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AvaliaÃÃo da fragilizaÃÃo por hidrogÃnio no aÃo maraging 300 / Evaluation of hydrogen embrittlement of 300 maraging steelLuis Paulo MourÃo dos Santos 23 May 2014 (has links)
CoordenaÃÃo de AperfeiÃoamento de NÃvel Superior / Os aÃos maraging sÃo ligas de ultra-alta resistÃncia com vasta aplicaÃÃo na engenharia, desde vasos de alta pressÃo de operaÃÃo em processos crÃticos, componentes aeronÃuticos, aplicaÃÃes militares atà equipamentos esportivos. O presente trabalho buscou avaliar os efeitos da fragilizaÃÃo por hidrogÃnio no aÃo maraging 18% Ni da classe 300, nas condiÃÃes solubilizada e envelhecida. As amostras foram solubilizadas a 1093 Â10K por 3,6 ks, seguido de um resfriamento ao ar e envelhecidas a 753 e 843 Â10K por 10,8 ks, respectivamente e resfriadas ao ar. Foi realizada uma caracterizaÃÃo microestrutural por difraÃÃo de raios-X, correntes parasitas, medidas de dureza Rockwell e microscopia eletrÃnica e Ãptica. Para avaliar os efeitos do ingresso de hidrogÃnio nas propriedades mecÃnicas do aÃo maraging 18% Ni da classe 300 foram realizados ensaios de traÃÃo com baixa taxa de deformaÃÃo (BTD). A taxa de deformaÃÃo aplicada foi 1,0 x 10-6 s-1. Os ensaios foram realizados ao ar (meio inerte) e em soluÃÃo de 3,5% NaCl sob o potencial catÃdico de -1,2 VECS. Foi observada uma reduÃÃo de 11,06 para 3,89% no alongamento e de 61,28 para 10% na reduÃÃo de Ãrea para as amostras solubilizadas. As amostras envelhecidas a 753 Â10K por 10.8 ks apresentaram maior reduÃÃo nessas propriedades. Nesta condiÃÃo a reduÃÃo observada foi de 1929,26 MPa para amostras ensaiadas ao ar para 447,64 MPa para amostras ensaiadas em soluÃÃo de 3,5% NaCl sob potencial catÃdico no limite de resistÃncia e de 7,30 para 1,62 % no alongamento. As amostras envelhecidas a 843 Â10K, as quais apresentaram de cerca de 10% de austenita sofreram fragilizaÃÃo similar as amostras envelhecidas a 753 Â10K. Trincas secundÃrias perpendiculares a carga aplicada foram observadas nas amostras solubilizadas e ensaiadas em soluÃÃo de 3,5% NaCl sob potencial catÃdico. Os resultados indicam que a presenÃa de precipitados e de austenita revertida impedem a propagaÃÃo de trincas secundÃrias na seÃÃo longitudinal nas condiÃÃes envelhecidas. A anÃlise da superfÃcie de fratura revelou caracterÃstica de uma fratura dÃctil nas amostras ensaiadas ao ar com dimples de diferentes tamanhos e profundidades, enquanto que nas amostras ensaiadas em soluÃÃo de 3,5% NaCl sob potencial catÃdico foram observadas trincas induzidas pelo hidrogÃnio e microcavidades e regiÃes de quase-clivagem para todas as condiÃÃes estudadas. / Maraging steels are ultra high strength alloys widely used in engineering applications from high pressure vessels operating in critical processes, aircraft components, military applications to sports equipment. This work assessed the effects of hydrogen embrittlement in 18% Ni maraging grade 300 steel in the solution annealed and aged conditions. Samples were solution annealed at 1093 Â10K for 3.6 ks, followed by air cooling and aging at 753 and 843 Â10K for 10.8 ks, respectively, and cooled by air. The microstructure was characterized by X-ray diffraction, eddy current, hardness measurement and optical and electron microscopy. To assess the effects of hydrogen ingress on the mechanical properties of 18% Ni maraging grade 300 steel, slow strain rate tests (SSRT) were performed. A strain rate of 1.0x10-6 s-1 was applied. The tests were carried out in air (middle inert) and the samples immersed in the electrolyte at a simultaneous potential of -1.2 VSEC. The results showed the reduction elongation from 11.06 to 3.89% and from 61,28 to 10% in reduction of area for samples in the solution annealed condition. The greatest reductions were observed in the samples aged at 753 Â10K for 10.8 ks. In this condition the reduction from 1929.26 MPa in air tests to 447.64 MPa in ultimate tensile strength and from 7.30 to 1.62% in elongation under cathodic polarization in the 3,5% NaCl solution was observed. The samples aged at 843 Â10K for 10.8 ks, where about 10% of reverted austenite was identified, showed evidence of hydrogen embrittlement as seen in the samples treated at different conditions. Secondary cracks, perpendicular to the loading direction at the longitudinal surface of the solution annealed fractured samples immersed in 3,5% NaCl solution under cathodic potential were seen. The results evidence that the precipitates and reverted austenite difficult secondary crack propagation in longitudinal section on aged samples. Scanning electron examination showed a change in fractografic features from ductile dimples to quasi-cleavage and microvoid modes when comparing samples without (air tested) and with hydrogen ingress.
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Corrosion sous contrainte et fragilisation par l'hydrogène d'alliages d'aluminium de la série 7xxx (Al-Zn-Mg) : identification des paramètres microstructuraux critiques pilotant l'endommagement à l'échelle locale. / Stress Corrosion Cracking and Hydrogen Embrittlement of a 7xxx (Al-Zn-Mg) aluminium alloy : identification of microstructural parameters controlling the damage at a local scale.Oger, Loïc 23 November 2017 (has links)
Dans un contexte normatif toujours plus sévère concernant les rejets automobiles polluants, la substitution des aciers par des alliages d’aluminium dans les structures des véhicules est en plein essor. Ce projet de thèse, qui s’inscrit dans un programme de développement de la société Constellium, cible plus précisément les alliages d’aluminium de la série 7xxx (Al-Zn-Mg) qui, malgré leurs propriétés mécaniques élevées, peuvent présenter une sensibilité à la corrosion sous contrainte (CSC) liée au phénomène de fragilisation par l’hydrogène (FPH). La compréhension des mécanismes mis en jeu dans ce type d’endommagement constitue donc une première étape vers une optimisation métallurgique en vue d’une industrialisation future de ces alliages dans le secteur automobile. La première partie de ces travaux est consacrée à l’étude de l’influence de l’état métallurgique de l’alliage 7046 sur son comportement en CSC et à l’identification des mécanismes de dégradation. Un lien direct a pu être mis en évidence entre l’abattement des propriétés mécaniques et les modes de rupture actifs et la quantité d’hydrogène dans l’alliage. Les deux modes d’endommagement observés, intergranulaire-fragile et transgranulaire-fragile, ont respectivement été attribués à un enrichissement en hydrogène aux joints de grains et au piégeage de l’hydrogène au niveau des précipités intragranulaires. Les interactions entre l’hydrogène et les précipités fins d’une part et les dislocations d’autre part, identifiés comme deux hétérogénéités microstructurales critiques vis-à-vis de la FPH, ont été étudiées à une échelle plus locale dans la seconde partie du travail de thèse. Les essais ont été réalisés sur des échantillons modèles, chargés en hydrogène en milieu H2SO4 sous polarisation cathodique et la profondeur de pénétration de l’hydrogène a été évaluée par SKPFM (Scanning Kelvin Probe Force Microscopy). L’ensemble des résultats obtenus met en évidence : 1/ un effet « barrière » des précipités fins et des dislocations sur la diffusion de l’hydrogène en relation avec un abattement des propriétés mécaniques moins important, 2/ un transport possible de l’hydrogène par les dislocations et 3/ l’efficacité du SKPFM pour déterminer précisément des coefficients de diffusion apparents de l’hydrogène. Ces résultats ouvrent ainsi de nouvelles pistes vers la compréhension des mécanismes de CSC dans les alliages Al-Zn-Mg. / Automotive industry is increasingly affected by standards requiring a major cut of polluting emissions, leading R&D policies to focus on replacing steel by aluminum alloys. This thesis project, initiated by the manufacturer Constellium, focuses on 7xxx (Al-Zn-Mg) aluminum alloys known to have high mechanical properties but also to be susceptible to stress corrosion cracking (SCC) partly attributed to hydrogen embrittlement (HE). Understanding the mechanisms involved would be a first step towards a metallurgical optimization and a future industrialization of these alloys. The first part focuses on the SCC behavior of the 7046 aluminum alloy, related to its microstructure, and the identification of degradation mechanisms involved. A hydrogen amount – loss of mechanical properties relationship was highlighted. The damage observed was explained by the presence of hydrogen in the grain boundaries and by a trapping effect of the intragranular hardening precipitates, limiting the hydrogen diffusion to the grain boundaries. Interactions between hydrogen and hardening precipitates and dislocations, both identified as critical microstructural heterogeneities for HE, are studied at a local scale in a second part. The hydrogen effect was characterized by penetration depth measurements made by SKPFM (Scanning Kelvin Probe Force Microscopy) on “model” samples cathodically charged in H2SO4. The whole results finally highlight: 1/ a “shielding” effect of fine precipitates and dislocations on hydrogen diffusivity related to a lower susceptibility to HE, 2/ hydrogen transport by dislocations and 3/ the efficiency of SKPFM to precisely measure effective diffusion coefficients of hydrogen. These results lead to new opportunities to understand SCC mechanisms in Al-Zn-Mg alloys.
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