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At least 73 records · Page 4

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DOE OSTI2026

Development of a Chlorine Cathode and Anode Basket Assembly for Production of Uranium Chloride

A chlorine cathode has been developed for in situ chlorination of metals, oxides, and oxychlorides in molten chloride electrolytes that could be used to support synthesis of chloride fuel salts for molten salt reactors. The chlorine cathode is designed to electrochemically reduce chlorine gas to generate chloride ions that, when paired with a metal anode, chlorinate that metal as it is oxidized into the salt. The designed porous carbon electrode effectively distributes Cl 2 to the electrode surface and efficiently generates Clions in the molten chloride electrolyte. This report highlights recent improvements made to the electrode assembly, with a focus on operational control of the anode basket stability. Synthesis tests demonstrated the successful chlorination of uranium metal, resulting in 3.6 wt% uranium generated in the LiCl-KCl base salt in 45 minutes, performed in a bench-scale chlorination apparatus. Higher concentrations could be achieved by applying longer chlorination times or increasing the amount of uranium loaded in the anode basket. Overall, the chlorine cathode can be used with an appropriately designed anode to chlorinate uranium in situ for synthesis of molten salt reactor fuel salts.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Electrochemical Reaction Engineering: A Lost (and Found) Art

The heart (or, perhaps more appropriately, the stomach) of any chemical manufacturing process is the reactor, where chemical and physical transformations occur under precisely controlled conditions. For non-electrochemical industrial processes, the design, optimization and operation of chemical reactors are extremely well developed, drawing upon the principles of chemistry, physics, calculus and economics. However, electrolytic processes face a dearth of well documented reaction engineering principles and design practices. This tutorial-style poster presentation introduces electrochemistry students and industrial practitioners to the "lost art" of reaction engineering and its organic extensions to electrochemical devices. Electrochemical reactor fundamentals and illustrative design equations are presented alongside a proposed five-step generalizable methodology for electrochemical reactor scale-up. Overall, this contribution seeks to educate electrochemistry researchers on practical means of reducing laboratory technologies to commercial practice.

electrochemistry↗

DOE OSTI2021

A mini-review on proton conduction of BaZrO 3 -based perovskite electrolytes

Abstract Proton conducting ceramics show promise in fuel cells, electrolyzers, permeation membranes, sensor applications, and membrane reactors. Among several types of materials that exhibit proton conduction, perovskite oxides show high proton conductivity at intermediate temperatures, presenting potential benefits for long-term use and lower costs for energy applications. Doped barium zirconate, BaZrO 3 , is a material that has shown high proton conductivity with encouraging chemical stability. Therefore, it is considered a promising material especially for proton-conducting solid oxide electrochemical cells. Although the proton conduction of doped BaZrO 3 has been extensively characterized, the specific phenomena behind its proton conduction are not fully understood. Only recently have specialized techniques and computational tools begun to elucidate the phenomena that determine the conduction properties of the material. In this mini review, an evaluation of the factors affecting the proton conductivity of doped BaZrO 3 perovskites and the phenomena governing variations in proton concentration and mobility are presented. Special attention is given to proton interactions with dopants and their resulting effect on hydration and transport properties. Technical strategies are provided to give some guidance on the development of protonic ceramics in energy conversion applications.

08 HYDROGEN↗

DOE OSTI2022

Effect of thermal aging on corrosion behavior of duplex stainless steels

Abstract Despite their exceptional mechanical and corrosion properties, duplex stainless steels (DSS) have not found widespread use in high-temperature applications due to concerns over thermal aging and embrittlement at elevated operational temperatures (> 300 °C). The present study investigated the effect of thermal aging time on the electrochemical properties of lean and standard grade DSS that are exposed to a range of pressurized water reactors containing LiOH and H 3 BO 3 . The results indicated that the electrolyte chemistry plays a significant role in the corrosion behavior of the DSS alloys. Corrosion resistance decreased with thermal aging time for all DSS alloys; however, standard grade DSS (2205 and 2209-w) alloys showed better corrosion resistance than lean grades (2003, 2101, 2101-w). The presence of dissolved oxygen in the electrolytes resulted in a significant increase in corrosion rate for the DSS alloys, but it did not affect the general trend of corrosion rates with aging time. All DSS alloys became vulnerable to pitting corrosion due to chloride addition, but the pitting resistance decreased with increasing thermal aging time. Increased boron B content resulted in degradation of corrosion resistance of the DSS alloys, while minor changes in pH did not show a significant change in corrosion resistance. Mechanical and metallurgical characterization coupled with electrochemical characterization of the DSS alloys gave a comprehensive insight into the effects of thermal aging on the electrochemical response of the DSS. Graphical abstract

Murkute, Pratik (ORCID:0000000278636346)↗

NASA NTRS2012

Joule-Heated Molten Regolith Electrolysis Reactor Concepts for Oxygen and Metals Production on the Moon and Mars

The maturation of Molten Regolith Electrolysis (MRE) as a viable technology for oxygen and metals production on explored planets relies on the realization of the self-heating mode for the reactor. Joule heat generated during regolith electrolysis creates thermal energy that should be able to maintain the molten phase (similar to electrolytic Hall-Heroult process for aluminum production). Self-heating via Joule heating offers many advantages: (1) The regolith itself is the crucible material, it protects the vessel walls (2) Simplifies the engineering of the reactor (3) Reduces power consumption (no external heating) (4) Extends the longevity of the reactor. Predictive modeling is a tool chosen to perform dimensional analysis of a self-heating reactor: (1) Multiphysics modeling (COMSOL) was selected for Joule heat generation and heat transfer (2) Objective is to identify critical dimensions for first reactor prototype.

Sibille, Laurent↗

NASA NTRS1977

Efficiency and cost advantages of an advanced-technology nuclear electrolytic hydrogen-energy production facility

The concept of an advanced-technology (viz., 1985 technology) nuclear-electrolytic water electrolysis facility was assessed for hydrogen production cost and efficiency expectations. The facility integrates (1) a high-temperature gas-cooled nuclear reactor (HTGR) operating a binary work cycle, (2) direct-current (d-c) electricity generation via acyclic generators, and (3) high-current-density, high-pressure electrolyzers using a solid polymer electrolyte (SPE). All subsystems are close-coupled and optimally interfaced for hydrogen production alone (i.e., without separate production of electrical power). Pipeline-pressure hydrogen and oxygen are produced at 6900 kPa (1000 psi). We found that this advanced facility would produce hydrogen at costs that were approximately half those associated with contemporary-technology nuclear electrolysis: $5.36 versus $10.86/million Btu, respectively. The nuclear-heat-to-hydrogen-energy conversion efficiency for the advanced system was estimated as 43%, versus 25% for the contemporary system.

Donakowski, T. D.↗

NASA NTRS2003

An Introduction to Mars ISPP Technologies

This viewgraph presentation provides information on potential In Situ Propellant Production (ISPP) technologies for Mars. The presentation discusses Sabatier reactors, water electrolysis, the advantages of methane fuel, oxygen production, PEM cell electrolyzers, zirconia solid electrolyte cells, reverse water gas shift (RWGS), molten carbonate electrolysis, liquid CO2, and ionic liquids.

Lueck, Dale E.↗

DOE OSTI2023

Improving Proton Conductivity by Navigating Proton Trapping in High Scandium-Doped Barium Zirconate Electrolytes

Proton-conducting oxides are used in intermediate-temperature (300 °C < T < 700 °C) applications of fuel cells, electrolyzers, membrane reactors, hydrogen pumps, and sensors. The proton conductivity of doped ABO 3 perovskites is partly dependent on the proton concentration and hence on the level of material hydration. However, how the material hydration ability is affected by differences in doping is not fully understood. Here, we show the prospect of proton trapping and detrapping that influences material hydration and dehydration. The proton-trapping influence is significant for Sc-doped BaZrO 3 compared to Y-doped BaZrO 3 . Here, our work offers a perspective to understand how defect interaction/associations influence the hydration ability of proton-conducting oxides. Furthermore, positron annihilation lifetime spectroscopy was revealed to be a valuable technique for studying the proton-trapping phenomena and the defect chemistry of dense proton conductors. Density functional theory calculations also showed that a high hydration level in Sc-doped BaZrO 3 boosts proton migration. In contrast, the effect of boosting the proton migration due to increased hydration is limited for Y-doped BaZrO 3 . This effect, in turn, might explain the trend of conductivity with dopant concentration in doped BaZrO 3 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Electrochemical Conversion of CO 2 to Methyl Formate in a Flow Electrolyzer with Mixed Propylene Carbonate/Methanol Catholyte

Despite the promise of electrochemical carbon dioxide reduction as a technology for the production of clean fuels and decarbonization of the chemical industry, research has mostly focused on aqueous systems with a relatively limited set of products that have been achieved via electrosynthesis. Increasingly, CO 2 electroreduction in nonaqueous solvents is being pursued to develop new avenues for expanding the suite of products that can be made with high selectivity. CO 2 reduction in alcohols coupled with in situ esterification to produce esters is one such route that utilizes nonaqueous electrolyte. To be practical, such electrochemical syntheses need to be translated to a high-performance reactor such as a flow electrolyzer. However, many organic solvents, such as alcohols, wet and flood porous electrodes, thus impeding reactor performance. In this work, methanol was mixed with propylene carbonate as a catholyte for a gas-fed CO 2 flow electrolyzer that avoided cathode flooding. Simultaneously, a dual aqueous anolyte was used for water oxidation as a scalable and sustainable anodic half-reaction. The performance effect of methanol concentration, catholyte acidity, CO 2 flow rate, and dilute water in the catholyte were investigated. With 10 vol % methanol in 90 vol % propylene carbonate, 63% faradaic efficiency for methyl formate ester product was sustained without cathode flooding. However, improvements are still needed to lower the cell resistance and further increase the operating current density.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Green Methanol via an Integrated Direct Air Capture, CO 2 Electrolyzer, and Hydrogenation Reactor

This project pioneered a groundbreaking reactor design to produce green methanol by harnessing the electrochemical CO 2 reduction reaction (eCO 2 RR), a cornerstone of power-to-fuels technology. The effort integrated three innovative technologies to achieve carbon-neutral methanol production at a target cost of under $\$$800/ton: 1. Direct Air Capture (DAC): Using a cutting-edge sorbent material developed at Holocene, scalable models were developed to integrate captured atmospheric CO₂ into the reactor system. 2. Intermediate-Temperature CO 2 Electrolyzer: Developed by the University of Tennessee (UTK), this electrolyzer utilizes a cost-effective, proton-conducting solid acid electrolyte (CsH 2 PO 4 , CDP) and a mixed-metal oxide cathode. It achieves high faradaic efficiencies (>98%) by effectively suppressing hydrogen evolution at high current densities, converting CO 2 to CO with remarkable selectivity. 3. Catalysis and Reactor Engineering: Oak Ridge National Laboratory (ORNL) contributed world-class expertise in heterogeneous catalysis and reactor design. Their advanced ASPEN modeling drove systems integration and supported techno-economic and life cycle analyses. This effort was further bolstered by partnerships with industry leaders Air Company and Plug Power, who provided critical guidance on scaling, systems engineering, and the integration of water electrolyzers into large-scale operations. During Phase 1, the team focused on modeling and validating a lab-scale reactor demonstrating the feasibility of the integrated approach. Key accomplishments include a 52% increase in current density at 0.8 V while maintaining >98% CO faradaic efficiency, successful 10× scale-up of the electrolyzer with performance within 5% of coin-cell results, best-in-class durability (168-hour test at 0.6 V with 0.14 mA/cm 2 -h degradation), validated TEA confirming the $\$$800/ton methanol target, and completed preliminary LCA showing potential for net-negative GHG emissions under renewable energy scenarios.

10 SYNTHETIC FUELS↗

DOE OSTI2026

Progress and Perspectives: Zirconium Electrodeposition from Different Electrolytes

Zirconium (Zr) possesses outstanding properties, including exceptional chemical resistance and a high melting point, and is therefore desirable for use in a wide variety of challenging environments, such as in nuclear reactors and the chemical processing industry. To minimize the amount of Zr required for any given application, developing methods for generating metallic Zr coatings is highly advantageous. Owing to Zr’s highly negative reduction potential, electrodeposition in traditional solvents at near ambient temperatures remains challenging and thus not well understood. Due to the extreme conditions required to deposit this metal, extensive work has been conducted in molten salt electrolytes, however the broad applicability of this methodology is limited due to its corrosivity. The primary focus of this article is to present an overview of Zr’s electrochemical behavior and to consolidate the efforts of researchers in exploring electrodeposition techniques for Zr involving aqueous, organic, ionic liquid, deep eutectic, and molten salt solvents. With this information, we highlight trends across solvent systems and opportunities for future research.

42 ENGINEERING↗

DOE OSTI2023

Electrochemical Residence Time Distribution as a Diagnostic Tool for Redox Flow Batteries

The fluid dynamic and electrochemical performance of redox flow batteries (RFBs) stems from the relationship between the flow field and the porous electrode, whose interplay determines how active species move and react during device operation. While characterization techniques, such as residence time distribution, offer insights into species mobility within a reactive volume for a traditional chemical reactor, electrochemical reactors also enable simultaneous measurement of the redox reactions, unlocking another dimension of analysis. Herein, we demonstrate how potentiodynamic measurements, using injections of electrolyte examined through moment analysis, can provide electrode-specific performance scaling relationships across a matrix of carbon paper and cloth electrodes with flow through and interdigitated flow fields. We further combine experimental campaigns with multiphysics simulations to demonstrate how electrode surface area can be estimated with this technique, which we then validate with activated and unactivated commercial carbon cloth electrodes. These studies reveal the multiscale observations that potentiodynamic measurements afford, augmenting existing electrochemical techniques for holistic electrochemical reactor diagnostics.

Electrochemistry↗

NASA NTRS2006

Experimental Demonstration of the Molten Oxide Electrolysis Method for Oxygen and Iron Production from Simulated Lunar Materials

This paper presents the results of a Marshall Space Flight Center funded effort to conduct an experimental demonstration of the processing of simulated lunar resources by the molten oxide electrolysis (MOE) process to produce oxygen and metal from lunar resources to support human exploration of space. Oxygen extracted from lunar materials can be used for life support and propellant, and silicon and metallic elements produced can be used for in situ fabrication of thin-film solar cells for power production. The Moon is rich in mineral resources, but it is almost devoid of chemical reducing agents, therefore, molten oxide electrolysis, MOE, is chosen for extraction, since the electron is the most practical reducing agent. MOE was also chosen for following reasons. 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. In the experiments reported here, melts containing iron oxide were electrolyzed in a low temperature supporting oxide electrolyte (developed by D. Sadoway, MIT).

Curreri, P. A.↗

NASA NTRS2006

Lunar Metal Oxide Electrolysis with Oxygen and Photovoltaic Array Production Applications

Curreri, P. A.↗

DOE OSTI2025

High-Temperature Reference Electrode for Chloride Salts

The unique properties of molten salts enable their use in a wide range of applications, including metal electrodeposition, electrorefining, and as electrolytes in high-temperature batteries. Moreover, molten salts will be used as a coolant in molten salt reactors and as working media in pyrorocessing for nuclear energy applications. As a result, predicting the behavior and properties of the elements involved in the technological processes that employ molten salts is important. The activity of chloride ions in chloride molten salts has a large influence on the behavior of the salts in these applications and one of the key components in measuring the chloride activity is a stable reference electrode. This project aims to develop a reliable and convenient method for measuring chloride ion activity over a wide range of temperatures and salt compositions in chloride salt mixtures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1975

A preliminary systems-engineering study of an advanced nuclear-electrolytic hydrogen-production facility

An advanced nuclear-electrolytic hydrogen-production facility concept was synthesized at a conceptual level with the objective of minimizing estimated hydrogen-production costs. The concept is a closely-integrated, fully-dedicated (only hydrogen energy is produced) system whose components and subsystems are predicted on ''1985 technology.'' The principal components are: (1) a high-temperature gas-cooled reactor (HTGR) operating a helium-Brayton/ammonia-Rankine binary cycle with a helium reactor-core exit temperature of 980 C, (2) acyclic d-c generators, (3) high-pressure, high-current-density electrolyzers based on solid-polymer electrolyte technology. Based on an assumed 3,000 MWt HTGR the facility is capable of producing 8.7 million std cu m/day of hydrogen at pipeline conditions, 6,900 kPa. Coproduct oxygen is also available at pipeline conditions at one-half this volume. It has further been shown that the incorporation of advanced technology provides an overall efficiency of about 43 percent, as compared with 25 percent for a contemporary nuclear-electric plant powering close-coupled contemporary industrial electrolyzers.

Escher, W. J. D.↗

DOE OSTI2020

Molten Chloride Thermophysical Properties, Chemical Optimization, and Purification

Next-generation concentrating solar power (CSP) technology requires high-temperature heat-transfer fluids and thermal energy storage that can operate in the temperature range of 500°–720°C. This high temperature demands a new chemistry for the heat-transfer fluids that must have high-temperature thermal and chemical stabilities, high energy density, and low corrosion rate on metallic materials used in the heat exchangers, piping, and thermal energy storage tanks. A ternary MgCl 2 -KCl-NaCl chloride-salt system has been proposed to achieve such goals, given its high-temperature thermal stability. The chloride-salt-based systems have been used by the metallurgy industry as the electrolyte to electrolytically extract metallic magnesium. They have also attracted attentions from the nuclear industry for developing the molten salt fast reactors that can operate at close to atmospheric pressure and at higher temperature than traditional light-water reactors. However, the corrosion properties of the ternary salt are not well known. The corrosion mechanism is believed to be correlated to the presence of MgOHCl impurity at the operation temperature. MgOHCl is fundamentally caused by the hygroscopic nature of the MgCl 2 component. Therefore, the first key objective of this project is to understand the nature of the corrosiveness of the ternary chloride-salt system and its prevention by designing new lab-scale purification processes. Because of its importance, a working group called the Chloride Salt Collective across multiple U.S. Department of Energy national laboratories is established to gain experimental agreement on the corrosion behaviors. In addition, water generation during salt dehydration could lead to highly corrosive HCl/water mixture via a hydrolysis process between water and anhydrous MgCl 2 or MgCl 2 hydrates. MgOHCl will eventually be converted to MgO particulates regardless of the chemical path chosen (i.e., by thermal decomposition, chemical purification with an active metal, or electrochemical purification utilizing the reduction power of electron flows). Large MgO particles with high hardness can wear out bearing and bushing and even clog the delicate channels in the primary heat exchanger. Because of this, a second objective is to understand the chemistry behind salt purification and transfer the scientific understanding to a set of engineering know-how for large-scale salt melter design. Because there is limited information on the thermophysical properties and the sensitivity of these properties around the targeted salt composition, a third objective is to measure thermophysical properties relevant to system and component design and support Topic 1 Liquid Pathway development. For example, composition shift due to salt reaction with water can be a potential issue because it can lead to changes of thermophysical properties, such as (1) melting point (or freeze point), which can jeopardize safe operation of the supercritical CO 2 power cycle proposed for next-generation CSP, and (2) heat capacity and density, which can decrease the overall power-generation capability of the plants. The value of the thermal conductivity of the selected salt composition is also a critical criterion for the solar receiver design.

14 SOLAR ENERGY↗

NASA NTRS1979

Dedicated nuclear facilities for electrolytic hydrogen production

An advanced technology, fully dedicated nuclear-electrolytic hydrogen production facility is presented. This plant will produce hydrogen and oxygen only and no electrical power will be generated for off-plant use. The conceptual design was based on hydrogen production to fill a pipeline at 1000 psi and a 3000 MW nuclear base, and the base-line facility nuclear-to-shaftpower and shaftpower-to-electricity subsystems, the water treatment subsystem, electricity-to-hydrogen subsystem, hydrogen compression, efficiency, and hydrogen production cost are discussed. The final conceptual design integrates a 3000 MWth high-temperature gas-cooled reactor operating at 980 C helium reactor-out temperature, direct dc electricity generation via acyclic generators, and high-current density, high-pressure electrolyzers based on the solid polymer electrolyte approach. All subsystems are close-coupled and optimally interfaced and pipeline hydrogen is produced at 1000 psi. Hydrogen costs were about half of the conventional nuclear electrolysis process.

Foh, S. E.↗