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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Long-Term 13 C Uptake by 12 C-Enriched Calcite

Knowledge of the exchange of carbon isotopes between dissolved inorganic carbon and calcite minerals is of long-standing importance for the interpretation of sedimentary paleoclimate records and 14 C transport in the geosphere. To assess the mechanism and rates of carbon isotope exchange, we equilibrated 12 C-pure synthetic calcite particles in water, first in a glovebox and then in contact with atmospheric P CO 2 and 13 C/ 12 C ratio, at two different temperatures. Cavity ring-down infrared spectroscopy δ 13 C measurements of the solid revealed sustained 13C incorporation for over a period of 500 days (21 °C) and 125 days (50 °C). We developed a quantitative model for recrystallization and isotope exchange, assuming that the interfacial free energy provides a thermodynamic driving force for the growth of larger particles at the expense of smaller ones. Furthermore, this Ostwald ripening model did not reproduce the kinetics of 13C uptake and required greater coarsening than observed. Rather, the data were best explained by a mechanism involving surface exchange and solid-phase diffusion of 13C into the particles with an inferred effective diffusion constant at 21 °C of about 10 –25 m 2 /s. Although this work cannot rule out the possibility that structural or chemical aspects of the synthetic particles enabled faster 13 C uptake than could be observed in natural systems, this study adds to the body of the recent work, suggesting that fast exchange processes are possible, likely through grain boundaries and other defects.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Investigating dry room compatibility of sulfide solid-state electrolytes for scalable manufacturing

All-solid-state batteries (ASSBs) are viewed as promising next-generation energy storage devices, due to their enhanced safety by replacing organic liquid electrolytes with non-flammable solid-state electrolytes (SSEs). The high ionic conductivity and low Young's modulus of sulfide SSEs make them suitable candidates for commercial ASSBs. Nevertheless, sulfide SSEs are generally reported to be unstable in ambient air. Moreover, instead of gloveboxes used for laboratory scale studies, large scale production of batteries is usually conducted in dry rooms. Thus, this study aims to elucidate the chemical evolution of a sulfide electrolyte, Li 6 PS 5 Cl (LPSCl), during air exposure and to evaluate its dry room compatibility. When LPSCl is exposed to ambient air, hydrolysis, hydration, and carbonate formation can occur. Moreover, hydrolysis can lead to irreversible sulfur loss and therefore LPSCl cannot be fully recovered in the subsequent heat treatment. During heat treatment, exposed LPSCl undergoes dehydration, decomposition of carbonate species, and reformation of the LPSCl phase. Lastly, LPSCl was found to exhibit good stability in a dry room environment and was subject to only minor conductivity loss due to carbonate formation. The dry room exposed LPSCl sample was tested in a LiNi 0.8 Co 0.1 Mn 0.1 O 2 |LiIn half-cell, exhibiting no significant loss of electrochemical performance compared with the pristine LPSCl, proving it to be compatible with dry room manufacturing processes.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Navigating the Path to Autonomy: Real-World Lessons from an Air-Free Self-Driving Laboratory

While autonomous experimentation has promise to accelerate discovery in physcial sciences, the real-world integration of predictive models and experimentation is non-trivial. Here we describe the genesis of a self-driving laboratory (SDL) for air-sensitive chemistry at Argonne National Laboratory and demonstrate the experimental design considerations needed for high-throughput experiments before predictive models can lead to scientific discovery. Our SDL was designed to explore battery electrolyte stability. Our final SDL utilized plate readers in a glovebox with a nitrogen atmosphere to perform kinetic assays and screen hundreds of battery-relevant solvents. However, the roadmap to autonomy and airfree-friendly experimentation required the complex evaluation of several spectroscopic and chromatographic methods. The greatest experimental challenges were (a) developing long-term sampling methods that remained air-free; (b) accelerating kinetics to advance reactivity projections; and (c) ensuring labware compatibility with nonaqueous solvents used in battery chemistry. Our experiences highlight the practical gap between closed-loop aspirations and the realities of chemical discovery, offering lessons on the challenges of transferring every day laboratory workflows to autonomy. These results suggest a more realistic blueprint for autonomy in chemistry—one that balances thoughtful and realistic experimental formulation.

Robertson, Lily A.↗
DOE OSTI2022

Observation of the surface layer of lithium metal using in situ spectroscopy

In this work, we have investigated the surface of lithium metal using x-ray photoemission spectroscopy and optical spectroscopic ellipsometry. Even if we prepare the surface of lithium metal rigorously by chemical cleaning and mechanical polishing inside a glovebox, both spectroscopic investigations show the existence of a few tens of nanometer-thick surface layers, consisting of lithium oxides and lithium carbonates. When lithium metal is exposed to room air (~50% moisture), in situ real-time monitoring of optical spectra indicates that the surface layer grows at a rate of approximately 24 nm/min, presumably driven by an interface-controlled process. Our results hint that surface-layer-free lithium metals are formidable to achieve by a simple cleaning/polishing method, suggesting that the initial interface between lithium metal electrodes and solid-state electrolytes in fabricated lithium metal batteries can differ from an ideal lithium/electrolyte contact.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Synthesis routes to eliminate oxide impurity segregation and their influence on intergrain connectivity in K-doped BaFe 2 As 2 polycrystalline bulks

The poor reproducibility of intergrain critical current density $J_c$ in Fe-based superconductors is often believed to result from uncontrolled grain boundary (GB) connectivity degraded by extrinsic factors such as the local or global impurity concentration or GB porosity or cracks. Earlier we found that Ba and K can appear as oxide impurities at GBs, along with GB-wetting FeAs. In this study, we evaluated how the sample preparation environment and purity of the starting materials influence the polycrystalline $J_c$ in K-doped BaFe 2 As 2 (Ba122) bulks. Using a high-performance glovebox, the oxygen and water levels were significantly reduced, eliminating traces of FeAs. We report oxide impurities and Ba (or K) segregation associated with oxygen in the starting materials were significantly reduced by using high purity starting materials. This combination essentially doubled the best $J_c$(4.2 K) values to 2.3 × 10 5 at self-field and 1.6 × 10 4 A cm –2 at 10 T and analytical scanning transmission electron microscopy showed no GB or O segregation in the best samples, but did show dark Z-contrast and distinct nanoscale porosity. Our work shows that an inert synthesis environment and high purity K and Ba do reduce current-blocking oxygen impurity and GB impurity phases, allowing deeper exploration of the role of extrinsic and intrinsic GB blocking effects in controlling the $J_c$ of polycrystalline Ba122.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Chelation Model Validation: Modeling of a Plutonium-238 Inhalation Incident Treated with DTPA at Los Alamos National Laboratory

Accidental inhalation of plutonium at the workplace is a non-negligible risk, even when rigorous safety standards are in place. The intake and retention of plutonium in the human body may be a source of concern. Thus, if there is a suspicion of a significant intake of plutonium, medical countermeasures such as chelation treatment may be administered to the worker. The present work aimed to interpret the bioassay data of a worker involved in an inhalation incident due to a glovebox breach at Los Alamos National Laboratory’s plutonium facility. The worker was treated with intravenous injections of calcium salts of diethylenetriaminepentaacetic acid (DTPA) in an attempt to reduce the amount of plutonium from the body and therefore reduce the internal radiation dose. It is well known in the internal dosimetry field that the administration of chelation treatment poses additional challenges to the dose assessment. Hence, a recently developed chelation model was used for the modeling of the bioassay data. The objectives of this work are to describe the incident, model the chelation-affected and non-affected bioassay data, estimate the plutonium intake, and assess the internal radiation dose.

238Pu↗
DOE OSTI2020

Pressurization Analysis for Heating of a Screw Top Utility Can Loaded With Plutonium Oxide Powder by a 1273 K Fire

The documented safety analysis for the Savannah River National Laboratory (SRNL) evaluates the consequences of a postulated 1273 K fire in a glovebox. The radiological dose consequences for a pressurized release of plutonium oxide powder during such a fire depend on the maximum pressure that is attained inside the oxide storage containers. The oxide storage configuration selected for analysis is can/bag/can, comprised of oxide powder inside an 8.38 × 10 -6 m 3 stainless steel B vial inside 0.006 kg of polyethylene bagging inside a one-quart screw top utility can of the type commonly used to package solvents or rubber cements. To enable evaluation of the dose consequences, temperature and pressure transients have been calculated for exposure of a typical set of storage containers to the fire. The pressurization analysis credits venting to and from the B vial but does not credit venting or leakage from the can. Due to the low rate of venting from the B vial into the can gas space, the can pressure is nearly independent of the B vial pressure. Calculated maximum pressures are compared to the utility can burst pressure. In lieu of a structural analysis of the utility cans, burst pressures and leakage rates were measured using compressed nitrogen gas. The measured gauge burst pressure was 0.250 ± 0.043 MPa. The measured burst pressures are lower than the calculated maximum pressure due to fire exposure, indicating that the utility cans could burst during exposure to a 1273 K fire.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2024

Radiation Monitoring for Volatilized Zinc Contamination Using Gamma-Ray Imaging and Spectroscopy

Gamma-ray imaging is a tool that has grown in importance in the applications of non-destructive assay (NDA) for radioactive survey and analysis of nuclear facilities. Imaging techniques have shown great promise in providing valuable information involving radioactive waste management and contamination prevention. For the application studied in this work, 65 Zn has been identified as a radioactive contaminant during tritium extraction. Due to the volatile nature of 65 Zn under the pressure and temperature changes during extraction operations, 65 Zn can easily travel through components of the extraction system as vapor, making it difficult to trap. Previous research involving the development of a filtration system showed that the 65 Zn can be trapped, mitigating product contamination. However, during the extraction process, direct analysis of the equipment to confirm that zinc contamination is trapped in the filter and has not spread to other components is impractical. Here, in this situation, the need to assay the location of the contamination with little-to-no interference with operations is vital. In this work, we demonstrate the use of a commercialized 3D position-sensitive CdZnTe (CZT) gamma-ray imaging spectrometer to provide analysis of the 65 Zn contamination. Onsite measurements during an extraction process are studied to assess the location and migration of the 65 Zn. The results obtained from real-time glovebox monitoring demonstrate the feasibility of gamma-ray imaging for localizing the contamination and providing a preliminary qualitative assessment that is intended to be used in future work quantifying the contamination build-up and activity over time.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

How To Maintain Effective IAEA Safeguards While Reducing Facility Impact

For almost twenty years, inspectors from the International Atomic Energy Agency have been visiting the K-Area Material Storage facility at the Savannah River Site where excess plutonium has been placed under IAEA safeguards as part of the United States Volunatary Offer Agreement. During that time, the mission of K-Area Complex has expanded from storage of nuclear matieral to glovebox operations in support of the National Nuclear Security Administration’s Plutonium Disposition program. With this change in mission, it is becoming increasingly challenging to manage facility staff radiation exposure and operating activities during the IAEA’s annual Physcial Inventory Verifications (PIV). This study has identified both near-term and long-term recommendations for IAEA monitoring protocols that would allow the IAEA to maintain effective safeguards of the material while decreasing the impact to the facility. A statisitical analysis has shown that reducing the number of containers measured during an annual PIV from 12 to 4 still ensures a high level of confidence in the confidence while reducing the inspector time in the facility amd with a corresponding significant reduction in personnel radiation exposure. A modified installation pattern of Remotely Monitored Sealing Arrays (RMSAs) is also proposed utilizing only the outer rows of arrays of stored material containers in the Stack Area (SA). The modified RMSA placement will provide equivalent protection, while significantly reducing personnel radiological exposure, manpower requirements and associated costs. With advances in technology, there are additional potential options in containment/surveillance and continuity of knowledge that would allow the agency to be outside of the facility during PIV measurements and have confidence in the accuracy and authencitity of the results.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2020

Physical Sciences Vistas Issue 2, 2020

Dedication and collaboration accelerate mission-essential LANSCE isotope production; Rigorous operations result in newly outfitted gloveboxes; Continuous improvements deliver high-value subcrit data; 'Magnet surge’ expands capabilities for higher tesla science.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2020

Evaluation of the Performance of the SAVY Container Subjected to Various Impact Events using Finite Element Methods

The SAVY container is a Safety Class Design Feature utilized both inside engineered features and outside engineered features (e.g. gloveboxes) at TA-55 Plutonium Facility Building 4. These containers were certified as low damage ratio containers by demonstrating their ability to retain material after exposure to impacts and elevated temperatures resulting from a design basis seismic event. Original testing of the SAVY did not evaluate the effects of various facility specific insults to the SAVY while within a DOT Type A Container, caused either by design basis accident or an operational mishap. These insults include: 1. Impact of a structural I-beam (drum upright & drum on side); 2. Impact of a section of Positive Pressure Chilled Water Pipe (PPCWS); 3. Forklift fork tine impact; 4. Fuel truck impact. Abaqus Explicit Dynamics Finite Element Analysis was performed on a nested SAVY/DOT Type 7A container configuration to assess the structural integrity of the SAVY under the accident conditions listed.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2020

Tritiated Water Disposition Strategies

Tritium, a radioactive isotope of hydrogen, is typically confined within one or more confinement barriers. Tritium readily reacts with oxygen to form tritiated water or can exchange with protium or deuterium atoms in water to create tritiated water which is around 10,000 times more toxic than elemental tritium. Primary tritium confinement systems can create small volumes of highly tritiated water. Secondary confinement systems, like inert gloveboxes, will produce larger volumes of lower concentration tritiated water. Much larger volumes of tritiated water of very low tritium content are produced by tritium permeation/diffusion. Tritium from inside primary and secondary confinement barriers will diffuse from these systems into cooling water systems. Closed loop, recirculating cooling water systems will slowly accumulate tritium and create concentrations which exceed drinking water (or permitted discharge) concentrations. The cooling water systems designed as series of interconnected cooling loops that can slowly transfer tritium from one cooling loop to another cooling loop through heat exchangers. These large volumes of tritiated water may be above federal discharge limits and also lack convenient disposition pathways. This document will discuss tritiated water management strategies from the perspective of large volume, low tritium concentrations that exceed drinking water or permitted discharge limits. Applicable US regulatory requirements for a Molybdenum-99 (Mo-99) production facility concerning tritiated water are also cited. Tritiated water disposition options, based on typical waste minimization strategies will guide dispositions options. A Case Study example is presented to illustrate the pros and cons of several disposition options. The report does not recommend any particular disposition pathway but discusses strategies to be explored by a producer to guide selection of processes which best fits the needs of a particular waste stream.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

PDRD Project 19039 - All metal vacuum scroll pump development for tritium

Currently the United States relies on a single source, foreign company, Eumeca (formerly Normetex) for the supply of an all metal vacuum scroll pump to process tritium. This “one of a kind”, all metal, vacuum scroll pump utilizes no “wetted”, polymeric materials that degrade prematurely when exposed to tritium. U.S. based vacuum scroll pump suppliers typically utilize a polymer, Teflon®, as a tip seal material at the edge of the scroll impellers for proper pump function. Teflon® is known to degrade within a relatively short time frame (approximately 1 year) when continually exposed to tritium gas. This degradation results in “flaking” of the Teflon® material which results in particulate contamination of the process gas stream. While filtration of the particulate is possible, doing so requires additional maintenance which is costly in a glovebox environment. In addition, filtration can degrade pumping system performance as particulate collects in the filter media over time. To date, all of the well established U.S and European based vacuum scroll pump manufacturers have been uninterested in developing an all metal vacuum scroll pump that does not use a polymeric scroll tip seal. This position is taken as the vacuum scroll pump manufacturers do not see a large enough market to make it profitable for them to develop and market an all metal vacuum scroll pump. In the mid 2000s, one company, Air Squared, Inc., a small Original Equipment Manufacturer (OEM) specializing in design and fabrication of custom scroll vacuum pumps and compressors, was willing to pursue the effort. The first design effort incorporated Vespel® as a polymeric tip seal material. Results of this effort led to realizing the affect that the Met-Bel MB-601 metal bellows pump has on performance when used as a backing pump for an all metal vacuum scroll pump without a scroll tip seal. As a result, Air Squared subsequently designed an all metal vacuum scroll pump without a tip seal material for evaluation. Although the initial, all metal version of the Air Squared pump was found deficient in regard to scroll impeller stiffness, which resulted in scroll contact, general design and pump performance was verified to be adequate. SRS PDRD Project 19039 was launched in 2019 as a 3rd attempt with Air Squared, Inc. in regard to development of an all metal vacuum scroll pump for consideration as an equivalent to the Eumeca/ Normetex pump. The effort specified 300 series stainless steel for the scroll impellers, all metal sealing, and design to meet tritium throughput and ultimate vacuum requirements. In addition, a 60 psig design pressure rating requirement was specified for the pump containment boundary. The 3rd generation Air Squared pump has been designed, fabricated, and has received preliminary testing. Preliminary testing has indicated proper leak tightness and pump performance. However, work continues regarding development of a pumping chamber containment bellows that can be subjected to 66 psig without damage to the bellows. Work will continue in 2020 and 2021 to pursue a pumping chamber containment bellows that meets the pressure rating requirement.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Demonstration of Integrated PostIrradiation Process Steps forMultikilogram Amounts of Low- and High-Burnup Used Nuclear Fuels

sponsored research and development (R&D) on the advanced, closed nuclear fuel cycle, including post-irradiation processing of used fuels, recovery of separated components, and preparation of recycle nuclear fuels. During the period 2007–2010, kilogram-scale demonstrations of the integrated processing steps were performed for actual light water reactor (LWR) used nuclear fuels (UNF). These integrated processing demonstrations were called “the Coupled-End-to-End” (CETE) campaigns and were associated with the Global Nuclear Energy Partnership program, which ran concurrently. The demonstrations were carried out in the shielded hot cells and associated gloveboxes located in the Irradiated Fuels Examination Laboratory (IFEL) and the Radiochemical Engineering Development Center (REDC) at the Oak Ridge National Laboratory (ORNL). Limited circulation program reports and a few technical papers were issued. The subject document provides a comprehensive summary of results, technical comparisons, and conclusions obtained from the demonstration campaigns and subsequent associated R&D.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Metal Bellows Valve Reliability Testing - Copper Stem Tip Testing

SRNL was funded in Mid-Year FY20 by NNSA NA-231 to continue evaluation of alternate valves for use in tritium service to support domestic Mo-99 production. The focus of the effort was to identify valve cycle life as a function of actuator size and stem tip material. Using the minimum size actuator to reliability open and close valves can reduce glovebox size and thus support domestic companies to “come to market” faster in supplying Mo-99 to the US market. This report serves as a continuation to the FY19 report and summarizes the task activities completed in FY20 after authorization to start work was obtained on May 5 th , 2020. Copper stem tips were tested on the Swagelok 1C and 5C actuated metal bellows valves. With ambitions to cycle each set 150,000 times, both 1C and 5C valves were met with high failure rates. The smaller 1C actuated valves required additional closing pressure to form a seal with the Cu stem tips installed however, excessive stem tip deformation may be the root cause of the majority of the valves failing before 500 cycles. The larger 5C actuated valves were cycled 150,000 times but still resulted in 80% failure rate, suspected of metal fatigue in the bellows due to high cycling frequencies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Using ROS for Robotic Control [Slides]

The use of robots is important, to help prevent people from being exposed to hazardous materials within a glovebox. The research proposal for the summer was to make a pick and place demo for a seven degrees-of-freedom Motoman Sia5d robot. The Robot Operating System (ROS) was used and the knowledge of C++ and Linux had to be applied. The robot was used to pick up and sort four objects (cylinder, sphere, rectangular prism, and cone) within a virtual environment.

42 ENGINEERING↗
DOE OSTI2021

Nuclear Enterprise Science & Technology (NEST) [Slides]

The NEST Certificate Program is designed to provide students with the skills and experience to qualify for entry-level positions in nuclear facilities as Fissile Material Handler and/or Glovebox Operator. The program goal is to provide for a technically qualified workforce who can execute a variety of programmatic work in modern nuclear materials handling and processing facilities. The program is designed to be completed in a minimum of 1 year (2 semesters) of university level courses (30 credit hours). A certificate will be offered and awarded through the University of New Mexico – Los Alamos (UNM-LA). NEST is unique in that it is an immersive education program. The NNSA-required training for nuclear material handlers and fissionable material handlers has been cross-walked with the educational Core Curricula. Academic content will be delivered that provides background scientific and engineering understanding of the fundamental concepts behind this training. It will be offered as a Pilot Program to an incumbent cohort to ensure that the Certificate meets programmatic needs. NEST is modelled after a Wharton County Junior College (Texas) program to attract and produce nuclear reactor operators.

96 KNOWLEDGE MANAGEMENT AND PRESERVATION↗