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DOE OSTI2021

In situ formation of polymer-inorganic solid-electrolyte interphase for stable polymeric solid-state lithium-metal batteries

Composite polymer electrolytes (CPEs) for solid-state Li-metal batteries (SSLBs) still suffer from gradually increased interface resistance and unconstrained Li-dendrite growth. Herein, we addressed the challenges by designing a LiF-rich inorganic solid-electrolyte interphase (SEI) through introducing a fluoride-salt-concentrated interlayer on CPE film. The rigid but flexible CPE helps accommodate the volume change of electrodes, while the polymeric highly concentrated electrolyte (PHCE) surface-layer regulates Li-ion flux due to the formation of a stable LiF-rich SEI via anion reduction. The designed CPE-PHCE presents enhanced ionic conductivity and high oxidation stability of >5.0 V (versus Li/Li + ). Furthermore, it dramatically reduces the interfacial resistance and achieves a high critical current density of 4.5 mA cm –2 . The SSLBs, fabricated with thin CPE-PHCE membranes (<100 μm) and Co-free LiNiO 2 cathodes, exhibit exceptional electrochemical performance and long cycling stability. Lastly, this approach of SEI design can also be applied to other types of batteries.

25 ENERGY STORAGE↗

DOE OSTI2019

A three-dimensional interconnected polymer/ceramic composite as a thin film solid electrolyte

In this work we introduce an approach to fabricate a solid composite electrolyte film that is thin, ionically conductive, and mechanically robust with good potential for manufacturability, in the application of lithium metal batteries. First a doped-lithium aluminum titanium phosphate ceramic thin film with thickness of ~25 μm is formed by aqueous spray coating, a scalable process. The film is partially sintered to form a three-dimensionally interconnected structure with a dense backbone. It is then backfilled with a crosslinkable poly(ethylene oxide) (PEO)-based polymer electrolyte. We report the composite has very high ceramic loading of 77 wt% (61 vol%) and an ionic conductivity of 3.5 × 10 -5 S/cm at 20 °C with an activation energy of 0.43 eV. The main ion transport pathway is through the ceramic network, predicted by modelling and verified by experiments. Owing to the interconnected structure of the ceramic, the composite electrolyte exhibits much improved mechanical strength.

25 ENERGY STORAGE↗

DOE OSTI2022

Chemical Challenges that the Peroxide Dianion Presents to Rechargeable Lithium–Air Batteries

Understanding the fundamental redox reactions and processes that occur in lithium–air and, more generally, metal–air batteries is important to the progress of this promising energy-storage technology. Knowledge of the chemistry of the peroxide dianion, O 2 2– , is especially crucial, as the dianion is at the nexus of the charge/discharge cycle of lithium–air batteries. The intrinsic electron transfer properties and redox chemistry of peroxide dianion are poorly defined because it is difficult to isolate the dianion free of protons and metal ions. We review the results of (i) the electron transfer kinetics and (ii) the redox reaction chemistry of isolated peroxide dianion encapsulated within the cavity of a hexacarboxamide cryptand. With regard to the former, electron transfer kinetics measurements provide fundamental Marcus parameters that will be useful for models that seek to disentangle the precise contributions of Li + ion-coupled electron transfer, electron transfer across the Li 2 O 2 solid particle interface, and charge hopping among Li 2 O 2 particles. With regard to the latter, an underappreciated chemistry of peroxide dianion with CO 2 produces peroxymonocarbonate (OOCO 2 2– ) and peroxydicarbonate (O 2 COOCO 2 2– ). An autocatalytic cycle will lead to oxidative degradation of traditional organic electrolytes and other vulnerable cell components employed in lithium–air batteries. Furthermore, this peroxycarbonate-derived chemistry, in addition to more commonly recognized solution-based oxidation chemistry, will need to be mitigated to realize the long-term cyclability of rechargeable lithium–air batteries.

25 ENERGY STORAGE↗

NASA NTRS1973

Instrumentation for air quality measurements.

Comparison of the new generation of air quality monitoring instruments with some more traditional methods. The first generation of air quality measurement instruments, based on the use of oxidant coulometric cells, nitrogen oxide colorimetry, carbon monoxide infrared analyzers, and other types of detectors, is compared with new techniques now coming into wide use in the air monitoring field and involving the use of chemiluminescent reactions, optical absorption detectors, a refinement of the carbon monoxide infrared analyzer, electrochemical cells based on solid electrolytes, and laser detectors.

Loewenstein, M.↗

NASA NTRS2003

Solid state potentiometric gaseous oxide sensor

A solid state electrochemical cell (10a) for measuring the concentration of a component of a gas mixture (12) includes first semiconductor electrode (14) and second semiconductor electrode (16) formed from first and second semiconductor materials, respectively. The materials are selected so as to undergo a change in resistivity upon contacting a gas component, such as CO or NO. An electrolyte (18) is provided in contact with the first and second semiconductor electrodes. A reference cell can be included in contact with the electrolyte. Preferably, a voltage response of the first semiconductor electrode is opposite in slope direction to that of the second semiconductor electrode to produce a voltage response equal to the sum of the absolute values of the control system uses measured pollutant concentrations to direct adjustment of engine combustion conditions.

Wachsman, Eric D.↗

DOE OSTI2025

Tunable Crosslinked Ether Polymer Network Electrolytes for High‐Performance All‐Solid‐State Sodium Batteries

All-solid-state batteries (ASSBs) are critical for achieving high energy density and enhanced safety. Solid polymer electrolytes (SPEs) offer key advantages over other electrolytes, including improved safety, flexibility, and interfacial contact. Among the SPEs, ether-based polymers are widely studied due to their ease of processing and high ionic conductivity (σi) in the amorphous state. In this work, the introduction of poly(ethylene glycol) methyl ether methacrylate (PEGMEMA) into an SPE matrix composed of poly(ethylene glycol) diacrylate (PEGDA), poly(ethylene glycol) (PEG2k), and sodium bis(fluorosulfonyl)imide (NaFSI) salt is investigated to facilitate the formation of amorphous, high σ i SPEs through end-group engineering and polymer ratio optimization. PEGMEMA enhances structural integrity via crosslinking with PEGDA through its methacrylate group, while its methyl end group aids ion conduction. A 2:1:7 ratio of PEGDA:PEGMEMA:PEG2k exhibits a σi of 1.16 x 10 -4 S cm -1 and oxidative stability up to 4.4 V at 60 °C. A solid-state cell incorporating this SPE, a Na 2/3 Ni 1/3 Mn 2/3 O 2 (NM12) cathode, and a sodium-metal anode demonstrates excellent cycling stability, retaining over 80 % of its initial capacity for 150 cycles at 60 °C. The findings highlight the potential of end-group engineering in improving the electrochemical performance of SPEs.

25 ENERGY STORAGE↗

DOE OSTI2023

Life cycle analysis of a hydrogen production system based on solid oxide electrolysis cells integrated with different energy and wastewater sources

Hydrogen production via water electrolysis is a promising and evolving technology. The solid oxide electrolysis cell (SOEC) is one of the several technologies for this purpose. They are alternatives to the traditional hydrogen production from fossil fuels to enhance global energy decarbonization. However, in the bid for sustainability and a green economy, these technologies are not free from causing some environmental burdens. Using life cycle assessment (LCA), the greenhouse gas emission and degree of environmental impacts by these technologies can be identified and measured throughout their lifespan. This study addresses how to quantify these CO 2 emission impacts for an electrolytic system with different energy sources. The LCA of a novel integrated hydrogen production SOEC system with energy from solar photovoltaic and bituminous powerplant is performed using simaPro, the leading global LCA solution software. Measuring the environmental impact of the electrolytic operation in terms of weight, the bituminous powerplant poses damage which is, on average 700% more than solar PV. The thermal-to-hydrogen efficiency of the SOEC system is 56%, and a probable 28% reduction in carbon footprint with heat integration. The steam generation and the manufacturing of the SOEC have a very high environmental impact potential on the system. Here, we recommend LCA and net energy analysis is carried out for every new hydrogen technology and adequate comparison to enhance sustainable and green economy.

08 HYDROGEN↗

DOE OSTI2025

Resistive Switching of Spinel Li 4 Ti 5 O 12 Lithium-Ion Battery Material for Neuromorphic Computing

The rapid rise of AI has exposed significant limitations in conventional Von Neumann computing architecture, particularly in regard to speed and energy efficiency. To address these challenges, researchers are exploring a brain-inspired neuromorphic architecture that mimics biological neural networks, enabling massive parallel processing with reduced power consumption for complex AI computational demands. Recent interest has focused on utilizing battery electrodes and solid electrolyte materials for their resistive switching properties in developing a neuromorphic architecture. These properties are precisely tuned through local- and bulk-level chemical composition modifications via voltage bias stimuli. In this study, we demonstrate fabricating a three-terminal lithium-ion electrochemical transistor based on lithium titanium oxide (Li 4 Ti 5 O 12 ), a popular lithium-ion battery anode material. We deposited and characterized LTO thin films using RF sputtering, demonstrating a 6 orders of magnitude increase in electronic conductivity upon lithiation, with conductivity plateauing after 20% lithiation. Density functional theory calculations revealed transformation from the insulating to conducting state, supported by experimental characterization through X-Ray Photoelectron Spectroscopy (XPS) and Direct Current (DC) polarization analyses. The fabricated transistor consisted of LTO as the channel layer, gold as source/drain terminals, lithium phosphorus oxynitride (LiPON) as the lithium-ion conductor, and copper as the gate terminal. The device exhibited clear hysteresis in transfer characteristics due to lithium insertion/extraction processes. Long-term potentiation (LTP) and long-term depression (LTD) measurements showed an asymmetric ratio of 1.425 and maximum/minimum conductance ratio of 7.83. When implemented in a deep neural network (DNN) for MNIST handwritten digit recognition, the device achieved 92.03% accuracy over 20 training epochs. Detailed transport mechanism analysis revealed the crucial role of oxygen vacancies and interface effects in device operation. Our preliminary findings establish LTO-based lithium-ion electrochemical transistors as promising candidates for energy-efficient neuromorphic computing applications, offering potential solutions to traditional Von Neumann architecture limitations.

25 ENERGY STORAGE↗

DOE OSTI2023

Enhancing the Faradaic efficiency of solid oxide electrolysis cells: progress and perspective

Abstract To reduce global warming, many countries are shifting to sustainable energy production systems. Solid oxide electrolysis cells (SOECs) are being considered due to their high hydrogen generation efficiency. However, low faradaic efficiency in scaling SOEC technology affects costs and limits large-scale adoption of hydrogen as fuel. This review covers SOECs’ critical aspects: current state-of-the-art anode, cathode, and electrolyte materials, operational and materials parameters affecting faradaic efficiency, and computational modeling techniques to resolve bottlenecks affecting SOEC faradaic efficiency.

Gaikwad, Prashik S. (ORCID:0000000179510115)↗

DOE OSTI2024

Methylation enables the use of fluorine-free ether electrolytes in high-voltage lithium metal batteries

Lithium metal batteries represent a promising technology for next-generation energy storage, but they still suffer from poor cycle life due to lithium dendrite formation and cathode cracking. Fluorinated solvents can improve battery longevity by improving LiF content in the solid-electrolyte interphase; however, the high cost and environmental concerns of fluorinated solvents limit battery viability. Here, for this work, we designed a series of fluorine-free solvents through the methylation of 1,2-dimethoxyethane, which promotes inorganic LiF-rich interphase formation through anion reduction and achieves high oxidation stability. The anion-derived LiF interphases suppress lithium dendrite growth on the lithium anode and minimize cathode cracking under high-voltage operation. The Li + -solvent structure is investigated through in situ techniques and simulations to draw correlations between the interphase compositions and electrochemical performances. The methylation strategy provides an alternative pathway for electrolyte engineering towards high-voltage electrolytes while reducing dependence on expensive fluorinated solvents.

25 ENERGY STORAGE↗

DOE OSTI2025

How Interface Evolution at the Nanoscale Dictates Protonic Ceramic Cell Behavior

Understanding the effects of heterointerfaces in nanodevices remains a challenge in interface engineering for systems applied in solid oxide fuel cells, catalysis, sensors, and memristors [1]. Previous studies have shown that the presence of interfaces in ceramic oxide nanodevices affects their impedance properties compared to bulk systems [2]. In this work, we analyze a thin-film model system designed to study the interfaces between representative electrode and electrolyte materials employed in protonic ceramic electrochemical cells for the reversible conversion of hydrogen o electricity. The investigated device features a 21-layer architecture that alternates between an electrode material PBSCF (PrBa 0.5 Sr 0.5 Co 1.5 Fe 0.5 O 5+ϵ ) and a proton-conducting electrolyte BZY (BaZr 0.8 Y 0.2 O 3-δ ), with uniform 20 nm thickness for each layer. Here, the device was fabricated using Pulsed Laser Deposition (PLD) and supported on a conductive Nb-doped STO (Nb-SrTiO 3 ) substrate.

dos Santos, Gabriel T. [Northwestern University, E↗

DOE OSTI2024

Cation Migration and LSCF/SDC Decomposition Related to Long-Term Operation Mode as Revealed by Electron Microscopy

This study utilized energy dispersive spectroscopy (EDS) in a scanning electron microscope (SEM) and a scanning transmission electron microscope (STEM) in order to track cation migration and related particle decomposition for air electrode components of solid oxide cells. The influence of a Sm-doped ceria (SDC) barrier layers was assessed for three operation modes (fuel cell, electrolysis, reversible) over long time periods (1000-1500 hours). Composition profiles across air electrode/electrolyte interfaces indicated negligible accumulation of La/Sr cations to the yttria-stabilized zirconia (YSZ) electrolyte during operation. Instead, air electrode particles composed of SDC and/or La-Sr-Co-Fe-oxides (LSCF) exhibited decomposition by Sr evaporation and Sm migration to LSCF particle edges.

Picard, Yoosuf↗

DOE OSTI2022

Ultrastable rechargeable manganese battery with solid-liquid-gas reactions

A rechargeable manganese battery includes: (1) a first electrode including a porous, conductive support; (2) a second electrode including a catalyst support and a catalyst disposed over the catalyst support; and (3) an electrolyte disposed between the first electrode and the second electrode to support reversible precipitation and dissolution of manganese at the first electrode and reversible evolution and oxidation of hydrogen at the second electrode.

Chen, Wei↗

DOE OSTI2023

Ultrastable rechargeable manganese battery with solid-liquid-gas reactions

Chen, Wei↗

DOE OSTI2023

Characterization of Annealing-Induced Phase Segregation in Composite Silicon Anodes for Li-ion Batteries

Silicon (Si) anodes present a promising alternative to graphite anodes for lithium-ion batteries (LIBs), as Si has a greater specific capacity. However, one major constraint is the volumetric change of Si during lithiation that results in an unstable solid-electrolyte interphase (SEI), so Si-containing electrodes require the use of various strategies to mitigate these effects and improve performance. One such solution is the use of Si nanoparticles (NPs) that maximize the surface area to volume ratio. Here, we discuss electrodes made with Si NPs treated with polyethylene oxide (PEO) (for improving dispersion during processing), conductive carbon NPs, and P84 polyimide binder which shows significant impacts of annealing treatment on improvements of active material utilization, first cycle efficiency, and capacity retention with extensive cycling . We used air-free argon ion polishing to create electrode cross sections and imaged through the electrode thickness using atomic force microscopy (AFM)-based nano-electrical characterization of scanning spreading resistance microscopy (SSRM), nano-mechanical characterizations of contact resonance and force volume (CR-FV), and scanning electron microscopy-based energy dispersive x-ray spectroscopy (SEM-EDS). Results show that the Si and conductive carbon segregate into phases with a distinctive carbon-rich banded morphology that surrounds the Si-rich phase during annealing. In pristine electrodes, the carbon- and SEI-rich bands exhibit a higher electronic conductivity and a lower elastic modulus than the Si active material phase. These structures, as well as distinct electronic and mechanical properties, remain during cycling, suggesting an improvement of electrical conduction pathways and a mechanical strain buffer for active Si material expansion during cycling. This phase separation may be a major factor in the improvement seen in electrochemical performance due to annealing. Additionally, our nm-scale and multi-mode characterizations provide a novel route for understanding and improving energy storage devices, which is advantageous due to the highly inhomogeneous of composite electrodes in nm-mm scales.

ENERGY STORAGE↗

DOE OSTI2022

Atmospheric plasma spraying to fabricate metal‐supported solid oxide fuel cells with open‐channel porous metal support

Abstract Metal‐supported solid oxide fuel cells (MS‐SOFCs) have been fabricated by applying phase‐inversion tape‐casting and atmospheric plasma spraying (APS). The effect of the binder amount of the phase‐inversion slurries on the microstructure development of the 430L stainless steel metal support was investigated. The pore structures, the viscosity of the slurry, porosity and permeability of the as‐prepared metal supports are significantly influenced by the amount of the binder. NiO–scandia‐stabilized zirconia (ScSZ) anode, ScSZ electrolyte and La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3−δ (LSCF) cathode layers were consecutively deposited on the metal support with an ideal microstructure by APS process. The effect of plasma power of the APS on the microstructure of the electrolyte and cathode was investigated. A dense electrolyte layer and a porous cathode layer were successfully obtained at 40 and 6 kW of the APS plasma power, respectively. MS‐SOFCs, with a cell configuration of 430L/Ni‐ScSZ/ScSZ/LSCF, achieved a maximum cell power density of 1079 mW cm −2 at 700°C using humidified H 2 as fuel and ambient air as oxidant. The corresponding ohmic resistance and total resistance of MS‐SOFCs was 0.14 and 0.32 Ω cm 2 , respectively. This work demonstrates the feasibility of fabricating high‐performance MS‐SOFCs with economical and scalable techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2020

A Fireproof, Lightweight, Polymer–Polymer Solid-State Electrolyte for Safe Lithium Batteries

Safety issues in lithium-ion batteries have raised serious concerns due to their ubiquitous utilization and close contact with the human body. Replacing flammable liquid electrolytes, solid-state electrolytes (SSEs) is thought to address this issue as well as provide unmatched energy densities in Li-based batteries. However, among the most intensively studied SSEs, polymeric solid electrolyte and polymer/ceramic composites are usually flammable, leaving the safety issue unattended. Here, we report the first design of a fireproof, ultralightweight polymer–polymer SSE. The SSE is composed of a porous mechanic enforcer (polyimide, PI), a fire-retardant additive (decabromodiphenyl ethane, DBDPE), and a ionic conductive polymer electrolyte (poly(ethylene oxide)/lithium bis(trifluoromethanesulfonyl)imide). The whole SSE is made from organic materials, with a thin, tunable thickness (10–25 μm), which endorse the energy density comparable to conventional separator/liquid electrolytes. The PI/DBDPE film is thermally stable, nonflammable, and mechanically strong, preventing Li–Li symmetrical cells from short-circuiting after more than 300 h of cycling. LiFePO 4 /Li half cells with our SSE show a high rate performance (131 mAh g –1 at 1 C) as well as cycling performance (300 cycles at C/2 rate) at 60 °C. Most intriguingly, pouch cells made with our polymer–polymer SSE still functioned well even under flame abuse tests.

25 ENERGY STORAGE↗

DOE OSTI2022

Enable High-Energy LiNi0.5Co0.2Mn0.3O2 by Ultra-Thin Coating through Wet Impregnation

A high cut-off voltage is required for nickel-rich layered oxide LiNixCoyMnzO2 (NCM) to meet the high energy density requirement of lithium-ion batteries in electric vehicles. However, such a high voltage application leads to an unstable interface between NCM and liquid electrolytes. To stabilize the interface, the facile wet impregnation method has been developed to apply an ultra-thin Al2O3 coating layer on the NCM particles. This coating layer was found to have a strong interaction with the NCM and resulted in Al-doped NCM at the surface structure of NCM. The change of surface structure can not only reduce the surface resistance of lithium diffusion of LiNi0.5Co0.2Mn0.3O2 (NCM523), but also stabilize the solid electrolyte interface between NCM523 and the electrolyte with the cut-off voltage of 4.5 V vs. Li/Li+. Compared to other coating methods, wet impregnation coating can provide an ultra-thin and uniform coating with surface doping on NCM particles. Furthermore, this scalable coating method can be applied to various electrode materials without adding much additional cost.

25 ENERGY STORAGE↗