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  1. Effects of temperature and dose rate on ion-irradiated γ-LiAlO2 pellets

    Defect accumulation and microstructural evolution during ion irradiation at elevated temperatures are governed by competing processes of defect production, driven by the dose rate, and defect recovery, controlled by diffusion, interaction, and annihilation. Here, this study investigates the effects of irradiation temperature and the dose rate on microstructural evolution, deuterium retention, and lithium volatilization in γ-LiAlO2 pellets subjected to sequential He+ and D+ ion irradiation. Experiments were performed to a total fluence of 3 × 1017 (He+ + D+)/cm2 at 623, 673, 723, and 773 K with an average He+ dose rate of 7.7 × 10−4 dpa/s, and to 2more » × 1017 (He+ + D+)/cm2 at 773 K with dose rates of 6.8 × 10−5, 2.9 × 10−4, and 7.3 × 10−4 dpa/s. At 623 K, the microstructure was dominated by cavities and fractures with no observable precipitate formation, while small precipitates emerged at 673 K. Increasing the irradiation temperature to 723–773 K promoted the formation of larger, faceted LiAl5O8 precipitates, and surface amorphization, accompanied by pronounced lithium depletion and H–D isotopic exchange. At 773 K, medium and high dose rates produced an amorphized surface layer over a crystalline subsurface containing LiAl5O8 precipitates and blisters at the crystalline–amorphous interface, whereas low-dose-rate irradiation preserved surface crystallinity with cavities distributed in the matrix, around precipitates, and along grain boundaries. Precipitate morphology was anisotropic with limited size dependence on the dose rate. These results elucidate the coupled effects of temperature and the dose rate and demonstrate that sequential He+ and D2+ irradiation at 773 K reproduces key microstructural features and H isotope behavior observed in neutron-irradiated γ-LiAlO2 at 573 K.« less
  2. Electric-field-assisted-sintering of rare-earth oxide dispersion strengthened Fe-Cr-Mo alloys

    Oxide-dispersion-strengthened (ODS) iron (Fe)-chromium (Cr)- molybdenum (Mo) alloys have promising applications in nuclear core components. In this study, Fe-Cr-Mo based ODS steels were prepared with additions of Y2O3, La2O3 and CeO2 through mechanical alloying, followed by electric field-assisted sintering. Microstructures were studied by atom probe tomography, electron back-scattered diffraction, and scanning electron microscopy. Tensile properties were measured using uniaxial tensile testing at room temperature. Grain refinement was achieved in the oxide dispersed specimens with the average grain size less than 1 µm. A uniform distribution of fine 2-4 nm size clusters formed in the matrix, which strengthened the alloys. Lanthanamore » bearing alloy had the highest number density of nanoparticles and the highest strength as compared to yttria and ceria bearing alloys. The uniform distribution and refinement of rare-earth metal oxide nanoparticles coupled with grain refinement enabled the development of high strength alloys. Electric field-assisted sintering techniques demonstrated the advantages of developing high-performance rare-earth bearing ferritic alloys, with potential applications for nuclear structure components.« less
  3. Abnormal grain growth driven by high-temperature proton irradiation in nanocrystalline Ni

    In this research we examine a nanocrystalline Ni thin film exposed to high-temperature proton irradiation and compare it with as-deposited and annealed-only counterparts. Despite lacking thermal spikes typical of heavy ions, 400 °C proton irradiation drives pronounced grain growth in select grains, whereas annealing alone yields only modest coarsening. Grain-boundary statistics show fewer low-angle boundaries (10–20°) and more high-angle boundaries (55–60°), consistent with irradiation-enhanced mobility of high-misorientation boundaries. The irradiated films retain a random texture, with no evidence of texture development or sharpening. Mechanisms, such as radiation-enhanced grain boundary diffusion, beam-induced heating, and ion channeling-mediated selective grain growth, are unlikelymore » to be the predominant drivers to explain the resultant microstructure. Instead, we suggest irradiation-induced modifications of grain-boundary structure, including possible complexion transitions, as one plausible explanation for this selective grain growth and retention of random texture. However, additional temperature–dose studies are required to confirm the mechanism.« less
  4. Combining four-point bending and corrosion to map stress-dependent corrosion susceptibility of 316H stainless steel in FLiNaK

    Understanding the effect of stress on the corrosion of steels in molten salts is important for material screening and safety assessment of molten salt reactors. We present a method that combines four-point bending with corrosion testing, enabling the mapping of corrosion susceptibility as a function of local stress from a single specimen. Guided by finite element analysis, a four-point bending setup was used to bend a 316H stainless-steel bar under controlled elastic stress during a 100-hour exposure in FLiNaK at 700 °C. Post-exposure characterization using scanning electron microscopy and energy-dispersive X-ray spectroscopy revealed a pronounced correlation between stress and corrosion.more » Regions under tensile stress exhibited significantly deeper attack depths and greater chromium depletion along grain boundaries, whereas compressive zones showed shallower corrosion cracks. The stress effect is attributed to stress concentration under tensile loading, which promotes chromium dissolution and crack propagation. This technique can be readily applied to other structural alloys, enabling quantitative measurement of corrosion susceptibility as a function of local stress.« less
  5. Corrosion susceptibility and chromium loss in Austenitic steels and Nickel-based alloys in molten FLiNaK at 700 °C

    A comparative study was conducted to evaluate the corrosion susceptibility of 316L, 316H, Ni 200, Inconel 625, and Hastelloy N in molten FLiNaK at 700 °C for 100 h. Top-view and cross-sectional scanning electron microscopy (SEM) imaging, combined with energy-dispersive X-ray spectroscopy (EDS) mapping, was performed to investigate microstructural and compositional changes. SEM images were further processed by introducing a contrast threshold to map cavity distribution. Using EDS mapping, intergranular and intragranular Cr loss were separately characterized. The ranking of mass loss after corrosion, from highest to lowest, is as follows: 316H > 316L > Inconel 625 > Hastelloy Nmore » > Ni 200. Cr loss was found to be correlated with Mo concentration, in agreement with many previous studies, with higher Mo content resulting in reduced Cr loss. On the other hand, there is no evidence that the high carbon content in 316H enhances corrosion resistance. The relatively low solubility of carbon in austenite at the testing temperature limits the amount of dissolved carbon. Therefore, the carbon-retarded vacancy diffusion, and consequently the reduced Cr diffusion, were not observed.« less
  6. Superior plastic flow stability of self-patterned carbide – amorphous ceramic nanostructures

    Amorphous ceramics and carbides exhibit superb strength but poor plasticity. Here, we synthesized TiC-SiOC nanostructures with TiC-nanocarbides embedded in amorphous ceramic SiOC by co-sputtering followed by high-temperature annealing and/or irradiation. TiC-SiOC nanostructures exhibit high strength and good plastic flow stability even after heavy irradiation, 7 GPa at room temperature and 3.6 GPa at 700 ℃ with a uniform strain of about 10%∼18%. The uniform deformation is accommodated by the shearing of amorphous ceramic and the rotation of nanocarbides. Nanocarbides inhibit the propagation of shear banding in amorphous SiOC, and amorphous-crystal interfaces act as sinks to manage irradiation-induced defects.
  7. A high-temperature Rutherford Backscattering Spectrometry apparatus for in situ material characterization

    A new methodology for high-temperature Rutherford Backscattering Spectrometry (HT-RBS) has been developed to enable in situ material characterization at elevated temperatures. A 3.5 MeV proton beam penetrates a 10-µm-thick 316L stainless steel foil mounted on a graphite substrate, with backscattered signals detected using an HT-RBS system. Conventional semiconductor detectors, primarily based on silicon, suffer significant performance degradation at temperatures higher than ~ 60 °C due to increased leakage current and noise, leading to signal distortion and failure. Here, to preserve spectral quality, a 5 µm aluminum foil shields the detector from thermal radiation, allowing reliable operation up to 900 °Cmore » at the target. A rotatable shutter provides additional thermal isolation during data collection pauses. In situ measurements of areal density changes of 316L stainless steel were conducted to validate the technique, revealing consistency with the known thermal expansion coefficient. The method facilitates seamless switching between irradiation and analysis, enabling continuous studies. This approach supports in situ investigations of diffusion, void swelling, creep, and corrosion, offering a versatile tool for advanced materials research.« less
  8. Microstructural features and deuterium diffusion in lithium penta-aluminate pellets under He+ and D+ ion irradiation

    Lithium (Li) penta-aluminate (LiAl5O8) is investigated as a potential tritium (T) breeding material, with a focus on microstructural response to ion irradiation and deuterium (D) diffusion behavior. Under high-fluence ion irradiation (2 x 1017 (He++D+)/cm2) at 773 K, LiAl5O8 exhibits significant disorder on the Li sublattice, as revealed by atomic-resolution scanning transmission electron microscopy, while the Al and O sublattices remain stable, demonstrating strong resistance to structural amorphization. Irradiation induces the formation of platelet-shaped antiphase boundaries (APBs), which may serve as effective D trapping sites. Atom probe tomography suggests the presence of 6LiD clusters in the mass spectra, though definitemore » conclusions regarding APB composition are hindered by signal overlap and limited data statistics. Time-of-flight secondary ion mass spectrometry reveals that D retention approaches to saturation at 3 x 1017 (He++D+)/cm2. Isothermal and isochronal annealing studies determine an average diffusivity of 1.6 x 10-13 at 773 K and an effective activation energy of 0.8 ± 0.1 eV for D migration. Compared to γ-LiAlO2, LiAl5O8 demonstrates superior irradiation resistance, minimal Li loss, and enhanced D retention, underscoring its potential as a durable breeder material for T production. In conclusion, these findings provide key insights into the microstructural evolution, defect dynamics, and D retention mechanisms in LiAl5O8 under reactor-relevant conditions.« less
  9. Finite element analysis of the impact of beam heating mode in molten salt corrosion experiments employing simultaneous ion irradiation

    Finite element analysis was used to investigate the temperature and stress profiles that develop in 316L stainless steel membranes being irradiated using different proton beam conditions in contact with a molten salt environment. It was shown that in addition to a nonuniform irradiation profile, a focused 2 MeV proton beam leads to very strong temperature and stress gradients in the membrane, introducing highly localized driving forces that complicate and even compromise the integrity and reliability of the experimental results of corrosion studies. Here, the use of a focused beam in corrosion studies can create experimental artifacts that may misrepresent themore » true corrosion behavior. In contrast, the use of a rastered beam is shown to distribute the protons and resulting radiation damage uniformly across the membrane face, and more importantly, results in temperature and stress profiles that are not only very uniform but are of much lower magnitude. The use of a rastered beam during molten salt corrosion experiments is therefore recommended to achieve uniform damage rates, thereby reducing both gradients and magnitudes of the temperature and stress distributions.« less
  10. Irradiation-induced formation of G-phase precipitates and M2X carbides in self-ion irradiated HT-9

    Ferritic-martensitic steels with high chromium content are a promising material group for advanced nuclear systems due to their high temperature strength and good irradiation tolerance. HT-9 is an optimized and often-studied alloy in this group, but additional studies are required on its radiation response under extreme conditions to be experienced in various types of nuclear reactors, especially with respect to phase stability under irradiation. Self-ion irradiation of HT-9 by 5 MeV Fe ions was used to simulate neutron-induced behavior reaching peak doses of 100 and 300 dpa at temperatures ranging from 450 to 550 °C. M23C6 carbides that existed priormore » to irradiation were found to remain stable under all examined irradiation conditions. As irradiation progressed at 450 and 500 °C, however, formation of spherical-like G-phase precipitates and needle-like M2X carbides was observed. G-phase precipitates were found to be enriched in Ni, Si, and Mn, and show no interface segregation, whereas needle-like M2X carbides were rich in Cr and Mo and clearly displayed interface segregation of Ni and Si. M2X carbide formation is believed to be assisted by vacancies, while G-phase precipitation is thought to be assisted by interstitials. Finally, this difference in defect-mediated formation leads to a difference in distribution with depth. M2X carbides are distributed over shallower depths than that of G-phase precipitates, consistent with defect imbalance predictions that consider the influence of the injected interstitial effect.« less
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