Lors de la synthèse des aciers ODS, la première étape consiste à réaliser un broyage actif, appelé mécano-synthèse, entre les matériaux de départ qui sont la poudre métallique et les renforts d’oxyde. Ce procédé peut se réaliser au moyen d’un broyeur à boulets, constitué d’une cuve cylindrique à l’intérieur de laquelle des billes en acier sont introduites. Le broyage résulte des combinaisons de chocs entre billes, poudre et paroi de la cuve, ce qui conduit à une évolution de la de la taille, de leur forme et de leur polydispersité. La première partie de cette thèse s’est attachée à élaborer un moyen de caractérisation de la poudre par des mesures ultrasonores. Une méthode qui consiste à sonder un échantillon de poudre métallique pour la mesure des paramètres acoustiques s’est avérée être adaptée pour la qualification de la poudre métallique en cours de broyage. Une dépendance des paramètres acoustiques avec les caractéristiques morphologiques du milieu a également été mise en évidence pour des échantillons granulaires. Dans une deuxième partie, l’optimisation du procédé par l’identification de la vitesse optimale de rotation de la cuve est recherchée dans un premier temps. Une mise en parallèle des signaux acoustiques et vibratoires en fonction de la vitesse de rotation de la cuve avec le mouvement des billes, montre que les énergies acoustique et vibratoire sont des indicateurs pouvant conduire à la vitesse de rotation optimale. Puis, il est montré comment des mesures acoustiques et vibratoires durant un broyage permettent de caractériser l’évolution de la nature des poudres et d’identifier la présence de colmatage de la poudre sur les parois de la cuve. / During the ODS steel (Oxide Dispersion Strengthened) synthesis, the first stage consists in an active milling between original materials, which are metallic powder and oxide to obtain reinforced micro/nanoscale dispersions. This process, known as mechanical alloying, could be realized by balls milling composed by a cylindrical tank rotating around its main axis, within which steel beads are introduced. The grinding results from different combinations of collisions between beads and powders on the tank walls, that lead to morphological grain powder evolution (grain size and shape). The first part of this thesis proposes an ultrasonic method to characterize the metallic powder. An experimental method, which consists in acoustic probing for measuring linear acoustic parameters (longitudinal wave velocity and elastic modulus) of a slab of powder sample, appears to be suitable to follow different mechanical alloying stages. A dependence of the acoustic parameters on the morphological characteristics of metallic powder (grain shape and grain size distribution) is shown with the same sample preparation and the same confining pressure. In the second part, optimization process by identification of ball milling optimal rotation speed is researched in a first step. Correlation between acoustic or vibration signals and bead motion versus rotation speed, shows that acoustic and vibration energy are good indicators that can be used to find the optimal rotation speed. In a second step, acoustic and vibration measures are used to follow grain material properties evolution during a grinding (for a period of 176hrs) and to identify powder clogging mechanism on a milling tank.

This thesis was most concerned with the mechanical response to irradiation of two in-house produced oxide dispersion strengthened (ODS) steels and two non-ODS coun- terparts. The steels, manufactured by Dr. M. J. Gorley (University of Oxford), were me- chanically alloyed from gas-atomised Fe-14Cr-3W-0.2Ti, with the addition of 0.25Y₂O₃ powder in the case of the ODS variants. The powders were hot isostatic pressed at consolidation temperatures of 950 °C and 1150 °C. The four steels were designated 14WT 950 (non-ODS), 14YWT 950 (ODS), 14WT 1150 (non-ODS) and 14YWT 1150 (ODS), and were used in the as-produced condition. Initially, the macroscale elastic modulus and yield stress were determined using a four-point flexure test, employing digital image correlation (DIC) as a strain gauge. The microcantilever size eects were then characterised, and it was determined that the yield stress signicantly diverged from macroscale values at microcantilever beam depths of < 4.5 μm. Using knowledge of this, the in-house produced alloys were irradiated with 2 MeV protons at the Surrey Ion Beam Centre (University of Surrey, UK) to a displacement damage of ∼ 0.02 dpa and 0.2 dpa (Bragg peak). This was to produce a deep irradiated layer for the fabrication of large microcantilevers with reduced size effects. The cross-sectional surface of the irradiated layer was then exposed and inclined linear arrays of 250 nm deep indents were placed across the damage prole. 14WT 1150 (non-ODS) revealed a clear proton damage prole in plots of hardness against irradiation depth, 14WT 950 (non-ODS) also showed modest hardening in the region of the Bragg peak. No appreciable hardening was observed in either 14YWT specimens, attributed to the fine dispersion of nanoscale oxides providing a high number density of defect sink sites. However, a large bimodal variation in hardness was measured in both ODS variants. This was investigated using EBSD and EDX, and was determined to be caused by a pronounced heterogeneity of the microstructure. While Hall-Petch strengthening and changes in the local chemistry had some effect on the measured hardness, the most likely cause of the large variation in local hardness was heterogeneity in the nanoscale oxide population. Microcantilevers were fabricated out of the irradiated layer cross-section in 14WT 1150 and 14YWT 1150. Larger microcantilevers, with ∼ 5 μm beam depth, were placed with their beam centre at ∼ 0.026 dpa. Smaller microcantilevers, with ∼ 1.5 μm beam depth, were placed with their beam centre at the Bragg peak, 0.2 dpa. Both the large and the small microcantilevers fabricated in 14WT 1150 (non-ODS) displayed significant irradiation hardening. In the ODS variant, 14YWT 1150, irradiation hardening appeared to be reduced. The work in this thesis successfully showed that it was possible to extract a close approximation of the macroscale yield stress from shallow irradiated layers, providing that the irradiation condition is carefully chosen in response to known size dependent behaviour. This thesis also investigated the size dependent behaviour of microcantilevers using a lengthscale dependent crystal plasticity UMAT, developed by Dunne et al. and implemented within ABAQUS 6.14-2 commercially available nite element software. The simulation of the GND density evolution with increasing plastic strain allowed their contribution to the microcantilever size effect, through mobile dislocation pinning, to be determined. This novel approach to modelling size effects in three dimensional finite element microcantilever models demonstrated that while it was possible to simulate a lengthscale-dependent response in finite element microcantilever models, the constitutive equation for the plastic velocity gradient needs to be more physically based in order the match the experimentally derived results; for example, a lengthscale-dependent term relating to the dislocation source density of the material. Although the apparent reduction of irradiation hardening in ODS in-house produced alloys showed great promise, these alloys also displayed a large amount of scatter in measured hardness and yield stress, attributed to the pronounced heterogeneity in the microstructure. Alloys with such signicant microstructural heterogeneity are not suitable for engineering or commercial use.