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At least 523 records · Page 29

Roles of Mn and Co in the Air Synthesizability of Layered Oxide Cathodes for Lithium-Based Batteries

High-nickel layered oxides (LiNi 1-x-y Mn x Co y O 2 ) are the prevailing cathode materials for high-energy-density lithium-based batteries, but they are plagued with deleterious surface air instabilities stemming from residual lithium formation. These issues severely hinder mass production as cathode calcination is limited to a flowing oxygen atmosphere, which entails high manufacturing costs as opposed to simpler and more economical air calcination. Here, while higher Ni contents are known to worsen air instabilities, the influence of Mn and Co contents on impacting these phenomena are less elucidated. We herein present the synthesis in ambient air and flowing oxygen atmospheres of three cathode variants with the same Ni contents, but varying Mn and Co contents: LiNi 0.7 Mn 0.3 O 2 , LiNi 0.7 Mn 0.15 Co 0.15 O 2 , and LiNi 0.7 Co 0.3 O 2 . It is found that the critical parameter influencing the air stability of the cathodes is the average Ni oxidation state, which is greatly dependent on the Mn and Co contents. Substitution of Mn for Ni drives down the Ni oxidation state as Mn exists as Mn4 + and reduces surface residual lithium formation, which vastly improves the overall air stability and, therefore, the synthesizability in air, but with a penalty of lowered capacity. In contrast, substitution of Co for Ni maintains Ni 3+ as Co exists as Co 3+ , offering increased initial capacity, but worsens the air stability and cyclability as the driving force for residual lithium formation and surface reactivity is increased.

25 ENERGY STORAGE↗

Redox Behaviors in Li-Excess Cation-Disordered Mn-Nb-O-F Rocksalt Cathode

Lithium-excess cation-disordered rocksalt oxide (DRX) is a new choice of high energy Li-ion cathode materials. DRX cathode can deliver an exceptionally high capacity of >250 mAh/g, implying the participation of cationic transition metal and anionic oxygen redox in the electrochemistry. Understanding the explicit roles of both redox reactions in the newly developed cathode is of critical importance to further development of these materials. Herein, we synthesize a representative Mn-redox-based fluorinated DRX material, Li1.2Mn0.625Nb0.175O1.95F0.05 (LMNOF). Using a comprehensive suite of electroanalytical methods, we probe the cationic and anionic redox processes and their evolution upon cycling exclusively from the electrochemical point of view. This work sheds light on understanding of cationic and anionic redox and their roles in the capacity loss for high-capacity fluorinated DRX cathode, meanwhile, showcases an explicit approach to study the electrochemistry of novel electrode materials using such non-disruptive electroanalytical methods.

Li-ion battery, high-capacity cathode, Li-excess m↗

Porosity Development at Li-Rich Layered Cathodes in All-Solid-State Battery during In Situ Delithiation

Structural evolutions are crucial for determining the performance of high-voltage lithium, manganese-rich layered cathodes. Moreover, interface between electrode and electrolyte plays a critical role in governing ionic transfer in all-solid-state batteries. In this work, we unveil two different types of porous structure in Li 1.2 Ni 0.2 Mn 0.6 O 2 cathode with LiPON solid-state electrolyte. Na-nopores are found near the cathode/electrolyte interface at pristine state, where cation mixing, phase transformation, oxygen loss and Mn reduction are also found. In situ Li + extraction induces the evolution of nanovoids, initially formed near the inter-face then propagated into the bulk. Despite the development of nanovoids, layered structure is conserved, suggesting the nature of nanopores and nanovoids are different and their impact would be divergent. This work demonstrates the intrinsic interfacial layer, as well as the dynamic scenario of nanovoid formation inside high-capacity layered cathode, which help understanding the performance fading in cathodes and offer insights into the all-solid-state battery design.

25 ENERGY STORAGE↗

Structural and Electrochemical Impacts of Mg/Mn Dual Dopants on the LiNiO 2 Cathode in Li-Metal Batteries

Doping chemistry has been regarded as an efficient strategy to overcome some fundamental challenges facing the “no-cobalt” LiNiO 2 cathode materials. By utilizing the doping chemistry, we evaluate the battery performance and structural/chemical reversibility of a new no-cobalt cathode material (Mg/Mn-LiNiO 2 ). The unique dual dopants drive Mg and Mn to occupy the Li site and Ni site, respectively. We report the Mg/Mn-LiNiO 2 cathode delivers smooth voltage profiles, enhanced structural stability, elevated self-discharge resistance, and inhibited nickel dissolution. As a result, the Mg/Mn-LiNiO 2 cathode enables improved cycling stability in lithium metal batteries with the conventional carbonate electrolyte: 80% capacity retention after 350 cycles at C /3, and 67% capacity retention after 500 cycles at 2 C (22 °C). We then take the Mg/Mn-LiNiO 2 as the platform to investigate the local structural and chemical reversibility, where we identify that the irreversibility takes place starting from the very first cycle. The highly reactive surface induces the surface oxygen loss, metal reduction reaching the subsurface, and metal dissolution. Our data demonstrate that the dual dopants can, to some degree, mitigate the irreversibility and improve the cycling stability of LiNiO 2 , but more efforts are needed to eliminate the key challenges of these materials for battery operation in the conventional carbonate electrolyte.

25 ENERGY STORAGE↗

LaCrO 3 -Coated La 0.6 Sr 0.4 Co 0.2 Fe0.8O3–δ Core–Shell Structured Cathode with Enhanced Cr Tolerance for Intermediate-Temperature Solid Oxide Fuel Cells

La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF) is a common cathode material for intermediate temperature solid oxide fuel cells due to its excellent oxygen reduction reaction catalytic activity. However, the Cr-poisoning effect is a severe issue causing its electrochemical performance degrada-tion. To develop a LSCF-based cathode with excellent Cr-tolerance, LaCrO 3 -coated LSCF core-shell structured (LCr@LSCF) cathode was prepared via solution infiltration method. After coated by LCr shell, the long-term stability and Cr-tolerance were obviously improved, at the price of sacrificing some electrochemical performance. As a result, the development of LCr@LSCF cathode with eye-catching Cr-tolerance is of great significance to the commercialization of LSCF.

36 MATERIALS SCIENCE↗

Iron-Doped Sodium Vanadium Oxyflurophosphate Cathodes for Sodium-Ion Batteries—Electrochemical Characterization and In Situ Measurements of Heat Generation

Sodium-ion batteries (NaIBs) are increasingly being envisioned for grid-scale energy-storage systems because of cost advantages. However, implementation of this vision has been challenged by the low-energy densities delivered by most NaIB cathodes. Toward addressing this challenge, the authors report the synthesis and characterization of a new iron-doped Na 3 Fe 0.3 V 1.7 O(PO 4 ) 2 F 2 cathode using a novel facile hydrothermal route. The synthesized material was characterized using scanning electron microscopy, X-ray diffraction, and Mössbauer spectroscopy techniques. The obtained discharge capacity in the half-cell configuration lies from 119 to 125 to 130 mA h/g at C/10 while tested using three different electrolyte formulations, dimethyl carbonate–ethylene carbonate (EC)–propylene carbonate (PC), diethyl carbonate–EC, and EC–PC, respectively. The synthesized cathodes were also evaluated in full-cell configurations, which delivered an initial discharge capacity of 80 mA h/g with NaTi 2 (PO 4 ) 3 MWCNT as the anode. Ionic diffusivity and interfacial charge transfer kinetics were also evaluated as a function of temperature and sodium concentration, which revealed that electrochemical rate performances in this material were limited by charge-transfer kinetics. To understand the heat generation mechanism of the Na/Na 3 Fe 0.3 V 1.7 O(PO 4 ) 2 F 2 half-cell during charge and discharge processes, an electrochemical isothermal calorimetry measurement was carried out at different current rates for two different temperatures (25 and 45 °C). The results showed that the amount of heat generated was strongly affected by the operating charge/discharge state, C-rate, and temperature. Altogether, this work provides a new synthesis route for the development of iron-doped Na 3 Fe 0.3 V 1.7 O(PO 4 ) 2 F 2 -based high-performance sodium cathode materials aimed at providing a viable pathway for the development and deployment of large-scale energy-storage based on sodium battery systems.

25 ENERGY STORAGE↗

Understanding the Effect of Cathode Composition on the Interface and Crosstalk in NMC/Si Full Cells

Crosstalk between the cathode and the anode in lithium-ion batteries has a great impact on performance, safety, and cycle lifetime. Still, no report exists for a systematic investigation on crosstalk behavior in silicon (Si)-based cells as a function of transition metal composition in cathodes. We studied the effect of crosstalk on degradation of Si-rich anodes in full cells with different cathodes having the same crystal structure but different transition metal compositions, such as LiNi 1/3 Mn 1/3 Co 1/3 O 2 (NM111), LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532), and LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811). We found that the transition metal composition in cathodes, especially Mn ion concentration, significantly affects electrolyte decomposition reactions, even from very early cycles. This change causes differences in the solid electrolyte interphase (SEI) chemistry of each aged Si sample. As a result, each of the aged Si samples has a different electrochemistry, in terms of initial Coulombic efficiency and the mechanism of capacity fade.

25 ENERGY STORAGE↗

Facile Dual-Protection Layer and Advanced Electrolyte Enhancing Performances of Cobalt-free/Nickel-rich Cathodes in Lithium-Ion Batteries

Despite cobalt (Co)-free/nickel (Ni)-rich layered oxides being considered as one of the promising cathode materials due to their high specific capacity, their highly reactive surface is one of the shortcomings that still hinder their practical usages in high-energy-density batteries. Herein, a polyimide/polyvinylpyrrolidone (PI/PVP, denoted as PP) coating layer is demonstrated as dual-protection for LiNi 0.96 Mg 0.02 Ti 0.02 O 2 (NMT) cathode material to suppress surface contamination against moisty air and to prevent unwanted side reactions between cathode and electrolyte during electrochemical cycling. The optimal PP-coated NMT (PP@NMT) preserves a clean surface without generation of lithium (Li) residues, structural degradation, and gas evolution after exposure to air with ~30% humidity for 2 weeks. Contrarily, the exposed bare NMT shows severe contamination, structural shrinkage due to Li loss, and increased gas release during charging. In addition, the exposed PP@NMT significantly enhances the electrochemical performance of graphite (Gr)||NMT cells by decreasing byproducts and maintaining structural stability. Moreover, the exposed PP@NMT achieves a high capacity retention of 86.7% after 500 cycles in Gr||NMT cells using an advanced localized high-concentration electrolyte. Furthermore, this work demonstrates a promising facile approach to the protection of Co-free/Ni-rich layered cathodes for their practical applications even after exposure to moisty air.

25 ENERGY STORAGE↗

Heuristics for Molten-Salt Synthesis of Single-Crystalline Ultrahigh-Nickel Layered Oxide Cathodes

In pursuit of Li-ion batteries with higher energy density, ultrahigh-nickel layered oxides are a leading candidate for next-generation cathode materials. Single-crystalline morphology offers a neat solution to the poor stability of ultrahigh-Ni cathodes; a lower active surface area mitigates electrolyte decomposition at high voltages, and the elimination of grain boundaries improves mechanical resilience and increases volumetric energy density. However, single-crystal cathodes possess their own challenges, several of which originate from synthesis at elevated temperatures meant to induce grain growth. Molten-salt synthesis is an alternative method for obtaining single crystals, accelerating grain growth through the presence of a molten flux without the need for increased temperature. Herein, we offer heuristic guidelines for molten-salt synthesis, discussing key factors for designing reaction mixtures and the necessary exploratory research for novel molten salt/cathode systems. Here, the influence of different salts and synthesis conditions on the morphology and properties of single-crystal LiNiO 2 is presented. It is found that oxidative salts, such as Li 2 O 2 and LiNO 3 , are crucial to supplementing dissolution of gaseous oxygen into the molten phase. Through these discussions, this work aims to provide a set of overarching principles for obtaining higher-quality single-crystal layered oxide cathodes and engender more rigorous and impactful investigation into their fundamental nature and applications.

25 ENERGY STORAGE↗

Enhancing the Electrode Gravimetric Capacity of Li 1.2 Mn 0.4 Ti 0.4 O 2 Cathode Using Interfacial Carbon Deposition and Carbon Nanotube-Mediated Electrical Percolation

Mn-based cation disordered rocksalt oxides (Mn-DRX) are emerging as promising cathode materials for next-generation Li-ion batteries due to their high specific capacities and cobalt and nickel free characteristic. However, to reach the theoretical capacity, solid-state method synthesized Mn-DRX materials require activation via post-synthetic ball milling, typically incorporating more than 20 wt.% conductive carbon that adversely reduces the electrode level gravimetric capacity. To solve this issue, we firstly deposit amorphous carbon on the surface of the Li 1.2 Mn 0.4 Ti 0.4 O 2 (LMTO) particles to increase the electrical conductivity by a five order of magnitude. Although the cathode material gravimetric first charge capacity reaches 180 mAh/g, its highly irreversible behavior leads to a 70 mAh/g first discharge capacity. Subsequently, to ensure a good electrical percolation network, the LMTO material is ball milled with multi-wall carbon nanotube (CNT) to obtain a 78.7 wt.% LMTO active material loading in the cathode electrode (LMTO-CNT). As a result, a 210 mAh/g cathode electrode gravimetric first charge and 165 mAh/g first discharge capacity are obtained, compared to the respective capacity values of 222 mAh/g and 155 mAh/g for the LMTO ball milled with 20 wt.% SuperP C65 electrode (LMTO-SP). After 50 cycles, the LMTO-CNT delivers a 121 mAh/g electrode gravimetric discharge capacity, largely outperforming the 44 mAh/g value of the LMTO-SP. In conclusion, our study demonstrates that while ball milling is necessary to achieve the theoretical capacity of LMTO, a careful selection of the additive, such as CNT, effectively reduces the required carbon quantity to achieve a higher electrode gravimetric discharge capacity.

25 ENERGY STORAGE↗

Novel Structural Motif To Promote Mg-Ion Mobility: Investigating ABO 4 Zircons as Magnesium Intercalation Cathodes

There is an increasing need for sustainable energy storage solutions as fossil fuels are replaced by renewable energy sources. Multivalent batteries, specifically Mg batteries, are one energy storage technology that researchers continue to develop with hopes to surpass the performance of Li-ion batteries. However, the limited energy density and transport properties of Mg cathodes remain critical challenges preventing the realization of high-performance multivalent batteries. In this work, ABO 4 zircon materials (A = Y, Eu and B = V, Cr) are computationally and experimentally evaluated as Mg intercalation cathodes. Remarkably good Mg-ion transport properties were predicted and Mg-ion intercalation was experimentally verified in sol-gel synthesized zircon YVO 4 , EuVO 4 , and EuCrO 4 . Among them, EuVO 4 exhibited the best electrochemical performance and demonstrated repeated reversible cycling. While we believe that the one-dimensional diffusion channels and redox-active species tetragonal coordination limit the value of many zircons as high-performance cathodes, their unique structural motif of overlapping polyhedra along the diffusion pathway appears instrumental for promoting good Mg-ion mobility. The motif results in a favorable "6-5-4" change in coordination that avoids unfavorable sites with lower coordination along the diffusion pathway and a structural design metric for future Mg cathode development.

25 ENERGY STORAGE↗

Unlocking the Potential of A-Site Ca-Doped LaCo 0.2 Fe 0.8 O 3-δ : A Redox-Stable Cathode Material Enabling High Current Density in Direct CO 2 Electrolysis

Massive carbon dioxide (CO 2 ) emission from recent human industrialization has affected the global ecosystem and raised great concern for environmental sustainability. The solid oxide electrolysis cell (SOEC) is a promising energy conversion device capable of efficiently converting CO 2 into valuable chemicals using renewable energy sources. However, Sr-containing cathode materials face the challenge of Sr carbonation during CO 2 electrolysis, which greatly affects the energy conversion efficiency and long-term stability. Thus, A-site Ca-doped La1– x CaxCo 0.2 Fe 0.8 O 3-δ (0.2 ≤ x ≤ 0.6) oxides are developed for direct CO 2 conversion to carbon monoxide (CO) in an intermediate-temperature SOEC (IT-SOEC). With a polarization resistance as low as 0.18 O cm 2 in pure CO 2 atmosphere, a remarkable current density of 2.24 A cm –2 was achieved at 1.5 V with La 0.6 Ca 0.4 Co 0.2 Fe 0.8 O 3-δ (LCCF64) as the cathode in La 0.8 Sr 0.2 Ga 0.83 Mg 0.17 O 3-δ (LSGM) electrolyte (300 µm) supported electrolysis cells using La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF) as the air electrode at 800 °C. Furthermore, symmetrical cells with LCCF64 as the electrodes also show promising electrolysis performance of 1.78 A cm –2 at 1.5 V at 800 °C. In addition, stable cell performance has been achieved on direct CO 2 electrolysis at an applied constant current of 0.5 A cm –2 at 800 °C. The easily removable carbonate intermediate produced during direct CO 2 electrolysis makes LCCF64 a promising regenerable cathode. The outstanding electrocatalytic performance of the LCCF64 cathode is ascribed to the highly active and stable metal/perovskite interfaces that resulted from the in situ exsolved Co/CoFe nanoparticles and the additional oxygen vacancies originated from the Ca 2 Fe 2 O 5 phase synergistically providing active sites for CO 2 adsorption and electrolysis. Here this study offers a novel approach to design catalysts with high performance for direct CO 2 electrolysis.

30 DIRECT ENERGY CONVERSION↗

Dual Passivation of Cathode and Anode through Electrode–Electrolyte Interface Engineering Enables Long-Lifespan Li Metal–SPAN Batteries

The reliability and durability of lithium metal (Li 0 )–sulfur batteries are largely limited by the undesired Li 0 plating-stripping irreversibility and the detrimental polysulfide dissolution, yet approaches that can simultaneously address the above anodic and cathodic problems are scarce. In this study, we report the stable operation of a Li 0 -SPAN (sulfurized polyacrylonitrile) battery via an anode–cathode dual-passivation approach. By combination of a fluorinated localized high concentration electrolyte (LHCE) and a Li 3 N-forming additive (TMS-N 3 ), robust and highly conductive electrode passivation layers are formed in situ on the surface of both the Li 0 anode and the SPAN cathode. The resulting highly reversible, dendrite-free, and high-density Li 0 plating morphology enables a high Coulombic efficiency of 99.4%. Advanced tender energy X-ray spectroscopy also reveals the eliminated Li 2 S formation and minimized polysulfide dissolution in SPAN cathodes, leading to a high capacity of 580 mAh/g SPAN and stable cycling with negligible capacity decay (0.7%) for 800 cycles. This electrode–electrolyte interphase engineering strategy has tackled the major limitations of Li–S batteries in both ether- and carbonate-based electrolyte systems and under a wide temperature range from –10 to +50 °C, thus providing insightful guidelines for the rational design of highly durable and high-energy-density Li 0 -S batteries.

25 ENERGY STORAGE↗

Quantitative Analysis and Prediction of Thermal Runaway Metrics of High-Nickel Oxide Cathodes by Machine Learning Models

The pursuit of higher energy density in lithium-ion batteries has made high-nickel (Ni) layered oxides leading cathode candidates for next-generation electric vehicles. However, their poor thermal stability, particularly at Ni contents ≥ 90%, increases the risk of cathode-initiated thermal runaway. Furthermore, we present a data-driven framework combining linear and nonlinear machine learning models to predict key thermal runaway descriptors from a high-throughput differential scanning calorimetry database. With cathode composition and state of charge (SOC) as input features, the ensemble model accurately predicts peak temperature, heat release, and peak heat flow. SHAP analysis identifies Ni content and SOC as the dominant factors controlling thermal runaway temperature, while SOC primarily governs heat release and peak heat flow. Al, Mg, and Mn improve thermal stability by strengthening metal–oxygen bonding and delaying structural transformation, whereas B mainly reduces heat release through surface passivation. Validation with a new cathode composition confirms accurate prediction of SOC-dependent thermal runaway behavior and critical SOC.

25 ENERGY STORAGE↗

Transition Metal Dissolution Mechanisms and Impacts on Electronic Conductivity in Composite LiNi 0.5 Mn 1.5 O 4 Cathode Films

The high-voltage LiNi 0.5 Mn 1.5 O 4 (LNMO) spinel cathode material offers high energy density storage capabilities without the use of costly Co that is prevalent in other Li-ion battery chemistries (e.g., LiNi x Mn y Co z O 2 (NMC)). Unfortunately, LNMO-containing batteries suffer from poor cycling performance because of the intrinsically coupled processes of electrolyte oxidation and transition metal dissolution that occurs at high voltage. In this work, we use operando electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) spectroscopies to demonstrate that transition metal dissolution in LNMO is tightly coupled to HF formation (and thus, electrolyte oxidation reactions as detected with operando and in situ solution NMR), indicative of an acid-driven disproportionation reaction that occurs during delithiation (i.e., battery charging). Leveraging the temporal resolution (s-min) of magnetic resonance, we find that the LNMO particles accelerate the rate of LiPF 6 decomposition and subsequent Mn 2+ dissolution, possibly due to the acidic nature of terminal Mn-OH groups. X-ray photoemission electron microscopy (XPEEM) provides surface-sensitive and localized X-ray absorption spectroscopy (XAS) measurements, in addition to X-ray photoelectron spectroscopy (XPS), that indicate disproportionation is enabled by surface reconstruction upon charging, which leads to surface Mn 3+ sites on the LNMO particle surface that can disproportionate into Mn 2+ (dissolved) and Mn 4+ (s) . During discharge of the battery, we observe high quantities of metal fluorides (in particular, MnF 2 ) in the cathode electrolyte interphase (CEI) on LNMO as well as the conductive carbon additives in the composite. Electronic conductivity measurements indicate that the MnF 2 decreases film conductivity by threefold compared to LiF, suggesting that this CEI component may impede both the ionic and electronic properties of the cathode. Ultimately, to prevent transition metal dissolution and the associated side reactions in spinel-type cathodes (particularly those that operate at high voltages like LNMO), the use of electrolytes that offer improved anodic stability and prevent acid byproducts will likely be necessary.

36 MATERIALS SCIENCE↗

In Situ Surface Reconstruction via Lithium Residue Regulation for Direct Recycling of Ni-Rich Cathodes

Surface stability is crucial for the long cycling performance of Ni-rich cathodes, as it dictates and governs side reactions, preserves crystal integrity, and mitigates capacity degradation during cycling. For spent Ni-rich cathodes targeted for one-step direct recycling, constructing a robust and stable surface is particularly challenging because prior cycling induces severe structural and morphological degradation. Here, in this study, we introduce an in situ surface reconstruction strategy that converts surface lithium residues into a protective layer via a direct liquid-phase coating with ammonium dihydrogen phosphate (ADP). During the process, residual lithium remaining after the hydrothermal relithiation is removed, while a conformal lithium phosphate (Li 3 PO 4 , LPO) layer is formed to act as both a chemical barrier and a structural stabilizer. This dual function enhances cycling stability and rate capability in regenerated cathodes, and the approach is applicable to various Ni-rich compositions including spent LiNi 0.6 Co 0.2 Mn 0.2 O 2 (NCM622) and scrap LiNi 0.866 Mn 0.066 Co 0.05 Al 0.018 O 2 (NCMA). Its scalability and compositional versatility make it a promising route for sustainable regeneration of high-performance cathode materials.

36 MATERIALS SCIENCE↗

Extended Interfacial Stability through Simple Acid Rinsing in a Li-Rich Oxide Cathode Material

Layered Li-rich Ni, Mn, Co (NMC) oxide cathodes in Li-ion batteries provide high specific capacities (>250 mAh/g) via O-redox at high voltages. However, associated high-voltage interfacial degradation processes require strategies for effective electrode surface passivation. Here, we show that an acidic surface treatment of a Li-rich NMC layered oxide cathode material leads to a substantial suppression of CO 2 and O 2 evolution, ~90% and ~100% respectively, during the first charge up to 4.8 V vs. Li +/0 . CO 2 suppression is related to Li 2 CO 3 removal as well as effective surface passivation against electrolyte degradation. This treatment does not result in any loss of discharge capacity and provides superior long-term cycling and rate performance compared to as-received, untreated materials. We also quantify the extent of lattice oxygen participation in charge compensation (“O-redox”) during Li + removal by a novel ex-situ acid titration. Our results indicate that the peroxo-like species resulting from O-redox originate on the surface at least 300 mV earlier than the activation plateau region around 4.5 V. X-ray photoelectron spectra and Mn -L X-ray absorption spectra of the cathode powders reveal a Li + deficiency and a partial reduction of Mn ions on the surface of the acid-treated material. More interestingly, although the irreversible oxygen evolution is greatly suppressed through the surface treatment, our O K-edge resonant inelastic X-ray scattering shows the lattice O-redox behavior largely sustained. The acidic treatment, therefore, only optimizes the surface of the Li-rich material and almost eliminates the irreversible gas evolution, leading to improved cycling and rate performance. This work therefore presents a simple yet effective approach to passivate cathode surfaces against interfacial instabilities during high-voltage battery operation.

25 ENERGY STORAGE↗

Probing the Thermal-Driven Structural and Chemical Degradation of Ni-Rich Layered Cathodes by Co/Mn Exchange

The intrinsic poor thermal stability of layered LiNi x Co y Mn 1-x-y O 2 (NCM) cathodes and the exothermic side reactions triggered by the associated oxygen release are the main safety threats for their large-scale implantation. In NCM family, it is widely accepted that Ni is the stability troublemaker, while Mn has long been considered as a structure stabilizer, whereas the role of Co remains elusive. Here, via Co/Mn exchange in Ni-rich LiNi 0.83 Co 0.11 Mn 0.06 O 2 cathode, we demonstrate that, the chemical and structural stability of the deep delithiated NCM cathodes are significantly affected by Co, rather than the widely reported Mn. Operando synchrotron X-ray characterization coupling with in situ mass spectrometry reveal that the Co 4+ reduces prior to the reduction of Ni 4+ , and could thus prolong the Ni migration by occupying the tetrahedra sites, and hence postpone the oxygen release and thermal failure. In contrast, the Mn itself is stable, but barely stabilizes the Ni 4+ . Our results highlight the importance of evaluating the intrinsic role of compositional tuning on Ni-rich/Co-free layered oxide cathode materials to guarantee the safe operation of high-energy Li-ion batteries.

25 ENERGY STORAGE↗