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Mechanical Properties of Additively Manufactured 316L Stainless Steel Before and After Neutron Irradiation–FY23

This report presents the observed mechanical behavior of the additively manufactured (AM) 316L stainless steel (SS) before and after neutron irradiation. In the Advanced Materials and Manufacturing Technologies (AMMT) program, a variety of mechanical and physical property data are generated and accumulated to assess the AM austenitic alloy for nuclear reactor applications. The testing and evaluation task in the FY 2023 focused on elucidating the effects of sampling location and build size on the mechanical properties of AM 316L SS (in stress-relieved condition) before and after neutron irradiation. The laser powder bed fusion (LPBF) process produced 316L plates of three distinct sizes from which SS-J3 miniature tensile specimens were machined from six different locations. The tensile specimens were irradiated in the High Flux Isotope Reactor (HFIR) normally to 2 and 10 dpa at the target temperatures of 300 °C and 600 °C. Post-irradiation tensile testing was performed at room temperature, 300 °C, and 600 °C. The mechanical properties of AM 316L SS were significantly influenced by the characteristic microstructures of printed materials, which include fine grains and high-density dislocations. Compared with the traditional 316L SS, AM 316L showed higher initial strength and lower ductility. Regardless of sampling location, the AM 316L steel retained relatively high strength and ductility to the highest irradiation dose. A prompt necking at yield (with little uniform ductility) was observed after irradiation at 300 °C but no embrittlement was observed up to 10 dpa. Ductilization by irradiation–the radiation-induced increase of ductility–was observed for the 600 °C irradiation only and it occurred in low dose range only. The neutron irradiation increased the data variation in many tensile property datasets, particularly after 600 °C irradiation, and no clear dependence of tensile properties on build thickness or sampling location was observed.

36 MATERIALS SCIENCE↗

Microstructural Simulation of Ion-Irradiated Natural Rocks and Minerals

This report details the contribution of Oak Ridge National Laboratory to the Nuclear Energy University Program (NEUP) project, "Rapid Characterization of Concrete Mineralogy using Multi-Scale Tools" led by the University of Illinois at Urbana-Champaign. To support the subsequent license renewal (SLR) of the US nuclear power plants (NPPs) fleet, the performance of concrete-forming aggregates against neutron irradiation needs to be assessed. Ion irradiation is proposed as a rapid, cost-effective surrogate method to full neutron irradiation testing. To complement the characterization of ion-irradiated rock specimens, ORNL has run finite-elements and fast-Fourier transform (FFT-based) simulations using the codes MARS and Microstructure-Oriented Scientific Analysis of Irradiated Concrete (MOSAIC). The main conclusion of this analysis is that the apparent post–ion-irradiation step-height underestimates the accumulated free radiation-induced volumetric expansion (RIVE) in the ion-implanted depth by about 15% at full amorphization and about 25% toward the beginning of the ion irradiation experiment. The discrepancy is explained by the fact that the step height is proportional to the sum of the RIVE (i.e., one third of the RIVE) and the irradiation-assisted plastic strains in the vertical direction (lower than two thirds of the RIVE). Because of the large lateral compressive stresses caused by the restraining effect of the unirradiated substrate, the stress field in the mineral grains and at the grain boundary (GB) in the ion-implanted layer is much different than the comparable stress field occurring during neutron irradiation. Hence, the mismatch RIVE causing cracks in the rock-forming minerals leads to different cracking patterns. Ion irradiation continues to be used as a rapid technique to assess the RIVE potential of rocks.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Status report on HFIR irradiation of optimized alumina forming alloys

Properties of FeCrAl alloys under neutron irradiation are of interest because of these materials’ potential application as accident-tolerant fuel cladding in nuclear systems. In parallel, alumina-forming austenitic (AFA) alloys are of interest for use as structural materials in advanced nuclear systems for their potential higher resistance to embrittlement and high-temperature steam oxidation resistance. An irradiation campaign for fiscal year 2024 has been developed under the Advanced Fuels Campaign to perform irradiation testing of various FeCrAl and AFA alloys in Oak Ridge National Laboratory’s High Flux Isotope Reactor (HFIR). The goals of this irradiation campaign are to (1) study the impact of minor alloying elements on the neutron-irradiated mechanical properties of FeCrAl alloys and (2) collect neutron-irradiated mechanical properties on AFA alloys for comparison with those of FeCrAl alloys. This campaign will include both tensile and fracture toughness specimens tested following HFIR irradiation at temperatures representative of normal operating conditions in light-water reactors. The pre-irradiation characterization to date, the irradiation plan for the FeCrAl and AFA specimens, and the subsequent post-irradiation experimental test plan are presented in this report, along with the status of HFIR builds and scheduled insertion dates.

36 MATERIALS SCIENCE↗

High-Fluence Active Irradiation and Combined Effects Testing of Sapphire Optical Fiber Distributed Temperature Sensors

The goal of this work was to investigate the in-core performance of sapphire optical fiber temperature sensors and to develop clad sapphire optical fibers for in-core instrumentation. We fabricated clad sapphire optical fibers and evaluated the distributed sensing performance of these sensors via optical backscatter reflectometry under high fluence and combined radiation and temperature effects. A series of irradiations was completed to evaluate the effect of irradiation on sapphire optical fiber temperature sensors and to determine the operational limits of these sensors. (1) Objective 1: Fabricate sapphire optical fiber sensors. (2) Objective 2: Evaluate the clad sapphire fiber to verify single-mode behavior and determine and characterize the light modes supported by optical fibers. (3) Objective 3: Characterize the in-core temperature sensing of sapphire optical fiber, as well as the combined temperature and irradiation effects. (4) Objective 4: Evaluate the lifetime and performance of the sensor under irradiation to high neutron fluence. Objectives 1, 2, and 3 were completed during the first 2 years of the project. Due to the Covid pandemic, Objective 4, a high-fluence irradiation performed at the Massachusetts Institute of Technology Research Reactor (MITR), was delayed, as partner facilities were subject to mandatory shutdowns and required a 1 year, no-cost extension. This irradiation was eventually completed on December 12, 2022. This work indicates that sapphire optical fiber sensors may be a solution for ultra-high-temperature applications in which traditional silica optical fibers are prone to fail. Sapphire sensors are potentially suitable for experiments featuring temperatures above 700°C for long periods of time, or for any length of time above 1000°C. Experiments featuring a low total fluence, such as irradiations conducted in the Transient Reactor Test (TREAT) facility, also represent good applications for sapphire optical sensors. Additional work is required to characterize the sapphire fiber cladding performance, which falls outside the scope of this project, as well as the effects of high temperatures on the response of the fiber. A comprehensive material study is recommended as future work to evaluate the attenuation in sapphire under irradiation, and how that attenuation changes with irradiation temperature. The drift and attenuation in the fiber at temperatures of up to 1600°C and a total fluence of up to 2.9 x 10 17 n/cm 2 was minimal, and the fibers returned to baseline after being heated to 1600°C under irradiation. This is promising for the future use of sapphire optical fibers in advanced reactors.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Conceptual Designs for Irradiation Creep Testing of SiC in HFIR

Understanding irradiation creep of nuclear fuel cladding is important to properly size the initial fuel-cladding gap and understand when pellet-cladding contact is expected to occur due to a combination of fuel swelling and cladding creep-down. Irradiation creep also plays a role in relaxing stresses that develop in-pile. Silicon carbide fiber–reinforced silicon carbide matrix (SiC/SiC) composites are the leading long-term accident-tolerant fuel cladding concept for light-water reactors (LWRs). Although some limited data are available regarding irradiation creep of the individual constituents (fibers, matrix), data regarding irradiation creep of SiC/SiC composites are currently insufficient. Additional data regarding irradiation creep compliance and the rupture lifetime (combination of creep and slow crack growth) are needed to understand material limitations. This work describes the design and development of two irradiation vehicles that are being pursued for testing SiC/SiC concepts in the High Flux Isotope Reactor (HFIR). The first is a passive experiment, referred to as the PRECISE experiment, that leverages the constant coolant pressure of HFIR to compress a metallic bellows and provide a well-characterized load to drive creep in a SiC/SiC dog bone specimen. The total creep strain would be quantified post-irradiation by measuring dimensional changes of the specimen length as well as local dimensional changes within the gauge region. Non-stressed specimens would also be irradiated under the same conditions to provide an indication of dimensional changes due to radiation-induced swelling in the absence of creep. A second, more complex experiment, referred to as the INSITE experiment, is being designed in parallel that would use pneumatics to pressurize a metal bellows and linear variable differential transformers (LVDTs) to measure the specimen displacement in situ during irradiation. Such an experiment would provide significantly more data regarding the evolution of the creep compliance as a function of dose and applied stress within a single experiment but would require significantly more development time and cost to execute. The primary concern with the INSITE experiment is the accuracy, reliability, and expected lifetime of the LVDTs during irradiation at elevated temperatures. Efforts are being made to adjust the experiment design and operating procedure to limit LVDT temperatures and mitigate or otherwise compensate for uncertainties due to factors such as temperature fluctuations, creep in the surrounding structural materials, and drift of the LVDTs. This work describes the experiment designs, thermal and structural analysis that were performed to ensure that the desired temperature and stress conditions can be achieved, some initial sensitivity analyses to predict the evolution of the radiation-induced specimen displacements, and potential sources of uncertainty in the measurements. Out-of-pile testing is being performed in parallel to confirm that the test trains achieve the expected stress states in the specimens and do not result in prohibitive stress concentrators (e.g., in the grip regions) that might risk pre-mature failure. The PRECISE experiments are proceeding toward fabrication and assembly with HFIR insertion planned during fiscal year 2026. The INSITE experiment is progressing toward out-of-pile demonstrations, which will provide more conclusive evidence regarding the feasibility of executing these tests in HFIR or whether alternative displacement monitoring techniques may need to be considered.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

BOILER Experiment Material Characterization and HFIR Irradiation Status

Pre-oxidized alumina-forming austenitic (AFA) steels have been previously identified as candidate alloys for structural components in lead-cooled fast reactors (LFRs). They offer compatibility with liquid Pb, high-temperature strength, formability, and cost advantages. However, variations in Ni content can affect the formation and stability of the Al 2 O 3 layer, influencing compatibility with liquid Pb. The effect of fast neutron irradiation on Al 2 O 3 stability in liquid Pb also requires evaluation. Therefore, understanding how Ni concentrations impacts pre-oxidized AFAs under combined extremes of irradiation and liquid metal corrosion is essential before safe deployment. The Behavior Of In-situ Lead Environments & Radiation (BOILER) experiment was developed under the Nuclear Science User Facilities (NSUF) program to integrate alloy development, irradiation experiment design, and irradiated materials characterization. In this effort, two pre-oxidized AFA steels with 20 wt% and 25 wt% Ni, hereinafter referred to as GA05-20Ni and GA05-25Ni, were produced. An irradiation experiment was then planned for the High Flux Isotope Reactor (HFIR), designed for passive heating of irradiation rabbit capsules from gamma heating in the HFIR flux trap (1 × 10 15 n/cm 2 ·s, >0.1 MeV). This heating melts Pb and exposes the pre-oxidized AFA steel specimens to nominal temperatures of 400 and 650°C. Detailed neutronics and thermal analyses were performed, though based on nominal design rather than as-built, as-irradiated conditions. This report documents further characterization of the pre-oxidized AFAs in the unirradiated condition. It also includes as-built thermal analysis using measured component dimensions, updated fill gas concentrations, and actual HFIR irradiation positions. Finally, the report summarizes capsule fabrication, current irradiation status, projected completion, estimated damage accumulation, and initial plans for post-irradiation examination plans.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Postirradiation Examination of WIRE-21 Experiment Irradiated in the High Flux Isotope Reactor

Westinghouse Electric Company is developing wireless sensors to monitor the centerline temperature and internal pressure of commercial light-water reactor fuel rods during irradiation. Oak Ridge National Laboratory and Westinghouse Electric Company developed the Wireless Instrumented RB Experiment 2021 (WIRE-21) to test wireless temperature and pressure sensor technologies in a removable beryllium position in the High Flux Isotope Reactor. The experiment was irradiated for a total of 75 days, at temperatures ranging from approximately 150°C to 400°C, resulting in a peak fast (energy > 0.1 MeV) neutron fluence of about 3 × 10 21 n/cm 2 . The temperature was intentionally cycled multiple times to compare the response of the wireless temperature sensor to collocated thermocouples. Similarly, the pressure sensor was actuated in multiple steps to compare the response of the wireless measurement to excore pressure transducers (Petrie et al., 2023). After irradiation, the experiment was disassembled in the Irradiated Fuels Examination Laboratory (IFEL) hot cell at Oak Ridge National Laboratory with the intent to recover sensor and dosimetry components, document the as-irradiated condition of the hardware, and investigate possible causes of the sensor behavior observed during irradiation. The postirradiation examination successfully recovered and preserved key WIRE-21 components. After the housing was removed using a milling machine, the internal experiment sections were examined. All eight fiber-optic sensors were recovered, cut, and stored. The silicon carbide thermometry, temperature sensor, pressure sensor, lower spacer, and selected pressure and temperature cable sections were also removed and stored. The metal bellows of the pressure sensor was found to be plastically deformed, indicating that it had been properly pressurized during irradiation and generally behaved as expected. X-ray diffraction analysis of a section of one of the irradiated inductor cores within the pressure sensor was performed and confirmed the presence of phase-pure alpha ferrite (i.e., no unexpected phase transformations). Inductance testing was performed on the irradiated pressure sensor cores using an unirradiated test coil, and DC resistance measurements of the transceiver coils were also performed. The measurements with irradiated inductor cores assembled inside unirradiated coils showed slightly reduced inductance compared to measurements made with unirradiated cores, but the difference was not sufficient to explain the more significant reductions in inductance that were observed in-pile. Therefore, it is suspected that degradation of the inductor coils (specifically the wire wrapping) is responsible for the reduced inductance observed in-pile.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

SILICON CARBIDE THERMOMETRY USING RAMAN SPECTROSCOPY ON IRRADIATED TRISO PARTICLES

Silicon carbide (SiC) passive thermometry has emerged as a promising post-irradiation examination (PIE) technique for estimating irradiation temperature near the end of irradiation. While dilatometry techniques have been traditionally used to analyze prismatic samples after irradiation, Raman spectroscopy has recently been shown to provide comparable results by analyzing Raman-active phonon modes. In this work, Raman spectroscopy has been applied to the SiC layer of cross-sectioned irradiation tristructural isotropic (TRISO) particles from the AGR-5/6/7 experiment to evaluate the feasibility of particle-scale passive thermometry. Two-dimensional Raman mapping was used to measure the position of the SiC longitudinal optical (LO) phonon, which was then converted to an apparent irradiation temperature using a previously established empirical correlation. Particles from AGR-5/6/7 Compacts 2-2-1 and 5-1-3 were selected as their calculated time-averaged, volume-averaged (TAVA) temperatures (828°C and 706°C, respectively) fall within the range of the sensitivity of the experimental approach. The use of SiC thermometry was anticipated to confirm or highlight potential deviations from calculated end-of-life TAVA temperature across compacts. Four particles from Compact 2-2-1 and two particles from Compact 5-1-3 were selected based on 110mAg inventory (either some measurable activity or below the minimum detection limit) which is commonly used as an indicator of in-pile temperature variation of particles within the same compact. Across every particle selected it was determined that the average LO peak position was located around 968 cm-1 to 969 cm-1. Using the previously determined empirical correlation, this corresponds to an irradiation temperature around 950°C to 966°C, which does not align with the reported TAVA temperature values. This discrepancy in apparent irradiation temperatures likely reflects a combination of uncertainties in the calculated particle temperatures and differences in irradiation history between the present specimens and those used to establish the empirical Raman calibration such as neutron flux (damage rate) and SiC microstructure (as fabricated and irradiated).

Vawdrey, Josh [ORNL]↗

Long-term variations in total solar irradiance

For more than a decade total solar irradiance has been monitored simultaneously from space by different satellites. The detection of total solar irradiance variations by satellite-based experiments during the past decade and a half has stimulated modeling efforts to help identify their causes and to provide estimates of irradiance data, using `proxy' indicators of solar activity, for time intervals when no satellite observations exist. In this paper total solar irradiance observed by the Nimbus-7/Earth Radiation Budget (ERB), Solar Maximum Mission (SMM)/Active Cavity Radiometer Irradiance Monitor (ACRIM) 1, and Upper Atmosphere Research Satellite (UARS)/ACRIM 2 radiometers is modeled with the Photometric Sunspot Index and the Mg II core-to-wing ratio. Since the formation of the Mg II line is very similar to that of the Ca II K line, the Mg core-to-wing ratio, derived from the irradiance observations of the Nimbus-7 and NOAA9 satellites, is used as a proxy for the bright magnetic elements. It is shown that the observed changes in solar irradiance are underestimated by the proxy models at the time of maximum and during the beginning of the declining portion of solar cycle 22 similar to behavior just before the maximum of solar cycle 21. This disagreement between total irradiance observations and their model estimates is indicative of the fact that the underlying physical mechanism of the changes observed in the solar radiative output is not well-understood. Furthermore, the uncertainties in the proxy data used for irradiance modeling and the resulting limitation of the models should be taken into account, especially when the irradiance models are used for climatic studies.

Pap, Judit M.↗

Surface Irradiances of Edition 4.0 Clouds and the Earth's Radiant Energy System (CERES) Energy Balanced and Filled (EBAF) Data Product

The algorithm to produce the Clouds and the Earth’s Radiant Energy System (CERES) Edition 4.0 (Ed4) Energy Balanced and Filled (EBAF)-surface data product is explained. The algorithm forces computed topof- atmosphere (TOA) irradiances to match with Ed4 EBAF-TOA irradiances by adjusting surface, cloud, and atmospheric properties. Surface irradiances are subsequently adjusted using radiative kernels. The adjustment process is composed of two parts: bias correction and Lagrange multiplier. The bias in temperature and specific humidity between 200 and 500 hPa used for the irradiance computation is corrected based on observations by Atmospheric Infrared Sounder (AIRS). Similarly, the bias in the cloud fraction is corrected based on observations by Cloud–Aerosol Lidar and Infrared Pathfinder Satellite Observations (CALIPSO) and CloudSat. Remaining errors in surface, cloud, and atmospheric properties are corrected in the Lagrange multiplier process. Ed4 global annual mean (January 2005 through December 2014) surface net shortwave (SW) and longwave (LW) irradiances increase by 1.3Wm22 and decrease by 0.2Wm22, respectively, compared to EBAF Edition 2.8 (Ed2.8) counterparts (the previous version), resulting in an increase in net SW 1LWsurface irradiance of 1.1Wm22. The uncertainty in surface irradiances over ocean, land, and polar regions at various spatial scales are estimated. The uncertainties in all-sky global annual mean upward and downward shortwave irradiance are 3 and 4Wm22, respectively, and the uncertainties in upward and downward longwave irradiance are 3 and 6Wm22, respectively. With an assumption of all errors being independent, the uncertainty in the global annual mean surface LW 1 SW net irradiance is 8Wm22.

Kato, Seiji↗

AGR-5/6/7 Irradiation As Run Predictions Using PARFUME

The PARticle FUel ModEl (PARFUME), a fuel performance modeling code used for high-temperature gas-cooled reactors, was used to model the Advanced Gas Reactor (AGR)-5/6/7 irradiation test using as-run physics and thermal data. The AGR-5/6/7 irradiation test consists of the combined fifth, sixth, and seventh planned irradiations of the AGR Fuel Development and Qualification Program. The AGR-5/6/7 test train is a multi-capsule, instrumented experiment that is designed for irradiation in the 133.4-mm diameter northeast flux trap position of the Advanced Test Reactor (ATR) at Idaho National Laboratory. Each capsule contains compacts filled with uranium oxycarbide unaltered fuel particles. This report documents the calculations performed to predict the failure probability of tristructural isotropic (TRISO)-coated fuel particles during the AGR-5/6/7 experiment. In addition, this report documents the calculated fission product release fraction from the fuel. The calculations include modeling of the AGR 5/6/7 irradiation that occurred from February 2018 to July 2020 over nine ATR cycles, including six normal cycles and three power axial locator mechanism cycles, for a total of approximately 376 effective full power days (EFPD). The irradiation conditions and material properties of the AGR-5/6/7 test predicted zero fuel particle failures in Capsules 1, 3, and 4. Fuel particle failures were predicted in two of the compacts in Capsule 2 and one particle failure is predicted in each one of the compacts in Capsule 5. All compacts that exhibited fuel particle failures predicted by PARFUME were caused by localized stress concentrations in the silicon carbide (SiC) layer caused by cracking in the inner pyrolytic (IPyC) layer. In addition, shrinkage of the buffer and IPyC layer during irradiation resulted in formation of a buffer-IPyC gap. Compacts with a lower irradiation temperature and fluence experienced the smallest buffer-IPyC gap formation. Conversely, higher irradiated temperature compacts with a high fluence experienced the largest buffer-IPyC gap formation. Compact 3-6-3 experienced the largest buffer IPyC gap formation of just under 21.7 µm. The release fraction of fission products silver (Ag), cesium (Cs), and strontium (Sr) vary depending on capsule location and irradiation temperature. The maximum release fraction of Ag occurs in Capsule 3, reaching up to 59.5% for the TRISO fuel particles (compact 3-6-3). The release fraction of the other two fission products, Cs and Sr, are much smaller. A maximum Cs release fraction of 1.1% occurred in compact 3-4-3 and 4.4% for Sr in compact 3-6-3.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

X-ray Computed Tomography of Irradiated and Unirradiated AGR-3/4 Compacts

X-ray Computed Tomography (XCT) has been utilized to image and characterize compacts from the combined third and fourth irradiation of the Advanced Gas Reactor (AGR) Program, AGR-3/4, fuel. The experiment contained tristructural isotropic (TRISO)-coated fuel particles as well as designed-to-fail (DTF) fuel particles. Two irradiated compacts, representing the lower and higher range of AGR-3/4 burnup (4.85% and 14.92% fissions per initial heavy metal atom FIMA) were examined. These represent the first known highly irradiated TRISO fuel compacts to be examined via X-ray CT. Additionally, two unirradiated compacts from the same production batch as the examined irradiation compacts were also imaged for a baseline comparison. As XCT of irradiated TRISO compacts is not a commonly implemented characterization technique, a significant portion of the report focuses on developed methodology and imaging conditions. A specialized sample shielding device was developed and fabricated specifically to limit received dose to staff during sample preparation for XCT and to minimize excess gamma radiation dose to sensitive electronic components with the utilized X-ray system. Significant penetration through the uranium oxycarbide fuel kernels by significantly hardening the X-ray beam with specialized proprietary filters acquired from Carl Zeiss NTS Ltd. The filter utilized resulted in an average X ray photon energy of ~110 keV which approaches uranium’s K-edge (~115 keV), maximizing penetration for a microfocus X-ray source. The gamma-radiation emitted from the irradiated AGR-3/4 TRISO compacts, has the same properties and mechanisms for interaction with matter as X-rays, thus the detection of gamma-radiation by the utilized X-ray detectors was initially a concern. However, although ?-rays did produce an observable signal on the X-ray detector, its contribution to the overall imaging results appeared negligible upon 3D reconstruction. The neglibile impact on the resulting 3D reconstructed volumes were likely the result of: (1) a significantly lower detection efficiency for ?-rays relative to X-rays; (2) An X-ray flux at the detector several orders of magnitude higher than that of the impinging ?-rays from the irradiated compacts. These results suggest that irradiated compacts with significantly higher radiation fields can be examined in the future if an acceptable route for sample handling and preparation can be determined. Additionally, the 3D imaging results of XCT can provide a valuable means of assessing compacts. While in many ways complimentary to traditional post irradiation examination techniques such as optical ceramography, XCT can provide additional insight into compact features traditionally difficult to discern directly from cross-sectional imaging alone. Preliminary analyses on kernel size, morphology (aspect ratio and sphericity), and kernel orientation were presented. Sphericity, a simple morphological shape descriptor, was utilized to screen for kernel extrusions within the high burnup compact. The number of kernel extrusions identified via XCT represented an approximate two-fold increase from the quantity of extruded particles observed (via optical ceramography) in adjacent compacts from the same irradiation capsule. While numerical analysis of the compact datasets was highly preliminary, initial results show promise for providing complimentary metrics to current AGR-3/4 PIE and potentially additional insight into the processes driving TRISO fuel degradation during reactor operation. Additional analyses to be performed at a later date include a more detailed examination of kernel size, kernel sphericity (and observed kernel extrusions), and sphericity. Given all particles can be observed in a single data volume possible correlation of spatial position with observed kernel features will also be made at a later date.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Performance Before and After Irradiation of Pixelated 3D Silicon Sensors for the HL-LHC CMS Tracker

The Large Hadron Collider (LHC) particle accelerator at European Center for Nuclear Research (CERN) will be shut down starting in 2026 to achieve the High Luminosity Large Hadron Collider (HL-LHC) upgrade. The upgrade will allow for higher fluences, in order to increase the probability of detecting increasingly rare particles, and to obtain higher precision measurements of known particles. To accommodate the new accelerator conditions, many aspects of the Compact Muon Solenoid (CMS) detector will be upgraded; of particular interest for this thesis are the silicon pixel detectors located in the inner tracker. These will be replaced and upgraded to accommodate the higher fluences of the HL-LHC upgrade, as well as to replace existing sensors which have sustained radiation damage. In order for the new sensors to operate under high luminosity conditions, they must be increasingly radiation hard, and in order to detect rare particles, they must be increasingly more precise. The performance of one Centro Nacional de Microelectronica (CNM) 3D silicon sensor before and after undergoing irradiation at fluences similar to those which will be observed at the HL-LHC was investigated to determine radiation hardness and precision. Data was collected at Fermi National Laboratory (Fermilab), in the Fermi National Laboratory Test Beam Facility (FTBF) silicon tracker telescope, which can be used to determine the number of particles, and tracks made by high energy protons passing through. The sensor was also irradiated at Fermilab in the Irradiation Test Area (ITA). Prior to data collection a tuning procedure is carried out to determine ideal bias voltage operating conditions, mask noisy and dead pixels, adjust to the ideal threshold, and map sensor gain. Data is then collected at the FTBF, where the sensor is installed in the center of the FTBF silicon telescope. Variables, including angle and bias voltage, are varied throughout data collection. Data is then processed using an alignment software to determine the exact telescope geometry, along with the tracks which were observed passing through the sensor and telescope. Sensor performance was found to be comparable before and after irradiation, with irradiated results showing slightly lower efficiencies and cluster sizes. Position resolution is comparable both before and after irradiation, and similar distributions of cluster shape are observed. After irradiation, the sensor shows increasing collected charge with bias, an indication of increased width of the depletion region. Peak charge pre-irradiation is higher than post-irradiation peak charge, indicating the irradiated results are not taken under fully-depleted conditions.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Determination of neutron irradiation temperatures of SiC using electrical resistivity method

The irradiation temperature of silicon carbide (SiC) was determined post-irradiation by examination of the recovery of the electrical resistivity due to thermal annealing in a rapid heating/cooling optical furnace. High-purity, high-resistivity grade SiC is routinely used as a passive temperature monitor in neutron irradiation studies at the High Flux Isotope Reactor (HFIR), and this paper presents an alternative automated technique for determination of the irradiation temperature the SiC experienced. Neutron collisions with the atoms results in displaced lattice atoms (interstitials) that act as electron donors yielding a significant decrease in electrical resistivity. The irradiation defects become thermodynamically unstable and start to recombine, when annealed above the irradiation temperature, resulting in a recovery of the electrical resistivity. The resistivity is measured at a fixed elevated temperature above ambient, which is below the target irradiation temperature. When the resistivity is plotted as a function of annealing temperatures, a clear increase is observed due to the recovery of irradiation defects. We have demonstrated that this electrical resistivity measurement of SiC is effective to determine irradiation temperature of SiC. In conclusion, energy levels of various defects in SiC were calculated from Arrhenius plots of electrical conductivity versus inverse temperature.

36 MATERIALS SCIENCE↗

Report on the Incorporation of Post-Irradiation Examination Results of Yttrium Hydride for Advanced Moderator Handbook

Department of Energy’s (DOE’s) Microreactor program (MRP) aims to provide the fundamental data to enable the development of microreactors. As such, material property data of critical materials for microreactor technologies are researched. Because substoichiometric yttrium dihydride (YHx, where x<2) is considered as a potential solid neutron moderator, its material property data has been combined in the Advanced Moderator Material Handbook which includes thermodynamic and thermophysical properties of YHx with the exception of irradiated material’s properties due to limited PIE. To fill the knowledge gap for the irradiated YHx, specimens and irradiation capsules were prepared at Los Alamos National Laboratory (LANL). Specimens were irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory’s (INL’s). post-irradiation examination (PIE) was performed at INL’s Materials and Fuels Complex (MFC). This report compiles the PIE results of irradiated YHx specimens through fiscal years 2022 and 2023 (FY22-23) . The PIE data will directly be incorporated into the newer version of the Advanced Moderator Material Handbook. The main takeaways include that (i) the geometrical stability and mechanical integrity of YHx was intact with couple exceptions after high-temperature irradiations (600-800°C), (ii) hydrogen content variation due to manufacturing or irradiation in YHx caused visible surface discoloration, that is also related to the microstructural changes, (iii) qualitative comparisons of PIE methods implied that H retention was significantly higher at 600°C as compared to 800°C, (iv) thermal properties included signatures correlated with the H loss or re-gain, (v) importance of manufacturing readiness and initial as-manufactured specimens history was emphasized, (vi) the needs of targeted irradiations focusing on temperature and time parameters and very targeted PIE were specified.

08 HYDROGEN↗

Hermeticity of SiC/SiC composite and monolithic SiC tubes irradiated under radial high-heat flux

Demonstration of hermetic SiC fiber–reinforced SiC matrix composite cladding under normal operating environments has been identified as one of the most critical feasibility issues for accident-tolerant fuel cladding in light-water reactors. This study provides critical experimental data needed for understanding the effects of irradiation on hermeticity. SiC composite and monolithic tubes were neutron-irradiated to 2 displacements per atom with and without a nominal radial heat flux of 0.6 MW/m2 to produce a simulated in-pile stress state for the normal operation of a light-water reactor. The through-thickness temperature gradient under irradiation results in a gradient in swelling, which causes a significant stress buildup. Such irradiation-induced stress was modeled using a commercial finite element analysis code. The radial heat flux–irradiation synergism was experimentally investigated by constructing a special irradiation capsule and evaluating the helium hermeticity of the specimens. The simulated stress state exhibited a near equi-biaxial tensile axial and hoop stress of ~150 MPa at the inner surface of the SiC composite tube. This stress level is potentially beyond the matrix cracking stress. Degradation of hermeticity of the SiC composite tubes was observed after irradiation, indicating irradiation-induced cracking, whereas the irradiated monolithic SiC tubes remained hermetic. In conclusion, the results indicate that loss of hermeticity caused by radiation-induced microcracking is a potential issue for SiC composite cladding, depending on the magnitude of the temperature gradients. Coating the outer surface of the cladding was identified as a mitigation strategy that might overcome the cracking issue.

36 MATERIALS SCIENCE↗

Annealing influence on the microstructure of irradiated U-Mo monolithic fuel foils

In this study we compared the microstructure evolution of U-Mo fuel foils produced with and without heat treatment at low burn-up via advanced post-irradiation examination. The aim of this study is to observe after irradiation the ways in which the fabrication processes have influenced fuel behavior at early-stage irradiation, as for very low burn up microstructural studies are lacking. In this work it was observed that the larger grain size detected in the heat-treated samples before irradiation led to decreased grain refinement after irradiation. Grain refinement was associated with the presence of small nano-size bubbles and precipitates. This phenomenon is hypothesized to influence early fuel swelling during reactor irradiation. Grain refinement was also observed to increase in regions where γ-U decomposition was present. Thus, it was enhanced in the samples fabricated without heat treatment. The heat treatment also increased the thickness of the U-Mo/Zr interface, namely of the UZr 2 layer. However, the influence of this layer on fuel performance needs further investigation. On one side, it may contribute to better mechanical bonding; on the other, it may influence swelling and blistering in the interaction layer as porosity increases when this layer is increased. This was observed especially in the presence of increased area containing low Mo concentration, and thus containing a higher fraction of the α-U phase, which is highly susceptible to irradiation induced swelling. Strong evidence of reverse transformation under irradiation (α-U + γ'-U2Mo → bcc γ-U) was observed in these samples. While the precipitates (carbides and oxide) seem to be unaffected by the irradiation at these low burnups. However, further analyses are necessary at higher burn-up to assess the exact impact different heat treatments have on fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Design and testing of an enriched uranium fueled molten salt irradiation vehicle

Molten salt reactors (MSRs) have garnered increasing attention recently with several demonstration efforts on the way. A key challenge to the licensing basis for these reactors is the lack of experimental data on fueled salts. This is expected to be crucial to the safety evaluation and licensing basis of reactors of this type deployed in the future. While capability for irradiating molten salts has started being reestablished in the recent decade, no enriched fuel irradiation capability has been developed and tested as of yet. A new experiment vehicle under development at Idaho National Laboratory (INL) is presented here. The Molten-salt Research Temperature-controlled Irradiation (MRTI) experiment was developed to host enriched-uranium bearing salt samples to be irradiated at a test reactor within the lab complex. One of the key scientific objectives is to provide irradiated salt samples for post irradiation examination (PIE) to study the impact of fission product generation and neutron/gamma radioactivity on the salt solution and salt-facing wall material. This paper provides a detailed overview of the mechanical design of the experiment, followed by an overview of the fabrication and assembly of an initial prototype vehicle (with non-fuel bearing salt). A summary of the key analyses conducted as a part of the performance and safety evaluation is then provided. Lastly, an overview of the test conducted in prototypic out-of-pile (non-neutron) environment are shown. These evaluations provide the foundation for a planned irradiation of and enriched uranium-bearing chloride salt sample in the near term. The upcoming irradiation will contain 13cm 3 of UCl 3 -NaCl salt (93% enrichment) generating around 20 W/cm 3 of fission energy during irradiation and a temperature range that can be contained between bounds of 525-900°C.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗