L'objectif de cette étude est d'aboutir à une meilleure compréhension de la fragilisation par les métaux liquides (FML) à travers l'étude des systèmes T91/Pb-Bi et 316L/Pb-Bi et notamment d'en établir les mécanismes mis en jeu lors du contact entre ces aciers sous tension et le métal liquide. Ce travail s'inscrit dans le cadre du projet MEGAPIE-TEST mis en place pour étudier la faisabilité d'une cible de spallation au plomb-bismuth liquide. L'effet de l'eutectique plomb-bismuth liquide sur le T91 et le 316L a été étudié en fonction de la température et de la vitesse de déformation, en utilisant des éprouvettes CCT adaptées à l'étude de propagation de fissures. La présence de Pb-Bi modifie le mécanisme de rupture du T91 au détriment de la germination, croissance et coalescence des cavités. La rupture procède alors par décohésion des bandes de cisaillement. L'effet fragilisant du Pb-Bi est très marqué aux très faibles vitesses de déformation. Une transition fragile-ductile se produit aux grandes vitesses de déformation (~10-5 m.s-1 à 160°C). Les propriétés mécaniques du 316L ne sont pas autant affectées par la présence de Pb-Bi, toutefois une transition réelle est observée sur les faciès de rupture, où là également il y a compétition entre l'effet fragilisant du métal liquide et la rupture ductile. Le mécanisme suggéré dans ce travail est fondé sur la localisation de la déformation en pointe de la fissure combinée au phénomène de réduction d'énergie de surface induite par adsorption de métal liquide (effet Rebinder) et ne fait intervenir aucun processus diffusionnel en particulier aux joints de grains. / The aim of this work is to study liquid metal embrittlement (LME) on the T91/Pb-Bi and 316L/Pb-Bi systems. A particular attention is paid to obtain a better understanding of the mechanisms of fracture when steels are in contact with liquid metal. This work has been performed within the European projects MEGAPIE-TEST and EUROTRANS which aim to prove the feasibility of lead-bismuth nuclear systems such as spallation target and subcritical reactors. The effect of liquid Lead Bismuth Eutectic (LBE) on 316L and T91 steels has been studied in plane stress conditions as a function of temperature and strain rate, using a CCT geometry adapted for the study of crack propagation. The presence of LBE modifies the fracture mechanism of T91 and prevents fracture by growth and coalescence of cavities. Cracking proceeds by shear band decohesion. This embrittlement effect is very pronounced at low deformation rate whereas at the high strain rate range investigated, a brittle to ductile transition is observed. The temperature variation of the transition rules out LME mechanisms based on dissolution. A fracture mechanics analysis by the J-µa methodology allowed the quantification of the embrittlement degree which is estimated to 30% reduction in the energy required for crack propagation. The mechanical properties of the 316L steel are weakly affected by the presence of LBE, in spite of a change in the plastic deformation at the highest triaxiality point which strongly affecting fracture surfaces. The mechanism of this embrittlement seems to be based on the deformation localization at the crack tip combined with the phenomenon of surface energy reduction induced by the liquid metal adsorption. It does not involve any diffusion process. The deformation localization is confirmed by an electron microscopy study of the crack tip plasticity of 316L under the influence of a liquid metal.

Nos últimos anos houve, no Brasil, um significativo investimento em usinas de álcool para suprir a demanda. Todavia, surgiram problemas de natureza econômica e ambiental, já que a tecnologia atualmente utilizada nas destilarias de álcool produz em média 13 litros de vinhaça para cada litro de álcool. Na busca de uma solução para reduzir o volume deste resíduo, desenvolveu-se um equipamento para concentração de vinhaça, denominado Ecovin, pela empresa Citrotec localizada em Araraquara-SP. Para cada Ecovin são utilizados cerca de 4000 tubos com costura nos trocadores de calor, e para reduzir seu custo de fabricação, avaliou-se como opção o uso de tubos da liga AISI 444. Inserido neste contexto, o presente trabalho procurou caracterizar os mecanismos de corrosão e mostrar de forma comparativa o desempenho dos tubos nas juntas tubo-espelho. Estudo-se, portanto, dois tipos de junta, a do projeto atual, composta por chapa e tubo da liga AISI 316L; e a nova proposta, composta por chapa da liga AISI 316L e tubo da liga AISI 444. Para tanto, iniciou-se com a avaliação da soldabilidade das ligas estudadas, através da caracterização microestrutural, qualificação do procedimento de soldagem da junta tubo-espelho e de ensaios de sensitização nas soldas. Em seguida, ensaios de perda de massa por imersão foram realizados nas soluções de 0,5 M \'H IND.2\'SO IND.4\' e 0,5 M \'H\'CL\', nas temperaturas de 30°C, 50°C, 70°C e 90°C, de acordo com o intervalo de temperatura de operação do Ecovin. Nas mesmas soluções, e na temperatura ambiente, foram realizados ensaios eletroquímicos de polarização potenciodinâmica em amostras que reproduziram o ciclo térmico de soldagem das juntas tubo-espelho estudadas, nas regiões do metal de base, zona afetada pelo calor (ZAC) e no metal de solda. Na junta tubo-espelho a corrosão ocorreu preferencialmente na ZAC formada entre a interface tubo-metal de solda, e no cordão de solda à margem do tubo, com a atuação de mecanismos de corrosão generalizada e localizada. Na junta tubo-espelho dissimilar observou-se que o processo corrosivo foi predominante na superfície do tubo AISI 444, típico do mecanismo de corrosão galvânica, onde o tubo AISI 444 caracterizou-se como a região anódica. O desempenho da liga AISI 316L, assim como a junta soldada composta somente por essa liga, apresentou um melhor desempenho em corrosão, porém, na solução contendo cloreto, a variação da temperatura exerceu uma influência proporcional para ambos os casos avaliados nesse estudo. Destaca-se ainda que a liga AISI 316L sofreu corrosão por pite na ZAC e no metal de solda, em ambas as soluções, com maior severidade do que a liga AISI 444. Os resultados obtidos indicam que para a aplicação requerida, o tubo AISI 444 pode ser utilizado na temperatura de 50°C com satisfatório desempenho e similar à junta composta somente por AISI 316L. / Recently in Brazil there has been constant investments in ethanol plants, to supply the internal and external market, resulting at a high increase of the volume of this product. However, economical and environmental problems arose because of this new demand, whereas the current technologies produce thirteen liters of vinasse for each liter of alcohol. Each ECOVIN uses nearly 4000 welded tubes in the heat exchangers, and there is an option to use welded AISI 444 alloy tubes in order to reduce the manufacture costs of the ECOVIN. In this context, this work determines the corrosion mechanisms and analyzes the performance of welded tubes and the tube-to-tubesheet welded joints. The following types of tube-to-tubesheet were evaluated: current welded joints of this project, with all components manufactured with AISI 316L alloy; and the welded joint suggested for the project, using the welded tubes of AISI 444 alloy and the plate of AISI 316L alloy. For this purpose, the first step was to evaluate the weldability of the studied alloys, through microstructural characterization, welding procedure qualification and the intergranular corrosion test. After that, mass loss tests were conducted in 0,5 M \'H IND.2\'SO IND.4\' and 0,5 M \'H\'CL\' solutions, at 30°C, 50°C, 70°C and 90°C, according to the temperature range of the equipment operating. Electrochemical polarization tests were made in the same solution concentration used in the mass loss tests, but only in room temperature. These tests were made in samples that were welded with the same thermal cycle of the tube-to-tubesheet welded joints, and the evaluations were made on the base metal, heat affected zones and weld metal. The uniform and localized corrosion process occurred preferentially in the interface formed between tube and weld metal, and on weld metal near the tubes. In the tube-to-tubesheet dissimilar welded joints, it was observed that the corrosion process was predominant on the surface of AISI 444 alloy, probably because of the galvanic corrosion process, where the AISI 444 was an anodic region. The best performance on corrosion process was observed in AISI 316L, both the base metal and the similar welded joints. However, for the tests in chloride environment, in this process, the temperature caused a proportional influence in the corrosion rate of AISI 316L and AISI 444. In the AISI 316L alloy it was observed nucleation of pitting in HAZ and in weld metal, in both solutions, and more aggressive than observed in the AISI 444 alloy. The results showed that the AISI 444 alloy can be applied for the initial ranging temperatures of the equipments operation, with satisfactory performance.

Projetos de instalações industriais com requisitos de assepsia e resistência à corrosão têm os aços inoxidáveis austeníticos como materiais de engenharia, e a liga AISI 316L é amplamente utilizada. A soldagem de chapas espessas é executada por processos MIG e a qualificação do procedimento de soldagem é realizada com base em propriedades mecânicas, avaliação insuficiente para aplicações que necessitam de uma película passiva resistente. A microestrutura da zona fundida da liga AISI 316L exerce influência sobre a resistência à corrosão, e há a necessidade de definir os mecanismos que governam a influência da fase sigma na resistência à corrosão. Inserido neste contexto, o objetivo do presente estudo foi avaliar a influência da fase sigma na resistência à corrosão em microrregiões de juntas soldadas multipasse da liga AISI 316L produzidas pelo processo MIG nos modos de transferência metálica pulsado, curto-circuito e spray. A metodologia consistiu em reproduzir amostras soldadas com parâmetros de soldagem aplicados na indústria para os modos de transferência metálica de interesse, com detalhada caracterização microestrutural da zona fundida de cada condição de soldagem. Em seguida, foram conduzidos ensaios eletroquímicos de corrosão em microrregiões da junta soldada em solução de 3,5% NaCl, e a influência da fase sigma na corrosão por pite foi avaliada por ensaio de imersão em solução de cloreto férrico (6% FeCl3). Caracterizou-se a área exposta à varredura por técnicas de microscopia ótica, microscopia eletrônica de varredura e microanálise química. A soldagem no modo pulsado resultou em uma zona fundida com microestrutura bifásica com a mais baixa fração volumétrica de ferrita delta, de refinada morfologia e isenta de fase sigma, proporcionando o mais nobre desempenho nos ensaios de corrosão, que se manifestou pelo mecanismo de corrosão localizada. A avaliação da área exposta à varredura demonstrou que, previamente a corrosão por pite, a corrosão incia-se de forma localizada, contudo, sem corrosão preferencial de uma das fases, característica que proporcionou parâmetros eletroquímicos mais nobres do que aqueles com corrosão seletiva de fases. Está característica é atribuída à ausência da fase sigma na microestrutura da zona fundida do modo pulsado. No modo curto-circuito ocorreu à decomposição eutetóide da ferrita delta formando a austenita secundária e a fase sigma, sendo está última precipitada principalmente no interior da ferrita delta. A morfologia da corrosão se dá, na fase inicial, como corrosão seletiva de fases, com degradação preferencial da austenita secundária e em direção a ferrita delta, devido à fragilização desta fase pela precipitação de fase sigma em seu interior. A degradação seletiva das fases austenita secundária e ferrita delta causam danos localizados ao filme passivo e, nestas regiões empobrecidas de cromo e molibdênio, ocorre à corrosão por pite. O modo spray com a mais elevada energia de soldagem resultou em uma ferrita delta grosseira e com estreitas bandas de austenita na microrregião de enchimento do chanfro e na raiz da solda, com alto índice de fase sigma nestas localizações. O processo corrosivo da zona fundida caracterizou-se por corrosão seletiva da fase austenita secundária e em direção à matriz austenítica, uma vez que a fase sigma revestiu a ferrita delta, tornando-a a região de comportamento catódico entre o par galvânico formado entre as fases austenita e ferrita delta. A corrosão seletiva da matriz austenítica causa a fragilização localizada do filme passivo com consequente corrosão por pite. O trabalho realizado permite concluir que o potencial de pite foi reduzido com a presença de fase sigma e fases a esta associada, e justamente o modo pulsado obteve destacada resistência à corrosão em função da ausência da fase sigma em sua microestrutura. / Industrial plant designs with asepsis and corrosion resistance requirements have austenitic stainless steels as engineering materials, and the AISI 316L alloy is widely used. The welding of thick plates is performed by MIG processes and the qualification of the welding procedure is carried out based on mechanical properties, insufficient evaluation for applications that require a resistant passive film. The microstructure of the molten zone of the AISI 316L alloy influences the corrosion resistance, and it is necessary to define the mechanisms that govern the influence of the sigma phase on corrosion resistance. In this context, the aim of the present study was to evaluate the influence of the sigma phase on the corrosion resistance in microrregions of multipass welded joints of the AISI 316L alloy produced by MIG process with metal transfer in pulsed, short circuit and spray modes. The methodology consisted in reproducing welded samples with welding parameters applied in the industry for the modes of metallic transfer of interest, with detailed microstructural characterization of the molten zone of each welding condition. Then, electrochemical corrosion tests were carried out in microrregions of the welded joint in 3.5% NaCl solution, and the influence of the sigma phase on pitting corrosion was evaluated by immersion test in ferric chloride solution (6% FeCl3). The area exposed to the scanning was characterized by optical microscopy, scanning electron microscopy and chemical microanalysis. Pulsed mode welding resulted in a molten zone with a biphasic microstructure with the lowest volume fraction of delta ferrite, refined morphology and sigma phase free, providing the noblest performance in the corrosion tests, which occurred in the form of localized corrosion. The evaluation of the area exposed to the scan showed that, prior to pitting corrosion, the corrosion started in a localized manner, however, without preferential corrosion of one of the phases, a characteristic that gave better electrochemical parameters than those with selective corrosion of phases. This characteristic is attributed to the absence of the sigma phase in the microstructure of the molten zone of the pulsed mode. In the short-circuit mode, the eutectoid decomposition of the delta ferrite formed the secondary austenite and the sigma phase, the latter being mainly precipitated inside the delta ferrite. The corrosion morphology occurs in the initial phase as selective corrosion of phases, with preferential degradation of the secondary austenite and towards the ferrite delta, due to the embrittlement of this phase by the precipitation of the sigma phase inside. The selective degradation of the secondary austenite and delta ferrite phases causes localized damage to the passive film and, in these impoverished regions of chromium and molybdenum, occurs to pitting corrosion. The spray mode with the highest welding energy resulted in a coarse delta ferrite with narrow bands of austenite in the chamfer filling microrregion and at the root of the weld, with a high sigma phase index at these locations. The corrosive process of the molten zone was characterized by selective corrosion of the secondary austenite phase and towards the austenitic matrix, since the sigma phase covered the delta ferrite, making it the region of cathodic behavior between the galvanic pair formed between the austenite and ferrite delta phases. Selective corrosion of the austenitic matrix causes localized embrittlement of the passive film with consequent pitting corrosion. The study accomplished allows concluding that the pitting potential was reduced with the presence of sigma phase and phases associated with it, and precisely the pulsed mode obtained outstanding corrosion resistance due to the absence of the sigma phase in its microstructure.

L’acier 316L(N) est le matériau de référence pour les structures du circuit primaire des réacteurs nucléaires de quatrième génération, en raison de leur résistance mécanique à la température de fonctionnement, de l’ordre de 550°C. La thèse a permis de développer un modèle polycristallin, capable de prédire le comportement de ces aciers, basé sur la description du glissement viscoplastique des dislocation à haute température, de mise en œuvre simple et avec l’identification d’un nombre de paramètres matériau limité. La démarche de modélisation a été progressive. Lors de la première étape, nous avons proposé et validé une loi d'homogénéisation élasto-viscoplastique à champs moyens, grâce à de nombreux calculs par éléments finis, en considérant des durcissements plastique et des viscosités cristallines. Ensuite, un modèle de viscoplasticité cristalline, reposant sur les lois d’évolution des densités de différents types de dislocations, a été implémenté et les prédictions ont été validés en considérant un très grand nombre de résultats expérimentaux à faible. Le modèle a ensuite été enrichi afin de prendre en compte les mécanismes physiques supplémentaires observés à température élevée, comme la montée des dislocations, le vieillissement dynamique et l’apparition d’une structure de dislocation très hétérogène. Le modèle proposé nécessite uniquement l’ajustement de trois paramètres par identification inverse, utilisant seulement des essais de traction monotone avec saut de vitesse. Les prédictions du comportement mécanique en chargement uniaxial et cyclique sont également en bon accord avec les mesures expérimentales aux températures élevées. / The 316L(N) stainless steels is the reference material for the primary circuit structures of fourth-generation nuclear reactors. This alloy present high mechanical resistance at the operation temperature range of these reactors, of the order of 550 °C. This PhD allowed to develop a polycrystalline model based on the description of the viscoplastic dislocation slip at high temperatures, with straightforward implementation and with identification of a limited number of material parameters. The modeling process was progressive. In a first step, we proposed and validated a mean-field elastic-viscoplastic homogenization law, in comparison to numerous finite element calculations, considering crystalline plastic hardening and crystalline viscosity. Then, a model of crystalline viscoplasticity, based on the evolution laws of the different dislocations densities was implemented and the predictions were validated considering a very large number of experimental results at low temperature. The model was then enhanced to take into account the additional physical mechanisms observed at high temperature, such as dislocation climb, dynamic strain aging and the appearance of a very heterogeneous dislocation structure. The proposed model requires the adjustment of only three parameters by inverse identification, using only monotonic tensile tests at different strain rates. The mechanical behavior predictions in uniaxial and cyclic loading are also in good agreement with experimental measurements at high temperature.

Submitted by Johnny Rodrigues (johnnyrodrigues@ufcg.edu.br) on 2018-04-05T18:10:49Z No. of bitstreams: 1 ANDRÉ LOPES SOARES - DISSERTAÇÃO PPG-CEMat 2014..pdf: 6257060 bytes, checksum: 6c6fb12b0cbaaafb3788e358c240a5d5 (MD5) / Made available in DSpace on 2018-04-05T18:10:49Z (GMT). No. of bitstreams: 1 ANDRÉ LOPES SOARES - DISSERTAÇÃO PPG-CEMat 2014..pdf: 6257060 bytes, checksum: 6c6fb12b0cbaaafb3788e358c240a5d5 (MD5) Previous issue date: 2014-08-28 / Filmes finos de Nitreto de zircônio (ZrN) e nitreto da mistura titânio-zircônio (TiZrN) foram depositados sobre substratos de aço inoxidável 316L usando o método de RF Sputtering para deposição dos filmes. O planejamento de experimentos (DOE) tem sido reconhecido como um método poderoso para otimizar um processo complexo na indústria. Os efeitos do presente estudo foram verificar a viabilidade e confiabilidade da aplicação do método DOE em processos de RF Sputtering, otimizar os parâmetros de processamento para o processo de deposição, identificando os parâmetros sensíveis que afetam a espessura da camada depositada (E.C.D) e a resistência à corrosão (Ecorr.) Para o método de RF Sputtering, dois parâmetros, a taxa e tempo de deposição foram escolhidos para serem os parâmetros do processo. Depois da deposição, a estrutura de camada depositada foi caracterizada por Difração de Raios X (DRX) e por Microscopia Eletrônica de Varredura (MEV). Após o ensaio de polarização, a corrosão foi realizada a fim de investigar a relação entre o início da corrosão e a espessura da camada depositada. A análise de variância (ANOVA) foi realizada para avaliar os parâmetros sensíveis e prever as condições ideais. Com base na análise estatística, os parâmetros mais sensíveis no processo de RF Sputtering foram tanto a taxa como também o tempo de deposição do filme fino. As melhores condições de deposição foram a taxa de deposição máxima e tempo máximo. / Zirconium nitride (ZrN) and titanium-zirconium nitride (TiZrN) thin films were deposited on 316L stainless steel substrates using de RF Sputtering methods. Design of experiment (DOE) has long been recognized as a powerful method to optimize a complex process in industry. The purposes of present study were to verify the feasibility and reliability of the application of DOE method on de RF Sputtering processes and optimize the processing parameters for the deposition process, in which the sensitive parameters that affected the film properties were also identified. For de RF Sputtering method, two parameters, deposition rate and time were chosen to be the operating parameters. After deposition, the thin film structure was characterized by X-ray diffraction (XRD), and high-resolution scanning electron microscopy (SEM). After the polarization test, the corrosion analysis was carried out in order to investigate the relationship between the corrosion initiation and the thickness of the deposited layer. The analysis of variance (ANOVA) was conducted to assess the sensitive parameters and predict the optimum conditions. Based on the statistical analysis, the most sensitive parameters in de RF Sputtering process were both the deposition rate and time. The optimum deposition conditions in each system were maximum deposition rate and time.

Projetos de instalações industriais com requisitos de assepsia e resistência à corrosão têm os aços inoxidáveis austeníticos como materiais de engenharia, e a liga AISI 316L é amplamente utilizada. A soldagem de chapas espessas é executada por processos MIG e a qualificação do procedimento de soldagem é realizada com base em propriedades mecânicas, avaliação insuficiente para aplicações que necessitam de uma película passiva resistente. A microestrutura da zona fundida da liga AISI 316L exerce influência sobre a resistência à corrosão, e há a necessidade de definir os mecanismos que governam a influência da fase sigma na resistência à corrosão. Inserido neste contexto, o objetivo do presente estudo foi avaliar a influência da fase sigma na resistência à corrosão em microrregiões de juntas soldadas multipasse da liga AISI 316L produzidas pelo processo MIG nos modos de transferência metálica pulsado, curto-circuito e spray. A metodologia consistiu em reproduzir amostras soldadas com parâmetros de soldagem aplicados na indústria para os modos de transferência metálica de interesse, com detalhada caracterização microestrutural da zona fundida de cada condição de soldagem. Em seguida, foram conduzidos ensaios eletroquímicos de corrosão em microrregiões da junta soldada em solução de 3,5% NaCl, e a influência da fase sigma na corrosão por pite foi avaliada por ensaio de imersão em solução de cloreto férrico (6% FeCl3). Caracterizou-se a área exposta à varredura por técnicas de microscopia ótica, microscopia eletrônica de varredura e microanálise química. A soldagem no modo pulsado resultou em uma zona fundida com microestrutura bifásica com a mais baixa fração volumétrica de ferrita delta, de refinada morfologia e isenta de fase sigma, proporcionando o mais nobre desempenho nos ensaios de corrosão, que se manifestou pelo mecanismo de corrosão localizada. A avaliação da área exposta à varredura demonstrou que, previamente a corrosão por pite, a corrosão incia-se de forma localizada, contudo, sem corrosão preferencial de uma das fases, característica que proporcionou parâmetros eletroquímicos mais nobres do que aqueles com corrosão seletiva de fases. Está característica é atribuída à ausência da fase sigma na microestrutura da zona fundida do modo pulsado. No modo curto-circuito ocorreu à decomposição eutetóide da ferrita delta formando a austenita secundária e a fase sigma, sendo está última precipitada principalmente no interior da ferrita delta. A morfologia da corrosão se dá, na fase inicial, como corrosão seletiva de fases, com degradação preferencial da austenita secundária e em direção a ferrita delta, devido à fragilização desta fase pela precipitação de fase sigma em seu interior. A degradação seletiva das fases austenita secundária e ferrita delta causam danos localizados ao filme passivo e, nestas regiões empobrecidas de cromo e molibdênio, ocorre à corrosão por pite. O modo spray com a mais elevada energia de soldagem resultou em uma ferrita delta grosseira e com estreitas bandas de austenita na microrregião de enchimento do chanfro e na raiz da solda, com alto índice de fase sigma nestas localizações. O processo corrosivo da zona fundida caracterizou-se por corrosão seletiva da fase austenita secundária e em direção à matriz austenítica, uma vez que a fase sigma revestiu a ferrita delta, tornando-a a região de comportamento catódico entre o par galvânico formado entre as fases austenita e ferrita delta. A corrosão seletiva da matriz austenítica causa a fragilização localizada do filme passivo com consequente corrosão por pite. O trabalho realizado permite concluir que o potencial de pite foi reduzido com a presença de fase sigma e fases a esta associada, e justamente o modo pulsado obteve destacada resistência à corrosão em função da ausência da fase sigma em sua microestrutura. / Industrial plant designs with asepsis and corrosion resistance requirements have austenitic stainless steels as engineering materials, and the AISI 316L alloy is widely used. The welding of thick plates is performed by MIG processes and the qualification of the welding procedure is carried out based on mechanical properties, insufficient evaluation for applications that require a resistant passive film. The microstructure of the molten zone of the AISI 316L alloy influences the corrosion resistance, and it is necessary to define the mechanisms that govern the influence of the sigma phase on corrosion resistance. In this context, the aim of the present study was to evaluate the influence of the sigma phase on the corrosion resistance in microrregions of multipass welded joints of the AISI 316L alloy produced by MIG process with metal transfer in pulsed, short circuit and spray modes. The methodology consisted in reproducing welded samples with welding parameters applied in the industry for the modes of metallic transfer of interest, with detailed microstructural characterization of the molten zone of each welding condition. Then, electrochemical corrosion tests were carried out in microrregions of the welded joint in 3.5% NaCl solution, and the influence of the sigma phase on pitting corrosion was evaluated by immersion test in ferric chloride solution (6% FeCl3). The area exposed to the scanning was characterized by optical microscopy, scanning electron microscopy and chemical microanalysis. Pulsed mode welding resulted in a molten zone with a biphasic microstructure with the lowest volume fraction of delta ferrite, refined morphology and sigma phase free, providing the noblest performance in the corrosion tests, which occurred in the form of localized corrosion. The evaluation of the area exposed to the scan showed that, prior to pitting corrosion, the corrosion started in a localized manner, however, without preferential corrosion of one of the phases, a characteristic that gave better electrochemical parameters than those with selective corrosion of phases. This characteristic is attributed to the absence of the sigma phase in the microstructure of the molten zone of the pulsed mode. In the short-circuit mode, the eutectoid decomposition of the delta ferrite formed the secondary austenite and the sigma phase, the latter being mainly precipitated inside the delta ferrite. The corrosion morphology occurs in the initial phase as selective corrosion of phases, with preferential degradation of the secondary austenite and towards the ferrite delta, due to the embrittlement of this phase by the precipitation of the sigma phase inside. The selective degradation of the secondary austenite and delta ferrite phases causes localized damage to the passive film and, in these impoverished regions of chromium and molybdenum, occurs to pitting corrosion. The spray mode with the highest welding energy resulted in a coarse delta ferrite with narrow bands of austenite in the chamfer filling microrregion and at the root of the weld, with a high sigma phase index at these locations. The corrosive process of the molten zone was characterized by selective corrosion of the secondary austenite phase and towards the austenitic matrix, since the sigma phase covered the delta ferrite, making it the region of cathodic behavior between the galvanic pair formed between the austenite and ferrite delta phases. Selective corrosion of the austenitic matrix causes localized embrittlement of the passive film with consequent pitting corrosion. The study accomplished allows concluding that the pitting potential was reduced with the presence of sigma phase and phases associated with it, and precisely the pulsed mode obtained outstanding corrosion resistance due to the absence of the sigma phase in its microstructure.

Nos últimos anos houve, no Brasil, um significativo investimento em usinas de álcool para suprir a demanda. Todavia, surgiram problemas de natureza econômica e ambiental, já que a tecnologia atualmente utilizada nas destilarias de álcool produz em média 13 litros de vinhaça para cada litro de álcool. Na busca de uma solução para reduzir o volume deste resíduo, desenvolveu-se um equipamento para concentração de vinhaça, denominado Ecovin, pela empresa Citrotec localizada em Araraquara-SP. Para cada Ecovin são utilizados cerca de 4000 tubos com costura nos trocadores de calor, e para reduzir seu custo de fabricação, avaliou-se como opção o uso de tubos da liga AISI 444. Inserido neste contexto, o presente trabalho procurou caracterizar os mecanismos de corrosão e mostrar de forma comparativa o desempenho dos tubos nas juntas tubo-espelho. Estudo-se, portanto, dois tipos de junta, a do projeto atual, composta por chapa e tubo da liga AISI 316L; e a nova proposta, composta por chapa da liga AISI 316L e tubo da liga AISI 444. Para tanto, iniciou-se com a avaliação da soldabilidade das ligas estudadas, através da caracterização microestrutural, qualificação do procedimento de soldagem da junta tubo-espelho e de ensaios de sensitização nas soldas. Em seguida, ensaios de perda de massa por imersão foram realizados nas soluções de 0,5 M \'H IND.2\'SO IND.4\' e 0,5 M \'H\'CL\', nas temperaturas de 30°C, 50°C, 70°C e 90°C, de acordo com o intervalo de temperatura de operação do Ecovin. Nas mesmas soluções, e na temperatura ambiente, foram realizados ensaios eletroquímicos de polarização potenciodinâmica em amostras que reproduziram o ciclo térmico de soldagem das juntas tubo-espelho estudadas, nas regiões do metal de base, zona afetada pelo calor (ZAC) e no metal de solda. Na junta tubo-espelho a corrosão ocorreu preferencialmente na ZAC formada entre a interface tubo-metal de solda, e no cordão de solda à margem do tubo, com a atuação de mecanismos de corrosão generalizada e localizada. Na junta tubo-espelho dissimilar observou-se que o processo corrosivo foi predominante na superfície do tubo AISI 444, típico do mecanismo de corrosão galvânica, onde o tubo AISI 444 caracterizou-se como a região anódica. O desempenho da liga AISI 316L, assim como a junta soldada composta somente por essa liga, apresentou um melhor desempenho em corrosão, porém, na solução contendo cloreto, a variação da temperatura exerceu uma influência proporcional para ambos os casos avaliados nesse estudo. Destaca-se ainda que a liga AISI 316L sofreu corrosão por pite na ZAC e no metal de solda, em ambas as soluções, com maior severidade do que a liga AISI 444. Os resultados obtidos indicam que para a aplicação requerida, o tubo AISI 444 pode ser utilizado na temperatura de 50°C com satisfatório desempenho e similar à junta composta somente por AISI 316L. / Recently in Brazil there has been constant investments in ethanol plants, to supply the internal and external market, resulting at a high increase of the volume of this product. However, economical and environmental problems arose because of this new demand, whereas the current technologies produce thirteen liters of vinasse for each liter of alcohol. Each ECOVIN uses nearly 4000 welded tubes in the heat exchangers, and there is an option to use welded AISI 444 alloy tubes in order to reduce the manufacture costs of the ECOVIN. In this context, this work determines the corrosion mechanisms and analyzes the performance of welded tubes and the tube-to-tubesheet welded joints. The following types of tube-to-tubesheet were evaluated: current welded joints of this project, with all components manufactured with AISI 316L alloy; and the welded joint suggested for the project, using the welded tubes of AISI 444 alloy and the plate of AISI 316L alloy. For this purpose, the first step was to evaluate the weldability of the studied alloys, through microstructural characterization, welding procedure qualification and the intergranular corrosion test. After that, mass loss tests were conducted in 0,5 M \'H IND.2\'SO IND.4\' and 0,5 M \'H\'CL\' solutions, at 30°C, 50°C, 70°C and 90°C, according to the temperature range of the equipment operating. Electrochemical polarization tests were made in the same solution concentration used in the mass loss tests, but only in room temperature. These tests were made in samples that were welded with the same thermal cycle of the tube-to-tubesheet welded joints, and the evaluations were made on the base metal, heat affected zones and weld metal. The uniform and localized corrosion process occurred preferentially in the interface formed between tube and weld metal, and on weld metal near the tubes. In the tube-to-tubesheet dissimilar welded joints, it was observed that the corrosion process was predominant on the surface of AISI 444 alloy, probably because of the galvanic corrosion process, where the AISI 444 was an anodic region. The best performance on corrosion process was observed in AISI 316L, both the base metal and the similar welded joints. However, for the tests in chloride environment, in this process, the temperature caused a proportional influence in the corrosion rate of AISI 316L and AISI 444. In the AISI 316L alloy it was observed nucleation of pitting in HAZ and in weld metal, in both solutions, and more aggressive than observed in the AISI 444 alloy. The results showed that the AISI 444 alloy can be applied for the initial ranging temperatures of the equipments operation, with satisfactory performance.

L'objectif de ces travaux de thèse est d'étudier l'influence de la microstructure et de défauts géométriques sur le comportement en fatigue à grand nombre de cycles (FGNC) d'un acier inoxydable austénitique 316L. La méthodologie proposée s'appuie sur des simulations par éléments finis (EF) d'agrégats polycristallins qui permettent de décrire les champs mécaniques à l'échelle des mécanismes impliqués dans les processus d'amorçage de fissures de fatigue.Une étude numérique préliminaire, s'appuyant sur des données expérimentales issues de la littérature, est conduite sur un cuivre électrolytique à l'aide de simulations numériques d'agrégats polycristallins en 2D. L'effet du trajet de chargement et de défauts artificiels de taille proche ou légèrement supérieure à celle de la microstructure sur les réponses mécaniques mésoscopiques sont analysés. Les capacités de prédiction de quelques critères de fatigue, s'appuyant sur des quantités mécaniques mésoscopiques, sont évaluées. Il est mis en évidence que les limites de fatigue macroscopiques prédites par un critère de fatigue probabiliste sont en accord avec les tendances expérimentales observées en fatigue multiaxiale et en présence de défauts.Une campagne expérimentale a été menée sur un acier austénitique 316L. Des essais de fatigue oligocyclique sont conduits afin de caractériser le comportement élasto-plastique du matériau. Des essais de FGNC, utilisant des éprouvettes avec et sans défaut de surface (défaut artificiel hémisphérique) ont été effectués pour estimer les limites de fatigue dans différentes conditions de sollicitation (traction, torsion, traction et torsion combinée, traction biaxiale) et pour plusieurs rayons de défaut. Dans le but de compléter la caractérisation du matériau, la microstructure est étudiée à l'aide d'analyses EBSD et la texture cristallographique est mesurée par diffraction des rayons X. Ces résultats expérimentaux sont utilisés pour reproduire, avec des simulations EF, les essais de FGNC sur des microstructures 2D et 3D représentatives de l'acier austénitique. L'hétérogénéité de quantités mécaniques mésoscopiques pertinentes en fatigue est discutée avec une attention particulière sur l'effet des défauts. L'approche probabiliste est appliquée aux résultats des modèles EF pour quantifier l'effet de la taille du défaut, pour différents trajets de chargement. La pertinence, vis-à-vis des observations expérimentales, des distributions de la limite de fatigue prédites est évaluée. / The aim of this study is to analyze the influence of both the microstructure and defects on the high cycle fatigue (HCF) behaviour of a 316L austenitic stainless steel thanks to finite element (FE) simulations of polycrystalline aggregates.%The scatter encountered in the HCF behavior of metallic materials is often explained by the anisotropic elasto-plastic behavior of individual grains leading to a highly heterogeneous distribution of plastic slip.Since fatigue crack initiation is a local phenomenon, intimately related to the plastic activity at the crystal scale, it seems relevant to rely on this kind of modeling to evaluate the mechanical quantities.A preliminary numerical study, based on experimental data drawn from the litterature, was conducted on an electrolytic copper using simulations of 2D polycrystalline aggregates. The effect of the loading path and small artificial defects on the mesoscopic mechanical responses have been analyzed separately. Moreover, the predictive capabilities of some fatigue criteria, relying on the mesoscopic mechanical responses, has been evaluated. It was shown that the macroscopic fatigue limits predicted by a probabilistic fatigue criterion are in accordance with the experimental trends observed in multiaxial fatigue or in the presence of small defects.An experimental campaign is undertaken on an austenitic steel 316L. Low cycle fatigue tests are conducted in order to characterize the elasto-plastic behavior of the material. Load-controled HCF tests, using both smooth specimens and specimens containing an artificial hemispherical surface defect, are carried out to estimate the fatigue limits under various loading conditions (tension, torsion, combined tension and torsion, biaxial tension) and several defect radii. To complete the characterization of the material, the microstructure is studied thanks to EBSD analyzes and the cristallographic texture is measured by X-ray diffraction. These experimental data are used to reproduce, with FE simulations, the HCF tests on 2D and 3D microstructures representative of the austenitic steel. The heterogeneity of the mesoscopic mechanical quantities relevant in fatigue are discussed in relation to the modeling. The results from the FE models are then used along with the probabilistic mesomechanics approach to quantify the defect size effect for several loading paths. The relevance, with respect to the experimental observations, of the predicted fatigue strength distributions is assessed.

Metal additive technology allows to create objects with complex shape that are very difficult to produce by conventional technologies. An example of such component is a porous structure which is composed of periodical truss cells. This diploma thesis deals with the prediction of the mechanical properties of very small lattice structures made of additive manufacturing technology Selective Laser Melting. Using the proposed test specimens it was found that real dimensions of the trusses varies with size and orientation to the base platform. It was proposed and tested samples for rod tensile test made of SLM. Based on the real information about dimensions and mechanical properties of rods were predicted mechanical properties of lattice structures. A lot of mechanical tests were carried out to obtain the real mechanical properties. Test results and conclusions are described in the thesis.

Ce travail porte sur l'élaboration et l'analyse du comportement mécanique d'alliages à distribution bimodale de taille de grains. Les applications concernent les aciers inoxydables austénitiques 304L et 316L. Une approche couplée expérience-modélisation est menée pour comprendre les réponses mécaniques macroscopiques et locales de ces nouveaux alliages en se basant notamment sur l'étude des mécanismes de déformation associés. L'utilisation de deux voies d'élaboration et l'optimisation de leurs paramètres a conduit à l'obtention d'un large choix d'échantillons avec différentes distributions bimodales et différentes proportions de chaque famille de taille de grains. L'influence de ces caractéristiques microstructurales sur le comportement a été analysée sur la base d'essais en traction simple sous chargement monotone ou en charges-décharges alternées. Une base de données étendue de propriétés a ainsi été constituée et des éléments de réponse concernant les mécanismes de déformation propres aux alliages bimodaux ont pu être apportés. La présence de grains de taille conventionnelle (Coarse Grain -CG) au sein d'une matrice à grains ultrafins (UltraFine Grain - UFG) semble favoriser la relaxation d'une partie des contraintes internes de la matrice et tend ainsi à retarder l'endommagement des alliages bimodaux en comparaison aux alliages unimodaux à grains ultrafins. Une modélisation à champs complets selon deux lois de plasticité cristalline tenant compte explicitement d'une longueur interne a été proposée. Sa première motivation est de fournir un outil de prédiction du comportement effectif des alliages bimodaux en fonction de leurs caractéristiques microstructurales. Elle donne par ailleurs accès aux champs locaux et permet d'appuyer les analyses expérimentales en partition des contraintes en montrant à la fois une relaxation partielle des contraintes dans la matrice UFG mais aussi des concentrations de contrainte aux interfaces CG/UFG. / This work is focused on the elaboration and the mechanical behaviour of 304L and 316L austenitic stainless steel alloys with bimodal grain size distribution. The complementary approach between experiments and modelling enables a better understanding of both macroscopic and local mechanical responses and also of the associated deformation mechanisms.The use of two elaboration routes and optimized process parameters results in a wide range of samples with different bimodal grain size distributions. Grain sizes and fractions of each population are modified in order to study the influence of these microstructural characteristics on mechanical behavior. Uniaxial tensile tests are used to realize a database of mechanical properties of bimodal alloys and loading-unloading tests provides valuable informations about deformation mechanisms in these materials. With coarse grains (CG) embedded in an ultrafine grained (UFG) matrix, a relaxation of a part of the internal stresses seems to take place and leads to a delayed embrittlement of bimodal alloys as compared to their unimodal counterparts. Full-field modelling, based on two crystal plasticity laws with an explicit account of an internal length, is proposed. It constitutes a valuable prediction tool of effective properties of bimodal alloys in order, in particular, to study the effect of several microstructural characteristics. An access to local fields is also possible and tend, so far, to show similar results compared to experimental ones : stress relaxation is observed in the UFG matrix as well as stress concentrations at the CG/UFG interfaces.