Search NASA⌕ Search

SEARCH · Search NASA

Results for “thin electrolyte film”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 37 records · Page 2

Toward quantifying capacity losses due to solid electrolyte interphase evolution in silicon thin film batteries

To understand the origins of failure and limited cycle life in lithium-ion batteries (LIBs), it is imperative to quantitatively link capacity-fading mechanisms to electrochemical and chemical processes. This is extremely challenging in real systems where capacity is lost during each cycle to both active material loss and solid electrolyte interphase (SEI) evolution, two indistinguishable contributions in traditional electrochemical measurements. Here, we have used a model system in combination with (1) precision measurements of the overall Coulombic efficiency via electrochemical experiments and (2) x-ray reflectivity measurements of the active material losses. The model system consisted of a 515 Å thick amorphous silicon (a-Si) thin film on silicon carbide in half-cell geometry using a carbonate electrolyte with LiPF6 salt. This approach allowed us to quantify the capacity lost during each cycle due to SEI evolution. Combined with electrochemical analysis, we identify SEI growth as the major contribution to capacity fading. Specifically, the continued SEI growth results in increasing overpotentials due to increased SEI resistance, and this leads to lower extent of lithiation when the cutoff voltage is reached during lithiation. Our results suggest that SEI grows more with increased time spent at low voltages where electrolyte decomposition is favored. Finally, we extracted a proportionality constant for SEI growth following a parabolic growth law. Our methodology allows for the quantitative determination of lithium-ion loss mechanisms in LIBs by separately tracking lithium ions within the active materials and the SEI and offers a powerful method of quantitatively understanding LIB loss mechanisms.

25 ENERGY STORAGE↗

Simultaneous Solid Electrolyte Deposition and Cathode Lithiation for Thin Film Batteries and Lithium Iontronic Devices

Here we show that the deposition of the solid-state electrolyte LiPON onto films of V 2 O 5 leads to their uniform lithiation of up to 2.2 Li per V 2 O 5 , without affecting the Li concentration in the LiPON and its ionic conductivity. Our results indicate that Li incorporation occurs during LiPON deposition, in contrast to earlier mechanisms proposed to explain postdeposition Li transfer between LiPON and LiCoO 2 . We use our discovery to demonstrate symmetric thin film batteries with a capacity of >270 mAh/g, at a rate of 20C, and 1600 cycles with only 8.4% loss in capacity. We also show how autolithiation can simplify fabrication of Li iontronic transistors attractive for emerging neuromorphic computing applications. Our discovery that LiPON deposition results in autolithiation of the underlying insertion oxide has the potential to substantially simplify and enhance the fabrication process for thin film solid state Li ion batteries and emerging lithium iontronic neuromorphic computing devices.

25 ENERGY STORAGE↗

Catalytic open-circuit passivation by thin metal oxide films of p-Si anodes in aqueous alkaline electrolytes

Ni and NiO x -based protective thin films are shown to catalyze the oxidation of Si in the presence of O 2 in strongly alkaline KOH(aq) even in the absence of illumination. The O 2 in solution drove the open-circuit potential of the electrode to >0.4 V, which is positive of the Si passivation potential. The elevated electrochemical potential of the surface promoted formation of passive oxides on exposed Si regions of Si/Ni electrodes. Catalytic passivation of Si extended the durability of an np + -Si(100)/NiO x photoanode to >400 h while operating under simulated day/night cycles. In contrast, electrodes without a Ni(O x ) layer and/or without O 2 in solution displayed direct etching of the Si and corrosion pitting during non-illuminated, simulated nighttime episodes of day/night cycling. The O 2 -derived catalyzed passivation of Si using thin films can be generalized to multiple phases of NiO x as well as to materials other than Ni. Finally, relative to operation in aqueous alkaline conditions, decreasing the pH of the electrolyte decreased the dissolution rate of the protective oxide layer formed by the catalyzed passivation process, and consequently increased the durability of the photoanode, but yielded lower photoelectrode fill factors for water oxidation due to the relatively large kinetic overpotentials for the electrocatalyzed oxygen-evolution reaction at near-neutral pH.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electrochemistry of Thin Films with In Situ/Operando Grazing Incidence X-Ray Scattering: Bypassing Electrolyte Scattering for High Fidelity Time Resolved Studies

Electroactive polymer thin films undergo repeated reversible structural change during operation in electrochemical applications. While synchrotron X-ray scattering is powerful for the characterization of stand-alone and ex situ organic thin films, in situ/operando structural characterization has been underutilized-in large part due to complications arising from supporting electrolyte scattering. This has greatly hampered the development of application relevant structure property relationships. Therefore, a new methodology for in situ/operando X-ray characterization that separates the incident and scattered X-ray beam path from the electrolyte is developed. As a proof of concept, the operando structural characterization of weakly-scattering, organic mixed conducting thin films in an aqueous electrolyte environment is demonstrated, accessing previously unexplored changes in the $\pi-\pi$ peak and diffuse scatter, while capturing the solvent swollen thin film structure which is inaccessible in previous ex situ studies. These in situ/operando measurements improve the sensitivity to structural changes, capturing minute changes not possible ex situ, and have multimodal potential such as combined Raman measurements that also serve to validate the true in situ/operando conditions of the cell. Finally, new directions enabled by this in situ/operando cell design are examined and state of the art measurements are compared.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unraveling the Stable Cathode Electrolyte Interface in all Solid‐State Thin‐Film Battery Operating at 5 V

Abstract Spinel‐type LiNi 0.5 Mn 1.5 O 4 (LNMO) is one of the most promising 5 V‐class cathode materials for Li‐ion batteries that can achieve high energy density and low production costs. However, in liquid electrolyte cells, the high voltage causes continuous cell degradation through the oxidative decomposition of carbonate‐based liquid electrolytes. In contrast, some solid‐state electrolytes have a wide electrochemical stability range and can withstand the required oxidative potential. In this work, a thin‐film battery consisting of an LNMO cathode with a solid lithium phosphorus oxynitride (LiPON) electrolyte is tested and their interface before and after cycling is characterized. With Li metal as the anode, this system can deliver stable performance for 600 cycles with an average Coulombic efficiency >99%. Neutron depth profiling indicates a slight overlithiated layer at the interface prior to cycling, a result that is consistent with the excess charge capacity measured during the first cycle. Cryogenic electron microscopy further reveals intimate contact between LNMO and LiPON without noticeable structure and chemical composition evolution after extended cycling, demonstrating the superior stability of LiPON against a high voltage cathode. Consequently, design guidelines are proposed for interface engineering that can accelerate the commercialization of a high voltage cell with solid or liquid electrolytes.

25 ENERGY STORAGE↗

3D Ion-Conducting, Scalable, and Mechanically Reinforced Ceramic Film for High Voltage Solid-State Batteries

Concerning the safety aspects of Li+ ion batteries, an epoxy-reinforced thin ceramic film (ERTCF) is prepared by firing and sintering a slurry-casted composite powder film. The ERTCF is composed of Li + ion conduction channels and is made of high amounts of sintered ceramic Li 1+ x Ti 2-x Al x (PO 4 ) 3 (LATP) and epoxy polymer with enhanced mechanical properties for solid-state batteries. The two- and three-dimensional characterizations are conducted not only for showing continuous Li+ ion channels thorough LATP ceramic channels with over 10-4 S cm-1 of ionic conductivity but also to investigate small amounts of epoxy polymer with enhanced mechanical properties. Solid-state Li + ion cells are fabricated using the ERTCF and they show initial charge–discharge capacities of 139/133 mAh g -1 . Furthermore, the scope of the ERTCF is expanded to high-voltage (>8 V) solid-state Li + ion batteries through a bipolar stacked cell design. Hence, it is expected that the present investigation will significantly contribute in the preparation of the next generation reinforced thin ceramic film electrolytes for high-voltage solid-state batteries.

25 ENERGY STORAGE↗

Three-Electrode Study of Electrochemical Ionomer Degradation Relevant to Anion-Exchange-Membrane Water Electrolyzers

Among existing water electrolysis (WE) technologies, anion-exchange-membrane water electrolyzers (AEMWEs) show promise for low-cost operation enabled by the basic solid-polymer electrolyte used to conduct hydroxide ions. The basic environment within the electrolyzer, in principle, allows the use of non-platinum-group metal catalysts and less-expensive cell components compared to acidic-membrane systems. Nevertheless, AEMWEs are still underdeveloped, and the degradation and failure modes are not well understood. To improve performance and durability, supporting electrolytes such as KOH and K 2 CO 3 are often added to the water feed. The effect of the anion interactions with the ionomer membrane (particularly other than OH – ), however, remains poorly understood. We studied three commercial anion-exchange ionomers (Aemion, Sustainion, and PiperION) during oxygen evolution (OER) at oxidizing potentials in several supporting electrolytes and characterized their chemical stability with surface-sensitive techniques. We analyzed factors including the ionomer conductivity, redox potential, and pH tolerance to determine what governs ionomer stability during OER. Specifically, we discovered that the oxidation of Aemion at the electrode surface is favored in the presence of CO 3 2– /HCO 3 – anions perhaps due to the poor conductivity of that ionomer in the carbonate/bicarbonate form. Sustainion tends to lose its charge-carrying groups as a result of electrochemical degradation favored in basic electrolytes. PiperION seems to be similarly negatively affected by a pH drop and low carbonate/bicarbonate conductivity under the applied oxidizing potential. Furthermore, the insight into the interactions of the supporting electrolyte anions with the ionomer/membrane helps shed light on some of the degradation pathways possible inside of the AEMWE and enables the informed design of materials for water electrolysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Solvent influence on non-adiabatic interfacial electron transfer at conductive oxide electrolyte interfaces

The kinetics for interfacial electron transfer (ET) from a transparent conductive oxide (tin-doped indium oxide, ITO, Sn:In 2 O 3 ) to molecular acceptors 4-[N,N-di(p-tolyl)amino]benzylphosphonic acid, TPA, and [Ru II (bpy) 2 (4,4' -(PO 3 H 2 ) 2 -bpy)] 2+ , RuP, positioned at variable distances within and beyond the electric double layer (EDL), were quantified in benzonitrile and methanol by nanosecond absorption spectroscopy as a function of the thermodynamic driving force, -ΔG ° . Relevant ET parameters such as the rate constant, k et , reorganization energy, λ, and electronic coupling, Hab, were extracted from the kinetic data. Overall, k et increased as the distance between the molecular acceptor and the conductor decreased. For redox active molecules within the Helmholtz planes of the EDL, k et was nearly independent of -ΔG° , consistent with a negligibly small λ value. Rips–Jortner analysis revealed a non-adiabatic electron transfer mechanism consistent with H ab < 1 cm -1 . The data indicate that the barrier for electron transfer is greatly diminished at the conductor–electrolyte interface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CRADA Number NFE-21-08827 with DayLyte, Inc. (CRADA Final Report)

DayLyte Batteries is developing an aqueous Sodium-Air battery made with abundant materials while being half to a third the weight of Li-ion to power electric aircraft, electric vehicles and provide renewable energy on demand. To make this battery practical, DayLyte is developing a thin film ceramic Nasicon solid electrolyte amenable to rapid scaleup as well as a protective coating that will protect the solid electrolyte from 50wt% NaOH during the battery’s end-of-discharge while still allowing Na-ions to pass back and forth. If the thin film solid electrolyte and stable coating can be developed it will open the world to step change in battery performance all while not sacrificing the environment on the way. The project was designed to first focus on making and characterizing the Nasicon membrane followed by measuring its electrochemical performance, then assembling a full cell, optimizing its NaOH stability and then optimize the overall prototype design. Over the past two years, we have significantly improved the Nasicon film uniformity, demonstrated protective ligands that are stable in 50wt% NaOH by measuring no mass change with a quartz crystal microbalance, tested different heating methods like tube furnace and rapid heating and developed glassy carbon coatings on the current collector to prevent Nasicon-current collector alloying. We have found that getting film uniformity as measured by electrochemical impedance spectroscopy (EIS) is difficult because of different factors like surface roughness, deposition uniformity and heat treatment time and uniformity. The glassy carbon coating should significantly reduce the surface roughness and by tuning the coating conditions the film deposition uniformity improves and using an automated heating method should lead to much improved film uniformity.

25 ENERGY STORAGE↗

Mild-Annealed Molecular Layer Deposition (MLD) Tincone Thin Film as Photoelectrochemically Stable and Efficient Electron Transport Layer for Si Photocathodes

Metalcone thin films, composed of inorganic–organic hybrids, are synthesized using molecular layer deposition (MLD) through reactions between organometallic precursors (e.g., Sn, Al, and Ti) and organic reactants (e.g., ethylene glycol and glycerol). Despite their unique properties, metalcones exhibit significant vulnerability to water due to their organic components, limiting their potential in electrochemical applications. This study focuses on enhancing the photoelectrochemical stability of tincone thin films in aqueous electrolyte while preserving their hybrid characteristics through mild annealing in air at 250 °C. As-deposited and vacuum-annealed tincone thin films exhibited significant degradation under these conditions, while high-temperature-annealed (500 °C) tincone thin films offered improved stability with a significant decline in charge transfer efficiency. In contrast, mild annealing in air maintained the C–O bond at half level and improved the stability and charge transport without compromising the unique characteristics of tincone. This was confirmed by ellipsometry, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FTIR). Mild-annealed tincone deposited on a lightly doped p-type silicon (p-Si) photocathode produced a 20-fold increase in CO volume compared to high-temperature annealed tincone in a CO 2 -saturated potassium bicarbonate (KHCO 3 ) electrolyte with dispersed graphene oxide–cobalt phthalocyanine (GO-CoPc) under 1 sun illumination at 0.9 V vs reversible hydrogen electrode (RHE), while maintaining the faradaic efficiency for CO and H 2 . These results suggest that mild-annealed tincone thin films hold significant potential as protective charge transport layers on silicon photocathodes for the aqueous CO 2 reduction reaction (CO 2 RR).

Annealing (metallurgy)↗

Al 2 O 3 Thin Films on Magnesium: Assessing the Impact of an Artificial Solid Electrolyte Interphase

Among the many emerging technologies under investigation as alternatives to the successful Lithium-ion battery, the magnesium battery is promising due to the wide availability of magnesium, its high volumetric capacity, and the possibility for safety improvements. One of the largest challenges facing rechargeable magnesium batteries is the formation of a passivation layer at the Mg metal anode interface when reactive species in the electrolyte are reduced at the electrode-electrolyte interface. To control the solid electrolyte interphase in Lithium batteries, protective layers called artificial solid electrolyte interphase (ASEI) layers have been successful in improving Li metal anode performance. The approach of protecting Mg metal anodes from electrolyte degradation has been demonstrated by fewer studies in the literature than Li systems. In this work, we discuss the properties of Al 2 O 3 thin films deposited using atomic layer deposition as an artificial solid electrolyte interphase at the Mg anode. Our results demonstrate that Al 2 O 3 does prevent electrolyte degradation due to the reductive nature of Mg. However, undesirable properties such as defects and layer breakdown lead to Mg growth that causes soft-shorting. The soft-shorting occurs with and without the protection layer, indicating the ALD layer does not prevent it and hinders Al 2 O 3 from being an ideal candidate for a protection layer. Crucial effects of this layer on Mg electrochemistry at the interface were observed, including growth of Mg deposits leading to soft-shorting of the cell whose morphology showed a dependence on the Al 2 O 3 layer. These results may provide guidelines for the future design and development of protective ASEI layers for Mg anodes.

25 ENERGY STORAGE↗

Nanoscale Li, Na, and K ion-conducting polyphosphazenes by atomic layer deposition

A key trailblazer in the development of thin-film solid-state electrolytes has been lithium phosphorous oxynitride (LiPON), the success of which has led to recent progress in thin-film ion conductors. Here we compare the structural, electrochemical, and processing parameters between previously published LiPON and NaPON ALD processes with a novel ALD process for the K analogue potassium phosphorous oxynitride (KPON). In each ALD process, alkali tert-butoxides and diethylphosphoramidate are used as precursors. To understand the ALD surface reactions, this work proposes a reaction mechanism determined by in-operando mass spectrometry for the LiPON process as key to understanding the characteristics of the APON (A = Li, Na, K) family. As expected, NaPON and LiPON share similar reaction mechanisms as their structures are strikingly similar. KPON, however, exhibits similar ALD process parameters but the resulting film composition is quite different, showing little nitrogen incorporation and more closely resembling a phosphate glass. Due to the profound difference in structure, KPON likely undergoes an entirely different reaction mechanism. Furthermore, this paper presents a comprehensive summary of ALD ion conducting APON films as well as a perspective that highlights the versatility of ALD chemistries as a tool for the development of novel thin film ion-conductors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Avoiding CO 2 Improves Thermal Stability at the Interface of Li 7 La 3 Zr 2 O 12 Electrolyte with Layered Oxide Cathodes

Abstract Solid‐state batteries promise higher energy densities and better safety than Li‐ion batteries with liquid electrolytes. However, the interface between solid electrolyte and cathode is unstable at the elevated temperatures that are needed while sintering to achieve good bonding between ceramic components. Here, the hypothesis is that, the gas environment, especially the presence of CO 2, is critical in determining the stability of the solid electrolyte–cathode interface. The effect of gas species on the interface is systematically probed, by a using Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte with a thin film LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode as a model system to enable interface sensitivity. Detrimental phases formed at the interface and their onset conditions are identified by X‐ray absorption spectroscopy, X‐ray diffraction, and Gibbs free energy analysis. As a result, removing CO 2 and minimizing H 2 O(g) during sintering is necessary to obtain good contact at the LLZO|cathode interface without forming secondary phases. Sintering in O 2 is ideal, yielding excellent chemical stability and low interfacial resistance. Secondary phases also do not form in N 2, but oxygen loss occurs at elevated temperatures. The interfacial resistance obtained upon sintering in pure O 2 is comparable to the lowest values at LLZO interfaces with protective coatings, but here without the need for interface coatings.

25 ENERGY STORAGE↗

Engineering Surface Oxygenated Functionalities on Commercial Carbon toward Ultrafast Sodium Storage in Ether-Based Electrolytes

The pursuit of a high-capacity anode material has been urgently required for commercializing sodium-ion batteries with a high energy density and an improved working safety. In the absence of thermodynamically stable sodium intercalated compounds with graphite, constructing nanostructures with expanded interlayer distances is still the mainstream option for developing high-performance carbonaceous anodes. In this regard, a surface-functionalized and pore-forming strategy through a facile CO 2 thermal etching route was rationally adopted to engineer negligible oxygenated functionalities on commercial carbon for boosting the sodium storage process. Benefitted from the abundant ionic/electronic pathways and more active reaction sites in the microporous structure with noticeable pseudocapacitive behaviors, the functionalized porous carbon could achieve a highly reversible capacity of 505 mA h g -1 at 50 mA g -1 , an excellent rate performance of 181 mA h g -1 at 16,000 mA g -1 , and an exceptional rate cycle stability of 176 mA h g -1 at 3200 mA g -1 over 1000 cycles. These outstanding electrochemical properties should be ascribed to a synergistic mechanism, fully utilizing the graphitic and amorphous structures for synchronous intercalations of sodium ions and solvated sodium ion compounds, respectively. Finally, the controllable generation and evolution of a robust but thin solid electrolyte interphase film with the emergence of obvious capacitive reactions on the defective surface, favoring the rapid migration of sodium ions and solvated species, also contribute to a remarkable electrochemical performance of this porous carbon black.

25 ENERGY STORAGE↗