A systematic approach to measuring radiation-induced segregation (RIS) was used on four ferritic-martensitic (F-M) alloys: T91, HCM12A, HT9, and a Fe-9Cr model alloy, irradiated with 2.0 MeV protons over a range of doses (1-10 dpa) and temperatures (300-700°C). The experimental conditions are established so as to isolate the dependence of RIS on the experimental parameters: temperature, dose and bulk composition. RIS is measured at prior austenite grain boundaries (PAGBs) using the STEM-EDS technique. Chromium is found to enrich at PAGBs in all conditions with the exception being T91 irradiated to 3 dpa at 700°C. The magnitude of enrichment is small (<2 at%). Minor elements Si, Ni, and Cu also enrich consistently. A bell-shaped temperature dependence of RIS is observed in all elements. The amount of Cr enrichment decreases as a function of increasing bulk Cr concentration. Lastly, it is found that the 9Cr model alloy reaches a steady-state Cr RIS behavior at approximately 7 dpa, while the T91 reaches what may be a steady state near 3 dpa, then the amount of enrichment decreases at 10 dpa.

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A model Fe-9%Cr oxide dispersion strengthened (ODS) steel was irradiated with protons or neutrons to a dose of 3 displacements per atom (dpa) at a temperature of 500°C, enabling a direct comparison of ion to neutron irradiation effects at otherwise fixed irradiation conditions. The irradiated microstructures were characterized using transmission electron microscopy and atom probe tomography including cluster analysis. Both proton and neutron irradiations produced a comparable void and dislocation loop microstructure. However, the irradiation response of the Ti-Y-O oxide nanoclusters varied. Oxides remained stable under proton irradiation, but exhibited dissolution and an increase in Y:Ti composition ratio under neutron irradiation. Both proton and neutron irradiation also induced varying extents of Si, Ni, and Mn clustering at existing oxide nanoclusters. Protons are able to reproduce the void and loop microstructure of neutron irradiation carried out to the same dose and temperature. However, since nanocluster evolution is controlled by both diffusion and ballistic impacts, protons are rendered unable to reproduce the nanocluster evolution of neutron irradiation at the same dose and temperature.

This paper provides an overview of advanced scanning transmission electron microscopy (STEM) techniques used for characterization of irradiated BCC Fe-based alloys. Advanced STEM methods provide the high-resolution imaging and chemical analysis necessary to understand the irradiation response of BCC Fe-based alloys. The use of STEM with energy dispersive x-ray spectroscopy (EDX) for measurement of radiation-induced segregation (RIS) is described, with an illustrated example of RIS in proton-and self-ion irradiated T91. Aberration-corrected STEM-EDX for nanocluster/nanoparticle imaging and chemical analysis is also discussed, and examples are provided from ion-irradiated oxide dispersion strengthened (ODS) alloys. Finally, STEM techniques for void, cavity, and dislocation loop imaging are described, with examples from various BCC Fe-based alloys.

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