on-insulator (SOI) is limited by the different crystal orientation (miscut) between the SOI layer and the Si-substrate, which serves as reference. Strain values in the SOI show an off-set of 0.2% in comparison to the unstrained Si-substrate. The miscut between SOI and Si-substrate is estimated to 0.3°. In transistor devices with tensile stress overlayers DFH is able to measure +0.3% tensile strain in excellent agreement with finite-element simulations. In devices with compressive overlayers and SiGe-source/drain a strain value of only -(0.1+/-0.05)% can be determined in the transistor channel 5nm beneath the gate oxide.

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Nous présentons deux approches différentes pour décrire le couplage hydromécanique des géomatériaux. Dans une approche de type phénoménologique nous traitons le milieu poreux comme un milieu continu équivalent dont les interactions entre la phase fluide et le squelette solide constituent le couplage du mélange à l'échelle macroscopique. En caractérisant le comportement de chaque phase nous arrivons à décrire le comportement couplé du milieu couplé saturé.Nous utilisons cette approche pour modéliser des essais expérimentaux faits sur un cylindre creux pour une roche argileuse (argile de Boom). Les résultats expérimentaux montrent de façon claire que le comportement de cette roche est fortement anisotrope. Nous avons choisi de modéliser ces essais en utilisant une lois de comportement élasto-plastique pour laquelle la partie élastique est transversalement isotrope.Le problème aux conditions aux limites étudié met en évidence des déformations localisées autour du forage intérieur. Afin de décrire de façon objective le développement de ces bandes de cisaillement nous avons considéré un milieu continu local de type second gradient qui permet d'introduire une longueur interne. De ce fait nous avons pu étudier le problème d'unicité en montrant qu'un changement de la discrétisation temporelle du problème aux limites peut conduire à des solutions différentes.Dans la deuxième approche étudiée nous caractérisons la microstructure du matériau avec des grains et un réseau de canaux pour la phase fluide. À l'aide d'un processus numérique d'homogénéisation nous arrivons à calculer numériquement la contrainte du mélange et le flux massique. Cette méthode d'homogénéisation numérique a été implémentée dans un code aux éléments finis afin d'obtenir des résultats macro. Une validation de l'implentation est proposée pour des calculs en mecanique pure et en hydromécanique. / We present two different approaches to describe the hydromechanical behaviour of geomaterials. In the first approach the porous media is studied through an equivalent continuum media where the interaction between the fluide and solid phases caracterize the coupling behaviour at the macroscale.We take into account this approach to model experimental tests performed over a hollow cylinder sample of clay rock (Boom Clay), considered for nuclear waste storage. The experimental results clearly show that the mechanical behaviour of the material is strongly anisotropic. For this reason we chose an elasto-plastic model based on Drucker-Prager criterion where the elastic part is characterized by cross anisotropy.The numerical results of boundary value problem clearly show localised strains around the inner hollow section. In order to regularize the numerical problem we consider a second gradient local continuum media with an enriched kinematic where an internal lenght can be introduced making the results mesh independent. The uniqueness study is carried out showing that changing the temporal discretization of the problem leads to different solutions.In the second approach we study the hydromechanical behaviour of a porous media that it is characterised by the microstructure of the material. The microstructure taken into account is composed by elastic grains, cohesives interfaces and a network of fluid channels. Using a periodic media a numerical homogenization (square finite element method) is considered to compute mass flux, stress and density of the mixture. In this way a pure numerical constitutive law is built from the microstructure of the media. This method has been implemented into a finite element code (Lagamine, Université de Liège) to obtain results at the macroscale. A validation of this implementation is performed for a pure mechanical boundary value problem and for a hydromechanical one.

Made available in DSpace on 2014-08-20T13:32:45Z (GMT). No. of bitstreams: 1 dissertacao_vanessa_silva_da_silva.pdf: 492130 bytes, checksum: 6301288f1de4d9363b332a15a2ad0a6e (MD5) Previous issue date: 2011-11-28 / Listeria monocytogenes is an infectious microorganism causing listeriosis, a foodborne illness affecting immunocompromised, pregnant, elderly and childrens. Pathogenic to men and animals is found naturally in the environment and has the ability to multiply on adverse conditions such as high salinity and chilling temperatures. However, their detection in food is difficult because it is laborious, time consuming and expensive. Therefore comes to searching for methods to detect simple and fast. Immunological methods are very promising in this regard, but the conditions under which the organism is grown should be ideal for maximizing the expression and subsequent detection of the target antigen. Internalin A protein (InlA) of L. monocytogenes is an excellent target for detection of this pathogen in immunological tests, but the ideal conditions to enhance its expression had not yet been described. Therefore thus study analyzed the expression of InlA in two strains of L. monocytogenes serotype 4b, a clínical and other non-clínical, in non selective enrichment broths Luria-Bertani (LB), Brain Heart Infusion (BHI), Tryptic Soy Broth (TSB) and selective broths Fraser Broth (FRA), Listeria Enrichment Broth (LEB), Listeria Enrichment Broth - University of Vermont Medium (UVM), to incubation at 29 and 37 °C, through the ELISA and real time RT-PCR. All data were statistically analyzed considering a significance level of 5% (p <0.05). In the ELISA it was found that expression of InlA is strain-specific, in other words, was influenced by the origin of the strain, because the strain non-clínical of L. monocytogenes showed higher InlA expression levels than the clínical strain, and the medium used directly interfere with the expression of this antigen, and the most appropriate medium of enrichment for use in detection methods, regardless of the origin of the strain,was FRA, TSB and LEB. It was also observed that there was no significant difference in the expression of InlA when strains were grown at 29 and 37 °C. The real-time RT-PCR data showed inconclusive, since there was no statistically significant difference between the conditions analyzed, requiring thus more study. In conclusion, it was found that InlA gene expression on influenced by origin of the strain and culture media. Regardless of the origin of the strain, the preferred media for use in InlA protein detection methods are FRA, TSB and LEB / Listeria monocytogenes é um microrganismo infeccioso causador de listeriose, uma doença de origem alimentar que acomete principalmente imunocomprometidos, gestantes, idosos e crianças. Considerado patogênico tanto para homens quanto para animais, está distribuído naturalmente no ambiente e possui a capacidade de multiplicar-se sobre condições adversas, como alta salinidade e temperaturas de refrigeração. Todavia, sua detecção em alimentos é dificultada por ser trabalhosa, demorada e dispendiosa. Por isso, vem-se buscando métodos de detecção mais simples e rápidos. Os métodos imunológicos são muito promissores neste sentido, mas as condições em que o microrganismo é cultivado devem ser ideais para maximizar a expressão e consequente detecção do antígeno alvo. A proteína internalina A (InlA) de L. monocytogenes é um excelente alvo para detecção desse patógeno em testes imunológicos, porém as condições ideais para potencializar sua expressão ainda não foram descritas. Portanto, nesse trabalho analisou-se a expressão de InlA em duas cepas de L.monocytogenes sorotipo 4b, uma de origem clínica e outra não-clínica, nos caldos de enriquecimento não seletivos Luria-Bertani (LB), Brain Heart Infusion (BHI) e Tryptic Soy Broth (TSB), assim como nos caldos seletivos Fraser Broth (FRA), Listeria Enrichment Broth (LEB) e Listeria Enrichment Broth - University of Vermont Medium (UVM), a 29 e 37 °C, utilizando ELISA indireto e RT-PCR em tempo real. Todos os dados obtidos foram submetidos a análises estatísticas considerando um nível de significância de 5% (p<0,05). Através do ELISA indireto verificou-se que a expressão da InlA é cepa-especifica, ou seja, foi influenciada pela origem da cepa, pois a L. monocytogenes não-clínica apresentou maiores níveis de expressão de InlA do que a cepa clínica, e que os meios utilizados interferem diretamente na expressão desse antígeno, sendo os meios de enriquecimento mais indicados para uso em métodos de detecção, independentemente da origem da cepa, o FRA, TSB e LEB. Observou-se também que não ocorreu diferença significativa na expressão de InlA quando as cepas foram cultivadas a 29 e 37°C. O RT-PCR em tempo real apresentou dados inconclusivos, visto que não houve diferença estatística significativa entre as condições analisadas, necessitando, dessa forma, de maiores estudos.

Submitted by Erika Demachki (erikademachki@gmail.com) on 2015-01-16T19:06:55Z No. of bitstreams: 2 Tese - Adriana da Silva Santos - 2014.pdf: 3299451 bytes, checksum: 52a612ede01e4713d7dd458d61176fe1 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) / Approved for entry into archive by Erika Demachki (erikademachki@gmail.com) on 2015-01-16T19:07:03Z (GMT) No. of bitstreams: 2 Tese - Adriana da Silva Santos - 2014.pdf: 3299451 bytes, checksum: 52a612ede01e4713d7dd458d61176fe1 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) / Made available in DSpace on 2015-01-16T19:07:03Z (GMT). No. of bitstreams: 2 Tese - Adriana da Silva Santos - 2014.pdf: 3299451 bytes, checksum: 52a612ede01e4713d7dd458d61176fe1 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) Previous issue date: 2014-05-30 / Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPq / Swine leptospirosis is a worldwide anthropozoonosis caused by spirochetes of the species Leptospira interrogans, predominantly by serovars Pomona, Icterohaemorrhagiae, Taravossi, Canicola Grippotyphosa and Bratislava. Experimental infection were performed in 18 sows at 40 days of age with L. interrogans serogroup Icterohaemorrhagiae serovar Conpenhageni strain Fiocruz L1-130, and serogroup Pomona serovar Kennewicki strain Pomona From divided in groups: GI (control), GII (inoculated with serogroup Pomona) and GIII (inoculated with serogroup Icterohaemorrhagiae). Clinical course of the disease, results of serological tests and detection of bacteria by polymerase chain reaction (PCR) and bacterial isolation during the experiment, were compared between groups. Additionally, the main histological changes observed in brain, liver, lymph nodes, lung and kidney of 12 animals experimentally infected and seropositive for leptospirosis were described. In lesions suggestive of the disease the technique of silver impregnation of Warthin-Starry, was used as direct detection method. During the experimental period, all samples of the GI (control) were negative in the microscopic agglutination test, with the GII positivity exclusive to serogroup Pomona in six animals from 6 dpi, and in GIII, only to serogroup Icterohaemorrhagiae in five animals from 3 dpi. At necropsy the only change was pale kidney in 50% of GI, 83.33% of GII and 83.33% of GIII (p> 0.05). Only in seropositive pigs was found lesions suggestive of leptospirosis as focal microgliosis in the brain (8.33%), lymphoid hyperplasia in lymph nodes of the mediastinum a nd mesentery (41.66%), mononuclear interstitial pneumonia (58.33 %), multifocal mononuclear hepatitis, further acute tubular nephrosis (100%) and interstitial nephritis (91.66%). There was a strong association between serological condition and lesions of mononuclear hepatitis (p = 0.0128), mononuclear interstitial nephritis (p = 0.0004), tubular nephrosis (p <0.0001) and mononuclear interstitial pneumonia (p = 0, 0377). / A leptospirose suína é uma antropozoonose difundida mundialmente e causada por espiroquetas da espécie Leptospira interrogans, principalmente pelos sorovares Pomona, Icterohaemorrhagiae, Taravossi, Canicola, Grippotyphosa e Bratislava. Neste trabalho descreve-se a infecção experimental por L. interrogans sorogrupo Icterohaemorrhagiae sorovar Conpenhageni estirpe Fiocruz L1 -130, e sorogrupo Pomona sorovar Kennewicki estirpe Pomona From, em 18 fêmeas suínas com 40 dias de idade divididas em três grupos: GI (controle), GII (inoculados com sorogrupo Pomona) e GIII (inoculados com sorogrupo Icterohaemorrhagiae). Compararam -se entre os grupos, o curso clínico da doença, os resultados dos exames sorológicos e de detecção da bactéria durante o período experimental pelas técnicas de reação em cadeia da polimerase (PCR) e isolamento bacteriano. Foram ainda descritas as principais alterações histológicas observadas em cérebro, fígado, linfonodos, pulmão e rins de 12 animais experimentalmente infectados e soropositivos para leptospirose. Em lesões sugestivas da doença utilizou-se a técnica de impregnação pela prata de Warthin-Starry, como método de detecção direta. Durante o período experimental foram negativas na soroaglutinação microscópica todas as amostras do GI (controle), havendo no GII positividade exclusiva ao sorogrupo Pomona nos seis animais a partir do 6º dia pós-infecção (dpi), e no GIII, apenas ao sorogrupo Icterohaemorrhagiae, em cinco animais a partir do 3º dpi. Na necropsia a única alteração observada foi rim pálido em 50% do G I, 83,33% do GII e em 83,33% GIII (p>0,05). Somente nos suínos soropositivos constataram-se lesões sugestivas de leptospirose, como microgliose mononuclear focal no cérebro (8,33%), hiperplasia linfoide em linfonodos do mediastino e mesentério (41,66%), pneumonia intersticial mononuclear multifocal (58,33%), hepatite mononuclear focal (41,66%), além de nefrose tubular aguda (100%) e nefrite intersticial (91,66%). Houve forte associação entre a condição sorológica e as lesões de hepatite mononuclear (p=0,0128), nefrite intersticial mononuclear (p=0,0004), nefrose tubular (p<0,0001) e pneumonia intersticial mononuclear (p=0,0377).

Objetivo principal desta dissertação foi verificar os efeitos da temperatura de laminação na formação de martensita induzida por deformação e na sua posterior reversão da martensita para austenita no aço inoxidável austenítico AISI 304L. O estudo foi predominantemente microestrutural e para análise e caracterização foram utilizadas as técnicas de microscopia óptica, microscopia eletrônica de varredura, difração de raios X, medidas de dureza Vickers e medidas de fases ferromagnéticas por ferritoscopia. As amostras foram inicialmente solubilizadas a 1100 ºC por uma hora, visando a dissolução de uma pequena quantidade residual de ferrita encontrada nas amostras na condição como recebida, depois laminadas em diferentes temperaturas, determinando-se curvas de endurecimento por deformação e de formação de martensita induzida por deformação em função do grau de deformação. Em seguida, foram realizados pré-recozimentos a 600 ºC, favorecendo apenas a reversão da martensita para austenita, de maneira que não ocorresse a recristalização. A quantidade e a temperatura de deformação apresentaram forte influência na quantidade de martensita formada, no endurecimento por deformação e na cinética de amolecimento durante o recozimento. Os pré-tratamentos realizados a 600 ºC causaram acentuada reversão da martensita, algum amolecimento e pequeno efeito no tamanho de grão recristalizado durante o posterior recozimento a 600 ºC. / The main objective of the present dissertation was to verify the effects of the rolling temperature on the formation of strain induced martensite and in its subsequent martensite reversion to austenite in a AISI 304L stainless steel. The study was predominantly microstructural and, for the analysis and characterization, several techniques have been used, namely optical microscopy, scanning electron microscopy, X-ray diffraction, Vickers hardness measurements and magnetic phase measurements, using the ferritoscope. The samples were initially solution annealed at 1100 ºC for one hour, aiming at the dissolution of a small quantity of the residual -ferrite found in the samples in the as-received condition; then rolling was performed at different temperatures, evaluating strain hardening and the strain induced martensite as a function of strain. Following, pre-annealing treatments at 600 ºC have been performed, favoring only the martensite to austenite reversion, in a way that no recrystallization would occur. Strain and temperature had a strong influence on the amount of formed martensite, on the strain hardening and on the softening kinetics during annealing. The pre-annealing treatments at 600 ºC caused an accentuated effect on the martensite reversion, some softening and a small effect on the recrystallized grain size during the subsequent annealing at 600 ºC.

L'Alliage 600 (Ni-15%Cr-10%Fe) est réputé sensible à la Corrosion Sous Contrainte (CSC) en milieu primaire des Réacteurs à Eau Pressurisée (REP). Des études récentes ont montré que la diffusion du chrome était une étape limitante dans la compréhension des mécanismes de CSC. En particulier, le mécanisme d'oxydation interne contrôlé par le taux de défauts local. Dans ce contexte, l'objectif de cette thèse a été de produire des données expérimentales concernant la cinétique de diffusion du chrome en fonction de différents états métallurgiques. Les coefficients de diffusion du chrome ont été mesurés par Spectrométrie de Masse des Ions Secondaires (SIMS) et Spectrométrie à Décharge Luminescente (SDL) en volume et aux joints de grains dans la gamme de température 678 K-1060 K sur des échantillons en nickel pur et d'Alliage 600 monocristallin ou polycristallin. Une partie de cette thèse s'est focalisée sur l'effet de la déformation plastique sur la cinétique de diffusion du chrome pour des échantillons en nickel monocristallin (orienté <101>). Les expériences de diffusion ont été réalisées sur des échantillons non déformés, pré-écrouis à 4% et 20% de déformation plastique et sur des essais in-situ de diffusion en fluage. Les résultats ont montré que les coefficients de diffusion mesurés sur les éprouvettes déformées plastiquement sous charge constante sont supérieurs de six ordres de grandeur à ceux obtenus à l'état non déformé ou pré-écroui. L'accélération de la cinétique de diffusion peut être attribuée à un couplage entre la mobilité des dislocations et la vitesse de déformation plastique. / Alloy 600 (Ni-15%Cr-10%Fe) is known to be susceptible to Stress Corrosion Cracking (SCC) in primary water of Pressurized Water Reactors (PWR). Recent studies have shown that chromium diffusion is a controlling rate step in the comprehension of SCC mechanism. In order to improve the understanding and the modelling of SCC of Alloy 600 in PWR primary medium the aim of this study was to collect data on kinetics diffusion of chromium. Volume and grain boundary diffusion of chromium in pure nickel and Alloy 600 (mono and poly-crystals) has been measured in the temperature range 678 K to 1060 K by using Secondary Ions Mass Spectroscopy (SIMS) and Glow Discharge-Optical Spectrometry (GD-OES) techniques. A particular emphasis has been dedicated to the influence of plastic deformation on chromium diffusion in nickel single crystals (orientated <101>) for different metallurgical states. The experimental tests were carried out in order to compare the chromium diffusion coefficients in free lattice (not deformed), in pre-hardening specimens (4% and 20%) and in dynamic deformed tensile specimens at 773 K. It has been found that chromium diffusivity measured in dynamic plastic deformed creep specimens were six orders of magnitude greater than those obtained in not deformed or pre-hardening specimens. The enhancement of chromium diffusivity can be attributed to the presence of moving dislocations generated during plastic deformation.

Ce travail s’inscrit dans le cadre d’un partenariat international Airbus Safran Launchers ", " Ecole Centrale de Lyon " et " Ecole Nationale d’Ingénieurs de Tunis ". Les composés élastomériques sont largement utilisés dans l’industrie pour leurs déformabilité et leurs capacités d’amortissement. Soumis aux combinaisons complexes de fabrication et de charges de service, les élastomères montrent la capacité de subir des conditions de chargement sévères et le cas de pré-déformation statique superposée par une excitation dynamique de petite amplitude est couramment utilisé pour des applications industrielles, par exemple des pneus, des amortisseurs, applications aérospatiales ... Pour concevoir efficacement ces composés industriels, il est primordial de prédire la réponse des produits à travers des processus de modélisation simples qui ont multiplié les méthodes d’analyse: expérimentale, théorique et numérique. Dans ce contexte, le présent travail se concentre sur la conception et l’analyse des propriétés dynamiques d’un dispositif élastomère autour d’une configuration préformée. À cette fin, trois mélanges de caoutchouc ont été expérimentés: Caoutchouc naturel (NR), Bromobutyl (BIIR) et un mélange des deux (NR / BIIR). Une discussion est faite avec préoccupation pour la mise en place expérimentale ainsi que les procédures utilisées pour des essais expérimentaux efficaces. Avec ces conclusions, nous avons fait un jugement sur les capacités de prévision, dans les domaines temporels et fréquentiels, de certains modèles hyper-visco-élastique à base d’intégrale unique sous l’hypothèse de séparabilité des effets temps-déformation. Les modèles considérés sont largement utilisés pour les applications d’ingénierie. Ce travail est suivi d’une application sur un composant industriel. Dans le cadre de cette thèse, le code de calcul d’éléments finis ABAQUS 6.14 a été utilisé pour étudier les propriétés dynamiques de cette structure. Une méthodologie d’analyse a été présentée pour identifier soigneusement l’ensemble des paramètres dans le but de satisfaire certaines exigences industrielles, principalement des capacités de masse, de rigidité et d’amortissement. / This work is conducted as international collaboration with " Airbus Safran Launchers ", " Ecole Centrale de Lyon " and " National Engineering School of Tunis ". Elastomeric compounds are widely used in industry for their high deformability and damping capabilities. Subjected to complex combinations of manufacturing and service loadings, elastomers show the fact to undergo severe loading conditions and the load case of large static predeformation superimposed by small amplitude dynamic excitation is commonly encountred for industrial applications e.g tires, shock-absorbing bushes, construction industry, aerospace applications... To design such industrial compounds efficiently, it is of major importance to predict the response of the products through simple modeling processes which have multiplied analysis methods: experimental, theoretical and numerical. Within this context, the present work focuses on design and analysis of dynamic properties of an elastomeric device at a predeformed configuration. To this end, three rubber mixtures have been experimentally investigated: Natural Rubber (NR), Bromobutyl (BIIR) and a mixture of both (NR/BIIR). A discussion is made with concern to experimental set-up as well as the used procedures for an efficient specimens testings. Within these findings, we made judgement on the predictive capabilities, in time and frequency domains, of some single integral based hyper-visco-elastic models under time-strain seperability assumption. The considered models are widely used for engineering applications and focus have been made on the Simo model implemented in finite element commercial software Abaqus. This work is followed by an application on an industrial component. In the framework of this thesis, the finite element calculation code ABAQUS 6.14 was used to investigate the dynamic properties of such structure. An analysis methodology have been presented to carefully identify the set of parameters with the objective of satisfaction of some industrial requirements mainly mass, stiffness and damping capabilities.

L'objectif de cette thèse est d'étudier expérimentalement les phénomènes de vieillissement dus à la diffusion des atomes en solution dans les alliages d’aluminium et les instabilités qui leur sont associées comme le phénomène Portevin-Le Châtelier ou les bandes de Lüders et de proposer une modélisation de ces phénomènes dans le cadre de la thermodynamique des processus irréversibles. Une étude expérimentale détaillée est alors entreprise sur les alliages d’aluminium AA5083-H116 et AA5182-O. Le comportement du premier présente l’effet PLC de façon prononcée et les deux types d’instabilités sont observées simultanément pour le second. La corrélation d'images numériques et la thermographie infrarouge sont essentiellement employées pour détecter et caractériser les aspects spatiotemporels des instabilités observées. La déformation non homogène due à l’apparition et la propagation de bandes de localisation est mise en évidence. Ces bandes de déformation sont visualisées, permettant à leurs diverses caractéristiques (vitesse, orientation, largeur, vitesse de déformation à l'intérieur des bandes, augmentation de la température à l'intérieur des bandes) d'être mesurées sur des éprouvettes lisses (plates, cylindriques ou prismatiques). Dans le cas des éprouvettes plates, l’effet des épaisseurs de l’éprouvette a aussi été examiné. Les caractéristiques des bandes sont aussi analysées sur d’autres géométries d’éprouvette (entaillées avec divers types d’entailles) à des vitesses de déformation différentes pour exhiber leur morphologie en présence de chargements multiaxiaux. Des simulations non linéaires et tridimensionnelles ont été effectuées en utilisant le modèle de McCormick pour montrer comment la prise en compte des phénomènes de vieillissement, même partielle, permet de décrire les hétérogénéités et le mouvement des bandes de déformation ainsi que de prévoir leurs différentes caractéristiques. Enfin, en se basant sur les mécanismes physiques à la base des phénomènes de vieillissement et en soulignant les limites du modèle de McCormick, un modèle élasto-viscoplastique prenant en considération les phénomènes de vieillissement est proposé dans le cadre de la thermodynamique des processus irréversibles. / The objective of this thesis is to study experimentally the ageing phenomena due to the atoms diffusion in solid solutions in aluminium alloys and associated instabilities as the Portevin-Le Châtelier phenomenon or the Lüders bands and to propose a model of these phenomena within the framework of thermodynamics of irreversible processes. Digital Image Correlation (DIC) and Digital Infrared Thermography (DIT) are essentially employed to capture and characterize the spatio-temporal aspects of these instabilities. Inhomogeneous deformation, due to the appearance and the propagation of various localization bands are observed. These deformation bands are visualized, allowing their various characteristics (velocity, orientation, width, strain rate inside the bands, temperature increase inside the bands) to be measured on smooth specimens (flat, cylindrical or prismatic). In the case of flat test, the effect of the specimen thickness was also examined. The band characteristics are also analyzed on other specimen geometries (notched with various kinds of notches) at different strain rates to exhibit their morphology in the presence of multiaxial loadings. Some nonlinear and three-dimensional simulations were carried out with McCormick model to show how the inclusions of ageing phenomena, even partial, makes possible to describe heterogeneities and the deformation bands but also reproducing qualitatively their various characteristics. Finally, based on the physical mechanisms of aging phenomena and underlying the limitations of the McCormick model, an elasto-viscoplastic model taking into account the aging phenomena is proposed in the framework of thermodynamics of irreversible processes.

Ce travail présente une caractérisation expérimentale du comportement mécanique et de la rupture par localisation de la déformation dans un grès des Vosges. L'évolution temporelle de la localisation a été caractérisée par des mesures de champs. Une nouvelle cellule triaxiale vraie a été développée au Laboratoire 3SR (Grenoble), qui permet une visualisation des échantillons sous chargement pour réaliser de la corrélation d'image numérique (CIN). Les essais ont été réalisés par compression en déformation plane (confinement de 20 à 50 MPa). La transition d'une déformation diffuse à localisée a été finement étudiée. Une analyse comparative a été ensuite effectuée entre les mesures de champs et la microstructure à l'échelle des grains observée par microscope (MEB). Enfin, une étude théorique basée sur une analyse en bifurcation a été menée pour comparer observations des bandes de cisaillement et prédiction sur la localisation de la déformation. / This work aims an experimental characterization of the mechanical behaviour and failure by strain localization on a Vosges sandstone. The time evolution of strain localization has been characterized by full-field measurements. A new true-triaxial apparatus has been developed at Laboratoire 3SR (Grenoble), which enables the observation of the specimens during mechanical loading for application of digital image correlation (DIC). Tests have been performed in plane strain compression (confining pressure from 20 to 50 MPa). The transition from diffuse to localised deformation regimes has been extensively studied. Then, a comparative analysis has been done between the strain fields (DIC) and microscope (SEM) observations to determine how closely the DIC fields are related to deformation mechanisms detected at the grain scale. Finally, a theoretical bifurcation analysis is presented to compare the experimental observations of shear bands with strain localization prediction.