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Fluage d'aciers renforcés par dispersion nanométrique : caractérisation, modélisation et optimisation de la microstructure

Abstract : Within the French research program for Sodium Fast Reactor (SFR) core material, oxide dispersion strengthened (ODS) steels are considered for their resistance to irradiation swelling and their good creep properties at high temperature. Their elaboration, their processing and their creep mechanism still represent challenges for material science. The aim of this work is to improve the understanding of the creep mechanisms and to investigate new fabrication route to improve these materials.First, the creep of dispersion strengthened ferritic steels produced by mechanical alloying and extrusion is studied, based on two ODS steels with 14wt.%Cr and 18wt.%Cr, and a nitride dispersion strengthened (NDS) steel with 18wt.%Cr. A microstructural (SEM-EBSD-STEM) characterization has been carried out on the two ferritic ODS steels loaded at 650°C and 800°C: a low creep strain (<0.5%) and a brutal fracture are observed. The continuous decrease of the creep rate without any microstructural change indicates a late primary stage. Then the tensile and creep behaviors of the NDS ferritic steel have been studied: a superplastic deformation, up to 110%, has been evidenced at 650°C between 10-3 s-1 and 10-2 s-1, as well as a continuous dynamic recrystallization at strain rate higher than 10-2 s-1. However, during creep tests at 650°C, the NDS steel presents the same characteristics as the ODS steels: low creep strain and brutal fracture. This behavior seems to be generic for dispersion strengthened ferritic steels obtained by mechanical alloying, regardless the type of precipitate. As the deformation occurs during the primary stage, a Kocks and Mecking model has been developed based on the thermal activation of the dislocation glide after crossing the precipitate by climb or cross-slip. This model provides a physical explanation for the threshold stress observed during the creep of ODS steels. The creep strain of the two ODS steels and the NDS steel has been simulated with experimentally determined coefficients and fitted parameters. The simulated Norton laws, dislocation density and yield stress are consistent with experimental data obtained respectively by the creep tests, by dislocation density determination (STEM-EFTEM) and tensile tests. An investigation of the creep fracture mechanisms has been performed. The creep fracture was delayed using high temperature heat treatments at 1050°C between interrupted creep tests at 800°C on the Fe14Cr ODS steel and a total elongation of 1.5% has been reached by this means. By analyzing X-ray tomography and creep test after ageing treatment, it appears that the macroscopic elongated cavities and sigma phase are not likely to explain the brutal fracture, therefore a scenario based on a critical deformation is proposed. Finally, the processing difficulties of the ferritic ODS steel lead to the design of a new martensitic 11wt. % Cr ODS steel and the evaluation of a new atomization process (GARS). This new atomization process did not improve the mechanical properties of these steels. However, after milling, encouraging results are observed since the first mechanical and microstructural characterizations displayed good tensile and creep properties.
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Submitted on : Monday, May 9, 2016 - 11:41:13 AM
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Hervé Nicolas. Fluage d'aciers renforcés par dispersion nanométrique : caractérisation, modélisation et optimisation de la microstructure. Matériaux. Université Grenoble Alpes, 2016. Français. ⟨NNT : 2016GREAI008⟩. ⟨tel-01312899⟩

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