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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 829 records · Page 46
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Ionomer-free nanoporous iridium nanosheet electrodes with boosted performance and catalyst utilization for high-efficiency water electrolyzers

Increasing the catalyst utilization efficiency and simplifying electrode fabrication processes are crucial to accelerate development of low-cost proton exchange membrane electrolyzer cells (PEMECs). Here, we develop a facile route to fabricate ionomer-free iridium nanosheet integrated electrodes, in which nanoporous iridium nanosheets (IrNS) with abundant exposed edges and nanopores are deposited on thin titanium liquid/gas diffusion layers (TT-LGDLs) via a low-temperature chemical synthesis strategy. Further, benefiting from high catalytic activity, good electrode conductivity and excellent liquid/gas transport properties, such nanoporous IrNS electrodes with low catalyst loadings require low cell voltages of 1.65 V and 1.78 V at 3000 and 6000 mA/cm 2 , respectively. More impressively, a stable performance can be well maintained under extremely high current density tests of 5000 mA/cm 2 , demonstrating the potential of low-loading nanoporous IrNS electrodes in solid-electrolyte based electrochemical conversion cells that require high current density operation.

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

Ionic liquid structure, dynamics, and electrosorption in carbon electrodes with bimodal pores and heterogeneous surfaces

In this paper, we investigate the aggregation, diffusion, and resulting electrochemical behavior of ionic liquids inside carbon electrodes with complex pore architectures and surface chemistries. Carbide-derived carbons (CDCs) with bimodal porosities and defunctionalized or oxidized electrode surfaces served as model electrode materials. Our goal was to obtain a fundamental understanding of room-temperature ionic liquid ion orientation, mobility, and electrosorption behavior. Neat 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide confined in CDCs was studied using an integrated experimental and modeling approach, consisting of quasielastic neutron scattering, small-angle neutron scattering, X-ray pair distribution function analysis, and electrochemical measurements, which were combined with molecular dynamics simulations. Our analysis shows that surface oxygen groups increase the diffusion of confined electrolytes. Consequently, the ions become more than twice as mobile in oxygen-rich pores. Although greater self-diffusion of ions translates into higher electrochemical mobilities in oxidized pores, bulk-like behavior of ions dominates in the larger mesopores and increases the overall capacitance in defunctionalized pores. Experimental results highlight strong confinement and surface effects of carbon electrodes on electrolyte behavior, and molecular dynamics simulations yield insight into diffusion and capacitance differences in specific pore regions. Finally, we demonstrate the significance of surface defects on electrosorption dynamics of complex electrolytes in hierarchical pore architectures of supercapacitor electrodes.

36 MATERIALS SCIENCE↗
DOE OSTI2023

An In Situ , multi-electrode electrochemical method to assess the open circuit potential corrosion of Cr in unpurified molten FLiNaK

An in situ electrochemical method to investigate the time-dependent spontaneous corrosion of pure Cr in an unpurified LiF-NaF-KF eutectic salt at 600 °C was developed. A multi-electrode electrochemical cell and a dual-electrode method were utilized to detect Cr(II) and Cr(III) ions on a platinum working electrode using cyclic voltammetry as a function of exposure time and compensating for the distance from the Cr electrode. XRD was performed to characterize the crystalline composition of the exposed FLiNaK and the salt films formed on the working electrodes. The fate of all electro-oxidized Cr must be accounted for to quantify corrosion rates. The concentrations of Cr(II) and Cr(III) species obtained were compared with the gravimetric mass change and ICP-OES analysis of the residual salt. Finally, outcomes, difficulties, and limitations are discussed.

ICP-OES↗
DOE OSTI2021

Morphology engineering of iridium electrodes via modifying titanium substrates with controllable pillar structures for highly efficient oxygen evolution reaction

Nowadays, Ti is the well-chosen anode substrate material for proton exchange membrane electrolyzer cells (PEMECs) and modifications of the substrate surfaces are essential for the fabrication of highly efficient electrodes. Herein, we introduce the morphology engineering of Ir/Ti electrodes with different acid treatments of hydrochloric acid (HCl) and oxalic acid (OA), and the comparative benefits of these two acid treatment methods are studied from the aspects of their impacts on the morphology, interfacial contact resistance (ICR), and oxygen evolution reaction (OER) performances of resultant electrodes. Notably, compared to the flat surface from OA treatment, Ti substrates with the pillar structure could be successfully achieved via HCl etching. Further, the HCl and the oxalic acid (OA) treatments would reduce the interfacial contact resistance (ICR) to 15.2% and 5.5% of the pristine Ti substrate at 1.38 MPa, respectively. By iridium electrodeposition on Ti substrates, Ir/Ti electrodes with different catalyst loadings are fabricated. With similar low-loadings of about 0.05 mgIr cm –2 , an Ir/Ti electrode with HCl treated substrate exhibits a lower overpotential of ~283 mV at 10 mA cm –2 current density than 305 mV from OA treatment, due to the boosted reaction areas from HCl treatment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Selective pseudocapacitive immobilization of REE elements on carbon based electrodes

Current extraction technologies for rare earth elements at ambient conditions are reagent and energy intensive, giving rise to significant quantities of secondary waste streams. Exploration of the removal of common cations from aqueous streams has been undertaken with carbon materials and have shown promising results. However, those promising materials have not been explored extensively for rare earth element capture from aqueous process streams. In this study, a carbon electrode was investigated for the adsorption and immobilization of REE elements from aqueous solutions. Cyclic voltammetry studies of the carbon electrode displayed a pseudocapacitive behavior where it was verified that cation adsorption is accompanied by an electron transfer process. Preliminary tests showed that a current density of 89.1 mA. g -1 , allowed for the pseudocapacitive adsorption (PSA) of Nd 3+ cation without the formation of rare earth hydroxides. Hence, the selective PSA of Nd 3+ was verified in an electrolyte solution with equimolar concentrations of Nd 3+ , Mg 2+ , Li + , Na + and K + , achieving separation factors of 8.6, 1.1, and 10.9 for Nd 3+ /Li + , Nd 3+ /Na + , and Nd 3+ /Mg 2+ , respectively. Analysis of the potential-time curves for the various cations suggests that storage of ions in the electrode involved pore-spacings rather than interlayer spacings and was corroborated by XRD analysis. Specific capacitance as high as >640 F.g -1 for Nd 3+ was also observed for the carbon electrode, with Faradaic efficiencies (FE) of > 20% for Nd 3+ and Mg 2+ , and > 9% for Na + . Furthermore, adsorption capacity of >125 mg g -1 after 4hrs of electrosorption was observed for Nd 3+ . In the presence of the Nd 3+ electrolyte, the electrode achieved increasing storage of Nd 3+ with >94% retention of Nd 3+ with a FE > 20% over 6 cycles between loading and releases in 1 M KCl solution. In conclusion, these preliminary results provide information and some guidance on the selective recovery of rare earth elements, such as Nd, in aqueous streams in the presence of competitive cations employing the use of carbon-based materials.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2022

Effect of particle size on thermodynamics and lithium ion transport in electrodes made of Ti 2 Nb 2 O 9 microparticles or nanoparticles

This study compares the charging mechanisms, thermodynamics, lithium ion transport, and operando isothermal calorimetry in lithium-ion battery electrodes made of Ti 2 Nb 2 O 9 microparticles or nanoparticles synthesized by solid-state or sol-gel methods, respectively. First, electrochemical testing showed that electrodes made of Ti 2 Nb 2 O 9 nanoparticles exhibited larger specific capacity, smaller polarization, and better capacity retention at large currents than those made of Ti 2 Nb 2 O 9 microparticles. Furthermore, potentiometric entropy measurements revealed that electrodes made of either Ti 2 Nb 2 O 9 microparticles or nanoparticles showed similar thermodynamics behavior governed by lithium intercalation in solid solution, as confirmed by in situ XRD measurements. However, electrodes made of Ti 2 Nb 2 O 9 nanoparticles featured smaller overpotential and faster lithium ion transport than those made of Ti 2 Nb 2 O 9 microparticles. In fact, operando isothermal calorimetry revealed smaller instantaneous and time-averaged irreversible heat generation rates at electrodes made of Ti 2 Nb 2 O 9 nanoparticles, highlighting their smaller resistive losses and larger electrical conductivity. Finally, the measured total heat generation over a charging/discharging cycle matched the measured net electrical energy loss. Overall, Ti 2 Nb 2 O 9 nanoparticles synthesized by the novel sol-gel method displayed excellent cycling performance and reduced heat generation as a fast-charging lithium-ion battery anode material. These features present major advantages for actual battery systems including larger energy and power densities, simpler thermal management, and enhanced safety.

25 ENERGY STORAGE↗
DOE OSTI2021

Favorable morphology and electronic conductivity of functional sublayers for highly efficient water splitting electrodes

Low electronic conductivities and improper morphologies of anode electrodes greatly limit the reaction area, catalyst utilization and efficiency in proton exchange membrane water electrolyzers. In this study, conductive sublayers with different conductivities and morphologies were introduced into anode electrodes in membrane-based water electrolyzers. In-situ and ex-situ investigation results showed that conductive sublayers (Au mesh and carbon nanotube (CNT) film) augmented the sheet conductivity of anode electrodes by up to 4000 times (from 2000 to 0.5 ohm square -1 ), and the ohmic resistance of water electrolyzers was reduced to 1/3 when inserting conductive sublayers. In addition, CNT film provided a higher electrochemical active area than Au mesh, because of favorable morphologies (large porosity and surface area) of CNT fibers on CNT films. Therefore, the current density of water splitting was increased by 3 times (from 4.55 mA cm -2 to 14.83 mA cm -2 ) at 2.5 V compared to a conventional anode electrode. Visualizations on bubble dynamics showed improved performances with conductive sublayers; this was mainly due to greatly increased number of reaction sites, highly spread reaction area (from 50 to 1000 um), and reduced activation overpotential. Therefore, a balance between high electronic conductivity and nanoporous morphology is essential to the anode electrode for larger reaction sites and areas in highly efficient water electrolyzers.

25 ENERGY STORAGE↗
DOE OSTI2022

Catalyst layer formulations for slot-die coating of PEM fuel cell electrodes

The series of electrodes were fabricated by the scalable and manufacturable slot-die coating method for proton exchange membrane fuel cell (PEMFC) application. The inks with different amounts of solids were studied by rheological methods in order to establish a coating window with minimum manufacturing defects. The obtained electrodes were characterized by SEM, AFM, and optical microscopy, which showed that they were uniform and homogeneous with minimum defects. The electrochemical evaluation of the manufactured gas diffusion electrodes (GDE) showed that the main characteristics of the electrodes, like electrochemical surface area, proton resistivity, and double layer capacitance, were found to be close for all samples confirming the reproducibility of the slot-die process. Additionally, we studied the effects of membrane thickness on the performance of the GDE membrane electrode assemblies and determined that a decrease in membrane thickness favored the performance. Furthermore, the obtained results clearly demonstrated the applicability and feasibility of the approach for the Manufacturing of catalyst layers for the fuel cell application with potential for future mass production.

08 HYDROGEN↗
DOE OSTI2023

Fundamental study of gas species transport in the oxygen electrode of solid oxide fuel and electrolysis cells

A fundamental analysis of multicomponent gas transport models was performed in application to the oxygen electrodes of solid oxide cells. It is common practice to neglect the effect of pressure gradients within oxygen electrodes, even though a net molar flux at the electrolyte surface implies that a pressure gradient must exist. The influence of both Darcy velocity and Knudsen flux are considered in the context of ordinary (Fickian) diffusion, the dusty gas model, and the binary friction model. Comparisons between the models and different sets of assumptions are made via parametric studies on operating load, oxygen partial pressure, microstructural properties, and electrode thickness. Results show that the pressure gradient will have a significant impact on the oxygen concentration distribution and therefore the concentration overpotential. In electrolysis mode, pressure increases up to 1 atm are predicted, indicating that pressure at the electrode/electrolyte interface could contribute to electrode delamination. Additionally, it is found that Darcy's law is insufficient for calculating the pressure distribution without accounting for the flux due to Knudsen diffusion. Additionally, it is found that for the range of properties typical of oxygen electrodes, there is a negligibly small difference between the dusty gas model and binary friction model from a practical standpoint.

08 HYDROGEN↗
DOE OSTI2018

Efficient 3D Printed Pseudocapacitive Electrodes with Ultrahigh MnO 2 Loading

Retaining sound electrochemical performance of electrodes at high mass loading holds critical importance to energy storage. Pseudocapacitive materials such as manganese oxide (MnO 2 ) deposited on current collectors have achieved outstanding gravimetric capacitances, sometimes even close to their theoretical values. However, this is only achievable with very small mass loading of active material typically less than 1 mg cm -2 . Increasing mass loading often leads to drastic decay of capacitive performance due to sluggish ion diffusion in bulk material. In this work, we demonstrate a 3D printed graphene aerogel electrode with MnO 2 loading of 182.2 mg cm -2 , which achieves a record-high areal capacitance of 44.13 F cm -2 . Most importantly, this 3D printed graphene aerogel/MnO 2 electrode can simultaneously achieve excellent capacitance normalized to area, gravimetry, and volume, which is the trade-off for most electrodes. This work successfully validates the feasibility of printing practical pseudocapacitive electrodes, which might revolutionize pseudocapacitor fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2013

A reduced graphene oxide/Co 3 O 4 composite for supercapacitor electrode

20 nm sized Co 3 O 4 nanoparticles are in-situ grown on the chemically reduced graphene oxide (rGO) sheets to form a rGO-Co 3 O 4 composite during hydrothermal processing. The rGO-Co 3 O 4 composite is employed as the pseudocapacitor electrode in the 2 M KOH aqueous electrolyte solution. The rGOCo 3 O 4 composite electrode exhibits a specific capacitance of 472 F/g at a scan rate of 2 mV/s in a two-electrode cell. 82.6% of capacitance is retained when the scan rate increases to 100 mV/s. The rGOCo 3 O 4 composite electrode shows high rate capability and excellent long-term stability. It also exhibits high energy density at relatively high power density. The energy density reaches 39.0 Wh/kg at a power density of 8.3 kW/kg. The super performance of the composite electrode is attributed to the synergistic effects of small size and good redox activity of the Co 3 O 4 particles combined with high electronic conductivity of the rGO sheets.

25 ENERGY STORAGE↗
DOE OSTI2017

Transition-metal redox evolution in LiNi 0.5 Mn 0.3 Co 0.2 O 2 electrodes at high potentials

The mixed transition-metal layered compound, LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532), is a promising high-energy cathode material. However, the required high-voltage (>4.3 V) cycling is accompanied by a rapid capacity fade associated with a complex redox mechanism that has not been clarified. Here in this paper, we report soft x-ray absorption spectroscopy of NMC532 electrodes, both pristine and those charged to 4.2, 4.35, or 4.5 V in graphite/NMC532 cells. A quantitative sXAS analysis shows that about 20% of the nickel exists as Ni 4+ in the as-synthesized NMC532. The Ni redox reaction contributes only to the experimental capacity obtained below 4.2 V, while Co redox reactions take place throughout the entire electrochemical cycling up to 4.5 V. In contrast to the changing ratio of the well-defined Ni 2+ , Ni 3+ and Ni 4+ ions, Co always displays ill-defined intermediate valence states in the charged NMC532 electrodes. This indicates an itinerant electron system in NMC electrodes related to the improved rate performance through Co doping. Furthermore, about 20% of Ni 2+ is found on the electrode surface at the high potential, which suggests that the electrode surface has either gone through surface reconstruction or reacted with the electrolyte at high voltage.

25 ENERGY STORAGE↗
DOE OSTI2019

Analysis of electrolyte imbibition through lithium-ion battery electrodes

A quantitative measurement of wettability between the porous electrode and the electrolyte in lithium-ion batteries can greatly improve our understanding of wetting behavior. Although the wetting balance method is widely used to measure the electrolyte transport rate in the porous electrodes, it suffers from several drawbacks and has limited accuracy. We here presented a combined experimental and theoretical investigation of the dynamics of electrolyte imbibition through electrodes. We suggested a novel method to accurately measure the electrolyte imbibition rate. Excellent agreement between the experimental data and the developed analytical model is obtained. The coefficient of penetrance (COP) and the solid permeability coefficient (SPC) are identified as important parameters, i.e., the electrolyte with higher COP value wets faster into an electrode, whereas for an electrolyte, the electrode with higher SPC value is more amenable to be impregnated. The effect of electrolyte salt concentration and electrolyte solvent has been studied in detail. The result implies that increasing salt concentration adversely influences electrolyte wetting rate, whereas switching from EC-DEC system to EC-EMC system improves electrolyte wetting rate. Moreover, for the electrolytes tested in this study, the imbibition into the uncalendered graphite anode is much faster than that into the uncalendered NMC532 cathode.

25 ENERGY STORAGE↗
DOE OSTI2019

High-throughput, super-resolution 3D reconstruction of nano-structured solid oxide fuel cell electrodes and quantification of microstructure-property relationships

Nano-structuring methods are actively applied to solid oxide fuel cell electrodes to reduce the operating temperature while preserving a high electro-catalytic activity. The unique nanoscale microstructure is vital to electrochemical performance, yet not well quantified in three dimensions. Here, with a multi-stage recovering principle of distance correlation functions, the three-dimensional microstructures of La 0.8 Sr 0.2 MnO 3-δ nanoparticles infiltrated porous Y 0.16 Zr 0.84 O 2-δ electrodes are reconstructed with a dimension of 1024 × 1024 × 1024 voxels at a resolution of 7.5 nm from one two-dimensional micrograph. The key geometric characteristics, such as tortuosity factors, active surface/interface areas and three-phase boundary length, are calculated from the reconstructed three-dimensional microstructures at various loadings of La 0.8 Sr 0.2 MnO 3-δ . Combining with the analysis of distribution of relaxation times, the active three-phase boundary length is shown to be the main factor governing the electrode impedance, and is related quantitatively to the electrochemical process at high frequency. The accuracy of capturing nanoscale features is validated by the focused ion beam sectioning dataset of a Ni-Y 0.16 Zr 0.84 O 2-δ electrode at nanoscale resolution. Lastly, this work provides a promising strategy for reconstructing three-dimensional heterogeneous nanostructures from one super-resolution two-dimensional micrograph, and demonstrates a quantitative approach for uncovering processing-structure-property relationships of nanostructured electrodes and beyond.

25 ENERGY STORAGE↗
DOE OSTI2022

The influence of temperature on area-specific impedance and capacity of Li-ion cells with nickel-containing positive electrodes

The temperature-dependent behaviors of five nickel-containing positive electrodes (NCA, NMC811, NMC622, NMC532, and NMC111) in lithium-ion batteries are investigated using an electrochemical protocol involving rate studies, mild aging (~100 cycles), and hybrid pulse power characterization (HPPC). Tests are conducted using coin-cells with graphite negative electrodes at -20 °C, 0 °C, 20 °C, and 40 °C. Three techniques are compared for determining the area-specific impedance (ASI): i) fits to the rate study average voltages, ii) fitting to the entire voltage curves using a regularization scheme, and iii) HPPC. When fit to an Arrhenius-type equation, all methods yield similar apparent activation energies (±2 kJ/mol) for the impedance, which range from -20 to -31 kJ/mol for the electrodes. Impedance growth increases with temperature but remains at less than 0.2% per cycle for most electrodes and temperatures. NCA and NMC811 are the exceptions, which yield 0.5% and 1.5% increases in ASI per cycle, respectively, at 40 °C. For cells with the same electrodes, the capacities are similar at 20 and 40 °C but reduce at lower temperatures, with up to a 52% reduction at -20 °C and 2C. The fade in energy of the cells during C/3 cycling is attributed to decreasing capacity as opposed to increasing ASI.

25 ENERGY STORAGE↗
DOE OSTI2025

Infiltrated electrodes for metal supported solid oxide electrolysis cells

Metal-supported solid oxide cells (MSOCs) are an alternative to conventional solid oxide cells (SOCs) based on ceramic cermets, offering lower material costs and higher operational flexibility. In this study symmetric MSOCs with infiltrated electrodes are explored for steam electrolysis operation to understand the underlying operation and degradation principles and suggest a direction for future MSOCs development. Two different fuel electrode backbones are used: an electronically-conductive lanthanum strontium co-doped iron nickel titanate (LSFNT) infiltrated with cerium-gadolinium oxide (CGO), or an ionic conductive zirconia based backbone (10ScYSZ) infiltrated with Ni:CGO. At the oxygen side, the backbone is 10ScYSZ, which is infiltrated with lanthanum-strontium co-doped cobalt oxide (LSC), or praseodymium oxide as cobalt-free alternative for comparison. This study suggests that the backbone electronic conductivity is key for good electrochemical performance as well as for boosting cell durability. Highly electronically conductive nanoparticles, especially nickel, were observed to irreversibly agglomerate driven by thermal conditions, whereas CGO proved to be a very stable electrocatalyst. At the fuel side, CGO (LSFNT) electrode showed lower ASR and degradation rate than Ni:CGO(ScYSZ) configuration with measured values of 0.50 Ω cm2 and 11 %/1000 h (at 0.60 A/cm2), and 0.70 Ω cm2 and 26 %/1000 h (at 0.50 A/cm2) at 1.30 V, respectively (700 °C, 50 % steam in hydrogen at the fuel side and air at the oxygen electrode side, LSC(ScYSZ) oxygen electrode).

25 ENERGY STORAGE↗
DOE OSTI2016

Construction of reduced graphene oxide supported molybdenum carbides composite electrode as high-performance anode materials for lithium ion batteries

Highlights: • Reduced graphene oxide supported molybdenum carbides are prepared by two-step strategy. • A unique sheet-on-sheet integrated nanostructure is favorable for fast ion/electron transfer. • The integrated electrode shows excellent Li ion storage performance. - Abstract: Metal carbides are emerging as promising anodes for advanced lithium ion batteries (LIBs). Herein we report reduced graphene oxide (RGO) supported molybdenum carbides (Mo{sub 2}C) integrated electrode by the combination of solution and carbothermal methods. In the designed integrated electrode, Mo{sub 2}C nanoparticles are uniformly dispersed among graphene nanosheets, forming a unique sheet-on-sheet integrated nanostructure. As anode of LIBs, the as-prepared Mo{sub 2}C-RGO integrated electrode exhibits noticeable electrochemical performances with a high reversible capacity of 850 mAh g{sup −1} at 100 mA g{sup −1}, and 456 mAh g{sup −1} at 1000 mA g{sup −1}, respectively. Moreover, the Mo{sub 2}C-RGO integrated electrode shows excellent cycling life with a capacity of ∼98.6 % at 1000 mA g{sup −1} after 400 cycles. Our research may pave the way for construction of high-performance metal carbides anodes of LIBs.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Improving the performance of stainless-steel DC high voltage photoelectron gun cathode electrodes via gas conditioning with helium or krypton

Gas conditioning was shown to eliminate field emission from cathode electrodes used inside DC high voltage photoelectron guns, thus providing a reliable means to operate photoguns at higher voltages and field strengths. Measurements and simulation results indicate that gas conditioning eliminates field emission from cathode electrodes via two mechanisms: sputtering and implantation, with the benefits of implantation reversed by heating the electrode. We have studied five stainless steel electrodes (304L and 316LN) that were polished to approximately 20 nm surface roughness using diamond grit, and evaluated inside a high voltage apparatus to determine the onset of field emission as a function of voltage and field strength. The field emission characteristics of each electrode varied significantly upon the initial application of voltage but improved to nearly the same level after gas conditioning using either helium or krypton, exhibiting less than 10 pA field emission at -225 kV bias voltage with a 50 mm cathode/anode gap, corresponding to a field strength of ~13 MV/m. Finally, field emission could be reduced with either gas, but there were conditions related to gas choice, voltage and field strength that were more favorable than others.

BastaniNejad, M.↗