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DOE OSTI2020

Designing an impedance-based technique for studying corrosion on cladding materials

In nuclear cladding materials, changes in structure and chemistry over the lifetime of claddings can have a significant impact on fuel and reactor performance. Currently, chemical evolution over the lifetime of the fuel and cladding materials can only be inferred using post-irradiation examination. As an alternative to post-irradiation measurements, electrochemical impedance spectroscopy (EIS) can provide an in-pile measurement of changes in chemistry in oxides and hydrides. The objective of this study is to develop an impedance based sensing technology for measuring spatial- and time-resolved in-pile changes in cladding chemistry in order to understand the mechanisms of hydride formation, hydride dealloying and associated cladding corrosion so that a mitigation strategy and technology can be developed for reactor safe operation. Two prototype impedance-based sensors were designed and assembled using Zr-4 as working electrode and Pt as counter and reference electrode. One sensor is tubular type and the other one is plate-type. These sensors will be tested in static autoclave to investigate the effects of various environmental conditions (including temperature, pressure, and water chemistry) on cladding material corrosion mechanisms. These in-situ EIS sensors would provide corrosion-layer parameters in high-temperature water, such as (1) total layer thickness, (2) the evolution of oxide structures as uniform layer dielectric or sublayer(s), and (3) the possible electrochemistry of the volume corrosion process and the solid/liquid interface, such as the cyclic nature of corrosion of Zr alloys in high-temperature water. This work was focused on electrochemical sensor development, targeting cladding oxides/hydrides under thermodynamic equilibria; characterization of samples using Kelvin probe force microscopy (SKPFM), Raman spectroscopy, and scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS) to provide high-resolution co-localized characterization of zirconium oxide and metal/oxide interface.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Thrifting iridium for hydrogen

Using renewable electricity to produce hydrogen fuel reduces reliance on fossil fuels. Proton exchange membrane water electrolyzers (PEMWEs) are the highest-performing commercialized technology. These devices split water into oxygen gas and hydrogen ions (protons) at the anode. The protons then migrate through an ion-conducting polymer membrane (ionomer) to be reduced to hydrogen gas at the cathode. Further, the anode reaction’s harsh environment requires the use of precious-metal catalysts, such as iridium oxide (IrO x ). Given the expense and scarcity, the design of electrodes that minimize the use of precious metals without compromising the requisite stability and activity is desired for large-scale hydrogen production. On page 791 of this issue, Shi et al. report that anchoring IrO x catalysts onto porous cerium-oxide (CeO x ) supports maintains performance even with much reduced precious metal use.

08 HYDROGEN↗

DOE OSTI2020

Highly-Active and Contaminant-Tolerant Cathodes for Durable Solid Oxide Fuel Cells

The objective of this project is to investigate the fundamental degradation methods occurring in solid oxide fuel cell (SOFC) cathodes when exposed to chromium and carbon dioxide contamination and to rationally design alkaline earth-based catalysts to increase stability and tolerance to contaminate poisoning. With a mechanistic and fundamental understanding of the degradation methods, advanced catalytic surface modifications can be applied to reduce degradation. The specific technical objectives are: (1) To identify/develop new catalysts (alkaline-earth based-) that are compatible chemically with the state-of-the-art cathode materials at high temperatures required for fabrication and with contaminates commonly encountered under operating conditions; (2) To improve the infiltration process for optimal control of the thickness, composition, and uniformity of the catalyst coatings; (3) To evaluate the electro-catalytic activity toward ORR of the chemically-stable materials when exposed to different types of contaminants using electrical conductivity relaxation measurements on bar samples and performance evaluation of catalyst-infiltrated cathodes; (4) To unravel the contamination-tolerant mechanisms of the new catalyst coatings under realistic environmental conditions (with different types of contaminants) using powerful in situ and in operando characterization techniques performed on model cells with thin-film/pattern electrodes, as guided by modeling and simulation; (5) To establish scientific basis for rational design of new catalysts of high tolerance to contaminants; (6) To validate the long term stability of modified LSCF cathodes in commercially available cells/stacks under ROC. Alkaline earth-based catalysts have been systematically explored and tested under various contamination conditions. BaCoO 3-δ (BCO) was shown to produce the best catalytic activity enhancement as well as stability in a variety of contaminating conditions, including CO 2 and chromium. The microstructural evolution was investigated with SEM, EDS, and Raman spectroscopy, showing the BCO catalyst prevents the formation of insulating SrCrO 4 by forming electrically conductive BaCrO 4 . Electrochemical relaxation measurements determined the BCO catalyst coatings increased the surface diffusion coefficient but did not significantly affect the diffusion coefficient and determined an optimum surface modification layer of 100 nm. A novel Ba 0.9 Co 0.7 Fe 0.2 Nb 0.1 O x (BCFN) catalyst was also shown to have excellent stability in chromium containing atmospheres. A novel surface sol-gel (SSG) surface modification, which offers superior thickness and compositional control, was applied to SOFCs to produce BaO catalyst coatings. SSG BaO coatings were shown to produce conformal coatings on the electrode surface, greatly 4 increasing stability in chromium containing atmospheres. An atomic level mechanistic approach was applied to investigate the stability of PrBa 0.8 Ca 0.2 Co 2 O 5+δ (PBCC) with respect to a variety of common contaminants, demonstrating thermodynamically its superior stability in CO 2 containing atmospheres. Finally, the best catalyst coatings demonstrated in this project, BCO and PBCC, were applied to full cells which demonstrated superior stability for over 300 hours in CO 2 and Cr atmospheres

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2022

Electrocatalytic water oxidation performance in an extended porous organic framework with a covalent alliance of distinct Ru sites

The rational synthesis of durable, earth-abundant efficient electrocatalysts for the oxygen evolution reaction (OER) from water is one of the most important routes for storing renewable energy and minimizing fossil fuel combustion. The prime hurdles for effectively utilizing commercial RuO 2 as (OER) electrocatalysts are its very low stability, catalyst deactivation, and high cost. In this work, we explored a Ru-integrated porous organic polymer (Ru@Bpy-POP) by a facile one-pot Friedel–Crafts alkylation strategy between redox-active (Ru(demob) 3 Cl 2 ) and a carbazole unit, which is composed of unique features including an extended framework unit, isolated active sites, and tunable electrode kinetics. Ru@Bpy-POP can serve as a bridge between a Metal–Organic Framework (MOF) and POP-based catalytic systems with a balanced combination of covalent bonds (structural stability) and open metal sites (single site catalysis). Ru@Bpy-POP, deposited on a three-dimensional nickel foam electrode support, exhibits a promising electrocatalytic OER activity with an ultra-low ruthenium loading compared to a benchmark RuO 2 catalyst, providing an overpotential of about 270 mV to reach 10 mA cm –2 in an alkaline medium. Moreover, a high current density of 248 mA cm –2 was achieved for the Ru@Bpy-POP catalyst at only 1.6 V (vs. RHE), which is much higher than 91 mA cm –2 for commercial RuO 2 . The robust, albeit highly conjugated, POP framework not only triggered facile electro-kinetics but also suppressed aggregation and metallic corrosion during electrolysis. In particular, the benefits of covalent integration of distinct Ru sites into the framework can modulate intermediate adsorption and charge density, which contributes to its exceptional OER activity. All of the critical steps involved in OER are complemented by Density Functional Theory (DFT) calculations, which suggest that electrocatalytic water oxidation proceeds from a closed-shell configuration to open-shell electronic configurations with high-spin states. Finally, these open-shell configurations are more stable than their closed-shell counterparts by 1 eV, improving the overall catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

A contactless in situ EFISH method for measuring electrostatic potential profile of semiconductor/electrolyte junctions

In photoelectrochemical cells, promising devices for directly converting solar energy into storable chemical fuels, the spatial variation of the electrostatic potential across the semiconductor–electrolyte junction is the key parameter that determines the cell performance. In principle, electric field induced second harmonic generation (EFISH) provides a contactless in situ spectroscopic tool to measure the spatial variation of electrostatic potential. However, the total second harmonic generation (SHG) signal contains the contributions of the EFISH signals of semiconductor space charge layer and the electric double layer, in addition to the SHG signal of the electrode surface. The interference of these complex quantities hinders their analysis. In this work, to understand and deconvolute their contributions to the total SHG signals, bias-dependent SHG measurements are performed on the rutile TiO2(100)–electrolyte junction as a function of light polarization and crystal azimuthal angle (angle of the incident plane relative to the crystal [001] axis). A quadratic response between SHG intensity and the applied potential is observed in both the accumulation and depletion regions of TiO2. The relative phase difference and amplitude ratio are extracted at selected azimuthal angles and light polarizations. At 0° azimuthal angle and s-in–p-out polarization, the SHG intensity minimum has the best match with the TiO2 flatband potential due to the orthogonal relative phase difference between bias-dependent and bias-independent SHG terms. We further measure the pH-dependent flatband potential and probe the photovoltage under open circuit conditions using the EFISH technique, demonstrating the capability of this contactless method for measuring electrostatic potential at semiconductor–electrolyte junctions.

Chemistry↗

DOE OSTI2025

Modeling a High-Temperature Electrochemically Driven Water-Gas-Shift Process Using a Mixed-Conducting Membrane without External Electrical Power

This paper develops a model to predict and interpret the performance of an elevated-temperature, electrochemical, membrane-assisted, water-gas-shift process. The process uses separated feed streams of H 2 O and CO to produce separated streams of H 2 and CO 2 , without an external electrical power source. The dense ceramic membrane is mixed ionic-electronic-conducting (MIEC) gadolinium-doped ceria (GDC) and the porous composite electrodes are Ni-YSZ. At elevated temperature, GDC conducts both oxygen ions and small polarons. The present process uses chemical potential to drive the process. Electrochemical oxidation of CO proceeds within the composite anode and H 2 O reduction proceeds within the composite cathode. At high temperature (e.g., T > 700 °C), GDC has significant electronic leakage in the form of a reduced-cerium small polaron, which supports the charge-transfer reactions. In a typical electrolyzer or fuel cell, this leakage is significantly problematic. However, the present process depends on the leakage current to complete the electrochemical circuit. Model development and validation is based on measured material properties and reactor performance. Potential applications include using CO-rich blast-furnace off gases in steel processing, producing separated streams of H 2 and CO 2 .

Zhu, Huayang↗

DOE OSTI2025

Constructing Highly Durable Fuel Cell Catalysts Through Integrating Graphitic Shell‐Protected Composite Carbon Support with Gaseous Co Deposition‐Driven PtCo Intermetallics

Metal dissolution, nanoparticle agglomeration, and carbon support corrosion cause significant performance degradation of current PtCo catalysts under acidic and oxidative oxygen reduction reaction. Here, in this study, an integrated strategy is presented to design high-performance Pt 3 Co intermetallic catalysts by regulating gaseous Co deposition-driven diffusion into Pt nanoparticles supported on a composite carbon. The composite carbon is derived from ZIF-8/polyaniline, consisting of a high-surface-area (HSC) core and a protective graphitic shell (GS), which is employed to design 40 wt.% Pt/HSC@GS catalyst. The corresponding membrane electrode assemblies (MEAs) can maintain 1.09 A cm −2 at 0.7 V (20. 7% loss) after 10 000 cycles (1.0–1.5 V for carbon stability) and 1.15 A cm −2 (16.1% loss) after 150 000 cycles (0.60–0.95 V for catalyst stability). A ordered Pt 3 Co intermetallic is synthesized via a gaseous Co-deposition process, which yields a homogeneous Co-rich layer onto the Pt nanoparticles on the composite support, thereby facilitating Co diffusion into Pt crystal during subsequent ordering annealing to form the ordered intermetallic structure. This gaseous deposition leads to a thin carbon layer on PtCo nanoparticles, inhibiting particle growth during the annealing and mitigating Co dissolution under dynamic electrochemical conditions. The PtCo catalyst achieves impressive MEA performance and long-term durability (1.45 A cm −2 at 0.7 V after 120 000 cycles) under heavy-duty conditions.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2023

Low-Temperature Electrochemical Wastewater Oxidation

Here, we demonstrated the Clean Sustainable Electrochemical Treatment (CleanSET) process that enables the distributed clean-up of biomass-derived wastewater while simultaneously generating hydrogen (H 2 ). The specific goal of this project is to 1) demonstrate the selective removal of chemical oxygen demand (COD), total carbon (TC), and total nitrogen (TN) of different wastewaters, 2) optimize the electrode composition to improve electrochemical performance, and 3) perform a high-level techno-economic analysis to obtain levelized costs of disposal (LCOD) .

08 HYDROGEN↗

NASA NTRS1989

A survey of advanced battery systems for space applications

The results of a survey on advanced secondary battery systems for space applications are presented. The objectives were: to identify advanced battery systems capable of meeting the requirements of various types of space missions, with significant advantages over currently available batteries, to obtain an accurate estimate of the anticipated improvements of these advanced systems, and to obtain a consensus for the selection of systems most likely to yield the desired improvements. Few advanced systems are likely to exceed a specific energy of 150 Wh/kg and meet the additional requirements of safety and reliability within the next 15 years. The few that have this potential are: (1) regenerative fuel cells, both alkaline and solid polymer electrolyte (SPE) types for large power systems; (2) lithium-intercalatable cathodes, particularly the metal ozides intercalatable cathodes (MnO2 or CoO2), with applications limited to small spacecrafts requiring limited cycle life and low power levels; (3) lithium molten salt systems (e.g., LiAl-FeS2); and (4) Na/beta Alumina/Sulfur or metal chlorides cells. Likely technological advances that would enhance the performance of all the above systems are also identified, in particular: improved bifunctional oxygen electrodes; improved manufacturing technology for thin film lithium electrodes in combination with polymeric electrolytes; improved seals for the lithium molten salt cells; and improved ceramics for sodium/solid electrolyte cells.

Attia, Alan I.↗

DOE OSTI2023

A scalable membrane electrode assembly architecture for efficient electrochemical conversion of CO2 to formic acid

Abstract The electrochemical reduction of carbon dioxide to formic acid is a promising pathway to improve CO 2 utilization and has potential applications as a hydrogen storage medium. In this work, a zero-gap membrane electrode assembly architecture is developed for the direct electrochemical synthesis of formic acid from carbon dioxide. The key technological advancement is a perforated cation exchange membrane, which, when utilized in a forward bias bipolar membrane configuration, allows formic acid generated at the membrane interface to exit through the anode flow field at concentrations up to 0.25 M. Having no additional interlayer components between the anode and cathode this concept is positioned to leverage currently available materials and stack designs ubiquitous in fuel cell and H 2 electrolysis, enabling a more rapid transition to scale and commercialization. The perforated cation exchange membrane configuration can achieve >75% Faradaic efficiency to formic acid at <2 V and 300 mA/cm 2 in a 25 cm 2 cell. More critically, a 55-hour stability test at 200 mA/cm 2 shows stable Faradaic efficiency and cell voltage. Technoeconomic analysis is utilized to illustrate a path towards achieving cost parity with current formic acid production methods.

08 HYDROGEN↗

NASA NTRS1978

Solid Polymer Electrolyte (SPE) fuel cell technology program

Many previously demonstrated improved fuel cell features were consolidated to (1) obtain a better understanding of the observed characteristics of the operating laboratory-sized cells; (2) evaluate appropriate improved fuel cell features in 0.7 sq ft cell hardware; and (3) study the resultant fuel cell capability and determine its impact on various potential fuel cell space missions. The observed performance characteristics of the fuel cell at high temperatures and high current densities were matched with a theoretical model based on the change in Gibbs free energy voltage with respect to temperature and internal resistance change with current density. Excellent agreement between the observed and model performance was obtained. The observed performance decay with operational time on cells with very low noble metal loadings (0.05 mg/sq cm) were shown to be related to loss in surface area. Cells with the baseline amount of noble catalyst electrode loading demonstrated over 40,000 hours of stable performance.

Source record↗

DOE OSTI2022

Crucible Melter Simulation in Nek5000

Nuclear tank waste at the Hanford site is slated for vitrification in large scale refractory-lined melters to transform it into a stable borosilicate waste form suitable for long-term storage or disposal. Molten glass corrodes the refractory lining over time at a rate correlated to the velocity of molten glass against the refractory-lined wall. To properly design a melter and plan for maintenance, it is necessary to accurately model the glass flow and find the correlation between flow velocity and corrosion rate. This modeling was started in STAR-CCM+ CFD software and is being continued in Nek5000 for its fast-running and quick turnaround code. This poster explains the basic process of reconstructing the geometry, fluid properties, and heating of test melters in Nek5000. The geometry is imported from a mesh file and boundary conditions assigned based on surface IDs. The fluid properties are set in the .par and .usr case files. The heating of the actual crucibles in joule heating with electrodes but simulated in Nek5000 with a volumetric heat source term. This volumetric heat source is fit to the actual heating profile with piecewise polynomials and exponentials. Basic results and verification methods are explained in the poster, as well as further work that must be done to complete modeling.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Electrochemical Manipulation and Radiolytic Evaluation of Organic Phase Neptunium

Post for LDRD Annual Poster Session Under envisioned used nuclear fuel reprocessing conditions, neptunium (Np) is present in a mixture of extractable Np(IV)/Np(VI) and inextractable Np(V) species, the distribution of which is dependent on several factors that lead to the unintentional partitioning of Np into various phases and product streams, reducing process and cost efficiency. With this in mind, we tested an innovative approach to precisely control the oxidation state distribution of Np using novel, high surface area, optically transparent, ligand modified tin-doped indium oxide electrodes (LMEs). These proof-of-concept experiments employed a variety of radiation and electrochemistry (echem) techniques to determine: electrode radiation stability; aqueous echem behavior of Np at nITO|P3 electrode surfaces; radiation-induced Np-extractant reaction kinetics; and non-aqueous echem of Np in diethylhexyl butyramide (DEHBA) solutions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2025

Photoionization of seeded combustion products as a method of enhancing the efficiency of magnetohydrodynamic power generators

Here, in this study, we performed an experimental and computational investigation into the feasibility of utilizing photoionization to enhance the electrical conductivity of seeded oxy-fuel combustion products and improve the performance of magnetohydrodynamic (MHD) power generators. We applied a variety of optical and microwave diagnostics to study the ionization and recombination processes of potassium excited by an excimer laser in a high-velocity oxy-fuel free jet. Computational fluid dynamic (CFD) simulations were performed to model the thermophysical properties and species densities of the free jet. The CFD results were validated with position-dependent potassium concentration measurements. Electron recombination exponential lifetimes were measured through time-resolved microwave transmission. The experimental electron lifetimes were compared with lifetimes calculated from CFD-predicted species densities and literature recombination rates. It was determined that K + or O 2 are the most likely recombination partners for photoionized electrons. Time-resolved fluorescence measurements provided evidence of an ionization pathway involving a two-photon ionization of KOH . Finally, a zero-dimensional chemical kinetic model was developed to assess the fundamental viability of inducing a non-equilibrium electron population to provide a net energy return in combustion-driven MHD power generators. We determined that a high energy return is feasible for targeting electrode boundary layers with ultraviolet photoionization. We also found that photoionization could potentially lower the required temperature of the bulk gas flow.

20 FOSSIL-FUELED POWER PLANTS↗

NASA NTRS1981

Preparation and evaluation of advanced electrocatalysts for phosphoric acid fuel cells

A number of electrocatalyst combinations were prepared and characterized. These electrocatalysts were formulated to contain platinum combined with transition metal carbide forming elements (W, Mo, V) for cathodes and platinum combined with palladium for anodes. High resolution electron microscopy was used to determine the crystallite size and dispersion of platinum-palladium alloy electrocatalysts in order to provide analytical support for the electrochemical determinations of the particle dispersions. An equation was derived which correlates palladium crystallite size with electrochemical hydrogen adsorption. Based on comparisons of electrocatalyst performances in the presence of pure hydrogen and hydrogen containing carbon monoxide, it was shown that the apparent poisoning of the electrocatalyst by carbon monoxide is influenced by the electrode structure.

Stonehart, P.↗

DOE OSTI2020

A high-temperature mixed potential CO gas sensor for in situ combustion control

An in situ, accurate and robust sensor that can sustain a high temperature of above 1000 °C is needed for on-site combustion monitoring because it can give real-time and local data to the control system to adjust the overall combustion efficiency. In this work, we find that nickel oxide (NiO) is a promising sensing material for CO which is a direct indicator of the status of the combustion process of a power plant. Under the conditions of 0.5–3% O 2 and 1000 °C, the fabricated yttrium-stabilized zirconia (YSZ)-based mixed potential sensor using porous NiO demonstrates good sensitivity to CO, showing a signal as high as 36 mV to 1000 ppm CO. The effects of gas transport, structure and geometry of the NiO electrode on the sensing performance are studied. Results show that fast gas transport is much beneficial to improved sensitivity. NiO having a porous structure is much more sensitive to CO than that having a dense structure. But the t90 (time to achieve 90% final signal magnitude) of the former is much longer due to slower gas diffusion inside the pores. It's worth noting that the NiO sensor exhibits a positive relationship with the CO content, opposite to other reported results of mixed potential sensors to detect CO. We find that this might be due to the electrochemical reduction, instead of oxidation of CO during the interaction with NiO at 1000 °C. Selectivity tests on how CO 2 , CH 4 and steam affect CO sensing are also demonstrated. NiO is insensitive to even 10% CO 2 . CH 4 does not shift the average value of the CO sensing response. However, it makes the sensing signal fluctuate more intensively. 2% steam exerts a great influence on NiO sensitivity to CO: it magnifies the sensitivity of the porous NiO electrode to a low CO range of 0–100 ppm, but inhibits its sensitivity to a CO range of 100 ppm to 1000 ppm. Lastly, an 11 day stability test demonstrates the promising stability property of the proposed NiO-based YSZ sensor.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2024

Stabilization of Ni-YSZ Anodes in Solid Oxide Fuel Cells using an ALD-Grown Aluminum Titanate Interlayer

The effect of an Al 2 TiO 5 (ALT) interlayer between Ni and YSZ on enhancing the thermal stability of Ni-YSZ solid oxide fuel cell was examined. Atomic layer deposition (ALD) was used to provide precise control of the structure and thickness of the ALT interlayer. The study's findings demonstrate that a 2 nm thick ALT interlayer deposited by ALD does not adversely affect the cell's ohmic resistance and effectively prevents Ni sintering and the loss of active area during high-temperature heat treatments. ALT layers thicker than 2 nm, although they enhanced Ni stability, were found to impede oxygen ion transport in the electrode and significantly increase the ohmic resistance of the cell, leading to a decline in performance.

25 ENERGY STORAGE↗

DOE OSTI2021

Direct Observation of Photoexcited Charge Carrier Dynamics and Electrostatic Fields at Photocatalytic Semiconductor/liquid Interfaces

Photoelectrochemical conversion of solar energy to fuels at semiconductor-liquid interfaces involves a complex set of processes, which include band bending, built-in electric fields, surface recombination of photoexcited carriers, and ultimately charge transfer to the ions in solution, in which the electrostatic fields within the depletion region of the semiconductor plays an important role. There are loss mechanisms associated with each of these key components in the overall photoelectrochemical conversion efficiency. Direct probe of these elementary processes is key to the rational improvement of photoeletrochemical cells and electrodes. In this collaborative project, Tianquan Lian at Emory University, Steve Cronin at University of Southern California and their students and postdoctoral fellows carried out a series of studies that are aimed at direct observation of photoexcited charge carrier dynamics at photocatalytic semiconductor/liquid interfaces. The collaborative work led to the development of transient reflectance spectroscopy as a tool for in situ probing of carrier dynamics in planar photoelectrode/electrode interface; and the demonstration that this tool can be used to study oxide protected GaP to identify key efficiency limiting factors in these photoelectrodes. This work has led to the development a tool for in situ probing of carrier dynamics in planar photoelectrodes, which will facilitate the mechanistic study of photoelectrochemical cells. This work informs the development of better photoelectrode materials for solar water splitting and CO 2 reduction. This work has contributed to the training of three PhD students in the area of photoelectrochemistry, ultrafast spectroscopy and solar energy conversion

14 SOLAR ENERGY↗