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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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Insight of BaCe 0.5 Fe 0.5 O 3– δ twin perovskite oxide composite for solid oxide electrochemical cells

One-pot synthesized twin perovskite oxide composite of BaCe 0.5 Fe 0.5 O 3–δ (BCF), comprising cubic and orthorhombic perovskite phases, shows triple-conducting properties for promising solid oxide electrochemical cells. Phase composition evolution of BCF under various conditions was systematically investigated, revealing that the cubic perovskite phase could be fully/partially reduced into the orthorhombic phase under certain conditions. The reduction happened between the two phases at the interface, leading to the microstructure change. As a result, the corresponding apparent conducting properties also changed due to the difference between predominant conduction properties for each phase. Based on the revealed phase composition, microstructure, and electrochemical properties changes, a deep understanding of BCF's application in different conditions (oxidizing atmospheres, reducing/oxidizing gradients, cathodic conditions, and anodic conditions) was achieved. Triple-conducting property (H + /O 2– /e – ), fast open-circuit voltage response (~16–~470 mV) for gradients change, and improved single-cell performance (~31% lower polarization resistance at 600°C) were comprehensively demonstrated. Besides, the performance was analyzed under anodic conditions, which showed that the microstructure and phase change significantly affected the anodic behavior.

08 HYDROGEN↗
DOE OSTI2020

Computational Modeling of Heterogeneity of Stress, Charge, and Cyclic Damage in Composite Electrodes of Li-Ion Batteries

Charge heterogeneity is a prevalent feature in many electrochemical systems. In a commercial cathode of Li-ion batteries, the composite is hierarchically structured across multiple length scales including the sub-micron single-crystal primary-particle domains up to the macroscopic particle ensembles. The redox kinetics of charge transfer and mass transport strongly couples with mechanical stresses. This interplay catalyzes substantial heterogeneity in the charge (re)distribution, stresses, and mechanical damage in the composite electrode during charging and discharging. We assess the heterogeneous electrochemistry and mechanics in a LiNi x Mn y Co z O 2 (NMC) cathode using a fully coupled electro-chemo-mechanics model at the cell level. A microstructure-resolved model is constructed based on the synchrotron X-ray tomography data. We calculate the stress field in the composite and then quantitatively evaluate the kinetics of surface charge transfer and Li transport biased by mechanical stresses. We further model the cyclic behavior of the cell. The repetitive deformation of the active particles and the weakening of the interfacial strength cause gradual increase of the interfacial debonding. The mechanical damage impedes electron transfer, incurs more charge heterogeneity, and results in the capacity degradation in batteries over cycles.

25 ENERGY STORAGE↗
DOE OSTI2022

Evaluation of Applied Stress on Atmospheric Corrosion and Pitting Characteristics in 304L Stainless Steel

For this study, the effects of applied stress, ranging from tensile to compressive, on the atmospheric pitting corrosion behavior of 304L stainless steel (SS304L) were analyzed through accelerated atmospheric laboratory exposures and microelectrochemical cell analysis. After exposing the lateral surface of a SS304L four-point bend specimen to artificial seawater at 50°C and 35% relative humidity for 50 d, pitting characteristics were determined using optical profilometry and scanning electron microscopy. The SS304L microstructure was analyzed using electron backscatter diffraction. Additionally, localized electrochemical measurements were performed on a similar, unexposed, SS304L four-point bend bar to determine the effects of applied stress on corrosion susceptibility. Under the applied loads and the environment tested, the observed pitting characteristics showed no correlation with the applied stress (from 250 MPa to -250 MPa). Pitting depth, surface area, roundness, and distribution were found to be independent of location on the sample or applied stress. The lack of correlation between pitting statistics and applied stress was more likely due to the aggressive exposure environment, with a sea salt loading of 4 g/m 2 chloride. The pitting characteristics observed were instead governed by the available cathode current and salt distribution, which are a function of sea salt loading, as well as pre-existing underlying microstructure. In microelectrochemical cell experiments performed in Cl - environments comparable to the atmospheric exposure and in environments containing orders of magnitude lower Cl - concentrations, effects of the applied stress on corrosion susceptibility were only apparent in open-circuit potential in low Cl - concentration solutions. Cl - concentration governed the current density and transpassive dissolution potential.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructure Scale Lithium-Ion Battery Modeling: Part II. On In-Plane Heterogeneities and the Mechanisms that Regulate Them

Li-ion batteries performance and degradation are typically modeled at the macroscopic scale, that is neglecting in-plane heterogeneities that can arise from non-uniform electrode microstructures. Herein, a microstructure scale electrochemical model is used to quantify the impact of microstructure heterogeneity on cell performance during fast charging. The model predicts the electrolyte and solid concentration in-plane standard deviation can reach, respectively, ≈200 mol·m −3 and 6–7 kmol·m −3 locally. Further, the intercalation current density in-plane relative standard deviation can reach extremely high values, around 100% in the cathode and well above 100% in the anode graphite. These denote highly non-uniform lithiation rates and material utilization within each slice of the microstructure along the cell thickness. Non-uniform curvatures, at the particle scale (surface roughness) and between particles (size distribution), were found to initiate these in-plane heterogeneities, while an OCP-induced mechanism subsequently regulates them. The present model provides new insights into small length scale heterogeneity impact on battery performance not available with standard macro-scale/P2D modeling.

25 ENERGY STORAGE↗
DOE OSTI2025

Laser ablation of high-loading Li-ion battery electrodes improves accessible capacity and cycle life for Behind-the-Meter Storage

Adoption of Behind-the-Meter Storage (BTMS) requires design of batteries that enable high safety, long cycle life, and low cost at the system level. Pairing Li 4 Ti 5 O 12 (LTO) with LiMn 2 O 4 (LMO) achieves targets related to safety and cycle life, but these materials' low energy densities contribute to higher cost at the system scale. Increasing electrode loading is a simple approach to improve energy density, but comes with a trade-off in electrode utilization due to long, tortuous Li + diffusion pathways. Here, laser ablation is used to microstructure (pattern) high-loading electrodes to enhance electrode performance through improved Li + diffusion pathways. Four cell types, comprising combinations of standard or patterned anode and cathode, were prepared to evaluate the effects of laser ablation at each electrode. A rate test shows that patterning electrodes enhances active material utilization at ≳1C rates. Patterning the cathode yields the most benefit, as cells with a patterned cathode demonstrate a ~20% higher accessible capacity than those without at 1.4C. Additionally, 1C capacity retention of cells with patterned cathode (91% through 3000 cycles) is significantly improved over cells with only the anode patterned (64%) and non-patterned electrodes (50%). Characterization of post-mortem cells before and after refreshing their electrolyte suggests that 1C capacity retention is improved by mitigation of electrode "dry-out". We hypothesize that the microstructure acts as a reservoir of additional electrolyte, or a path for gas to escape, so that active material remains wetted throughout long-term cycling, and/or the microstructure may reduce localized, gas-forming overpotentials in the high-loading electrode.

25 ENERGY STORAGE↗
DOE OSTI2021

High-performing commercial Fe–N–C cathode electrocatalyst for anion-exchange membrane fuel cells

Here, to reduce the cost of fuel cell stacks and systems, it is important to create commercial catalysts that are free of platinum group metals (PGMs). To do this, such catalysts must have very high activity, but also have the correct microstructure to facilitate the transport of reactants and products. Here, we show a high-performing commercial oxygen reduction catalyst that was specifically developed for operation in alkaline media and is demonstrated in the cathode of operating anion-exchange membrane fuel cells (AEMFCs). With H 2 /O 2 reacting gases, AEMFCs made with Fe–N–C cathodes achieved a peak power density exceeding 2 W cm –2 (>1 W cm –2 with H 2 /air) and operated with very good voltage durability for more than 150 h. These AEMFCs also realized an iR-corrected current density at 0.9 V of 100 mA cm –2 . Finally, in a second configuration, Fe–N–C cathodes paired with low-loading PtRu/C anodes (0.125 mg PtRu per cm 2 , 0.08 mg Pt per cm 2 ) demonstrated a specific power of 10.4 W per mg PGM (16.25 W per mg Pt).

25 ENERGY STORAGE↗
DOE OSTI2024

Slug-flow synthesis of NCMA: Effect of substitution of cobalt with aluminum on the electrochemical performance of Ni-rich cathode for lithium-ion battery

Nickle-rich Li[Ni 1-x-y Co x Mn y ]O 2 (x, y≤0.1) (NCM) layered materials are known as promising cathode materials for next-generation lithium-ion batteries and electric vehicles owing to their high-reversible capacity and operating voltage of up to 3.6 vs Li/Li + . However, issues, such as irreversible phase transition, cation mixing, microcrack formation, thermal and structural stability of the material prevent its widespread adoption. Although, cation doping is a well-known technique to enhance the electrochemical performance of the NCM-based cathode material, the performance of the material is very sensitive to the doping amount. In this study, three Al-doped quaternary Ni-rich cathode materials Li[Ni 0.85 Co (0.1-x) Mn 0.05 Al x ]O 2 (where, x=0–0.04) (NCMA) are synthesized through three-phase slug-flow based continuous manufacturing process followed by high temperature calcination to study the effect of Aldoping on the performance of the cathode material while reducing Co. The slug flow-based production platform has several advantages, like particle size uniformity, high production rate, and homogeneity in elemental distribution. It is found that with an increase in Al content, the specific capacity decreases but the cyclic stability and rate capability increases. Furthermore, optimum Al-doping not only compensates for the adverse effect of low Co by decreasing the extent of cation mixing, but it also minimizes the electrode polarization and cracking of the particles.

25 ENERGY STORAGE↗
DOE OSTI2024

Low-Temperature Molten Salt Electrochemical CO 2 Upcycling for Advanced Energy Materials

One strategy for addressing the climate crisis caused by CO 2 emissions is to efficiently convert CO 2 to advanced materials suited for green and clean energy technology applications. Porous carbon is widely used as an advanced energy storage material because of its enhanced energy storage capabilities as an anode. Herein, we report electrochemical CO 2 upcycling to solid carbon with a controlled microstructure and porosity in a ternary molten carbonate melt at 450 °C. Controlling the electrochemical parameters (voltage, temperature, cathode material) enabled the conversion of CO 2 to porous carbon with a tunable morphology and porosity for the first time at such a low temperature. Additionally, a well-controlled morphology and porosity are beneficial for reversible energy storage. In fact, these carbon materials delivered high specific capacity, stable cycling performances, and exceptional rate capability even under extremely fast charging conditions when integrated as an anode in lithium-ion batteries (LIBs). In conclusion, the present approach not only demonstrated efficient upcycling of CO 2 into porous carbon suitable for enhanced energy storage but can also contribute to a clean and green energy technology that can reduce carbon emissions to achieve sustainable energy goals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Flash electropolishing for TEM: Reducing FIB‐induced defects in tungsten with protocols for new materials

Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Using a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.

TEM sample preparation↗
DOE OSTI2022

Performance of Different Water-Based Binder Formulations for Ni-Rich Cathodes Evaluated in LiNi 0.8 Mn 0.1 Co 0.1 O 2 //Graphite Pouch Cells

Water-based processing for lithium-ion battery electrodes is attractive due to its lower manufacturing cost and smaller environmental impact. However, multiple challenges associated with aqueous cathode processing have hindered commercial adoption. Polymer binders are an important component of the electrode, and thus the choice of binders can alter electrode cycling performance significantly. In this work, four different water-based binder combinations are investigated for Ni-rich LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811)-based cathodes, with a focus on the long-term electrochemical performance in practical-format full pouch cells. No additional pH-modulating additives were added to the aqueous cathode slurries, and no protective coatings were present on the cathode or aluminum current collector. Results are compared with the standard PVDF/NMP-based binder/solvent combination, used as a baseline. The influence of water-based binder type on slurry rheology and electrode microstructure are also discussed. All cells made by water-processing had worse rate performance compared to the baseline. However, the cell discharge capacity after 1000 U.S. Advanced Battery Consortium (USABC) cycles at C/3 charge/discharge rate was comparable to the baseline for two of the water-based cathode formulations (CMC & JSR, and LiPAA), demonstrating the potential viability of aqueous-processed Ni-rich cathodes at a commercial scale.

25 ENERGY STORAGE↗
DOE OSTI2022

Uncertainty Quantification for Dissimilar Material Joints Under Corrosion Environment

Abstract Self-Piercing Riveting (SPR) is one of the most commonly used methods for joining dissimilar materials in the automotive industry. These joints are popular due to their adaptability, high performance and short cycle time. However, since these joints involve two dissimilar materials, they are susceptible to galvanic corrosion in the presence of an electrolyte which is driven by the difference in the equilibrium potential of the metals. This can affect the safety and resilience of these joints. In this paper, we focus on galvanic corrosion in Al-Fe SPR joints. A Machine learning (ML) based surrogate model, which is based off of FE simulations, for statistical corrosion analysis is developed. This model enables the resilience and reliability analysis of SPR joints under corrosion environment. In this study, first a physics-based finite element (FE) corrosion model has been developed to simulate the galvanic corrosion between a Fe cathode and an Al anode of a SPR joint. This model takes into account the effect of the crystal microstructure of the Al anode and the precipitation of the corrosion product. Several geometric and environmental factors including crevice gap, roughness of anode, conductivity, pH and the temperature of the electrolyte that effect corrosion are investigated. A thorough Uncertainty Quantification (UQ) analysis is conducted for the overall corrosion behavior of the Fe-Al SPR joints using a novelistic Probabilistic Confidence-Based Adaptive Sampling (PCAS) technique. PCAS is used to train the surrogate model by identifying the critical sampling points and thus reducing the overall computational costs. It is found that the electrolyte temperature has the largest effects on the material loss and needs to be managed closely for better corrosion control. By understanding the corrosion performance and resultant uncertainty impact on SPR joints, the reliability and resilience of these joints can be improved.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Heterogeneity of the Dominant Causes of Performance Loss in End-of-Life Cathodes and Their Consequences for Direct Recycling

Recycling Li-ion batteries from electric vehicles is critical for reducing costs and supporting the development of a domestic battery supply chain. Direct recycling of cathodes, like LiNixMnyCozO2 (NMC), is attractive due to its low cost, energy use, and emissions compared to traditional recycling techniques. However, a comprehensive understanding of the active material properties at end-of-life is needed to guide direct recycling processes and the performance-dependent reuse applications. Here, NMC material from an end-of-life commercial pouch cell is characterized and bench-marked against pristine non-cycled counterparts with respect to capacity, impedance, crystallography, morphology, and microstructure to identify major degradation modes and understand variability in the end-of-life material. The spatial heterogeneity of each property throughout the cell is also quantified. While the degraded material demonstrated similar capacity as the pristine, its impedance and rate capability are severely diminished. Furthermore, samples from the periphery of the electrode layers showed more severe performance loss compared to samples extracted from central regions. The dominant culprit of performance loss is the material microstructure, where the magnitude of particle cracking showed the strongest correlation to the impedance components that are most unfavorably impacted. This work suggests severe cracks in cathode active materials are the primary challenge that direct recycling methods must overcome.

25 ENERGY STORAGE↗
DOE OSTI2021

Multifunctional Utilization of Pitch-Coated Carbon Fibers in Lithium-Based Rechargeable Batteries

This work reports carbon fibers as an electrode material and current collector for dual-carbon and lithium-ion batteries. Here, fully graphitic and semigraphitic carbon fibers undergo anion intercalation beyond 4.5 V versus Li/Li + . Symmetric dual-carbon full cells using a pitch-coated fully graphitic carbon fiber mat as both cathode and anode delivers an energy-density of 276 and 322 Wh kg -1 at 342 W kg -1 power density in the voltage range of 3.0–5.0 and 3.0–5.2 V, respectively. On the other hand, nongraphitic carbon fibers do not exhibit anion intercalation up to 5.2 V and can be used as a current collector. They also possess a larger number of Li + storage sites in their randomly oriented microstructure when used as an anode. A lithium-ion full cell with double carbon-coated C-LiFePO 4 loaded on nongraphitic carbon fiber as a cathode and pitch-coated nongraphitic carbon fiber as an anode exhibits 202.6 and 75.2 Wh kg -1 energy density at power densities of 46.75 W kg -1 and 11.7 kW kg -1 , respectively in 2.0–3.5 V range. This pitch-coated carbon fiber-based battery configuration eliminates the need for metal foils and costly fluorinated binders, lowers overall weight of the cell, and is capable of sustaining mechanical stress and thermal shock.

PF6− intercalation↗
DOE OSTI2023

The effect of ink ball milling time on interparticle interactions and ink microstructure and their influence on crack formation in rod-coated catalyst layers

This work investigates the influence of ballmilling (sometimes also referred to as jar roller milling) time on cathode catalyst layer (CL) inks and electrode properties using formulations and coating methods relevant for industrial manufacturing. Four CL inks with the same composition were milled for 24, 48, 72, or 96 h. Rheological investigation of these inks showed a reduction of elastic moduli and steady-shear viscosity with continuous ink milling, which is correlated to a decrease in particle-particle interactions as well as formation of smaller agglomerates. Optical microscopy (OM) analysis of the fabricated electrodes revealed a trend in surface crack formation; formulations milled for 24 h contained the lowest average surface crack area percentages of 0.370% at heavy-duty loadings of ~0.300 mg Pt cm -2 , compared to 2.418% for the ink milled for 96 h. Further characterization of the CL through transmission electron microscopy (TEM) imaging showed a decrease in the mean agglomerate and pore size with milling time. Furthermore, these smaller electrode features were consistent with reduced fracture resistance and, hence, development of larger stresses during drying. Our results highlight the need to consider ink processing as an important component in defect-free CL manufacturing.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2022

Effect of the grain arrangements on the thermal stability of polycrystalline nickel-rich lithium-based battery cathodes

One of the most challenging aspects of developing high-energy lithium-based batteries is the structural and (electro)chemical stability of Ni-rich active cathode materials at thermally-abused and prolonged cell cycling conditions. Here, we report in situ physicochemical characterizations to improve the fundamental understanding of the degradation mechanism of charged polycrystalline Ni-rich cathodes at elevated temperatures (e.g., ≥ 40 °C). Using multiple microscopy, scattering, thermal, and electrochemical probes, we decouple the major contributors for the thermal instability from intertwined factors. Our research work demonstrates that the grain microstructures play an essential role in the thermal stability of polycrystalline lithium-based positive battery electrodes. We also show that the oxygen release, a crucial process during battery thermal runaway, can be regulated by engineering grain arrangements. Furthermore, the grain arrangements can also modulate the macroscopic crystallographic transformation pattern and oxygen diffusion length in layered oxide cathode materials.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Operating Stresses and Their Effects on Degradation of LSM-Based SOFC Cathodes

The performance of solid oxides fuel cells (SOFCs) with four different Mn excess of lanthanum strontium manganite (LSM) -based cathodes were examined under different temperatures (1,000 °C, 900 °C), current densities (0, 380, and 760 mA cm -2 ), and cathode atmospheres (p O 2 )=0.1,0.15,0.21) for durations ranging from 58 to 1,008 h. Each yttria-stabilized zirconia (YSZ) electrolyte-supported “button” cell had a porous Ni/YSZ composite anode and a porous LSM/YSZ composite cathode. The cells’ output voltage versus time were recorded and electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV) measurements were performed every 24 hours. The total area specific resistance (ASR) was calculated from these measurements. The values of ASR from both EIS and LSV were comparable between each other but lower than that from durability test. Distribution of relaxation times (DRT) analysis was performed to investigate the electrochemical processes and their corresponding relaxation frequencies as well as their attributions to the total ASR. The series resistance and parallel resistance that obtained from the equivalent circuit fit of the Nyquist plot were higher at low temperature and low p O 2 regardless of LSM compositions. The area of the peaks derived from DRT analysis increased with time during individual tests. The microstructures of the tested cells were examined using scanning electron microscopy and energy-dispersive x-ray spectroscopy (SEM/EDS). Manganese oxide particles were observed near the cathode-electrolyte interface after prolonged (1,008 h) testing in air of a cell with LSM of 11% manganese excess, and after a short test (58 h) under low oxygen (p O 2 = 0.10) in a cell with LSM of 5% manganese excess. However, the role of MnOx in cell degradation is still unknown.

08 HYDROGEN↗
DOE OSTI2020

Structural Distortion Induced by Manganese Activation in a Lithium-Rich Layered Cathode

The search for batteries with high energy density has highlighted lithium-rich manganese-based layered oxides due to their exceptionally high capacity. Although it is clear that both cationic and anionic redox are present in the charge compensation mechanism, the microstructural evolution of the Li 2 MnO 3 -like phase during anionic redox and its role in battery performance and structural stability are still not fully understood. Here, we systematically probe microstructural evolution using spatially resolved synchrotron X-ray measurements and reveal an underlying interaction between the Li 2 MnO 3 -like domains and bulk rhombohedral structure. Mn ion activation and a previously unobserved structural distortion are discovered at high voltages, and can be related to structural strain present in the Li 2 MnO 3 -like phase upon substantial lithium ion extraction. Moreover, we elucidate a correlation between this structural distortion and irreversible phase transitions by thermally perturbing delithiated samples. These insights highlight a pathway toward achieving high capacity cathode materials required for future commercial applications.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Modeling the 4D discharge of lithium-ion batteries with a multiscale time-dependent deep learning framework

The lithium-ion battery (LIB) field is moving towards the direction of investigating spatially resolved physical phenomena in the 3D porous microstructure of electrodes. These pore-scale simulations give new insights into the local dynamics of lithiation/de-lithiation and charge transport, Nevertheless, the computational time of these simulations limits the integration of these models in optimization workflows of cycling conditions or electrode manufacturing processes. Machine learning models present a way of assessing in real-time the performance of materials. While several successful techniques for replicating simulations with machine learning have been proposed, this case study presents a more demanding problem, due to the necessity of understanding the behavior of heterogeneous 3D local data, as it evolves in time: this poses both a scientific and a technical challenge. To this end, we propose an autoregressive multiscale convolutional neural network model to predict relevant quantities at the pore-scale in the solid phase: the lithium concentration (in the active material) and potential (in the active material and carbon binder). Here, these are ultimately used to reconstruct the battery discharge curve. 3D images of the electrode microstructures are the input to the network, trained with a dataset of finite element method simulations to predict the discharge behavior of the cathode side in lithium ion batteries. We propose this machine learning model as a proof-of-concept of the applicability of multiscale networks for time-dependent physics problems. The trained model exhibits very high accuracy (with errors lower than 2 %) in forecasting the discharge behavior of new unseen cathodes.

25 ENERGY STORAGE↗