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36 records · Page 2

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DOE OSTI2020

In Situ Investigation of Chemomechanical Effects in Thiophosphate Solid Electrolytes

Solid-state batteries can suffer from catastrophic failure at high current densities due to solid electrolyte fracture, interface decomposition, or lithium filament growth. Failure is linked to chemomechanical material transformations that can manifest during electrochemical cycling. We systematically investigate how solid electrolyte microstructure and interfacial decomposition (e.g., interphase) affect failure mechanisms in lithium thiophosphates (Li3PS4, LPS) electrolytes. Kinetically metastable interphases are engineered with iodine doping, and microstructural control is achieved using milling and annealing processing techniques. In situ transmission electron microscopy reveals iodine diffusion to the interphase, and upon electrochemical cycling, pores are formed in the interphase region. In situ synchrotron tomography reveals that interphase pore formation drives edge fracture events, which are the origin of through-plane fracture failure. Fractures in thiophosphate electrolytes actively grow toward regions of higher porosity and are affected by heterogeneity in microstructure (e.g., porosity factor). This report provides fundamental design guidelines for high-performance solid-state batteries.

25 ENERGY STORAGE↗

DOE OSTI2022

Accurately measuring the ionic conductivity of membranes via the direct contact method

Accurately measuring the ionic conductivity of membranes is important both for assessing the performance of new membranes as well as for advancing the fundamental understanding of electric field-driven ion transport in membranes. Yet, despite a considerable number of reports on the topic, there is no standardized method for ionic conductivity measurements. One of the main challenges with ionic conductivity measurements is isolating the membrane resistance from the other resistances in the electrochemical cell. In this study, we present a detailed discussion of factors that affect ionic conductivity measurements with the commonly used direct contact method, in which the membrane contacts the electrodes. Such factors include external resistances due to imperfect contact between the membrane and electrodes, residual impedances due to the sample holder and wiring, and fringe effects. Further, we also present and validate simple methods for isolating the true membrane ionic conductivity in both the through-plane and in-plane orientations. These methods can be implemented with virtually any membrane to obtain accurate and reproducible ionic conductivity values. Finally, we outline recommendations for performing ionic conductivity measurements with the direct contact method and a set of parameters to verify when reporting these results.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Probing the Influence of Multiscale Heterogeneity on Effective Properties of Graphite Electrodes

Graphite electrodes in the lithium-ion battery exhibit various particle shapes, including spherical and platelet morphologies, which influence structural and electrochemical characteristics. It is well established that porous structures exhibit spatial heterogeneity, and the particle morphology can influence transport properties. The impact of the particle morphology on the heterogeneity and anisotropy of geometric and transport properties has not been previously studied. Herein, this study characterizes the spatial heterogeneities of 18 graphite electrodes at multiple length scales by calculating and comparing the structural anisotropy, geometric quantities, and transport properties (pore-scale tortuosity and electrical conductivity). We found that the particle morphology and structural anisotropy play an integral role in determining the spatial heterogeneity of directional tortuosity and its dependency on pore-scale heterogeneity. Our analysis reveals that the magnitude of in-plane and through-plane tortuosity difference influences the multiscale heterogeneity in graphite electrodes.

25 ENERGY STORAGE↗

DOE OSTI2020

Fabrication of a composite anion exchange membrane with aligned ion channels for a high-performance non-aqueous vanadium redox flow battery

Fabrication of high-conductivity ion exchange membranes (IEMs) is crucial to improve the performance of non-aqueous vanadium redox flow batteries (NAVRFBs). In the present work, anion exchange membranes with high-conductivity were fabricated by aligning ion channels of the polymer electrolyte impregnated in porous polytetrafluoroethylene (PTFE) under electric fields. It was observed that the ion channels of the polymer electrolyte were uniformly orientated in the atomic-force microscopy image. Its morphological change could minimize detouring of the transport of BF 4 - ions. The results showed through-plane conductivity was improved from 12.7 to 33.1 mS cm -1 . The dimensional properties of the fabricated membranes were also enhanced compared with its cast membrane owing to the reinforcing effect of the substrate. Especially, the NAVRFB assembled with the optimized membrane showed increased capacities, with a 97% coulombic efficiency and 70% energy efficiency at 80 mA cm -2 . Furthermore, the optimized membrane made it possible to operate the NAVRFB at 120 mA cm -2 . Its operating current density was 120 times higher than that of a frequently used AHA membrane for RFBs.

25 ENERGY STORAGE↗

DOE OSTI2021

Operando video microscopy of Li plating and re-intercalation on graphite anodes during fast charging

Despite the demand for fast-charging lithium (Li)-ion batteries, high-energy-density batteries with thick graphite anodes are limited by Li plating when charging at >4C rates. In this work, plan-view operando video microscopy is applied on >3 mA h cm –2 calendared graphite electrodes to study the dynamic evolution of local state-of-charge (SoC) and Li plating during fast charging. This technique allows for visualization of the spatial heterogeneity in SoC across the electrode, nucleation and growth of Li filaments, Li re-intercalation into graphite, “dead Li” formation, and SoC equilibration. The operando microscopy analysis is complemented by ex situ imaging of through-plane gradients in SoC to gain a three-dimensional visualization of spatial heterogeneity. We demonstrate that (1) Li plating preferentially nucleates on the graphite particles that lithiate fastest during fast charging; (2) the onset of Li plating correlates with the local minimum of the graphite electrode potential; (3) galvanic corrosion currents are responsible for Li re-intercalation, dead Li formation, and SoC re-equilibration after fast charging; and (4) electrochemical signatures during OCV rest or discharge are associated with Li re-intercalation into graphite. Furthermore, this work provides insight into the Li–graphite interactions at the composite electrode level and can be used to inform strategies to diagnose and mitigate Li plating during fast charging.

25 ENERGY STORAGE↗

DOE OSTI2024

Probing the active sites of oxide encapsulated electrocatalysts with controllable oxygen evolution selectivity

Electrocatalysts encapsulated by nanoscopic overlayers can control the rate of redox reactions at the outer surface of the overlayer or at the buried interface between the overlayer and the active catalyst, leading to complex behavior in the presence of two competing electrochemical reactions. This study investigated oxide encapsulated electrocatalysts (OECs) comprised of iridium (Ir) thin films coated with an ultrathin (2–10 nm thick) silicon oxide (SiO x ) or titanium oxide (TiO x ) overlayer. The performance of SiO x |Ir and TiO x |Ir thin film electrodes towards the oxygen evolution reaction (OER) and Fe(II)/Fe(III) redox reactions were evaluated. An improvement in selectivity towards the OER was observed for all OECs. Overlayer properties, namely ionic and electronic conductivity, were assessed using a combination of electroanalytical methods and molecular dynamics simulations. SiO x and TiO x overlayers were found to be permeable to H 2 O and O 2 such that the OER can occur at the MO x |Ir (M = Ti, Si) buried interface, which was further supported with molecular dynamics simulations of model SiO 2 coatings. In contrast, Fe(II)/Fe(III) redox reactions occur to the same degree with TiO x overlayers having thicknesses less than 4 nm as bare electrocatalyst, while SiO x overlayers inhibit redox reactions at all thicknesses. This observation is attributed to differences in electronic transport between the buried interface and outer overlayer surface, as measured with through-plane conductivity measurements of wetted overlayer materials. These findings reveal the influence of oxide overlayer properties on the activity and selectivity of OECs and suggest opportunities to tune these properties for a wide range of electrochemical reactions.

08 HYDROGEN↗

DOE OSTI2020

Accuracy of volumetric flow rate inflow/outflow measurement by integrating PIV velocity fields

In this paper, the usefulness of planar Particle Image Velocimetry (PIV) measurements to determine the volumetric flow rate from a rectangular or round jet exit is assessed. Both two-component PIV (2C–PIV) and through-plane three-component (3C) stereo PIV (SPIV) data sets were acquired at the exit of a turbulent, rectangular nozzle and a round nozzle with Reynolds numbers between 10 000 and 100 000. The PIV data sets were processed using a variety of algorithms. The time-averaged results were then spatially integrated across the jet exits and compared to a calibrated flow meter. Recommendations for each method are developed and discussed with potential drawbacks. The accuracy of the measurement was found to be a weak function of the Reynolds number of the flow. Furthermore, two-component PIV was found to underestimate the volumetric flow rate by 1%–4% depending on the integration scheme and SPIV underestimated volumetric flow rate by 2%.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Relationship between molecular structure and corrugations in self-assembled polypeptoid nanosheets revealed by cryogenic electron microscopy

Designing conformationally dynamic molecules that self-assemble into predictable nanostructures remains an important unmet challenge. This paper describes how atomic-scale cryogenic transmission electron microscopy (cryo-TEM) can be used to explore the relationship between molecular structure and self-assembly of block copolymers. We examined sheetlike micelles formed in water using a series of diblock copolypeptoids with the same hydrophilic block and three distinct crystalline hydrophobic blocks. Our cryo-TEM images revealed all the structures share nansoscale features, but differ in their intermolecular packing geometries. Different molecular arrangements, parallel and antiparallel V-shaped crystal motifs, were revealed by two-dimensional atomic-scale through-plane images. However, images from tilted samples revealed an unexpected feature when the hydrophobic polypeptoid block comprised phenyl rings with substituted bromine atoms at the para position. The nanosheets contained atomic-scale corrugations that were absent in the other systems which comprised unsubstituted aliphatic and aromatic side chains. We hypothesize that these corrugations are due to the dipolar characteristics of the brominated phenyl group and interactions between this group and water molecules. Published by the American Physical Society 2024

36 MATERIALS SCIENCE↗

DOE OSTI2020

Architecture-Based Control of Temperature Gradient-Driven Water Transport in Polymer Electrolyte Fuel Cells

Temperature gradients can move water within the porous media of a polymer electrolyte fuel cell through phase-change-induced (PCI) flow. It is critical to understand PCI flow so that control and distribution of water within a fuel cell can be accomplished. This work investigates the role of architecture, specifically anode land width, on overall cell water content and distribution in the through-plane direction. A specially-designed 4.8 cm 2 fuel cell with precise thermal boundary conditions was imaged with neutrons using two different anode flow field configurations. A new, non-dimensional thermal transport number was developed which quantifies the relative influence of PCI flow on cell water transport. It was found that anode lands larger than the cathode lands cause large thermal gradients that instigate net water flux from the cathode to the anode. An asymmetric configuration with larger anode lands was found to have large changes in water content that were strongly sensitive to cell operating conditions. The thermal transport number developed here enables deduction of the net flux condition based on operating conditions and architecture. This approach enables design of high-performance systems with balanced water management.

25 ENERGY STORAGE↗

DOE OSTI2020

Investigating Liquid Water Transport in Different Pore Structure of Gas Diffusion Layers for PEMFC Using Lattice Boltzmann Method

Proton exchange membrane fuel cells (PEMFC) require a gas diffusion layer (GDL) to aid in the transport of liquid fuel to the catalyst layer. In this work, direct modeling using the Lattice Boltzmann Method (LBM) was applied to X-ray CT scans of four different carbon gas diffusion layers to understand the mass transport properties through the samples. Three injection orientations were used to study local saturation levels, water evolution through the sample, and mass transport behavior at breakthrough conditions. The LBM, combined with computational fluid dynamic modeling techniques, can accurately predict liquid saturation at the macro and micro scale, which provides more insight into the mass transport phenomena through the GDL. The change of pore structure and orientation in both the in-plane and through-plane determines the path that liquid water must take, which could aid or impact PEMFC performance. The outcomes from this work will also benefit any research that needs knowledge of internal mass transport qualities of gas diffusion media.

Sepe, M.↗

DOE OSTI2020

Bridging Scales to Model Reactive Diffusive Transport in Porous Media

Published by ECS. Two novel scale-bridging algorithms to model reaction-diffusion transport in porous media are presented. The algorithms are based on direct numerical simulations and couple the information of a micro-scale model, which accounts for the large field of view provided by micro X-ray computed tomography (X-ray CT), and a nano-scale model, which locally resolves transport in the fine structure extracted from nano X-ray CT. The micro-scale model is discretized in the through-plane direction into a 1D grid, where effective properties and internal boundaries are determined based on the results from the nano-scale model. The validated algorithms are used to examine transport of oxygen in precious group metal-free electrodes considering both zero- and first-order kinetics. Unlike conventional methods, the results show that the effective diffusivity is not a passive property but increases in regions where the reaction-rate coefficient is large. The proposed algorithms account for the multiscale coupling of reaction-diffusion transport and material microstructure, thus improving the predictions compared to conventional methods.

42 ENGINEERING↗

DOE OSTI2020

Modeling Single and Two-Phase Transport in Thin Porous Layers Using a Composite Continuum-Pore Network Formulation

In this work, a composite continuum-pore network formulation is presented to model single and two-phase transport thin porous layers, such as gas diffusion layers in polymer electrolyte fuel cells (PEFCs) and active electrodes in redox flow batteries (RFBs). The formulation can be integrated into CFD codes, thus combining the ease of implementation of continuum-based modeling and the computational power of pore-network modeling. The composite model includes a control volume (CV) mesh at the layer scale, which embeds a cubic pore network [1,2]. The pore-network model is used to determine analytically local anisotropic effective transport properties (local effective diffusivity and permeability), which are mapped onto the CV mesh to simulate transport in the porous transport layer [3,4]. Good agreement is found between the predicted global effective transport properties (global effective diffusivity and permeability) under dry and wet conditions and previous experimental data reported in the literature for Toray TGP-H series carbon paper. Water saturation distributions are also compared with results obtained using X-ray computed tomography [4]. [1] P.A. García-Salaberri, I.V. Zenyuk, J.T. Gostick, A.Z. Weber, Modeling Gas Diffusion Layer in Polymer Electrolyte Fuel Cells Using a Continuum-Based Pore-Network Formulation, ECS Trans. 97 (2020) 615. [2] P.A. García-Salaberri, Modeling diffusion and convection in thin porous transport layers using a composite continuum-network model: Application to gas diffusion layers in polymer electrolyte fuel cells, Int J. Heat Mass Transf. (2020), submitted. [3] P.A. García-Salaberri, J.T. Gostick, G. Hwang, A.Z. Weber, M. Vera, Effective diffusivity in partially-saturated carbon-fiber gas diffusion layers: Effect of local saturation and application to macroscopic continuum models, J. Power Sources 296 (2015) 440–453. [4] P.A. García-Salaberri, G. Hwang, M. Vera, A.Z. Weber, J.T. Gostick, Effective diffusivity in partially-saturated carbon-fiber gas diffusion layers: Effect of through-plane saturation distribution, Int. J. Heat Mass Transf. 86 (2015) 319–333.

Garcia-Salaberri, Pablo↗

DOE OSTI2020

High Performing and Durable Pyrophosphate Based Composite Membranes for Intermediate Temperature Fuel Cells [Slides]

Objective: Develop a novel proton conducting electrolyte operating at >200°C with conductivity σ ≥ 100 mScm –1 and RH < 1%. Fabrication of membranes of less than 40μm thickness while retaining high conductivity will result in ASR <0.04 Ωcm 2 . Evaluate membrane durability in terms of crossover, shorting resistance, and open circuit voltage, as well as against temperature cycling. Relevance: Operating FCs in the intermediate temperature range has the potential to greatly reduce cost and simplify water and thermal management. This effort requires novel materials and approaches to meet DOE membrane performance and durability targets. MPP/Polymer composite membranes show promise in early development for application in IT-FCs for transportation applications. Approach: We have demonstrated that both cation dopants and phosphate precursor influence MPP conductivity and identified the most promising MPP compositions for membrane fabrication. The ceramic MPP materials are fabricated as a composite membrane in a 90:10 wt% ratio with Nafion. We have modified our membrane fabrication procedure to improve the density of our membranes. Accomplishments: We demonstrated through-plane membrane conductivity of 95mScm -1 at T > 200°C and RH<0.04bar with a thickness 50μm. We demonstrated FC performance up to 94hrs at 220°C and <1% RH with a 50μm thick membrane exhibiting an OCV of 0.98V and ASR of 0.08 Wcm 2 . Future work: Further decrease in ASR is expected by decreasing the membrane thickness to <40μm. ITPP with higher P:M ratio will be used to increase the conductivity of the starting material. Long term durability will be assessed against DOE technical targets

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2025

Multilayer Electrodes with Metalized Polymer Current Collector for High-Energy Lithium-Ion Batteries with Extreme-Fast-Charging Capability

The pursuit of batteries capable of extreme fast charging (XFC), that also satisfy high energy and safety criteria, poses a significant challenge to current lithium-ion battery technologies. Additionally, the increasing demand for aluminum (Al) and copper (Cu) in electrification, and vehicle light weighting is driving these metals towards near-critical status in the medium term. This study introduced metalized polymer films by depositing an Al or Cu thin layer onto two sides of a polyethylene terephthalate (PET) film – named mPET/Al and mPET/Cu, as lightweight, cost-effective alternatives to traditional metal current collectors in LIBs. We have utilized current collectors that significantly reduce weight (by 73%), thickness (by 33%), and cost (by 85%) compared to traditional metal foil counterparts. We conducted an extensive evaluation of their mechanical and electrical properties, including in-plane and through-plane resistivities, affirming their suitability for the roll-to-roll battery manufacturing process. Additionally, a novel XFC testing protocol was employed to thoroughly assess the cells' (both half and full-cell) performance across various C-rates and under long-term tests. These advancements have the potential to enhance energy density to 280 Wh/kg at the electrode level under 10-minute charging at 6C. Through testing, including a novel XFC protocol across various C-rates and long-term cycling (up to 1000 cycles) in different cell configurations, we have demonstrated the superior performance of these metalized polymer films. Notably, mPET/Cu and mPET/Al foils exhibited comparable capacities to conventional cells under XFC, with the mPET cells showing a 27% improvement in energy density at 6C and maintaining significant energy density after 1000 cycles. This study underscored the potential of mPET foils to revolutionize the roll-to-roll battery manufacturing process and significantly advance the performance metrics of LIBs in EV applications. Moreover, our results suggest that there is potential to enhance the performance of mPET foils, especially mPET/Al, by optimizing the manufacturing process to achieve higher conductivity.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2026

Towards a Unified Low-Cost Flow Plate, Flow-Field, PTL Solution for Proton Exchange Membrane Electrolyzers

Proton exchange membrane (PEM) water electrolysis is a highly efficient method for hydrogen production. Research cells typically consist of one proton exchange membrane, two catalyst layers, two porous transport layers, two flow-field plates, and two endplates. In commercial systems, the machined flow-field plates that are employed in research cells are typically replaced by stamped parts or open mesh material solutions to reduce manufacturing cost at scale. Nonetheless, the cell contains about 8 total interfaces: bipolar plate / flow plate material / porous transport medium / electrode / membrane / electrode / porous transport medium / flow plate material / bipolar plate. All these materials and interfaces need to be optimized for maximum performance and efficiency. Reducing the amount of interfaces by combining individual cell components directly benefits the fabrication cost (by reducing the parts count and the needs for surface coatings) and the electrochemical performance (by reducing ohmic losses). We have designed a novel PEM electrolysis cell with a piece of channeled titanium felt functioning as both the anode flow-field and the PTL, referred to as the channeled diffusion layer (CDL). The pores of the felt facilitate both in-plane and through-plane diffusion, ensuring maximum catalyst utilization while also minimizing mass transport loss. The titanium felt can be mass manufactured with existing stamping and forming methods and is therefore a promising candidate to reduce the capital cost of PEM electrolyzers whilst improving hydrogen production efficiency. Experiments conducted with 3mg IrOx/cm2 loading MEAs have shown a approximately 40% boost in peak current by implementing the CDL design. Low catalyst-loading MEAs are being tested in ongoing experiments and their results will be discussed and compared.

08 HYDROGEN↗

DOE OSTI2022

Measurement of ion transport properties in ion exchange membranes for photoelectrochemical water splitting

Photoelectrochemical (PEC) water-splitting systems have the unique ability to produce renewable hydrogen directly from sunlight, independent of the electrical grid. These systems are therefore appealing technological options for resilient long-term energy storage. Ion selective membranes, such as monopolar and bipolar membranes, are a vital component of PEC water-splitting systems. These membranes allow for ionic conduction between the cathode and anode chambers, separation of products, and improved catalyst environments for reactions. In order to measure key properties and to study the performance of these ion exchange membranes, it is imperative to develop a robust testing protocol that can be used across the field. This paper introduces two standard electrochemical cells designed to directly measure ion transport properties in monopolar and bipolar membranes. The first electrochemical cell uses commercially available Pt disk electrodes to preform electrochemical impedance spectroscopy (EIS) and reliably measure through-plane conductivity of monopolar membranes. The second electrochemical cell uses four-point measurements with Luggin capillaries and a series of membrane configurations to perform current density-voltage and Faradaic efficiency (FE) measurements for water dissociation (WD) reactions on bipolar membranes. The cell designs and techniques laid out below allow for accurate measurement of ion transport parameters in ion exchange membranes, direct comparison of membranes being developed across the field, and in turn, greater advancements in ion exchange membranes and PEC water-splitting systems.

cation exchange membrane↗

DOE OSTI2023

Using light and X-ray scattering to untangle complex neuronal orientations and validate diffusion MRI

Disentangling human brain connectivity requires an accurate description of nerve fiber trajectories, unveiled via detailed mapping of axonal orientations. However, this is challenging because axons can cross one another on a micrometer scale. Diffusion magnetic resonance imaging (dMRI) can be used to infer axonal connectivity because it is sensitive to axonal alignment, but it has limited spatial resolution and specificity. Scattered light imaging (SLI) and small-angle X-ray scattering (SAXS) reveal axonal orientations with microscopic resolution and high specificity, respectively. Here, we apply both scattering techniques on the same samples and cross-validate them, laying the groundwork for ground-truth axonal orientation imaging and validating dMRI. We evaluate brain regions that include unidirectional and crossing fibers in human and vervet monkey brain sections. SLI and SAXS quantitatively agree regarding in-plane fiber orientations including crossings, while dMRI agrees in the majority of voxels with small discrepancies. We further use SAXS and dMRI to confirm theoretical predictions regarding SLI determination of through-plane fiber orientations. Scattered light and X-ray imaging can provide quantitative micrometer 3D fiber orientations with high resolution and specificity, facilitating detailed investigations of complex fiber architecture in the animal and human brain.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2017

Synthesis and Thermal Conductivity of Exfoliated Hexagonal Boron Nitride/Alumina Ceramic Composite

Exfoliated hexagonal boron nitride (hBN)/alumina composite can be fabricated by following the process of (1) heating a mixture of hBN, AlCl3, and NaF in nitrogen for intercalation; (2) heating the intercalated product in air for exfoliation and at the same time converting the intercalate (AlCl3) into Al2O3, (3) rinsing the oxidized product, (4) coating individual exfoliated hBN platelets that contain Al2O3 with new layers of aluminum oxide, and finally, (5) hot pressing the product into the composite. The composite thus obtained has a composition of approximately 60 percent by weight hBN and 40 percent by weight alumina. Its in-plane and through-plane thermal conductivity were measured to be 86 and 18 watts per meter Kelvin, respectively, at room temperature.

Hung, Ching-cheh↗