Made available in DSpace on 2017-07-21T19:25:52Z (GMT). No. of bitstreams: 0 Previous issue date: 2016-03-10 / This work aimed at study the correlation of variables in a plasma immersion ion implantation (PIII) system, as well as their synergistic combination for the nitriding of the UNS S32750 super duplex stainless steel ( SD 2507). The research comprised two phases, as follows. (i) Study of the system. The interconnection of variables, namely voltage (V), pulse width (L), frequency (f) and current (I), were systematically analyzed with respect to the cathode heating. A mathematical formulation was proposed for the ion average energy and the substrate temperature, which took into consideration the energy conservation in the system, and the basic theories for plasma and sheaths and the ion interaction with matter. Hereafter, such model is thought to be experimentally demonstrated, allowing inferring the actual PIII fraction of energy that is converted to heat. (ii) N-PIII of the SD. Mirror-like samples were nitrided under different V, f and L combinations, leading to the temperatures 295, 325, 355 and 400 oC. The surface characterization methods were the optical, field emission electron, and atomic force microscopies, X-ray diffraction, energy dispersive X-ray spectroscopy, backscattered electron diffraction, and instrumented indentation. The austenite and ferrite fraction in the as received material amounted to 43,7 % and 56,3 %, respectively. After nitriding, the modified layers were 0,5-1,5 m thick. Up to 355 ºC, the expanded phase N was produced in originally austenite grains, whereas Fe2-3N e Fe4N precipitates were formed in ferrite grains. The hardness profiles were similar among different temperatures and between the two phases in the same sample. However, in ferritic regions, the mechanism for plastic deformation changed from ductile to brittle. In the 400 ºC treatments, only N was formed. Finally, a correlation for the production of the expanded phase in PIII and the mean pulse energy Ei was attained, given by and . Where IN and I are the integrated intensities of diffraction peaks for austenite and expanded austenite, respectively. / O objetivo deste trabalho foi estudar o comportamento de um sistema de implantação iônica por imersão em plasma (PIII: “plasma immersion ion implantation”), em função de suas variáveis, bem como a influência destas na nitretação de superfícies do aço super duplex UNS S32750 (ou SD 2507). O trabalho foi dividido em dois momentos, como segue. (i) Estudo do sistema. O comportamento das variáveis associadas à implantação iônica, especificamente tensão (V), largura de pulsos (L), frequência (f) e corrente (I), foi sistematicamente analisado com relação ao aquecimento do cátodo. Com base na conservação de energia, física de plasmas e bainhas catódicas e interação de íons com a matéria, propôs-se uma formulação matemática relacionado a energia média dos íons à temperatura do substrato, a qual poderá, futuramente, ser posta à prova experimental, mensurando-se a fração de energia que é, de fato, transformada em calor. (ii) Nitretação por PIII do SD. Amostras com superfície especular foram nitretadas sob diferentes combinações de V, f e L, em temperaturas de 295, 325, 355 e 400 oC. As superfícies foram caracterizadas por métodos de microscopia (ótica, eletrônica com efeito de campo, de força atômica), difração de raios X, espectroscopia de raios X por energia dispersiva, difração de elétrons retroespalhados, e indentação instrumentada. O SD apresenta estrutura cristalina de austenita e ferrita na proporção de 43,7/56,3. A nitretação produziu camadas modificadas com espessura de 0,5 a 1,5 m. Observou-se, nos tratamentos até 355 ºC, a formação da fase expandida N nos grãos que originalmente eram austenita, e de precipitados de nitretos -Fe2-3N e -Fe4N em grãos de ferrita. Embora não houve diferenças significativas nos perfis de dureza, tanto entre as temperaturas quanto entre as fases em uma mesma amostra, o mecanismo de deformação plástica nas regiões ferríticas transitou de dúctil para frágil. Nas nitretações em 400 ºC, houve apenas a formação de N. Finalmente, determinou-se que a obtenção da fase expandida por PIII no SD se relaciona com a energia média por pulso Ei por e . Onde I e I são as intensidades integradas dos picos de difração da austenita expandida e da austenita, respectivamente.

Made available in DSpace on 2017-07-21T19:26:00Z (GMT). No. of bitstreams: 1 Andre Assmann.pdf: 3125745 bytes, checksum: 38854736eae2fcc4e8c2c21a2668f387 (MD5) Previous issue date: 2011-04-27 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / In the present work showing the results on mechanical and tribological properties of duplex stainless steel LDX2101 nitriding by Ion Implantation (II), Plasma Immersion Ion Implantation (PI3) and Glow Discharge (GD). Nitrogen ion implantation was performed at room temperature and 350 C. The nitrogen fluencies were combined to obtain an atomic nitrogen concentration of 27 %. The PI3 was carried out with temperatures of 300 and 350 C working in N2 atmosphere during 3 hours. For GD, the working conditions were gas mixture N2/H2 (in the ratio 80%/20%, 60%/40% and 20%/80%) and N2/CH4 (in the ratio 98%/02%) during 3 hours at temperatures of 300, 350 and 380 C. Structural characterizations of the modified layers were performed by X-Ray Diffraction (XRD) with Bragg-Brentano geometry. Hardness was obtained by instrumented indentation using Oliver and Pharr method’s with Berkovich indenter. Tribological tests were evaluated by reciprocating sliding with a WC(Co) sphere (counter body). XRD patterns for II samples showing only the formation of γN, however, samples treated by GD and PI3 showed the formation of γ’Fe4N and Fe2+XN, over there γN, as a function of the working temperature and nitriding atmosphere. After the nitriding hardness values between 8 and 20 GPa in comparison to 3 GPa of the bulk was obtained. The hardness profile of samples treated by GD at 350 and 380 C exhibit plateaulike for values of hardness between 13 and 20 GPa, indicate the formation of a thicker nitrited layer. The friction coefficient for II samples showed a strong adhesive wear. PI3 samples exhibit long running-in regimes compared to II and untreated samples. GD samples showing a predominant abrasive wear because ploughing of surface for asperities and wear particles formed between the surface and counter body. The significant decrease in the wear was observed in all GD samples, with a reduction of one order of magnitude compared to untreated sample. / No presente trabalho, são apresentados os resultados sobre as propriedades mecânicas e tribológicas do aço inoxidável duplex LDX 2101 nitretado por Implantação Iônica (II), Implantação Iônica por Imersão em Plasma (3IP) e Descarga Luminosa (DL). A Implantação Iônica de nitrogênio foi realizada em temperatura ambiente e em 350 C. As fluências utilizadas foram combinadas para obter uma concentração de átomos de nitrogênio de 27 %. A nitretação 3IP, foi realizada nas temperaturas de 300 e 350 C em atmosfera de N2 durante 3 horas. Para o tratamento por DL as condições de tratamento foram em diferentes atmosferas de N2/H2 (nas proporções de 80%/20%, 60%/40% e 20%/80%) e N2/CH4 (na proporção de 98%/02%) durante 3 horas nas temperaturas de 300, 350 e 380 C. A caracterização estrutural das camadas modificadas foi obtida através de Difração de Raios-X (DRX) com geometria Bragg-Brentano. Os perfis de dureza foram obtidos por indentação instrumentada usando o método de Oliver e Pharr com indentador do tipo Berkovich. Testes tribológicos foram realizados com tribômetro do tipo pino sobre disco em movimento recíproco com uma esfera de WC(Co) de contra corpo. Os padrões de DRX para amostras tratadas por II apresentaram apenas a formação de γN, contudo, as amostras tratadas por DL e 3IP apresentaram a formação de γ’-Fe4N e Fe2+XN, além de γN, como função da temperatura de tratamento e da atmosfera de nitretação. Após as nitretações durezas entre 8 e 20 GPa em comparação a 3 GPa para o substrato foram obtidas. Perfis de dureza para amostras tratadas por DL em 350 e 380 C exibiram valores entre 13 e 20 GPa em forma de platô, indicando a formação de uma espessa camada nitretada. O coeficiente de atrito para as amostras tratadas por II apresentaram um forte desgaste adesivo. Amostras tratadas por 3IP exibiram longos regimes de acomodação comparados as amostras tratadas por II e a amostra referência. Amostras tratadas por DL apresentaram um predominante desgaste abrasivo devido à deformação plástica da superfície causada pelas asperidades e pelas partículas de desgaste formadas entre a superfície e o contra corpo. Uma significante diminuição no desgaste foi observada em todas as amostras tratadas por DL, com uma redução de uma ordem de grandeza quando comparado a amostra sem tratamento.

Made available in DSpace on 2014-12-17T14:07:06Z (GMT). No. of bitstreams: 1 PolianaRFS_DISSERT.pdf: 3998823 bytes, checksum: e0480a4a5d6b04450e748434898535a9 (MD5) Previous issue date: 2013-03-01 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The technique of plasma nitriding by the cathode cage mainly stands out for its ability to produce uniform layers, even on parts with complex geometries. In this study, it was investigated the efficiency of this technique for obtaining duplex surface, when used, simultaneously, to nitriding treatment and thin film deposition at temperatures below 500?C. For this, were used samples of AISI 41 0 Martensitic Stainless Steel and performed plasma treatment, combining nitriding and deposition of thin films of Ti and/or TiN in a plasma atmosphere containing N2-H2. It was used a cathodic cage of titanium pure grade II, cylindrical with 70 mm diameter and 34 mm height. Samples were treated at temperature 420?C for 2 and 12 hours in different working pressures. Optical Microscopy (OM), Scanning Electron Microscopy (SEM) with micro-analysis by Energy Dispersive Spectroscopy (EDS), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and analysis of Vickers Microhardness were used to investigate coating properties such as homogeneity and surface topography, chemical composition, layer thickness, crystalline phase, roughness and surface microhardness. The results showed there is a direct proportionality between the presence of H2 in plasma atmosphere and the quantity of titanium in surface chemical composition. It was also observed that the plasma treatment at lowpressure is more effective in formation of TiN thin film / A t?cnica de nitreta??o a plasma por gaiola cat?dica vem se destacando, principalmente, pela sua capacidade de produzir camadas uniformes mesmo em pe?as com geometria complexa. Neste trabalho, investigou-se a efici?ncia desta t?cnica para obten??o de superf?cie duplex, quando utilizada, simultaneamente, para tratamento de nitreta??o e deposi??o de filmes finos em temperaturas inferiores a 500?C. Para tal, foram utilizadas amostras do a?o inoxid?vel martens?tico AISI 410 e realizados tratamentos a plasma, combinando a nitreta??o e deposi??o de filmes finos de Ti e/ou TiN, em uma atmosfera contendo N2-H2. Foi utilizada uma gaiola cat?dica de tit?nio puro grau II em forma cil?ndrica, com 70 mm de di?metro e 34 mm de altura. As amostras foram tratadas numa temperatura de 420?C, com dura??o de 2 e 12 horas e em diferentes press?es de trabalho. Microscopia ?ptica (MO), Microscopia Eletr?nica de Varredura (MEV) com microan?lise por Espectroscopia de Energia Dispersiva (EDS), Difra??o de Raios-X (DRX), Microscopia de For?a At?mica (MFA) e ensaio de Microdureza Vickers foram empregados para investigar as propriedades do revestimento, tais como homogeneidade e topografia superficial, composi??o qu?mica, espessura da camada, fases cristalinas, rugosidade e microdureza superficial. Os resultados mostraram existir uma proporcionalidade direta entre a presen?a de H2 na atmosfera do plasma e a quantidade do elemento qu?mico tit?nio na composi??o qu?mica superficial. Observou-se, tamb?m, que o tratamento a plasma em baixa press?o ? mais eficaz na forma??o do filme fino de nitreto de tit?nio

Les aciers inoxydables duplex présentent une combinaison intéressante entre des propriétés mécaniques élevées, une faible conductivité thermique et un coût relativement faible. Ils sont couramment employés dans le domaine du bâtiment comme rond à béton, application qui requière notamment une résistance élevée (Rm > 950 MPa) et une ductilité importante (A% > 15). Cette thèse a pour objectif d’améliorer le compromis résistance / allongement, en développant de nouvelles nuances duplex présentant une transformation martensitique induite par la plasticité (effet TRIP) aux caractéristiques contrôlées. L’optimisation de ce compromis a nécessité en particulier une compréhension détaillée des mécanismes de transformation et de déformation plastique associés à chaque phase : la ferrite (BCC), l’austénite (FCC) et la martensite (BCC).L’influence de la transformation martensitique sur le comportement mécanique est étudiée pour quatre alliages duplex de stabilité variable de la phase austénitique en fonction de leur composition chimique. L’influence d’une microstructure multiphasée sur la cinétique de transformation est déterminée grâce à l’élaboration de trois nuances modèles représentant respectivement une nuance duplex et es deux compositions représentatives de ses constituants austénite et ferrite. L’utilisation de plusieurs techniques de caractérisation à différentes échelles a permis de décrire à la fois les mécanismes de transformation de phase et leur cinétique en fonction de la déformation, donnant ainsi accès à leur influence sur le comportement mécanique. L’étude des champs cinématiques a mis en évidence l’impact de la phase martensitique sur la répartition des déformations dans la microstructure multi-phasée. Finalement l’utilisation d’un modèle mécanique prenant en compte explicitement la transformation martensitique a permis de reproduire le comportement mécanique d’un alliage duplex. / Duplex stainless steels offer an attractive combination of high mechanical properties, low thermalconductivity and a relatively low cost. They are increasingly used as structural materials such as inthe construction sector as concrete reinforcement bars, where both high strength (Rm > 900 MPa)and high elongation to failure (A% > 15 %) are required. This thesis aims at improving the strength/ elongation compromise by developing new duplex stainless steel compositions experiencing a wellcontrolledmartensitic transformation induced by plasticity (TRIP effect). The optimisation of thiscompromise has required a good understanding of the transformation mechanisms and of plasticdeformation associated with each phase : ferrite (BCC), austenite (FCC) and martensite (BCC).The influence of martensitic transformation on mechanical behavior has been studied in four duplexgrades of variable austenite stability as a function of their chemical composition. The influence ofmultiphase microstructure on martensitic transformation kinetics has been determined by makingthree alloys respectively representative of a duplex grade and its two constituents (austenite andferrite). Using multiple characterization techniques at different scales has allowed determiningboth the transformation mechanisms and its kinetics as a function of strain, giving thus accessto the influence of transformation on the mechanical behavior. The study of kinematic fields hashighlighted the impact of the martensitic phase on the distribution of deformations. Finally, theuse of a mechanical model taking explicitly into account the phase transformation has allowed theduplication of the mechanical behavior of a duplex stainless steel.

Le développement d’une troisième génération d’aciers Fe-Mn-Al-C à structure duplex, pour des teneurs en Mn et Al inférieures à 8 %mass, pourrait être une réponse prometteuse aux objectifs d’allègement de 20% des véhicules automobiles, tout en garantissant des propriétés de haute résistance mécanique et haute formabilité.Le choix des nuances et l’optimisation des conditions d’élaboration nécessitent de prévoir en particulier les compositions et proportions des phases existantes en fonction de la route métallurgique. Une base de données thermodynamiques fiable et précise est donc requise. Cependant les données de la littérature sur le système quaternaire Fe-Mn-Al-C, dans les domaines de composition envisagés, sont limitées.Ce mémoire est consacré à l’établissement des équilibres de phases ferrite-α, austénite-γ et carbure-κ (Fe,Mn)3AlC entre 700 et 1000°C par une approche couplée d’expériences ciblées et de modélisation thermodynamique. Pour appuyer l’évolution expérimentale des fractions de phases et des compositions, une modélisation cinétique (DICTRA) est proposée. La cinétique de formation de l’austénite en fonction de la composition de l’alliage et de la température de maintien dans le domaine intercritique a été caractérisée. Les phases en équilibre, caractérisées par DRX, MEB, microsonde, sont représentées sous forme de conodes α/γ, γ/κ, α/γ/κ, ce qui permet de définir les domaines de stabilité de l’austénite et du carbure κ. Ces données expérimentales sont utilisées pour affiner la description thermodynamique du système quaternaire mais il est nécessaire de réviser la modélisation du carbure κ. / A third generation of Fe-Mn-Al-C steels with a duplex structure, for Mn and Al contents less than 8%mass, could be a promising response to the 20% weight lightening of automotive vehicles, by keeping a high strength and a high formability.The knowledge of the corresponding quaternary phase diagram serves as a roadmap for the choice of compositions and the optimization of elaboration conditions. A reliable and precise thermodynamic database is therefore required. However, the literature data on the Fe-Mn-Al-C quaternary system in the targeted domains are limited.This study is devoted to the establishment of phase equilibria involving ferrite-α, austenite-γ and carbide-κ (Fe,Mn)3AlC between 700 and 1000°C by a coupled approach of experiments and thermodynamic modeling. A kinetic model (DICTRA) is proposed to support the experimental evolution of phase fraction and composition. The kinetics of austenite formation as a function of the alloy composition and of the maintaining temperature in the intercritical domain have been calculated. The phases in equilibrium, characterized by XRD, SEM, EPMA, are represented as α/γ, γ/κ, α/γ/κ tie-lines in order to specify the stability fields of γ and κ. These data are used to refine the thermodynamic description of the quaternary system but it is necessary to revise the modeling of κ carbide.

γ-TiAl based alloys have attracted considerable research interest in the past few decades and have gained niche high temperature applications in aero-engines and automobiles. As high temperature structural materials, these alloys require stable microstructures. This thesis aims at addressing knowledge gaps in the understanding of microstructural stability in two technologically important γ-TiAl based alloys in different microstructures, viz. fully lamellar (FL) and duplex. Creep and exposure tests were complemented with a variety of microstructural characterization tools (SEM, EBSD, TEM, XRD). Density functional theory based calculations were also performed to further the understanding of stability of phases. In the first part of the thesis, microstructural stability of a FL microstructure was studied under creep and high temperature exposure conditions. An aim of these studies was to probe the effect of stress orientation with respect to lamellar plates on microstructural changes during primary creep. It was observed that retention of excess α2 resulted in an unstable microstructure and so under stress and temperature, excess α2 was lost. However, depending on stress orientation, the sequence of precipitates formed was different. In particular, for certain stress orientations, the formation of the non-equilibrium C14 phase was observed. The stress dependence of microstructural evolution was found to be stem from internal stresses due to lattice misfit and elastic moduli mismatch between α2 and γ. In the second part of this thesis, microstructural stability of a duplex alloy was probed, with an emphasis on understanding mechanisms that lead to tertiary creep. The as-extruded microstructure consisted of bands of equiaxed grains and lamellar grains. During creep, loss of lamellar grains was observed and this was attended by kinking of laths and formation of dynamically recrystallized equiaxed grains. Significant dislocation activity was seen in both lamellar and equiaxed grains at all stages of creep. Initially, dislocation activity leads to strengthening and primary creep behavior, but at later stages, it triggers dynamic recrystallization. Dynamic recrystallization was found to be the rate controlling creep mechanism. Accelerating creep behavior was due to strain localization during the constant load tensile test resulting from microstructural instabilities such as kinking.

Le medium sans fil est une ressource partagée et limitée. Les normes sans fil actuelles partagent toujours le principe de partage du medium Half-Duplex: la transmission et la réception de signaux sont effectuées dans deux intervalles de temps distincts ou deux bandes de fréquences différentes. En outre, l'émetteur-récepteur ne peut émettre et recevoir qu’un signal à la fois. Cette thèse suit une autre approche: au lieu de partager le support avec le principe de Half-Duplex, toute la bande de fréquence autorisée est partagé pour la transmission et la réception simultanée, approche qui est appelée Full-Duplex. Dès lors, on peut concevoir une architecture d'un émetteur-récepteur radio flexible à large bande pour traiter deux types de signaux différents à la fois. Pour approcher cet objectif, nous utilisons une méthode de suppression active analogique de l’auto-interférence (AARFSIC) et l'annulation active numérique d'auto interférence dans le domaine temporel (ADSICT) pour annuler la forte auto-interférence (SI) induite par le principe Full-Duplex. Basé sur la radio Full-Duplex, nous proposons un système flexible Dual-Band (FDDB) émetteur-récepteur radio OFDM-Full Duplex en la combinant avec un front-end RF double bande. S'appuyant sur ces principes, nous exposons trois contributions principales: Nous présentons une technique d’annulation analogique de l’auto-interférence (ASIC), qui peut annuler complètement l’auto-interférence à trajet direct ou multi-trajets, basée sur la combinaison des méthodes AARFSIC et DSICT. Ensuite, nous présentons la conception et l'évaluation d'une radio OFDM Full-Duplex, y compris l'analyse et la qualification de l'impact du bruit thermique et du bruit de phase sur les performances du système. Enfin, nous développons une radio dual-bande FDDB OFDM qui peut fonctionner sur deux fragments de spectre séparés. Afin d'éliminer l'impact du déséquilibre I/Q sur la radio FDDB, une méthode d’estimation des déséquilibres I/Q et de compensation, simple mais efficace, est présentée. La simulation au niveau système menée avec ADS et Matlab montre que cette méthode peut effectivement compenser des déséquilibres I/Q aussi bien élevés que faibles. / The wireless medium is a shared and limited resource. Current wireless standards always share the medium with Half-Duplex principle: the transmission and reception of signals are done in two separate time slots or two different frequency bands. Besides, the transceiver can only transmit and receive one signal at a time. This dissertation takes an alternate approach: Instead of sharing the medium with Half-Duplex principle, the entire licensed frequency band is shared for simultaneous transmission and reception, which we call Full-Duplex. Besides, the design concept for a wideband flexible radio transceiver can process two different types of signals at a time. To approach this goal, we use an active analog radio frequency self-interference cancellation (AARFSIC) method or a combination scheme of the AARFSIC and active digital self interference cancellation in time domain (ADSICT) to cancel the strong self-interference (SI) induced by the Full-Duplex principle. Based on the Full-Duplex radio, we propose a flexible Full-Duplex Dual-Band (FDDB) OFDM radio transceiver by combining it with a Dual-Band RF front-end. Building on these, we make three main contributions: We present an active self-interference cancellation (ASIC) scheme, which can cancel both the strong one-path and multi-path SI completely, based on the combination of the AARFSIC and DSICT. Next, we introduce the design and evaluation of a Full-Duplex OFDM radio, including the analysis and qualification of the impact of the thermal noise and phase noise on the system performance. Finally, we develop a FDDB OFDM radio that can work on two separate spectrum fragments. In order to eliminate the impact of the I/Q imbalance on the FDDB radio, a simple but practical digital I/Q imbalance estimation and compensation method is presented. The system level simulation conducted with ADS and Matlab software shows that this method can effectively compensate both high and low I/Q imbalance.

Les aciers inoxydables duplex (DSS) sont caractérisés par une structure biphasée comprenant un mélange de ferrite et d’austénite. La proportion entre les deux phases est d'habitude environ 50 %. Ils sont de plus en plus employés dans les industries chimiques, pétrochimiques, nucléaires, marines et de papier, principalement en raison de leurs excellentes propriétés mécaniques couplées à une bonne résistance à la corrosion par piqûre (basse teneur en nickel et molybdène). L’austénite ayant une composition chimique différente de celle de la ferrite, un film hétérogène se forme à la surface des aciers inoxydable duplex. Par ailleurs, les deux phases métalliques ayant des propriétés mécaniques différentes, un champ de contrainte hétérogène est généré dans les grains. Sous certaines conditions, l’existence de gradients de contraintes peut conduire à des hétérogénéités du film passif. Dans ce travail , on étudie l’effet des éléments d’alliages sur les propriétés physico-chimiques du film passif et le comportement en corrosion par piqures avant et après vieillissement en milieu chlorurés, pour une surface de référence respectant certains critères à savoir une surface lisse exempt de tout défauts (pas de couche écrouie, rugosité faible..). Les propriétés physico- chimiques du film sont étudiés à l’aide des analyses Auger et XPS à l’échelle locale et globale. Le comportement en corrosion des alliages duplex a été ensuite déterminé à partir d’essais TCP (détermination de la température critique de piqûration). Les résultats avant vieillissement ont montré que le film passif est homogène à l’échelle macroscopique et que l’amorçage des piqûres semblent être liée à la taille des grains et à la texture cristallographique décrit par le GOS. Après vieillissement de longue durée en milieu représentatif, les analyses de surface montrent un renforcement de la passivité par un épaississement du film passif, une augmentation significative du rapport Cr/Fe ce qui ont pour effet d’améliorer le comportement en corrosion par piqures des alliages. Des critères métallurgiques ont été proposés pour expliquer l’amorçage de piqûres pour ces alliages. / Duplex stainless steels (DSS) are characterized by a two-phase structure comprising a mixture of ferrite and austenite. The proportion between the two phases is usually about 50%. They are increasingly used in the chemical, petrochemical, nuclear, marine and paper, mainly because of their excellent mechanical properties coupled with good resistance to pitting corrosion (low grade nickel and molybdenum). The austenite having a different chemical composition than the ferrite, a heterogeneous film is formed on the surface of duplex stainless steels. Furthermore, the two metallic phases having different mechanical properties, a field of heterogeneous stress is generated in the grains. Under certain conditions, these differences may also yield formation of a heterogeneous passive film. In this work, we study the effect of alloying elements on the physico-chemical properties of the passive film and behavior pitting corrosion before and after ageing in chloride media for a reference surface that meet certain criteria ie a smooth surface free from any defects (no hardened layer .. low roughness). The physicochemical properties of the film are studied using Auger and XPS analysis at the microscale. The corrosion behavior of duplex alloys was then determined from CPT tests (determination of the Critical Pitting Temperature). The results before ageing have shown that the passive film is homogeneous on a macroscopic scale and that pitting corrosion appear to be related to the grain size and crystallographic texture described by GOS. After ageing, surface analysis shows a strengthening of passivity by thickening of the passive film and the ratio Cr/Fe are significantly increased which has the effect of improving behavior pitting alloys. Metallurgical criteria for pitting were proposed.

Ce travail présente deux contributions clés dans le domaine des réseaux de communication sans fil 4G+/5G, en particulier dans le domaine de la détection MIMO d’ordre supérieur et le design (conception) de réseau relai semi-duplex. La première partie de ce travail de recherche s’intéresse au développement d’une stratégie de détection MIMO d’ordre supérieur pour les terminaux 4G+/5G existants et futurs, d’un point de vue à la fois théorique et pratique. Une nouvelle technique de décomposition QR Bloc de prétraitement est proposée pour un récepteur LTE dans un scénario limité à un seul utilisateur, interférence limitée, ainsi qu’un scénario point par point dont les résultats surlignent les avantages et inconvénients en performance et complexité. La deuxième partie de cette étude comprend une étude de faisabilité d’une stratégie de message novatrice à deux phases et trois parties pour un réseau relai semi-duplex à couche physique, qui comporte un codage de superposition et un décodage d’annulation d’interférence successif, conscient des interférences. Un point clé de cette étude était d’analyser la performance du schéma d’adaptation des liaisons proposées dans le régime non asymptotique et d’évaluer l’efficacité spectrale (ES) par rapport aux hypothèses théoriques des blocs d’asymptotiquement grandes longueurs. Une comparaison ES supplémentaire est également présentée, avec une transmission de relais à deux étapes non coopérative et une stratégie de transmission point à point. Les résultats obtenus révèlent les gains d'ES qui peuvent être obtenus en exploitant la coopération de couche physique entre le relais et la station de base. / The evolution of wireless communication networks has always been rapidly progressive partly due to the demands of today’s data hungry users. This dissertation presents two key contributions to the body of knowledge in the evolving area of physical layer 4G+/5G communication technologies, especially in the domain of Higher-order MIMO detection and half-duplex relay network design. The initial part of this research investigates the development of a higher-order MIMO detection strategy for existing and future 4G+/5G receivers, from both a theoretical and practical perspective. A novel pre-processing Block QR decomposition technique has been proposed for an LTE receiver in a single-user interference-limited scenario as well as a point-to-point scenario with the results highlighting the complexity advantages and limitations in performance. The second part of this study involves a practical feasibility study of a novel two-phase three-part-message strategy for a physical layer half-duplex relay network, which features superposition coding and interference-aware successive interference cancellation decoding. A key aim of this study was to analyze the performance of the proposed link adaptation scheme in the non-asymptotic regime (finite block-length and discrete constellation signaling), and evaluate the spectral efficiency (SE) against the theoretical assumptions of asymptotically large block-lengths. An additional SE comparison with a non-cooperative two-hop relay transmission and point-to-point transmission strategy is also presented. The resulting outcomes reveal the SE gains that can be had by exploiting physical layer cooperation between the relay and base station.

[pt] Atualmente, pesquisas envolvendo metais e suas ligas têm como um de seus objetivos o controle microestrutural, como forma de aprimorar as propriedades de interesse, para as aplicações desejadas. Um fator importante que possui influência nas propriedades dos materiais policristalinos são os tipos, e distribuições de contornos de grãos e/ou de fase. A aplicação de processos que envolvam altas temperaturas, como tratamentos térmicos ou processos de soldagem, podem levar a transformações de fase, as quais modificam a cristalografia, composição química, distribuição e tamanho dos grãos. Os aços inoxidáveis duplex são ligas bifásicas constituídas de proporções aproximadamente iguais de ferrita e austenita pertencentes ao sistema Fe-Cr-Ni. Essa estrutura bifásica combina elevada resistência, boa tenacidade e excelente resistência à corrosão. Devido à essas excelentes propriedades são utilizadas em vários setores industriais como: indústrias químicas, petroquímicas, de petróleo e gás, e de construção naval. Incrementos na concentração de Cr e Ni nestes aços levam a formação de duas novas classes, os aços super e hiper duplex, cujas propriedades são semelhantes aos aços duplex, porém superiores. Neste caso, devido ao aumento no teor dos elementos de liga os processos de soldagem podem levar a formação de fases intermetálicas e/ou precipitados, as quais são deletérias as propriedades dos aços, facilitando o processo de corrosão. Muitas das transformações no estado sólido que ocorrem nos aços, seguem determinadas relações de orientação cristalográfica. Essas relações descrevem as interfaces de baixa energia que determinam os processos de nucleação e crescimento de novas fases. Portanto a determinação das relações de orientação presente nos aços duplex, super-duplex e hiper-duplex, a partir de transformações de fase obtidas em condições de equilíbrio e paraequilíbrio foram estudadas com a intenção de correlacionar com a susceptibilidade à corrosão por pites. Foram estudados os aços UNS S32205, UNS S32750 e UNS S33207, respectivamente pertencendo as classes duplex, super e hiperduplex A determinação das relações de orientação e fração de fases foi obtida por difração de elétrons retroespalhados (Electron Backscattering Diffraction - EBSD). A composição química das fases foi obtida por Espectroscopia de Energia Dispersiva (Energy Dispersion Spectroscopy - EDS). Estes dados foram correlacionados com os resultados obtidos após testes de corrosão ASTM G-48. Para todos os aços se observa a tendência do aumento da relação de orientação KS após submissão aos ciclos térmicos. No entanto, para as condições estudadas não foi encontrada uma correlação clara entre a presença da orientação KS com a formação de pites na ferrita. / [en] Currently, research involving metals and their alloys has microstructural control as one of its objectives, to improve the properties of interest, for the desired applications. An important factor that influences the properties of polycrystalline materials are the types and distributions of grain and/or phase boundaries. The application of processes involving high temperatures, such as heat treatments or welding processes, can lead to phase transformations, which modify the crystallography, chemical composition, distribution and size of the grains. Duplex stainless steels are biphasic alloys made up of approximately equal proportions of ferrite and austenite belonging to the Fe-Cr-Ni system. This two-phase structure combines high strength, good toughness and excellent corrosion resistance. Due to these excellent properties, they are used in various industrial sectors such as: chemical, petrochemical, oil and gas, and shipbuilding industries. Increases in the concentration of Cr and Ni in these steels lead to the formation of two new classes, super and hyper duplex steels, whose properties are like duplex steels, but superior. In this case, due to the increase in the content of alloying elements, the welding processes can lead to the formation of intermetallic phases and/or precipitates, which are deleterious to the properties of the steels, facilitating the corrosion process. Many of the solid-state transformations that occur in steels follow certain crystallographic orientation relationships. These relationships describe the lowenergy interfaces that determine the processes of nucleation and growth of new phases. Therefore, the determination of orientation relationships presents in duplex, super-duplex and hyper-duplex steels, from phase transformations obtained under equilibrium and paraequilibrium conditions, were studied with the intention of correlating with the susceptibility to pitting corrosion. The UNS S32205, UNS S32750 and UNS S33207 steels were studied, respectively belonging to the duplex, super and hyperduplex classes. of the phases was obtained by Energy Dispersion Spectroscopy (EDS). These data were correlated with the results obtained after ASTM G-48 corrosion tests. For all steels, there is a trend towards an increase in the KS orientation ratio after submission to thermal cycles, however no clear correlation between the presence of the KS orientation and the formation of pits in the ferrite was found.