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DOE OSTI2025

Hierarchical domain structures in buckled ferroelectric free sheets

Flat elastic sheets tend to display wrinkles and folds. From pieces of clothing down to two-dimensional crystals, these corrugations appear in response to strain generated by sheet compression or stretching, thermal or mechanical mismatch with other elastic layers, or surface tension. Extensively studied in metals, polymers and, — more recently — in van der Waals exfoliated layers, with the advent of thin single crystal freestanding films of complex oxides, researchers are now paying attention to novel microstructural effects induced by bending ferroelectric-ferroelastics, where polarization is strongly coupled to lattice deformation. Here we show that wrinkle undulations in BaTiO3 sheets bonded to a viscoelastic substrate transform into a buckle delamination geometry when transferred onto a rigid substrate. Using spatially resolved techniques at different scales (Raman, scanning probe and electron microscopy), we show how these delaminations in the free BaTiO3 sheets display a self-organization of ferroelastic domains along the buckle profile that strongly differs from the more studied sinusoidal wrinkle geometry. Moreover, we disclose the hierarchical distribution of a secondary set of domains induced by the misalignment of these folding structures from the preferred in-plane crystallographic orientations. Our results disclose the relevance of the morphology and orientation of buckling instabilities in ferroelectric free sheets, for the stabilization of different domain structures, pointing to new routes for domain engineering of ferroelectrics in flexible oxide sheets.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Consistent Controls on Trace Metal Micronutrient Speciation in Wetland Soils and Stream Sediments

Trace metal are essential for microbially-mediated biogeochemical processes occurring in anoxic wetland soils and stream bed sediments, but low availability of these elements may inhibit anaerobic element cycling and transformations. Solid-phase speciation is likely a critical control on trace metal availability but has seen limited study in anoxic systems having concentrations similar to geological background levels, where metal limitations may be most prevalent. We have investigated trace metal concentrations and solid-phase speciation in three freshwater subsurface aquatic systems: marsh wetland soils, riparian wetland soils, and the sediments of a streambed. These systems displayed low solid-phase trace metal concentrations, generally at or below geological background levels, which generally followed the trend Zn > Cu ≈ Ni > Co and showed no correlation with major element compositions. All soils and sediments were dominated by quartz but varied in clay mineralogy as well as the organic matter, total sulfur, and total iron contents. X-ray absorption near-edge structure (XANES) spectroscopy shows that sulfur speciation in both wetlands is dominated by organic sulfur. Elemental sulfur and iron sulfides together made up <25% of the sulfur in the wetland soils, but the distribution between inorganic and organic forms was reversed in the stream sediments. Ferrous and ferric iron in clay minerals were common species identified by both XANES and extended X-ray absorption fine structure (EXAFS) spectroscopies at all sites. Iron(III) oxides were substantial components in all but the marsh wetland soils. Quantitative analysis of copper, nickel, and zinc XANES spectra revealed similar metal speciation across all sites. Copper speciation was dominated by sulfides, adsorbed species, and minor amounts of copper bound to organic matter; no metallic copper was detected. Nickel speciation also varied little and was dominated by nickel in clay mineral octahedral sheets and nickel sulfide, with adsorbed species also present. Zinc speciation was slightly more varied, with the marsh wetland soils and stream bed sediments containing adsorbed species, zinc associated with clay mineral structures, and zinc bound to reduced sulfur groups on organic matter, whereas the riparian wetland soils lacked clay-associated zinc but contained zinc sulfide. Trace metals bound to reduced sulfur occurred at every site, with a greater sulfur-bound fraction for copper. The fractional abundance of sulfur-bound species showed no relationship with soil or sediment total sulfur content, which varied by two orders of magnitude. More broadly, the observations in this study suggest that trace metal speciation in freshwater wetland soils and stream sediments is consistently dominated by a small set of recurring components which are distinct for each metal. Furthermore, this may represent a general geochemical phenomenon in anoxic soils and sediments containing trace metals at background concentrations (as low as 3 µg g -1 ) that was not predicted from systems that are contaminated with or naturally-enriched in copper, nickel, or zinc.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Copper Reductase Activity and Free Radical Chemistry by Cataract-Associated Human Lens γ-Crystallins

Cataracts are caused by high-molecular weight aggregates of human eye lens proteins that scatter light, causing lens opacity. Metal ions have emerged as important potential players in the etiology of cataract disease, as human lens γ-crystallins are susceptible to metal-induced aggregation. Here, the interaction of Cu 2+ ions with γD-, γC-, and γS- crystallins, the three most abundant γ-crystallins in the lens, has been evaluated. Cu 2+ ions induced non-amyloid aggregation in all three proteins. Solution turbidimetry, SDS-PAGE, circular dichroism and differential scanning calorimetry showed that the mechanism for Cu-induced aggregation involves: i) loss of beta-sheet structure in the N-terminal domain; ii) decreased thermal and kinetic stability; iii) formation of metal-bridged species; and iv) formation of disulfide-bridged dimers. Electron paramagnetic resonance (EPR) revealed two distinct Cu 2+ binding sites in each protein. Spin quantitation demonstrated reduction of γ-crystallin-bound Cu 2+ ions to Cu + under aerobic conditions, while X-ray absorption spectroscopy (XAS) confirmed the presence of linear or trigonal Cu + binding sites in γ-crystallins. Our EPR and XAS studies revealed that γ-crystallins’ Cu 2+ reductase activity yields a protein-based free radical that is likely a Tyr-based species in human γD-crystallin. This unique free radical chemistry carried out by distinct redox-active Cu sites in human lens γ-crystallins likely contributes to the mechanism of copper-induced aggregation. Finally, in the context of an aging human lens, γ-crystallins could be acting, not only as structural proteins, but also as key players for metal and redox homeostasis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

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 OSTI2020

Observation of single-defect memristor in an MoS2 atomic sheet

Non-volatile resistive switching, also known as memristor effect, where an electric field switches the resistance states of a two-terminal device, has emerged as an important concept in the development of high-density information storage, computing and reconfigurable systems. The past decade has witnessed substantial advances in non-volatile resistive switching materials such as metal oxides and solid electrolytes. It was long believed that leakage currents would prevent the observation of this phenomenon for nanometre-thin insulating layers. However, the recent discovery of non-volatile resistive switching in two-dimensional monolayers of transition metal dichalcogenide and hexagonal boron nitride sandwich structures (also known as atomristors) has refuted this belief and added a new materials dimension owing to the benefits of size scaling. Here we elucidate the origin of the switching mechanism in atomic sheets using monolayer MoS 2 as a model system. Atomistic imaging and spectroscopy reveal that metal substitution into a sulfur vacancy results in a non-volatile change in the resistance, which is corroborated by computational studies of defect structures and electronic states. These findings provide an atomistic understanding of non-volatile switching and open a new direction in precision defect engineering, down to a single defect, towards achieving the smallest memristor for applications in ultra-dense memory, neuromorphic computing and radio-frequency communication systems.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2023

Simultaneous determination of electrical conductivity and thickness of nonmagnetic metallic foils using two-sided multifrequency eddy current techniques

Here, in this paper, we describe a simple method for performing multifrequency eddy current characterization of free-standing uniform-thickness metallic foils using a forked inductive coil arrangement. The method involves measuring the mutual inductance between two coils when a foil is present between the coils, and when it is not present; the ratio of these mutual inductances is compared with an analytical solution, and foil conductivity, thickness, and sheet resistance are simultaneously estimated using numerical inversion and least-squares fitting. This method was used to characterize 34 non-ferrous metallic samples with thicknesses between 50 and 640 μm and with conductivities between 0.8 × 10 7 and 5.8 × 10 7 S/m. The estimated thicknesses from eddy current characterization agreed well with those measured using confocal optical techniques; the two approaches agreed to within 1 μm for samples that were thinner than 200 μm, and to within 0.5% for samples that had a thickness of 200 μm or greater. The estimated conductivities from eddy current characterization were in close agreement with expected values, given knowledge of the materials used. A particular strength of this approach is that the instrumentation needed is broadly available in research and development laboratories and the associated fixturing is easy to manufacture and assemble. A calibration procedure is described that can be used to reduce errors from geometric uncertainties. This calibration requires a sample that has only a known conductivity or thickness; both do not need to be known. The method described herein is likely extensible to conductivities and thickness well outside the ranges measured as part of this work.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

History and State of the Art in Advanced Thermal Protection Systems

This report documents the current state of the art of thermal protection systems (TPS) relevant to missile application materials and MTCR control language. The information is intended to provide data on current TPS for determining the current state of development and identifying potential research directions. Various vehicle configurations and types of TPS are described, including the evolution of materials and systems. Vehicle configurations such as high drag rocket and capsule systems and low-drag air-breathers are discussed. TPS are complex, transitioning from often very low temperatures to temperatures exceeding 3000°C and heat fluxes of up to 30,000 W/cm 2 . They can take the form of blankets, sheets, tiles and fabricated rigid structures, and can be made from high temperature capable alloys, refractory metals, ceramics, ceramic matrix composites, ultra-high temperature ceramics, carbon-carbon composites or ablative carbonaceous materials. Current state of the art in TPS is based on materials any systems developed for the initial space program. TPS was upgraded to the point of the Space Shuttle development and has stagnated since them.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Experimental and Theoretical Studies of the Surface Oxidation Process of Rare–Earth Tritellurides

Recent studies have established Van der Waals (vdW) layered and 2D rare-earth tritellurides (RTe 3 ) as superconductors and near room-temperature charge density wave (CDW) materials. Their environmental stability raises natural concern owing to aging/stability effects observed in other tellurium-based layered crystals. Here, the results establish the stability and environmental aging characteristics of these RTe 3 systems involving a variety of metals such as La, Nd, Sm, Gd, Dy, and Ho. The atomic force microscopy (AFM) and scanning electron microscopy (SEM) results show that all the RTe 3 sheets oxidize to form thin TeO x layers that are primarily confined to the surface, edges, and grain boundaries. Time-resolved in situ Raman spectroscopy measurements are used to understand the kinetics of the oxidization process for different lanthanide metal cations and establish their relative stability/resilience to oxidization. Overall results indicate that the vdW layers show higher air stability as the 4f electron number decreases going from Ho to La, resulting in the most stable LaTe 3 compared to the least stable HoTe 3 . Comprehensive quantum mechanical simulations reveal that environmental degradation originates from a strong oxidizing reaction with O 2 molecules, while humidity (H 2 O) plays a negligible role unless Te vacancies are present. Moreover, the simulations explain the effects of 4f electrons on the work function and Te vacancies formation, which directly impact the aging characteristics of RTe 3 layers. Interestingly, optical and electrical measurements show that the CDW response is still observed in aged RTe 3 layers owing to the presence of underlying pristine/nonoxidized RTe 3 layers, except CDW transition temperatures increase due to the thickness effect. Overall results offer the first in-depth environmental aging studies on these materials, which can be applied to engineer and design their chemical stability, surface properties, and overall CDW characteristics.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Dominant Role of Hole Transport Pathway in Achieving Record High Photoconductivity in Two‐Dimensional Metal–Organic Frameworks

Abstract Metal–organic frameworks (MOFs) with mobile charges have attracted significant attention due to their potential applications in photoelectric devices, chemical resistance sensors, and catalysis. However, fundamental understanding of the charge transport pathway within the framework and the key properties that determine the performance of conductive MOFs in photoelectric devices remain underexplored. Herein, we report the mechanisms of photoinduced charge transport and electron dynamics in the conductive 2D M−HHTP (M=Cu, Zn or Cu/Zn mixed; HHTP=2,3,6,7,10,11‐hexahydroxytriphenylene) MOFs and their correlation with photoconductivity using the combination of time‐resolved terahertz spectroscopy, optical transient absorption spectroscopy, X‐ray transient absorption spectroscopy, and density functional theory (DFT) calculations. We identify the through‐space hole transport mechanism through the interlayer sheet π–π interaction, where photoinduced hole state resides in HHTP ligand and electronic state is localized at the metal center. Moreover, the photoconductivity of the Cu−HHTP MOF is found to be 65.5 S m −1 , which represents the record high photoconductivity for porous MOF materials based on catecholate ligands.

Wang, Denan↗

DOE OSTI2023

Dominant Role of Hole Transport Pathway in Achieving Record High Photoconductivity in Two‐Dimensional Metal–Organic Frameworks

14 SOLAR ENERGY↗

DOE OSTI2020

Data Report: High-Resolution Microscopy Images of Sediments from Green Canyon Block 955, Gulf of Mexico

We took Leica microscopy images of sediment samples acquired at Holes H002 (4 samples) and H005 (1 sample) during the UT-GOM2-1 Expedition in Green Canyon Block 955, in the northern Gulf of Mexico. A total of 37 images were acquired. The images document a prevalence of spherical conchoidal minerals, cleavage planes typical of feldspar or mica, and black fragmented minerals which stand out from the surrounding matrix. Drilling mud intrusion is thought to contribute to a grey metallic matrix observed across multiple samples.

03 NATURAL GAS↗

DOE OSTI2020

Standalone sulfide based lithium ion-conducting glass solid electrolyte and associated structures, cells and methods

A standalone lithium ion-conductive solid electrolyte including a freestanding inorganic vitreous sheet of sulfide-based lithium ion conducting glass is capable of high performance in a lithium metal battery by providing a high degree of lithium ion conductivity while being highly resistant to the initiation and/or propagation of lithium dendrites. Such an electrolyte is also itself manufacturable, and readily adaptable for battery cell and cell component manufacture, in a cost-effective, scalable manner.

Visco, Steven J.↗

DOE OSTI2020

Vitreous solid electrolyte sheets of Li ion conducting sulfur-based glass and associated structures, cells and methods

A lithium ion-conductive solid electrolyte including a freestanding inorganic vitreous sheet of sulfide-based lithium ion conducting glass is capable of high performance in a lithium metal battery by providing a high degree of lithium ion conductivity while being highly resistant to the initiation and/or propagation of lithium dendrites. Such an electrolyte is also itself manufacturable, and readily adaptable for battery cell and cell component manufacture, in a cost-effective, scalable manner.

Visco, Steven J.↗

DOE OSTI2023

Vitreous solid electrolyte sheets of Li ion conducting sulfur-based glass and associated structures, cells and methods

Visco, Steven J.↗

DOE OSTI2023

Standalone sulfide based lithium ion-conducting glass solid electrolyte and associated structures, cells and methods

Visco, Steven J.↗

DOE OSTI2024

Vitreous solid electrolyte sheets of Li ion conducting sulfur-based glass and associated structures, cells and methods

Visco, Steven J.↗

DOE OSTI2025

Order-to-disorder transition due to entropy in layered and 2D carbides

In compositionally complex materials, there is controversy on the effect of enthalpy versus entropy on the structure and short-range ordering in so-called high-entropy materials. Here, to help address this controversy, we synthesized and probed 40 M 4 AlC 3 layered carbide phases containing two to nine metals and found that short-range ordering from enthalpy was present until the entropy increased enough to achieve complete disordering of the transition metals in their atomic planes. We transformed all of these layered carbide phases into two-dimensional (2D) sheets and showed the effects of the order versus disorder on their surface properties and electronic behavior. This study suggests the key effect that the competition between enthalpy and entropy has on short-range order in multicompositional materials.

Wyatt, Brian C. [Purdue Univ., West Lafayette, IN ↗

DOE OSTI2025

Enhanced Activity in Layered Metal-Oxide-Based Oxygen Evolution Catalysts by Layer-by-Layer Modulation of Metal-Ion Identity

Few-layered potassium nickel and cobalt oxides show drastic differences in catalytic activity based on metal ion preorganization. Uniform compositions [(CoO 2 /K) 6 or (NiO 2 /K) 6 ] show limited activity, while homogeneously mixed-metal cobalt/nickel oxides [(Co n Ni (1–n) O 2 /K) 6 ] display moderate improvement. However, a layer-by-layer arrangement of alternating cobalt and nickel oxide sheets [e.g., (CoO 2 /K/NiO 2 /K)] provides superior catalytic performance, reducing the oxygen evolution overpotential by ∼200–400 mV. Density functional theory simulations provide an illustration of the electronic properties (density of states and localization of orbitals) that promote catalysis in the layer-segregated materials over those of homogeneous composition. This study reveals that atomic preorganization of metal ions within layered catalysts plays a more crucial role than the overall metal composition in enhancing catalytic efficiency for oxygen evolution.

catalysts↗