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URL : https://hal.archives-ouvertes.fr/hal-01668802
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Compléments sur le protocole de chargement en hydrogène à 500°C ,
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Répartition de l'hydrogène dans les échantillons en Zy4 à l'issue du chargement, p.254 ,
Traitement thermique d'homogénéisation de l'hydrogène ,
Mise au point du protocole d'homogénéisation des matériaux « modèles » chargés en oxygène et en hydrogène ,
Compléments sur la mise en capsule des échantillons avant traitement thermique ,
Compléments sur la microstructure des échantillons en M5Framatome à l'issue du traitement thermique à 1200 -1300°C ,
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, Principes de détermination des températures de dissolution et de précipitation des hydrures
Températures de disparition au chauffage et d'apparition au refroidissement des hydrures pour le M5Framatome contenant plus de 5000 ppm-mass ,
Compléments sur les résultats des essais de calorimétrie effectués sur Zy4 préhydruré, p.266 ,
Lien entre l'enthalpie et la teneur globale en hydrogène ,
Microstructure des échantillons analysés aux diffractions de neutrons et DRX ,
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Courbes des essais de traction uniaxiale en température ,
Compléments sur les corrélations et la modélisation ,
Compléments sur la loi de comportement mécanique ,
Corrélations et modélisation exprimées en fonction des concentrations atomiques en hydrogène et oxygène, p.253 ,
, Limite d'élasticité Rp0,2 et résistance mécanique Rm
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, Teneur en hydrogène (CH) dans les tubes en Zy4 et M5Framatome chargés en oxygène à 0,9 et 1,1 %-mass. avant et après les traitements thermiques effectués à 1300°C, vol.1
, 2007) fonctionne très bien pour les cas des tubes en M5Framatome et en Zy4 oxydés à moins de 0,5 %-mass., mais il doit être amélioré et adapté pour les matériaux préhydrurés ou contenant de fortes teneurs en oxygène
Tentatives d'optimisation du protocole Pour tenter d'homogénéiser les tubes en Zy4 contenant 0,9 %-mass. d'oxygène, de nouveaux traitements thermiques ont été réalisés sur des tubes en Zy4 oxydés à 0,8 -1,07 %-mass., mais cette fois-ci avec une durée de maintien à 1300°C de ,
, On constate toujours la présence de couches de phase ?Zr(O) d'environ 150 ?m d'épaisseur à l'extérieur et à l'intérieur des tubes, comme observé après traitement de 3h à 1300°C pour le Zy4 oxydé à 0,86 %-mass. (Figure B.2). Il semble donc que la phase ?Zr soit déjà saturée en oxygène à 1300°C, comme le prévoient d'ailleurs les calculs thermodynamiques à l'équilibre effectués avec Thermo-Calc et Zircobase (Figure B.5), Plusieurs mesures de microdureté Vickers 100g ont été effectuées le long d'une direction à 45° dans le plan radial-circonférentiel, balayant ainsi toute l'épaisseur des échantillons ; les résultats sont illustrés sur la Figure B.4
, Une nouvelle tentative a donc consisté à traiter les échantillons (oxydés sous vapeur d'eau à 1000°C) à 1400 ou 1500°C dans un four nommé I2T-Ox (CEA/DEN/DMN/SRMA/LA2M), sous hélium, vol.99, p.9999
, Une prise d'oxygène très importante, conduisant à une teneur en oxygène moyenne déduite de gain de masse de l'ordre de 3 -4 %-mass., a été relevée sur ces échantillons
Compléments sur les essais de calorimétrie précipiter, 2014. ,
L'identification des points MST et PT est plus facile et objective. De nombreux auteurs utilisent MST, considérant qu'elle est proche de la moyenne de CT et PT, pour déterminer la TSSD et la TSSP, comme fait par exemple pour interpréter les courbes de DSC obtenues sur des échantillons en Zy2, Zy4 et Zr-2,5Nb (Zr-2,5 %-mass. de Nb) préhydrurés à des teneurs en hydrogène allant jusqu'à environ 700 ppm-mass., avec une température maximale lors des cycles thermique de 500 -600°C et une vitesse de chauffage ou de refroidissement de 10 -20°C/s, MST et PT (cf. Figure IV.6 et Figure IV.7) devraient être identiques, 1967. ,
PT obtenus à partir d'expériences de DSC effectuées sur du Zr-2,5Nb préhydruré à des teneurs en hydrogène inférieures à 1000 ppm-mass., en appliquant une température maximale de 340°C et une vitesse de chauffage et de Vierge 0 ,