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Etude Des Évolutions Microstructurales Sous Irradiation De L’Alliage D’Aluminium 6061-T6

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Etude Des Évolutions Microstructurales Sous Irradiation De L’Alliage D’Aluminium 6061-T6 THÈSE Pour obtenir le grade de DOCTEUR DE L’UNIVERSITÉ GRENOBLE ALPES Spécialité : Matériaux, Mécanique, Génie Civil, Electrochimie (2MGE) Arrêté ministériel : 7 août 2006 Présentée par Camille FLAMENT Thèse dirigée par Alexis DESCHAMPS et codirigée par Jérôme GARNIER et Joël RIBIS préparée au sein du Laboratoire d’étude du Comportement Mécanique des Matériaux (CEA) dans l'École Doctorale Ingénierie, Matériaux, Mécanique, Energétique, Environnement, Procédés, Production (I-MEP2) Etude des évolutions microstructurales sous irradiation de l’alliage d’aluminium 6061-T6 Thèse soutenue publiquement le 01 décembre 2015, devant le jury composé de : M. Alexis DESCHAMPS Professeur à l’INP de Grenoble, Directeur Mme. Myriam DUMONT Maître de conférences à l’Université Aix-Marseille, Rapporteur M. Thierry EPICIER Directeur de recherche au CNRS, Président M. Jérôme GARNIER Ingénieur de recherche au CEA, Co-encadrant M. Alexandre LEGRIS Professeur à l’Université Lille 1, Rapporteur M. Joël RIBIS Ingénieur de recherche au CEA, Co-encadrant REMERCIEMENTS Remerciements Cette thèse a été réalisée au Service de Recherches Métallurgiques Appliquées (SRMA) du Département des Matériaux pour le Nucléaire du CEA Saclay (DMN). Je souhaite donc tout d’abord remercier Messieurs Philippe Chapelot et Pascal Yvon de m’avoir accueillie respectivement au SRMA et DMN. Je remercie également Madame Laetitia Nicolas, ex-chef du Laboratoire d’étude du Comportement Mécanique des Matériaux qui fut mon laboratoire de rattachement et Monsieur Jean- Luc Béchade, ex-chef du Laboratoire d’Analyse Microstructurale des Matériaux (dorénavant chef du Service de Recherche de Métallurgie Physique) au sein duquel j’ai pu m’installer et utiliser les différents outils de caractérisation. Je tiens à remercier Monsieur Thierry Epicier, directeur de recherches à l’INSA de Lyon, de m’avoir fait l’honneur de présider mon jury de thèse, ainsi que Monsieur Alexandre Legris, professeur de l’Université Lille 1 et Madame Myriam Dumont, maître de conférences à l’Université d’Aix Marseille d’avoir accepté d’évaluer ce travail en qualité de rapporteurs. Je suis extrêmement reconnaissante envers Monsieur Alexis Deschamps, professeur à l’Université Grenoble-Alpes, d’avoir accepté de diriger la thèse. Toujours disponible pour répondre à mes interrogations, son regard aiguisé et ses conseils ont permis de tirer à chaque fois le meilleur profit des résultats. Je souhaite également exprimer ma gratitude à mes encadrants Jérôme Garnier et Joël Ribis, ingénieurs de recherche au SRMA. Sans leur soutien, leur implication, leur confiance et leur enthousiasme ce travail de thèse n’aurait pu aboutir. J’ai beaucoup appris au cours de nos discussions tant sur le monde de l’irradiation que sur le métier de chercheur. Je tiens également à remercier Bruno Maugard, chef du projet MTRH, pour l’intérêt qu’il a porté à mes résultats expérimentaux tout au long de la thèse. Je remercie l’ensemble des chercheurs et techniciens du SRMA pour leur aide et plus particulièrement Jean Henry, Thierry Vandenberghe et Justine Roubaud pour les irradiations in-situ au THT ; Benoit Arnal pour la préparation des pointes SAT au FIB ; Alexandra Renault et Sylvie Doriot en charge des Microscopes Electroniques en Transmission ; Karl Buchanan et France Dalle pour leur contribution dans le dépouillement des données SAT ; Elodie Rouesne pour les essais EBSD. Je tiens à remercier chaleureusement tous les permanents et non permanents du LA2M qui ont rendu l’atmosphère de travail très agréable. REMERCIEMENTS Ce travail de thèse a fait l’objet de nombreuses collaborations. Je tiens donc à remercier le SRMP-Jannus Saclay et plus particulièrement Yves Serruys, Frédéric Leprêtre, Eric Bordas et Hervé Martin pour les irradiations aux ions ex-situ ; le CSNSM-Jannus Orsay et plus particulièrement Aurélie Gentils, Cédric Baumier et Odile Kaïtasov pour la réalisation des irradiations in-situ ; Sylvie Poissonnet pour les essais de nano-indentation sur lames minces au DMN/SRMP ; Annabelle Lopez et Kimberly Colas pour les analyses en Sonde Atomique au DMN/SEMI ; Dominique Mangelinck et Marion Descoins pour les analyses en Sonde Atomique à l’IM2NP Marseille ; Patricia Donnadieu pour ses précieux conseils en Microscopie Electronique en Transmission ; Frédéric De Geuser pour les analyses en Diffusion de Neutrons aux Petits Angles réalisées à l’ILL et pour son regard sur les résultats obtenus en SAT ; Marie-Hélène Mathon pour les analyses DNPA réalisées au LLB. Je souhaiterais également remercier Loïc Perrière, ingénieur de recherche à l’ICMPE, pour son aide dans l’élaboration d’alliages d’aluminium 6061 enrichis en Si réalisée par la technique de trempe sur roue. Je souhaite remercier de tout cœur mes amis qui m’ont soutenue pendant ces trois années et ce jusqu’au jour de la soutenance. Et enfin un grand merci à mes parents qui m’ont toujours poussée à donner le meilleur de moi-même. SOMMAIRE Sommaire Introduction……………………………………………………………………..5 Chapitre 1. L’alliage d’aluminium 6061-T6 : microstructure et stabilité sous irradiation……………………………………………………………….............9 1.1. Les alliages d’aluminium Al-Mg-Si-Cu .................................................................... 10 1.1.1. Généralités sur l’alliage d’aluminium .......................................................................................10 1.1.2. La séquence de précipitation dans les alliages Al-Mg-Si-Cu ....................................................11 1.2. L’alliage d’aluminium 6061-T6 ................................................................................. 14 1.2.1. Traitements thermomécaniques .................................................................................................15 1.2.2. Description des précipités en présence dans l’alliage à l’état T6 ..............................................18 1.3. Effets d’irradiation sur les alliages Al-Mg-Si-(Cu) ................................................. 27 1.3.1. Généralités sur l’irradiation : création de dommages et stabilité des phases ............................27 1.3.2. Stabilité de l’alliage 6061-T6 en condition réacteur .................................................................39 1.3.3. Comportement de l’alliage sous irradiation aux ions ................................................................45 1.4. Conclusions du chapitre 1 .......................................................................................... 47 1.5. Références bibliographiques du chapitre 1 .............................................................. 48 Chapitre 2. Matériau de l’étude et moyens expérimentaux………………...55 2.1. Matériau de l’étude .................................................................................................... 56 2.1.1. Composition et taille de grains ..................................................................................................56 2.1.2. Traitements thermomécaniques à l’origine de la nuance J47 ....................................................57 2.2. Conditions des irradiations expérimentales ............................................................. 57 2.2.1. Irradiation in-situ aux électrons .................................................................................................57 2.2.2. Irradiations aux ions ..................................................................................................................58 2.2.3. Irradiations aux neutrons ...........................................................................................................60 2.3. Caractérisation des précipités ................................................................................... 61 2.3.1. Mesure de la taille et de la densité des précipités ......................................................................61 2.3.2. Caractérisation de la structure des précipités ............................................................................63 2.3.3. Caractérisation de la chimie des précipités ...............................................................................64 2.4. Références bibliographiques du chapitre 2 .............................................................. 66 1 SOMMAIRE Chapitre 3. Stabilité des dispersoïdes sous irradiation aux ions et aux électrons……………………………………………………………………………………....69 3.1. Caractérisation des dispersoïdes à l’état non irradié .............................................. 70 3.1.1. Taille et dispersion ....................................................................................................................70 3.1.2. Structure des dispersoïdes et de l’interface dispersoïde/matrice ...............................................72 3.1.3. Composition chimique des dispersoïdes ...................................................................................75 3.1.4. Hétérogénéité de distribution des éléments : Mise en cœur/coquille ........................................79 3.2. Stabilité des dispersoïdes sous irradiation ............................................................... 83 3.2.1. Stabilité des dispersoïdes après irradiation aux ions (165 dpa) .................................................83 3.2.2. Stabilité de la structure cœur/coquille sous irradiation aux électrons (150 dpa) .......................87 3.3. Conclusions du chapitre 3 .......................................................................................... 95 3.4. Références bibliographiques du chapitre 3 .............................................................. 96 Chapitre 4. Stabilité
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