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At least 127 records · Page 7

Technical Basis Update for the Design Life Extension of the SAVY-4000® Series of Containers

This technical basis update focuses on the design life of the SAVY-4000® (hereafter “SAVY”) series of nuclear material storage container (e.g., used to store, transport, and handle special nuclear material outside of a glovebox), previously approved under DOE Manual 441.1-1, Nuclear Material Packaging Manual. The SAVY is approved for storing all authorized contents for a period of 15 years. The lifetime extension technical basis is established on the compiled technical data from the on-going SAVY and Hagan surveillance programs, destructive analysis results, accelerated aging studies, and performance testing, in line with the regulatory rigor of DOE M441.1-1.

42 ENGINEERING↗

Setup for Optical Absorption Measurements of Molten Salt Mixtures

In this work we describe the setup of a spectrophotometer to take absorbance measurements of a heated sample in an inert atmosphere. By using fiber optics to bring light into and out of a glovebox we are able to use a pitch-catch optical setup to observe samples in a cuvette heated up to 400℃. The functionality of the setup is demonstrated by observing the signal produced by Li 2 S in a eutectic mixture of LiCl/LiBr/KBr at elevated temperature overtime.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Water-Resistant Container Testing: A426-7, A426-25, and A426-50 Container Designs

The purpose of this report is to detail the results of water ingress testing conducted on the A426-7, A426-25, and A426-50 Mini-Pot container designs and discuss these results against the water-resistant container requirements of TA55-AP-522 and PA-RD-01009. The A426 design series is a proposed commercially off the shelf inner container option for material storage inside of a glovebox and/or as an approved nonhermetically sealed inner of an approved packaging configuration inside of an approved outer container as listed in PA-RD-01022. The A426-25 and A426-50 are shaped similar to an ointment jar, made of 316L stainless steel, and utilize a threaded lid for closure and containment. The A426-7 container is shaped similar to a vial, made of 316L stainless steel, and utilizes a threaded lid for closure and containment. See Figure 1 and Table 1-3 for a summary of the container specifications. For more details on the container design, see Section 1.4.

42 ENGINEERING↗

Development of PNNL’s Plutonium Metallography Capability

The goal of this project was to develop plutonium metallography capabilities and establish workflows for characterization at PNNL’s Radiological Processing Facility (RPL). Developing and expanding on this capability opens more opportunities for PNNL to better support science through collaborations with other labs, plants, and sites withing the Department of Energy Complex and through programs within the National Nuclear Security Administration. This project established metallography equipment in an air glovebox, polishing protocols, as well as radiological and facility controls and procedures so that gram quantities of plutonium metal could be analyzed on multiple characterization tools. Data was collected and analyzed on two different delta phase plutonium - Gallium samples and a calciothermically reduced alpha plutonium metal using a combination of optical and electron microscopy, powder X-ray diffraction, and atom probe tomography. This report highlights the metallography capabilities, some preliminary data collections, and plans at PNNL to support plutonium material science.

36 MATERIALS SCIENCE↗

Crossroads of Nonproliferation and Safeguarding Technologies for Implementation in Molten Salt Reactors

Idaho National Laboratory (INL) recently conducted a workshop endorsed by the National Nuclear Security Administration (NNSA) under the auspices of the Defense Nuclear Nonproliferation R&D (DNN R&D) Office's Safeguards Portfolio. The workshop's primary objective was to foster an engaging dialogue among researchers, with a specialized emphasis on the safeguards pertaining to molten salt reactors. At INL, the installation of the state-of-the-art Molten Salt Thermophysical Examination Capability (MSTEC) is underway. This shielded argon glovebox facility, designed for both irradiated and non-irradiated actinide materials, represents the cutting edge of research infrastructure. MSTEC is poised to serve as a pivotal research platform in the realm of molten salt technology, with significant implications for safeguards applications. Participants of the workshop had the opportunity to tour the facilities, including the site where MSTEC is being installed, as well as to observe the INL's molten salt and pyroprocessing research hot cells. The event featured insightful presentations delving into molten salt chemistry and the MSTEC project. Each participating laboratory contributed to the discourse with presentations on their respective research efforts addressing safeguards in relation to molten salt reactors. The workshop culminated with a generative brainstorming session, where participants shared their thoughts on strategic integration with partner agencies, aiming to synergize efforts in advancing the field of nuclear safeguards.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Development and Implementation of a Bag Degradation Predictive Tool at Los Alamos National Laboratory

Nuclear material packaging involves many complex variables derived from the stored material's properties, the storage environment, and the synergistic interaction of said material and its environment on the containment boundary. In the Plutonium Facility (PF-4) at Los Alamos National Laboratory (LANL) the typical containment boundary found, starting from the stored material itself to the outermost containment layer, consists of the material contained within a stainless steel (typically 304) slip-lid (or other equivalent stainless steel packaging layer) wrapped in an sPVC bag-out bag contained within a facility approved outer container stored within the boundaries of an approved facility (i.e., a building designed and approved to store nuclear material). This packaging configuration, though occasionally deviated from in the past, represents the current procedurally enforced, expected containment structure for all interim nuclear material containment outside of an engineered control barrier (e.g., a glovebox). Over the life of containerization research at LANL, packaging engineers have become increasingly concerned with the degradation of the sPVC bag-out bag, which can cause corrosion to the outermost packaging layer as well as possible exposure to alpha contamination if the bag-out bag layer is degraded to the point of containment failure. A bag-out bag degradation predictive tool (BDT) is therefore needed to assess the current and future nuclear material inventory for possible bag degradation in order to continue to ensure safe operations for the facility and its workers to deliver on the vital national security mission of 30 PPY.

42 ENGINEERING↗

Identifying the speciation of salt-based actinides in the presence of contaminants [Slides]

Molten salt reactors (MSR) present advantages over light water reactors, such as higher safety and energy efficiency, convenient waste processing, and the ability to use more abundant thorium instead of uranium as the fuel source. However, due to the high temperatures associated with these reactors the reactor container corrosion product can have a high influence on the molten salt system, and they are considered as a part of the fuel salt system. It is essential to have a comprehensive understanding of the chemical reactions that are occurring in the molten salt in the presence of contaminants such as nickel, manganese, chromium chlorides and oxides. Because they can change the local structure of these salts and the local structures of these salts govern the thermophysical properties of the molten salts, which would determine the safety and operational parameters of the reactor. This study is focused on identifying f-element materials speciation resulting from reaction with corrosion/degradation products in a molten salt environment to understand the flow of MSR. In this work, f-element chlorides are mixed with alkali and alkali earth metals and corrosion products such as transition metal chlorides are introduced systematically, inside a glovebox. Then these are heated to around 700 ? and slowly cooled to room temperature. Afterwards, these are analyzed using different characterization techniques such as powder X-ray diffraction, UV-vis and Raman spectroscopy and solid-state NMR. The initial work was conducted with lanthanide chlorides as a surrogate for actinides and the acquired data strongly indicates that in the presence of corrosion products new phase formation/ change in coordination environments occurs. This work has been presented at multiple conference presentations. The proposed work would allow to extend this work to actinides (depleted uranium and thorium) and this would assist to identify the speciation of actinide chloride in the presence of corrosion products. Also, this work would open an opportunity to compare the coordination behavior of lanthanides with the actinides.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗

Moisture Stability of Sulfide Solid-State Electrolytes

In this report we detail a comprehensive study on the moisture stability of sulfide solid-state electrolytes in dry room environments. Although sulfide SSEs have many favorable attributes, this class of materials suffers from poor stability with water. Sulfide SSEs react with water to form gaseous H 2 S and a variety of solid byproducts like Li 3 PO 4 and LiOH, which go on to increase the interfacial impedance of solid-state batteries. Lab-scale research typically utilizes gloveboxes with <1 ppm water, however, the large-scale manufacturing of Li-ion batteries occurs in –40°C dewpoint dry rooms with around 126 ppm water. Consequently, the moisture stability of sulfide SSEs must be addressed if the manufacture of solid-state batteries based on sulfide SSEs is to be scaled up. Here, we are the first to characterize the moisture stability of sulfide SSEs according to both H 2 S and the degradation of ionic conductivity at different moisture setpoints ranging from –76°C to –40°C dewpoint. A variety of different SSE compositions are studied; namely, (Li 2 S) 75 (P 2 S 5 ) 25 , (Li 2 S) 70 (P 2 S 5 ) 30 , (Li 2 O) 7 (Li 2 S) 68 (P 2 S 5 ) 25 , (Li 2 O) 7 (Li 2 S) 63 (P 2 S 5 ) 30 , and (Li 2 S) 75 (P 2 S 5 ) 25 + 20 mol% LiI. We find that moisture stability improves with 75 mol% Li2S modifier content and the introduction of a Li 2 O co-modifier. After a 30 min exposure in a –40°C dewpoint dry room environment we found that (Li 2 S) 75 (P 2 S 5 ) 25 + 20 mol% LiI powder generated 0.1 cc/g H 2 S and its ionic conductivity decreased by over 50%. However, when SSE powder was exposed as a slurry in a dodecane carrier the same SSE composition generated 0 cc/g H 2 S and its ionic conductivity only dropped by 14%. Our results show that sulfide SSEs have acceptable moisture stability when appropriately processed in a dry room environment.

25 ENERGY STORAGE↗

Scalable and Quench-Free Processing of Metal Halide Perovskites in Ambient Conditions

With the rise of global warming and the growing energy crisis, scientists have pivoted from typical resources to look for new materials and technologies. Perovskite materials hold the potential for making high-efficiency, low-cost solar cells through solution processing of Earth-abundant materials; however, scalability, stability, and durability remain key challenges. In order to transition from small-scale processing in inert environments to higher throughput processing in ambient conditions, the fundamentals of perovskite crystallization must be understood. Classical nucleation theory, the LaMer relation, and nonclassical crystallization considerations are discussed to provide a mechanism by which a gellan gum (GG) additive—a nontoxic polymeric saccharide—has enabled researchers to produce quality halide perovskite thin-film blade coated in ambient conditions without a quench step. Furthermore, we report on the improved stability and durability properties inherent to these films, which feature improved morphologies and optoelectronic properties compared to films spin-coated in a glovebox with antisolvent. We tune the amount of GG in the perovskite precursor and study the interplay between GG concentration and processability, morphological control, and increased stability under humidity, heat, and mechanical testing. The simplicity of this approach and insensitivity to environmental conditions enable a wide process window for the production of low-defect, mechanically robust, and operationally stable perovskites with fracture energies among the highest obtained for perovskites.

14 SOLAR ENERGY↗

Optimizing Magnetic Force Microscopy Resolution and Sensitivity to Visualize Nanoscale Magnetic Domains

Magnetic force microscopy (MFM) enables mapping local magnetic fields across a sample surface with nanoscale resolution. To perform MFM, an atomic force microscopy (AFM) probe whose tip has been magnetized vertically (i.e., perpendicular to the probe cantilever) is oscillated at a fixed height above the sample surface. The resultant shifts in the oscillation phase or frequency, which are proportional to the magnitude and sign of the vertical magnetic force gradient at each pixel location, are then tracked and mapped. Although the spatial resolution and sensitivity of the technique increases with decreasing lift height above the surface, this seemingly straightforward path to improved MFM images is complicated by considerations such as minimizing topographical artifacts due to shorter range van der Waals forces, increasing the oscillation amplitude to further improve sensitivity, and the presence of surface contaminants (in particular water due to humidity under ambient conditions). In addition, due to the orientation of the probe's magnetic dipole moment, MFM is intrinsically more sensitive to samples with an out-of-plane magnetization vector. Here, high-resolution topographical and magnetic phase images of single and bicomponent nanomagnet artificial spin-ice (ASI) arrays obtained in an inert (argon) atmosphere glovebox with <0.1 ppm O 2 and H 2 O are reported. Further, optimization of lift height and drive amplitude for high resolution and sensitivity while simultaneously avoiding the introduction of topographical artifacts is discussed, and detection of the stray magnetic fields emanating from either end of the nanoscale bar magnets (~250 nm long and <100 nm wide) aligned in the plane of the ASI sample surface is shown. Likewise, using the example of a Ni-Mn-Ga magnetic shape memory alloy (MSMA), MFM is demonstrated in an inert atmosphere with magnetic phase sensitivity capable of resolving a series of adjacent magnetic domains each ~200 nm wide.

47 OTHER INSTRUMENTATION↗

Benchtop-Scale High Temperature Molten Salt Electrochemical Reactors: Experimental Setup and Considerations

Molten salt electrochemical reduction (MSER) is the dominant production method for aluminum and titanium, and emerging technologies for producing other commodity metals with these highly electrified techniques have demonstrated promising results. However, the scale up of MSER of materials such as iron and silicon are limited by the challenging issues of materials compatibility and impurity control. This work describes an experimental MSER setup using both chloride and carbonate salts. This setup is designed for operations outside of a glovebox, which is practical from an industrial perspective, but creates unique challenges. This work serves as a practical guide to discuss some key operational difficulties such as temperature control, air and humidity, material compatibility, developing strong electrical measurements and techniques, and safety.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tritium cleanup system and method

Work area cleanup systems and methods are described for removing tritium from the atmosphere of a work area such as inert gas gloveboxes. Systems utilize a multi-column approach with parallel processing. Tritium of a tritium-contaminated stream is converted into tritiated water and adsorbed onto the separation phase of a first column as a second, parallel column can be simultaneously regenerated. The gaseous stream that exits the column during the regeneration phase can carry a high tritium concentration. The system can also include and a separation stage during which the tritium of the gaseous regeneration stream can be separated from the remainder of the regeneration product.

Xiao, Xin↗

Resource loading system and method for use in atmosphere containment scenarios

The invention provides a system for preventing fluid exchange between the interior and exterior of containment enclosures such as process-, hazard-, and research-enclosure systems generally, gloveboxes, containment systems, isolation systems, confinement systems, cleanrooms, negative air systems, and positive air system areas while simultaneously providing material transfer into and out of the enclosures. The invention also provides a method for transporting material into or out of a containment structure.

Dilday, Jr., Daniel R.↗

Developing a New Criticality Safety Hands-On Training Utilizing ZPPR Plates

Nuclear criticality safety is an extremely important part of the work at Los Alamos National Laboratory (LANL). As part of the work LANL performs to continue to keep criticality safety a top priority, LANL has developed and regularly teaches nuclear criticality safety training classes for both the United States Department of Energy Nuclear Criticality Safety Program as well as internal trainings for LANL employees. A portion of the training classes is comprised of hands-on demonstrations, where students get the opportunity to handle special nuclear material at the National Criticality Experiments Research Center (NCERC). One hands-on demonstration uses the “Class foils,” thin HEU foils which are stacked with lucite moderator plates. A hand-stack is performed until the multiplication reaches the “three-quarters rule,” where the demonstration is continued remotely on a vertical lift assembly up until the system is critical. This hands-on demonstration eventually achieves a critical configuration and follows the ANS-1 guidelines on an approach to critical. Another hands-on demonstration involves handling clad plutonium and neptunium spheres, and follows procedures using criticality safety evaluations to ensure that the hands-on demonstrations remain subcritical.This hands-on demonstration also involves the use of polyethylene shells around the plutonium sphere to demonstrate how additional reflector increases the criticality of a system. This paper is focused on developing a new hands-on demonstration using Zero Power Physics Reactor (ZPPR) plates. This new hands-on demonstration will follow the ANS-8 standards as it is not desired to achieve criticality with the ZPPR plates during the hands-on demonstration. A hands-on demonstration using multiple plutonium parts will likely be more applicable to personnel who handle plutonium on a daily basis, such as LANL glovebox operators.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Removal of Bond Sodium from Full-Length Unirradiated Fermi-1 Blanket Elements and Assembly via Melt-Drain-Evaporate Process

Equipment was designed, fabricated, tested, and operated in an inert atmosphere radiological glovebox at Idaho National Laboratory to demonstrate the removal of bond sodium from full-length unirradiated Fermi-1 radial blanket elements and an entire radial blanket assembly using a Melt-Drain-Evaporate process. A series of three runs was performed with individual and multiple radial Fermi-1 blanket elements, and a fourth run was conducted with an entire Fermi-1 radial blanket assembly. After each run, the depleted uranium alloy slugs in every element slid out of its cladding, mechanically exhibiting the effectual absence of bond sodium. Quantitative and further qualitative analyses of the treated Fermi-1 material revealed the substantive, if not complete, absence of sodium metal in blanket element components. Indeed, entire columns of depleted uranium alloy slugs and associated cladding from select treated elements were separately contacted with water to react with residual sodium metal on the element surfaces, forming hydrogen gas. Samples of the resultant gas were analyzed to quantify the hydrogen concentration, which correlated to a residual sodium metal content for the treated element. Accordingly, no detectable sodium metal (<7 µg) was found on the surfaces of multiple depleted uranium alloy slugs after removal from its cladding. Detectable sodium metal, ranging from 14 to 30 µg, was found on the surfaces of one separated column of slugs and two separated full-length cladding segments. Each element originally contained ~25 g of bond sodium, resulting in quantitative sodium metal removal efficiencies of =99.9998%. The remaining separated uranium alloy slugs and cladding segments from the four runs were piece-wise immersed in alcohol while videorecording possible gas bubble formation as an additional qualitative analysis for residual sodium metal on treated surfaces, which identified the predominant absence of sodium reactivity on the balance of treated Fermi-1 blanket material. The results of this demonstration substantiate a path forward for treatment and disposal of 34 metric tons heavy metal of irradiated sodium-bonded Fermi-1 blanket material currently stored at Idaho National Laboratory.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

3D Source Reconstruction Using Coded Aperture Gamma-Ray Imaging

Recent measurements with coded-aperture imagers demonstrate material mass determination in a holdup setting to an accuracy within a few percent. This capability is of particular interest to the Surplus Plutonium Disposition (SPD) project, which aims to dilute and dispose of surplus plutonium oxide. Gamma-ray imagers can be used to determine holdup without interrupting normal operations. In this work, we examine techniques for 3D source localization and mass determination using gamma-ray imagers. Coded-aperture imagers provide excellent source localization within the 2D image plane; however, multiple imagers operating in tandem are necessary to identify source location in 3D space. A Maximum Likelihood Expectation-Maximization (MLEM) method for fitting detector mappings is a powerful tool for accomplishing this task. MLEM allows 3D source localization to be simultaneously constrained using multiple gamma-ray imagers by constructing the basis for the MLEM fit using detector mappings from different detector locations stitched together. Each of these basis points represents a singular response from a source in 3D space and is generated using Monte Carlo simulations of sources placed individually at different locations throughout the imager’s field of view. Additionally, implementing knowledge of the physical equipment in the simulations of the glovebox used for the SPD project incorporates attenuation effects that are needed to calculate material holdup.

Laminack, Alex↗

CHALLENGES IN THE DEVELOPMENT OF THE ELECTROREFINING PROCESS AT Y-12

In order to ensure future capabilities of the Y-12 site as older buildings retire, a new process was developed, the Metal Purification Process. The purpose of this new process is to provide a simpler and more efficient uranium metal purification that the previous multi-staged, complex chemical processes. The basis for this technology currently exists in the US DOE complex, but it has not been utilized on a large scale for uranium at higher enrichments. The system requires larger-geometry vessels and furnaces in order to meet the through-put requirements. The crux of the process is the electrorefining cell, consisting of several concentric liners and an unfavorable geometry cylindrical crucible. Within the crucible, a molten Li-CL-KCL-UCL3 salt electrolyte is present. ‘Dirty’ metal is placed into a loading basket and loaded into an electrorefining cell. Here, the metal reacts into the molten salt within the cell to form UCL3, while ‘clean’ metal simultaneously plates out from the salt electrolyte in the form of metal dendrites. These dendrites are then collected and removed from the cell. After removal from the cell, the dendrites are taken to a furnace to remove adhered salts. Then, the salt-free dendrites are moved to a separate furnace for consolidation into the final product form. The development of the Criticality Safety Evaluation for this complex system brought with it many NCS Challenges and lessons learned. These challenges include: design decisions for ensuring subcriticalty in the electrorefining cell during abnormal conditions, the interface of the main glovebox system with auxiliary systems such as the purification system and designated storage, implementation of mass tracking, and concerns from production and operation regarding the movement of material within the system.

36 MATERIALS SCIENCE↗

SR23012, A Pragmatic Approach to Laser Drilling and Rewelding of Fill Stems, SRNL-TR-2023-00551

The current approach to disposing unloaded reservoirs is to snap the remaining stem, and seal the hole with JB weld, a two-part epoxy mix that is messy to work with and that takes many hours to ensure it is property cured. During this time, reservoirs may be outgassing and cause higher than desired activity in the glovebox. This project will develop, characterize, and deploy a method to drill stems to unload the reservoirs (already in use in the facility, but may require some simple process / procedure modifications), demonstrate that the reservoirs are fully unloaded, and reweld stems by returning to the unloading station and firing the laser to weld the unloading hole closed.

Korinko, Paul S.↗