Zhijie Jiao

Designing materials for performance in high-radiation fields can be accelerated through a carefully chosen combination of advanced multiscale modeling paired with appropriate experimental validation. The studies reported in this work, the combined efforts of six universities working together as the Consortium on Cladding and Structural Materials, use that approach to focus on improving the scientific basis for the response of ferritic–martensitic steels to irradiation. A combination of modern modeling techniques with controlled experimentation has specifically focused on improving the understanding of radiation-induced segregation, precipitate formation and growth under radiation, the stability of oxide nanoclusters, and the development of dislocation networks under radiation. Experimental studies use both model and commercial alloys, irradiated with both ion beams and neutrons. Transmission electron microscopy and atom probe are combined with both first-principles and rate theory approaches to advance the understanding of ferritic–martensitic steels.

Dual ion irradiations using 5 MeV defocused Fe2+ ions and co-injected He2+ ions were conducted on a ferritic-martensitic steel alloy, T91, in the temperature range of 406 °C–570 °C over a damage range of 14.6–35 dpa followed by characterization of the microstructure using transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). Dislocation loops were observed to increase in diameter and decrease in density with temperature until only network dislocations were observed at the highest temperatures of 520 °C and 570 °C. Swelling exhibited the expected bell-shaped trend with temperature following the number density of cavities, peaking at 460 °C and with a bimodal size distribution except at 520 °C and 570 °C. Nickel- and silicon-rich clusters formed under dual ion irradiations near the surface at all but the highest temperatures of 520 °C and 570 °C. Very little Cr and Si segregation was observed at lath boundaries while Ni enriched at all temperatures examined. Segregation of Cr and Ni appeared to saturate by 17 dpa, while Si enriched up to 35 dpa. The dislocation and cavity microstructures of dual ion irradiated T91 and T91 irradiated in the BOR-60 fast reactor matched extremely well using a temperature shift of +60–70 °C. However, segregation to grain boundaries and formation of nickel-silicon rich clusters were minimal in the dual ion irradiated T91 and less than that in T91 irradiated in the BOR-60 fast reactor.

The effects of transmutation produced helium and hydrogen must be included in ion irradiation experiments to emulate the microstructure of reactor irradiated materials. Descriptions of the criteria and systems necessary for multiple ion beam irradiation are presented and validated experimentally. A calculation methodology was developed to quantify the spatial distribution, implantation depth and amount of energy-degraded and implanted light ions when using a thin foil rotating energy degrader during multi-ion beam irradiation. A dual ion implantation using 1.34 MeV Fe+ ions and energy-degraded D+ ions was conducted on single crystal silicon to benchmark the dosimetry used for multi-ion beam irradiations. Secondary Ion Mass Spectroscopy (SIMS) analysis showed good agreement with calculations of the peak implantation depth and the total amount of iron and deuterium implanted. The results establish the capability to quantify the ion fluence from both heavy ion beams and energy-degraded light ion beams for the purpose of using multi-ion beam irradiations to emulate reactor irradiated microstructures.

The widely experienced problem of carbon uptake in samples during ion irradiation was systematically investigated to identify the source of carbon and to develop mitigation techniques. Possible sources of carbon included carbon ions or neutrals incorporated into the ion beam, hydrocarbons in the vacuum system, and carbon species on the sample and fixture surfaces. Secondary ion mass spectrometry, atom probe tomography, elastic backscattering spectrometry, and principally, nuclear reaction analysis, were used to profile carbon in a variety of substrates prior to and following irradiation with Fe2+ ions at high temperature. Ion irradiation of high purity Si and Ni, and also of alloy 800H coated with a thin film of alumina eliminated the ion beam as the source of carbon. Hydrocarbons in the vacuum and/or on the sample and fixtures was the source of the carbon that became incorporated into the samples during irradiation. Plasma cleaning of the sample and sample stage, and incorporation of a liquid nitrogen cold trap both individually and especially in combination, completely eliminated the uptake of carbon during heavy ion irradiation. While less convenient, coating the sample with a thin film of alumina was also effective in eliminating carbon incorporation.