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At least 55 records · Page 3

Voltage and temperature effects on low cobalt lithium-ion battery cathode degradation

Degradation of low cobalt lithium-ion cathodes was tested using a full factorial combination of upper cut-off voltage (4.0 V and 4.3 V vs. Li/Li + ) and operating temperature (25 °C and 60 °C). Half-cell batteries were analyzed with electrochemical and microstructural characterization methods. Electrochemical performance was assessed with galvanostatic cycling, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) supported by distribution of relaxation times (DRT) analysis. Electrode microstructure was characterized with scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray absorption near edge structure (XANES) imaging. Higher cut-off voltage cycling shows presence of NiO x formation, a low diffusivity rock-salt phase, in both CV and XRD data. XRD patterns confirmed that the rock-salt phase was beginning to form at the low cut-off voltage at high temperature, but in much lower intensity than at the high cut-off voltage. Higher temperature accelerates degradation processes at both voltages. Degradation factors at high temperature include NiO x formation, cathode material dissolution, and electrolyte decomposition. SEM analysis suggests that supporting phases may isolate and disconnect active material particles reducing capacity retention and battery life cycle. DRT analysis and XANES imaging show that both high temperature samples revealed a NiO x phase based on an increased diffusive impedance and a visible shift in the XANES spectra. The low cut-off voltage, high temperature sample showed a split peak and shift to lower energies indicating early formation of the NiO x phase. The diffusive impedance, which hinders intercalation and deintercalation, is driven by the formation of the NiO x phase. While primarily driven by cut-off voltage, elevated temperature also contributes to this degradation mechanism.

electrochemical impedance spectroscopy↗

Scalable mechanochemical synthesis of high-quality Prussian blue analogues for high-energy and durable potassium-ion batteries

Prussian blue analogues (PBAs) are recognized as promising cathode materials for potassium-ion batteries (PIBs), particularly the low-cost and high-energy K 2 Mn[Fe(CN) 6 ](KMnF). However, conventional solution-based synthesis inevitably introduces [Fe(CN) 6 ] 4− defects and lattice water while suffering low synthesis efficiency, unfavorable to the improvement of electrochemical performance and scalability. Here, in this work, we report a simple solvent-free mechanochemical strategy for the synthesis of a wide variety of K 2 M[Fe(CN) 6 ] (M = Mn, Mg, Ca, etc.) with negligible defects and water, and it is unprecedented to achieve kilogram-level products of high-quality KMnF within just 10 minutes. The as-prepared KMnF delivers a high energy density of 590 Wh kg −1 at 0.2 C and exhibits an astonishing stability over 10 000 cycles and rate ability up to 50 C in a potassium metal half-cell. Encouragingly, a high-areal-capacity pouch cell with 2.2 mAh cm −2 (16.5 mg cm −2 ) exhibits a capacity retention of 80.7% after 500 cycles. Furthermore, systematic in situ characterization reveals underlying mechanism insights into structure–performance relationships. Specifically, the fully coordinated Mn–N 6 octahedral configuration effectively suppresses Mn 3+ Jahn–Teller distortion, enabling reversible phase transitions under both high-voltage and long-term cycling conditions. In addition, minimal defects provide sufficient redox centers, while the continuous three-dimensional framework facilitates rapid K + diffusion kinetics. This work provides a new opportunity for the ultrafast, universal and scalable synthesis of high-quality PBAs, facilitating the practical application of PIBs while enabling precise structural and compositional design of novel PBAs.

Mechanochemical method↗

Understanding the Mn dissolution mechanism in rock salt-type Li 4 Mn 2 O 5 cathodes

For the first time, a detailed exploration of Mn dissolution in disordered rock salt (DRX) Li 4 Mn 2 O 5 is presented. Herein, we apply a suite of synchrotron and lab scale X-ray techniques to both the cathode and the separator harvested from pristine, charged, or cycled lithium half-cells containing the disordered rock salt (DRX) material Li 4 Mn 2 O 5 , in order to understand Mn dissolution processes throughout charging and discharging. Previous research has hypothesized two concurrent effects that may drive Mn dissolution in cells during cycling: acid-induced disproportionation of Jahn–Teller active Mn 3+ and structural rearrangement of the cathode lattice. Through depth probing of the Mn oxidation state in both the cathode and separator via soft X-ray absorption spectroscopy (XAS), hard XAS, and X-ray photoelectron spectroscopy (XPS) in progressive states-of-charge, as well as extended X-ray absorption fine structure (EXAFS) analysis of the local Mn environment, the primary driving force of Mn dissolution is determined to be high-voltage structural rearrangement above 4.2 V. Mn dissolution is, additionally, a main source of capacity fade in Li 4 Mn 2 O 5 DRX cells, which retain only 59% capacity after 20 cycles.

Theibault, Monica↗

In situ catalyst activation and regeneration enable energy-efficient high-current CO 2 reduction to ethanol-rich C 2+ mixtures

Electrochemical conversion of dissolved CO 2 in bicarbonate electrolytes, i.e., bicarbonate electrolysis, offers distinct advantages over gas diffusion electrode systems by enabling direct utilization of the CO 2 capture electrolyte while bypassing the energy-intensive CO 2 release step. However, bicarbonate electrolysis faces challenges such as CO 2 mass-transfer limitation, local pH-driven CO 2 depletion, and high cathodic potentials. The higher potential often causes catalyst surface reorganization, leading to a gradual loss of active sites and variations in selectivity during CO 2 reduction. Here, we report a directed, in situ activation and regeneration method that allows precatalysts to equilibrate under dynamic (pulsed) electrolysis conditions. We demonstrate in situ activation of a scalable Cu 2 O/Cu mesh that, under short-width (t = 4 s) pulsed electrolysis, provides stable mixed oxidation states of Cu, favoring the formation of an ethanol-rich crude mixture. The pulsed electrolysis waveform, consisting of six distinct segments, is tuned to form Cu + oxides, which are then reduced to generate local alkaline conditions favoring C–C coupling. This synergistic effect results in FEs of 73% for C2+ products and 39% for ethanol at an applied current density of −150 mA cm −2 and a cathodic potential of −1.45 V (vs. RHE). The overall half-cell energy efficiency is ∼30% for C 2+ products. The in situ Raman experiments confirm the role of pCO 2 R in dynamically regenerating Cu+-containing surface species during pulsed operation, thereby steering selectivity towards C 2+ products. A comprehensive multiscale, multiphysics model is developed to investigate the dynamic behavior of copper surface species (Cu, Cu + , and Cu 2+ ) and local microenvironmental conditions during the pCO 2 R. The results reveal that the coexistence of different copper oxidation states, especially the Cu+ intermediate, is critical in steering selectivity towards multicarbon (C 2+ ) products. The dynamic modulation of surface redox states via tailored pulsing strategies favors C–C coupling pathways by inducing localized alkaline conditions and stabilizing reactive intermediates. This work establishes a predictive modeling platform that links pulse waveform design with mechanistic insights into catalyst state evolution and product selectivity. Overall, this study provides valuable insights into the synergistic effect of in situ activation of pre-catalysts and pulsed electrolysis for higher selectivity towards C 2+ products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Role of microstructure on flux expulsion of superconducting radio frequency cavities

The trapped residual magnetic flux during the cool-down due to the incomplete Meissner state is a significant source of radio frequency losses in superconducting radio frequency cavities. Here, in this study, we clearly correlate the niobium microstructure in elliptical cavity geometry and flux expulsion behavior. In particular, a traditionally fabricated Nb cavity half-cell from an annealed poly-crystalline Nb sheet after an 800 °C heat treatment leads to a bi-modal microstructure that ties in with flux trapping and inefficient flux expulsion. This non-uniform microstructure is related to varying strain profiles along the cavity shape. A novel approach to prevent this non-uniform microstructure is presented by fabricating a 1.3 GHz single cell Nb cavity with a cold-worked sheet and subsequent heat treatment leading to better flux expulsion after 800 °C/3 h. Microstructural evolution by electron backscattered diffraction-orientation imaging microscopy on cavity cutouts, and flux pinning behavior by dc-magnetization on coupon samples confirms a reduction in flux pinning centers with increased heat treatment temperature. The heat treatment temperature-dependent mechanical properties and thermal conductivity are reported. The significant impact of cold work in this study demonstrates clear evidence for the importance of the microstructure required for high-performance superconducting cavities with reduced losses caused by magnetic flux trapping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Stabilizing Cathode–Electrolyte Interphase of Nickel-Rich Single-Crystal Cathodes for Lithium-Ion Batteries

Nickel-rich single-crystal (SC) layered oxides are promising cathode candidates for next-generation lithium-ion batteries (LIBs) owing to their high energy density and structural robustness against intergranular cracking. However, their intrinsic surface reactivity with liquid electrolytes accelerates parasitic reactions at the cathode–electrolyte interphase (CEI), leading to transition-metal dissolution, gas generation, and impedance buildup. In this work, we synthesized SC-Li x Ni 0.9 Mn 0.05 Co 0.05 O 2 (NMC9055, 1 ≤ x ≤ 1.2) using a eutectic-assisted method and investigated interface stabilization strategies. A nickel-deficient Li x Ni 0.6 Mn 0.2 Co 0.2 O 2 (NMC622, 1 ≤ x ≤ 1.2) coating was applied via evaporation-based deposition to suppress CEI degradation pathways. Structural and compositional analyses confirmed uniform shell formation and preserved particle integrity. Half-cell electrochemical testing against lithium metal revealed ∼10% higher capacity retention and improved reversibility compared with pristine SC NMC9055, particularly under high-voltage operation. In conclusion, these results highlight the critical role of controlled surface chemistry in mitigating CEI instability in nickel-rich SC cathodes, offering a pathway toward enabling durable high-energy LIBs.

Coating processes↗

Surfactant Effects in Porous Electrodes for Microemulsion Redox Flow Batteries

The effect of surfactant additives on electrochemical behavior in porous electrodes was investigated using vanadium redox flow battery half-cells and the dependence of volumetric kinetics and mass transport on electrolyte, surfactant, and electrode type was explored. Without surfactant added, carbon paper electrodes demonstrated greater kinetics and transport compared to carbon felt, for a given electrolyte. Additionally, posolyte kinetics are greater than negolyte kinetics by one to three orders of magnitude, depending on the electrode type. Addition of surfactant increased electrode wettability and possibly electrochemical surface area. However, this was accompanied by a decrease in volumetric mass transport, due to stronger electrolyte-electrode interactions. The presence of sodium dodecyl sulfate (SDS) influenced posolyte and negolyte kinetics differently. Kinetics showed a dependence on electrode type and surfactant. On carbon felt, volumetric kinetics decreased for both posolyte and negolyte with SDS addition. On carbon paper, SDS decreased volumetric kinetics for the posolyte but increased (>2X) kinetics for the negolyte! This kinetic enhancement depends on surfactant chemistry: cetyltrimethylammonium bromide, a cationic surfactant, failed to increase kinetics. Furthermore, SDS did not increase areal specific resistance. Furthermore, these findings show the superior performance of carbon paper compared to carbon felt and suggest SDS as a possible VRFB negolyte additive.

25 ENERGY STORAGE↗

Multiscale Modeling Framework for Lithium Nucleation in 3D Porous Carbon Anodes

Porous carbon scaffolds offer a promising route for mitigating non-uniform lithium (Li) plating to enhance the safety and longevity of Li metal batteries. However, the influence of microstructural morphology on Li nucleation is not well understood. Here, we present a multiscale modeling framework to investigate how the porous microstructure of carbon materials affects Li nucleation behavior. Ab initio molecular dynamics simulations quantify the nucleation energy barriers of Li on graphene as a function of Li content, surface curvature, and applied potential, providing key parameters for a classical nucleation theory (CNT) model. From macroscale half-cell simulations, we obtained Li concentration and electrical potential profiles to define boundary conditions for mesoscopic simulations. At the mesoscale, three distinct synthetic 3D microstructures with different porosities and characteristic feature sizes are generated to resolve local distributions of Li flux, current density, and mechanical stress. These outputs are integrated into the CNT model to map spatial variation in nucleation rates. Our findings reveal trade-offs between suppressing nucleation rates and achieving spatial uniformity, offering design guidelines for optimizing porous carbon anodes to balance nucleation control and mechanical integrity.

Materials science↗

Lithium-Ion Batteries with Lithium Manganese Iron Phosphate Cathodes and Lithium Titanate Anodes: Linking Electrode Dynamics to Cell Performance

This study examines the electrochemical performance, impedance behavior, and aging mechanisms of lithium-ion cells pairing lithium manganese iron phosphate (LiMn 0.6 Fe 0.4 PO 4 , LMFP64) cathodes with lithium titanate (Li 4 Ti 5 O 12 , LTO) anodes. LMFP64 half-cells display distinct Fe and Mn redox plateaus at ∼3.5 and ∼4.1 V, respectively, and deliver excellent rate capability. Three-electrode measurements show that LMFP64 dominates cell impedance, which changes sharply across the Fe–Mn redox transition and decreases with increasing temperature (30 °C–50 °C). Voltage hysteresis arises mainly from the cathode, with higher C-rates shortening redox plateaus and broadening the transition region. Elevated temperature lowers impedance, especially near the Mn-redox and transition regions, but accelerates capacity fade. Post-cycling analyses of electrodes confirm structural stability of LMFP64 and indicate loss of lithium inventory (LLI) as the source of capacity fade. This LLI causes potential slippage between the LMFP64 and LTO electrodes, which decreases the Fe-redox plateau width. Long-term cycling highlights the critical role of electrode overhang: cathode overhang mitigates capacity fade by buffering lithium loss, whereas anode overhang cells experience faster capacity decline due to uncompensated lithium depletion. These results clarify LMFP64/LTO battery impedance evolution, thermal effects, and degradation pathways and provide insights for their applications in electric vehicles.

Area Specific Impedance↗

Mathematical Modeling of the Potential and Time Dependence of Ir Dissolution from Hydrous Ir Oxide Oxygen Evolution Catalysts

One of the main degradation mechanisms of hydrous iridium oxide acidic oxygen evolution reaction (OER) catalysts is dissolution and loss into the acidic membrane. While degradation models have been proposed, there is a gap in understanding the potential and time dependence of the iridium dissolution reaction and its mechanistic underpinnings. In this work, Ir dissolution rates measured as a function of time and potential via time-resolved inductively-coupled plasma mass spectrometry (ICP-MS) in aqueous acidic electrolyte are used to establish a mathematical model for Ir dissolution. The mathematical model is generated using proposed formation and dissolution reactions for Ir species. Through comparison with the ICP-MS data and existing information on the potential-dependent Ir phase, we find that the potential and time-dependence of dissolution can be modeled as dissolution of an oxide phase, here represented as IrO 2 , with potential dependent kinetics and formation of a passivating species, a process with a rate-limiting step that is not potential dependent. This understanding of the potential dependence of dissolution and passivation kinetics using aqueous electrolyte half-cell measurements can be used to predict the degradation of Ir oxide in operating energy conversion devices relying on the OER, such as proton-exchange membrane water electrolyzers.

Kariuki, Nancy N. [Argonne National Laboratory (AN↗

RF AND MECHANICAL DESIGN OF A 915 MHz SRF CAVITY FOR CONDUCTION-COOLED CRYOMODULES

Conduction-cooled SRF niobium cavities are being developed for use in compact, continuous-wave electron linear accelerators for a variety of industrial applications. A 915MHz two-cell cavity has been designed to achieve an energy gain of 3.5 MeV. The design of the cell shape aims at minimizing the peak surface magnetic field. Field flatness is achieved by adjusting the length of the outer end half-cells. The higher-order mode analysis shows that absorbers are not required for a moderate beam current of 5 mA. One of the beam tubes has two side-ports for insertion of coaxial fundamental power couplers. The mechanical design and analysis were done to maintain a stress near or less than 15.5 MPa for all anticipated loading conditions. This is half the measured yield strength and is to provide relief from creep when cavity is evacuated and stored with outside atmospheric pressure.

Ciovati, Gianluigi↗

Unveiling the Interplay: Cold Work, Recrystallization, and Flux Expulsion in SRF Cavities

The fabrication of SRF cavities from sheet materials includes deep-drawing, electron beam welding, chemical and mechanical polishing, high-temperature heat treatment, and material diffusion. The performance of these cavities is frequently limited by magnetic flux trapping giving rise to additional rf loss. In this presentation, we thoroughly examine how recrystallization influences flux expulsion in SRF cavities, using cold-worked niobium sheets from various suppliers. Our findings reveal that cold-worked sheets enhance flux expulsion, especially at lower heat treatment temperatures, by promoting improved recrystallization. In particular, a traditionally fabricated Nb cavity half-cell from an annealed poly-crystalline Nb sheet after an 800 C heat treatment leads to a bi-modal microstructure that ties in with flux trapping and inefficient flux expulsion. This non-uniform microstructure is related to varying strain profiles along the cavity shape. A novel approach to prevent this non-uniform microstructure is presented by fabricating a 1.3 GHz single cell Nb cavities with a cold-worked sheet and subsequent heat treatment leading to better flux expulsion after 800 C/3h

Dhakal, P. [Old Dominion Univ., Norfolk, VA (Unite↗

RF and Mechanical Design of a 915 MHz SRF Cavity for Conduction-Cooled Cryomodules

Conduction-cooled SRF niobium cavities are being developed for use in compact, continuous-wave electron linear accelerators for a variety of industrial applications. A 915 MHz two-cell cavity has been designed to achieve an energy gain of 3.5 MeV. The design of the cell shape aims at minimizing the peak surface magnetic field. Field flatness is achieved by adjusting the length of the outer end half-cells. The higher-order mode analysis shows that absorbers are not required for a moderate beam current of 5 mA. One of the beam tubes has two side-ports for insertion of coaxial fundamental power couplers. The mechanical design and analysis were done to maintain a stress near or less than 15.5 MPa for all anticipated loading conditions. This is half the measured yield strength and is to provide relief from creep when cavity is evacuated and stored with outside atmospheric pressure.

Ciovati, Gianluigi↗

Advanced Processing of Coal and Coal Waste to Produce Graphite for Fast-Charging Lithium-Ion Battery Anode

The University of North Dakota (UND) Energy & Environmental Research Center (EERC), in collaboration with the UND Center for Process Engineering Research (CPER), conducted a project to validate two technologies capable of converting North Dakota lignite and lignite coal waste to high-quality graphite for fast-charging lithium-ion battery (LIB) anode. The project was conducted over about 3 years from April 7, 2022, to July 6, 2025. The two technological paths pursued in this project include path A – direct conversion of coal or coal waste to graphite by the upgraded carbon ores to products (UCOP) process being developed at the EERC and path B – lignite-derived coal tar pitch (CTP) conversion to graphite (CTP2G) process being developed at CPER. The results from this project validate the two technological approaches and are expected to be an integral part of a portfolio of emerging technologies for making high-quality graphite not only from North Dakota lignite, but from all ranks of U.S. domestic coal and coal waste resources. The quality of the graphite produced by these technologies is high enough for various applications, including batteries for the fast-growing electric vehicle industry, energy storage applications, electric arc furnace electrodes for steel production, and graphene production, among others. Although the two technologies can produce high-quality graphite, they are fundamentally different in that the UCOP technology provides a direct path to transform coal to graphite, while the CTP2G technology needs to go through a CTP intermediate and a coking process for the intermediate, which requires a special facility to accomplish. For application in the industry, the UCOP process is designed to be more flexible, with feedstock to include potentially any carbonaceous material such as all coal ranks and biochar, while the CTP2G process is designed to utilize CTP as the starting precursor. The key project accomplishments include the following: • Successful preparation of high-quality synthetic graphite from North Dakota lignite coal/coal wastes and lignite-derived CTP. • Patent application has been filed for the UCOP process and an internal invention disclosure has been filed for the CTP2G process. • The produced graphite performs better than a commercial battery-grade sample in LIB coin cells, especially fast-charging capability, stability, and long-duration cycling. • Coin-type Li-ion half-cells with CTP2G graphite showed excellent performance, with >370 mAh/g capacity, >90% initial coulombic efficiency, and 93%/67% retention at 1C/2C rate, which outperforms commercial graphite in charging speed, stability, and cycling. • Results of fabricated 18650 cells were consistent with the observations in coin cells. • Preliminary techno-economic analysis (TEA) estimates for the UCOP technology indicate a manufacturing cost of about $\$$39/kg based on 50-metric ton/year capacity. • Preliminary TEA estimates for the CTP2G technology indicate a market price of about $\$$7107/ton ($\$$7/kg) based on 22,000-ton/year production capacity.

01 COAL, LIGNITE, AND PEAT↗

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↗

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↗

Advanced Manufacturing of Cathode Materials for Lithium-ion Batteries

Original objectives (per the Statement of Project Objectives) centered on developing and translating a continuous pilot process for cathode materials production while targeting (i) a 29% manufacturing cost reduction, (ii) an 82% energy consumption reduction for cathode production, and (iii) a doubling of manufacturing productivity. Planned validation included characterization at appropriate analytical facilities and electrochemical performance evaluation progressing from half-cells to pouch-cell formats, with a pathway to kilogram-scale production of finished cathode materials for representative testing. Scope evolution: During execution, the project team identified that the surfactant-enabled chemistry offered high selectivity for lithium precipitation from brine sources. A formal scope revision shifted the final project year from cathode manufacturing development to direct lithium extraction/lithium recovery, while maintaining the overarching intent of cost reduction and process simplification relevant to the battery supply chain.

25 ENERGY STORAGE↗

Battery Material Synthesis and Scalability using a 50L Taylor Vortex Reactor (Final CRADA Report)

Under this agreement, Laminar will loan Argonne a 50L Taylor Vortex Reactor (TVR) and provide mechanical troubleshooting guidance and consulting to ensure the successful setup of the pilot-scale synthesis process. The U.S. Department of Energy (DOE) will allocate funding for the labor and materials required for the study. To evaluate the physical and electrochemical properties of the materials produced by the 50L TVR, Argonne will perform comprehensive characterizations, including XRD, SEM, PSA, ICP, tap density, and coin half-cell testing. Throughout the collaboration, Argonne will provide feedback and recommendations for mechanical improvements to the reactor system. Furthermore, Argonne will credit Laminar as a collaborator in any presentations or publications resulting from data generated by the system. Laminar will retain no rights to experimental results or intellectual property generated through the experiments conducted with the 50L TVR at Argonne.

25 ENERGY STORAGE↗