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DOE OSTI2020

Laser-Produced Coherent X-ray Sources. Final report

This is the final report for the DOE-AMO DE-FG02-05ER15663 grant. Using a high-peak-power laser system at the Extreme Light Laboratory of the University of Nebraska-Lincoln, we develop novel femtosecond radiation sources and use them to investigate ultrafast photo-induced processes. Pulses of high energy electrons and x-rays are generated when an optical pulse is focused to ultra-high intensity. The radiation is used to probe the evolution of matter under highly non-equilibrium conditions with atomic-scale temporal and spatial resolution. Moreover, the facility is small enough to fit in a university laboratory and is operated by graduate students and postdocs.

74 ATOMIC AND MOLECULAR PHYSICS↗

DOE OSTI2025

Low-temperature access to active iron and iron/nickel nitrides as potential electrocatalysts for the oxygen evolution reaction

Low-temperature, scalable routes to transition metal nitride (TMN) nanoparticles are desirable for a wide range of applications, yet their synthesis typically requires high temperatures (>350 °C) and reactive gas environments (e.g., NH 3 or H 2 /N 2 ). Here, we report a colloidal synthesis of mono- and bimetallic TMN nanoparticles using preformed metal carbonyl clusters as precursors and urea or diethylenetriamine (DETA) as nitrogen sources. This strategy enables access to size-controlled, phase-pure ε-Fe 3 N x and Fe y Ni 3−y N nanoparticles at temperatures below 300 °C, without the need for flowing reactive gas atmospheres. By systematically varying nitrogen precursor, reaction temperature, and cluster identity, we achieve tunable nitrogen stoichiometry (x) and phase selectivity between N-rich and N-poor TMNs. Structural and magnetic characterization confirms clean decomposition of the precursors and phase formation consistent with controlled nitridation at the nanoscale. Preliminary electrochemical measurements in alkaline media demonstrate that these materials exhibit oxygen evolution reaction (OER) overpotentials comparable to RuO 2 , highlighting their viability for future electrocatalytic applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

Engineered Barrier System Research Activities at SNL: FY25 Report

This report describes research and development (R&D) activities conducted at Sandia National Laboratories (SNL) during Fiscal Year 2025 (FY25) specifically related to the Engineered Barrier System (EBS) Properties & Processes Work Package in the Spent Fuel and High-Level Waste Disposition (SFHLWD) Campaign supported by the United States (U.S.) Department of Energy (DOE). SNL activities focus on understanding EBS component evolution and interactions within the EBS, as well as interactions between the host media and the EBS. The team represented in this report consists of individuals from SNL, Argonne National Laboratory (Advanced Photon Source), and Vanderbilt University. The activities represented in this report include development of anion sorbent materials for buffer formulations, properties of pure bentonite and bentonite mixtures, and characterization of cement interfaces relevant to the EBS. The SNL EBS activities also leverage interactions with EBS teams from other national laboratories, and international collaborations to ensure that the DOE program is active and abreast of the latest advances in nuclear waste disposal.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

Intermediate-Scale Experimental Study to Improve Fundamental Understanding of Attenuation Capacity for Leaking CO 2 in Heterogeneous Shallow Aquifers

In order to assess the risks of Geologic Carbon Sequestration (GCS), it is crucial to understand the fundamental physicochemical processes that may occur if and when stored CO 2 leaks upward from a deep storage reservoir into the shallow subsurface. Intermediate-scale experiments allow for improved understanding of the multiphase evolution processes that control CO 2 migration behaviour in the subsurface, because the boundary conditions, initial conditions, and porous media parameters can be better controlled and monitored in the laboratory than in field settings. For this study, a large experimental test bed was designed to mimic a cross-section of a shallow aquifer with layered geologic heterogeneity. As water with aqueous CO 2 was injected into the system to mimic a CO 2 -charged water leakage scenario, the spatiotemporal evolution of the multiphase CO 2 plume was monitored. Similar experiments were performed with two different sand combinations to assess the relative effects of different types of geologic facies transitions on the CO 2 evolution processes. Significant CO 2 attenuation was observed in both scenarios, but by fundamentally different mechanisms. When the porous media layers had very different permeabilities, attenuation was caused by local accumulation (structural trapping) and slow re-dissolution of gas phase CO 2 . When the permeability difference between the layers was relatively small, on the other hand, gas phase continually evolved over widespread areas near the leading edge of the aqueous plume, which also attenuated CO 2 migration. In conclusion, this improved process understanding will aid in the development of models that could be used for effective risk assessment and monitoring programs for GCS projects.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Technology Development for Dry Storage of Aluminum-Clad Spent Nuclear Fuel - 20490

A candidate disposition pathway for the > 13 MTHM of aluminum-clad spent nuclear fuel (ASNF), owned and managed by the U.S. Department of Energy, is the drying and placement of the SNF into sealed-canister dry storage, with the ASNF-in- canisters 'road-ready' for transportation to and final direct disposal in a repository waste package. Technical information gaps in fuel drying, and fuel dry storage behavior, have previously challenged the declaration of technology readiness for drying and placement of this fuel into the DOE Standard Canister design for > 50 years of safe dry storage. The principal technical information gaps included: i) characterization and thermal dehydration behavior of aluminum (oxy)hydroxide films attendant on the cladding due to film formation during reactor operation and during post-discharge up to long-term wet storage histories; and ii) G-value data to enable estimation of the radiolytic gas generation from the cladding with its (oxy)hydroxide films. Thus, the oxide films on the ASNF challenged the safety of a sealed storage canister with thermal and radiolytic decomposition of the waters on the films that can lead to corrosion, pressurization, and flammability issues. These gaps in the technical information base have largely been closed. This paper discusses the investigations at the Idaho National Laboratory (INL) and the Savannah River National laboratory (SRNL), and outlines the pending technology development work for input to an engineering design to enable a road-ready dry storage system for ASNF. The ASNF inventory considered for road-ready dry storage is stored at the Savannah River Site (SRS) and at the Idaho Nuclear Technology and Engineering Center (INTEC) at the INL. The ASNF inventory in the SRS L Basin is from foreign and domestic research reactors (FRR and DRR), and is diverse in terms of design, irradiation, and post-reactor-discharge storage conditions; these factors yield a range of characteristics of cladding oxide films on ASNF. Mixed aluminum (oxy)hydroxide (boehmite and bayerite/gibbsite) films, non-uniform in thicknesses up to a maximum local thickness bounded by 25 μm, were observed on ASNF materials removed from wet storage in the L Basin and in non-sealed dry storage at the SRS following reactor service and a long-term (up to 40+ years) interim storage history. The ASNF inventory at INTEC, in both wet and vented dry storage, is predominantly from the Advanced Test Reactor (ATR), but it also includes DRR and FRR fuel. To address a profound behavior of these films, radiolysis testing of aluminum specimens with mixed type boehmite/bayerite oxide films was performed to develop basic data on G-values for production of radiolytic hydrogen under dry storage conditions with nominal relative humidity, temperature, and cover gas. Modeling and simulation of canister internal environments with postulated inventories of oxide films provides estimation of the evolution of the conditions of the canister loaded with ASNF. Simultaneous Thermal Analysis (TGA/DSC) of hydrated oxide powders, and laboratory-scale aluminum specimens with a bayerite film (∼10 μm) using TGA methods, inform drying time/temperature conditions to be used for the ASNF. A demonstration project is recommended for Verification and Validation of the drying and storage of the ASNF. Remaining major tasks leading up to the hot demonstration include scale-up radiolysis testing and scale-up drying testing. Engineering design with the information from the technology program will establish the safety basis and enable long-term (> 50 years) dry storage compatibility with ASNF in the DOE Standard Canister pending its transportation to and disposal in a repository. This full capability would show the ASNF-in-canister storage system to be road-ready. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2013

Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials

The Curiosity Rover landed on the Peace Vallis alluvial fan in Gale crater on August 5, 2012. A primary mission science objective is to search for past habitable environments, and, in particular, to assess the role of past water. Identifying the minerals and mineraloids that result from aqueous alteration at Gale crater is essential for understanding past aqueous processes at the MSL landing site and hence for interpreting the site's potential habitability. X-ray diffraction (XRD) data from the CheMin instrument and evolved gas analyses (EGA) from the SAM instrument have helped the MSL science team identify phases that resulted from aqueous processes: phyllosilicates and amorphous phases were measure in two drill samples (John Klein and Cumberland) obtained from the Sheepbed Member, Yellowknife Bay Fm., which is believed to represent a fluvial-lacustrine environment. A third set of analyses was obtained from scoop samples from the Rocknest sand shadow. Chemical data from the APXS instrument have helped constrain the chemical compositions of these secondary phases and suggest that the phyllosilicate component is Mg-enriched and the amorphous component is Fe-enriched, relatively Si-poor, and S- and H-bearing. To refine the phyllosilicate and amorphous components in the samples measured by MSL, we measured XRD and EGA data for a variety of relevant natural terrestrial phyllosilicates and synthetic mineraloids in laboratory testbeds of the CheMin and SAM instruments. Specifically, Mg-saturated smectites and vermiculites were measured with XRD at low relative humidity to understand the behavior of the 001 reflections under Mars-like conditions. Our laboratory XRD measurements suggest that interlayer cation composition affects the hydration state of swelling clays at low RH and, thus, the 001 peak positions. XRD patterns of synthetic amorphous materials, including allophane, ferrihydrite, and hisingerite were used in full-pattern fitting (FULLPAT) models to help determine the types and abundances of amorphous phases in the martian rocks and sand shadow. These models suggest that the rocks and sand shadow are composed of approx 30% amorphous phases. Sulfate-adsorbed allophane and ferrihydrite were measured by EGA to further understand the speciation of the sulfur present in the amorphous component. These data indicate that sulfate adsorbed onto the surfaces of amorphous phases could explain a portion of the SO2 evolution in the Rocknest SAM data. The additional constraints placed on the mineralogy and chemistry of the aqueous alteration phases through our laboratory measurements can help us better understand the nature of the fluids that affected the different samples and devise a history of aqueous alteration for the Sheepbed Member of the Yellowknife Bay Fm. at Gale crater.

Rampe, Elizabeth B.↗

DOE OSTI2021

Materials Challenges and Opportunities for Energy Generation, Conversion, Delivery, and Storage (Applied Energy Tri-Laboratory Consortium Workshop Report)

This report documents the outcomes of the Tri-Laboratory Materials Workshop that was held July 31 and August 1, 2019 to begin addressing the needs, opportunities, and challenges associated with the development, fabrication, and testing of the needed materials and components for integrated hybrid energy systems (i.e., incorporating nuclear, fossil, and renewables for electric and thermal applications). This was accomplished by assembling the research program leads and principal investigators at Idaho National Laboratory (INL), National Energy Technology Laboratory (NETL), and National Renewable Energy Laboratory (NREL), who support the research and development of new technology and system integration. The team then identified and prioritized key materials development needs. This effort was intended to enhance communications and synergy among the Tri-Lab partners. Advanced functional and structural materials are central to transformative energy technologies for energy generation, conversion, delivery, and storage. With that in mind, the workshop focused on identifying and assessing the foundational materials research needs at both the basic and applied levels. Materials challenges include the ability to withstand harsh environments, such as high temperatures and pressures, corrosion, oxidation, or irradiation while maintaining flexible mission profiles and long service lifespans. Advanced energy system material challenges and needs range from materials for the capture, upgrading/concentration, storage, and delivery of low-grade heat to materials for high temperature environments that involve liquid metals, molten salt, and very high temperature gas heat delivery and storage systems. Material improvements are needed for hybrid energy systems due to accelerated corrosion and stress-fatigue failure of materials and equipment, which results from increased frequency and amplitude of thermal, mechanical, and electrical cycling of systems components. Multifunctional materials are needed for high temperature solid-oxide fuel cells, advanced electrochemical reactors, and in-process separation. Relative to materials manufacturing, application of advanced additive and subtractive methods need to be understood to develop both thin-layer homogenous materials and materials of graded composition. Materials modeling and machine learning will be critical to accelerate the design and production of power electronics, and nuclear reactor materials and fuel, as well as to gain an understanding of beneficial materials phenomena or deleterious microstructure evolution. There is also a need for standardized models, computational structures, data reporting protocols and modeling tools across the three laboratories. This would allow consistent results, analysis, and data sharing. Combining computational capabilities between the three laboratories (e.g., hardware, software) would greatly increase computational capabilities and throughput. The workshop identified the need for laboratories to anticipate and address problems that will occur during scale-up. Laboratory work must connect with industry to ensure that research focuses on processes that are scalable and marketable. Industry input and perspective are essential to guide laboratory research to meet these requirements and deploy new technology in industrial demonstrations. Another aspect of scale-up is the integration of multiple systems since new challenges often arise at the subsystem interfaces. Establishing a scale-up manufacturing demonstration/pilot plant, potentially as an industrial user facility, would be beneficial to the laboratories and industry. That modular scale-up manufacturing demonstration/pilot plant would allow researchers to find and resolve interface problems that cannot be identified by focusing only on individual parts. Communication exchanges among the organizers, attendees, and workshop survey responses indicate that the workshop was successful in achieving its goal to identify key technology gaps and research needs. Strong positive feedback was received on the sharing of ideas, capabilities, talent, and passion to move forward on the materials-related action items.

36 MATERIALS SCIENCE↗

NASA NTRS1985

The spatial evolution of energetic electrons and plasma waves during the steady state beam plasma discharge

Experiments, involving the injection of energetic (keV) electron beams into the ionosphere-upper atmosphere system from rocket-borne electron guns, have provided evidence for the occurrence of strong beam-plasma interactions (BPI) both near to and remote from the injection point. However, the flight experiments have not provided clear and unambiguous evidence for the basic physical processes which produce the variety of confusing signatures. A laboratory experimental program was initiated to clarify some of a number of ambiguities regarding the obtained results. The present investigation is concerned with some experimental studies of the evolution of both the beam energy spectrum and the local wave amplitude-frequency spectrum at increasing axial distances from the electron gun for a variety of experimental conditions. The results of the studies show that the high frequency beam-plasma interaction represents the most important process.

Llobet, X.↗

NASA NTRS1990

Evolution paths for advanced automation

As Space Station Freedom (SSF) evolves, increased automation and autonomy will be required to meet Space Station Freedom Program (SSFP) objectives. As a precursor to the use of advanced automation within the SSFP, especially if it is to be used on SSF (e.g., to automate the operation of the flight systems), the underlying technologies will need to be elevated to a high level of readiness to ensure safe and effective operations. Ground facilities supporting the development of these flight systems -- from research and development laboratories through formal hardware and software development environments -- will be responsible for achieving these levels of technology readiness. These facilities will need to evolve support the general evolution of the SSFP. This evolution will include support for increasing the use of advanced automation. The SSF Advanced Development Program has funded a study to define evolution paths for advanced automaton within the SSFP's ground-based facilities which will enable, promote, and accelerate the appropriate use of advanced automation on-board SSF. The current capability of the test beds and facilities, such as the Software Support Environment, with regard to advanced automation, has been assessed and their desired evolutionary capabilities have been defined. Plans and guidelines for achieving this necessary capability have been constructed. The approach taken has combined indepth interviews of test beds personnel at all SSF Work Package centers with awareness of relevant state-of-the-art technology and technology insertion methodologies. Key recommendations from the study include advocating a NASA-wide task force for advanced automation, and the creation of software prototype transition environments to facilitate the incorporation of advanced automation in the SSFP.

Healey, Kathleen J.↗

DOE OSTI2017

Evolution of the Field of Statistics at Los Alamos

Through years of technological improvements, cultural change, advances in statistical theory, revisions of federal government structure and policies, Laboratory re-organizations, offce re-locations, and so on, the practice of statistics at Los Alamos has evolved from its origins in the early 1950s, with a handful of statisticians working in LASL group T-1, to present-day group CCS-6. This report chronicles that history.

97 MATHEMATICS AND COMPUTING↗

NASA NTRS1981

Evolution of the atmosphere of Venus

The photochemistry of the stratosphere of Venus was modeled using an updated and expanded chemical scheme, and the results of recent laboratory studies. The model satisfactorily accounts for the observations of CO, O2, (1) and SO2 in the stratosphere. Oxygen, derived from CO2 photolysis, is primarily consumed by CO2 recombination and oxidation of SO2 to H2SO4. Photolysis of HCl in the upper stratosphere provides a major source of odd hydrogen radicals essential for the catalytic oxidation of CO. Oxidation of SO2 by O occurs in the lower stratosphere, with the O-O bond broken by S + O2 and SO + HO2. The sensitivity of stratospheric chemistry to ambient H2 abundance was studied and the model prefers the high value (1 10 ppm) recently inferred from the Pioneer Venus ionospheric measurements. The importance of the photochemical production of S2O, (SO)2, S2, H2S2O2 and H2S2O3 is speculated. A number of previously unsuspected similarities between the chemistry of the stratospheres of Venus and the Earth, presented and discussed.

Yung, Y. L.↗

DOE OSTI2023

Multi-scale modeling of the evolution of structure and properties in materials for nuclear energy applications

Nuclear energy is an important component of an overall strategy to address climate change. Idaho National Laboratory (INL) is the U.S. Department of Energy’s primary facility for research and development in nuclear science and technology for energy generation, supporting the improvement and life extension of the existing reactor fleet and the development and licensing of new reactor designs. Computational modeling is an important component of these activities, particularly in the area of materials for nuclear applications, where experimental data can be very challenging and expensive to acquire, and where data is especially scarce for new reactor designs. INL has used multi-scale modeling – linking atomistic, mesoscale, and engineering scales – to improve the ability to predict the performance of materials for nuclear energy applications. These modeling efforts make extensive of MOOSE (Multiphysics Object-Oriented Simulation Environment), a general-purpose open source finite element framework developed at INL. In this talk, I will give an overview of the approach and tools used, and several examples of application, including performance of nuclear fuels, understanding radiation-driven formation of nanoscale void and gas bubble superlattices, and powder densification through electric field assisted sintering.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Multi-scale modeling of the evolution of structure and properties in materials for nuclear energy applications

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1989

The nitrogen cycle on Mars

Nirtogen is an essential element for the evolution of life, because it is found in a variety of biologically important molecules. Therefore, N is an important element to study from a exobiological perspective. In particular, fixed nitrogen is the biologically useful form of nitrogen. Fixed nitrogen is generally defines as NH3, NH4(+), NO(x), or N that is chemically bound to either inorganic or organic molecules, and releasable by hydrolysis to NH3 or NH4(+). On Earth, the vast majority of nitrogen exists as N2 in the atmosphere, and not in the fixes form. On early Mars the same situations probably existed. The partial pressure of N2 on early Mars was thought to be 18 mb, significantly less than that of Earth. Dinitrogen can be fixed abiotically by several mechanisms. These mechanisms include thernal shock from meteoritic infall and lightning, as well as the interaction of light and sand containing TiO2 which produces NH3 that would be rapidly destroyed by photolysis and reaction with OH radicals. These mechanisms could have been operative on primitive Mars.The chemical processes effecting these compounds and possible ways of fixing or burying N in the Martian environment are described. Data gathered in this laboratory suggest that the low abundance of nitrogen along (compared to primitive Earth) may not significantly deter the origin and early evolution of a nitrogen utilizing organisms. However, the conditions on current Mars with respect to nitrogen are quite different, and organisms may not be able to utilize all of the available nitrogen.

Mancinelli, Rocco L.↗

DOE OSTI2025

Total absorption spectroscopy for the 𝛽 + decay strength distribution of 60 Ga

𝛽-decay properties play an important role in most astrophysical processes. In the absence of experimental data, astrophysical models rely on global theoretical calculations to provide the relevant properties. It is therefore important to provide strong experimental constraints when possible. In the case of 𝛽-decay, the most sensitive probe is the 𝛽-decay strength distribution. We report here on the first measurement of the latter quantity for the 𝛽 + decay of 60 Ga using the total absorption spectroscopy technique. The experimental results are compared to theoretical calculations often used in astrophysical models, namely the shell model and the quasiparticle random phase approximation (QRPA), as well as an extension of QRPA that includes higher-order nucleonic calculations. Both models are in reasonable agreement with the experimental results.

59 ≤ A ≤ 89↗

DOE OSTI2017

Analysis of thermal history effects on mechanical anisotropy of 3D-printed polymer matrix composites via in situ X-ray tomography

The tensile behavior of an additively manufactured (AM) polymer matrix composite (PMC) is studied with in situ X-ray computed microtomography (CT) and digital volume correlation (DVC). In this experiment, the effects of recycled material content and print direction on the selective laser-sintered (SLS) material's mechanical response are explored. The PMC samples are printed in a tensile specimen geometry with gage lengths parallel to all three orthogonal, primary sintering directions. In situ tensile-CT experiments are conducted at Argonne National Laboratory's Advanced Photon Source 2-BM beamline. Analysis of the AM PMC's tensile response, failure, and strain evolution is analyzed both from a conventional standpoint, using the load-displacement data recorded by the loading fixture, and from a microstructural standpoint by applying DVC analysis to the reconstructed volumes. Significant variations on both strength and ductility are observed from both vantages with respect to print direction and the recycled material content in the printed parts. As a result, it is found that the addition of recycled source material with a thermal history reduces the tensile strength of the SLS composite for all directions, but the effect is drastic on the strength in the layering direction.

36 MATERIALS SCIENCE↗

DOE OSTI2025

4D Observations of the initiation of abnormal grain growth in commercially pure Ni

Abnormal grain growth (AGG), where a small fraction of grains grow faster than others, is critical to predict because it can significantly impact material properties. However, the mechanism behind AGG remains unclear. In this study, laboratory-based x-ray diffraction contrast tomography (LabDCT) is employed to non-destructively track the 3D microstructural evolution of high-purity nickel during the onset of AGG at 800 °C. The initial microstructure state is used to test hypothesized microstructure predictors of the initiation of AGG. The change in grain size was not related to the initial grain size or normalized integral mean curvature. Additionally, the grain boundary energy distributions of abnormal grains were indistinguishable from those of control groups exhibiting normal grain growth. However, the grains that later became abnormal exhibit large areas of asymmetric tilt boundaries that were previously found to be fast. This 3D microstructure dataset is useful to investigate new hypotheses for the initiation of AGG.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Hydromechanical impact of basement rock on injection-induced seismicity in Illinois Basin

Abstract The common explanation of observed injection-induced microseismicity is based on the measured stress state at the injection interval and the assumption that it remains the same in the vicinity. We argue here that representing the stress state in different geologic formations over the injection site with the single Mohr’s circle is insufficient due to local stratigraphic features and contrast in compressibilities of the involved formations. The role of hydromechanical coupling in the microseismic response is also crucial for the proper assessment of the problem. Thoroughly monitored Illinois Basin Decatur Project revealed the majority of CO 2 injection-associated microseismic events being originated in the crystalline basement. Even though basement faults can serve as the conduits for fluid flow—the predicted pressure increase seems to be insufficient to trigger seismicity. To address this issue, accurate laboratory measurements of rock properties from the involved formations are conducted. The pre-injection stress state and its evolution are evaluated with the hydromechanically coupled numerical model. It appears that the presence of an offset in a stiff competent layer affects the stress state in its vicinity. Therefore, both the pre-injection stress state and its evolution during the fluid injection should be addressed during the induced seismicity assessment.

54 ENVIRONMENTAL SCIENCES↗