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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

In situ X-ray spatial profiling reveals uneven compression of electrode assemblies and steep lateral gradients in lithium-ion coin cells

Coin cells are used extensively as test devices in battery research for evaluation of new materials and optimization of cycling protocols. Here, in situ X-ray diffraction profilometry is used to characterize spatial distribution of the active materials, lithiation, and phase distribution in electrodes of NCM523/graphite coin cells. The X-ray data indicate uneven areal compression of the electrode assembly in such cells, which we trace to a specific design feature that leads to elastic deformation of a metal spacer. Steep lithiation gradients observed in the electrodes imply radially-dependent resistivity, for which uneven compression of the separator is a likely cause. Electrochemical model calculations suggest that variable porosity of the polymer separator would account for the salient features of spatial profiles observed in these coin cells.

25 ENERGY STORAGE↗
DOE OSTI2021

Achieving Highly Reproducible Results in Graphite-based Li-ion Full Coin Cells

Electrode materials, cathodes or anodes, are mostly evaluated in half coin cells where lithium (Li) metal is used. However, due to the instability nature of Li metal, the cycling performances of the half cells is more likely reflecting Li anode stability instead of the coupled electrodes, questioning the conclusions. Full coin cells utilizing graphite as the anode effectively assesses materials. But the key factors of preparing full coin cells with reproducible performances have rarely been discussed and overlooked leading to many inconsistent results. This work discusses the scientific gap between cell preparation and observed electrochemical performances to unveil the key parameters for achieving consistent and reliable results in full coin cells, critical for effective evaluation of any new materials tested under relevant conditions. The knowledge from this work is broadly applicable in other full cells systems such as Si-based full cells or Na-ion batteries.

Hu, Jiangtao↗
DOE OSTI2025

Lithium–Sulfur Batteries: 3D Printed Tools and Assembly Techniques for Repeatable Lab-Scale Coin Cell Manufacturing

The coin cell form factor has become a standard in energy storage research owing to its relatively low cost, low quantity of requisite electroactive material, fast experimental turnover, and capability to generate publishable quality data. Coin cell assembly at the lab-scale requires precise manual alignment of the many internal components of a cell to yield a properly functioning device. Truly repeatable device assembly presents a significant challenge to the acquisition of reliable data. In this report, we present a three-dimensional (3D) printable design for a coin cell alignment device and describe techniques for a generalized workflow to achieve reproducible coin cell assembly of lithium-based batteries. Standardized assembly techniques using readily accessible, purpose-built tools were demonstrated for labscale production of lithium−sulfur (Li−S) coin cells. Li−S batteries fabricated using the alignment device as well as conductive adhesive incorporated workflows afforded coin cells with up to 35% reduction of assembly times, comparable or better functional cell yields, and improved electrochemical device performance with more consistent and up to 150 mAh/g higher average discharge capacities coupled with Coulombic efficiency increases of up to 2.0% over manually aligned cell assembly techniques.

Batteries↗
DOE OSTI2025

Characterizing Hazardous Gases from NMC811 Materials and Coin Cells with TGA and Tube-Furnace FTIR-MS Evolved-Gas-Analysis

Abuse testing is useful for informing the risks of different battery chemistries but has been limited to larger formats. This paper conducted thermal abuse tests at the smaller coin cell level to determine its relevance in specifying vent gas flammability and toxicity. A nitrogen purge carried the evolved gases into a parallel Fourier-transform infrared spectrometer (FTIR) and a mass spectrometer (MS) downstream of the tube furnace. The experimental system was validated by comparing evolved gas data for single components between the tube furnace system and a thermogravimetric analysis (TGA) instrument. Multiple samples were tested during validation, including CaCO3, electrolyte, delithiated NMC 811 cathode, and lithiated graphite anode. Temperature-resolved gas evolution of HF, CO2, CO, H2, and hydrocarbons from isolated components helped to characterize the emission sources. A previously unreported H2 generation mechanism was found. It was shown that the reduced NMC cathode acts as a catalyst to crack polypropylene-decomposed hydrocarbons into H2 at around 450 degrees C. It was also shown, while studying LiPF6 thermal decomposition, that using the tube furnace with a coin cell casing as the sample holder has some advantages for evolved-gas analysis of environmentally sensitive samples relative to testing in TGA instruments. After validation with single components, a fully charged NMC 811 coin cell was failed in the tube furnace. The measured evolved gases were found to be a combination of the species measured from the single component tests. H2 formation related to the reduced cathode was found to have greater abundance than H2 formed from the anode. Hydrogen fluoride emission factors and diethyl carbonate conversion emission factors assist in understanding the gaseous hazards for larger format cells.

25 ENERGY STORAGE↗
DOE OSTI2021

NMR spectroscopy of coin cell batteries with metal casings

Battery cells with metal casings are commonly considered incompatible with nuclear magnetic resonance (NMR) spectroscopy because the oscillating radio-frequency magnetic fields (“rf fields”) responsible for excitation and detection of NMR active nuclei do not penetrate metals. Here, we show that rf fields can still efficiently penetrate nonmetallic layers of coin cells with metal casings provided “B 1 damming” configurations are avoided. With this understanding, we demonstrate noninvasive high-field in situ 7 Li and 19 F NMR of coin cells with metal casings using a traditional external NMR coil. This includes the first NMR measurements of an unmodified commercial off-the-shelf rechargeable battery in operando, from which we detect, resolve, and separate 7 Li NMR signals from elemental Li, anodic β-LiAl, and cathodic Li x MnO 2 compounds. Real-time changes of β-LiAl lithium diffusion rates and variable β-LiAl 7 Li NMR Knight shifts are observed and tied to electrochemically driven changes of the β-LiAl defect structure.

25 ENERGY STORAGE↗
DOE OSTI2025

The Role of Catholyte Modulation in Suppressing the Initial Capacity Fade of Zinc Electrolytic Manganese Dioxide Coin Cells

Despite its potential for zinc–manganese oxide batteries, electrolytic manganese dioxide (EMD) can experience capacity fade due to a deficiency in the Mn 2+ supply at the cathode electrolyte interphase (CEI) from side reactions, even in the presence of an electrolyte additive. In this work, electrolyte loading modulation at the cathode electrolyte interface (CEI) was correlated with Zn∥EMD cell capacity retention and cycling performance, as a proposed measure to curb the initial capacity fade observed in EMD. Initial galvanostatic charge/discharge cycling, with varied electrolyte loading, revealed severe capacity fade (from ~188 to 10 mAh g –1 for the highest loading of 200 μL) within the first 15 cycles. Such a decrease in cell capacity is correlated with the formation of a Mn 4+ deposit on the current collector and consequently, the Mn 2+ depletion at CEI, as was supported by elemental and Raman analyses. Interestingly, confinement of the electrolyte to the CEI at a lower (≤15 μL) electrolyte loading mitigated Mn 4+ side-deposition, maintaining the cell capacity at >80% over the first 15 cycles. Interfacial Mn supply/depletion could be monitored via voltammetric analysis based on changes of the Zn 2+ insertionreduction peak. Additional galvanostatic experiments corroborated the voltammetric interpretation and the proposed degradation pathway in the studied cell conditions. The outcomes of this work provide practical insight into coin-cell design and configuration strategies for developing Zn∥EMD batteries.

25 ENERGY STORAGE↗
DOE OSTI2023

Overcoming magnetic susceptibility broadening in NMR of coin cell batteries to achieve chemical resolution

We develop methods for previously introduced NMR hardware that enables sensitive, noninvasive spectroscopic study of coin cell batteries, by overcoming the magnetic field distortions intrinsic to the battery limited chemical resolution. Specifically, we employ an interferometric NMR technique to overcome field heterogeneity, reducing peak widths by two orders of magnitude and obtaining chemically resolved solution-state spectra.

25 ENERGY STORAGE↗
DOE OSTI2023

Evaluation of Cathode Materials with Lithium-Metal Anodes: Baseline Performance and Protocol Standardization of Coin Cells

The collaborative evaluation of electrode materials across multiple research entities requires standardized electrochemical testing protocols to produce reliable, one-to-one comparisons between different systems of interest. Similar to the work done by Long et al. on protocol standardization for coin-cell testing with graphite anodes [J. Electrochem. Soc., 163, A2999, (2016)], here we introduce two standardized testing protocols designed to quickly evaluate important electrochemical properties of cathode materials using lithium-metal anodes. The two protocols measure kinetic and thermodynamic capacity losses, rate- and voltage-dependent cycling capacities, instabilities at high voltage and high cycling rate, and overpotentials at various states of charge. We then apply these protocols to four commercially available cathode materials to establish benchmark performance metrics that can be used to screen and evaluate new cathode materials.

25 ENERGY STORAGE↗
DOE OSTI2022

Robust hierarchical three dimensional nickel cobalt tungstate-MXene nanocomposite for high performance symmetric coin cell supercapacitors

Design of rational electrode materials with hierarchically structured pseudocapacitive materials has been identified as a successful strategy for revamping the electrochemical characteristics of supercapacitors. However, the simultaneous assurance of strong electrical conductivity and higher specific capacitance via a simple and cost-effective synthesis protocol is of concern today. In this work, Ni-CoWO 4 incorporated MXene nanocomposite has been successfully prepared by a facile hydrothermal process. The structure, morphology, stoichiometry, and chemical characterization of the prepared Ni-CoWO 4 , Ti 3 C 2 T x , and Ni-CoWO4@MXene nanocomposite were explored extensively. MXene demonstrated a layered 2D nanoscale structure whereas pure Ni-CoWO 4 was composed of spherical nanoparticles. The composite Ni-CoWO 4 @MXene revealed the morphology of spherical Ni-CoWO 4 nanoparticles decorated on MXene sheets. Furthermore, a series of electrochemical characterizations illustrated the contribution of the delightful morphology of Ni-CoWO 4 @MXene composite to excellent electrochemistry. The resultant Ni-CoWO 4 @MXene electrode exhibited high specific capacitance of 582 Fg -1 at 1 A g -1 and 93.5 % capacitance retention over the 10,000 cycles., which is higher than that of the individual counterparts Ni-CoWO 4 and MXene. The excellent electrochemical performance of Ni-CoWO 4 @MXene is attributed to the synergistic interaction between Ni-CoWO4 nanoparticles and nanolayered MXene that may create new active sites that enhanced the charge transfer, charge/discharge kinetics and the electrical conductivity. Significantly, the unique Ni-CoWO 4 @MXene supercapacitor prototype delivered a higher energy density of 85.7 Wh kg -1 and power density of 0.85 kW kg -1 establishing its superiority over other Cosingle bondW based supercapacitors. A theoretical study was also performed to correlate the improved charge storage capacity of the prepared Ni-CoWO 4 @MXene composite.

25 ENERGY STORAGE↗
DOE OSTI2025

Neutron-Friendly Li-Ion Battery Coin Cell for In Situ 3D Visualization of Li Plating

Advanced battery characterization using in situ/operando neutron imaging is critical for uncovering degradation modes such as lithium (Li) plating in Li-ion batteries (LIBs). However, conventional LIBs hinder operando neutron radiography (NR) and in situ neutron micro-computed tomography (N-μCT) for visualizing Li plating near the graphite-separator interface due to strong attenuation from hydrogen-rich components like PP–PE–PP separators, electrolyte, and Fe-based spacers. In this work, we designed and tested a neutron-friendly battery (NFB) optimized for in situ Li detection during extreme fast charging (XFC). Guided by neutron attenuation cross-sections and material transmission, the NFB enables clear visualization at the graphite–separator interface, which is typically opaque in standard LIBs. Electrochemical tests show the NFB exhibits voltage/current responses like standard cells for up to 50 XFC cycles. However, its lower reversibility and capacity are likely due to Cu-coated Al spacer degradation from delamination or corrosion. We propose titanium spacers as a more stable alternative, albeit requiring custom machining. Using this optimized cell, we achieved simultaneous neutron tomography of multiple cells, capturing in situ 3D images of dead Li accumulation, particularly near graphite edges. These heterogeneous deposits and disconnected Li clusters suggest localized current density hotspots during XFC.

25 ENERGY STORAGE↗
DOE OSTI2020

SiO 2 Is Wasted Space in Single-Nanometer-Scale Silicon Nanoparticle-Based Composite Anodes for Li-Ion Electrochemical Energy Storage

The electrode processing conditions of silicon-based composite anodes play a pivotal role in the resulting interfacial chemical speciation and, thus, the electrochemical cycling behavior of the electrode. Systematically investigating how small chemical changes to the surface of the silicon nanoparticle (NP) affect larger, electrode-level properties is a strategy that will inform design principles to maximize electrode energy density and extend electrode lifetime. Here, we incorporate silicon nanoparticles (NPs) with an average diameter of 5.5 nm synthesized from the gas phase through a nonthermal plasma method into composite anode half-cell coin cells. We perform chemistry to functionalize the native hydride-terminated silicon NP surface with N-methylpyrrolidone (NMP) to improve slurry properties and reduce the silicon reactivity prior to composite electrode fabrication. We construct composite electrodes from these silicon NPs and observe an 86% capacity retention over 100 cycles at a rate of C/5, with an initial silicon specific capacity of 2600 mAh/g. We expose the same Si NPs to water that completely oxidizes these small-diameter NPs to SiO 2 and find that the SiO 2 NPs in the same electrode configuration exhibit no obvious lithium alloying capacity in the electrochemical potential range of lithium silicide alloy formation. As this result stands in contrast to existing literature, we provide a discussion on the origin of the discrepancies.

25 ENERGY STORAGE↗
DOE OSTI2025

Lower Cost Renewable Nanoparticle Platform to Increases Production of Cathode Material (CRADA Final Report)

Employees of Sylvatex synthesized candidate cathode materials for lithium-ion batteries in PI’s labs and at the Molecular Foundry using sustainable methods. They then benchmarked the synthesized materials against available commercial cathode materials in lithium half-cells (coin cell configurations) to compare performance and ensure that their materials met or exceeded metrics of the commercial materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Carbon Anode Material from Biomass Pyrolysis Oil

Lithium-ion batteries (LIB) are an important component of electric vehicles and sodium-ion batteries (SIB) are an attractive alternative for grid electric storage. We are investigating a novel approach to synthesizing the carbon anode materials for these batteries from biomass pyrolysis oil as part of conversion processes to produce biofuels. Graphite is used as anode material in LIB and is exclusively produced from petroleum residue or mined mineral carbon. We have synthesized drop-in graphite by coking the heavy residual oil from the distillation of catalytic fast pyrolysis oil and by catalytic graphitizing raw pyrolysis oil. XRD and Raman spectroscopies were used to verify the production of high purity crystalline graphite. Figure 1 shows typical XRD spectra of the bio-graphite compared to commercial material as well as the charge/discharge cycle. Graphite particle sizes and morphologies were adjusted to improve performance using jet milling and carbon coating. The bio-graphite delivered a high capacity (335 mAh/g) when tested in a graphite half-cell. Full cell coin cell experiments were also conducted to verify the observations from half-cell testing. The high value of graphite (>$9/kg) can positively impact the economics of biofuels production and can be an important part of a future circular carbon economy. We have also investigated synthesizing hard carbon from pyrolysis oil for use as anode material in SIB. These batteries are not commercially mature but have great promise in grid storage and use earth abundant elements. We have demonstrated that pyrolysis oil can be used to synthesize hard carbon, which was subsequently be used in SIB experiments. This material achieved a sodium-ion capacity of 250 mAh/g and a first cycle efficiency of 78%, with opportunities to further optimize this performance from optimizing the composition of the pyrolysis oil to shaping the hard carbon particles. As with graphite, hard carbon is a high value (> $10/kg) material that could facilitate biofuels production.

BIOMASS FUELS,INORGANIC, ORGANIC, PHYSICAL, AND AN↗
DOE OSTI2022

Probe for operando in situ electrochemical nuclear magnetic resonance spectroscopy

Electrochemical devices with metal casings have been considered incompatible with nuclear magnetic resonance (NMR) spectroscopy because the oscillating magnetic fields (“rf fields”) responsible for excitation and detection of NMR active nuclei do not penetrate metals. According to the present invention, rf fields can still efficiently penetrate into nonmetallic layers of electrochemical cells (such as a coin cell battery configuration) provided the magnetic field is oriented tangentially to the electrochemical cell electrodes in a “skimming” orientation. As an example, noninvasive high field in situ 7Li and 19F NMR of an unmodified commercial off-the-shelf rechargeable coin cell was demonstrated using a traditional external NMR coil setup. The in operando NMR measurements revealed that irreversible physical changes accumulate at the anode during electrochemical cycling.

Sorte, Eric Glenn↗
DOE OSTI2025

End of (3rd) Month Progress Report - PhD Committee

For the months of (May-August), the focus has been to: ● Comply and attend all mandatory LLNL training(s). ● Practice & gain experience, using a 3D printer for direct-ink writing application. ● Construct & Test Cu-Si anodes for battery application: - Si nanoparticles (<100 nm) is alloyed within a Cu-based current collector, via direct-ink writing. - Tuning the overall architecture of the current collector (to accommodate the volume expansion of Si more efficiently/ stabilize its kinetics - of active Si loss). - Based on the following designed configurations: tape-casted, 2D (spiral-square), and 3D (spiral-square/ zig-zag) structures; utilizing commercial-based Cu paste. - Fabricated (half-cell) coin-cells are currently cycling long-term. ● Synthesize new Cu-Si paste, to further tune the rheology properties, for further comparison with commercial Cu-based paste.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2025

Lithium Growth on Alloying Substrates and Effect on Volumetric Expansion

The widespread implementation of next-generation Li metal anodes is limited, in part, due to the formation of dendritic and/or mossy electrodeposits during cycling. These morphologies can lead to battery failure due to the formation of short circuits and significant volumetric expansion at the anode. One strategy to control the electrodeposition of Li metal is to use lithiophilic materials at the anode. Here, we evaluate the impact of Ag and Au on the early stages of Li metal electrodeposition and cycling. The alloying substrates decrease the voltage for Li reduction and improve Li wetting/adhesion. We probe volumetric expansion directly through dilatometry measurements and find that the degree of volumetric expansion is less when lithium is cycled on an alloying substrate compared to a non-alloying substrate (Cu). Dilatometry experiments reveal that Au has the least amount of volumetric expansion and coin cell cycling experiments indicate that Ag yields more stable cycling compared to Au or Cu. The evaluation of in situ cross-sectional images of cycled coin cells shows that Ag has the lowest volumetric expansion in a coin cell format.

alloys↗