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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 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

In Situ Liquid Electron Microscope Cells Strongly Attenuate Electrochemical Behavior

In situ electrochemical Scanning Transmission Electron Microscopy (ec-S/TEM) probes the dynamics of electrochemical processes in real time and at high spatial resolution. This method utilizes microfabricated electrochemical cells, with enclosed dimensions of 800 μm wide, 800 μm long, and 1–2 μm tall, with electron-transparent silicon nitride windows. Working, counter, and reference electrodes in the configuration studied are deposited Pt with a planar surface area of about 1 μm 2 and a height of 50 nm. The cell confines the electrolyte within a 1 μm tall channel, and the microfabricated electrodes have a non-standard geometry, are coplanar, and are not front-facing. As such, standard assumptions of electrochemical experiments do not apply. COMSOL modeling was used to compare and contrast differences in electrochemical behavior between conventional experimental setups and the in situ ec-S/TEM cells. Cell height strongly affected voltammogram measurements: peak magnitudes and shifts correlate directly to cell height. Reactant concentration above the electrode quickly decreases during deposition, leading to a planar diffusion-dominated regime. The concentration gradient prioritizes particle growth along the thin edges of the electrode and not on the planar part of the electrode. Experiments done in the ec-S/TEM ex situ of a TEM verify the model’s accuracy.

Wittman, Reed M. [Oak Ridge National Laboratory (O↗
DOE OSTI2025

Behavior of the Cadmium Pool in the INL Mk-IV Electrorefiner

The Mk-IV electrorefiner has been in service since 1996 recovering uranium from spent fuels from the Experimental Breeder Rector II and Fast Flux Test Facility sodium-cooled fast reactors. The electrorefiner vessel includes a cadmium pool beneath the salt. The voltage signal between the cadmium pool and reference electrode (Ag/AgCl type) provides information about the chemical condition of the cadmium pool with respect to uranium and zirconium saturation. This information is used to guide process control and sampling decisions. This paper describes how the voltage signal is related to chemistry by the analyses of data from Mk-IV operations and confirmatory experimentation.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Investigation Into LiCl-LiF+Li 2 O as a Low Temperature Electrolyte in Direct Electrolytic Reduction of UO 2

Direct electrolytic reduction (DER) of UO 2 in a binary LiCl-Li2O (1–3 wt%) at 650 °C has been widely reported. The process temperature can be reduced to 550 °C in theory by using a near eutectic ternary LiCl-LiF+Li 2O (∼2 wt%) electrolyte, which will result in substantial reduction in rate of salt vaporization. The feasibility of using the ternary electrolyte for the process was tested via material compatibility testing, electrochemical polarization testing, and controlled potential or current DER experiments. MgO, Pt, and 625 nickel samples were each contacted with the ternary salt for 168 h. Negligible changes to dimensions and mass of the samples were measured, and concentrations of corrosion products in the salt were 102 ppm or less. O2−oxidation was observed to occur at a lower potential than Cl-or F-on a Pt anode. DER of UO2was performed in six trials. Process variables included type of reference electrode, electrochemical control method, type of cathode basket, and electrolyte composition. UO 2conversion ranged from 28.2 to 99.9 % , and current efficiency ranged from 38 to 52%. Overall, results indicate that the use of the ternary salt is feasible for DER.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Galvanostatic Plating with a Single Additive Electrolyte for Bottom-Up Filling of Copper in Mesoscale TSVs

A methanesulfonic acid (MSA) electrolyte with a single suppressor additive was used for potentiostatic bottom-up filling of copper in mesoscale through silicon vias (TSVs). Conversly, galvanostatic deposition is desirable for production level full wafer plating tools as they are typically not equipped with reference electrodes which are required for potentiostatic plating. Potentiostatic deposition was used to determine the over-potential required for bottom-up TSV filling and the resultant current was measured to establish a range of current densities to investigate for galvanostatic deposition. Galvanostatic plating conditions were then optimized to achieve void-free bottom-up filling in mesoscale TSVs for a range of sample sizes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Dissection of the Voltage Losses of an Acidic Quinone Redox Flow Battery

We measure the polarization characteristics of a quinone-bromide redox flow battery with interdigitated flow fields, using electrochemical impedance spectroscopy and voltammetry of a full cell and of a half cell against a reference electrode. We find linear polarization behavior at 50% state of charge all the way to the short-circuit current density of 2.5 A/cm 2 . We uniquely identify the polarization area-specific resistance (ASR) of each electrode, the membrane ASR to ionic current, and the electronic contact ASR. We use voltage probes to deduce the electronic current density through each sheet of carbon paper in the quinone-bearing electrode. By also interpreting the results using the Newman 1-D porous electrode model, we deduce the volumetric exchange current density of the porous electrode. We uniquely evaluate the power dissipation and identify a correspondence to the contributions to the electrode ASR from the faradaic, electronic, and ionic transport processes. We find that, within the electrode, more power is dissipated in the faradaic process than in the electronic and ionic conduction processes combined, despite the observed linear polarization behavior. We examine the sensitivity of the ASR to the values of the model parameters. The greatest performance improvement is anticipated from increasing the volumetric exchange current density.

25 ENERGY STORAGE↗
DOE OSTI2019

Fabrication of Uniform Nanoparticulate Gold through Potential-Modulated Electrochemical Deposition and Dissolution of Silver in Ionic Liquids

Nanoparticulate gold (NPG) has been successfully produced from polycrystalline Au by a novel method based on potential-modulated electrochemical deposition and dissolution of silver in an ionic liquid bath comprising of 1-ethyl-3-methylimidazolium chloride and silver nitrate at elevated temperatures. Cyclic voltammetric measurements exhibit that the potential cycles between -1.0 and 0.75 V versus a silver pseudo reference electrode can drive the electrochemical deposition and dissolution of silver onto and away from the Au electrode. Scanning electron microscope studies show that the NPG resulting from the potential cycles has very narrow particle size distribution with an average diameter of approximately 50 nm and is free of elemental Ag residue. As compared to a bulk Au electrode, the NPG electrode demonstrates substantially enhanced electrochemical responses. It exhibits a seven-time higher electro-catalytic activity towards the electrooxidation of nitrite in acidic media.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Review—Electrochemical Measurements in Molten Salt Systems: A Guide and Perspective

Practical information is provided on electrochemical measurements in molten salt systems. The emphasis is on chloride and fluoride systems, but the principles are applicable to any high temperature molten salt or molten oxide electrolyte system. Considerations are given to topics such as the functionality of electrochemical measurement equipment, reference electrodes, materials selection and chemical compatibility, interpretation of electrochemical measurement signals, molten salt properties, and laboratory practices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Redox potential in Typha-dominated tidal brackish marsh, PIE LTER, Plum Island Sound, MA, June–December 2022

This dataset includes soil redox potential measurements collected at multiple depths within a tidal brackish wetland in the upper estuary of the Plum Island Ecosystems Long-Term Ecological Research site (PIE LTER), Plum Island Sound, Newbury, Massachusetts. Measurements were taken to evaluate temporal variation in redox potential in relation to hydrological events at three replicate locations. Data were recorded every 5 minutes using a Campbell Scientific Volt116 connected to a CR6 datalogger with SWAP instrument redox probes (ORP-30-4-B) and reference electrodes. Measurements were made at the AmeriFlux site US-PLo at four soil depths (5, 10, 15, and 30 cm). The file redox_soiltemp_2022.csv contains temperature-corrected redox values and soil temperature following Silva-Machado et al. (2024). Metadata files redox_soiltemp_dd.csv and redox_soiltemp_flmd.csv provide detailed descriptions of variables and site locations.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Redox potential in Typha-dominated tidal brackish marsh, PIE LTER, Plum Island Sound, MA, 2023

This dataset includes soil redox potential measurements collected at multiple depths within a tidal brackish wetland in the upper estuary of the Plum Island Ecosystems Long-Term Ecological Research site (PIE LTER), Plum Island Sound, Newbury, Massachusetts (MA). Measurements were taken to evaluate temporal variation in redox potential in relation to hydrological events at three replicate locations. Data were recorded every 5 minutes using a Campbell Scientific Volt116 connected to a CR6 datalogger with SWAP instrument redox probes (ORP-30-4-B) and reference electrodes. Measurements were made at the AmeriFlux site US-PLo at four soil depths (5, 10, 15, and 30 cm). The file redox_soiltemp_2023.csv contains temperature-corrected redox values and soil temperature following Silva-Machado et al. (2024). Metadata files redox_soiltemp_dd.csv and redox_soiltemp_2023_flmd.csv provide detailed descriptions of variables and site locations.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

Development and Demonstration of an In-Situ Tritium Scavenger

The objective of this project was to use an inherent feature of salt-cooled reactors towards the capture and removal of tritium from the primary coolant system: the presence of the graphite moderator. The fuel elements fluoride-salt cooled high-temperature (FHR) reactors consist of a graphite matrix that encapsulates TRISO fuel particles, and the total fuel element surface area of Mark I PB-FHR is 7780 m 2 . Therefore the FHR fuel inherently provides removable graphite of high surface area. The goal of this project was to understand the transport of tritium across the salt-graphite interface. The following was achieved: 1. Electrochemical techniques were demonstrated for studying the entry, diffusion, and trapping of hydrogen isotopes in graphite. 2. Electrochemical techniques were used to demonstrate the relationship between galvanic corrosion between graphite and stainless steel 316 and hydrogen uptake in graphite. 3. Electrochemical techniques were demonstrated for studying the dissolution and diffusion of hydrogen isotopes in molten FLiBe. 4. Thermodynamic reference electrodes were tested for FLiBe and FLiNaK. 5. Electrochemical techniques were demonstrated as an in-salt hydrogen thermal desorption measurement, which had previously only been achieved in gas environments. 6. FLiBe exposure of graphite lead to graphite fluorination and an increase of defects, which indicate an increase of reactive carbon sites available for tritium uptake. 7. TRIDENT modeling was used to perform sensitivity analysis of FHR design parameters on tritium uptake fraction in graphite, showing high sensitivity to tritium diffusivity and solubility. 8. A cross-cutting effort with another NEUP-funded project was initiated for application of the SAM mass-transport module to system-scale tritium modeling.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

0D Modeling of Reactor Networks Within Zuzax

We report on progress in developing macroscopic balance equations for combustion and electrochemistry systems. A steady state solution capability is described for the macroscopic reactor network, with an associated steady state continuation method and solution storage capability added in. An example is provided of continuation of a hydrogen flame versus the equivalence ratio. The reactor modeling capability is extended to charged fluid systems, with a description of the new ChargedFluidReactor, SubstrateElement, and MetalCurrentElement reactor classes and novel setup of unknowns within these reactors that preserve charge neutrality. Zuzax's setup for electrochemistry is explained including the specification of the electron chemical potential and the adherence to the SHE Reference electrode specification. The description of the different ways to enter electrochemical reaction rates are described, contrasted, and their derivations with respect to one another are derived. An example of using the ChargedFluidReactor within corrosion problems is provided. We present a description of calculations to understand the phenomena of corrosion of copper from a micron sized droplet of NaCl water droplet, where secondary spreading occurs. An analysis of the discrepancies with experiment is carried out, demonstrating that macroscopic balances can be an important tool for understanding what major factors need to be addressed for a better understanding of a physical system.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Integrity Monitoring and Assessment, Prediction, Repair, and Corrosion Control of the Hanford Storage Tanks — 25213

BACKGROUND AND PROJECT TASKS Proposed work addresses focus area 1: Waste Retrieval, Transport and Closure, with particular focus on increasing volume available for tank storage 1) Refurbish/fortify existing double shell storage tanks (Tank Refurbish – Polymer Grout) 2) Robust monitoring tools for internal corrosion (Integrity Monitoring -Reference Electrodes) 3) Mitigate external corrosion (Degradation Prevention - Cathodic Protection) 4) Determine viability of constructing new tanks, and storage room creation by way of evaporation (Cost Benefit Analysis)

Shukla, Pavan K. [Savannah River National Laborato↗
DOE OSTI2024

Multiport high-pressure synchrotron x-ray microscopy cell (CRADA Final Report)

The LBNL team developed a multiport cell allowing for fluid flow, with electrical contacts for sample bias, and with reference electrodes. The cell is currently installed and operating in beam-line 11.0.2 of the ALS, the Berkeley Synchrotron. The cell is closed by a membrane consisting of several stacked layers of graphene (1 to 3). The graphene membrane is supported on a 100 nm thick Si3N4 membrane covered with a 20 nm thin gold film for improved adhesion of the graphene and to ensure electrical conductivity. The Si3N4 film is perforated with a periodic array of holes 1 to 2 micrometers diameter. The cell can withhold an internal pressure (gas or liquid) of up to 10 atmospheres for in situ/operando studies using X-ray Photoelectron emission (XPS), and X-ray Absorption Spectroscopy (XAS). It is also ideal for tip-enhanced nano-Infrared Spectroscopy studies of molecules at the interface between the graphene and the liquid or gas filling the cell. Materials studied in the LBNL laboratory are in the form of nanoparticles, or thin films (few nm) deposited on the side of the graphene membrane facing the solution or gas inside the cell.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Demonstration of Electroreduction Technology to Convert GNF Uranium Oxide Powder to Metal

Global Nuclear Fuel – Americas LLC (GNF) has partnered with Argonne National Laboratory to demonstrate electroreduction of uranium oxides produced by deconversion of UF 6 to uranium metal through the Gateway for Accelerated Innovation in Nuclear (GAIN) program under the U.S. Department of Energy to accelerate the domestic production of metallic advanced reactor fuels. Electroreduction of uranium oxide was first demonstrated and patented by Argonne in the early 2000s as a technology to convert used oxide nuclear fuel from light water reactors to metal for further fuel reprocessing. More recently, electroreduction has been proposed as a front-end technology for metallization of uranium oxides produced by deconversion of UF 6 and for scrap recovery of oxide materials. During the electroreduction process, UO 2 powder is contained in a stainless-steel mesh basket with a cathode lead located in the center of the UO 2 bed. The basket is immersed in lithium chloride molten salt electrolyte containing 1 wt% lithium oxide along with a platinum anode and a nickel/nickel oxide (Ni/NiO) reference electrode. Current is applied to the cell between the cathode and anode to reduce the UO 2 to metallic uranium via a solid-state reduction reaction. Oxide ions released from the UO 2 during reduction are transported through the salt to the anode where oxygen gas is evolved. Once reduction is complete, the basket containing the metallicized uranium is removed from the salt and can be processed to remove the salt and consolidate the uranium into an ingot for use in metallic fuel fabrication. This project was performed to provide evidence of the electroreduction technology readiness level for metallization of UO 2 powder, identify and retire technical risks for industrialization of electroreduction, and accelerate the path to commercialization for metallic fast reactor fuel production. To that end, five electroreduction tests were performed with UO 2 provided by GNF and the resulting product was analyzed for the extent of conversion to metal and for impurity contents of the metal product to verify that electroreduction does not introduce impurities that would prevent use of the product in metallic fuel fabrication.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Roadmap for Assessing Fuel Reprocessing in Fluoride-Based Salts

This joint report assesses the pyroprocessing of used nuclear fuel from molten fluoride salts being conducted between Idaho National Laboratory and Argonne National Laboratory. The goal of this report is to identify the research and development gaps needed to reduce the technical risks of extending pyroprocessing technologies and unit operations to molten fluoride salts used in molten salt reactors (MSRs). Assessing and performing the tasks outlined in this report will help mitigate the technical risks and design appropriate flowsheets for reprocessing fuel and coolant salts. These suggested tasks will provide necessary data to implement the development of unit operations. Sections are highlighted to identify processes that need to be assessed and unit operations that may be used in fluoride-based chemistries. Research and development needs are listed and discussed including re-fluorination methods, electrowinning for separations, reference electrode development, materials compatibility, salt purification/re-fluorination, and waste disposition. This report will examine the technical challenges associated with pyroprocessing in molten fluoride-based salt and outline approaches to increase the technical readiness level of pyroprocessing in molten fluoride salts.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1966

Simple, nondestructive test identifies metals

Rapid, nondestructive test for identifying metals measures the characteristic potential difference produced by galvanic reaction between a reference electrode and the test metal. A drop of water is used as an electrolyte.

Dodds, D. J.↗
NASA NTRS1972

Bacteria detection instrument and method

A method and apparatus for screening a sample fluid for bacterial presence are disclosed wherein the fluid sample is mixed with culture media of sufficient quantity to permit bacterial growth in order to obtain a test solution. The concentration of oxygen dissolved in the test solution is then monitored using the potential difference between a reference electrode and a noble metal electrode which are in contact with the test solution. The change in oxygen concentration which occurs during a period of time as indicated by the electrode potential difference is compared with a detection criterion which exceeds the change which would occur absent bacteria.

Renner, W.↗