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DOE OSTI2025

Copper-containing layered oxide cathodes for sodium-ion batteries

Layered transition metal oxides are among the most promising cathode materials for sodium-ion batteries due to their high theoretical capacity, structural tunability, and cost-effectiveness. However, conventional Ni- and Co-based layered oxides are hindered by high raw material costs, limited elemental abundance, and phase instability during electrochemical cycling. Recently, copper has emerged as an attractive alternative transition metal, offering significant advantages in terms of redox activity, structural stabilization, voltage regulation, and rate performance. Unlike Ni and Co, Cu can facilitate unique redox mechanisms and enable more sustainable material design. This review systematically summarizes recent progress on Cu-containing layered sodium oxides, with emphasis on their structural characteristics, electrochemical behavior, and the critical roles that Cu plays within the host lattice. The insights provided herein aim to highlight the potential of Cu-substituted or Cu-containing layered oxides as a viable pathway toward high-performance and resource-accessible SIB cathodes for future energy storage applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Index tests for geosynthetic clay liners containing bentonite–polymer composites

The hydraulic conductivity of geosynthetic clay liners (GCLs) containing bentonite–polymer composites (BPCs) is controlled by a pore clogging mechanism related to the swelling of sodium bentonite (NaB) granules and formation of polymer gel in the pore space. Three index testing procedures that are influenced by bentonite swelling and rheology of the polymer gel were evaluated in this study for screening BPC GCLs for hydraulic conductivity: viscosity, liquid limit by fall-cone penetration and active water content. Experiments were conducted using polyacrylamide (PAM) polymer, dry-blended mixtures of PAM and NaB and a BPC from a commercially available GCL. These materials were contacted with inorganic solutions representing leachates from a range of waste containment scenarios. For the BPC that was evaluated, hydraulic conductivities less than 10 -10 m/s were obtained when the viscosity exceeded 220 mPa s and the active water content exceeded 300%. Hydraulic conductivities less than 10 -11 m/s were achieved for viscosity exceeding 350 mPa s, fall-cone liquid limit exceeding 190 and active water content exceeding 300%. Additional testing is needed to assess the generality of these index tests and the identified thresholds when applied to other BPC GCLs and other permeant liquids.

Engineering↗

DOE OSTI2021

Seaborgite, LiNa6K2(UO2)(SO4)5(SO3OH)(H2O), the First Uranyl Mineral Containing Lithium

Abstract Seaborgite (IMA2019-087), LiNa6K2(UO2)(SO4)5(SO3OH)(H2O), is a new mineral species from the Blue Lizard mine, Red Canyon, San Juan County, Utah, U.S.A. It is a secondary phase found on gypsum in association with copiapite, ferrinatrite, ivsite, metavoltine, and römerite. Seaborgite occurs in sprays of light-yellow, long flattened prisms or blades, up to about 0.2 mm in length. Crystals are elongated on [100], flattened on {010}, and exhibit the forms {100}, {010}, {001}, and {101}. The mineral is transparent with vitreous luster and very pale-yellow streak. It exhibits bright lime-green fluorescence under a 405 nm laser. The Mohs hardness is ~2½. The mineral has brittle tenacity, curved or conchoidal fracture, and one good cleavage on {100}. The measured density is 2.97(2) g/cm3. The mineral is immediately soluble in H2O at room temperature. The mineral is optically biaxial (–), α = 1.505(2), β = 1.522(2), γ = 1.536(2) (white light); 2Vmeas = 85(1)°; moderate r < ν dispersion; orientation X ^ a ≈ 10°; pleochroic X colorless, Y and Z light green-yellow; X < Y ≈ Z. EPMA and LA-ICP-MS analyses of seaborgite undermeasured its Li, K, and Na. The empirical formula using Li, Na, and K based on the structure refinement is Li1.00Na5.81K2.19(UO2)(SO4)5(SO3OH)(H2O). Seaborgite is triclinic, P1, a = 5.4511(4), b = 14.4870(12), c = 15.8735(15) Å, α = 76.295(5), β = 81.439(6), γ = 85.511(6)°, V = 1203.07(18) Å3, and Z = 2. The structure (R1 = 0.0377 for 1935 I = 2σI) contains [(UO2)2(SO4)8]4– uranyl-sulfate clusters that are linked into a band by bridging LiO4 tetrahedra. The bands are linked through peripheral SO4 tetrahedra forming a thick heteropolyhedral layer. Channels within the layers contain a K site, while an additional K site, six Na sites, and an SO3OH group occupy the space between the heteropolyhedral layers.

Geochemistry & Geophysics↗

DOE OSTI2020

Status of the Characterization of DEs from the Full Circumference Examination of the Inner Container Closure Weld Region (FY2020)

One of the main focus areas of the 3013 Surveillance Program is a thorough evaluation of the inner container closure weld region (ICCWR) opened for destructive examination (DE). As part of the protocol to investigate the corrosion in the ICCWR a laser confocal microscope (LCM) is used to perform close visual examination of the surface and measurements of corrosion features on the surface. DE containers from FY13 through FY16 were screened with three candidates selected for full circumference evaluation (FCE) according to the ICCWR examination protocol, During the FCE, FY16 DE05 and FY15 DE07 showed suspect major corrosion events, FY16 DE05 Section C2 shows two crack-like features, identified as Denebola and Draco. Both features are located at the boundary of Zone 2 and Zone 3. Consequently, Section C2 of FY16 DE05 was selected for examination by serial metallography at Savannah River National Laboratory (SRNL). For FY15 DE07 the suspect corrosion events were observed on Sections Cl and C2. Section Cl shows one crack-like feature, identified as Acrux. Section C2 shows three crack-like features, identified as Bellatrix, Cursa Minor and Cursa Major. Unlike Acrux and Bellatrix, which are located at the boundary of Zone 2 and Zone 3, Cursa Minor and Cursa Major are located in Zone 2. Sections Cl and C2 of FY15 DE07 were sent to Los Alamos National Laboratory (LANE) for characterization by X-Ray Tomography (XRT).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Wide Area 3D Measurement System for Analysis of 3013 Inner Container Closure Weld Region

One of the main focus areas of the 3013 Surveillance Program is a thorough evaluation of the inner container closure weld region (ICCWR) opened for destructive examination (DE). As part of the protocol to investigate the corrosion in the ICCWR, a laser confocal microscope (LCM) is used to perform close visual examination of the surface and to measure corrosion features on the surface. However, in FY20, the introduction of the Wide Area 3D Measurement System (WAMS) was tested as a method for faster inspection of the ICCWR. Optimization of the WAMS parameters for data collection was carried out using a generic tear-drop type sample containing large and fine Stress Corrosion Cracking (SCC) fractures and high resolution images were compared to the image obtained with the LCM. Although the image with the LCM shows higher resolution than the WAMS images, the small features can be still identified in the WAMS images. The advantage of collecting data for the full circumference using the WAMS is that it can take about a week to complete, which represents 1/16 of the time needed with the LCM. Nonetheless, both systems offer capabilities that combined can be utilized to expedite the examination of the ICCWR. The WAMS can be utilized to obtain images for faster screening or identification of corrosion features on the surface while the LCM can be utilized to obtain higher resolution images of those areas identified by the WAMS.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Filter Test System for Nuclear Container Filters

The purpose of this procedure is to measure the collection efficiency of the filters that are integrated into the lids of containers for nuclear material at Los Alamos National Laboratory (LANL). As an application of this procedure, a filter test report certificate can be created to document the measurement process. This procedure is intended to describe the TA-55, PF-4 (room 6A) operation of a Filter Test System (FTS) for Hagan and SAVY storage containers.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2020

TWF Waste Container Receipt, Inspection and Transfer to Storage

This procedure provides instructions for the receipt, inspection, and transfer to storage of Transuranic (TRU) Waste Containers and Pipe Overpack Containers (POC) within the Transuranic Waste Facility (TWF) (Waste Storage Buildings [WSBs] and Characterization and Waste Storage Building [CWSB]). Performance of this procedure meets the requirements of AC 5.8.9, AC 5.8.13 2nd Bullet, SAC 5.9.1, SAC 5.9.3, SR 4.2.1.1, 4.2.1.2, 4.2.1.5, 4.2.1.6, 4.2.2.1, 4.2.2.2, 4.2.2.3, 4.2.2.4, 4.2.3.1, 4.2.3.2, 4.2.3.3, 4.3.4.1, 4.4.1.1, 4.4.1.2 and 4.4.1.3.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Additively Manufactured Tamper Evident Container (TEC)

Researchers at Los Alamos National Laboratory have developed a tamper evident container (TEC) to secure a broad variety of items from adversarial disclosure and espionage accidents. The new technology uses additive-manufacturing (AM) techniques for the concurrent creation of a container and arbitrarily complex-shaped three-dimensional tamper-sensitive features within its walls that authenticate the package. Analog and encrypted digital boards safely stored inside the TEC permanently record the complete security history of the protected items. Los Alamos is seeking commercial partners interested in further development and engineering prototype work.

42 ENGINEERING↗

DOE OSTI2020

Peer Review Comments on the Authorized Limits Technical Document (OREM-19-2573) for Disposal of Waste Containing Residual Radioactive Material at the U.S. Department of Energy Industrial Landfill IV, Y-12 National Security Complex, Oak Ridge, Tennessee

Argonne National Laboratory is assigned responsibility by DOE/EM-4 to conduct a peer review of the proposed Authorized Limits (ALs) for disposal of waste containing residual radioactive material at the U.S. Department of Energy (DOE) Industrial Landfill IV, Y-12 National Security Complex, Oak Ridge, Tennessee. The ALs document package (Document Number OREM-19-2573, dated May 2020) was sent to Argonne by DOE on June 1, 2020 (Oak Ridge 2020a). Argonne started the review immediately and held several BlueJeans meetings with Oak Ridge and DOE to discuss review comments. The first BlueJeans meeting was June 17, 2020. Oak Ridge presented a briefing of the AL package, followed by discussion of the assumptions, methodology, and parameters used in the analysis. A follow-up BlueJeans meeting was held on June 24, 2020, at which Argonne presented both general and specific review comments in PowerPoint slides. This set of slides - Review Comments on the “Authorized Limits for Disposal of Waste Containing Residual Radioactive Material at DOE Industrial Landfill IV, Y-12 National Security Complex, Oak Ridge, Tennessee” - was then emailed to Oak Ridge and DOE after the BlueJeans meeting on June 24, 2020. A PDF version of this slide set is included as Appendix A.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

Lightning Burnthrough to Containment Breach of 55-Gallon TRU Waste Drums

We investigated by arc-plasma heating the feasibility of attributing inherent lightning protection to 55-gallon DOT 7A, Type A, open head carbon steel drums made of 1.5 millimeter painted carbon steel, designed to protect Department of Energy transuranic nuclear waste. The Sandia Lightning Simulator transferred continuing current in 300 ampere (A), 400 A, and 500 A tests to achieve a 350 coulomb charge transfer and simulate cloud-to-ground lightning attachment to test coupons and 9 drums. A tungsten electrode was placed 0.75 inch from the drums. High-speed photography was recorded to observe the exterior containment breach, or "first light," seen on camera when burnthrough opened a hole in the containment. Sheet metal burnthrough occurred between 18 and 71 coulombs in lid and rolling hoop tests, but 12-gauge closure ring tests did not result in burnthrough, which suggests this feature may provide an inherent air terminal protective feature.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

Selection of 3013 Containers for Field Surveillance (FY 2021 Update)

This Update is the ninth in a series of reports that document the binning and sample selection of 3013 containers for the Field Surveillance program as part of the Integrated Surveillance Program. The last Update was in 2016. This Update documents changes to the binning and changes to the random and engineering judgment samples since 2016. This Update also documents field surveillance activities since 2016 and describes plans to complete random sampling in 2025. In addition, this Update describes a new effort to collect surveillance data as part of down blending operations and updates assumptions about Advanced Recovery and Integrated Extraction System (ARIES) 3013 containers.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Gamma ray analysis of the K2 containers

The K2 containers contain PuO2 with 238 Pu being the most abundant isotope of all plutonium isotopes. The purpose of this analysis is to determine the light element impurities in the PuO2. These light elements can interact with the alpha particles from plutonium decay to release gamma rays, protons, and neutrons through the reactions (α,α’), (α,p), and (α,n) respectively. The gamma rays released by the interactions can be measured and compared with the gamma rays released by the plutonium. The ratios of the gamma rays from the interactions and the plutonium gamma rays allow for the determination of the impurities in the items. The elements that can be detected are Lithium (Z=3), Beryllium (Z=4), Boron (Z=5), Fluorine (Z=9), Sodium (Z=11), Magnesium (Z=12), Aluminum (Z=13), Silicon (Z=14), Phosphorous (Z=15), Chlorine (Z=17), and Potassium (Z=19).

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2022

FY22 Progress on Multicontinuum Methods in Containment

Estimation of two-phase fluid flow properties is important to understand and predict water and gas movement through the vadose zone for agricultural, hydrogeological, and engineering applications, such as containment transport and/or containment of gases in the subsurface. To estimate rock fluid flow properties and subsequently predict physically realistic processes such as patterns and timing of water, gas, and energy (e.g., heat) movement in the subsurface, laboratory spontaneous water imbibition with simultaneous temperature measurement and numerical modeling methods are presented in the FY22 progress report. A multiple-overlapping-continua conceptual model is used to explain and predict observed complex multi-phenomenological laboratory test behavior during spontaneous imbibition experiments. This report primarily addresses two complexities that arise during the experiments: 1) capturing the late-time behavior of spontaneous imbibition tests with dual porosity; and 2) understanding the thermal perturbation observed at or ahead of the imbibing wetting front, which are associated with adsorption of water in initially dry samples. We use numerical approaches to explore some of these issues, but also lay out a plan for further laboratory experimentation and modeling to best understand and leverage these unique observations.

58 GEOSCIENCES↗

DOE OSTI2023

Relative humidity threshold for oxygen generation by high-purity plutonium dioxides in 3013 containers

High-purity plutonium dioxide with adsorbed water in a sealed container can generate oxygen, but oxygen will not be generated in low water loading conditions. A threshold for oxygen generation has been observed in the hydrogen generation rate normalized by the specific power for high-purity plutonium dioxide. Normalized hydrogen generation rates above this threshold generate oxygen and below the threshold consume oxygen. The threshold rate is determined by the amount of water adsorbed onto the surface of the oxide. The relative humidity of the atmosphere that the oxide is in equilibrium with determines the amount of physisorbed water adsorbed on the surface. We calculate the relative humidity corresponding to the threshold rate as a function of mass and specific surface area of material stored in 3013 containers. Exceeding the calculated relative humidity may result in flammable gas mixtures of hydrogen and oxygen at some time during storage.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Mean Time to Failure Analysis for the Los Alamos National Laboratory Weapons Engineering Tritium Facility Tritium Containment Vessels

The Weapons Engineering Tritium Facility (WETF) is a Hazard Category 2 nonreactor nuclear facility located in Technical Area 16 (TA-16) of Los Alamos National Laboratory. Tritium related research, development, and processing in support of stockpile stewardship program activities is conducted at WETF. Within WETF, various devices can be used to contain tritium and certain devices are designated as Tritium Containment Vessels (TCVs). Several different device types are identified as TCVs within WETF such as LP-50s and AL-M1s. Historically, a threshold tritium mass value has been used as the mechanism for designating a device as a TCV. When the tritium content of the device was below the tritium mass threshold it was not considered to be a TCV in the formal context. When the tritium content was above the administrative threshold, the device was considered to be a TCV. An upper tritium mass limit was also established for TCVs.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Technical Basis for Extending Storage Life of DOE-STD-3013 Containers

The U.S. Department of Energy (DOE) Technical Standard for Stabilization, Packaging, and Storage of Plutonium-Bearing Materials, DOE-STD-3013 [USDOE 2018], provides requirements for packaging stabilized metals, alloys, and oxides containing at least 30 weight percent (wt%) plutonium (Pu) plus uranium for storage for up to 50 years. This document provides the technical basis for extending that storage duration to up to 100 years for metals and alloys, and oxides that do not present a corrosion risk to the integrity of the container.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

High-Energy Laser Direct Strike Assessment for NIF CryoXNBS Snout and Naiad SNM Container

An experimental IPT performed two NIF shots as an assessment of the effect of a direct laser beam strike impact on the NIF CryoXNBS snout and Naiad container. Four aligned NIF outer cone beams at best focus, 42 kJ total, struck a four millimeter thick stainless plate. In the first shot, the struck plate was followed by a 1.75 mm gap and a 2.0 millimeter stainless plate to create a surrogate geometry for the current CryoXNBS snout and Naiad container. There was minor plastic deformation of the rear plate rear surface with no evidence of bulk failure. The second shot tested a layered glass-filled polycarbonate and titanium shield placed in the gap. Nondestructive assay was sufficient to metrologize the beam strike area and the damage induced to the NIF target assemblies.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Considerations for Improving the Technoeconomic Viability of Heat Pipe Microreactors by Employing a Functional Containment Approach

The economic cost of a microreactor is being investigated by leveraging MARVEL cost information in conjunction with some simplified design and analysis activities to present a hypothetical, yet feasible, option for investigation. This bottom-up cost estimate for a hypothetical commercial microreactor will be used to provide guidance to the industry and research communities regarding where priorities should be set to improve the viability of broad microreactor deployment. To support the design and analysis activities required to present a feasible option, some understanding of maximum accidental radionuclide releases and consequences is needed to provide bounding estimates on containment or confinement systems for radionuclide retention. To estimate fission product barrier and retention performance, a gaussian plume dose and dispersion model is employed, with isotopic inventories being propagated between barriers assuming conservative fractional release rates. Demonstrably conservative meteorological assumptions are also assumed. Standard reference release rates are assumed where safety requirements could be easily and economically employed. Results are provided in units of total effective dose equivalent as a function of distance from the release (i.e., the reactor). Initial results indicate that the hypothetical microreactor will likely need to credit the fuel cladding and at least one other barrier, or combination of barriers, to ensure public health and safety as required during a postulated accident. This approach is referred to as “functional containment,” since no single barrier will be relied upon for satisfying regulatory requirements and fundamental safety functions for radionuclide retention. Finally, a set of barrier options are provided so that future economic analyses can select the most viable design path.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗