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Initial development of a method for correlating indentation test results to damage accumulation in high temperature structural materials

This report describes an experimental approach based on microindentation creep or relaxation tests for assessing the remaining creep life of a sample material. The objective for this experimental program is to complement the development of passively loaded in situ surveillance specimens. These surveillance specimens could be placed in future advanced reactors to assess the degradation of structural properties, primary creep and creep-fatigue life, when the material is exposed to actual reactor operating conditions. The specimens and the corresponding indentation test protocol could form the basis of a structural health monitoring program designed to ensure the safe continued operation of the component given the relatively unknown effect of the reactor coolant chemistry, radiation exposure, and other environmental effects on the material properties of the constituent structural materials.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Quality Assurance of the Irradiated EBR-II Metallic Fuels Data

The U.S. DOE-NE’s Advanced Reactor Technologies (ART) Fast Reactor Program (FRP) and the NE-4 Advanced Fuels Campaign (AFC) have jointly undertaken efforts to qualify post-irradiation examination (PIE) data for Experimental Breeder Reactor II (EBR-II) and Fast Flux Test Facility (FFTF) metallic fuels. Among the thousands of PIE datasets in the Metallic Fuels Irradiation & Physics Database (FIPD), data from selected EBR-II experiments have been prioritized as the most valuable to the U.S. nuclear industry for licensing activities related to metallic fuel-based advanced fast reactors. This report summarizes the general data qualification progress of the EBR-II and FFTF experiments, with focus on the selected EBR-II experiments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Conceptual Design of Neutron Sensor Qualification Device

The Advanced Sensors and Instrumentation Program at Idaho National Laboratory has been formulating strategies to qualify sensors for use in nuclear environments, particularly in irradiation experiments and advanced reactors. When qualifying neutron sensors for use in high-temperature environments, the wide range of neutron flux levels and representative energy spectra presents significant challenges. This paper discusses the development of the Neutron Sensor Qualification Device (NQD), which is designed to test neutron sensors in high temperature controlled environments with known neutron spectra, addressing the spatial and spectral complexities of neutron fluxes in reactor cores. The proposed NQD will be situated in the exposure room at the Armed Forces Radiobiology Research Institute, thus affording a unique capability to expose sensors to high neutron and gamma fluxes. To achieve thermal control, the device will utilize a radiation-hardened tube furnace, accommodating multiple sensors and neutron activation dosimetry wires. Titanium, iron, and cobalt dosimeter wires are chosen from the American Society for Testing and Materials and International Reactor Dosimetry and Fusion File libraries as references for providing energy-dependent fluence measurements. The design ensures precise sensor positioning to minimize mutual shielding and flux perturbation, which are evaluated via Monte Carlo N particle Transport Code (MCNP) simulations. These simulations have informed the development of guidelines on sensor placement within the NQD. The NQD is essential to the qualification of neutron sensors for advanced reactor technologies. It enables controlled testing of a statistically significant number of sensors, thereby supporting assessments of sensor performance across various neutron flux levels and temperatures. This paper highlights the detailed planning for the NQD prototype, along with its inaugural irradiation (scheduled for fiscal year [FY] 2025). The results from this initial testing will be fundamental in evaluating the device’s performance and establishing measurement uncertainty for in-pile neutron sensor measurements.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Intracore Natural Circulation Study in the High Temperature Test Facility

The development of the Modular High-Temperature Gas-Cooled Reactor is a significant milestone in advanced nuclear reactor technology. One of the concerns for the reactor’s safe operation is the effects of a loss-of-flow accident (LOFA) where the coolant circulators are tripped, and forced coolant flow through the core is lost. Depending on the steam generator placement, loop or intracore natural circulation develops to help transfer heat from the core to the reactor cavity, cooling system. This paper investigates the fundamental physical phenomena associated with intracore coolant natural circulation flow in a one-sixth Computational Fluid Dynamics (CFD) model of the Oregon State University High Temperature Test Facility (OSU HTTF) following a loss-of-flow accident transient. This study employs conjugate heat transfer and steady-state flow along with an SST k-ω turbulence model to characterize the phenomenon of core channel-to-channel natural convection. Previous studies have revealed the importance of complex flow distribution in the inlet and outlet plenums with the potential to generate hot coolant jets. For this reason, complete upper and lower plenum volumes are included in the analyzed computational domain. CFD results also include parametric studies performed for a mesh sensitivity analysis, generated using the STAR-CCM+ software. The resulting channel axial velocities and flow directions support the test facility scaling analysis and similarity group distortions calculation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

REBUS-PC v1.5 Verification Test Summary

Motivated in part by its usage for analysis of the University of Missouri Research Reactor (MURR), the verification of the REBUS-PC software for θ-R-Z geometries is discussed and displayed in this manuscript. Of particular importance is to show that the eigenvalue, flux, power, and burnup outputs of the software given a user problem is correct. REBUS-PC contains many features and MURR only makes use of some of those aspects. As an example, the use of region specific cross section sets, interpolation of the cross section data with respect to burnup, and automatic movement of control rods during the fuel cycle is discussed and displayed. To demonstrate the accuracy, 22 verification tests based upon 7 physical geometries are discussed. Geometry descriptions are provided in Section 2 and the REBUS-PC results for each verification test are discussed in Section 3. These verification tests consist of both analytic problems with known solutions and a more complicated input consistent with usage of REBUS-PC on the MURR reactor itself called STRZ. In this verification test summary report, the REBUS-PC software is repeatedly demonstrated to reproduce, or closely match, the eigenvalue, flux, and power distributions from analytic test problem solutions, demonstrating that the implemented finite difference approximation in θ-R-Z is working as intended. Several additional REBUS-PC features are tested, such as control rod movement by detailed comparisons of the results against reference solutions obtained using an auxiliary implemented MatLab program. As expected, the REBUS-PC software produces results that are 100% consistent with the stated capabilities and thus the verification exercise is completed. These verification tests should be executed with each re-compilation of the REBUS-PC source and after any source code changes. All output results from any such new work should be rigorously compared against the stored output of the 22 verification tests cited in this report that forms the basis of the verification process.

97 MATHEMATICS AND COMPUTING↗

As-run thermal-hydraulic analysis of the EPRI-3 experiment

The EPRI-3 experiment was designed to irradiate various types of reactor internal component steels at a temperature of 288°C. The specimens were irradiated in an instrumented test train inside a pressurized water loop in the center lobe of the ATR during cycles 155B and 158B. Temperature was monitored using thermocouples placed at the top of the test train and melt wires placed within the test train. The purpose of this analysis is to calculate specimen temperature using measured data on reactor power and as-run calculations of heating rates of the test train. The experiment contains four thermocouples and several melt wires spanning the temperature range 239°C to 327°C. The accuracy of the model is assessed by comparing the measured and calculated in-pile tube inlet to outlet temperature difference, comparing the measured and calculated thermocouple temperatures, and comparing the calculated melt wire temperature to the temperature range indicated by examination of the melt wires.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Cracking Behavior of Irradiated Ex-Plant Materials

The cracking behavior of reactor core internal materials is a key factor for the long-term safety and availability of light water reactors. Subject to high-temperature coolant, thermal and mechanical loading, and neutron irradiation, reactor core internal materials are susceptible to several degradation mechanisms during power operation. To understand the long-term effects of neutron irradiation, irradiated materials harvested from a decommissioned reactor were studied for their cracking susceptibility and fracture resistance. Small compact-tension specimens were machined from different locations on the baffle plates with irradiation doses ranging from 0.06 to 48.5 dpa. Crack growth rate and fracture toughness J-resistance (J-R) curve tests were performed on these specimens in a simulated light water reactor environment, and the fracture morphologies of the tested samples were examined with a scanning electron microscope. All samples behaved similarly under cyclic loading, and no deteriorated corrosion-fatigue behavior was observed in the test environments. Under constant load, no elevated cracking susceptibility was observed either in these samples at low stress intensity factors. However, a rapid cracking behavior featuring very high crack growth rates was observed in several high-dose samples. This rapid crack growth behavior was activated when the applied stress intensity factor, K, was sufficiently high. Once activated, the rapid crack growth remained steady even when the K was lowered to the pre-activation level and stopped only when the K was reduced drastically. Yet, the rapid crack growth could be re-activated repeatedly in these samples by raising the K above the initial activation level. This rapid cracking response may be related to the severe irradiation embrittlement experienced by these samples. The J-R curve tests performed with these samples showed a significant decline in fracture toughness with increasing neutron irradiation. Local cracking at the crack tip facilitated by the severe irradiation embrittlement of this material may be responsible for the rapid crack growth behavior demonstrated by this decommissioned material.

36 MATERIALS SCIENCE↗

Final report on assessment of molten salt corrosion testing of unirradiated and ion irradiated advanced manufactured high entropy alloys

Generation IV reactors and future fusion reactor designs have led to more demanding materials performance requirements due to their increased operating temperatures, corrosive coolants, and increased radiation doses compared to the current light-water reactor fleet. Among the innovative nuclear technologies under development, molten salt reactors stand out for their potential to offer superior fuel utilization, intrinsic safety characteristics, and economic viability. Of the proposed Generation IV designs, the gas fast reactor operates at 450 to 850°C and the molten salt reactor operates at 565 to 850°C, with the molten salt reactor design needing molten salt corrosion resistant materials [1, 2]. These increased temperatures and more extreme corrosion environments necessitate higher material performance, such as creep strength, radiation-tolerant microstructures, corrosion resistance, and high-temperature tensile properties. Hastelloy-N, a nickel-based alloy with additions of molybdenum and chromium, has been successfully employed to contain molten fluoride salt at temperatures up to 705°C. However, Hastelloy-N becomes embrittled upon neutron irradiation, primarily due to the accumulation of helium produced by (n,a) transmutation reactions. Furthermore, the corrosive nature of molten fluoride and chloride salts presents a formidable challenge, as these salts can react with and dissolve alloying elements such as Cr, Mo, and Fe, leading to selective leaching, loss of protective oxide layers, and accelerated degradation. High entropy alloys (HEAs) and refractory high entropy alloys (RHEAs) have emerged as a prominent area of interest, due to their ability to achieve tailored chemical compositions for specific applications. Unlike conventional alloys, HEAs are characterized by having multiple principal elements in equimolar or near equimolar ratios, leading to an unconventional alloying strategy [3]. This alloying strategy is believed to promote unique properties, such as single-phase stabilization of chemically compatible elements, lattice distortion effects due to atomic radius differences, and proposed sluggish diffusion effects. For extreme-environment applications, RHEAs have garnered much research interest because of the possibility of creating relatively ductile materials that can operate in extremely high-temperature environments, beyond the operating temperatures where other Ni-based superalloys begin to lose strength [4-6]. Idaho National Laboratory (INL) initiated a joint international effort with the Czech Republic to explore the feasibility of manufacturing HEAs for high-temperature nuclear applications using advanced manufacturing. This effort was funded at INL by the United States Department of Energy's Office of Nuclear Energy under the Advanced Reactor Technologies and Advanced Materials and Manufacturing Technologies (AMMT) Program. The HEAs were specifically designed for the corrosive and irradiation environments experienced in gas-cooled fast reactors, molten salt reactors, and fusion power. These alloys have been manufactured by multiple processes to determine the impact of manufacturing processes on the performance of the alloys in corrosive and irradiation environments. Preliminary molten salt corrosion testing showed that equimolar MoNbTiV and MoNbTi alloys exhibit exceptional performance, with arc-melted variants demonstrating only minimal degradation after 1000 hours of exposure to molten chloride salt at 700°C. Conversely, Nb2TiVZr2 showed significant molten salt corrosion susceptibility and microstructural instability during high-temperature molten salt exposures, and was, therefore deemed unfit for molten salt reactor applications. The MoNbTiV, MoNbTi, and Nb2TiVZr2 alloys were further evaluated through ion irradiation experiments conducted at the Michigan Ion Beam Laboratory at the University of Michigan. The microstructural stability and the evolution of irradiation-induced defects were characterized to assess the irradiation resistance of each of these alloys.

36 - MATERIALS SCIENCE↗

IASCC of 304 SS in BWR environments: Effects of post-irradiation annealing and surface condition

To investigate the impact of low-temperature post-irradiation annealing (PIA) on the stress corrosion cracking of neutron-irradiated 304 stainless steel, constant extension rate tests were conducted in simulated boiling water reactor normal water chemistry (BWR-NWC) and hydrogenated water chemistry (HWC) environments. Ten tensile samples, comprising five as-irradiated and five PIA specimens, were prepared by electropolishing the gauge section of electric discharge machined (EDM) samples. Here, the annealing treatment reduced the yield strength from approximately 550 MPa to around 425 MPa and significantly restored the ductility and the strain hardening capability of the alloy. Consequently, the susceptibility of this material to irradiation-assisted stress corrosion cracking (IASCC) was effectively mitigated, which is more prominent in HWC, as evident from fractography, which indicated a decreased propensity for intergranular (IG) fracture. Furthermore, it was observed that the polished surface facilitated crack initiation more readily than the EDM surface, suggesting that the EDM process suppressed crack initiation to some extent.

Crack initiation↗

Thermal diffusivity and thermal conductivity of SiC composite tubes: the effects of microstructure and irradiation

Cladding thermal conductivity is an important physical property in assessing the performance of silicon carbide (SiC)-cladded fuels for nuclear reactors. However, there is a significant lack of reliable data, particularly for irradiated materials, because the geometry complicates the measurement. This study investigates the thermal diffusivity of coupons with a curvature, machined from SiC fiber–reinforced SiC matrix composite tubes, with and without neutron irradiation under light water reactor–relevant temperature and dose conditions. The tested materials included full composite and duplex SiC composite tubes. The measurements were conducted using a modern flash diffusivity apparatus. The analyzed area on the specimen during diffusivity testing was reduced for improved measurement accuracy due to sample curvature. Post-irradiation measurements showed that the effects of neutron irradiation on thermal conductivity (e.g. thermal defect resistivity) are different between SiC composite plates versus tubes. The difference was explained by higher matrix density of the tube than the plate. This study provides reliable thermal properties of prototypic SiC composite tubes useful for fuel performance modeling of SiC-based cladding.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Determining the oxidation behavior of matrix graphite

This work presents the oxidation behavior of matrix graphite in air. Matrix graphite, graphite powder/flakes bonded by a small amount of non-graphitic carbon, surrounds coated fuel particles in order to form cylindrical fuel compacts (in prismatic core designs) or spheres (in pebble-bed reactor designs). This work focuses on oxidation tests conducted on two matrix graphite materials, one provided by Kairos Power and the other A3 matrix graphite. Some of the tests followed American Society for Testing and Materials (ASTM) oxidation testing standards using a vertical furnace system and others were performed in a thermogravimetric analyzer (TGA). It was determined that, at temperatures of 450 °C–700 °C, the oxidation rate of the Kairos matrix graphite follows the Arrhenius equation. In comparison with A3 matrix graphite, the Kairos matrix graphite shows better oxidation resistance at high temperatures (≥550 °C), but also a higher oxidation rate at low temperatures. Both the A3 matrix graphite and the Kairos matrix graphite materials may experience preferential oxidation of the partially graphitized binder. An oxygen penetration gradient was also observed when using the three characterization methods (i.e., optical microscope, x-ray tomography [XCT], and density profile by the lathe) enlisted in this research. In conclusion, the oxygen penetration depth increases with decreasing isothermal oxidation temperature, while the center of the oxidized samples (10% weight loss) remains almost untouched even at 500 °C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Mechanisms of stored energy release in silicon carbide materials neutron-irradiated at elevated temperatures

Understanding the stored energy release behavior of SiC is crucial for the design of SiC-based fuel cladding for light water reactors because stored energy release affects response during accident conditions. Differential scanning calorimetry was used to evaluate the stored energy of monolithic SiC and SiC fiber–reinforced SiC matrix composite variants following neutron irradiation under light water reactor–relevant dose and temperature conditions. The tests were performed at heating rates of 0.5, 3, and 20 K/min up to 1,273 K. The onset temperature of the energy release roughly corresponded to the irradiation temperature, and energy release was delayed as the heating rate increased. The monolithic and composite specimens exhibited similar stored energy release behavior up to ~1,000 K, and above that temperature, the energy release depended more on material type. The energy release measured in this study is below the material-specific heat capacity at temperatures below ~1,000 K but exceeds it under certain material and annealing conditions at temperatures above ~1,000 K. The amount of irradiation-induced volumetric swelling of the specimens was an indication of the total stored energy. Based on this observation, the energy release behavior was described by a swelling recovery model.

36 MATERIALS SCIENCE↗

Sensitivity analysis of thermal contact conductance modeling to inform MiniFuel irradiation capsule designs

The MiniFuel irradiation platform has been developed by Oak Ridge National Laboratory as a flexible, high-throughput separate effects testing capability within the High Flux Isotope Reactor (HFIR). Finite element thermal models are relied upon to design MiniFuel experiments to achieve a specific time-averaged irradiation temperature for experimental objectives. A previous study identified that uncertainty in the component heat generation rates and thermal contact conductance (TCC) model are the most significant contributors to predicted fuel temperature variance. To address both sources of uncertainty, this work performs sensitivity analysis on the TCC model to identify high-impact, high-uncertainty parameters that contribute to fuel temperature variance. The TCC model is analyzed in increasing detail, first using a standalone Python code, then again after coupling Python to the BISON fuel performance code. Furthermore, the parameters with the largest contributions to fuel temperature variance which can be reduced through design changes are identified as the initial subcapsule gas pressure, contact pressure between the fuel and dish, and the effective surface roughness of the interface. A set of design recommendations for future capsule designs has been established and applied to reduce the previously quantified average fuel temperature uncertainty ranges of ± 40 °C in the HFIR vertical experiment facilities (VXF) and ± 80 °C in the removable beryllium (RB) reflector to approximately ± 32 °C and ± 53 °C, respectively. This equates to a 21 % and 33 % reduction in the uncertainty range of the average fuel temperature for VXF and RB, respectively.

BISON↗

Enhanced mechanical properties of additive manufactured Grade 91 steel

High temperature stability of the mechanical properties, including creep behavior, are important factors to consider in certifying additive manufactured (AM) steels for reactor operation. AM-Grade 91 steel, tested at RT is shown to possess high yield strength, strain hardening and ductility even after high temperature aging for extended hours. Enhanced creep resistance at 650 ⁰C is also evident in the AM Grade 91 steel compared to wrought Grade 91 steel tested at the same conditions. In conclusion, the diverse and complex microstructure of this AM steel allows for both enhanced strength and ductility but increases the ductile-to-brittle transition temperature in these steels.

36 MATERIALS SCIENCE↗

Ce stabilized Ni–SrO as a catalytic phase transition sorbent for integrated CO 2 capture and CH 4 reforming

Integration of carbon dioxide capture from flue gas with dry reforming of CH 4 represents an attractive approach for CO 2 utilization. The selection of a suitable bifunctional material serving as a catalyst/sorbent is the key. This paper reports Ni decorated and CeO x -stabilized SrO (SrCe 0.5 Ni 0.5 ) as a multi-functional, phase transition catalytic sorbent material. The effect of CeO x on the morphology, structure, decarbonation reactivity, and cycling stability of the catalytic sorbent was determined with TEM-EDX, XRD, in situ XRD, CH 4 -TPR and TGA. Here, cyclic process tests were conducted in a packed bed reactor. The results indicate that large Ni clusters were present on the surface of the SrNi sorbent, and the addition of CeO 2 promoted even distribution of Ni on the surface. Moreover, the Ce–Sr interaction promoted a complex carbonation/decarbonation phase-transition, i.e. SrCO 3 + CeO 2 ↔ Sr 2 CeO 4 + CO 2 as opposed to the conventional, simple carbonation/decarbonation cycles (e.g. SrCO 3 ↔ SrO + CO 2 ). This double replacement crystalline phase transition mechanism not only adjusts the carbonation/calcination thermodynamics to facilitate SrCO 3 decomposition at relatively low temperatures but also inhibits sorbent sintering. As a result, excellent activity and stability were observed with up to 91% CH 4 conversion, >72% CO 2 capture efficiency and ~100% residual O 2 capture efficiency from flue gas by utilizing the CeO 2 ↔ Ce 2 O 3 redox transition. This renders an intensified process with zero coke deposition. Moreover, the SLDRM with SrCe 0.5 Ni 0.5 has the flexibility to produce concentrated CO via CO 2 -splitting while co-producing a syngas with tunable H 2 /CO ratios.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Document-Based Nuclear Archaeology

Deeper reductions in the nuclear arsenals will require better understanding of historic fissile material management and production. The concept of “nuclear archaeology” has been considered since the 1990s to provide the tools and methods to develop independent production estimates, primarily based on nuclear forensic techniques. Here, we propose to add a framework for reconstructing the history of a nuclear program that complements traditional nuclear archaeology techniques by examining the role of operating records to support such an effort. As a test case, we use the JEEP II reactor, a 2 MW civilian research reactor at Norway’s Institute for Energy Technology (IFE), in operation for more than fifty years, however, recently shut down permanently. We have collected, analyzed, and started to preserve the reactor’s operating records, which exist on both analog and digital media, and to simulate parts of its history using OpenMC/ONIX neutronics calculations. Here, a particular focus of this project has been on digital data curation and preservation to confirm and maintain the integrity, authenticity, and provenance of these records. In developing guidelines for best practices that conform to existing standards for long-term digital preservation and curation, we hope this project can help lay the basis for future nuclear archaeology efforts to support nuclear arms control and disarmament.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

Luminescent silica microagglomerates, synthesis, and environmental testing

Abstract Tracking mass through harsh environments requires surrogate particles that withstand the event and endure until sampling. Silica-covered quantum dots have been shown to withstand a range of environmental pHs from months to years; in this work they are shown to endure in anticipated local environments. Two methods of particle synthesis were employed to produce luminescent silica with particle diameters 0.1–4 μm. These tracer particles scale for mass production, tolerate harsh environments, and endure in debris. They could be deployed in places such as chemical explosions, industrial processes, geologic test beds, oil and gas fields, nuclear reactors, and geothermal plants to track mass under harsh conditions. Graphical abstract

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterizing the Performance of Fission Chambers for Local Neutron Flux and Spectrum Measurement

Three fission chambers were tested at The Ohio State University Research Reactor (OSURR) to evaluate fission chambers for neutron flux and spectrum measurements. Two of the fission chambers are commercial Photonis CFUR43 fission chambers—one utilizing highly enriched uranium-235 fissile deposits for thermal neutron detection and the other with highly depleted uranium-238 for fast neutron detection. This experiment was also performed in collaboration with French Alternative Energies and Atomic Energy Commission (CEA) with CEA suppling a uranium-235 loaded fission chamber built from the Photonis CFPR CE8/9 kit. The fission chambers were irradiated in a movable 6.5 inch dry tube at reactor powers of 50 kW, 200 kW, and 450 kW at ambient temperature and at 350°C. While all sensors demonstrated good linear sensitivity to reactor power, a leakage current of 6 nA was measured for the CFUR43 detectors. Additionally, the measured signal ratios of the two CFUR43 detectors did not match the theoretical values and are subject to further investigation on individual signal contributors.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗