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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Multi-Sourced Collaboration for the Production and Refining of Rare Elements and Critical Metals (Final Technical Report)

The project objective was to develop a feasible and cost-effective method for recovering rare earth elements (REEs) and critical materials (CMs) from coal and coal byproducts, resulting in high-purity individually separated REEs and CMs. The targeted REEs included Y, Pr, Nd, Gd, Dy, and Sm, with a purity of over 99.5%, while the CMs included Co, Mn, Ga, Sr, Li, Ni, Zn, and Ge, with a purity of over 90%. The project aimed to design a prototype facility capable of producing 1-3 tonnes/day of high-purity REO mixes. The work was divided into four designated circuits: 1) REE extraction and concentration, 2) REE separation and purification, 3) RE metal production, and 4) CM production. To achieve these goals, the project involved 11 tasks, including technology reviews, research, process flow diagram development, mass balance estimation, and preliminary technical-economic analysis. The project team included researchers from the University of Kentucky, University of Alabama and Virginia Tech as well as process specialists from Argonne National Laboratory. MP Materials provided technical support regarding rare earth markets and processing while Alliance Coal performed resource assessment. The project included a market analysis for Nd/Pr, Tb, Dy, Gd, Y, Co, Mn, Li, Sr, Ga, Ni, Zn, and Ge. These analyses provided insights into the supply and demand trends as well as historic and future projections of market price relative to purity requirements for these elements. Two coal resources were selected for the project: the West Kentucky No. 13 (Baker) Seam and an undisclosed lignite resource in the Illinois coal basin. The estimated quantities of REEs in these resources were calculated based on production samples and drilling data. It was estimated that there is adequate supply for an operation producing one metric ton daily of higher purity mixed rare earth oxides (MREO) for approximately 20 years at a site located in western Kentucky. In Circuit 1, project data was obtained from a pilot heap leach and REE concentration facility. It was concluded that the existing circuit, which generated a MREO concentrate, two types of CM mixed products, and Li- and Sr-containing waters, would be suitable feed for circuits 2-4. Data from the first-of-its-kind coal coarse refuse heap leach pilot pad played a crucial role in estimating reliable elemental concentrations of the pregnant leaching solution (PLS). The average total REE concentration in the PLS was found to be 28.6 ppm. In Circuit 2, several concepts were explored including a novel process referred to as solvent-assisted chromatography (SAC). This concept involved a novel columnar reactor that incorporated multiple mixer/settlers, thereby enabling the operation of counter-flowing aqueous and organic phases. Unfortunately, due to project time constraints, a complete fundamental modeling analysis could not be completed to fully evaluate the technology. Molten salt electrowinning was considered as an alternative for circuit 3 following circuit 2 purification circuit utilizing the novel SAC process. A mass and energy balance of Nd reduction to metal in a fluoride containing molten salt electrolyte was conducted. Comparisons were made with the current state of Asian molten salt electrorefining, and potential improvements in siphoning rare earth metals (REM) from the reactor were presented. A cost estimate was performed for the production of 1 tonne per day, which yielded a total of $2.29 million for the nine electrowinning (EW) cells required. The selected option for circuits 2 and 3 was a plasma distillation process, which initially separates rare earth elements (REEs) from other elements. This is followed by selective electrowinning in various ionic liquids. The selection was made on the basis of thermodynamic modeling and experimental data previously published by a project partner. The combination offers an innovative approach to integrated refining and RE metal production. For Circuit 4, an extensive literature review was conducted for the processing of the CMs. The ultimate decision was to utilize a combined plasma and ionic liquid process as well to produce individual high-purity concentrates of Zn, Ni, Co, Mn, and Mg. A separate flowsheet for Li and Sr was recommended, which would yield carbonates of these elements. Due to the lack of suitable experimental data at this time, a process recommendation could not be provided but several methods have been proposed for consideration. Lastly, a techno-economic analysis (TEA) was conducted to assess the effectiveness of the proposed process for further investigation. The TEA results revealed a capital expense (CapEx) of $737 million and an annual operational expense (OpEx) of $220 million. Due to the selected elements, the hypothetical heap leach pad can produce 1 metric tonne per day of REO equivalent, but a conscious decision was made to only treat targeted REEs, resulting in the production of 0.4 metric tonne of REM. An estimated annual revenue of $90.87 million was projected based on standard market pricing information provided by the funding agency. During the TEA, ten different modules were evaluated for costing purposes. The precipitation circuit was identified as the largest single operational expense, followed by the Mg/Mn process due to the amount of treated metal. In terms of capital expenditures, the heap leach process incurred the highest cost, followed by the Mg/Mn process. The scalability of the plasma process is a crucial consideration since the reactors cannot be scaled beyond the largest demonstrated size due to their reliance on surface area of the slag and vapor phase. The purity estimate for the REEs are generally 98%±2% to produce a metal. The purity level being lower than the project objective was due to the lack of specific experimental data needed to tighten the tolerance of the estimates. Based on literature and previous experience, the CMs are estimated as follows; Ga (95%+, metal), Sr (95%+, carbonate), Li (95%+, carbonate), Ni (98%±2%, metal), Zn (95%+, metal sponge), Ge (95%+, metal), Co (98%±2%, metal), and Mn (98%±2%, metal).

01 COAL, LIGNITE, AND PEAT↗
NASA NTRS2009

Production of Oxygen from Lunar Regolith by Molten Oxide Electrolysis

This paper describes the use of the molten oxide electrolysis (MOE) process for the extraction of oxygen for life support and propellant, and silicon and metallic elements for use in fabrication on the Moon. The Moon is rich in mineral resources, but it is almost devoid of chemical reducing agents, therefore, molten oxide electrolysis is ideal for extraction, since the electron is the only practical reducing agent. MOE has several advantages over other extraction methods. First, electrolytic processing offers uncommon versatility in its insensitivity to feedstock composition. Secondly, oxide melts boast the twin key attributes of highest solubilizing capacity for regolith and lowest volatility of any candidate electrolytes. The former is critical in ensuring high productivity since cell current is limited by reactant solubility, while the latter simplifies cell design by obviating the need for a gas-tight reactor to contain evaporation losses as would be the case with a gas or liquid phase fluoride reagent operating at such high temperatures. Alternatively, MOE requires no import of consumable reagents (e.g. fluorine and carbon) as other processes do, and does not rely on interfacing multiple processes to obtain refined products. Electrolytic processing has the advantage of selectivity of reaction in the presence of a multi-component feed. Products from lunar regolith can be extracted in sequence according to the stabilities of their oxides as expressed by the values of the free energy of oxide formation (e.g. chromium, manganese, Fe, Si, Ti, Al, magnesium, and calcium). Previous work has demonstrated the viability of producing Fe and oxygen from oxide mixtures similar in composition to lunar regolith by molten oxide electrolysis (electrowinning), also called magma electrolysis having shown electrolytic extraction of Si from regolith simulant. This paper describes recent advances in demonstrating the MOE process by a joint project with participation by NASA KSC and MSFC, and Ohio State University and MIT. Progress in measuring cell efficiency for oxygen production, development of non reacting electrodes, and cell feeding and withdrawal will be discussed.

Curreri, Peter A.↗
DOE OSTI2025

Undercooling minimization in ultrasound coupled DTA measurements of molten salts

Molten salts are ionic liquids that are used for the electrolytic pyroprocessing of metals and as heat transfer fluids in very high temperature processes. Recently, halide-based molten salt reactors (MSR) have gained momentum for high density and environmentally responsible electricity generation. The function of these reactors and their fuel cycle depend on a knowledge of the halide salt’s thermodynamic properties [1]. Therefore, high accuracy phase equilibria of MSR relevant base halide and actinide containing salts are needed. Modern thermal analysis of the phase transitions of halide salts is usually done during heating at relatively high scan rates with commercial devices. Normally such measurements are adequate for pure or pseudo-binary salts. However, as the number of components in the mixture increases, accurately resolving the liquidus becomes increasingly difficult. Reversing the scanning mode greatly increases the sensitivity of phase transition measurements but can decrease accuracy due to undercooling [2] — a common occurrence in molten halide systems [3]. This work presents the development of a differential thermal analysis (DTA) cell intended for use in radiological gloveboxes. Non-contact ultrasonic agitation of the halide salt is implemented to limit kinetic limitations on crystallization during cooling to minimize undercooling [4]. Measurements on halide salts are also presented to elucidate the effect of non-contact mixing on undercooling. Reference [1] S. Boyd and C. Taylor, “3 - Chemical fundamentals and applications of molten salts,” in Molten Salt Reactors and Thorium Energy, T. J. Dolan, Ed., Woodhead Publishing, 2017, pp. 29–91. doi: 10.1016/B978-0-08-101126-3.00003-8. [2] K. Nitsch, A. Cihlár, and M. Rodová, “Molten state and supercooling of lead halides,” J. Cryst. Growth, vol. 264, no. 1, pp. 492–498, Mar. 2004, doi: 10.1016/j.jcrysgro.2004.01.011. [3] L. Rycerz, “Practical remarks concerning phase diagrams determination on the basis of differential scanning calorimetry measurements,” J. Therm. Anal. Calorim., vol. 113, no. 1, pp. 231–238, Jul. 2013, doi: 10.1007/s10973-013-3097-0. [4] Md. H. Zahir, S. A. Mohamed, R. Saidur, and F. A. Al-Sulaiman, “Supercooling of phase-change materials and the techniques used to mitigate the phenomenon,” Appl. Energy, vol. 240, pp. 793–817, Apr. 2019, doi: 10.1016/j.apenergy.2019.02.045.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Organic wastewater treatment by a single-atom catalyst and electrolytically produced H2O2

The presence of organic contaminants in wastewater poses considerable risks to the health of both humans and ecosystems. Although advanced oxidation processes that rely on highly reactive radicals to destroy organic contaminants are appealing treatment options, substantial energy and chemical inputs limit their practical applications. Here we demonstrate that Cu single atoms incorporated in graphitic carbon nitride can catalytically activate H 2 O 2 to generate hydroxyl radicals at pH 7.0 without energy input, and show robust stability within a filtration device. We further design an electrolysis reactor for the on-site generation of H 2 O 2 from air, water and renewable energy. Coupling the single-atom catalytic filter and the H 2 O 2 electrolytic generator in tandem delivers a wastewater treatment system. These findings provide a promising path toward reducing the energy and chemical demands of advanced oxidation processes, as well as enabling their implementation in remote areas and isolated communities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Activating magnetite ores for aqueous ironmaking at high current densities

Low-temperature electrochemical cells reducing iron oxides to metal in alkaline electrolytes can support fully electrified steelmaking processes. Previous studies on these cells have primarily focused on high-surface-area hematite, Fe 2 O 3 , reactants whereas attempts to reduce suspensions of magnetite, Fe 3 O 4 —one of the two feedstocks for existing ironmaking reactors—have generally been limited to low rates of reaction (<30 mA cm −2 ). Here, in this study, we control the crystalline domain size of Fe 2 O 3 and Fe 3 O 4 particles in 10 M NaOH electrolytes to study how the nanoscale morphology of oxides controls the rate of electrochemical ironmaking. Rotating-ring disk electrode measurements of Fe 2+ , in situ Raman spectroscopy of the electrode surface, and ex situ electron microscopy were consistent with a hypothesized passivation process at Fe 3 O 4 surfaces that may prevent the continuous formation of soluble intermediates. Sufficiently small (<100 nm diameter) oxide particles yielded Fe partial current densities >160 mA cm −2 , a fivefold increase relative to previously reported rates for Fe 3 O 4 suspensions and comparable to active Fe 2 O 3 . Electron microscopy revealed that electrodeposited films were composed of micron-scale crystalline Fe domains with a porous film of Fe 3 O 4 nanoparticles and supports a model where Fe is grown primarily from soluble Fe 2+ intermediates. Based on these insights, inactive blast-furnace-grade iron-oxides were transformed into high surface area nanoparticles (1.6 to 229.2 m 2 g −1 ) via reprecipitation, leading to a ninefold enhancement in faradaic efficiency and an Fe partial current density of 120 mA cm −2 . When integrated with chlor-iron cells producing reagents for reprecipitation, this approach could lead to a cost-competitive process for electrochemical ironmaking from industrially relevant feedstocks.

TEM↗
DOE OSTI2023

RECLAIM: Electrochemical Lithium and Nickel Extraction with Concurrent Carbon Dioxide Mineralization

This project aims to develop technologies toward the production of Li and Ni from CO 2 -reactive minerals and rocks that contain Ca and Mg, while sequestering CO 2 . The technologies include acoustic stimulation and electrolytic proton production, which use electricity to liberate valuable metal ions from the surrounding mineral matrix at sub-boiling temperatures (~20-80°C). Feedstocks include Li/Ni/Ca/Mg-rich igneous and sedimentary rocks and minerals such as holmquistite, hectorite, lateritic Ni ores enriched in Mg-rich serpentine. Other examples of feedstocks that could be used include coarse grained orthocumulate, mine tailings, etc. In the first step, the electrolytic breakdown of water to H + and OH – (as well as O 2 and H 2 ) will be induced by applying an electric potential to simultaneously produce acidity and alkalinity. The solid feedstocks will be dissolved in the acidic anolyte under acoustic stimulation. Solubilized species will then undergo separation using our unique Li + -selective membranes driven by electrodialysis, leading to concentration of Li as soluble lithium silicate, from which Li 2 CO 3 can be derived by reaction with CO 2(g) while supplying cathode alkalinity. Also at the cathode, stepwise electrolytic precipitation of metal hydroxides, including Ni(OH) 2 , Ca(OH) 2 , and Mg(OH) 2 is performed along a cascade reactor in which both the applied potential and pH increase downstream, thereby simultaneously extracting and separating the metals. Finally, exposure of Ca(OH) 2 and Mg(OH) 2 to dilute CO 2 will result in CO 2 uptake in the form of Ca and Mg carbonates. The primary accomplishments include sample procurement and characterization. Progress has been made on precursor identification and mapping, establishing protocols for assessing metal extractability under sonication, and preliminary technoeconomic analysis (TEA) and life cycle analysis (LCA).

36 MATERIALS SCIENCE↗
DOE OSTI2024

Screening aqueous organic redox couples for spontaneous hydrogen generation on catalysts

Two low-cost redox couples with near neutral or alkaline pH - 7,8-dihydroxyphenazine-2-sulfonic acid (DHPS) and chrome chelated ethylenediaminetetraacetic acid (Cr-EDTA) with ammonia – are identified to generate hydrogen evolution spontaneously on Pt/C catalysts. Cr-EDTA redox couple has two times higher hydrogen evolution rate than that of DHPS, and the charged Cr-EDTA molecules are fully utilized to generate hydrogen gas, while ~ 50% of DHPS molecules are utilized to produce hydrogen spontaneously on Pt/C catalysts. The Cr-EDTA electrolyte enables cost reduction by allowing cheap raw material of Cr and corrosion resistant alloy instead of costly superalloy for catalytic reactor systems. Furthermore, the Cr-EDTA with ammonia as a negolyte for flow batteries was validated to suppress hydrogen evolution side reaction, reach 99% of coulombic efficiency in flow cell operation paired with Fe(CN)6 redox couple near neutral pH.

08 HYDROGEN↗
DOE OSTI2023

Membrane–Electrolyte System Approach to Understanding Ionic Conductivity and Crossover in Alkaline Flow Cells

Membrane transport properties are crucial for electrochemical devices, and these properties are influenced by the composition and concentration of the electrolyte in contact with the membrane. We apply this general membrane-electrolyte system approach to alkaline flow batteries, studying conductivity and ferricyanide crossover of Nafion and E-620. We report undetectable crossover for as-received Nafion and E-620 after both sodium and potassium exchange, but high ferricyanide permeability of 10 –7 to 10 –8 cm2 s –1 for Nafion subjected to pre-treatment prevalent in the flow battery literature. We show how the electrolyte mass fraction in hydrated membranes regulates the influence of ion concentration on membrane conductivity, identifying that increasing electrolyte concentration may not increase 1 membrane conductivity even when it increases electrolyte conductivity. To illustrate this behavior we introduce a new metric, the membrane penalty, as the ratio of the conductivity of the electrolyte to that of the membrane equilibrated with the electrolyte. We discuss the tradeoff between flow battery volumetric capacity and areal power density that arises from these findings. Finally, we apply insights from this approach to provide recommendations for use of membranes in alkaline flow cells, and electrochemical reactors in general.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

The Future of Nuclear Energy: Electrochemical Reprocessing of Fuel Takes Center Stage

Nuclear power plants use energy-dense fuel and provide dependable baseload energy without generating greenhouse gas emissions. Despite these advantages, the long-term management of used nuclear fuel (UNF) remains a key challenge due to its lifetime (hundreds of thousands of years) and radiotoxicity. The components of UNF that contribute the most to this challenge are the actinide elements. A potential solution to this issue is to separate these radioisotopes from the bulk of the UNF and recycle them as fuel in advanced nuclear reactors. These separations can be achieved using electrochemical reprocessing, which employs electrochemical conversion and electrodeposition in a high-temperature molten salt electrolyte medium to separate the actinides from UNF. In this work, we review the current status, fundamental challenges, and future prospects of electrochemical reprocessing as they relate to UNF recycling.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Electrochemical Characterization of Bromine Reduction to Tribromide in Individual Nitrobenzene-in-Water Emulsion Droplets

We report an electrochemical study of bromine reduction to tribromide in a single nitrobenzene (NB) droplet during a single collision event. The feasibility of this study is based on the favorable distribution of Br 2 in NB rather than in water, which was demonstrated by voltammetry at the NB/water interface. The NB-in-water emulsions containing the ionic liquids trihexyltetradecylphosphonium bis(trifluoromethylsulfonyl)amide (ILPA) as the supporting electrolyte and sodium dodecyl sulfate (SDS) as the surfactant were prepared by a high-power ultrasonication. Its single droplet as an attoliter reactor, colliding on a 25 μm Pt UME, was monitored by chronoamperometry. The spike-type current transients of Br 2 reduction can elucidate the size and size distribution of NB, and measure the diffusion in the droplet as analyzed by a bulk electrolysis model. The frequency of collisions can provide diffusion coefficient of the droplets to the UME. Moreover, the i-t decay behavior can be simulated, which fits well with the experimental one.

25 ENERGY STORAGE↗
NASA NTRS1979

Evaluation of Selected Chemical Processes for Production of Low-cost Silicon, Phase 3

Refinements of the design of the 50 MT/year Experimental Process System Development Unit were made and competitive bids were received from mechanical, electrical, and structural contractors. Bids on most of the equipment were received and cataloged. Emergency procedures were defined to counter a variety of contingencies disclosed in operations and safety reviews. Experimental work with an electrolytic cell for zinc chloride disclosed no significant increase in power efficiency by steps taken to increase electrolyte circulation. On the basis of materials compatibility and permeability tests, 310 stainless steel was chosen for the shell of the fluidized-bed reactor and SiC-coated graphite for the liner.

Blocher, J. M.↗
NASA NTRSDate not supplied

Feasibility Testing of Silver Electrolysis for Disinfection of Spacecraft Potable Water Systems

Anodic dissolution of silver electrodes, or “silver electrolysis,” is being investigated as a means of introducing biocidal silver into potable water on exploration spacecraft. A proof-of-concept prototype of a silver electrolysis reactor was developed, and feasibility was demonstrated for imparting a target silver concentration into a spacecraft water system. Prototype testing showed that the primary initial concerns related to the technology - inefficiencies of electrolysis in low conductivity water, the potential formation of resistive oxides on the electrode surfaces, and the potential for release of electrolytically-generated silver particles to the effluent water - were not problematic over the duration of the feasibility testing. The testing also demonstrated advantages of the technology, including the ability to consistently deliver silver at targeted concentrations and the ability to directly correlate the silver concentration to measurements of water conductivity. On the other hand, the reliability of the system has not yet been demonstrated. During prototype testing, intermittent periods of poor reactor performance manifested as a decrease in voltage accompanied by a decrease in silver output. It was determined that the cause of this behavior was silver-based deposits on inter-electrode wetted surfaces forming a conductive “bridge” between electrodes. Ongoing testing and refinement of the prototype reactor design seek to elucidate the root cause the bridging phenomenon and identify associated mitigation strategies. Once resolved, long-term performance testing is planned as part of continued development of the electrolytic silver dosing system.

Silver↗
DOE OSTI2020

Electrochemical Salt Wasteform Development: A Review of Salt Treatment and Immobilization Options

Electrochemical reprocessing, also referred to as pyroprocessing, is a technique for recycling actinides from used nuclear fuel (UNF) to produce fuel for future reactors. Here, UNF is dissolved in a molten salt (e.g., LiCl-KCl eutectic) within an electrorefiner. After UNF dissolution, fission products are released into the electrolyte salt and converted to chlorides. This paper discusses wasteform options for processing the base electrolyte salt with the fission product salts as well as just the rare-earth fission products (as RECl 3 , REOCl, or REO x ) with the intent of finding optimal methods for reducing total waste salt volumes or partitioning the salt for alternate wasteform options. Furthermore, two of the more detailed partitioning options discussed herein include halide removal from the salt (dehalogenation), which accounts for more than half of the salt on a molar basis, and RE fission product removal for wasteforms with high-RE loadings. Wasteform properties are compared with emphasis on wasteform volume starting from a given amount of (1) total salt cations or (2) RE cations. Comparisons are also made of wasteform chemical durabilities, with the data available from like testing methods. A main conclusion from this work is the justification of subsequent salt processing after electrorefiner operations for achieving significant wasteform volume reduction.

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

Plasma diagnostics and modeling of lithium-containing plasmas

Thin-film deposition from chemically reactive multi-component plasmas is complex, and the lack of electron collision cross-sections for even the most common metalorganic precursors and their fragments complicates their modeling based on fundamental plasma physics. This study focuses on understanding the plasma physics and chemistry in argon (Ar) plasmas containing lithium bis (trimethylsilyl) amide used to deposit Li x Si y thin films. These films are emerging as potential solid electrolytes for lithium-ion batteries, and the Li-to-Si ratio is a crucial parameter to enhance their ionic conductivity. We deposited Li x Si y films in an axial flow-through plasma reactor and studied the factors that determine the variation of the Li-to-Si ratio in films deposited at various points on a substrate spanning the entire reactor axis. While the Li-to-Si ratio is 1:2 in the precursor, the Li-to-Si ratio is as high as 3:1 in films deposited near the plasma entrance and decreases to 1:1 for films deposited downstream. Optical emission from the plasma is dominated by Li emission near the entrance, but Li emission disappears downstream, which we attribute to the complete consumption of the precursor. We hypothesized that the axially decreasing precursor concentration affects the electron energy distribution function in a way that causes different dissociation efficiencies for the production of Li and Si. We used Li line intensities to estimate the local precursor concentration and Ar line ratios to estimate the local reduced electric field to test this hypothesis. This analysis suggests that the mean electron energy increases along the reactor axis with decreasing precursor concentration. As a result, the decreasing Li-to-Si ratio with axially decreasing precursor concentration may be explained by Li release from the precursor having lower threshold energy than Si release.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Separation and conversion of carbon dioxide to syngas using a porous ceramic dual membrane in a thermo-electrochemical reactor

A thermo-electrochemical reactive capture apparatus includes an anode and a cathode, wherein the anode includes a first catalyst, wherein the cathode includes a second catalyst, a porous ceramic support positioned between the anode and the cathode, an electrolyte mixture in pores of the ceramic support, and a steam flow system on an outer side of the cathode. The outer side of the cathode is opposite an inner side of the cathode and the inner side of the cathode is adjacent to the ceramic support. In addition, the electrolyte mixture is configured to be molten at a temperature below about 600° C.

Campbell, Patrick↗
DOE OSTI2021

Atomic layer deposition of sodium fluoride thin films

The need for advanced energy conversion and storage devices remains a critical challenge amid the growing worldwide demand for renewable energy. Metal fluoride thin films are of great interest for applications in lithium-ion and emerging rechargeable battery technologies, particularly for enhancing the stability of the electrode-electrolyte interface and thereby extending battery cyclability and lifetime. Reported within, sodium fluoride (NaF) thin films were synthesized via atomic layer deposition. NaF growth experiments were carried out at reactor temperatures between 175 and 250 °C using sodium tert-butoxide and HF-pyridine solution. Here, the optimal deposition temperature range was 175–200 °C, and the resulting NaF films exhibited low roughness (R q ≈ 1.6 nm for films of ~8.5 nm), nearly stoichiometric composition (Na:F = 1:1.05) and a growth per cycle value of 0.85 Å/cycle on SiO 2 substrates. These results are encouraging for future applications of NaF thin films in the development of improved energy capture and storage technologies.

25 ENERGY STORAGE↗
DOE OSTI2021

Parametric Study of Used Nuclear Oxide Fuel Constituent Dissolution in Molten LiCl-KCl-UCl 3

Prior work identified dissolution of used nuclear oxide fuel constituents from a uranium oxide matrix into molten LiCl-KCl-UCl 3 at 500°C, prompting a subsequent series of three progressive studies (including an initial scoping study, an electrolytic dissolution study, and a chemical-seeded dissolution study) to further investigate associated parameters and mechanisms. Thermodynamic calculations were performed to identify possible reaction mechanisms and their propensities in used oxide fuel constituent dissolution. Used nuclear oxide fuels with varying preconditions from fast and thermal test reactors were separately immersed in the subject salt system to assess fuel constituent migration from the bulk fuel matrix to the salt phase in an initial scoping study. Dissolution of expected fuel constituents, including alkali, alkaline earth, lanthanide, and transuranium oxides, into the chloride salt phase varied widely, ranging from 12% to 99% in the initial study. Uranium isotope blending between the salt phase and bulk fuel matrix was also observed, which was attributed to reducing conditions in the fuel matrix. Electrolytic and chemical-seeded dissolution studies were subsequently performed to effect reducing conditions in the fuel. Other parameters, including temperature (at 500°C, 650°C, 725°C, and 800°C) and uranium trichloride concentrations (at 6, 9, and 19 wt% uranium), were investigated in the latter two studies, resulting in fuel constituent dissolution above 90%. Extents of dissolution were based on initial and final fuel constituent concentrations in the oxide fuels following operations in the salt and subsequent removal of the salt via distillation. Finally, in this series of progressive studies, oxide fuel preconditioning and in situ reducing conditions, along with elevated temperature and uranium trichloride concentrations, were the primary parameters promoting used nuclear oxide fuel constituent dissolution in accordance with identified reaction mechanisms.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Pilot microbial electrolysis cell closes the hydrogen loop for hydrothermal wet waste conversion to jet fuel

The global shift toward net-zero emissions necessitates resource recovery from wet waste. In this study, we demonstrate the first feasibility of combining pilot-scale microbial electrolytic cells (MECs) with hydrothermal liquefaction (HTL) for simultaneous post-hydrothermal liquefaction wastewater (PHW) treatment and efficient hydrogen (H₂) production to meet biocrude upgrading requirements. Long-term single reactor operation revealed that fixed anode potential enabled rapid startup, and low catholyte pH and high salinity were effective in suppression of cathodic methanogenesis and acetogenesis – resulting in high current density of 16.6 A m –2 and 9.3 A m –2 when feeding synthetic wastewater and PHW respectively. Additionally, the anode biofilm exhibited spatial variations in response to local environmental conditions. In conclusion, onsite parallel or serial operations of multiple MECs showed good performance using actual PHW with a record-high H 2 production rate of 0.5 L L R day –1 for MEC over 10 liters scale, and the optimal chemical oxygen demand (COD)-to-H 2 yield reached 0.127 kg-H 2 per kg-COD, supporting a self-sufficient, closed-loop upgrade to jet fuel.

08 HYDROGEN↗