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DOE OSTI2024

Interfacial Pressure Improves Calendar Aging of Lithium Metal Anodes

Lithium metal is a very attractive anode material because its theoretical specific capacity is approximately 10 times higher than conventional graphite anodes. Despite great promise, Li anodes suffer from capacity fade due to instabilities with the electrolyte as well as stranding of active Li. We have previously shown that applied interfacial pressure improves Li anode cycling because the pressure reduces the propensity for Li isolation and enables easier reconnection. Many researchers have also shown that calendar aging can lead to Li capacity loss and this has been attributed to either electrolyte decomposition with concurrent Li corrosion or to the formation of stranded Li. Our prior research focused on calendar aging during cycling suggests the mechanism for calendar aging is largely related to stranding of Li during rest and reconnection of the stranded Li upon further cycling, evidenced by similar average Coulombic efficiencies and Li loss in cells with and without rest. Because our calendar aging studies suggest Li stranding as a major cause of Coulombic efficiency drops and our Li cycling studies suggest this can be mitigated partially through applied interfacial pressure, we hypothesized that applied pressure would improve calendar aging by reducing stranded Li and enabling reconnection. We systematically varied applied pressure (0-1000 kPa) on Li metal anodes during cycling tests with and without intermittent calendar aging periods. Though the Coulombic efficiency decreases during aging periods, the lost capacity is recovered during subsequent cycles, as shown though average Coulombic efficiency and cumulative Li capacity loss analysis. We find that application of pressure partially mitigates calendar aging, in accordance with our hypothesis that calendar aging is caused by Li standing and can be mitigated to some degree with interfacial pressure. This is further supported by our results showing that the average Coulombic efficiency and cumulative Li capacity losses are similar over 50 cycles for cells that were continuously cycled and cells with periodic calendar aging periods. This result indicates that the losses during aging are reversible, which is consistent with Li stranding and reconnection. We show that pressure is one mitigation technique that helps reduce Li calendar aging in this study, but our finding that calendar aging is primarily governed by the stranding and reconnection of dead Li has wider implications. This research suggests that other mitigations which have been shown to prevent dead Li formation or encourage reconnection during cycling would also likely be successful for the purpose of improving calendar aging. The authors were supported by a Laboratory Directed Research and Development (LDRD) program. This work was performed, in part, at the Center for Integrated Nanotechnologies, an Office of Science User Facility operated for the U.S. Department of Energy (DOE) Office of Science. Sandia National Laboratories is a multi-mission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC (NTESS), a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy's National Nuclear Security Administration (DOE/NNSA) under contract DE-NA0003525. This written work is authored by an employee of NTESS. The employee, not NTESS, owns the right, title and interest in and to the written work and is responsible for its contents. This work was authored in part by the National Renewable Energy Laboratory, operated by Alliance for Sustainable Energy, LLC, for the U.S. Department of Energy (DOE) under Contract No. DE-AC36-08GO28308. Any subjective views or opinions that might be expressed in the written work do not necessarily represent the views of the U.S. Government.

applied pressure↗

DOE OSTI2020

Numerical modeling and performance analysis of a membrane-based air dehumidifier using ionic liquid desiccant

Membrane-based Liquid Desiccant Air Dehumidifier (MLDAD) has the potential to overcome the shortcomings of the conventional open-tower liquid desiccant air dehumidifier. The MLDAD uses membranes with high water vapor permeability to separate air stream from the liquid desiccant and thus eliminates carry-over and the resulting corrosion issues. Recently, the ionic liquid desiccant becomes a promising alternative to conventional liquid desiccant. The ionic liquid desiccant has a large potential of dehumidification, which is also non-corrosive to metals and non-crystallizable. A two-dimensional numerical heat and mass transfer model of the MLDAD using a recently identified ionic liquid desiccant, [EMIM]OAc, is presented in this paper. We report this model can simulate the performance of the MLDAD with various designs, including different selections of liquid desiccant and membrane materials, dimensions of the MLDAD, and flow patterns. For porous membranes, this model accounts for several micro-scale mass transfer mechanisms of vapor transportation across the membrane. It can also model the mass transfer performance of dehumidifiers using non-porous membranes based on the experimentally measured membrane permeance. The numerical model was validated against the performance data available from literature and experimental tests. The maximum discrepancy of the latent effectiveness between the measured and the model-predicted results was about 6% when porous membranes were used. A parametric study was conducted with the numerical model. The results indicated that the membrane permeability, air path height, and solution to air mass ratio were the most critical parameters, determining the dehumidification performance of the MLDAD.

42 ENGINEERING↗

DOE OSTI2025

New class of tritium breeders for fusion applications: Metal-reinforced composite breeders

Commercial fusion reactors operating on a D-T fuel cycle will require a steady supply of tritium to maintain the burning plasma required for continuous power generation. Since tritium has a short half-life, there is negligible natural abundance which necessitates fusion reactors to produce their own source of tritium. Tritium is most easily produced by surrounding a fusion reactor core with lithium (Li), which reacts under the intense neutron flux leaving the reactor core to form tritium and helium. Due to the hazards and technical challenges associated with surrounding a fusion reactor core with many tons of molten Li, other Li-bearing tritium breeder materials have been pursued. Unfortunately, most of the liquid breeders historically examined are exceedingly corrosive to reactor structural materials while many solid breeders in the form of ceramics are forced to make tradeoffs between Li content and mechanical integrity. In this work, to break the historic limit between Li-density and mechanical integrity of traditional solid breeders, a new class of solid tritium breeders is developed: metal-reinforced composite (MERC) breeders. Specifically, the high Li-density of lithium oxide (Li 2 O) is exploited through the addition of a metal reinforcing phase, producing a composite breeder material exhibiting high splitting tensile strength and quasi-ductility with a Li-density greater than other leading solid breeder candidates, including lithium orthosilicate (Li 4 SiO 4 ) and lithium metatitanate (Li 2 TiO 3 ). Mechanical testing, microstructural characterization, and neutronic simulation results are presented and discussed in light of fusion reactor design considerations.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Characterization of Fe and Cr Dissolution and Reaction Product Formation in Molten Chloride Salts With and Without Impurities

There is considerable interest in molten chloride salts for several applications including thermal storage and next-generation molten salt reactors (MSRs). Several studies have concluded that Cl salts are highly corrosive to structural materials. Using Oak Ridge National Laboratory’s established methodology, Cl salt compatibility was assessed for candidate Ni-based alloys 230, 600 and 740 H at 600°–800°C in static welded capsules and in flowing thermal convection loop (TCL) salt experiments. Simply drying commercial Cl salt at 550°–650°C and adding~0.05 wt.%Mg was able to produce small specimen mass changes and limited surface attack after 100–1000 h exposures. Intentional additions of H 2 O, NiCl 2 and undried salt were used to better understand the role of impurities and achieve the>50 µm levels of attack reported in other studies. Further, characterisation of Cr depletion and oxide formation in conjunction with pre- and post-test salt chemistry measurements are being used to understand salt compatibility of structural materials.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Photoluminescence in Tagging: A Glowing Review

This literature review explores the options of using photoluminescence for tagging uranium fuel and zirconium cladding in order to easily and quickly associate interdicted material to its facility of origin or pathway after loss of institutional control. Photoluminescence is the spontaneous emission of radiation by a substance when excited by interaction with light. The source of photoluminescence can be from organic, inorganic, and organometallic compounds. Each luminophore, or compound responsible for luminescent properties, has individual strengths and weaknesses, depending on the intended use. Many factors can affect the brightness, lifetime, color, and detectability of luminophores, such as humidity, temperature, oxygen availability, noise from radiation–induced luminescence, and the presence of quenching substances like iron. Application of luminescent compound to the surface of an item can be done using paint, dye, thin film, thick film, or electrochemical coating. Several of the application techniques may have secondary functions such as corrosion resistance and detection, heat resistance, protective properties, and more. When considering cladding, there are various successful studies on the application of luminescent coatings on zirconium. However, significant research will be necessary to explore which luminophore and which application technique would best fit the intended use. In order to proceed with this research, a baseline of the natural luminescence of the intended base material (nuclear fuel or cladding) is necessary. While there may be issues with background noise, quenching from the environment, quenching from the substrate, signal to noise weakness, etc. the multitude of options may make photoluminescent tagging an option. In summary, this review has demonstrated that photoluminescence is a potential option to tag nuclear fuel and cladding, but additional paper–studies, testing, and research is required to understand the compatibility of luminescent tags in nuclear reactor environments, manufacturability, and detectability.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Interfacial stabilization for inverted perovskite solar cells with long-term stability

Perovskite solar cells (PSCs) commonly exhibit significant performance degradation due to ion migration through the top charge transport layer and ultimately metal electrode corrosion. Here, we demonstrate an interfacial management strategy using a boron chloride subphthalocyanine (Cl 6 SubPc)/fullerene electron-transport layer, which not only passivates the interfacial defects in the perovskite, but also suppresses halide diffusion as evidenced by multiple techniques, including visual element mapping by electron energy loss spectroscopy. As a result, we obtain inverted PSCs with an efficiency of 22.0% (21.3% certified), shelf life of 7000 h, Τ 80 of 816 h under damp heat stress (compared to less than 20 h without Cl 6 SubPc), and initial performance retention of 98% after 2000 h at 80 °C in inert environment, 90% after 2034 h of illumination and maximum power point tracking in ambient for encapsulated devices and 95% after 1272 h outdoor testing ISOS-O-1. Our strategy and results pave a new way to move PSCs forward to their potential commercialization solidly.

14 SOLAR ENERGY↗

DOE OSTI2021

Assessing subtle variations in the actinyl oxo reactivity through characterization of neptunyl complexes. Final Report

Formation of the actinyl cation, [An(V,VI)O 2 ] n+ (n = 1,2), imparts unique chemical properties to the lighter actinide elements (U, Np, and Pu) that has yet to be fully understood. The axial O atoms (oxo) of the [An(VI)O 2 ] 2+ are considered weak Lewis bases that exhibit only meager interact with other metal cations and regarded as poor hydrogen acceptors for nearby water molecules. Oxo atoms of [An(V)O 2 ] + should engage in stronger bonding interactions due to a higher degree of Lewis basicity, but the actual interactions have yet to be fully explored. Intermolecular interactions can impact radionuclide separations, corrosion of spent fuel, and mobility of actinides in environmental systems; there is, therefore, a critical need to understand how the subtle difference in electronic properties of the An(V) and An(VI) metal center influence actinyl chemistry. The objective of this proposal was to determine the chemical components that influence the intermolecular interactions occurring between neptunyl ([Np(V)O 2 ] + and [Np(VI)O 2 ] 2+ ) cations and neighboring species. My overall hypothesis was that the intermolecular attraction that occurs between the neptunyl oxo atoms and neighboring species (H atoms, low-valent cations, actinyl cations) is primarily controlled by the electronic properties of the actinyl cation, but can be further influenced by the electron donating properties of the equatorial ligands. The hypothesis was tested through the following research objectives: (1) Determine the fundamental differences in H-bonding between Np(V)O 2+ and Np(VI)O 2 2+ and neighboring donor molecules; (2) Identify the major differences in bonding between low-valence metal cations and neptunyl oxo groups, and (3) Assess the impact of the equatorial ligand on the formation of cation-cation interactions within molecular species. Major outcomes of the research include: (1) More precisely identifying oxo interactions (actinyl-cation; actinyl-actinyl, actinyl-hydrogen) and the factors that impact the vibrational modes for actinyl cation; (2) Identification of H-bonding modes for the [An(V,VI)O 2 ] n+ (n = 1,2), with direct H-bonding interactions to the oxo group of the Np(V)O 2+ cation more prevalent than in hexavalent species and recognition of the importance of H-bonding networks, that can impart bond asymmetry and activation of vibrational modes with the actinyl moiety; (3) Delineation of the importance of charge density for engaging the cation-oxo interaction for both pentavalent and hexavalent species; (4) Determining the importance of sterics and ligand binding in formation of specific actinyl-actinyl interactions and the resulting vibrational modes associated with this bonding motify and (5) Understanding how the functionalization of the ligand can impact redox stability of neptunyl cations. Deliverables from this work include 11 peer-reviewed manuscripts and 13 (including six by graduate students) oral/poster presentations.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Rapid Bayesian High Entropy Alloy Designs Fabricated via Wire Arc Additive Manufacturing

Purpose: This project seeks to demonstrate a new high-throughput (rapid) alloy design technique applied to creating new high entropy alloys (HEAs) for extreme environments. High entropy alloys shift the design paradigm from being focused on a single principal element (e.g. nickel-based alloys) to target alloys that include high atomic fractions (X >10%) of multiple elements. These HEA materials can exhibit sluggish diffusion and enhanced corrosion resistance, ideal for potential applications in advanced ultra supercritical (A-USC) steam cycles for power generation. Scope: The addition of multiple elements in high atomic fractions creates an enormous design space that cannot easily be investigated by traditional material design strategies such as designed of experiments (DOE). This project utilizes a Bayesian machine learning algorithm that has been modified to work with calculation of phase diagrams (CALPHAD) software. This Bayesian algorithm reduces manual inputs and increase the likelihood of achieving an optimal solution. Compositional inputs to this algorithm will be assessed using existing material property models for high temperature strength and corrosion resistance. The target for alloy performance will be a 15% (~100 ⁰C) increase in allowable service temperature beyond heat-resistant stainless steels while maintaining or improving alloy cost and corrosion resistance. Haynes 230 was selected as a baseline, which is 57 wt% Ni with 22 wt% Cr 14 wt% W, and 2 wt% Mo as solid solution strengtheners. In addition to rapid design via Bayesian machine learning, the alloys were rapidly fabricated using a multi-wire arc additive manufacturing (mWAAM) technique which allows for precise control of alloy composition and assessing of alloy design “windows” to study composition effects. Build speeds for wire-arc additive processes are among the highest for additive technologies enabling rapid and reliable sample fabrication when compared to conventional methods such as arc button melting. The mWAAM samples will be rapidly characterized via instrumented indentation for room temperature modulus and strength and for elevated temperature strength via hot hardness tests. After being screened with hardness testing, potential alloys will be further evaluated with conventional microscopy techniques including scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to assess agreement with modeling results. The most promising compositions will also be evaluated by printing full sized tensile specimens for mechanical behavior tests at elevated temperatures. Results: Bayesian machine learning of a single performance function was initially used to optimize five performance metrics: 1) single phase stability, 2) yield strength, 3) creep resistance (low diffusion coefficient), 4) freezing range (weldability), and 5) material cost. The single performance function was suboptimal as assumptions had to be made about the results while formulating the optimization. A goal-oriented Bayesian optimization strategy (Hanaoka, 2021) was implemented with CALPHAD for use with the five metrics above. This multi-objective Bayesian optimization (MOBO) enabled the design of NiCrCoFe alloys with V and W additions. A base composition of NiCoCr was selected as Ni provides a stable FCC matrix, Cr aids corrosion/oxidation resistance, and Co is a solid-solutions strengthener that also improves creep by increasing the activation energy. Fe helps reduce diffusion coefficients and cost. Finally, V and W were selected for their reasonable solubility and high atomic misfit to aid in solid solution strengthening. Cracking of the mWAAM specimens was an early issue, and the Easton solidification cracking model (Easton et al., 2014a) was selected for addition to the MOBO function. High performing alloys fabricated by mWAAM included Ni 28 Cr 25 Co 26 Fe 15 V 8 and Ni 62 Cr 18 Co 1 Fe 3 W 15 . It was observed that even after adapting the mWAAM process for W, the W did not fully dissolve. To fully evaluate the Ni 62 Cr 18 Co 1 Fe 3 W 15 composition, a cored wire (80-20 NiCr sheath/powder core) was manufactured and printed via WAAM, and HIP’ing was utilized to homogenize and densify the printed alloy. The V and W alloys produced met metrics 1 (solid solution), 4 (solidification cracking), and 5 (cost). However, an unmodeled mechanism of thermal stress cracking was identified in the WAAM produced materials, perhaps exacerbated by the lack of grain boundary strengthening elements (B, C). Conclusions & Recommendations: A high-throughput (rapid) alloy design technique was applied to designing and manufacturing new high entropy alloys (HEAs) for extreme environments utilizing MOBO and mWAAM. The developed process was rapid and effective in addressing the mechanisms included in the model. The lack of grain boundary strengthening element additions (e.g., B, C) was a simplification that likely produced thermal stress cracking that turned into a large part of the investigation. Additions on the order of 0.005 wt% B and 0.05 wt% C likely would have minimized thermal stress grain boundary cracking. Overall, the high throughput design strategy is promising for rapid design of metrics-driven alloys for advanced ultra supercritical (A-USC) steam cycles for power generation. The MOBO and mWAAM process could be commercialized to accelerate metrics-driven alloy design. In addition, the cored-wire process utilized for scale-up is a promising high-volume process for WAAM alloy development and scale-up.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Experimental Evaluation of Deformation and Fracture Mechanisms in Highly Irradiated Austenitic Steels

The present report documents recent experimental results of analysis using scanning electron microscopy/electron backscatter diffraction (SEM-EBSD) of plastic deformation mechanisms and strain localization phenomena in austenitic steels irradiated by neutrons. Experiments were performed with specimens irradiated to 125 dpa and, additionally, with specimens that experienced radiation-induced swelling up to 3%. Section 1 briefly analyzes the deformation localization in irradiated steels and its consequences on the material performance. The section describes the advantages and importance of the SEM-EBSD approach combined with in situ mechanical testing capability. Section 2 briefly introduces the experimental tools and methods (i.e., SEM/EBSD in situ tensile frame, electric discharge machine to manufacture irradiated specimens) and describes the investigated materials (i.e., element composition, irradiation conditions, and general microstructure). Section 3 describes the key experimental results and provides a brief analysis and comparison with the datasets obtained earlier within the same task (i.e., low-dose specimens). The discussion focuses on EBSD microstructure maps with strain localization features, misorientation evolution as a function of strain, and observed deformation mechanisms. Section 4 evaluates data collected in recent years on highly irradiated steel and estimates the possible misorientation evolution under irradiation. The section introduces and discusses the concept of in-service-induced damage as an irradiation-assisted stress-corrosion cracking precursor. Section 5 summarizes the work performed. As expected, the present work results are beneficial for exploring and understanding degradation mechanisms in highly irradiated in-core materials found in light water reactors after long-term in-service life.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Monitoring of Photovoltaic (PV) Performance and Degradation: Integrated Renewable Energy Systems (IRES) - PV Monitoring Task

The Integrated Renewable Energy System (IRES) testbed demonstration at the Pacific Northwest National Laboratory (PNNL) Sequim campus includes development of a suite of capabilities for tracking the performance of photovoltaic (PV) renewable energy components located on a floating platform (floating PV) and on a shoreline building rooftop. The marine environment represents potentially harsh and corrosive conditions for PV modules. Compared to terrestrial PV, potential concerns for offshore PV arising from high humidity and occasional contact with saltwater, marine wildlife, and aquaculture. These environmental factors can reduce electricity generation efficiency and increase the risk of electrical faults, polymer insulation or jacketing degradation and hydrolysis of the PV cell encapsulant materials. Offshore PV modules may also be exposed to lower temperatures and buoyant and vibrating motions with a floating platform. It is not clear how the long-term performance of floating PV will be affected by these factors. To understand expected energy generation through solar cells on a floating platform, monitoring of the performance of PV modules in the marine environment is needed. This report outlines a plan for long-term testing of IRES PV components utilizing resources of the PNNL Material Aging and Detection (MAaD) Science team and the Marine and Coastal Research Laboratory (MCRL). Equipment applicable for onsite testing and real-time monitoring of the PV performance associated with environmental conditions including temperature, solar irradiance, shading and soiling is included. In case of performance loss, equipment for fault detection, failure analysis, material testing, and further troubleshooting are also available. Through establishment of this capabilities, the enabling IRES project sets the stage for future research to advance off-shore and near-shore energy options for businesses and communities.

14 SOLAR ENERGY↗

DOE OSTI2022

System Integration of Rationally Designed Dilute Alloy Catalysts for Energy-Efficient Electrochemical CO 2 -To-Fuel Conversion

Energy effiecient electrochemical conversion of CO 2 to high-demand chemicals and transportation fuels using renewable solar and wind energy is a key technology needed for a high-productivity, low-carbon future. However, the development of scalable, low-cost, active, selective, and stable electrocatalysts remains a key challenge that needs to be overcome to enable high-volume conversion of CO 2 to feedstock chemicals for the chemical industry. In previous work, Lawrence Livermore National Laboratory (LLNL) has developed a rational design platform for dilute alloy transition metal electrocatalysts that promise to make electrochemical CO 2 conversion more energy efficient and selective. In this project, we worked with our industrial partners, Twelve and TotalEnergies, to improve scale up, integration, and stability of LLNL’s dilute alloy catalyst technology into an industry-relevant zero gap electrolyzer platform. Through virtual experiments and data analysis, we designed efficient and cost-effective copper-based catalysts. The catalyst was specifically designed to streamline the slowest and most energy-intensive step of the electrochemical chemical transformation of CO 2 to multi-carbon products – that is making the carbon-carbon bond by dimerization of the reaction intermediate carbon monoxide - resulting in up to 10% improvement in energy efficiency for C 2 products while simultaneously increasing the selectivity towards C 2 products. We tested two different scalable catalyst coating technologies and down-selected magnetron sputtering as the technique that provided the best control over catalyst loading, composition, and morphology. Using this technology, we successfully demonstrated integration of our dilute alloy catalysts into a 100 cm 2 electrolyzer platform with Faradaic efficiencies for ethylene production reaching 40% at a current density of 200 mA/cm 2 . We also developed the technology to integrate a well-defined nanoscale porosity by depositing alloy compositions that were compatible with dealloying, that is, selective leaching of an alloy component to generate nanoscale porosity. We observed that integration of the dealloying-derived nanoporosity improved catalyst performance and stability by leading to a more hydrophobic catalyst/anion exchange membrane interface. Unsolved problems that still need to be addressed are corrosion of the Cu catalyst -specifically if the used catalyst is exposed to air - as well as long term stability do to salt formation/deposition and flooding of the catalyst/electrolyzer flow channels, especially at higher current densities. As we only worked on optimization of catalyst composition, coating thickness, and morphology, further performance optimization will require a system level approach that includes optimization of electrolyzer design and membrane technology.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Direct Feed High-Level Waste APPS Model Glass Testing (DFHLW APPS) Matrix, Phase 2

This report summarizes the data collected during the batching and melting of a second matrix of Direct Feed High-Level Waste (DFHLW) glasses generated using the preliminary enhanced waste glass models (EWG2.5) and the Britton and Anderson (2024) preliminary DFHLW feed vector. The purpose of these glasses is two-fold: 1. Validate EWG2.5 glass calculations being used in the Aspen Process Performance Simulation (APPS) model. 2. Evaluate and ultimately improve the glass property models and formulation methods used for design of DFHLW glasses as part of an iterative process of data collection and model refinement. Some of the 16 APPS2 glasses tested did not satisfy all target property constraints due to the limited data on DFHLW glass supporting the EWG2.5 models. • One glass, APPS2-10, formed nepheline on canister centerline cooling (CCC) heat-treatment and failed the product consistency test (PCT) response limits. This glass also had high B and Cr release rates for the toxicity characteristic leaching procedure (TCLP). All other glasses were found to satisfy the PCT and TCLP constraints for both quenched and CCC samples. • One glass, APPS2-08, had higher than acceptable viscosity due to magnetite crystallization. • One glass, APPS2-09, formed greater than 2 vol% crystals at 950 °C. As the glass design criterion was that the temperature at 2 vol% crystal (T 2% ) be less than 950 °C, only one glass failed the criteria. However, this criterion is being reevaluated. Four additional glasses formed crystal fractions between 1 and 2 vol% at 950 °C (APPS2-03, -08, -12, and -14). • Four glasses – APPS2-01, -02, -04, and -16 – failed the Monofrax K-3 refractory neck corrosion (k neck ) design limit of 0.04 in. at 1208 °C for 6 d. This is another criterion being reevaluated. Four additional glasses (APPS2-05, -06, -11, and -13) exhibited 0.025 = k neck = 0.04 in. • All 16 glasses passed the sulfur solubility and TCLP constraints. The measured property values were compared to predicted values using EWG2.5 and a selection of other existing models. A few models (e.g., electrical conductivity, TCLP) were found to be adequate for designing DFHLW glasses in the near future, while others require refits or offsets. It is recommended that new property models be developed for EWG3.0, as a large amount of DFHLW glass property data (> 14 × existing data) is expected to be collected in the compositional spaces where no data was previously available. To enable near-term calculations and formulations for designing DFHLW glasses and processing rate estimations, a formulation algorithm with minor modifications will be developed, EWG2.6.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Observed volatilization behavior of silicon carbide in flowing hydrogen above 2000 K

In this work, the intrinsic compatibility of silicon carbide (SiC) and hydrogen (H 2 ) at high temperatures (2000-2473 K) and pressure near one atmosphere was evaluated through a combination of thermodynamic calculations and hot hydrogen exposure testing. Thermodynamic calculations predict the decomposition of SiC in a hydrogen environment to form free silicon (Si) and free carbon (C). Free Si is predicted to vaporize from the surface as a volatile species, while free C may interact with H 2 to form the hydrocarbons CH 4 (T < 2100 K) or C 2 H 2 (T > 2100 K). Coupons of high purity chemical vapor deposition (CVD) β-SiC were exposed to slowly flowing hydrogen at temperatures ranging between 2000 and 2473 K. SiC experienced active attack as the result of H 2 exposure, exhibiting linear weight loss kinetics and an Arrhenius dependence of weight loss on exposure temperature. The linear volatilization constant was experimentally evaluated to correspond with an activation energy of 370 ± 18 kJ/mol. Due to the dependence of observed corrosion rates on gas velocity, corrosion of SiC in flowing H 2 was determined to be governed by external mass transfer of volatile Si species through the boundary layer. Experimentally derived mass losses were in good agreement with mass losses predicted by a boundary layer limited gas diffusion model.

36 MATERIALS SCIENCE↗

DOE OSTI2021

High-Temperature Compatibility of Structural Alloys with Supercritical and Subcritical CO 2

In searching for new working fluids for power generation, supercritical CO 2 (sCO 2 ) offers some attractive features for efficient cycles. However, compatibility with structural alloys is a concern. NiCr-based alloys have excellent compatibility at 600°-800°C at 20-30 MPa sCO 2 . However, conventional steels have restrictions in temperature because of carburization and accelerated oxidation in sCO 2 , similar to observations in CO 2 . To assess the impact of carburization on steel mechanical properties, small (25mm long) dogbone tensile bars are being exposed and tested after exposure at 450°-650°C. Only highly alloyed advanced austenitic steels are resistant to carburization at 650°-750°C, suggesting that Crrich oxide scales are good barriers to C ingress. Above 800°C, it is only possible to conduct subcritical evaluations at this time, but initial results suggest most conventional high-temperature Fe- and Ni-based alloys are more rapidly degraded by CO 2 at higher temperatures. Coatings are a potential solution that require more study.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Bounding Pressure and Flammability Evaluations of Aluminum-Clad Spent Nuclear Fuel Department of Energy Standard Canisters

This paper presents bounding pressure and flammability evaluations for DOE Standard Canister loaded with DOE-managed aluminum-clad spent nuclear fuel (ASNF). The objective of these evaluations is to gain confidence in the safety and feasibility of possible loading configurations for extended (>50 years) periods of dry storage, with particular focus on the dry storage canister pressures and potential for formation of a flammable atmosphere. The primary concern about the extended dry storage of ASNF is radiolytic gas generation. The aluminum cladding of these materials tends to corrode, and these corrosion products—typically aluminum oxides, such as boehmite, bayerite, or gibbsite—could carry water. This makes ASNF dry storage canisters difficult to dry. The gamma radiation field in dry storage environments could cause a radiolytic breakdown of residual water, forming chemical species such as molecular hydrogen (H2). The release of these species could increase the canister pressure and lead to the generation of a flammable canister atmosphere. The bounding evaluations presented within this study surmise conservative, but credible, conditions and processes. This includes the assumption of a full breakdown of a large quantity of free, physisorbed, and chemisorbed water (bound in a trihydrate, i.e., Al2O3 • 3H2O, layer). The considered dry storage configurations include a ~3 m (10 ft) long, ~46 cm (18 in) diameter (10 x 18) DOE Standard Canister loaded with 32 Advanced Test Reactor (ATR) ASNF elements, and a ~3 m (10 ft) long, ~61 cm (24 in) (10 x 24) diameter DOE Standard Canister loaded with 40 ATR ASNF elements. While the results of this study indicate the possibility of atmospheric hydrogen concentrations above the lower flammability limit, insufficient concentrations of oxygen will prevent the formation of flammable atmospheres. The maximum credible pressures remain well within the structural limits of the DOE Standard Canister.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Welded and Hydrogen Charged Zircaloy-4 and Welded Stainless Steel 347 Property Data and Microstructures for the Target Solution Vessel and Support Lines of SHINE

SHINE Medical Technologies is developing a facility that will produce molybdenum-99 for medical isotope procedures. As part of this facility, a metal tank, called the target solution vessel (TSV), will hold a uranyl sulfite solution. The TSV must withstand neutron irradiation near room temperature and potential corrosion from the aqueous solution. The large cylindrical TSV will be fabricated by welding and will have numerous pipes and connections also attached via welding. The vessel and those pipes will have varying thicknesses so both gas tungsten arc welding (GTAW) and flux-cored arc welding (FCAW) will be necessary to fabricate different sections. The original material under consideration for the TSV was Zircaloy-4 (Zry-4), but it is known to form a hydride which can degrade its mechanical properties. Thus, some investigation here is focused on the effects of hydrogen uptake in the Zry-4. Additionally, the alternative material being considered is AISI 347, a stainless steel. Both materials have little existing data for their neutron irradiation behavior below 100°C, and both have open questions on the weld behavior under neutron irradiation. Testing has focused on characterizing their weld properties with tensile tests and performing neutron irradiation of samples in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL).

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2021

Rheological investigation of effect of high temperature on geothermal drilling fluids additives and lost circulation materials

High temperatures (HT) and the corrosive environment make the design of a geothermal drilling fluid a highly complex task. The presence of HT exacerbates the problems due to thermal degradation. Geothermal aquifers usually combine high-temperature and complex chemistry, making them highly corrosive. Although geothermal drilling fluids are exposed to thermal degradation, research of the effect on mud rheological properties in temperatures near or above 149°C (300°F) is limited. In this study, a High Pressure-High Temperature (HPHT) rheology setup was used to measure drilling fluids' properties up to 204.4°C (400°F). Rheological behavior of viscosity, density, lost circulation, and alkalinity control additives were analyzed at HT. It was found experimentally that Bentonite alone is thermally stable at HT. In contrast, Caustic Soda showed a tendency to gelate at temperatures above 93.3°C (200°F), adversely affecting mud rheology. Alkalinity control materials to replace Caustic Soda were evaluated. Among them, Lime presented the best thermal stability at 204.4°C with a range of variation of 0.0024 Pa.s (2.4 cP) on apparent viscosity after three consecutive tests. Besides, it was tested 11 different lost circulation materials (LCM) for understanding their rheological behavior at HT. Further, it was found that HT has less impact on fine granular materials rheological behavior with an average increase of 17.7% compared with the baseline. In contrast, flaky, fibrous, and coarse granular materials presented a more apparent impact in WBM rheology with a deviation of 166% compared with the baseline.

15 GEOTHERMAL ENERGY↗

DOE OSTI2026

Mechanical Behavior of Neutron Irradiated Refractory Multi-Principal Element Alloys Processed via Spark Plasma Sintering

The search for advanced materials capable of withstanding the extreme conditions of Generation IV reactors is a critical area in materials science research. These reactors operate under severe environments, including high temperatures, corrosion, stress, and irradiation damage. Consequently, there is a need for innovative alloy systems to ensure the reliability and longevity of proposed Generation IV reactor components. Refractory multi-principal-element alloys (RMPEA) have emerged as a promising candidate due to their exceptional properties. These alloys, characterized by their composition of multiple principal elements in near-equiatomic ratios, exhibit superior resistance to irradiation damage, reduced void swelling, enhanced microstructural stability, and minimal irradiation-induced hardening. While initial studies on RMPEAs have shown promising results, most research has been limited to thin films, nanocrystalline microstructures, and ion irradiation, which do not accurately represent the behavior of bulk materials. To address this gap, our research focused on the neutron irradiation of bulk RMPEAs. We aim to conduct comprehensive post-irradiation examinations (PIE) of RMPEAs irradiated at the Advanced Test Reactor at Idaho National Laboratory. The RMPEAs were synthesized using spark plasma sintering (SPS) with mechanically alloyed metallurgical powder. The RMPEA specimens are a MoNbTi alloy system with additions of -Zr, and -ZrV. Furthermore, PIE consisted of mechanical testing and advanced materials characterization. The mechanical testing consisted of sub-sized tensile testing, micro- and nano- indentation. Microstructural characterization included scanning electron microscopy and transmission electron microscopy. Mechanical testing coupled with advanced microscopy techniques provides insight into phase morphology and its effects on the mechanical properties of the RMPEA specimens. The results indicate that both pristine and irradiated RMPEA specimens exhibited brittle behavior during tensile testing, which can be attributed to their heterogeneous microstructure. The SPS manufacturing process did not include any post treatment, which resulted in a heterogeneous microstructure. Energy-dispersive X-ray spectroscopy revealed the presence of intermetallic such as laves phases within the microstructure. Specifically, Ti-rich precipitates were observed in the MoNbTi specimen, while Mo-rich precipitates were found in the MoNbTiZrV specimen. Nano-hardness testing of pristine samples showed that the laves phases exhibited higher hardness values compared to the matrix phase, suggesting that precipitate hardening is likely the dominant hardening mechanism in these specimens. The results from this work will be used to build a finite element model to predict mechanical behavior of future MPEA compositions. Thus, enabling for a streamlined approach to developing novel MPEAs for the nuclear industry.

36 - MATERIALS SCIENCE↗