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DOE OSTI2023

Biopolymer‐assisted Synthesis of P‐doped TiO 2 Nanoparticles for High‐performance Lithium‐ion Batteries: A Comprehensive Study

Abstract TiO 2 material has gained significant attention for large‐scale energy storage due to its abundant, low‐cost, and environmentally friendly properties, as well as the availability of various nanostructures. Phosphorus doping has been established as an effective technique for improving electronic conductivity and managing the slow ionic diffusion kinetics of TiO 2 . In this study, non‐doped and phosphorus doped TiO 2 materials were synthesized using sodium alginate biopolymer as chelating agent. The prepared materials were evaluated as anode materials for lithium‐ion batteries (LIBs). The electrodes exhibit remarkable electrochemical performance, including a high reversible capacity of 235 mAh g −1 at 0.1 C and excellent first coulombic efficiency of 99 %. An integrated approach, combining operando XRD and ex‐situ XAS, comprehensively investigates the relationship between phosphorus doping, material structure, and electrochemical performance, reinforced by analytical tools and first principles calculations. Furthermore, a full cell was designed using 2 %P‐doped TiO 2 anode and LiFePO 4 cathode. The output voltage was about 1.6 V with high initial specific capacity of 148 mAh g −1 , high rate‐capability of 120 mAh g −1 at 1 C, and high‐capacity retention of 96 % after 1000 cycles at 1 C.

El Halya, Nabil↗

DOE OSTI2017

Latent Effects of Radiation on Li-ion Batteries in Robots

The rapid development of Li-ion batteries (LIBs) is due to their high energy-density storage capability, which makes them suitable for application in both vehicles (e.g., electrified car) and electronic devices (e.g., cell phone, laptop, etc.), which are currently ubiquitous. Another less common but important application of LIBs is the powering of equipment in extreme environments such as robots operating in a nuclear rescue mission, unmanned vehicles surveying environments exposed to radiation, or vehicles and probes for outer space exploration. In our previous study, coin cells with lithium metal serving as the reference and counter electrode were assembled with either an irradiated cathode or irradiated electrolyte. We have observed an increase in premature battery failure and degradation of capacity of the battery made from irradiated cathodes and battery made from the irradiated electrolyte. For the group with cathodes irradiated to a 9.8 Mrad cumulative dose, the resistance was 2-3 times higher than the control group. On the other hand, cells with irradiated electrolyte showed increased resistance even at very low dose levels. Most importantly, a significant color change to the irradiated electrolyte after a long-term storage in a glove box has been observed. However, the electrolyte did not show any noticeable change immediately after irradiation. We name this phenomenon latent effects, which is more significant than the damage received by batteries due to initial dose. Also, electrolyte irradiated to a medium dose (1.6 Mrad) showed a poorer performance (higher failure rate, higher resistance) than those cells which received high dose (5 Mrad). We attribute this to the latent effect because this group battery was unintentionally assembled 3 days after initial electrolyte irradiation. The existence of latent effects implies that in space missions or post-accident events, instruments equipped with LIBs may fail unpredictably at post-irradiation stages, even if they survive the initial dose or the performance tests conducted after the initial dose. These instruments may fail several days or even weeks after irradiation, depending on the initial cumulative dose and dosage rate. For comprehending the influence of latent effects on the entire battery instead of on the individual components, we performed an in-situ cycling of coin cells made in-house, where the batteries were cycled under irradiation and then cycled again to evaluate their overall capacity fade, cyclability, and cell resistance. Additionally we investigated the effects of battery fading due to radiation on the performance of a drone.

25 ENERGY STORAGE↗

DOE OSTI2023

3D–Integrated, Multi–Functional Carbon Fibers for Stable, High–Areal–Capacity Batteries

Increasing lithium-ion batteries' (LIBs) electrode areal capacity can boost energy density and lower manufacturing costs, but faces challenges in manufacturing, rate performance, and cycling stability. A conductive framework made of commercial micro-sized carbon fibers (Cfs) is presented that serves as a host for both the LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC 532) cathode and Cfs anode. The Cf framework has multiple functions that offer high electronic conductivity (270 mS cm –1 ), low tortuosity (1.7), low Li + diffusion resistance (22 Ω), and high thermal conductivity (200 W mK –1 ). Additionally, the Cf-integrated electrodes can have an extremely high mass loading of NMC 532 (70 mg cm –2 ) with a theoretical capacity of 14 mAh cm –2 . Thus, the practical full cells assembled with the Cfs-enabled electrodes exhibit an initial areal capacity of 4.1 mAh cm –2 and capacity retention of 90.4% at 500 cycles at a cycling rate of C/3, 1.5 mA cm –2 . Data collected from the operando isothermal microcalorimetry suggest that full cells utilizing the Cf anode experience less heat release from side reactions compared to cells utilizing a conventional graphite anode. Finally, this present approach is scalable and cost-effective and can fabricate practical LIBs that boast high areal capacity, rate performance, and a lengthy cycling lifetime.

25 ENERGY STORAGE↗

DOE OSTI2017

Unique aqueous Li-ion/sulfur chemistry with high energy density and reversibility

Leveraging the most recent success in expanding the electrochemical stability window of aqueous electrolytes, in this work we create a unique Li-ion/sulfur chemistry of both high energy density and safety. We show that in the superconcentrated aqueous electrolyte, lithiation of sulfur experiences phase change from a high-order polysulfide to low-order polysulfides through solid–liquid two-phase reaction pathway, where the liquid polysulfide phase in the sulfide electrode is thermodynamically phase-separated from the superconcentrated aqueous electrolyte. The sulfur with solid–liquid two-phase exhibits a reversible capacity of 1,327 mAh/(g of S), along with fast reaction kinetics and negligible polysulfide dissolution. By coupling a sulfur anode with different Li-ion cathode materials, the aqueous Li-ion/sulfur full cell delivers record-high energy densities up to 200 Wh/(kg of total electrode mass) for >1,000 cycles at ~100% coulombic efficiency. These performances already approach that of commercial lithium-ion batteries (LIBs) using a nonaqueous electrolyte, along with intrinsic safety not possessed by the latter. We conclude the excellent performance of this aqueous battery chemistry significantly promotes the practical possibility of aqueous LIBs in large-format applications.

25 ENERGY STORAGE↗

DOE OSTI2022

Anomalous Thermal Decomposition Behavior of Polycrystalline LiNi 0.8 Mn 0.1 Co 0.1 O 2 in PEO-Based Solid Polymer Electrolyte

we report that replacing liquid electrolytes (LEs) with polymer electrolytes has been considered a promising approach to developing next-generation lithium-ion batteries (LIBs) with high energy density and superior safety. Nevertheless, compared with the extensive research on the electrochemical stability of the cathode/polymer electrolyte interfaces, reports on their thermal behaviors are rare to date. Herein, this work systematically investigates the thermal stability of two typical layered oxide cathodes, LiCoO 2 (LCO) and LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811), with poly(ethylene oxide) (PEO) electrolyte and with carbonate LEs, respectively. It is found that the oxygen release from the cathodes plays a central role in thermal runaway. Replacing the LE with PEO electrolyte can considerably improve the thermal stability of LCO, but surprisingly, deteriorate that of NMC811. The reason is that the surface of single-crystalline LCO particles can be effectively passivated by the PEO electrolyte during heating, but PEO cannot sufficiently passivate all the primary particles of NMC811 owing to insufficient interface wettability of PEO electrolyte within the polycrystalline secondary NMC811 particles. The findings in this work collectively formulate valuable guidance for improving the safety of polymer-electrolyte-based as well as other types of all-solid-state lithium-ion batteries.

25 ENERGY STORAGE↗

DOE OSTI2023

Understanding the Role of Zinc Hydroxide Sulfate and its Analogues in Mildly Acidic Aqueous Zinc Batteries: A Review

Abstract Mildly acidic aqueous zinc batteries (AZBs) have attracted tremendous attention for grid storage applications with the expectation to tackle the issues of Li‐ion batteries on high cost and poor safety. However, the performance, particularly energy density and cycle stability of AZBs are still unsatisfactory when compared with LIBs. To help the development of AZBs, a lot of effort have been made to understand the battery reaction mechanisms and precedent microscopic and spectroscopic analyses have shown flake‐like large particles of zinc hydroxide sulfate (ZHS) and its analogues formed on the surfaces of cathodes and anodes in sulfate and other electrolyte systems during cycling. However, because of the complexity of the thermodynamics and kinetics of aqueous reactions to understand different battery conditions, controversies still exist. This article will review the roles of ZHS discussed in recent representative references aiming to shine light on the fundamental mechanisms of AZBs and pave ways to further improve the battery performance.

25 ENERGY STORAGE↗

DOE OSTI2021

Understanding multi-scale battery degradation with a macro-to-nano zoom through its hierarchy

Lithium-ion batteries (LIBs) feature structural and chemical complexities across a broad range of length scales. It is the hierarchy of the battery structure that determines its functionality. An in-depth understanding of the battery function, degradation, and failure mechanisms requires a thorough and systematic investigation from structural, chemical, mechanical, and dynamic perspectives. Here we present a macro-to-nano zoom through the hierarchy of a commercial 18650 type LIB using a suite of state-of-the-art X-ray microscopy techniques. Damage, deformation, and heterogeneity at different length scales are visualized and are associated with different degradation phenomena and mechanisms. Our results highlight the importance of the mechanical properties of the cathode material, which could impact both the immediate and the long-term cell behaviors significantly. While this study focuses on a commercial lithium cell with a standard configuration, our findings can be extrapolated and are applicable to the development of next-generation energy storage technology, e.g. solid-state batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Laboratory-Based X-ray Absorption Spectroscopy on a Working Pouch Cell Battery at Industrially-Relevant Charging Rates

Li-ion battery (LIB) research has continuing importance for the entire range of applications from consumer products to vehicle electrification and grid stabilization. In many cases, standard electrochemical methods only provide an overall voltage or specific capacity, giving an inadequate description of parallel redox processes or chemical gradients at the particle and pack level. X-ray absorption fine structure (XAFS) is frequently used to augment bulk electrochemical data, as it provides element-specific changes in oxidation state and local atomic structure. Such microscopic descriptors are crucial for elucidating charge transfer and structural changes associated with bonding or site mixing, two key factors in evaluating state of charge and modes of cell failure. However, the impact of XAFS on LIB research has been significantly constrained by a logistical barrier: contemporary XAFS work is performed almost exclusively at synchrotron X-ray light sources, where beamtime is infrequent and experiment time-frames are limited. In this report we show that modern laboratory-based XAFS cannot only be applied to, e.g., characterization of ex situ LIB electrode materials, but can also be used for operando studies at industrially-relevant charging rates in a standard pouch cell preparation. Such capability enables accelerated discovery of new materials and improved operation modes for LIBs.

25 ENERGY STORAGE↗

DOE OSTI2021

The Quest for Stable Potassium‐Ion Battery Chemistry

Abstract Potassium‐ion batteries (KIBs) have attracted wide interest for energy storage because of the abundance of the electrode materials involved; however, their electrochemical performances are far behind what can be achieved from lithium‐ion batteries (LIBs) or sodium‐ion batteries (SIBs). Herein, key promising electrode and electrolyte materials for potassium‐ion batteries are identified, the coupled electrochemical reactions in the cell are investigated, and the compatibility between different materials is demonstrated to play the most important role. K 2 Mn[Fe(CN) 6 ] cathode can deliver a high capacity of ≈125 mAh g −1 and exceptional cycling stability over 61 000 cycles (≈9 months) if the side reactions from the anode can be prevented. Graphite is a good anode material but is subjected to degradation in traditional carbonate electrolytes. New concentrated electrolytes are developed and evaluated. A stable KIB system is demonstrated by coupling a stable K 2 Mn[Fe(CN) 6 ] cathode, a prepotassiated graphite anode with a concentrated electrolyte to achieve a high energy density of ≈260 Wh kg −1 (based on the active mass of cathode and anode) and good cycling of over 1000 cycles.

Wu, Xianyong↗

DOE OSTI2022

Electrification and decarbonization of spent Li-ion batteries purification by using an electrochemical membrane reactor

The expanding electric vehicle market brings with it exponential growth in the use of lithium (Li)-ion batteries (LIB) for which a wave of spent LIB is expected to come within the next 5 to 10 years. Due to the economic and strategic value imbedded within the metals contained in LIB, different recycling technologies, including hydrometallurgy, pyrometallurgy and direct recycling, are under development. Being different from previous hydrometallurgical methods, which may have high chemical consumption and negative environmental impact, an electrochemical membrane reactor is designed and validated for the first time, to electrify and decarbonize the impurity removal process. This reactor electroplates copper (Cu) and electrochemically precipitates aluminum (Al) and iron (Fe) from simulated spent LIB leachates, by consuming only air, water, and electricity, and the impurities are reduced to <1 ppm. The purified leachate maintains 99.5 % of the nickel (Ni), 95.4 % of the cobalt (Co) and 99.14 % of manganese (Mn) from the original leachate solution, and then can be directly applied for cathode precursor synthesis. Additionally, the purification process doesn’t introduce extra impurity, and the reactor restoration process generates valuable by-product hydro sulfate (H2SO4). This electrochemical process can reduce the cost, because of the much less chemical consumption and the valuable by-product generation, and mitigates the waste emissions, because of no extra impurity introduced and no greenhouse gas (GHG) produced. In conclusion, the chemical precipitation method uses significant amount of NaOH, which induced GHG emission during the manufacturing process.

25 ENERGY STORAGE↗

DOE OSTI2018

Understanding Conversion-Type Electrodes for Lithium Rechargeable Batteries

The need/desire to lower the consumption of fossil fuels and its environmental consequences has reached unprecedented levels in recent years. A global effort has been undertaken to develop advanced renewable energy generation and especially energy storage technologies, as they would enable a dramatic increase in the effective and efficient use of renewable (and often intermittent) energy sources. The development of electrical energy storage (EES) technologies with high energy and power densities, long life, low cost, and safe use represents a challenge from both the fundamental science and technological application points of view. While the advent and broad deployment of lithium-ion batteries (LIBs) has dramatically changed the EES landscape, their performance metrics need to be greatly enhanced to keep pace with the ever-increasing demands imposed by modern consumer electronics and especially the emerging automotive markets. Current battery technologies are mostly based on the use of a transition metal oxide cathode (e.g., LiCoO 2 , LiFePO 4 , or LiNiMnCoO 2 ) and a graphite anode, both of which depend on intercalation/insertion of lithium ions for operation. While the cathode material currently limits the battery capacity and overall energy density, there is a great deal of interest in the development of high-capacity cathode materials as well as anode materials. Conversion reaction materials have been identified/proposed as potentially high-energy-density alternatives to intercalation-based materials. Yet, conversion reaction materials react during lithiation to form entirely new products, often with dramatically changed structure and chemistry, by reaction mechanisms that are still not completely understood. This makes it difficult to clearly distinguish the limitations imposed by the mechanism and practical losses from initial particle morphology, synthetic approaches, and electrode preparations. Transition metal compounds such as transition metal oxides, sulfides, fluorides, phosphides, and nitrides can undergo conversion reactions yielding materials with high theoretical capacity (generally from 500 to 1500 mA h g –1 ). Specifically, a number of transition metal oxides and sulfides have shown excellent electrochemical properties as high-capacity anode materials. In addition, some transition metal fluorides have shown great potential as cathode materials for Li rechargeable batteries. In this Account we present mechanistic studies, with emphasis on the use of operando methods, of selected examples of conversion-type materials as both potentially high-energy-density anodes and cathodes in EES applications. We also include examples of the conceptually similar conversion-type reactions involving chalcogens and halogens, with emphasis on the Li–S system. In this case we focus on the problems arising from the low electrical conductivities of elemental sulfur and Li 2 S and the “redox shuttle” phenomena of polysulfides. In addition to mechanistic insights from the use of operando methods, we further cover several key strategies in electrode materials design such as controlling the size, morphology, composition, and architecture.

25 ENERGY STORAGE↗

DOE OSTI2023

A04-0491 - Reduced Electrolyte Reactivity of Pitch-Carbon Coated Si Nanoparticles for Li-Ion Battery Anodes

Silicon-based anodes for Li-ion batteries (LIB) have the potential to increase the energy density over graphite-based LIB anodes. However, silicon anodes exhibit poor cycle and calendar lifetimes due to mechanical instabilities and high chemical reactivity with the carbonate-based electrolytes that are typically used in LIBs. In this work, we synthesize a pitch-carbon coated silicon nanoparticle composite active material for LIB anodes that exhibits reduced chemical reactivity with the carbonate electrolyte compared to an uncoated silicon anode. Silicon primary particle sizes <10 nm minimize micro-scale mechanical degradation of the anode composite, while conformal coatings of pitch-carbon minimized the parasitic reactions between the silicon and the electrolyte. When matched with a high voltage NMC622 cathode, the pitch-carbon coated Si anode retains -75% of its initial capacity over 1000 cycles. Efforts to increase the areal loading of the pitch-carbon coated silicon anodes to realize real energy density improvements over graphite anodes results in severe mechanical degradation on the electrode level. Developing procedures to engineer the architecture of the composite silicon anode may be a solution to this mechanical challenge.

DIRECT ENERGY CONVERSION,ENERGY STORAGE↗

DOE OSTI2017

In situ Visualization of State-of-Charge Heterogeneity within a LiCoO 2 Particle that Evolves upon Cycling at Different Rates

For designing new battery systems with higher energy density and longer cycle life, it is important to understand the degradation mechanism of the electrode material, especially at the individual particle level. Using in situ transmission X-ray microscopy (TXM) coupled to a pouch cell setup, the inhomogeneous Li distribution as well as the formation, population, and evolution of inactive domains in a single LiCoO 2 particle were visualized in this paper as it was cycled for many times. It is found that the percentage of the particle that fully recovered to the pristine state is strongly related to the cycling rate. Interestingly, we also observed the evolution of the inactive region within the particle during long-term cycling. The relationship between morphological degradation and chemical inhomogeneity, including the formation of unanticipated Co metal phase, is also observed. Finally, our work highlights the capability of in situ TXM for studying the degradation mechanism of materials in LIBs.

25 ENERGY STORAGE↗

DOE OSTI2023

Basics of the scanning electrochemical microscope and its application in the characterization of lithium-ion batteries: a brief review

A scanning electrochemical microscope (SECM) can directly monitor electrochemical processes at interfaces of electrodes and electrolytes and has been used as an analytical tool for lithium-ion battery (LIB) studies. Through SECM, we can visualize the electrochemical reactivities of active species in LIBs in-situ during cycling. This review begins with introducing SECM-based LIB research and then summarizes the working mechanism and operating modes of the technique as well as combinations of SECM with other techniques for LIB studies. We review the results with a focus on the interfacial properties, surface reactions and electrochemical activity of different electrode materials for LIBs. The investigations of battery degradation, kinetic parameters and electrolyte swelling by SECM are also discussed. Finally, the current limitations and perspectives are also described regarding future developments.

25 ENERGY STORAGE↗

DOE OSTI2025

Improved internal short circuit models for thermal runaway simulations in lithium-ion batteries

Thermal runaway (TR) modeling is one of the primary tools that can be used to overcome challenges associated with lithium-ion battery (LIB) safety. Among all LIB accidents that have occurred over the past decade, Internal Short Circuit (ISC) remains the most common trigger mechanism. Many available models in the literature either use a simplified approach to simulate ISC or completely ignore its contribution. The aim of this study is to understand the nature of the heat released for different types of ISC scenarios, including aluminum-anode, anode–cathode, and copper-cathode ISC. We study ISC behavior using a coupled electrochemical–thermal model with an integrated TR chemical kinetics solver built in the COMSOL Multiphysics framework. The time duration of heat release and the magnitude of the peak ISC current are studied as functions of parameters such as the size of the penetrating filament and the capacity of the cell. The numerical results are used to build an empirical model validated against the published experimental TR propagation data. Our model can be successfully used as a viable low-cost substitute in lower order (lumped) TR simulations to enable TR prevention and mitigation.

Singh, Bakhshish Preet (ORCID:0000000264751992)↗

DOE OSTI2023

Pitch Carbon-coated Ultrasmall Si Nanoparticle Lithium-ion Battery Anodes Exhibiting Reduced Reactivity with Carbonate-based Electrolyte

Silicon anodes for lithium-ion batteries (LIBs) have the potential for higher energy density compared to conventionally used graphite-based LIB anodes. However, silicon anodes exhibit poor cycle and calendar lifetimes due to mechanical instabilities and high chemical and electrochemical reactivity with the carbonate-based electrolytes that are typically used in LIBs. In this work, we synthesize a pitch carbon-coated silicon nanoparticle composite active material for LIB anodes that exhibits reduced chemical reactivity with carbonate-based electrolytes compared to an uncoated silicon anode. Silicon primary particle sizes less than 10 nm diameter minimize micro-scale mechanical degradation of the anode composite, while conformal coatings of pitch carbon minimize the parasitic reactions between the silicon and the electrolyte. When matched with a high voltage NMC622 (LiNi 0.6 Mn 0.2 Co 0.2 O 2 ) cathode, the pitch carbon-coated silicon anode retains approximately 75% of its initial capacity at the end of 1000 cycles. Increasing the areal loading of the pitch carbon-coated silicon anodes to realize energy density improvements over graphite anodes results in severe mechanical degradation on the electrode level, highlighting a remaining challenge to be addressed in future work.

25 ENERGY STORAGE↗

DOE OSTI2019

High performance lithium-ion and lithium–sulfur batteries using prelithiated phosphorus/carbon composite anode

Controlled chemical prelithiation of high capacity phosphorous/carbon (P/C) composite anode has been applied to develop advanced lithium-ion batteries (LIBs). The initial coulombic efficiency (CE) of P/C is significantly improved (up to 93% for fully-prelithiated P/C) owing to the formation of an artificial solid electrolyte interface (SEI) layer, which is characterized by SEM, Raman and XPS analyses. It ensures the application of P/C anode in real battery assembly. A partly-prelithiated P/C anode prepared by 20 sec prelithiation treatment is paired with a LiCoO2 (LCO) cathode. Here, the full cell delivers a highly reversible capacity of ~ 104 mAh g -1 LCO at 1C rate and retains a CE close to 100% over 2000 cycles. Moreover, a fully-prelithiated P/C anode prepared by 10 min prelithiation treatment is paired with a high-capacity Lifree sulfur/carbon (S/C) cathode. This newly configured full cell delivers a good rate and cycling performance and a high energy density of 358 Wh kg -1 .

25 ENERGY STORAGE↗

DOE OSTI2024

Sulfur Solutions: Advancing High Voltage and High Energy Lithium Batteries with Organosulfur Electrolytes

Achieving energy densities exceeding 350 Wh kg -1 while operating at elevated voltages (>4.5 V vs Li/Li + ) is attainable through judicious selection of electrochemical pairs at the cathode and anode. However, current state-of-the-art electrolytes exhibit limited stability when exposed to systems operating at or above 4.3 V. This limitation contributes to the degradation of electrode materials and raises critical safety concerns, impeding the commercialization of such systems. Consequently, there has been a notable surge in research efforts aimed at developing innovative electrolyte compositions capable of supporting high-voltage lithium-ion batteries (LIBs). A substantial portion of this research has focused on the family of organosulfur molecules, which possess high oxidative stability. Organosulfur salts also facilitate the formation of dense, ionically conductive solid electrolyte interfaces (SEI) and demonstrate excellent solubility. This article provides a comprehensive overview of the field of organosulfur electrolyte components for their applications in energy storage, encompassing solvents, alternative conducting salts, and additives. It emphasizes the idea that the deliberate design of electrolyte compositions is instrumental in controlling electrode passivation, with organosulfur-based structures historically proving advantageous in every aspect of the electrolyte. Crucially, it should be noted that many of these components are commercially available, holding significant implications for industrial applications.

25 ENERGY STORAGE↗