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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Metallicity, Atomic Disorder, and Li-Ion Storage in Fast-Charging Anodes

Oxides of Nb with Wadsley-Roth shear structures comprise a family of stable, high-rate anode materials for Li-ion batteries. A particular pair of them offers the unusual opportunity to test how important metallic conduction of the starting electrode is for electrode performance. The selected pair of compounds with similar 4 × 3 Wadsley-Roth block structures are insulating Ti 2 Nb 10 O 29 and metallic Nb 12 O 29 . A combination of diffraction, electrochemistry, magnetic measurements, and entropic potential measurements is employed to establish key findings for these two anode materials. We find that starting with a metallic oxide is not especially advantageous over a comparable material that readily transitions into a metallic state upon lithiation. Second, the rate performance appears to be dictated by ion mobility, and atomic Ti/Nb disorder in Ti 2 Nb 10 O 29 contributes to improved capacity retention at high rates by suppressing Li-ion ordering. However, subtle details in the nature of redox processes make Nb 12 O 29 a slightly better electrode material for long-term cycling at slower rates.

crystal structure↗
DOE OSTI2025

Operando neutron imaging-guided gradient design of Li-ion solid conductor for high-mass-loading cathodes

High-mass-loading cathodes are crucial for achieving high energy density in all-solid-state batteries from the lab scale to industry. However, as mass-loading increases, electrochemical performance is significantly compromised due to sluggish kinetics. In this work, operando neutron imaging is deployed on a high-mass-loading NMC 811 cathode of 33 mg/cm 2 (5.0 mAh/cm 2 ) and directly visualizes the lithiation prioritization of the cathode active material (CAM) from the solid electrolyte membrane side to the current collector side. In addition to the tortuosity, another key limitation on ion transfer in the cathode arises from the mismatch between the uniform distribution of the solid electrolyte (catholyte) in the conventional composite cathode and the non-uniform Li + flux generated by the faradaic reaction of CAMs. Therefore, we engineer a gradient in the catholyte concentration to match the Li + flux distribution as a means of eliminating the ion transfer obstacle. This approach demonstrates enhanced rate performance, even with high-mass-loading cathodes. A LiCoO 2 composite cathode with 100 mg/cm 2 high-mass-loading exhibits an areal capacity of 10.4 mAh/cm 2 at a current density of 2.25 mA/cm 2 . This work provides insight into the ion-transport limitation in thick cathodes and demonstrates an effective gradient design to overcome the kinetic barrier and achieve high battery performance.

Batteries↗
DOE OSTI2025

Unusual Li 2 O sublimation promotes single-crystal growth and sintering

Li 2 O is rarely used for cathode material synthesis due to its high melting point (1,438 °C). Here we discover that Li 2 O can sublimate at 800-1,000 °C under ambient pressure, opening new possibilities for cathode synthesis. We propose a mechanism that enables synthesis of single crystals-such as LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) or LiNi 0.9 Mn 0.05 Co 0.05 O 2 (NMC90)-without direct contact with Li 2 O salts. We show that Li 2 O vapour successfully converts spent polycrystalline NMC811 into segregated single crystals without milling or post-treatment. The Li 2 O vapour, derived from Li 2 O solids, diffuses rapidly and reacts with precursors, mimicking a molten-salt environment, which facilitates single-crystal growth. The chemical lithiation process continuously drives Li 2 O sublimation, sintering the crystals. Single crystals derived from Li 2 O and fresh precursors or spent polycrystals exhibit outstanding cycling after 1,000 cycles in full cells. The demonstrated Li 2 O sublimation and its universal role in promoting single-crystal growth provides an effective approach for single-crystal synthesis, scale-up and recycling.

25 ENERGY STORAGE↗
DOE OSTI2025

A formal Fe III/V redox couple in an intercalation electrode

Iron redox cycling between low-valent oxidation states of Fe II and Fe III drives crucial processes in nature. The Fe II/III redox couple charge compensates the cycling of lithium iron phosphate, a positive electrode (cathode) for lithium-ion batteries. High-valent iron redox couples, involving formal oxidation higher than Fe III , could deliver higher electrochemical potentials and energy densities. However, because of the instability of high-valent Fe electrodes, they have proven difficult to probe and exploit in intercalation systems. Here, in this study, we report and characterize a formal Fe III/V redox couple by revisiting the charge compensation mechanism of (de)lithiation in Li 4 FeSbO 6 . Valence-sensitive experimental and computational core-level spectroscopy reveal a direct transition from Fe III (3d 5 ) to a negative-charge-transfer FeV (3d 5 L 2 ) ground state on delithiation, without forming Fe IV , or oxygen dimers. We identify that the cation ordering in Li 4 FeSbO 6 drives a templated phase transition to stabilize the unique Fe V species and demonstrate that disrupting cation ordering suppresses the Fe III/V redox couple. Exhibiting resistance to calendar aging, high operating potential and low voltage hysteresis, the Fe III/V redox couple in Li 4 FeSbO 6 provides a framework for developing sustainable, Fe-based intercalation cathodes for high-voltage applications.

Ramachandran, Hari [Stanford Univ., CA (United Sta↗
DOE OSTI2024

Earth-abundant Li-ion cathode materials with nanoengineered microstructures

Manganese-based materials have tremendous potential to become the next-generation lithium-ion cathode as they are Earth abundant, low cost and stable. Here we show how the mobility of manganese cations can be used to obtain a unique nanosized microstructure in large-particle-sized cathode materials with enhanced electrochemical properties. By combining atomic-resolution scanning transmission electron microscopy, four-dimensional scanning electron nanodiffraction and in situ X-ray diffraction, we show that when a partially delithiated, high-manganese-content, disordered rocksalt cathode is slightly heated, it forms a nanomosaic of partially ordered spinel domains of 3–7 nm in size, which impinge on each other at antiphase boundaries. The short coherence length of these domains removes the detrimental two-phase lithiation reaction present near 3 V in a regular spinel and turns it into a solid solution. This nanodomain structure enables good rate performance and delivers 200 mAh g –1 discharge capacity in a (partially) disordered material with an average primary particle size of ~5 µm. The work not only expands the synthesis strategies available for developing high-performance Earth-abundant manganese-based cathodes but also offers structural insights into the ability to nanoengineer spinel-like phases.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Exploring a new synthesis route to lithium-excess disordered rock salt (DRX) cathode materials

Lithium-excess disordered rock salt (DRX) materials are promising candidates for Co/Ni-free Li-ion cathodes due to their high specific energy (800+ W h kg −1 ) and compositional flexibility. DRX cathodes are typically synthesized using solid-state reactions, which are difficult to scale and provide little-to-no control over particle morphology. Here, to address this bottleneck, the present study reports a two-step, solution-based reaction route to prepare Mn/Ti-based DRX oxyfluoride cathodes with nominal compositions of Li 1.25 Mn 0.5 Ti 0.3 O 1.95 F 0.05 and Li 1.35 Mn 0.7 Ti 0.1 O 1.85 F 0.15 . More specifically, a glycine–nitrate combustion reaction is used to produce a lithiated transition metal oxide, which is further reacted with LiF to produce high-purity DRX powders. Remarkably, this route yields 80–90% pure DRX after annealing for 1 h at 800–1000 °C, and 19 F solid-state nuclear magnetic resonance (ssNMR) spectra demonstrate that F− anions are successfully incorporated into the DRX structure. Cathodes prepared using this approach exhibit promising electrochemical performance, with Li 1.35 Mn 0.7 Ti 0.1 O 1.85 F 0.15 attaining reversible capacities ∼210 mA h g −1 and moderate cycling stability in half cells (65% capacity retention over 150 cycles). Overall, these results demonstrate that utilizing novel metal oxide precursors presents a viable and largely unexplored method to produce high-performance Co/Ni-free DRX cathodes.

25 ENERGY STORAGE↗
DOE OSTI2026

Solid-state prealkylation of electrode architectures to tune solid electrolyte interphase composition

Efficient electrochemical cycling of certain Si anodes is limited by irreversible Li consumption to form and continually reform the solid electrolyte interface (SEI) due to Si expansion/contraction and fracture. Prelithiation can compensate for these losses; however, the starting open circuit potential (VOC) becomes highly reducing and, therefore, the electrolyte reduction chemistry that influences the SEI composition can change. Herein, we compare SEI formation for electrodes prelithiated using Solid State Prealkylation of Electrode Architectures (SPEAR) versus traditional electrochemically lithiated architectures (ECLAR), focusing on SEI compositional changes as a function of stoichiometry (0.28 ≤ x ≤ 1.38 in LixSi). Increasing SPEAR prelithiation decreased the initial VOC of Si anodes vs. Li/Li+ from ∼3 V (Li0.28Si) to < 0.5 V for Li1.38Si, enabling simultaneous competitive reduction of EC, EMC, and LiPF6 at low potentials. Ex situ7Li and 29Si cross-polarization NMR and XPS reveal that SPEAR drives thicker SEI formation with substantially increased P/F contributions and a predominantly inorganic insoluble SEI (71.4% inorganic for Li1.38Si), consistent with accelerated LiPF6-derived POx/LiPFx/LiF formation relative to ECLAR analogs which exhibit carbonate-rich organic SEI compositions. Symmetric-cell EIS further indicates SPEAR-specific impedance features consistent with pore reduction (filling) during LixSi formation. In full cells, SPEAR prelithiation increases the initial coulombic efficiency (ICE) and accelerates SEI formation and stabilization with Li1.38Si reaching 99.4% coulombic efficiency (CE) by cycle 2.

Musgrove, Amanda [ORNL] (ORCID:0009000220910389)↗
DOE OSTI2024

Simulating hindered grain boundary diffusion using the smoothed boundary method

Abstract Grain boundaries can greatly affect the transport properties of polycrystalline materials, particularly when the grain size approaches the nanoscale. While grain boundaries often enhance diffusion by providing a fast pathway for chemical transport, some material systems, such as those of solid oxide fuel cells and battery cathode particles, exhibit the opposite behavior, where grain boundaries act to hinder diffusion. To facilitate the study of systems with hindered grain boundary diffusion, we propose a model that utilizes the smoothed boundary method to simulate the dynamic concentration evolution in polycrystalline systems. The model employs domain parameters with diffuse interfaces to describe the grains, thereby enabling solutions with explicit consideration of their complex geometries. The intrinsic error arising from the diffuse interface approach employed in our proposed model is explored by comparing the results against a sharp interface model for a variety of parameter sets. Finally, two case studies are considered to demonstrate potential applications of the model. First, a nanocrystalline yttria-stabilized zirconia solid oxide fuel cell system is investigated, and the effective diffusivities are extracted from the simulation results and are compared to the values obtained through mean-field approximations. Second, the concentration evolution during lithiation of a polycrystalline battery cathode particle is simulated to demonstrate the method’s capability.

Materials Science↗
DOE OSTI2024

Stability and transport of gyrokinetic critical pedestals

Abstract A gyrokinetic threshold model for pedestal width–height scaling prediction is applied to multiple devices. A shaping and aspect ratio scan is performed on National Spherical Torus Experiment (NSTX) equilibria, finding Δ ped = 0.92 A 1.04 κ − 1.24 0.38 δ β θ , ped 1.05 for the wide-pedestal branch with pedestal width Δ ped , aspect ratio A , elongation κ , triangularity δ , and normalized pedestal height β θ , ped . The width–transport scaling is found to vary significantly if the pedestal height is varied either with a fixed density or fixed temperature, showing how fueling and heating sources affect the pedestal density and temperature profiles for the kinetic-ballooning-mode (KBM) limited profiles. For an NSTX equilibrium, at fixed density, the wide branch is Δ ped = 0.028 ( q e / Γ e − 1.7 ) 1.5 ∼ η e 1.5 and at fixed temperature Δ ped = 0.31 ( q e / Γ e − 4.7 ) 0.85 ∼ η e 0.85 , where q e and Γ e are turbulent electron heat and particle fluxes and η e = ∇ ln ⁡ T e / ∇ ln ⁡ n e for an electron temperature T e and density n e . Pedestals close to the KBM limit are shown to have modified turbulent transport coefficients compared to the strongly driven KBMs. The role of flow shear is studied as a width–height scaling constraint and pedestal saturation mechanism for a standard and lithiated wide pedestal discharge. Finally, the stability, transport, and flow shear constraints are combined and examined for an NSTX experiment.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Unlocking iron metal as a cathode for sustainable Li-ion batteries by an anion solid solution

Traditional cathode chemistry of Li-ion batteries relies on the transport of Li-ions within the solid structures, with the transition metal ions and anions acting as the static components. Here, we demonstrate that a solid solution of F – and PO 4 3– facilitates the reversible conversion of a fine mixture of iron powder, LiF, and Li 3 PO 4 into iron salts. Notably, in its fully lithiated state, we use commercial iron metal powder in this cathode, departing from electrodes that begin with iron salts, such as FeF 3 . Our results show that Fe-cations and anions of F – and PO 4 3– act as charge carriers in addition to Li-ions during the conversion from iron metal to a solid solution of iron salts. This composite electrode delivers a reversible capacity of up to 368 mAh/g and a specific energy of 940 Wh/kg. Our study underscores the potential of amorphous composites comprising lithium salts as high-energy battery electrodes.

25 ENERGY STORAGE↗
DOE OSTI2024

Understanding and Enhancing Silicon Nanoparticle Distribution during Electrode Processing

Silicon-dominant anodes are of great interest because of their potential to boost the cell-level energy of state-of-the-art Li-ion batteries. While silicon materials have been extensively studied, understanding interactions at the electrode level has recieved little attention, especially the coating process of Si particles, which plays an equally important role in unlocking the full potential of silicon anodes. Herein, the electrode processing of a Si-dominated anode (52.8 wt%, 3.5–4.5 mAh cm −2 ) is being investigated to understand the relationship of processing on the morphology and properties of Si anodes at the electrode level. It has been found that almost-undetectable Si agglomerates easily form during electrode processing, which grow into largeprotrusions after lithiation and trigger potential internal shorting and self-discharge problems. A facile slurry filtration step is proposed to homogenize the particle distribution within Si-dominant electrodes which improves the electrochemical performance and storage stability of Si-based Li ion batteries.

Wu, Bingbin↗
DOE OSTI2024

Quantifying the Temperature Dependence of the Multi-Species, Multi-Reaction Model: Part II. Estimation of Entropy Coefficient for Meso-Carbon Micro-Bead Graphite

In Part 1 of this paper, the temperature impact on the Multi-Species, Multi Reaction (MSMR) model was studied. This was accomplished by acquiring data from slow rate lithiation and delithiation of a meso-carbon micro-bead (MCMB) graphite. Through this analysis, the temperature impact on the total fraction of available host sites in a particular MSMR gallery (X j ), the impact on the reference potential (U$^o_j$), and the impact on the parameter detailing the deviation from Nernstian behavior (ω j ) was determined. Here, the intercalation material is discussed, compared to traditional methods of acquiring the entropy coefficient, and comparison is made to previous mathematical estimates. Some of the challenges in using temperature dependent constant rate charge and discharge data as compared to the potentiodynamic entropy coefficient calculation method are also discussed, and a recommendation for future applications is proposed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Modeling Reversible Volume Change in Automotive Battery Cells with Porous Silicon Oxide-Graphite Composite Anodes

Automotive battery manufacturers are working to improve the individual cell and overall pack design by increasing durability, performance, and range, while reducing cost, and active material volume change is a key aspect that needs to be considered during this design process. Recently, silicon oxide-graphite composite anodes are being explored to increase total anode capacity while maintaining a tolerable amount of cell level reversible volume expansion due to the relatively lower reversible volume change of the silicon oxide compared to pure battery grade or metallurgical grade silicon. To predict the blended anode response and contribution to the overall cell volume change, we integrated the mechanical behavior of the individual active materials with the multi-species, multi-reaction model to predict the state-of-lithiation of the active materials in the cell at a given potential. The resulting simulations illustrate the tradeoff in volume change between the silicon oxide and the graphite during cell operation. This type of modeling approach will allow designers to virtually consider the impact of cell level and pack level design changes on overall system mechanical performance for automotive and grid storage applications, namely that relatively small addition of silicon containing materials can drive a significant increase in the volume change at the cell level, as demonstrated by the 5 wt% addition of silicon oxide accounting for half of the overall volume change in the cell.

Garrick, Taylor R. (ORCID:0000000322518129)↗
DOE OSTI2024

Bipolar Membrane Capacitive Deionization for the Selective Capture of Lithium Ions from Brines and Conversion to Lithium Hydroxide

Meeting the increasing demand for lithium in vehicle electrification and renewable energy storage requires innovations in lithium-ion (Li + ) separations. Traditional solar evaporation methods for lithium recovery are slow and consume tremendous volumes of water and secondary chemicals (acids and bases). This study introduces a bipolar membrane capacitive deionization (BPM-CDI) unit for direct lithium extraction and LiOH production without the external addition of acids and bases. Utilizing de-lithiated lithium-iron-phosphate (LFP) coated carbon cloth electrodes, the BPM-CDI unit demonstrates selective Li + capture over competing ions. Molecular dynamics simulations and H-cell experiments elucidate pH inversion mechanisms during Li + release, yielding LiOH. The BPM-CDI platform efficiently removes Li + from synthetic brines featuring 8x higher Mg 2+ concentrations (200 ppm Mg 2+ ) and 26x higher Na + concentrations (682 ppm Na + ), achieving a LiOH concentration of 124 ppm (36 ppm Li + ) after 8 cycles of recirculation. Post-mortem analysis confirms electrode integrity and stability. BPM-CDI integrated with selective electrodes is a promising electrochemical separation-reactor platform for lithium recovery while producing LiOH.

Kulkarni, Tanmay↗
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 OSTI2024

Quantifying the Temperature Dependence of the Multi-Species, Multi-Reaction Model. Part 1: Parameterization for a Meso-Carbon Micro-Bead Graphite

In this work, the temperature impact on the Multi-Species, Multi-Reaction (MSMR) model is studied. This is accomplished by acquiring data from slow rate lithiation and delithiation of a meso-carbon micro-bead (MCMB) graphite. The MSMR model is used to simulate linear-sweep voltammetry data of a porous electrode composed of graphite, and because the electrode is close to a state of dynamic equilibrium, the peaks in the differential voltage spectroscopy plot can be analyzed. Through this analysis, the temperature impact on the total fraction of available host sites in a particular MSMR gallery (X j ), the impact on the reference potential (U° j ), and the impact on the parameter detailing the deviation from Nernstian behavior ( ω j ) can be found. This is the first time the temperature dependence of the MSMR parameters have been experimentally analyzed. In Part 2, the impact of the temperature dependence of the MSMR parameters on the entropy coefficient of an intercalation material will be studied.

Paul, Abigail (ORCID:0000000172892069)↗
DOE OSTI2024

Electrolyte and Cutoff Potential Effects on Cycle Life of Li4Ti5O12/LiNi0.9Mn0.1O2 Batteries for Behind-the-Meter Storage Applications

Behind-the-Meter Storage (BTMS) is a stationary battery energy storage system that is connected to the electrical distribution system on the customer's side of the utility's service meter. BTMS systems are used to store electrical energy from the grid as well as inconstant, renewable energy, such as local solar and wind generation. A successful BTMS system will allow the customer to pair their energy generation and storage to optimize electrical consumption from the grid, improving reliability and minimizing cost. For BTMS applications, batteries must be designed and optimized with different set of criteria from other leading segments of the Li-ion battery market, like transportation, due the system being stationary and proximal to the residential or commercial building it's benefitting. BTMS applications prioritize safety, cost (low/no-critical materials), reliability (20-year calendar life), and durability (10,000 cycle life), while having the ability to (minimally) compromise energy density and rate capability. Lithium titanate (Li4Ti5O12-, LTO) is a promising anode candidate for BTMS applications due to its high safety and capacity retention, while maintaining a reasonable 160 mAhg-1 reversable capacity and composition of relatively abundant materials. (1) Specifically, LTO has a high working voltage which helps to prevent Li dendrite formation, improving safety. Furthermore, LTO also has negligible lithiation-based volume change, leading to less mechanical pulverization, or loss of active material, upon cycling. For the cathode, materials with little or no Co are of high interest due to the high cost and low abundance of Co. LiMn2O4 (LMO) has been paired with LTO for BTMS applications in the past due to its safety, low cost (abundancy), and reasonably high operating voltage. (2-4) However, the low capacity of LMO limits energy density and specific energy. While not the highest priority for BTMS applications, increasing energy density will enable deployment in space constrained BTMS applications and decrease total cost. LiNi0.9Mn0.1O2 (LN-MO) is a recently developed material with promise due to its high operating voltage and relatively low price. (5) However, Ni-rich layered oxides, including LNMO, tend to struggle with capacity retention during high-voltage cycling due to mechanical pulverization, irreversible phase transitions, and unstable solid-electrolyte interphase. The study presented here focuses on building an understanding of how electrolyte solvent and varied cutoff potentials will impact the cycle life of LTO/LN-MO cells. Specifically, a comparison is provided between ethylene carbonate (EC), ethyl methyl carbonate (EMC), fluoroethylene carbonate (FEC), and Gen2 electrolyte solvents with 1M Lithium hexafluorophosphate (LiPF6) salt, cycling to two upper termination potentials, 2.6V and 2.7V. Electrochemical testing and diagnostics (e.g., differential capacity analysis, area specific impedance, constant voltage hold, and rate capability) and post-mortem characterization will be used to understand the aging behavior and failure mechanisms of the 8 cell combinations (four electrolytes and two voltage cutoffs). Cells with FEC electrolyte showed a lower initial capacity compared to cells with Gen2, EMC, and EC cycling at both voltages; however, the cells with FEC showed consistent trends in capacity retention with 2.6V and 2.7V termination potentials, while the cells with the other electrolytes showed much higher rates of capacity loss when cycling to the higher voltage. These results indicate that FEC may play a role in improving durability of high-voltage, Ni-rich electrode systems for use in high-cycle applications, such as BTMS.

electrolyte↗
DOE OSTI2025

The Solid Electrolyte Interphase Dispersion Can Predict Cycle and Calendar Lifetimes in Silicon Anodes for Lithium-Ion Batteries

The solid electrolyte interphase (SEI) plays a critical role in lithium-ion battery (LIB) anodes. It is responsible for passivating the reactive surface of lithiated anodes against degradation of the electrolyte which enables long cycle and calendar lifetimes for LIBs. This role is especially important in high energy density anodes like silicon, that undergo massive volumetric changes during electrochemical cycling. The mechanism by which the SEI performs this role, however, is not clear which makes designing an SEI to passivate silicon anodes impossible. Through decades of research, dozens of chemical species have been identified within the SEI ranging from inorganic solids to polymeric coatings all of which simultaneously exist in a 'mosaic' composition at the anode surface. This mosaic creates a highly dispersive environment in which electrostatic screening of the anode surface from the electrolyte is not always complete. Here, we present an electrochemical technique to directly test the dispersion at the anode surface. We use this technique to screen more than 20 different electrolytes against silicon anodes and find correlations between both the cycle life and calendar life. The insights from this study offer a new framework to think about the SEI and a rapid screening method to test novel electrode/electrolyte combinations.

battery↗