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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Bobfinchite, Na[(UO2)8O3(OH)11]·10H2O, a new Na-bearing member of the schoepite family

Abstract The new mineral bobfinchite (IMA2020-082), Na[(UO2)8O3(OH)11]·10H2O, was found in the Burro mine, Slick Rock district, San Miguel County, Colorado, U.S.A., where it occurs as an oxidation product of uraninite on asphaltite matrix in intimate association with gypsum, natrozippeite, metaschoepite, and uranopilite. Bobfinchite crystals are transparent to translucent, yellow, lozenge-shaped disks up to 0.3 mm wide. Crystals are flattened on [100] and exhibit the forms {100}, {011}, {021}, {021}, and {011}. Bobfinchite has a pale-yellow streak and emits very dim yellow fluorescence under 365 nm ultraviolet illumination. The crystals are brittle with very good {100} cleavage and irregular, stepped fracture. The Mohs hardness is ca. 2 based on scratch tests. The calculated density is 5.044 g/cm3 based on the empirical formula and 5.036 g/cm3 for the ideal formula. Bobfinchite is optically biaxial (–), with α = 1.690(5), β = 1.7205(5), and γ = 1.730(5) (white light). The measured 2V, estimated from the interference figure, is 55(5)° and the calculated value is 59.1°. Dispersion is moderate, r > v; orientation: X = a, Y = b, Z = c; pleochroism: X nearly colorless, Y yellow, Z yellow; X < Y ≈Z. Electron microprobe analysis provided the empirical formula (Na0.99Pb0.02)[(UO2)7.99O3(OH)11]·10H2O. The five strongest X-ray powder diffraction lines are [dobs in Å(I)(hkl)]: 7.34(100)(200), 3.59(50)(024), 3.23(60)(224), 3.18(36)(240), and 2.01(23)(624,551,208,640,346). Bobfinchite is orthorhombic, Pbcn, a = 14.6249(9), b = 14.0389(10), c = 16.6923(10) Å, V = 3427.2(4) Å3, and Z = 4. The structure of bobfinchite (R1 = 0.0330 for 3770 I > 4σI) is built from uranyl oxide-hydroxide sheets that adopt the fourmarierite topology, with interlayer Na+ and H2O groups. Both the sheet and interlayer topology mimic those observed in natural and synthetic Na-metaschoepites studied previously, and as seen in other uranyl oxide hydrate minerals, charge balance is achieved at specific sites in the sheet through the substitution O2– ↔ (OH)–.

Geochemistry & Geophysics↗
DOE OSTI2024

Ultrathin Boron Growth onto Nanodiamond Surfaces via Electrophilic Boron Precursors

Diamond as a templating substrate is largely unexplored, and the unique properties of diamond, including its large bandgap, thermal conductance, and lack of cytotoxicity, makes it versatile in emergent technologies in medicine and quantum sensing. Surface termination of an inert diamond substrate and its chemical reactivity are key in generating new bonds for nucleation and growth of an overlayer material. Oxidized high-pressure high temperature (HPHT) nanodiamonds (NDs) are largely terminated by alcohols that act as nucleophiles to initiate covalent bond formation when an electrophilic reactant is available. In this work, we demonstrate a templated synthesis of ultrathin boron on ND surfaces using trigonal boron compounds. Boron trichloride (BCl 3 ), boron tribromide (BBr 3 ), and borane (BH 3 ) were found to react with ND substrates at room temperature in inert conditions. BBr 3 and BCl 3 were highly reactive with the diamond surface, and sheet-like structures were produced and verified with electron microscopy. Surface-sensitive spectroscopies were used to probe the molecular and atomic structure of the ND constructs’ surface, and quantification showed the boron shell was less than 1 nm thick after 1–24 h reactions. Observation of the reaction supports a self-terminating mechanism, similar to atomic layer deposition growth, and is likely due to the quenching of alcohols on the diamond surface. X-ray absorption spectroscopy revealed that boron-termination generated midgap electronic states that were originally predicted by density functional theory (DFT) several years ago. DFT also predicted a negative electron surface, which has yet to be confirmed experimentally here. The boron-diamond nanostructures were found to aggregate in dichloromethane and were dispersed in various solvents and characterized with dynamic light scattering for future cell imaging or cancer therapy applications using boron neutron capture therapy (BNCT). The unique templating mechanism based on nucleophilic alcohols and electrophilic trigonal precursors allows for covalent bond formation and will be of interest to researchers using diamond for quantum sensing, additive manufacturing, BNCT, and potentially as an electron emitter.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Supramolecular bending and twisting in the hierarchical self-assembly of monodisperse mesogenic oligomers

Understanding how different forms of supramolecular curvature arise during assembly is crucial to designing and tuning the microstructure of hierarchically self-assembled materials. Here, we show that in crystalline phases of mesogenic oligomers, the oligomer length is a critical parameter that determines the type of curvature (Gaussian or cylindrical) exhibited by the self-assembled structures. We use iterative exponential growth to synthesize monodisperse mesogenic oligomers ranging from dimer to octamer. By analyzing their phase behavior and microstructure, we elucidate how length-dependent thermodynamic and kinetic effects tune their hierarchical degree of ordering. The oligomers’ length-dependent crystalline order drives the formation of scrolled sheets in shorter oligomers and twisted ribbons in longer oligomers. These studies highlight how oligomer length interplays with mesogen geometry and crystalline packing to drive self-assembly, introducing oligomer length as a powerful design parameter toward tailored applications of mesogenic systems.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Intermediate States Enable Keratin-like α-To-β Transformations in Strain-Responsive Synthetic Polypeptides

Nature’s fibrous proteins, such as α-keratin, achieve remarkable mechanical properties by undergoing strain-induced α-to-β conformational transitions. Inspired by these materials, we report a strategy for designing synthetic polypeptides that undergo similar transformations at elevated temperatures far exceeding keratin’s operational range. By employing helix-confined ring-opening polymerization (ROP) of N -carboxyanhydrides (NCAs) initiated by a short poly(γ-benzyl- L -glutamate) (PBLG) precursor, we synthesized poly( O -benzyl- L -serine) (PBLS) chains that adopt an α-helical structure yet transition into β-sheets upon heating. Compression molding at carefully chosen temperatures drives PBLS segments into an α-β intermediate state, characterized by relaxed intrachain hydrogen bonds and a hexagonal packing arrangement. Under mechanical strain, these intermediate states convert in situ into β-sheets, producing significant strain-hardening well below the spontaneous α-to-β temperature threshold. Further, this approach extends to polypeptides bearing different side chains, such as poly(S-benzyl- L -cysteine), demonstrating robust mechanical reinforcement across a wide temperature window up to ∼ 200 °C. In situ synchrotron X-ray analysis confirms that chain alignment, β-sheet formation, and domain growth occur stepwise during deformation. By harnessing the intermediate states and the supramolecular cooperativity conferred by compression-molded films, our method provides a versatile platform for developing next-generation polypeptide materials with tunable mechanical resilience and responsiveness─surpassing the temperature limitations of natural fibrous proteins and enabling potential applications demanding broad-temperature mechanical adaptability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Neutrino and pair creation in reconnection-powered coronae of accreting black holes

A ubiquitous feature of accreting black hole systems is their hard X-ray emission which is thought to be produced through Comptonization of soft photons by electrons and positrons in the vicinity of the black hole, in a region with optical depth of order unity. The origin and composition of this Comptonizing region, known as the corona, is a matter open for debate. In this paper we investigate the role of relativistic protons accelerated in black-hole magnetospheric current sheets for the pair enrichment and neutrino emission of AGN coronae. Our model has two free parameters, namely the proton plasma magnetization σ p , which controls the peak energy of the neutrino spectrum, and the Eddington ratio λ X,Edd (defined as the ratio between X-ray luminosity L X and Eddington luminosity L Edd ), which controls the amount of energy transferred to secondary particles. For sources with λ X,Edd ≳ λ Edd,crit (where λ Edd,crit ∼ 10 -1 for σ p = 10 5 or ∼ 10 -2 for σ p = 10 7 ), proton-photon interactions and γγ annihilation produce enough secondary pairs to achieve Thomson optical depths τ T ∼ 0.1-10. In the opposite case of λ X,Edd ≲ λ Edd,crit , the coronal pairs cannot originate only from hadronic interactions. Additionally, we find that the neutrino luminosity scales as L 2 X /L Edd for λ X,Edd ≲ λ Edd,crit , while it is proportional to L X for higher λ X,Edd values. We apply our model to four Seyfert galaxies, including NGC 1068, and discuss our results in light of recent IceCube observations.

active galactic nuclei↗
DOE OSTI2025

Synthetic Pathways to gamma-Graphyne and Related Allotropes of Carbon

Graphynes, two-dimensional carbon lattices combining sp 1 and sp 2 hybridized atoms, were predicted theoretically more than three decades ago, but few structures have been realized to date. These carbons are believed to possess remarkable mechanical and electronic properties, including high charge carrier mobilities comparable to those in graphene (10 4 to 10 5 cm 2 V -1 s -1 ). Unlike graphene, certain graphynes are predicted to be intrinsic semiconductors. Among these intriguing structures, γ-graphyne stands out as the structurally simplest and most symmetric sp 1 /sp 2 lattice. γ-Graphyne was first theorized in 1987. In contrast with graphene, γ-graphyne will be a semiconductor with a small band gap suitable for fabrication of electronic devices. This solves one of the fundamental problems of carbon-based electronics, the necessity for inducing a band gap in graphene. γ-Graphyne has the potential to form the basis for the next generation of carbon-based electronics operating at speeds unattainable by traditional silicon chips. Unlike silicon, γ-graphyne is a direct band gap semiconductor, and it will feature exceptional strength comparable to that of other 2D carbon allotropes. Such combination of properties may enable a new generation of highly efficient, ultra-light and flexible solar cells. Despite being a potentially “magical” material, γ-graphyne remained synthetically elusive for over three decades. The primary goals of this project were: (1) Synthesis of bulk γ-graphyne phases through solution-phase 2D polymerizations; (2) Experimental exploration of the physical and chemical properties of γ-graphyne; and (3) Mechanistic and theoretical studies of the novel chemical transformations developed in Goal 1. Common pyrolytic and vapor-deposition methodologies used for the synthesis of graphitic allotropes are unsuitable for graphyne and other sp 1 -contaning structures, as acetylenes readily convert to graphene and amorphous carbon at high temperatures. In contrast, this proposal is based on solution-based 2D polymerization. The major advantages of this approach over the traditional high temperature techniques are the potential to adjust the structure of the material with atomic precision, and the possibility of using structurally complex and relatively fragile repeat units. The outcomes of this research can revolutionize carbon nanotechnology, expanding the field’s structural toolbox beyond primarily graphitic and benzenoid structures. Understanding the chemistry of sp 1 carbon allotropes can lead to entirely new classes of structures with unique properties, including graphyne ribbons, nanotubes, quantum dots, and heterostructures with other 2D materials. Furthermore, the development of reliable and robust synthetic pathways towards periodic covalent molecular sheets with atomically precise structures shall have a profound impact on chemistry and materials science.

2D polymerization↗
DOE OSTI2025

Chemical Process Safety at TRISO-Based, Metal-Based, and Salt-Based Fuel Fabrication Facilities: Technical Assessment and Guidance Assessment

As part of efforts to prepare for potential and ongoing safety reviews for licensing of advanced non-light-water reactor fuel cycles, the U.S. Nuclear Regulatory Commission (NRC) tasked Pacific Northwest National Laboratory to prepare an assessment on the state of knowledge of potential chemical processes at fuel cycle facilities supporting the front end of these fuel cycles, and to assess the associated regulatory guidance. This report provides a technical assessment of chemical process safety considerations to support NRC licensing reviews of fabrication processes for tri-structural isotropic (TRISO) based, metallic-based, and salt-based fuels. The assessments involved collecting publicly available information on the fuel fabrication processes to (i) identify the operational process steps, characteristics and chemicals involved, (ii) identify the physical safety considerations and health safety considerations during licensing reviews of the various process steps, and (iii) collect information to support assessments of severity of accidents and potential mitigative measures to be implemented. The assessment provides a foundational basis on chemical process safety considerations for advanced fuel fabrication activities, although it is recognized that licensing reviews may necessitate design-specific considerations. The specific conditions under which chemical hazards emerge will require process-specific considerations, highlighting the importance of process-informed interpretation. The assessment also determined that exposure guidelines and limits to assess the consequences of acute exposures are limited for some chemicals, although alternative limits and supplementary information from databases or safety data sheets provide sufficient information to evaluate consequences of acute exposures. In addition, it was identified that metallic and salt fuel fabrication processes may involve beryllium, which is an exposure hazard. The regulatory framework for the licensing of advanced fuel cycle facilities, per 10 CFR Part 70 Domestic Licensing of Special Nuclear Material, is deemed robust and flexible to address the chemical safety considerations in this report. A review was conducted on various regulatory guidance and technical basis documents. This included reviewing NUREG-1520, Revision 2, Standard Review Plan for Fuel Cycle Facilities License Applications – Final Report and the process descriptions in Appendix A of NUREG/CR-6410, Nuclear Fuel Cycle Facility Accident Analysis Handbook, to address advanced fuel types. As new fuels will involve process-specific chemical uses, process-specific considerations are provided in this report. Additionally, it is noted that the U.S. Department of Energy protective action criteria database includes Temporary Emergency Exposure Limits (TEELs) for process-specific chemicals. This report provides technical information to support chemical safety assessments of new advanced fuel cycle facilities and identifies technical and safety information to support licensing reviews. No regulatory barriers were identified for the licensing of advanced fuel cycle facilities.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Topological Surface Superconductivity via Josephson Coupling in Bi 2 Te 3 /Nb

Since discoveries of protected conducting surface states, topological superconducting qubits have enchanted quantum science as prime elements in future fault-tolerant devices, particularly those based on Josephson junctions containing topological insulators. Still, Josephson coupling is often eclipsed by other proximity effects that can dilute topological superconducting pairing at the nontrivial insulator’s boundaries. Here, however, using an ultra-low-temperature scanning tunneling microscope, we detect Josephson physics in topological Bi 2 Te 3 films on superconducting Nb. At low temperatures, a previously undetected proximity gap varies little with Bi 2 Te 3 thickness and the density of states exhibits normal and superconducting components. Such observations are rationalized via Josephson pair tunneling through the (nearly) insulating Bi 2 Te 3 bulk, creating a rare, pure topological superconducting sheet. Our findings establish routes toward accessible topological superconducting states in qubits.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Tantalum Experiments in Fully-Reflected Water-Moderated Triangular-Pitched U(6.90)O 2 Fuel Rod Lattices (1.02 cm Pitch)

The United States (US) Department of Energy (DOE) Nuclear Energy Research Initiative funded the design and construction of the Seven Percent Critical Experiment (7uPCX) at Sandia National Laboratories (SNL). The start-up of the experiment facility and the execution of the experiments described here were funded by the DOE Nuclear Criticality Safety Program. The 7uPCX is designed to investigate critical systems with fuel for light water reactors in the enrichment range above 5 % 235 U. The 7uPCX assembly is a water moderated and — reflected array of aluminum-clad U(6.90 %)O 2 fuel rods. Other critical experiments performed in the 7uPCX assembly are documented in LEU-COMP-THERM-078, LEU-COMP-THERM-080, LEU-COMP-THERM 096, LEU- COMP-THERM-097, LEU-COMP-THERM-101, LEU-COMP-THERM-102, and LEU-COMP-THERM-111. Applied interests in neutron-absorbing elements at epithermal and intermediate neutron energy ranges at DOE’s Hanford Site and Savannah River Site were identified through DOE Office of Environmental Management (EM) workshops and needs surveys performed in conjunction with the National Nuclear Security Administration/Nuclear Criticality Safety Program. In response, a team lead by Oak Ridge National Laboratory (ORNL) performed a study evaluating the use of 7uPCX for testing the epithermal cross sections of materials at SNL. This marked the inception of the set of experiments described here. The purpose of these experiments was to measure the effects of tantalum in nearly-critical systems. The tantalum was introduced into the fuel arrays as experiment rods within a central test region. The central test region was designed to target the epithermal neutron energy range by providing a dry cylindrical cavity constructed of aluminum and lined with 0.04 in (0.1016 cm) thick cadmium sheet. The central test region has an outer diameter of 3.75 in (9.525 cm) length of 31 in (78.74 cm) and can hold 85 tantalum rods nominally 0.25 in (0.635 cm) outside diameter and 31.25 in (79.375 cm) long. The critical experiments were done using a set of triangular-pitched grid plates fabricated for these experiments. The grid plate set accommodated a fuel array of a total of 2016 fuel rod positions on a pitch of 0.4 in (1.016 cm) in a series of 21 hexagonal rings positioned around the central test region. The fuel used in these experiments was fabricated using unirradiated 6.90 % enriched UO 2 fuel pellets from fuel elements designed to be used in the internal nuclear superheater section of the Pathfinder boiling water reactor operated in South Dakota by the Northern States Power Company in the 1960s. The fuel elements were obtained from The Pennsylvania State University where they had been stored for many years. The fuel pellets in those fuel elements were removed from the original Incoloy cladding and reclad in 3003 aluminum tubes and end caps for use in the experiments reported here. The eight cases in this experiment series were performed in 2024 in the Sandia Critical Experiments (SCX) at the Sandia Pulsed Reactor Facility by varying the number of fuel rods in the critical assembly. The personnel involved in conducting these experiments included David Ames, Elijah Lutz, Beth Hanson, Patrick Ward, Jason Soares, and Augie Chapa from SNL, as well as Mathieu Dupont and B.J. Marshall from ORNL. Case 1 had no tantalum experiment rods. Case 2 had seven tantalum rods in the center of the central test region. Case 3 had 18 tantalum rods in the third hexagonal ring of the central test region. Case 4 had 19 tantalum rods in the center of the central test region. Case 5 had 30 tantalum rods in the outer most positions of the central test region. Case 6 had 37 tantalum rods in the center of the central test region. Case 7 had 61 tantalum rods in the center of the central test region. Case 8 had 85 tantalum rods filling all positions in the central test region. All eight critical experiments are judged to be acceptable as benchmark experiments.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2026

Synthesis and Characterization of Layered Actinide (U, Np, Pu) Oxide and Hydroxide Phases

Systematic structural comparisons across the early actinides remain limited by the scarcity of well-defined transuranic layered oxide and oxyhydroxide phases. Here, we report the synthesis and single-crystal characterization of new layered actinide compounds spanning U, Np, and Pu obtained under mild hydrothermal conditions in concentrated alkali hydroxide media. These include hydrated oxides α-Cs 2 U 2 O 7 •0.5H 2 O and Rb 2 An 2 O 7 •0.5H 2 O (An = Np, Pu), oxy-hydroxides Rb 6 [(AnO 2 ) 6 O 8 (OH) 2 ]•xH 2 O x = 0, 0.5 (An = U, Np) and Rb 4 [(UO 2 ) 5 O 6 (OH) 2 ]•2H 2 O, as well as nitrate-intercalated compounds Cs 6 [(AnO 2 ) 3 O 4 (OH) 2 ](NO 3 ) 2 (An = Np, Pu). Single-crystal X-ray diffraction studies reveal extended two-dimensional architectures constructed from edge- and vertex-sharing actinyl polyhedra, with systematic evolution in equatorial coordination, hydration, and anionic sheet topology across the U–Np–Pu series. Incorporation of nitrate anions within the interlayer region of Cs 6 [(AnO 2 ) 3 O 4 (OH) 2 ](NO 3 ) 2 establishes a previously unobserved structural motif in layered transuranic oxyhydroxides, demonstrating an additional pathway for anion-mediated framework stabilization. Correlation of crystallographic metrics with single-crystal Raman spectroscopy provides new vibrational benchmarks linking differences in An═O yl bond lengths to the equatorial coordination and the interstitial cations. These findings expand the structural hierarchy of layered actinide materials and address clarifying periodic trends governing topology, bonding, and vibrational signatures in high-valent 5ƒ oxide systems.

actinides↗
DOE OSTI2024

Near Room Temperature Solvothermal Growth of Ferroelectric CsPbBr 3 Nanoplatelets with Ultralow Dark Current

CsPbBr 3 exhibits outstanding optoelectronic properties and thermal stability, making it a coveted material for detectors, light-emitting diodes, and solar cells. Despite observations of ferroelectricity in CsPbBr 3 quantum dots, synthesizing bulk ferroelectric CsPbBr 3 crystals has remained elusive, hindering its potential in next-generation optoelectronic devices like optical switches and ferroelectric photovoltaics. Here, a breakthrough is reported: a novel solvothermal technique enabling the growth of ferroelectric CsPbBr 3 nanoplatelets with lateral dimensions in the tens of micrometers. This represents a significant step toward achieving large-area ferroelectric CsPbBr 3 crystals. Unlike traditional methods, this approach allows for growth and crystallization of CsPbBr 3 in alcohol solutions by enhancing precursor solubility. Further this study confirms the ferroelectric nature of these nanoplatelets using second harmonic generation, electrical characterizations, and piezoresponse force microscopy. This work paves the way for utilizing ferroelectric CsPbBr 3 in novel optoelectronic devices, significantly expanding the potential of this material and opening doors for further exploration in this exciting field.

25 ENERGY STORAGE↗
DOE OSTI2025

Surface structure of water from soft X-ray second harmonic generation

The microscopic structure of water’s surface is crucial to many natural and industrial processes, but studying its hydrogen bond (H-bond) network directly remains challenging due to the required interfacial sensitivity of experimental techniques. By leveraging advances in flat liquid sheet microjets and terawatt-scale attosecond soft X-ray pulses from the LCLS X-ray free electron laser, we employed soft X-ray second harmonic generation (SXSHG) spectroscopy to examine the liquid water/vapor interface. SXSHG combines the elemental selectivity of X-ray spectroscopies with the surface selectivity of SHG and gives access to the electronic structure of interfacial species. Here, we show the SXSHG spectrum differs from bulk water’s X-ray absorption, with its peak shifted several eV, indicating a vastly different electronic environment at the interface as compared to the bulk. First-principles electronic structure calculations show the signal is highly sensitive to H-bond interactions, such as water molecules accepting a single H-bond, which are surface abundant.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Characterization and automated optimization of laser-driven proton beams from converging liquid sheet jet targets

Compact, stable, and versatile laser-driven ion sources hold great promise for applications ranging from medicine to materials science and fundamental physics. While single-shot sources have demonstrated favorable beam properties, including the peak fluxes necessary for several applications, high-repetition-rate operation will be necessary to generate and sustain the high average flux needed for many of the most exciting applications of laser-driven ion sources. Further, to navigate through the high-dimensional space of laser and target parameters toward experimental optima, it is essential to develop ion acceleration platforms compatible with machine learning techniques and capable of autonomous real-time optimization. Here, we present a multi-Hz ion acceleration platform employing a liquid sheet jet target. We characterize the laser-plasma interaction and the laser-driven proton beam across a variety of key parameters governing the interaction using an extensive suite of online diagnostics. We also demonstrate real-time, closed-loop optimization of the ion beam maximum energy by tuning the laser wave front using a Bayesian optimization scheme. This approach increased the maximum proton energy by 11% compared to a manually optimized wave front by enhancing the energy concentration within the laser focal spot, demonstrating the potential for closed-loop optimization schemes to tune future ion accelerators for robust high-repetition-rate operation.

Glenn, G. D. [SLAC National Accelerator Laboratory↗