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At least 37 records · Page 2

Irradiation Effects on Stability of δ-UZr2 phase in U-50 wt% Zr Alloy

U-50wt%Zr is a candidate metallic nuclear fuel with potential application in light water reactors due to its excellent thermal properties and high radiation tolerance. The Zr-rich UZr fuels possess greater swelling resistance and fission gas release characteristics compared with U-rich UZr fuels. In this current study, the δ-phase U-50wt%Zr is proton irradiated at room temperature to 1 displacement per atom (dpa) to provide insights on phase stability under irradiation conditions. High resolution characterization of Transmission Electron Microscopy (TEM) and Atom Probe Tomography (APT) characterization techniques are used to elucidate microstructural changes due to irradiation. TEM and APT results show highly oriented bcc β-Zr-rich platelet precipitates nucleating adjacent to α-U phases inside the UZr 2 matrix. Formation of this platelet morphology is characteristic of Widmänstatten structure which can be attributed to a variety of factors such as differences in thermal expansion coefficient between the phases, grain size, alloy composition, and cooling rate. The phases present are distinctly different than those observed through in situ annealing, but irradiation accelerates diffusion and phase separation kinetics. These microstructural changes in U-50wt%Zr are different from those achieved by pure thermodynamic or high temperature heavy ion irradiation experiments. Finally, our work, together with previous ones, highlight the necessity to study the U-Zr phase diagram under non-equilibrium thermodynamics conditions to support this material's deployment as a viable nuclear fuel form.

36 MATERIALS SCIENCE↗

Effects of high temperature and e-beam irradiation on the stability of refractory thin films

Refractory thin films of Al2O3, ZrO2, MgO, ThO2, and BN have been investigated in situ in an UHV transmission electron microscope. The electron transparent refractory films were prepared by electron-beam evaporation, anodization, RF sputtering, and thinning of bulk crystal materials. The study concentrates on monitoring the thermal and mechanical stability of the films, phase and structural changes, and electron irradiation effects as a function of film-preparation conditions. With increasing temperatures, five different crystallographic phases were observed for both anodized and electron-beam-evaporated alumina films. Zirconia films exhibited two phase transitions upon heating to 1200 C and electron-irradiation-induced crystallization of ZrO2 even at room temperature. MgO, ThO2, and BN films did not undergo any noticeable phase transformation but ruptured due to sintering below 1200 C.

Lee, E. H.↗

Thermal Stability and Ion Irradiation Response of Refined Grained V – 4Cr – 4Ti

Since the 1960’s, there has been interest in V-4Cr-4Ti and similar alloys as candidates for low activation structural materials for advanced nuclear reactors. V-4Cr-4Ti was produced using arc melting and subsequently subjected to large strain extrusion machining to produce a multimodal microstructure largely composed of nanocrystalline and ultrafine grain sizes. In-situ thermal stability of the multimodal V-4Cr-4Ti to 800 °C shows the formation of vanadium carbides with negligible grain growth. In-situ dual-beam 16 KeV He+ and 1 MeV Kr2+ ion irradiation performed at 700 °C to a final dose of ~5 displacements per atom show the formation of small He cavities well distributed throughout the system, with preferential clustering at grain boundaries. This work provides insight into how the increased fraction of grain boundaries affect the simultaneous dual beam ion irradiation response of multimodal V – 4 wt.% Cr – 4 wt.% Ti at elevated temperatures. Analysis of the cavities reveal an areal density of 0.024±0.007 cavities/nm2 and swelling of 0.236% after the dual-beam ion irradiation. Nanoindentation shows a ~50% increase in hardening after the ion irradiation at 700 °C.

TEM↗

X-ray photoelectron and mass spectroscopic study of electron irradiation and thermal stability of polytetrafluoroethylene

Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. A quantitative comparison of the radiation dose rate with that in other reported studies showed that, for a given total dose, the damage observed by XPS is greater for higher dose rates. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS that were associated with damage diminished, giving the appearance that the radiation damage annealed. The apparent annealing of the radiation damage was found to be due to the covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

Wheeler, Donald R.↗

Far-infrared spectral studies of phase changes in water ice induced by proton irradiation

Changes in the FIR spectrum of crystalline and amorphous water ice as a function of temperature are reported. The dramatic differences between the spectra of these ices in the FIR are used to examine the effect of proton irradiation on the stability of the crystalline and amorphous ice phases from 13 to 77 K. In particular, the spectra near 13 K show interconversion between the amorphous and crystalline ice phases beginning at doses near 2 eV/molecule and continuing cyclically with increased dose. The results are used to estimate the stability of irradiated ices in astronomical environments.

Moore, Marla H.↗

Effects of ZrN coating and heat treatment on U-Mo dispersion fuel systems under irradiation

The stability of U-Mo fuel particles embedded in an Al matrix under irradiation can be enhanced through ZrN coatings and/or heat treatment. Here, the present study investigates the irradiation behavior of fuel plates containing U-Mo fuel particles fabricated under various heat-treatment conditions and ZrN coating thicknesses. Different fission densities were also applied to each fuel plate to evaluate the effects of these variables. Results indicate that higher fission densities lead to more grain recrystallization and high burnup structure (HBS) development in the fuel particles. Heat treatment was found to mitigate the accumulation of fission gas bubbles in fuel particles at low fission densities by coarsening their grains. Fuel particles with ZrN coatings of a 1.2 μm thickness or above exhibited reduced formation of U-Mo/Al interaction layers, suggesting the existence of a critical ZrN coating thickness that minimizes the development of these layers. Fission gas bubbles were predominantly observed at grain boundaries of U-Mo fuel particles irradiated at low fission densities. Subgrain boundaries, which appeared to originate from the original grain boundaries containing fission gas bubbles or HBSs, were also observed, indicating the early stage of HBS propagation in the fuel particles.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effects of ZrN Coating and Heat Treatment on U-Mo Dispersion Fuel under Irradiation

The stability of U-Mo fuel particles in Al matrix can be improved using ZrN coating and heat treatment. This study investigated irradiation behaviors of fuel plates containing U-Mo fuel particles fabricated with different conditions including heat treatment and the thickness of ZrN coating. Additionally, different fission densities were applied to each fuel plate to understand how varying fission densities affect its irradiation behaviors. This study showed that more recrystallization of grains and development of high burnup structure (HBS) occurred in irradiated fuel particles with higher fission densities. Heat treatment reduced the accumulation of fission gas bubbles in the fuel particles by coarsening their grains. The fuel particles with a ZrN coating thickness of 1.2-1.8 µm showed less significant development of U-Mo/Al interaction layers than the particles with a coating thickness of 0.5 µm after irradiation. This might indicate the existence of a critical thickness of ZrN coating to minimize the formation of the interaction layers. Fission gas bubbles were observed at grain boundaries of irradiated U-Mo fuel particles at low fission densities, and the formation of dendritic features with a darker contrast was identified in backscattered electron images. These features stemmed from grain boundaries with fission gas bubbles or HBS, and some of them contained the bubbles, indicating that they might represent an early stage of HBS propagation in the fuel particles.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Design and development of equi-atomic refractory High Entropy Alloys for use in radiation environments

Development of new structural materials that can withstand the extreme environments of nuclear reactors where the materials are exposed to high dose rate of ~ 30 200 dpa, high temperatures of the order of 500 1000 o C and tens of years of operation is vital for exploiting the “smallest carbon footprint energy source” to its fullest, in order to deal with the energy crisis worldwide. Recently, HEAs have shown superior irradiation properties over conventional alloys like higher resistance to defect formation, lower void swelling, limited irradiation hardening and higher microstructural stability under irradiation, making them potential structural material candidates for reactors. Proper characterization and testing of these materials are essential before they can replace the conventional alloys.

36 MATERIALS SCIENCE↗

MX precipitate behavior in an irradiated advanced Fe-9Cr steel: Self-ion irradiation effects on phase stability

In an effort to optimize Fe-9Cr reduced activation ferritic/martensitic (RAFM) steels and to inform the design and operation of fusion reactors, this work represents the first in a series of cohesive studies dedicated to the evolution of MX-TiC precipitates under accelerated single and dual ion irradiations. This study investigates CNA9, a simplified Fe-9Cr RAFM steel featuring initial MX-TiC precipitate densities of (2.3±0.3)×10²¹ m⁻³. This material was subjected to single self-ion irradiation at damage levels ranging from 1 to 100 displacements per atom (dpa) over a temperature range of 300 to 600°C, with a nominal dose rate of 7×10⁻⁴ dpa/s. Irradiation-induced coarsening was observed, as evidenced by statistically significant increases in mean diameter sizes, at 15 dpa at both 500°C and 600°C, whereas no coarsening was noted at 300°C or 400°C. Further, complete dissolution of precipitates occurred at damage levels of 50 and 100 dpa across the two temperatures tested (300°C and 500°C) while no significant changes were observed at any doses below 15 dpa at 500°C. Experimentally parameterized recoil resolution modeling suggests that the observed radiation stability of MX-TiC precipitates is intricately linked to diffusional changes of solutes resulting from the co-evolution of microstructural features within the experiments. The findings align with current theoretical perspectives on radiation-induced precipitate stability in complex alloys.

36 MATERIALS SCIENCE↗

Influence of Joule Heating on the Stability of High Temperature Irradiation Resistant Thermocouples

Development of in-core instrumentation is driven by the pursuit of safer and more economic energy production from both existing nuclear reactors and Generation IV reactor designs. Idaho National Laboratory (INL) has developed high temperature irradiation resistant thermocouples (HTIR-TCs) for temperature sensing inside Generation IV nuclear reactors. These thermocouples are composed of phosphorus-doped niobium (Nb-P) and lanthana-doped molybdenum (Mo-LaO) thermoelements, an alumina (Al2O3) insulation, and a niobium sheath. HTIR-TCs require an initial heat treatment exceeding the maximum service temperature to stabilize the generated electromotive force (EMF) signal; however, the mechanism behind this stabilization is not well understood. This work evaluates the impact of Joule heating on the thermoelements' microstructures, chemical stability, and mechanical properties to determine the mechanisms by which the EMF signal stabilization occurs. Accordingly, during the Joule heat treatment, a secondary Nb3P phase coarsened along the length of the Nb-P thermoelement, along with the formation of an interaction region at the Al2O3/niobium interface. The interaction between the alumina insulation and the Nb-P thermoelement was also observed within the Mo-LaO thermoelement. Joule heating induced stability within the generated EMF signal of HTIR-TCs through the formation of secondary phases within the Nb-P and the interaction of the alumina insulation with the thermoelements.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Thermal stability of electron-irradiated poly(tetrafluoroethylene) - X-ray photoelectron and mass spectroscopic study

Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species were evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS spectrum that were associated with damage diminished, giving the appearance that the radiation damage had annealed. The observations were interpreted by incorporating mass transport of severed chain fragments and thermal decomposition of severely damaged material into the branched and cross-linked network model of irradiated PTFE. The apparent annealing of the radiation damage was due to covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

Wheeler, Donald R.↗

Ta–Zr carbides: Synthesis advances via carbothermal reduction and defect evolution observed through transmission electron microscopy ion irradiation

The thermodynamic stability of six distinct compositions within the Zr—Ta—C ternary system is investigated in this study, marking the first report of their synthesis through carbothermic reduction in vacuum. A prolonged annealing process at 2200°C enabled high densification and phase equilibrium. Detailed phase identification and microstructural characterization through microscopy and X-ray diffraction techniques revealed clear compositional trends and stable phase formations. Two compositions ((Ta 0.2 Zr 0.8 )C 0.6 and (Ta 0.5 Zr 0.5 )C 1 ) were selected for ion irradiation experiments using 200 keV Kr + at 600°C—representing the first-ever irradiation study on the Zr—Ta—C system. The findings indicated defect accumulation and nanoscale cavity formation without any evidence of amorphization, highlighting the system's structural stability under irradiation. Together, the synthesis and irradiation results provide a basis for further investigation of the system and suggest its relevance for applications under extreme environments.

36 MATERIALS SCIENCE↗

Ion irradiation testing of 14YWT ODS and HT-9

Ion irradiations were performed to compare a new generation of 14YWT, NFA-2, to the prior generation NFA-1. Irradiations were performed at 450 °C and to a peak dose of 500 dpa. The irradiation condition was chosen as a relevant temperature for scoping for an upcoming JOYO neutron irradiation, and the high dose was chosen to evaluate the exceptional microstructural stability to irradiation induced changes of 14YWT. For comparison, HT-9 was irradiated as the benchmark. Irradiation induced changes to the microstructures were limited for the 14YWT samples and extensive for the HT-9 benchmark.

36 MATERIALS SCIENCE↗

In situ ion irradiation of amorphous TiO 2 nanotubes

Understanding of structural and morphological evolution in nanomaterials is critical in tailoring their functionality for applications such as energy conversion and storage. Here, we examine irradiation effects on the morphology and structure of amorphous TiO 2 nanotubes in comparison with their crystalline counterpart, anatase TiO 2 nanotubes, using high-resolution transmission electron microscopy (TEM), in situ ion irradiation TEM, and molecular dynamics (MD) simulations. Anatase TiO 2 nanotubes exhibit morphological and structural stability under irradiation due to their high concentration of grain boundaries and surfaces as defect sinks. On the other hand, amorphous TiO 2 nanotubes undergo irradiation-induced crystallization, with some tubes remaining only partially crystallized. The partially crystalline tubes bend due to internal stresses associated with densification during crystallization as suggested by MD calculations. Furthermore, these results present a novel irradiation-based pathway for potentially tuning structure and morphology of energy storage materials.

36 MATERIALS SCIENCE↗