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DOE OSTI2022

Post-irradiation Examination Status for the BSU-269 Project

High-density uranium inter-metallic uranium silicide (U 3 Si 2 ) was initially considered as a potential advanced nuclear fuel for light water reactor (LWR) systems due to several advantages it demonstrated in thermophysical properties, chemical, and irradiation stability. In addition to understanding the basic thermophysical and mechanical properties of U 3 Si 2 under LWR irradiation conditions, it is important to assess its performance with advanced claddings such as FeCrAl, SiC, or conventional Zr-based claddings. Several aspects of the fuel cycle and fuel performance are being evaluated for U 3 Si 2 coupled with different types of claddings. To thoroughly characterize the U 3 Si 2 -cladding system, their chemical compatibilities and the potential for fuel-cladding chemical interaction (FCCI) must be addressed. Interdiffusion studies have been performed between U 3 Si 2 /Zry-4 and U 3 Si 2 /FeCrAl using diffusion couples. For the U 3 Si 2 /Zry-4 system, ZrSi 2 was the primary interdiffusion product observed at 800°C in addition to other secondary phases from the Zr alloying elements such as Fe and Cr. Low melting point U 6 Fe was also observed at 1000°C. For the U 3 Si 2 /FeCrAl system, at temperatures above 500°C, chemical diffusion Fe-U and Fe-U-Si was observed, increasing with rising temperatures. Although information from these non-irradiated tests is a fundamental first assessment, follow-up with focused irradiation tests is necessary. Irradiation can significantly alter the structure and evolution of the FCCI layers compared to the non-irradiated conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

ULTIMATE Phase I project: Development of Niobium-based alloys for Turbine Applications

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer. The first class of alloys developed in this project was a Nb-alloy designed to serve as the turbine blade core with excellent room temperature strength, ductility, and high temperature strength and creep resistance required for 1300°C operation. These alloys were designed to contain sufficient solute solution strengthening elements (W, Mo) but constrained by the density of alloy, along with the addition of elements such as Zr, Hf, Ta, C, and N to achieve a combination of primary and secondary carbide precipitation. A total of 38 “creep-resistant” alloys were designed and cast during the duration of the project. Processing techniques were developed to keep the oxygen contents as low as possible with typical oxygen contents less than 250 ppm. One alloy with a density of < 9.5 g/cc was successful in meeting the Phase 2 intermediate project mechanical property milestone requirements of room temperature ductility greater than 1.0%, 1200°C creep strain of less than 3% at 150 MPa and 100 hours in vacuum, and with solidus temperature greater than 1500ᵒC. The second class of alloys was designed to be a Nb-rich alloy with improved oxidation resistance when compared to the core layer and was designed specifically to be compatible with the core layer and the outer environmental barrier coating. This Nb- alloy will be specifically designed to be microstructurally stable at these temperatures when in contact with the core alloy and provide protection against catastrophic failure of the barrier coating. Two alloys were cast and processed but further development was discontinued to focus on the development of the creep resistant alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Development of Niobium-based alloys for Turbine Applications: 20/CJ000/08/09 (ULTIMATE Phase I project)

36 MATERIALS SCIENCE↗

DOE OSTI2025

Operation of Argonne's Liquid Salt-Liquid Metal Separation Testbed for U/TRU Product Processing

Argonne National Laboratory has constructed a liquid salt-liquid metal separation testbed for use in the development and advancement of cathode processing of U/TRU co‑deposits generated by pyroprocessing of used nuclear fuel. The U/TRU product recovered from the electrorefiner contains adhered and entrained salt that must be removed prior to consolidation of the U/TRU alloy for use in advanced reactor fuel fabrication. The bottom pour operation utilizes the low melting points of U/TRU co‑deposits and higher densities of molten metals compared to molten salts to separate and consolidate the U/TRU product. Argonne’s testbed is designed to support the development and optimization of bottom-pouring configurations for batch and semi-continuous operations, integration of process monitoring and control technologies, and determination of operational requirements for implementing in an industrial setting. Scoping tests were performed to demonstrate operational aspects of the testbed, including operation using single-pour spout and dual-pour spout configurations, effectiveness of salt containment and extent of salt vaporization, and the use of sensor probes to detect the location of the interface between the metal and salt phases during pouring. Recommendations for process optimization testing for further development of bottom pour processing to separate U/TRU alloys from adhered salt were made based on the results of scoping tests. Completing the recommended activities will increase the technical readiness level (TRL) of the liquid salt-liquid metal separation operation and consolidation of U/TRU alloys to support industrialization of pyroprocessing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Designing Recyclable Biomass-Based Polyesters (Final Technical Report)

This project successfully demonstrated the production of sustainable polyesters from biomass-derived monomers, offering properties on par with or superior to fossil-based plastics such as LLDPE and PBAT. Using renewable chemical platforms like furfural and HMF, we synthesized over eight novel monomers and nearly 100 aliphatic-aromatic polyesters. Among these, PPeAT and PDDF emerged as highly promising candidates for flexible packaging applications, exhibiting excellent mechanical performance, tunable thermal properties, and enhanced barrier characteristics. Key advances included the development of ring-opening polymerization strategies using cyclic monomer intermediates to produce high molecular weight materials with excellent control. The resulting polymers achieved biobased content of at least 44 wt.%. We also implemented chemical recycling via catalytic methanolysis, recovering over 90% of monomers from PPeAT at semi-pilot scale. This supports a circular economy approach by enabling material reuse without performance loss. Techno-economic and life cycle assessments confirmed that these polyesters can reduce greenhouse gas emissions by up to 50% compared to petroleum-derived alternatives. Favorable mechanical properties may further reduce material demand, and cost competitiveness was demonstrated under specific market conditions. Feedstock cost and environmental footprint were identified as primary levers for future optimization. In summary, the project met or closely approached all technical targets, including biodegradability, strength, and processing compatibility. While minor issues such as color and melting point variation remain, the results strongly support continued development and scale-up of these sustainable materials.

09 BIOMASS FUELS↗

DOE OSTI2025

Validation of Numerical Tools for Calculating Reactivity Feedback in Sodium Fast Reactors Using SEFOR Experimental Data

The Southwest Experimental Fast Oxide Reactor (SEFOR) was an experimental sodium-cooled fast breeder reactor operated from 1969 to 1972 with experiments designed to measure Doppler reactivity feedback in a wide temperature range from around 350 °F to temperatures approaching the melting point of mixed oxide fuel of around 5000 °F, providing valuable data for code validations. Co-supported by the Department of Energy (DOE) Fast Reactor Program (FRP) and the DOE Nuclear Energy Advanced Modeling and Simulation (NEAMS) program, the SEFOR benchmark project focused on using the experimental data to validate numerical tools that are used in industry and academia to design and license sodium-cooled fast reactors (SFRs). By the end of FY-25, substantial progress was achieved in the SEFOR benchmark study. A variety of numerical tools commonly used for modeling SFRs were applied to develop models for SEFOR core configurations I-D, I-E, I-I, and I-J. These included Monte Carlo codes such as MCNP, Serpent, and Shift; deterministic codes such as the legacy Argonne Reactor Computation (ARC) suite and the high-fidelity NEAMS code Griffin; and the system analysis code SAS4A/SASSYS-1 (SAS). Using these models, both SEFOR zero-power experiments and power-ascending tests were successfully simulated. Comparisons were performed against experimental measurements of core criticalities, reflector worth, kinetics parameters (Λ/βeff), isothermal reactivity feedback (from 350 °F to 760 °F at zero power), and power-ascending reactivity feedback (as power increased from 0.4 MW to 17 MW). In general, these comparisons demonstrated very good agreement between numerical results and experimental data. In Fiscal Year 26 (FY-26), the SEFOR benchmark project will continue to address the modeling issues identified in FY-25. Effort will focus on the simulation of reactivity insertion transients in SEFOR core II using the ARC/SAS model. Future work will also focus on incorporating BISON into the SEFOR core modeling process to enable the first Multiphysics simulations of the isothermal tests based on the MOOSE framework.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2025

Advanced Materials & Manufacturing Technology (AMMT): Process understanding for qualifying LPBF 316H SS

Investigations were conducted in fiscal years (FY) 2023 and 2024 to gather relevant data sets addressing challenges related to qualifying 316H stainless steel (SS) for use in future nuclear reactors. This work was a collaborative effort involving researchers from Idaho National Laboratory (INL), Argonne National Laboratory (ANL), and Oak Ridge National Laboratory (ORNL). Key outcomes included: • Development of process-structure-property data sets to better understand the relationships between manufacturing processes, material structure, and performance characteristics. • Establishment of an in-situ monitoring system to link these various data sets together. • Detailed characterization of the raw material feedstock to further strengthen the understanding of process-structure and process-property relationships. Building on this foundation, in FY25 there was interest in exploring the behavior of additively manufactured 316H SS under different test conditions to support the overall material qualification process. Los Alamos National Laboratory (LANL) was tasked with providing specimen samples to the collaborating labs, who then conducted a round-robin study examining factors like selective heat treatment, low-cycle fatigue (LCF), and tensile-creep (T-C) properties. Additionally, high-temperature differential scanning calorimetry (DSC) was performed by LANL to better understand how the material's thermal characteristics change as it is heated up to the melting point. This provided a more comprehensive understanding of the material's behavior. The combined results from these investigations could potentially be used to support the inclusion of 316H stainless steel in Section III, Division 5 of the relevant codes and standards, allowing its use in future nuclear reactor applications.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Towards engineering the growth morphology of anisotropic bicrystals

Eutectic alloys, such as Pb-free Bi-Sn-Ag or Sn-Ag-Cu, are essential for their low melting points in solder joints but suffer from brittle intermetallic phases, reducing reliability. Traditional solder design relies on equilibrium phase diagrams, often neglecting the kinetic influence of crystalline anisotropy during solidification. This study hypothesizes that the energetics at the solid-solid-liquid trijunction dictate crystalline facet selection. Using the Al-Al 3 Ni alloy as a model, this project combines atomistic simulations and experimental methods to understand interfacial energies and develop predictive models. This approach aims to mitigate the negative effects of intermetallics, enhancing component reliability in electronic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Assessment of 180,182, 183,184,186 W Photonuclear Data

When electron beams from accelerators are stopped in thick targets made of materials with a high atomic number (or high-Z targets), they produce photons through braking radiation (commonly known as bremsstrahlung). The efficiency of photon production increases with the atomic number (Z). Tungsten is commonly chosen as a bremsstrahlung converter in both research and medical linear accelerators due to its high Z, large bremsstrahlung cross section, high melting point, and excellent thermal conductivity.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2022

Chloride Salt Purification by Reaction With Thionyl Chloride Vapors to Remove Oxygen, Oxygenated Compounds, and Hydroxides

Molten chloride salts (including MgCl 2 , KCl, NaCl, and ZnCl 2 ) are being considered for heat transfer media for renewable (solar) and nuclear power generators, as fuel carrier for nuclear reactors, and as thermal energy storage media. Impurities such as oxygen, hydroxides, moisture, and sulfur are known to negatively influence the corrosion of materials in contact with the salt (e.g., structural metals). Commercially available chloride salts come with a range of impurities. Before using the chloride salts at high temperature, it is desirable to remove the impurities to increase the performance of the salt and reduce corrosion. In this study, we tested the use of thionyl chloride vaporized into a stream of argon to react with oxygenated impurities in a mixture of MgCl 2 -KCl-NaCl, removing them as HCl and SO 2 . The reagent was bubbled through the salt when both above and below the melting point. The reaction was followed using thermocouple data from the salt and by Fourier transform infrared (FTIR) spectroscopy on the exhaust of the reactor. The reaction kinetics were followed by comparing the peaks from SO 2 product to SOCl 2 reagent in the FTIR spectra. The purity of the salt was assessed at the end of the purification process by x-ray diffraction and inductively coupled plasma analysis. Although the process was effective in removing the oxygen content of the mixture, ternary compounds were formed in the process, including KNiCl 3 and KMgCl 3 . The nickel in KNiCl 3 came from the reaction between the salt and the nickel vessel. Thus, these experiments suggest that improvements to the process must be made before using SOCl 2 vapors for the purification of chloride salts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Building Structure-Property Relationships of Cycloalkanes in Support of Their Use in Sustainable Aviation Fuels

In 2018 13.7 EJ of fuel were consumed by the global commercial aviation industry. Worldwide, demand will increase into the foreseeable future. Developing Sustainable Aviation Fuels (SAFs), with decreased CO 2 and soot emissions, will be pivotal to the on-going mitigation efforts against global warming. Minimizing aromatics in aviation fuel is desirable because of the high propensity of aromatics to produce soot during combustion. Because aromatics cause o-rings to swell, they are important for maintaining engine seals, and must be present in at least 8 vol% under ASTM-D7566. Recently, cycloalkanes have been shown to exhibit some o-ring swelling behavior, possibly making them an attractive substitute to decrease the aromatic content of aviation fuel. Cycloalkanes must meet specifications for a number of other physical properties to be compatible with jet fuel, and these properties can vary greatly with the cycloalkane chemical structure, making their selection difficult. Building a database of structure-property relationships (SPR) for cycloalkanes greatly facilitates their furthered inclusion into aviation fuels. The work presented in this paper develops SPRs by building a data set that includes physical properties important to the aviation industry. The physical properties considered are energy density, specific energy, melting point, density, flashpoint, the Hansen solubility parameter, and the yield sooting index (YSI). Further, our data set includes cycloalkanes drawn from the following structural groups: fused cycloalkanes, n-alkylcycloalkanes, branched cycloalkanes, multiple substituted cycloalkanes, and cycloalkanes with different ring sizes. In addition, a select number of cycloalkanes are blended into Jet-A fuel (POSF-10325) at 10 and 30 wt%. Comparison of neat and blended physical properties are presented. One major finding is that ring expanded systems, those with more than six carbons, have excellent potential for inclusion in SAFs. Our data also indicate that polysubstituted cycloalkanes have higher YSI values.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Thermodynamics of Liquid Uranium from Atomistic and Ab Initio Modeling

We present thermodynamic properties for liquid uranium obtained from classical molecular dynamics (MD) simulations and the first-principles theory. The coexisting phases method incorporated within MD modeling defines the melting temperature of uranium in good agreement with the experiment. The calculated melting enthalpy is in agreement with the experimental range. Classical MD simulations show that ionic contribution to the total specific heat of uranium does not depend on temperature. The density of states at the Fermi level, which is a crucial parameter in the determination of the electronic contribution to the total specific heat of liquid uranium, is calculated by ab initio all electron density functional theory (DFT) formalism applied to the atomic configurations generated by classical MD. The calculated specific heat of liquid uranium is compared with the previously calculated specific heat of solid γ-uranium at high temperatures. The liquid uranium cannot be supercooled below T sc ≈ 800 K or approximately about 645 K below the calculated melting point, although, the self-diffusion coefficient approaches zero at T D ≈ 700 K. Uranium metal can be supercooled about 1.5 times more than it can be overheated. The features of the temperature hysteresis are discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2020

A Thermal and Nanomechanical Study of Molecular Crystals as Versatile Mocks for Pentaerythritol Tetranitrate

Pentaerythritol tetranitrate (PETN) is a commonly used high explosive (HE) in detonators. Often, surrogate or “mock” materials are used in place of HE for mechanical tests, proofing out equipment, or developing new diagnostics. However, there is no commonly accepted mock for PETN. A good mock should match at least one physical property of the target material, and ideally mimic multiple thermal and mechanical properties. Here, we investigate several molecular crystals to evaluate their efficacy in mocking PETN density, melting point, elastic modulus, hardness, plastic deformation, and fracture behavior. Materials were tested with a combination of calorimetry and nanoindentation. Two materials, 2,4,6-trifluorobenzoic acid (246 TFBA) and mesoerythritol, were downselected for detailed indentation study after the initial round of screening experiments, both were found to mimic PETN mechanical behavior quite well, 246 TFBA closer to PETN in most properties (hardness, modulus, and density) than erythritol, but erythritol having advantages in relative cost and matching the onset of yield. Depending on the desired implementation of the mock, one material may be preferred over the other, but both have potential as generic mocks for PETN. Nanoindentation is demonstrated as a versatile tool to provide rapid screening of these materials’ mechanical properties.

42 ENGINEERING↗

DOE OSTI2023

Structural and Improper Ferroelectric Properties of TbInO 3 Single Crystal Grown by Laser Floating Zone

The honeycomb TbInO 3 has attracted wide research attention due to its fascinating physical properties. However, TbInO 3 single crystal was difficult to grow owing to the high melting point and serious volatilization of indium during the crystal growth. In this study, the volatilization of the indium element was effectively suppressed by controlling the growth atmosphere and pressure. The excess ratio of indium oxide was determined, and pure hexagonal TbInO 3 crystal was obtained by the laser floating zone method. Systematic studies on the crystal structure and optical and ferroelectric properties were carried out. The structure distortion resulted in the improper geometric ferroelectric revealed by single crystal diffraction and Raman spectrum measurements. The topological vortex domains and P-E hysteresis loop demonstrated the presence of ferroelectricity. TbInO 3 crystal has great potential application in vortex memory.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Synthesis and Thermal Oxidation Resistance of Boron-Rich Boron–Carbide Material

A boron-rich boron–carbide material (B4+δC) was synthesized by spark plasma sintering of a ball-milled mixture of high-purity boron powder and graphitic carbon at a pressure of 7 MPa and a temperature of 1930 °C. This high-pressure, high-temperature synthesized material was recovered and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy, Vickers hardness measurements, and thermal oxidation studies. The X-ray diffraction studies revealed a single-phase rhombohedral structure (space group R-3m) with lattice parameters in hexagonal representation as a = 5.609 ± 0.007 Å and c = 12.082 ± 0.02 Å. The experimental lattice parameters result in a value of δ = 0.55, or the composition of the synthesized compound as B4.55C. The high-resolution scans of boron binding energy reveal the existence of a B-C bond at 188.5 eV. Raman spectroscopy reveals the existence of a 386 cm−1 vibrational mode representative of C-B-B linear chain formation due to excess boron in the lattice. The measured Vickers microhardness at a load of 200 gf shows a high hardness value of 33.8 ± 2.3 GPa. Thermal gravimetric studies on B4.55C were conducted at a temperature of 1300 °C in a compressed dry air environment, and its behavior is compared to other high-temperature ceramic materials such as high-entropy transition metal boride. The high neutron absorption cross section, high melting point, high mechanical strength, and thermal oxidation resistance make this material ideal for applications in extreme environments.

36 MATERIALS SCIENCE↗

DOE OSTI2024

A First-Principles Study of the Structural and Thermo-Mechanical Properties of Tungsten-Based Plasma-Facing Materials

Tungsten (W) and tungsten alloys are being considered as leading candidates for structural and functional materials in future fusion energy devices. The most attractive properties of tungsten for the design of magnetic and inertial fusion energy reactors are its high melting point, high thermal conductivity, low sputtering yield, and low long-term disposal radioactive footprint. Despite these relevant features, there is a lack of understanding of how the structural and mechanical properties of W-based alloys are affected by the temperature in fusion power plants. In this work, we present a study on the thermo-mechanical properties of five W-based plasma-facing materials. First-principles density functional theory (DFT) calculations are combined with the quasi-harmonic approximation (QHA) theory to investigate the electronic, structural, mechanical, and thermal properties of these W-based alloys as a function of temperature. The coefficient of thermal expansion, temperature-dependent elastic constants, and several elastic parameters, including bulk and Young’s modulus, are calculated. Our work advances the understanding of the structural and thermo-mechanical behavior of W-based materials, thus providing insights into the design and selection of candidate plasma-facing materials in fusion energy devices.

42 ENGINEERING↗

DOE OSTI2025

Rapid Screening of Liquid Metal Wetting for a Materials Compatibility Library

Wetting behavior of molten metals on solid substrates is a critical phenomenon influencing numerous industrial applications, including welding, anti-corrosion coatings, and metal additive manufacturing (AM). In particular, molten metal jetting (MMJ), an emerging AM technology, requires that the molten metal remain pinned at the nozzle exit. Thus, each new metal requires a specific nozzle material to ensure consistent droplet ejection and deposition, making it important to rapidly identify the appropriate wetting combinations. However, traditional measurements of wetting angles require expensive equipment and only allow one combination of materials to be investigated at a time which can be time consuming. This work introduces a rapid screening method based on sessile droplet experiments to evaluate wetting profiles across multiple metal–substrate combinations simultaneously. This study investigates the wetting interactions of molten Al alloy (Al4008), Cu, and Sn on various ceramic and metal substrates to identify optimal material combinations for MMJ nozzle designs. Results demonstrate that Al4008 achieves wetting on ceramic substrates such as AlN, TiO 2 , and SiC, with varying mechanisms including chemical reactions and weak surface interactions. Additionally, theoretical predictions regarding miscibility gaps and melting point differences were verified for Cu and Sn on refractory metals like Mo and W. Findings from this study contribute to the establishment of a materials compatibility library, enabling the selection of wetting/non-wetting combinations for stable MMJ operation. This resource not only advances MMJ technologies but also provides valuable insights for broader applications such as welding, coating, and printed electronics.

Materials science↗

DOE OSTI2021

Microwave-Assisted Preparation of Luminescent Inorganic Materials: A Fast Route to Light Conversion and Storage Phosphors

Luminescent inorganic materials are used in several technological applications such as light-emitting displays, white LEDs for illumination, bioimaging, and photodynamic therapy. Usually, inorganic phosphors (e.g., complex oxides, silicates) need high temperatures and, in some cases, specific atmospheres to be formed or to obtain a homogeneous composition. Low ionic diffusion and high melting points of the precursors lead to long processing times in these solid-state syntheses with a cost in energy consumption when conventional heating methods are applied. Microwave-assisted synthesis relies on selective, volumetric heating attributed to the electromagnetic radiation interaction with the matter. The microwave heating allows for rapid heating rates and small temperature gradients yielding homogeneous, well-formed materials swiftly. Luminescent inorganic materials can benefit significantly from the microwave-assisted synthesis for high homogeneity, diverse morphology, and rapid screening of different compositions. The rapid screening allows for fast material investigation, whereas the benefits of enhanced homogeneity include improvement in the optical properties such as quantum yields and storage capacity.

59 BASIC BIOLOGICAL SCIENCES↗