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DOE OSTI2021

Intentional Uranium Tagging for Material Provenance and Pathway Forensics (LA19-Intentional-Forensics-NDD3Bb) (Annual Report for FY21)

This report describes the outcomes of the third and final year of a project to research the feasibility of tagging uranium materials, especially nuclear fuels. The experimental focus remained on metallic uranium forms under prospective surface and bulk tagging scenarios. Overall, the results showed that the tags could be successfully imparted and characterized in both as-built and degraded conditions. This was in line with expectations coming into this project, indicating promise for both surface and bulk tagging of metallic forms of uranium. Multiple surface tagging techniques and detection strategies were explored in FY21, with an emphasis on improving tag quality, readability, and detection in the field. Non-radioactive materials were used as a testbed. Selective deposition via laser beam was determined to be successful in imparting a readable titanium deposit on a stainless steel base plate, and can be read with high resolution characterization techniques (e.g., scanning electron microscopy) and field capable tools (e.g., eddy current testing). Other deposition techniques, such as selective deposition via electron beam and photoluminescent tags, were explored in FY21, and while success for these techniques would be dependent on additional work, these techniques showed potential for surface tagging applications. To survey bulk taggant elements for bulk uranium metal, 16 tagging elements were spread among 18 depleted uranium castings (4 baseline, 3 mix, 1 dilution, and 10 recycle). Most of these were made and characterized in FY21. Taggant acceptability was based upon manufacturability, detectability, and persistence from the standpoint of two detection options: bulk chemical analysis (for “chemical taggants”) and microstructural analysis (for “second phase taggants”). Taggant detection in both up-front manufacturing and in the face of “degradations” such as dilution, mixing, and recycling was generally good. Two independent laboratories carried out chemical analysis on most of the castings, and often at several locations within a casting, and the results are discussed. Scanning electron microscopy+EDS microanalysis revealed the second phases mostly contained the expected tagging elements. The shapes and 2 spatial distributions of these micron-sized carbides, oxides, and intermetallic particles offers opportunities for further science-based investigation and tagging optimization. Overall, V and Co currently appear as the best choices for chemical taggants while Al, Ti, Mn, Co, Pd, and Tb all look good as second phase taggants. The other elements considered here – Sc, Ni, Ge, Nb, Ce, Ta, W, Ir, and Au – while not being ruled out, require more study to become viable options. It is of special note that in the recycling study only one of the 12 elements fell out of detection even after 10 meltings, demonstrating their persistence. An Appendix tabulates all chemical analysis results to enable more quantitative and statistical studies of detection opportunities and limitations, as a part of a related project.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Plutonium Signatures in Molten-Salt Reactor Off-Gas Tank and Safeguards Considerations

Fluid-fueled molten-salt reactors (MSRs) are actively being developed by several companies, with plans to deploy them internationally. The current IAEA inspection tools are largely incompatible with the unique design features of liquid fuel MSRs (e.g., the complex fuel chemistry, circulating fuel inventory, bulk accountancy, and high radiation environment). For these reasons, safeguards for MSRs are seen as challenging and require the development of new techniques. This paper proposes one such technique through the observation of the reactor’s off-gas. Any reactor design using low-enriched uranium will build up plutonium as the fuel undergoes burnup. Plutonium has different fission product yields than uranium. Therefore, a shift in fission product production is expected with fuel evolution. The passive removal of certain gaseous fission products to the off-gas tank of an MSR provides a valuable opportunity for analysis without significant modifications to the design of the system. Uniquely, due to the gaseous nature of the isotopes, beta particle emissions are available for observation. The ratios of these fission product isotopes can, thus, be traced back to the relative amount and types of fissile isotopes in the core. This proposed technique represents an effective safeguards tool for bulk accountancy which, while avoiding being onerous, could be used in concert with other techniques to meet the IAEA’s timeliness goals for the detection of a diversion.

Dunkle, Nicholas (ORCID:000000027323011X)↗

DOE OSTI2026

Co-sputter deposition of Nb₃Sn layer into SRF cavity using Nb-Sn composite target

Nb₃Sn, with its superior superconducting critical temperature (Tc ~18.3 K) and superheating field (Hsh ~400 mT), is considered a promising material for superconducting radiofrequency (SRF) cavities, offering enhanced cryogenic performance compared to bulk niobium cavities. A Nb₃Sn coating technique has been developed for Nb SRF cavities using co-sputtering of Nb-Sn composite target in a DC cylindrical magnetron sputtering system. The composite target configuration and discharge conditions for co-sputtering were optimized to deposit Nb-Sn films on flat Nb substrates, followed by annealing to form Nb₃Sn. Multiple strategies have been explored to improve the surface homogeneity of the Nb₃Sn coating, including optimizing a two-step annealing process, annealing in Sn vapor, and a light Sn recoating process. A 1.5 µm Nb-Sn co-sputtered film was deposited on the interior of a 2.6 GHz Nb SRF cavity and annealed at 600 °C for 6 h, followed by 950 °C for 1 h. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, confirming the formation of Nb₃Sn. Then, the annealed cavity underwent a light recoating treatment and attained a quality factor (Q0) of 8.5E+08 at 2.0 K.

Accelerator Physics↗

DOE OSTI2021

The dynamic evolution of swelling in nickel concentrated solid solution alloys through in situ property monitoring

Defects and microstructural features spanning the atomic level to the microscale play deterministic roles in the expressed properties of materials. Yet studies of material evolution in response to environmental stimuli most often correlate resulting performance with one dominant microstructural feature only. In this work, the dynamic evolution of swelling in a series of Ni-based concentrated solid solution alloys under high-temperature irradiation exposure is observed using continuous, in situ measurements of thermoelastic properties in bulk specimens. Unlike traditional evaluation techniques which account only for volumetric porosity identified using electron microscopy, direct property evaluation provides an integrated response across all defect length scales. In particular, the evolution in elastic properties during swelling is found to depend significantly on the entire size spectrum of defects, from the nano- to meso-scales, some of which are not resolvable in imaging. Observed changes in thermal transport properties depend sensitively on the partitioning of electronic and lattice thermal conductivity. This emerging class of in situ experiments, which directly measure integrated performance in relevant conditions, provides unique insight into material dynamics otherwise unavailable using traditional methods.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Nanoporous Titanium (Oxy)nitride Films as Broadband Solar Absorbers

Broadband absorption of solar light is a key aspect in many applications that involve an efficient conversion of solar energy to heat. Titanium nitride (TiN)-based materials, in the form of periodic arrays of nanostructures or multilayers, can promote significant heat generation upon illumination thanks to their efficient light absorption and refractory character. In this work, pulsed laser deposition was chosen as a synthesis technique to shift metallic bulk-like TiN to nanoparticle-assembled hierarchical oxynitride (TiO x N y ) films by increasing the background gas deposition pressure. The nanoporous hierarchical films exhibit a tree-like morphology, a strong broadband solar absorption (~90% from the UV to the near-infrared range), and could generate temperatures of ~475 °C under moderate light concentration (17 Suns). The high heat generation achieved by treelike films is ascribed to their porous morphology, nanocrystalline structure, and oxynitride composition, which overall contribute to a superior light trapping and dissipation to heat. These properties pave the way for the implementation of such films as solar absorber structures.

14 SOLAR ENERGY↗

DOE OSTI2026

From closed shells to open shells: Coupled-cluster calculations of atomic nuclei

Coupled-cluster theory is a powerful tool for first-principles calculations of atomic nuclei, enabling accurate predictions of nuclear observables across the Segrè chart. While coupled-cluster computations are especially efficient at shell closures, extensions have been developed to tackle open-shell nuclei, by exploiting the equation-of-motion method or by expanding the coupled-cluster wave function on top of a symmetry-breaking (either deformed or superfluid) reference state. In this study, we provide a comprehensive comparison of these different formulations applied to the calcium and nickel isotopes using nuclear two-and three-body interactions from chiral effective field theory. Here, based on ground-state energies, two-neutron separation energies, and two-neutron shell gaps, different coupled-cluster computations—based on symmetry-broken reference states and equationof-motion techniques— offer consistent descriptions of bulk properties across medium-mass isotopic chains.

Marino, Francesco [Johannes Gutenberg-Universität ↗

DOE OSTI2025

Physical properties, internal structure, and the three‐dimensional petrography of CI chondrites

physical properties and the nature of their breccation, we investigated nine samples of the Ivuna and Orgueil CI chondrites ranging in size from 1 mm to 4 cm in approximate diameter. The combined mass of unique material investigated in this work is 113 g. For our investigations, we use ideal gas pycnometry, 3-D laser scanning, x-ray computed microtomography (μCT), and accompanying digital data extraction techniques. We found that the bulk density of the samples ranged from 1.61 to 2.10 g cm −3 . Larger samples tend to have a lower bulk density. Grain density (ranging from 2.44 to 2.55 g cm −3 ) is significantly less variable than the bulk density in our samples and the quantity of porosity (ranging from 14.6% to 33.8%) is the dominant factor in determining the bulk density of CI chondrite material. Our μCT results show that the visible porosity across all sizes of our CI chondrite samples is in the form of cracks, but these cracks can account for less than two-thirds of the porosity in the CI chondrites. Other porosity is not visible, even at μCT resolutions of 2.7 μm voxel edge −1 and we conclude that it is sub-micron in nature. It is not clear if the cracks seen in our samples are indigenous to the chondrites or are a result of terrestrial processes. We also find that the CI chondrites are excellent examples of the fractal-like nature of brecciation, where clasts can be observed at all scales we imaged. The breccias are composed of sub-equant-shaped and sub-rounded-textured clasts like melt-free impact breccias on other solar system bodies. From our μCT volume and digital data extraction, we determine that the Ivuna CI chondrite breccia is organized: the mostly sub-equant clasts within our ~2 cm chunk of Ivuna have a mean diameter of 1.33 mm and their aligned longest axes define a lineation structure. We speculate that the lineation was imparted after fragmentation of the clasts by slight shear on the parent asteroid which could be the result of seismic-related granular flow or mild non-axial impact-related compaction. These data will help to place returned asteroidal material from asteroids 162173 Ryugu and 101955 Bennu and the CI chondrites into a mutual geological context.

CI chondrite↗

DOE OSTI2020

Microstructural Assessment of a Multiple-Intermetallic-Strengthened Aluminum Alloy Produced from Gas-Atomized Powder by Hot Extrusion and Friction Extrusion

An aluminum (Al) matrix with various transition metal (TM) additions is an effective alloying approach for developing high-specific-strength materials for use at elevated temperatures. Conventional fabrication processes such as casting or fusion-related methods are not capable of producing Al–TM alloys in bulk form. Solid phase processing techniques, such as extrusion, have been shown to maintain the microstructure of Al–TM alloys. In this study, extrusions are fabricated from gas-atomized aluminum powders (≈100–400 µm) that contain 12.4 wt % TM additives and an Al-based matrix reinforced by various Al–Fe–Cr–Ti intermetallic compounds (IMCs). Two different extrusion techniques, conventional hot extrusion and friction extrusion, are compared using fabricating rods. During extrusion, the strengthening IMC phases were extensively refined as a result of severe plastic deformation. Furthermore, the quasicrystal approximant IMC phase (70.4 wt % Al, 20.4 wt % Fe, 8.7 wt % Cr, 0.6 wt % Ti) observed in the powder precursor is replaced by new IMC phases such as Al3.2Fe and Al45Cr7-type IMCs. The Al3Ti-type IMC phase is partially dissolved into the Al matrix during extrusion. The combination of linear and rotational shear in the friction extrusion process caused severe deformation in the powders, which allowed for a higher extrusion ratio, eliminated linear voids, and resulted in higher ductility while maintaining strength comparable to that resulting from hot extrusion. Results from equilibrium thermodynamic calculations show that the strengthening IMC phases are stable at elevated temperatures (up to ≈ 600 °C), thus enhancing the high-temperature strength of the extrudates.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Iron nitride permanent magnet and technique for forming iron nitride permanent magnet

A bulk permanent magnetic material may include between about 5 volume percent and about 40 volume percent Fe16N2 phase domains, a plurality of nonmagnetic atoms or molecules forming domain wall pinning sites, and a balance soft magnetic material, wherein at least some of the soft magnetic material is magnetically coupled to the Fe16N2 phase domains via exchange spring coupling. In some examples, a bulk permanent magnetic material may be formed by implanting N+ ions in an iron workpiece using ion implantation to form an iron nitride workpiece, pre-annealing the iron nitride workpiece to attach the iron nitride workpiece to a substrate, and post-annealing the iron nitride workpiece to form Fe16N2 phase domains within the iron nitride workpiece.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Iron nitride permanent magnet and technique for forming iron nitride permanent magnet

Wang, Jian-Ping↗

DOE OSTI2022

Ultrasonic Elastography for Nondestructive Evaluation of Dissimilar Material Joints

Dissimilar material joints or multilayered metals have become inevitable in the manufacturing industry due to the increasing demand for multifunctional materials with variable mechanical, thermal, or electrical characteristics in a single assembly. Lattice mismatch of materials at the interface of dissimilar materials leads to inferior mechanical characteristics. In particular, the mismatch in elastic properties indicated by a large initial elastic deformation is critical to determine the extent of variation in stress. However, nanoindentation, the most common and accepted technique to measure elastic modulus, is destructive, time-consuming, and can only examine mechanical properties within a limited area. A non-invasive elastographic mapping technique evaluates the mechanical properties using ultrasonic elastography to study incompressibility. The dissimilar joint between steel and copper was obtained via friction stir welding. The variation of the stress developed at the welded joint of the two different metals was evaluated from the dynamic bulk modulus map. A tensile test of the involved workpiece confirmed a good agreement with our analysis based on the dynamic bulk modulus elastographic mapping results. This study provides a rapid and non-invasive technique for the bulk metallurgic elastic modulus inspection to overcome the limitations of conventional methods.

Jin, Yuqi↗

DOE OSTI2024

Continuously tunable uniaxial strain control of van der Waals heterostructure devices

Uniaxial strain has been widely used as a powerful tool for investigating and controlling the properties of quantum materials. However, existing strain techniques have so far mostly been limited to use with bulk crystals. Although recent progress has been made in extending the application of strain to two-dimensional van der Waals (vdW) heterostructures, these techniques have been limited to optical characterization and extremely simple electrical device geometries. Here, we report a piezoelectric-based in situ uniaxial strain technique enabling simultaneous electrical transport and optical spectroscopy characterization of dual-gated vdW heterostructure devices. Critically, our technique remains compatible with vdW heterostructure devices of arbitrary complexity fabricated on conventional silicon/silicon dioxide wafer substrates. We demonstrate a large and continuously tunable strain of up to –0.15% at millikelvin temperatures, with larger strain values also likely achievable. We quantify the strain transmission from the silicon wafer to the vdW heterostructure, and further demonstrate the ability of strain to modify the electronic properties of twisted bilayer graphene. Our technique provides a highly versatile new method for exploring the effect of uniaxial strain on both the electrical and optical properties of vdW heterostructures and can be easily extended to include additional characterization techniques.

Electrical properties and parameters↗

DOE OSTI2024

Unlocking Mesoscopic Disorder in Graphitic Carbon with Spectroelectrochemistry

Intrinsic structural and oxidic defects activate graphitic carbon electrodes towards electrochemical reactions underpinning energy conversion and storage technologies. Yet, these defects can also disrupt the long-range and periodic arrangement of carbon atoms, thus, the characterization of graphitic carbon electrodes necessitates in-situ atomistic differentiation of graphitic regions from mesoscopic bulk disorder. Here, we leverage the combined techniques of in-situ attenuated total reflectance infrared spectroscopy and first-principles calculations to reveal that graphitic carbon electrodes exhibit electric-field dependent infrared activity that is sensitive to the bulk mesoscopic intrinsic disorder. With this platform, we identify graphitic regions from amorphous domains by discovering that they demonstrate opposing electric-field-dependent infrared activity under electrochemical conditions. Our work provides a roadmap for identifying mesoscopic disorder in bulk carbon materials under potential bias.

Disordered graphitic carbon electrodes↗

DOE OSTI2023

Advancing radioactive material research method: the development of a novel in situ particle-attached microfluidic electrochemical cell

This study aims to develop a microgram-scale microfluidic electrochemical cell (E-cell) for investigating the redox behavior of uranium oxide (UO 2 ). The traditional bulk electrochemical methods may require shielded facilities to investigate the hazardous materials, e.g., spent nuclear fuel, due to high radiation levels. Microfluidic E-cells offer advantages such as reduced radiation exposure, control over fluid flow rates, and high-throughput capabilities. Methods: The design of the E-cell considers electrode morphology, adhesion to a thin membrane, electrode configuration, and vacuum compatibility. Three techniques, including FIB-SEM lift-out, Au coating, and polyvinylidene fluoride (PVDF) binder, are explored for fabricating and attaching microgram quantities of UO 2 as working electrodes. The PVDF binder method proves to be the most effective, enabling the creation of a vacuum-compatible microfluidic E-cell. Results and discussion: The PVDF binder method demonstrates successful electrochemical responses and allows for real-time monitoring of UO 2 electrode behavior at the microscale. It offers chemical imaging capabilities using in situ SEM/EDS analysis. The technique provides consistent redox outcomes similar to bulk electrochemical analysis. Conclusion: The development of a microgram-scale microfluidic electrochemical cell using the PVDF binder technique enables the investigation of UO 2 redox behavior. It offers a low-risk approach with reduced radiation exposure and high-throughput capabilities. The technique provides real-time monitoring and chemical imaging capabilities, making it valuable for studying spent nuclear fuel systems and material characterization.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

An approach for the measurement of the bulk temperature of single crystal diamond using an X-ray free electron laser

We present a method to determine the bulk temperature of a single crystal diamond sample at an X-Ray free electron laser using inelastic X-ray scattering. The experiment was performed at the high energy density instrument at the European XFEL GmbH, Germany. The technique, based on inelastic X-ray scattering and the principle of detailed balance, was demonstrated to give accurate temperature measurements, within 8% for both room temperature diamond and heated diamond to 500 K. Here, the temperature was increased in a controlled way using a resistive heater to test theoretical predictions of the scaling of the signal with temperature. The method was tested by validating the energy of the phonon modes with previous measurements made at room temperature using inelastic X-ray scattering and neutron scattering techniques. This technique could be used to determine the bulk temperature in transient systems with a temporal resolution of 50 fs and for which accurate measurements of thermodynamic properties are vital to build accurate equation of state and transport models.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

An approach for the measurement of the bulk temperature of single crystal diamond using an X-ray Free Electron Laser

We present a method to determine the bulk temperature of a single crystal diamond sample at an X-Ray Free Electron Laser using inelastic X-ray scattering. The experiment was performed at the High Energy Density (HED) instrument at the European XFEL GmbH, Germany. The technique, based on inelastic X-ray scattering and the principle of detailed balance, was demonstrated to give accurate temperature measurements, within 8% for both room temperature diamond and heated diamond to 500 K. Here, the temperature was increased in a controlled way using a resistive heater to test theoretical predictions of the scaling of the signal with temperature. The method was tested by validating the energy of the phonon modes with previous measurements made at room temperature using inelastic X-ray scattering and neutron scattering techniques. This technique could be used to determine the bulk temperature in transient systems with a temporal resolution of 50 fs and for which accurate measurements of thermodynamic properties are vital to build accurate equation of state models.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Detecting missing struts in metallic micro-lattices using high speed melt pool thermal monitoring

Metal lattices are an important class of cellular materials that offer great advantages by providing high-strength and lightweight structures as compared to bulk materials. Progress in additive manufacturing techniques has led to increased complexity in design and shape of produced objects and is greatly beneficial for the development of metallic lattice structures. However additive manufacturing of lattices suffers from unpredictable defect creation that can compromise its mechanical integrity. Although post-build inspection techniques can provide quality assurance of the process, accurate assessment can be technically challenging, time consuming and costly. In this work, we investigate the use of high-speed measurements of thermal emission from the melt pool to identify defective individual struts formed with a missing bottom half in an otherwise fully built lattice structure produced with laser powder bed fusion. Surprisingly, results indicate lower photodiode signal, suggesting colder melt pool surface temperature, when printing struts with missing bottom half as compared to nominal struts. Additional thermographic imaging and multi-physics simulations reveal that the low photodiode signal is accompanied by presence of hot spatters carrying heat away from detection and continuous avalanche of powder on the melt pool. Based on these observations, a method was developed to identify defective individual struts with missing bottom half in full built lattices. This prediction approach provides valuable insights about part quality which are important for process qualification and illustrates the utility of melt pool thermal emission monitoring for identifying specific defects introduced by laser powder bed fusion.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Quasicrystal stability and nucleation kinetics from density functional theory

The aperiodic order of quasicrystals bridges the amorphous and crystalline regime, so it has remained unclear whether quasicrystals are metastable or stable phases of matter. Density functional theory is often used to evaluate thermodynamic stability, but quasicrystals are long-range aperiodic and their energies cannot be calculated using conventional ab initio methods. Here, in this work, we perform first-principles calculations on quasicrystal nanoparticles of increasing size, from which we can directly extrapolate their bulk and surface energies. Using this technique, we determine with high confidence that the icosahedral quasicrystals ScZn 7.33 and YbCd 5.7 are ground-state phases, thus revealing that translational symmetry is not a necessary condition for the zero-temperature stability of inorganic solids. Although we found the ScZn 7.33 quasicrystal to be thermodynamically stable, we show on a mixed thermodynamic and kinetic phase diagram that its solidification from the melt is limited by nucleation, which illustrates why even stable materials may be kinetically challenging to grow. Our techniques broadly open the door to first-principles investigations into the structure–bonding–stability relationships of aperiodic materials.

density functional theory↗