Aços inoxidáveis dúplex apresentam uma estrutura composta por ferrita e austenita. O fato de a austenita ser estável à temperatura ambiente possibilita que esses aços sejam usados no estudo da reação de formação da austenita a partir da ferrita, podendo os resultados ser aplicados a aços de baixa liga, em que a austenita se transforma em martensita no resfriamento brusco, e a outros sistemas com transformações entre fases cúbicas de corpo centrado (CCC) e cúbicas de face centrada (CFC). Foram realizados estudos em um aço inoxidável dúplex do tipo DIN W.Nr. 1.4462 (UNS 31803). As amostras foram solubilizadas no campo ferrítico a 1325°C e resfriadas em água. As amostras foram ainda tratadas isotermicamente em temperaturas entre 700°C e 1100°C por tempos entre 5.000 e 30.000 segundos. Deste modo, a formação de austenita a partir da ferrita foi estudada em seu estágio inicial e em estágios avançados da reação, com relação aos seus aspectos morfológicos e cristalográficos. As morfologias encontradas apresentaram variações dependentes dos segmentos de contorno de grão em que as partículas se formam. As partículas nucleadas nos contornos de grão podem ser adequadamente descritas pela classificação morfológica de Dubé. Além disso, essas partículas apresentaram, em geral, relações de orientação do tipo Kurdjumov-Sachs e Nishyiama-Wassermann com pelo menos um dos dois grãos, podendo ser encontradas relações intermediárias entre essas duas. . Em alguns casos, as partículas mantêm relações de orientação com os dois grãos adjacentes, apresentando pequenos desvios das relações exatas relatadas na literatura. As partículas de austenita intragranulares apresentam desvios em relação à relações exatas maiores do que os encontrados nas partículas de contornos de grão. Em alguns casos, as partículas intragranulares aparentam não apresentar relações de orientação com a matriz ferrítica. / Duplex Stainless Steels have a structure composed by ferrite and austenite. The fact that austenite, in these steels, is stable at low temperatures, allows the use of these steels in studies of austenite formation from ferrite, in such way that the results can be applied to low alloy steels, in which austenite transforms to martensite upon rapid cooling, and to other systems containing transformations between body-centred cubic (BCC) and face-centred cubic (FCC) phases. Studies were performed on a DIN W.Nr. 1.4462 (UNS 31803) duplex stainless steel. The samples were solution treated in the ferrite region at 1325°C and water cooled. Samples were then submitted to isothermal treatments at temperatures between 700°C and 1100°C for up to 30.000 seconds. In this way, austenite formation from ferrite was studied on initial and advanced stages of the reaction, concerning morphological and crystallographic aspects. The morphologies observed varied with the grain boundary segment in which the particles were formed. The grain boundary particles may be adequately described by the Dubé classification. Moreover, these particles presented Kurdjumov-Sachs and Nishyiama-Wassermann orientation relationships with at least one of the adjacent grains, with possibilities of occurrence of intermediate relationships between K-S and N-W relationships. In some cases, the particles show orientation relationships with both adjacent grains, with small deviations form the exact relationships reported in literature. Intragranular austenite particles show higher deviations from the exact relationships than grain boundary particles. In some cases, intragranular particles have no apparent orientation relationships with the ferrite matrix.

Made available in DSpace on 2016-03-15T19:37:01Z (GMT). No. of bitstreams: 0 Previous issue date: 2010-03-02 / Fundo Mackenzie de Pesquisa / Given the variety of metallic materials used in orthopedic implants, the austenitic stainless steel type 316L and F138 have been widely used in Brazil as biocompatible material. Used by the public health, mainly due to it is low cost of manufacture compared to other materials, and because of the good combination of properties of which can be highlighted: The biocompatibility, the mechanical strength and corrosion resistance. However, these materials in contact with physiological fluids of the human body, allow the emergence of mechanisms of degradation such as corrosion, causing adverse reactions to patients.This fact causing possible premature failure of these implants, thus causing inconvenience to them and an additional cost the Unified Health System (SUS) replacement in these products. This work was developed in partnership with the Department of Graduate Studies of Engineering Materials, University of Mackenzie and the Department of Orthopedics and Tramautolog, Santa Casa de Misericordia de São Paulo (DOT-SCM-SP), motivated to perform a research study of the quality of orthopedic surgical implants, particularly osteosynthesis (plates and screws), removed from patients to identify the causes and failures, and possibly to use these results in the prevention of future occurrences of errors. Following the criteria specified in ISO 5832-1 and ASTM F138 that use a methodology, which consists of techniques for visual inspection, chemical analysis, macro and micro-structural characterization and examination fractographic. / Dada a diversidade de materiais metálicos utilizados em implantes ortopédicos, os aços inoxidáveis austeníticos do tipo 316L e F138 têm sido amplamente empregados no Brasil como materiais biocompatíveis. Eles são utilizados pela Rede Pública de Saúde, devido principalmente ao seu baixo custo de fabricação, em relação aos outros materiais e por apresentarem uma boa combinação de propriedades, das quais podem ser destacadas: a biocompatibilidade, a resistência mecânica e a corrosão. Porém, estes materiais, em contato com fluídos fisiológicos do corpo humano, possibilitam o surgimento dos mecanismos de degradação, tais como a corrosão, causando reações adversas aos pacientes, possíveis falhas prematuras destes implantes, gerando assim transtornos a estes e um custo adicional ao Sistema Único de Saúde (SUS), nas recolocações destes produtos. Este trabalho foi elaborado em parceria com o Departamento de Pós-Graduação de Engenharia de Materiais da Universidade Mackenzie e o Departamento de Ortopedia e Tramautologia da Santa Casa de Misericórdia de São Paulo (DOT-SCM-SP), motivado na elaboração de um estudo investigativo, da qualidade desses implantes cirúrgicos ortopédicos, em especial osteossínteses (placas e pinos), removidos de pacientes com o objetivo de identificar as causas e falhas, e possivelmente utilizar estes resultados na prevenção de ocorrências de futuros erros. Seguindo os critérios especificados nas normas ISO 5832-1 e ASTM F138 em que se aplica uma metodologia, que consiste em técnicas de inspeção visual, análise química, caracterização macro e microestrutural e exame fractográfico das superfícies.

O aço ferrítico-martensítico ODS Eurofer com 9%pCr (ODS - do inglês oxide dispersion strengthened), objeto de estudo dessa dissertação, é um potencial candidato para fins estruturais em reatores de fusão nuclear. Este material foi produzido via metalurgia do pó e consolidado por prensagem isostática. Em seguida sofreu laminação cruzada a quente e revenimento em 750°C por 2h. Esta foi a condição como recebida desse aço, o qual foi cedido pelo KIT (Karlsruher Institut für Technologie - Alemanha). Este aço possui 0,3%p de partículas de ítria (Y2O3) com diâmetro entre 10 e 30 nm. Uma das finalidades dessa dispersão de partículas de óxido é impedir a livre movimentação de contornos de grão no material, de modo a garantir a estabilidade microestrutural do mesmo sob recozimento. O aço ODS Eurofer como recebido foi laminado a frio com reduções de 20, 40, 60 e 80% da espessura e, posteriormente, foi recozido em diversas temperaturas entre 300 e 1350°C por 1h. Como o enfoque desse trabalho é sobre o aço ODS Eurofer recozido em altas temperaturas, para as temperaturas de 1250, 1300 e 1350°C foram feitos recozimentos adicionais (para o material com 80% de redução) variando-se o tempo de recozimento de 1 a 8 h. Para todos os recozimentos, com exceção dos realizados em 1350°C, o resfriamento das amostras se deu ao ar. Para a temperatura de 1350°C isso não foi possível e o resfriamento das amostras se deu no interior do forno. As amostras foram caracterizadas utilizando-se de medidas de dureza, medidas magnéticas e microscopia eletrônica de varredura (MEV). Amostras representativas também foram analisadas utilizando-se de difração de elétrons retroespalhados (EBSD) e espectroscopia por energia dispersiva (EDS). Para recozimentos em temperaturas acima de 800°C seguidos de resfriamento ao ar o material sofreu uma transformação martensítica. Na faixa de temperatura entre 800°C e 1300°C verificou-se um ligeiro decréscimo na dureza do material. Para as amostras com 80% de redução e recozidas em 1250 e 1300°C por diversos tempos até 8 h, seguido de resfriamento ao ar, não ocorreu uma variação significativa tanto nos valores de dureza e de campo coercivo das amostras com o tempo de recozimento. Estes valores se mantiveram em um patamar bem superior ao verificado para as amostras sem recozimento. Para as amostras recozidas em 1350°C, devido às características do resfriamento a microestrutura resultou em grãos ferríticos, aproximadamente equiaxiais e com tamanho de grão médio da ordem de 15 ?m. Observou-se uma notável queda tanto no valor de dureza como de campo coercivo dessas amostras. A observação mais importante nesse caso foi a observação de partículas da ordem de 100 nm ricas em ítrio no interior dos grãos, uma evidência de que ocorre o engrossamento das partículas de ítria nessa temperatura. Em virtude disso, a capacidade dessa dispersão de óxidos em impedir a livre movimentação de contornos de grãos no material fica prejudicada em 1350°C. / The object of this study is Eurofer 9% Cr Oxide Dispersion Strengthened (ODS) steel. This ferritic/martensitic steel is a potential candidate for structural applications in nuclear fusion reactors. It is produced through powder metallurgy and consolidated by hot isostatic pressing. The material undergoes hot cross lamination and is tempered at 760 °C. This was the condition of the steel as received, which was provided by KIT (Karlsruher Institut für Technologie, Germany). This steel contains 0.3 wt% yttria particles (Y2O3) with a diameter in the range 10-30nm. The main purpose of this oxide particle dispersion is to prevent the free movement of the grain boundaries in the material, so as to ensure stability of the microstructure during annealing. The material as received was cold rolled to reduce thickness by 20, 40, 60 and 80%. It was annealed at different temperatures from 300 to 1350 °C for 1 h. The focus of this study is the effects of high temperature annealing on the microstructure of ODS Eurofer. For this purpose, additional heat treatments were carried out on the steel that had been rolled to reduce thickness by 80% at temperatures of 1250, 1300 and 1350 °C. Annealing time varied between 15 min and 8 h. For all annealing conditions, except those carried out at 1350 °C, the samples were air cooled. For the temperature of 1350 °C, this was not possible. These samples were cooled in the oven. The samples were characterized using hardness testing, magnetic testing, and scanning electron microscopy (SEM). Representative samples were also analyzed using electron backscatter diffraction (EBSD) and energy dispersive spectroscopy (EDS). For annealing at temperatures above 800 °C, the material underwent a martensitic transformation after air cooling. Between 800 and 1300 °C, there was a slight decrease in the hardness of the material. For samples with 80% reduction annealed at 1250 and 1300 °C followed by air cooling, annealing time up to 8h didn\'t lead to a significant variation in either the hardness or the coercive field. Both hardness and coercive field of these samples were at a level well above the samples without annealing. For samples annealed at 1350 °C, due to the cooling characteristics of the samples, the microstructure took on a ferritic matrix with equiaxed grains with an average grain size of 15 um. There was a remarkable decrease in hardness and coercive field values of these samples. The most important result in this case was the observation of yttria-rich particles of the order of 100nm inside the grains. This is an evidence of the coarsening of the yttria particles at this temperature. As a result, the capacity of oxide dispersion to prevent the free movement of grain boundaries in the material is impaired at 1350°C.

Este trabalho teve por objetivo estudar o efeito dos parâmetros de corte e dos tratamentos térmicos na usinagem de três aços inoxidáveis austeníticos (ABNT 303, 304 e 310). Estes aços apresentam mesma estrutura cristalina e microestrutura semelhante. O aço ABNT 303 tem composição próxima ao ABNT 304, exceto pelo elevado teor de enxofre. Já o aço ABNT 310 apresenta maiores teores de elementos de ligas. Esses materiais foram tratados termicamente (solubilização ou envelhecimento). Os aços estudados foram caracterizados microestruturalmente e foram realizadas medidas de dureza Vickers. Os aços foram então torneados em várias condições de usinagem, variando principalmente a relação avanço por profundidade de corte. Foram medidas as forças de corte e de avanço em algumas das condições e coletados os cavacos resultantes para análise morfológica, que foram realizadas utilizando-se principalmente microscopia óptica e eletrônica de varredura. Foram também medidas as rugosidades e determinados os perfis das superfícies usinadas para a avaliação do acabamento superficial. Os resultados obtidos neste trabalho permitiram determinar algumas diferenças no comportamento dos três aços inoxidáveis estudados. As maiores diferenças foram verificadas quando as superfícies foram observadas utilizando microscopia. O aço ABNT 303 apresentou as piores superfícies e os menores esforços de corte em relação aos aços ABNT 304 e 310. A utilização de diferentes ferramentas neste trabalho mostrou influência principalmente na formação do cavaco, não tendo muita influencia nos esforços de corte e tão pouco no acabamento superficial. Os tratamentos térmicos realizados propiciaram a formação de outras fases, as quais causaram alterações na microestrutura. No entanto, esses tratamentos térmicos não alteraram de forma significativa o processo de torneamento. Finalmente, a formação de martensitas induzidas por deformação foi identificada no cavaco, mas não pode ser quantificada. / The main objective of this work is to study and evaluate the effect of cutting parameters, the cutting tool and the heat treatments in the turning process of three different types of austenitic stainless steels (ABNT 303, 304 e 310). The steels studied are structurally and microstructurally comparable. The chemical composition of the ABNT 303 and the ABNT 304 is similar except for the presence of sulfur in the ABNT 303 steel which alloeds the manganese sulfide formation. On the other hand, the ABNT 310 steel is richer in alloying elements and has lower tendency to strain induced martensite formation than the other steels studied. The steels studied were also heat treated in different conditions (annealed and aged). The materials were microstructurally characterized and Vickers hardness was also measured. The turning tests were carried out by using different cutting parameters, mainly the feedcutting depth relations. These relations lead to a plane state of tension or a plane state of deformation. The cutting and feed forces were measured during turning tests. During the tests the chips were also collected for morphological analysis through optical and scanning electron microscopies. The roughness and the surfaces characteristics were also determined to evaluate the surface finishing. The major difference in the steels turned was related to surface finishing observed by using optical and scanning electron microscopies. On the whole, the ABNT 303 steel presented the worst surface and the lowest cutting forces. However, the differences among all results were not significant. The tests carried out also showed there was not considerable difference between the tools used except for the chip morphology. The heat treatments led to precipitation in the steels studied and changes in their microstructure. However, the microstructural changes hardly affected the results of the turning tests. Finally, the martensite formation was detected although this phase could be not quantified.

Abstract This thesis studies controlling factors that govern transverse hydrogen cracking in high-strength multipass weld metal (WM). The experiments were concerned with heavy-restraint Y- and U-Groove multipass cracking tests of shielded-metal arc (SMAW) and submerged-arc (SAW) weld metals. Results of tensile tests, hardness surveys, weld residual stress measurements and microstructural investigations are discussed. The analytical phase comprised numerical calculations for analysing the interactions between crack-controlling factors. The objectives were: (i) the assessment of WM hydrogen cracking risk by defining the Crack-No Crack boundary conditions in terms of 'safe line' description giving the desired lower-bound estimates, and (ii) to derive predictive equations capable of giving reliable estimates of the required preheat/interpass temperature T0/Ti for the avoidance of cracking. Hydrogen cracking occurred predominantly in high strength weld metals of Rp0.2 ≈ 580-900 MPa. At intermediate strengths of Rp0.2 ≈ 500-550 MPa, cracking took place in the cases where the holding time from welding to NDT inspection was prolonged to 7 days. Low strength WMs of Rp0.2 ≤ 480 MPa did not exhibit cracking under any conditions examined. Cracking occurrence was, above all, governed by WM tensile strength, weld diffusible hydrogen and weld residual stresses amounting to the yield strength. The appearance of cracking vanished when transferring from 40 to 6 mm thick welds. The implications of the holding time were more significant than anticipated previously. A period of 16 hrs in accordance with SFS-EN 1011 appeared much too short for thick multipass welds. Interpass time and heat input showed no measurable effect on cracking sensitivity, hence being of secondary importance. Equations were derived to assess the weld critical hydrogen content Hcr corresponding to the Crack-No Crack conditions as a function of either weld metal Pcm, yield strength Rp0.2 or weld metal maximum hardness HV5(max). For the calculation of safe T0/Ti estimates, a formula incorporating: (i) WM strength as a linear function of either weld carbon equivalent CET or weld HV5(max), (ii) weld build-up thickness aw in the form of tanh expression and (iii) weld diffusible hydrogen HD in terms of a combined [ln / power law] expression was found descriptive.

The crack-tip displacement concept has been applied to austenitic steels at 25°C and in the temperature range 400-800°C. The measurement of a maximum load crack-tip displacement in a notch bend test, provided a good indication of fracture-toughness since it included a portion of slot: crack-growth. The ability of these alloys to tolerate slow crack-growth, and even to arrest cracks without becoming unstable, is of considerable engineering importance since many service failures originate at stress concentrations produced by welding of poor design. Slow crack-growth was intermittent and highly dependent upon microstructural irregularities in the immediate vicinity of the crack-tip. The stress concentration at the crack-tip could be relieved (and the fracture-toughness improved) by localized plastic deformation. The degree of stress relief depended upon the locality and proximity of the various microstructural features as determined by the alloy manufacturing process. The temperature sensitivity of the bond strengths of the various interfaces particularly in cast alloys, had a marked-effect on fracture-toughness. This may have been the result of segregation of trace elements e.g. lead to the interface. Above the equicohesive temperature, the greatest contribution to fracture-toughness was associated with the presence of large amounts of second phase particles in the boundaries. In many cases, and particularly cast alloys, more than one crack formed at the notch root. Only one of these cracks propagated to failure. Heterogeneous cracking of this kind (itself an indication of fracture-toughness), lead to difficulties in correlating an initiation C. O. D. with the macroscopic plastic properties of the material. Similar correlations were however possible with the maximum load crack opening displacement.

Lors du traitement de nitruration, la diffusion de l'azote dans les aciers entraîne la transformation des carbures de revenu en nitrures. Durant cette transformation, du carbone est relâché dans la matrice ferritique. L'étude expérimentale a mis en avant que cette décarburation est observable quel que soit le type de nitruration et pouvait aller jusqu'à 20 % dans le cas où la couche nitrurée ne comportait pas de couche de combinaison. Cette décarburation est induite par la réaction du carbone relâché au cours de la transformation de la cémentite avec l'hydrogène issu de la décomposition de l'ammoniac pour former une espèce carbonée, cette réaction a lieu tant qu'aucune couche de combinaison n'est présente à la surface. Cette redistribution du carbone influe sur la microstructure et les profils de contraintes résiduelles des couches nitrurées. Grâce aux résultats expérimentaux, ce phénomène a été implémenté dans le modèle de simulation de la nitruration développé au laboratoire. Cette implémentation porte essentiellement sur les conditions initiales et aux limites qui ont été obtenues en complétant les résultats expérimentaux par une simulation thermodynamique permettant de simuler des profils d'azote et de carbone proches de ceux obtenus expérimentalement. Le modèle permet également de calculer la variation de volume accompagnant la précipitation et ainsi de calculer les champs des contraintes résiduelles générées à la température de nitruration et leurs modifications lors du refroidissement. Le caractère polyphasé du matériau est pris en compte, la simulation permettant de connaître les contraintes résiduelles dans la ferrite, les précipités et les contraintes résiduelles macroscopiques grâce à un modèle micromécanique de transition d'échelles de type auto-cohérent. Cette approche multiphysique est applicable à l'ensemble des aciers au carbone allié (Cr, Mo, V). Ce modèle a été plus particulièrement appliqué à la nuance industrielle 33CrMoV12-9. L'ensemble de cette étude a permis de comprendre l'influence du carbone sur les propriétés mécaniques des couches nitrurées et de mettre au point un cycle industriel de nitruration en se basant sur les résultats expérimentaux et la simulation. / During the nitriding treatment, the diffusion of nitrogen in the steels causes the transformation of initial carbides into nitrides. During this transformation, carbon is released into the ferritic matrix. The experimental study has highlighted that the decarburization of the nitride layer occurs regardless of the type of nitriding and could reach 20% when the nitriding surface is not composed of compound layer This decarburization is induced by the reaction of the carbon released during the transformation of the cementite, with the hydrogen produced by the decomposition of ammonia to give a carburized species ?, this reaction occurs as long as any compound layer exists at the surface of the sample. This carbon redistribution has an influence on the microstructure and the residual stresses of the nitride layers. Based on experimental results, this phenomenon has been implemented in the nitriding simulation model developed in the laboratory. This implementation focuses on initial and boundary conditions obtained by complementing the experimental results with a thermodynamic simulation, to simulate nitrogen and carbon profiles close to those obtained experimentally. The model also calculates the volume change due to ? the precipitation and calculates the fields of residual stresses generated at the nitriding temperature and their evolution during cooling.. The multiphase character of the material is taken into account; the simulation allowing knowing the residual stresses in the ferrite, the precipitates and macroscopic residual stresses through a micromechanical model of scale transition like self-consistent. This multiphysics approach is applicable to all alloy carbon steels (Cr, Mo, V). This model has specifically been applied to industrial grade 33CrMoV12-9. The entire study allows understanding the influence of carbon on the mechanical properties of nitrided layers and the development of an industrial nitriding cycle based on experimental results and simulation

La thèse porte sur deux aciers emboutissables à chaud, soudés en configuration homogène ou hétérogène en termes de composition chimique et d'épaisseur. Les solutions en flans raboutés laser présentent en effet de remarquables performances à l'impact et connaissent un fort développement dans le contexte actuel de l'industrie automobile (réduction des émissions de CO2 et amélioration de la sécurité passive des véhicules). L'opération de soudage laser peut générer une hétérogénéité de la jonction soudée, due au mélange imparfait des deux matériaux et des conditions thermiques de solidification et d'emboutissage à chaud. Les propriétés mécaniques du joint soudé sont donc déterminées par la qualité du mélange, la composition chimique locale et le cycle thermique.La première partie de l'étude est consacrée à la quantification de l'hétérogénéité du joint soudé et la compréhension de la microstructure. Une nouvelle méthodologie a été développée pour étudier le comportement métallurgique et mécanique de ces joints hétérogènes, en élaborant des coulées synthétiques représentant les différentes compositions chimiques attendues dans le joint réel. Le comportement du joint soudé est reconstruit à partir des données obtenues par la caractérisation de ces coulées synthétiques. La deuxième partie de l'étude porte sur la compréhension de la formation de la microstructure de la zone fondue avant et après traitement thermomécanique simulant l'emboutissage à chaud. Des modèles quantitatifs ont été établis pour calculer les températures de changement de phase, les proportions relatives des constituants microstructuraux ainsi que la dureté de ces alliages en fonction de la composition chimique et du cycle thermique. La dernière partie de l'étude porte sur le comportement mécanique après traitement thermique. Des lois de comportement des matériaux synthétiques ont été déterminées en fonction de leur composition chimique et du cycle thermique. La sensibilité à la rupture fragile par clivage a été évaluée par des essais de traction sur éprouvettes sévèrement entaillées. Les lois de comportement obtenues ont été appliquées pour déterminer la tolérance du joint soudé à un défaut géométrique, sous sollicitation de traction uniaxiale. / This thesis is focused on the study of welded steel grades deformed by hot stamping. Typically, a laser welded blank is formed by butt joining two steel sheets, which can be identical or differ in chemical composition and/or sheet thickness. Such laser welded blank solution offers excellent crash performance, significant CO2 emission reduction and passive car safety thus it is of great interest for the automotive industry. The laser welding process may induce chemical and metallurgical heterogeneities arising from an incomplete mixture of the two base metals and from the thermal cycle conditions during welding and the subsequent heat treatment. The mechanical behaviour of the weld is therefore determined by the mixing quality, the chemical composition and the thermal cycle.The first part of the study aims at the quantification of the weld heterogeneity and the characterisation of the resulting microstructure. In this work, a new method is proposed to study the metallurgical and mechanical behaviour of those heterogeneous welds, by elaborating synthetic casted alloys representative of the different chemical compositions that can be locally found in the weld. The behaviour of the weld is then reconstructed from the results obtained from the characterisation of those synthetic casted alloys. The second part of the study concerns the understanding of the microstructure formation in the molten zone before and after a thermo-mechanical treatment which replicates the hot stamping conditions. Quantitative models have been established to calculate the phase transformation temperatures, the proportion of the principal constituents in the microstructure, and hardness of the weld as a function of chemical composition and thermal cycle parameters. The last part of the study is dedicated to the evaluation of the mechanical behaviour of the synthetic alloys after heat treatment. The constitutive material behaviour laws for each alloy have been identified. The sensitivity to brittle cleavage fracture has been assessed by tensile tests on severely notched bars. The constitutive material models are then applied to determine the sensitivity of the weld to geometrical defects under uniaxial loading.

Les métaux à l’état semi-solide présentent un comportement rhéofluidifiant caractérisé par une forte chute de la viscosité avec la vitesse de déformation facilitant le remplissage des matrices lors de la mise en forme. L’exploitation de ce comportement donne lieu à un procédé de mise en forme appelé « thixoforgeage ». L’état semi-solide est obtenu en refusion partielle à partir de l’état solide et la fraction de solide est supérieure à 0.8. Les plus hautes températures mises en jeu dans le cas des matériaux à haut point de fusion comme les aciers rendent la maîtrise du procédé plus complexe. Cependant, les travaux antérieurs sur le thixoforgeage d’aciers ont montré le potentiel de ce procédé pour réduire la consommation en matière première et en énergie. La thèse s’inscrit dans le cadre du projet TACA «Thixoforgeage d’Aciers pour la fabrication de Composants Automobiles» piloté par l’IRT-M2P. Il ambitionne le développement industriel du thixoforgeage des aciers pour la fabrication de pièces automobiles. La maîtrise et le développement du thixoforgeage nécessite une bonne connaissance du comportement mécanique du matériau à l’état semi-solide et le développement d’outils de simulation numérique adaptés. Ce travail de thèse a pour objectifs de (i) caractériser expérimentalement le comportement thermomécanique des aciers à l’état semi-solide, (ii) développer un modèle de comportement destiné à être implanté dans le logiciel FORGE® pour simuler le thixoforgeage. Une attention particulière a été portée sur le comportement en traction pour caractériser l’intervalle de température dans lequel le matériau devient très sensible à la fissuration à chaud. Des essais en traction menés à différentes températures ont permis de déterminer la température à partir de laquelle la résistance et la ductilité du matériau chutent drastiquement. Les mécanismes conduisant à ces chutes ont été identifiés et sont conformes à ceux décrits dans la littérature. Un modèle basé sur une approche d’homogénéisation qui prend en compte explicitement le rôle mécanique des phases liquide et solide a été développé. Ce modèle repose sur une approche viscoplastique établie antérieurement puis enrichie afin (i) d’intégrer le comportement élastique du squelette solide saturé en liquide et (ii) distinguer les évolutions de distribution spatiale des phases liquide et solide selon le trajet de chargement en traction ou en compression. Il permet de décrire avec succès, pour la première fois, les trois stades de la réponse mécanique en traction (augmentation, stabilisation puis chute de la contrainte en fonction du déplacement). Le modèle a ensuite été implanté dans le code éléments finis FORGE®. Les simulations des essais de traction GLEBBLE ont permis d’identifier les paramètres du modèle. Des comparaisons des résultats expérimentaux et numériques ont permis de reproduire des phénomènes de localisation de la déformation réelle. Après la validation sur des essais de traction, des simulations de procédés de thixoforgeage industriel, tels que le forgeage de U, ont été étudiées et comparées aux résultats expérimentaux réalisés sur la plateforme Vulcain de l'ENSAM de Metz. Un critère permettant de définir des zones sensibles à la fissuration à chaud a été proposé. La comparaison avec des observations expérimentales a montré que ce critère constitue une première approche encourageante pour prédire les zones de fragilité de la pièce en thixoforgeage. / Semi-solid metals and alloys exhibit a shear thinning behavior characterized by a sharp drop in viscosity with increasing strain rate. This property promotes a smooth die filling during forming. To exploit this advantage, several semi-solid forming process have been developed. Among these processes, we find the thixoforging when the semi-solid state is obtained by a partial remelting from solid state. The solid fraction is above 0.8. Thixoforging of high melting point alloys such as steels is particularly challenging because of about 1400°C temperatures involved. However, previous works showed that this process reveals high potential to reduce material as well as energy consumption. The present PhD thesis is part of a French research project named TACA «Thixoforging of steels for fabrication of automative parts» leaded by IRT-M2P. It aims at industrial development of steel thixoforging for manufacturing automotive components. The mastery and the development of steel thixoforging require a good knowledge of the mechanical behavior of semi-solid steels and appropriate numerical tools to simulate the process. The PhD work aims to (1) characterize the thermomechanical behavior of semi-solid steels and (2) develop constitutive equations that have to be implemented into the commercial code FORGE® to simulate thixoforging. A special attention was paid to the tensile behavior to investigate the temperature range in which the material is very sensitive to hot cracking. Tensile tests provided the temperature from which the material lost its tensile strength and its ductility. Mechanisms leading to the drop of these two properties were identified and were found to be consistent with mechanisms described in literature. A model based on homogenization approach, namely taking explicitly into account the mechanical role of the liquid and solid phases was developed. This model is based on a viscoplastic approach previously developed that was enhanced to (1) include the elastic response of the solid skeleton saturated with liquid and to (2) distinguish the evolution of the spatial liquid/solid distribution according to the tensile or compressive loading path. It successfully describes the three stages of the response in tension: increase, stabilization and decrease of the stress with increasing displacement. The model was implemented in the FORGE® finite element code. The experimental tensile tests were simulated to provide identification of the model parameters. The simulation results showed that strong deformation localization zones were predicted consistently with experiments. Simulations of thixoforging industrial processes such as forging U were studied and compared with experimental results achieved on the Vulcan platform (ENSAM Metz). In addition, a criterion determining the zones without any tensile strength and so sensitive to hot cracking was proposed. Comparison with experimental observations showed that this criterion is an encouraging first approach to predict the brittle zones of thixoforging parts.

Dans le cadre de ces travaux, il a clairement été établi que l’hydrogène piégé ou diffusible pouvait avoir une forte influence sur les propriétés mécaniques des matériaux. Cependant, cet effet varie de façon importante en fonction de leur microstructure, leur composition chimique et leur traitement thermique. En effet, les aciers martensitiques trempés/revenus dédiés à des tubes pour des milieux sous-service présentent, de par leur structure, différents types de pièges tels que les dislocations, les joints de grains, les précipités, les inclusions, les lacunes et d’autres interfaces qui jouent un rôle important dans les mécanismes endommageants. Ces aciers de haute résistance mécanique, lorsqu’ils sont soumis à des contraintes mécaniques et à un environnement agressif (qui dépend de la pression en H2S et du pH de la solution) peuvent rompre à cause du phénomène de Sulphide Stress Cracking (SSC). Ce dernier est une forme de fragilisation par l’hydrogène (FPH) qui inclut un amorçage de fissure suivi d’une étape de propagation conduisant à la rupture, dont la contribution de l’hydrogène reste encore mal comprise. En parallèle de l’impact de la microstructure de l’acier, les champs de contrainte et déformation subis par le matériau modifient les effets induits par l’hydrogène. C’est pourquoi un montage de perméation sous contrainte a été utilisé afin de pouvoir réaliser des essais mécaniques jusqu’à rupture sous flux d’hydrogène et les comparer au comportement du matériau lorsque celui-ci est sollicité à l’air ou dans un environnement H2S. Ainsi, l’impact sur le comportement mécanique du flux d’hydrogène mais également de son piégeage peut être étudié. Dans ce cadre, des éprouvettes plates et axisymétriques, lisses et entaillées ont été employées. Les informations expérimentales obtenues dans ce travail ont servi à alimenter un modèle numérique qui a permis de caractériser localement l’état mécanique et les concentrations d’hydrogène piégé et diffusible dans le matériau. Ceci a rendu possible la définition d’un critère local de rupture. / The findings of this work established that the diffusible and trapped hydrogen could have a strong influence on the mechanical properties of materials. However, this effect varies significantly with the materials’ microstructure, chemical composition, and heat treatment. Due to their structure, quenched and tempered martensitic steels (developed for tubes suitable for sour service environments) have different types of traps such as dislocations, grain boundaries, precipitates, inclusions, vacancies and other interfaces that play an important role in the damage mechanisms. These high strength steels may break due to Sulphide Stress Cracking (SSC) if subjected to mechanical stress and an aggressive environment (which depends on the H2S partial pressure and pH solution). This phenomenon is a form of hydrogen embrittlement (HE) that includes a crack initiation followed by a propagation step leading to failure. However the hydrogen contribution is still insufficiently understood. In addition to the impact of the microstructure on the steel, the stress and the deformation fields in the material also modify the effects induced by hydrogen. To investigate this event, electrochemical permeation tests under stress were used to perform mechanical tests under hydrogen flux until failure is reached. The results were compared to those mechanically loaded in air or in a H2S environment. This enabled the examination of the impact of the hydrogen flux and trapping on the mechanical behavior of martensitic steel. In this framework, flat and axisymmetric, smooth and notched specimens were employed. Experimental data obtained in this work were used to provide a numerical model that enables the locally characterization of the mechanical condition and the concentrations of trapped and diffusible hydrogen in the material. These outcomes enabled us to determine a local failure criterion.