International Space Station Lithium-Ion Battery Safety Considerations
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Monitoring Redox Processes in Lithium-Ion Batteries by Laboratory-Scale Operando X-ray Emission Spectroscopy
Tracking changes in the chemical state of transition metals in alkali-ion batteries is crucial to understanding the redox chemistry during operation. X-ray absorption spectroscopy (XAS) is often used to follow the chemistry through observed changes in the chemical state and local atomic structure as a function of the state-of-charge (SoC) in batteries. In this study, we utilize an operando X-ray emission spectroscopy (XES) method to observe changes in the chemical state of active elements in batteries during operation. Operando XES and XAS were compared by using a laboratory-scale setup for four different battery systems: LiCoO 2 (LCO), Li[Ni 1/3 Co 1/3 Mn 1/3 ]O 2 (NMC111), Li[Ni 0.8 Co 0.1 Mn 0.1 ]O 2 (NMC811), and LiFePO 4 (LFP) under a constant current charging the battery in 10 h (C/10 charge rate). We show that XES, despite narrower chemical shifts in comparison to XAS, allows us to fingerprint the battery SOC in real time. We further demonstrate that XES can be used to track the change in net spin of the probed atoms by analyzing changes in the emission peak shape. As a test case, the connection between net spin and the local chemical and structural environment was investigated by using XES and XAS in the case of electrochemically delithiated LCO in the range of 2–10% lithium removal.
25 ENERGY STORAGE↗
Polythiophene side chain chemistry and its impact on advanced composite anodes for lithium-ion batteries
Tailored side chains can improve structural stability, ion transport and capacity retention, offering a solution to key challenges such as capacity fade and electrode degradation in lithium-ion batteries.
Li, Han [Department of Chemical and Bimolecular En↗
Restorable Neutralization of Poly(acrylic acid) Binders toward Balanced Processing Properties and Cycling Performance for Silicon Anodes in Lithium-Ion Batteries
Neutralization of poly(acrylic acid) (PAA)-based binders using lithium hydroxide is a common strategy for fabricating silicon anode laminates, which improves rheological properties of slurries toward high-quality electrode laminates. However, the significantly increased basicity causes degradation of Si particles while the irreversible conversion of carboxylic acid groups to lithium carboxylates undermines the binding strength, collectively leading to adverse cycling performance of the fabricated Si anodes. Herein, a novel neutralization process for PAA binders is developed. A weak base, ammonia (NH 3 ), was discovered as a neutralizing agent that still promotes rheological response of binder solutions but results in a reduced pH increase. Interestingly, the resulting ammonium carboxylate groups may cleave during the drying process to restore the neutralized PAA (PAA-NH 3 ) binders to their pristine states. The best-performing composition of 50% neutralization (PAA-50%NH 3 ) provides comparable rheological response as a PAA-Li binder as well as much improved cycling performance. Additionally, the half-cells using the PAA-50%NH 3 binder can deliver 60% capacity retention over 100 cycles at C/3 rate, affording a 23.8% increase compared to PAA-Li half-cells. This restorable neutralization process of PAA binders represents an innovative strategy of mitigating issues from slurry processing of Si particles to achieve concurrent improvements in high-quality lamination and cycling performance.
25 ENERGY STORAGE↗
Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
The processing and extraction of critical metals from black mass is important to battery recycling. Separation and recovery of critical metals (Co, Ni, Li, and Mn) from other metal impurities must yield purified metal salts, while avoiding substantial losses of critical metals. Solvent extraction in batch experiments were conducted using mixed metal sulphates obtained from the leach liquor obtained from spent and shredded lithium-ion batteries. Selective extraction of Mn 2+ , Fe 3+ , Al 3+ and Cu 2+ from simulated and real leached mixed metals solution was carried out using di-2-ethylhexylphophoric acid (D2EPHA) and Cyanex-272 at varying pH. Further experiments with the preferred extractant (D2EPHA) were performed under different conditions: changing the concentration of extractant, organic to aqueous ratio, and varying the diluents. At optimum conditions (40% v/v D2EPHA in kerosene, pH 2.5, O:A = 1:1, 25 °C, and 20 min), 85% Mn 2+ , 98% Al 3+ , 100% Fe 3+ , and 43% Cu 2+ were extracted with losses of only trace amounts (<5.0%) of Co 2+ , Ni 2+ , and Li + . The order of extraction efficiency for the diluents was found to be kerosene > Exxal-10 >>> dichloromethane (CH 2 Cl 2 ) > toluene. Four stages of stripping of metals loaded on D2EPHA were performed as co-extracted metal impurities were selectively stripped, and a purified MnSO 4 solution was produced. Spent extractant was regenerated after Fe 3+ and Al 3+ were completely stripped using 1.0 M oxalic acid (C 2 H 2 O 4 ).
25 ENERGY STORAGE↗
Highly Ordered Carbon Coating Prepared with Polyvinylidene Chloride Precursor for High‐Performance Silicon Anodes in Lithium‐Ion Batteries
Abstract A highly ordered carbon structure based on polyvinylidene chloride precursor has been developed to host silicon nanoparticles. The stoichiometric ratio of sacrificial H and Cl elements facilitated full utilization of the carbon content of the precursor that produced robust carbon coatings on silicon nanoparticles with excellent mechanic properties and electrochemical stabilities. The optimal sintering temperature and carbon content have been investigated. When evaluated as the anode of a lithium‐ion battery (LIB), the Si : C 1 : 2 composite sintered at 800 °C (SiC12‐800) provided excellent capacity retention of 85 % at 0.1 C after 50 cycles with an enhanced CE, which reached 99 % only after 10 cycles. The SiC12‐800 electrode maintained a specific capacity of 709.2 mAh/g after 300 cycles at 0.3 C, and delivered a high rate performance of 737.9 mAh/g and 485.6 mAh/g at 5 C and 10 C, respectively. The results indicate that polymer precursors with stoichiometric ratio of sacrificial elements have high potential for generating highly robust carbon coatings for silicon anodes in high energy density LIBs.
Zhou, Shuo↗
Unlocking the self-supported thermal runaway of high-energy lithium-ion batteries
Layered Ni-rich LiNi x Mn y Co 1-x-y O 2 (NMC) materials are the most promising cathode materials for Li-ion batteries due to their favorable energy densities. However, the low thermal stability typically caused by detrimental oxygen release leads to significant safety concerns. Determining the pathways of oxygen evolution reaction is essential, as the ideal safety countermeasure is to break the reaction chain of thermal runaway. In this study, we demonstrate that two endogenous pathways of oxygen involved in strong exothermic reactions lead the NMC811|graphite pouch cell to an uncontrollable state, and we quantify the individual contribution of the pathways to thermal runaway. Approximately 41% of thermal-induced oxygen reacts aggressively with ethylene carbonate (EC) at the cathode/electrolyte interface with 16% heat generation, accelerating the self-heating rate and thereby further triggering thermal runaway. The residual oxygen that survives the reaction with carbonate spreads to the lithiated anode with major heat generation (65%), bringing the battery to the maximum destructive temperature during thermal runaway. By confirming the significant roles of EC and anode, a deeper understanding on battery fire was achieved. Finally, the revealed mechanism can help guide studies on stopping the two reaction pathways, allowing for the safer use of high-energy lithium-ion batteries in the future.
25 ENERGY STORAGE↗
Toward the Practical Use of Cobalt-Free Lithium-Ion Batteries by an Advanced Ether-Based Electrolyte
The criticality of cobalt (Co) has been motivating the quest for Co-free positive electrode materials for building lithium (Li)-ion batteries. However, the Co-free positive electrode materials usually suffer from relatively fast capacity decay when coupled with conventional LiPF 6 -organocarbonates electrolytes. To address this issue, a 1,2-dimethoxyethane (DME) based localized high concentration electrolyte (LHCE) was developed and evaluated in a Co-free Li-ion cell chemistry (Graphite||LiNi 0.96 Mg 0.02 Ti 0.02 O 2 ). Extraordinary capacity retentions were achieved with the LHCE in coin cells (95.3%), single layer pouch cells (79.4%) and high capacity loading double layer pouch cells (70.9 %) after being operated within the voltage range of 2.5-4.4 V for 500 charge/discharge cycles. The capacity retentions of counterpart cells using LiPF6 based conventional electrolyte only reached 61.1%, 57.2% and 59.8%, respectively. Mechanistic studies reveal that the superior electrode/electrolyte interphases formed by the LHCE and the intrinsic chemical stability of the LHCE account for the excellent electrochemical performance in the Co-free Li-ion cells.
25 ENERGY STORAGE↗
Lithium-Ion Battery Diagnostics Using Electrochemical Impedance via Machine-Learning
Diagnosing battery states such as health, state-of-charge, or temperature is crucial for ensuring the safety and reliability of electrochemical energy storage systems. While some states, such as temperature, may be measured using cheap sensors, accurate diagnosis of battery health metrics usually requires time-consuming performance measurements, making them infeasible for use in real-world operation. These health metrics can be measured during lab-testing and then estimated on-line using predictive life models or via state observer algorithms such as Kalman filters, but these predictive methods should be supplemented by actual measurement of battery health whenever possible to ensure reliability. Rapid measurement of battery health may be done by various types of fast diagnostic techniques such as electrochemical impedance spectroscopy (EIS), which can be performed in only a few minutes and require only a fraction of the energy and power needed for a full charge and discharge measurement. But there is a substantial challenge for estimating battery health using EIS data, as EIS is sensitive to cell temperature, state-of-charge, current, and resting time in addition to health. Thus, utilizing EIS data to predict battery capacity requires correcting for all these additional variables, a task that is extremely difficult to handle analytically. This talk utilizes machine-learning methods to estimate the effectiveness of battery capacity prediction from EIS data, leveraging a data set of hundreds of EIS measurements recorded at varying temperature and state-of-charge throughout a 500-day aging study of 32 commercial, large-format NMC-Graphite lithium-ion batteries. Using EIS as input to machine-learning models is complicated by the nonlinear response of impedance to battery health, temperature, and state-of-charge, as well as the collinearity between the impedance response at neighboring frequencies, which can easily lead to overfit models. To train robust models, features from EIS data need to be extracted from the data or some subset of critical frequencies selected. Many approaches for extracting and selecting features from EIS data from electrochemical analysis and machine-learning fields were identified for analysis: using the entire raw spectra; selection of one, two, or many frequencies from the entire spectra; selecting interesting points from the EIS measurement using domain knowledge; fitting EIS with an equivalent-circuit model; calculating statistics on the raw impedance values; and reducing the dimensionality of the data using unsupervised linear (principal component analysis) and non-linear (uniform manifold approximation and projection) methods. These approaches were rigorously compared using a machine-learning pipeline approach, training linear, Gaussian process, and random forest regression models and quantifying performance using cross-validation as well as a held-out test set. An artificial neural network model trained on the raw spectra was also tested. Promising pipelines were fine-tuned via Bayesian hyperparameter optimization using cross-validation loss and training with class-specific weights to counter data set imbalance. The most reliable method for utilizing impedance in this work was the selection of two optimal frequencies through an exhaustive search, resulting in about 2% mean absolute error on test data for both Gaussian process and random forest model architectures. Interrogation of a variety of models reveals critical frequencies of 100 Hz and 103 Hz for this data set, though the optimal set of frequencies is not necessarily intuitive, i.e., the best performing models are not simply those that use impedance at frequencies that have the highest correlation to the relative discharge capacity. The best performing model is an ensemble model, which is able to predict battery capacity with 1.9% mean absolute error for unseen cells using impedance recorded at a variety of temperatures and states-of-charge.
battery↗
Hydrometallurgical Recycling of Black Mass of Spent Lithium-Ion Batteries Using Methanesulfonic Acid: Leaching, Kinetic Studies, and Potential for Total Recovery of Valuable Components
Methanesulfonic acid (MSA) exhibits several advantageous properties rendering it a promising candidate for circular hydrometallurgical processes. These properties include a high acidity (pKa = - 1.9) comparable to that of classical mineral acids as well as biodegradability, high stability, and high solubility of metal-MSA complexes in aqueous solutions. In this study, MSA was employed as a lixiviant for the leaching of metals (lithium, nickel, cobalt, and manganese) from the black mass of spent lithium-ion batteries (LIBs). The effect of various parameters, including MSA concentration, H 2 O 2 concentration, temperature, and pulp density, was systematically investigated. Under the optimized conditions (1.5 M MSA, 0.2 M H 2 O 2 , 60 °C, and 50 g/L pulp density), quantitative leaching of lithium was achieved within 30 min, while for nickel and cobalt it was after 2 h, and 4 h for manganese leaching. The leaching kinetics of Li, Ni, Co, and Mn were studies using the shrinking particle models (SPM) and the Avrami model. The results indicated that the Avrami model provided the best fit to the kinetic data, with apparent activation energies of 46.81 kJ/mol for Li, 58.61 kJ/mol for Ni, 59.69 kJ/mol for Co, and 58.86 kJ/mol for Mn, within the temperature range of 25-70 °C (except for Li, which was analyzed in the range of 25-60 °C), consistent with chemical reaction control. Subsequently, residual contaminants in the leaching residue were eliminated through pyrolysis. The quantitative leaching of metals in MSA solution (a green lixiviant), combined with the pyrolytic treatment of leaching residues, represents a circular strategy for the total recovery of valuable components from the black mass of spent LIBs.
25 ENERGY STORAGE↗
Lithiated and passivated lithium ion battery anodes
An electrode material includes a lithium active material composition. The lithium active material composition includes lithium and an active anode material. The lithium active material composition is coated with a lithium ion conducting passivating material, such that the electrode material is lithiated and pre-passivated. An electrode and a battery are also disclosed. Methods of making an electrode material, electrode and battery that are lithiated and pre-passivated are also disclosed.
Sacci, Robert L.↗
International Space Station Lithium-Ion Battery Status
When originally launched, the International Space Station (ISS) primary Electric Power System (EPS) used Nickel-Hydrogen (Ni-H2) batteries to store electrical energy. The electricity for the space station is generated by its solar arrays, which charge batteries during insolation for subsequent discharge during eclipse. The Ni-H2 batteries were designed to operate for ten years at a 35 percent depth of discharge (DOD) maximum during normal operation in a Low Earth Orbit. For service beyond that period, upgraded Li-Ion Orbital Replacement Units (ORUs) were designed. These are the largest Li-Ion batteries ever utilized for a human rated spacecraft. With the oldest 12 Ni-H2 battery ORUs cycling since September 2006, the first set of six was replaced by Li-Ion batteries in December 2016; the second set of six is planned for replacement in September 2018. This paper will include an overview of the ISS Li-Ion battery system architecture, on-orbit status of the first 6 batteries, start up of the second 6 batteries, and the status of the Li-Ion cell and ORU life cycle testing.
International Space Station↗
Chasing protons in lithium-ion batteries
Parasitic reactions between delithiated cathode materials and non-aqueous electrolytes have been a major barrier that limits the upper cutoff potential of cathode materials. It is of great importance to suppress such parasitic reactions to unleash the high-energy-density potential of high voltage cathode materials. Although major effort has been made to identify the chemical composition of the cathode electrolyte interface using various cutting edge characterization tools, the chemical nature of parasitic reactions remains a puzzle. This severely hinders the rational development of stable high voltage cathode/electrolyte pairs for high-energy density lithium-ion batteries. This report highlights our latest effort in understanding the chemical/electrochemical role of the cathode electrolyte interface using protons as a chemical tracer for parasitic reactions.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Gradient porosity electrodes for fast charging lithium-ion batteries
The tendency of Li plating at the surface of thick graphite electrodes greatly limits their application in electrical vehicle (EV) batteries for fast charging applications. To address this concern, we proposed an innovative gradient porosity architecture to facilitate mass transport and suppress Li plating in the thick anodes for fast charging applications. This concept was approved through a thick 3-layered graphite electrode with the highest porosity in the top layer and the lowest porosity in the bottom layer, in contact with the current collector. Here, the gradient porosity structure in the 3-layered graphite electrodes was confirmed by electron microscopy and mercury porosimetry measurements. Used as the anodes of lithium-ion batteries, 3-layered graphite electrodes demonstrated unprecedentedly rate capability and durability superior to 1-layered electrodes. The post-mortem analysis on the cycled cells shows that 3-layered electrodes can significantly suppress Li plating at a high rate up to 4C, which might be responsible for the improved performance of the derived cells. The excellent electrochemical behaviors of 3-layered graphite electrodes are associated with the favored mass transport originating from the unique gradient porosity structure. This is consistent with theoretical studies showing that gradient porosity lowers the Li-ion concentration gradient in the electrolyte in the region close to the separator and slows down the process of reaching the Li plating threshold.
25 ENERGY STORAGE↗
Nanostructured Block Polymer Electrolytes: Tailoring Self-Assembly to Unlock the Potential in Lithium-Ion Batteries
Ion-containing solid block polymer (BP) electrolytes can self-assemble into microphase-separated domains to facilitate the independent optimization of ion conduction and mechanical stability; this assembly behavior has the potential to improve the functionality and safety of lithium-ion batteries over liquid electrolytes to meet future demands (e.g., large capacities and long lifetimes) in various applications. However, significant enhancements in the ionic conductivity and processability of BPs must be realized for BP-based electrolytes to become robust alternatives in commercial devices. Toward this end, the controlled modification of BP electrolytes’ intra-domain (nanometer-scale) and multi-grain (micrometer-scale) structure is one viable approach; intra-domain ion transport and segmental compatibility (related to the effective Flory–Huggins parameter, χ eff ) can be increased by tuning the ion and monomer-segment distributions, and the morphology can be selected such that the multi-grain transport is less sensitive to grain size and orientation.
25 ENERGY STORAGE↗
Stable fluorinated alkylated lithium malonatoborate salts for lithium-ion battery applications
The invention is directed in a first aspect to electrolyte salt of the general formula Li+Z−, wherein Z− has the following chemical formula: wherein R1 is an alkyl group (R′) containing at least one and up to twelve carbon atoms, and R2 and R3 are independently selected from fluorine atom, hydrocarbon groups R, alkoxy groups (—OR), and ester groups —OC(O)R, wherein R2 and R3 can optionally interconnect via R functionalities to form a boron-containing ring. The invention is also directed to electrolyte compositions in which the above electrolyte salt is incorporated. The invention is further directed to lithium-ion batteries containing these electrolytes.
Sun, Xiao-Guang↗
Surpassing the Organic Cathode Performance for Lithium-Ion Batteries with Robust Fluorinated Covalent Quinazoline Networks
Organic electrode materials have promising application prospects in energy storage, but issues including rapid capacity fading and poor power capacity restrict their practical applications. In this study, nanoporous fluorinated covalent quinazoline networks (F-CQNs) were constructed by condensation of fluorinated aromatic aminonitrile precursors via an ionothermal pathway. Precise control of the reaction parameters afforded F-CQN-1-600 material featuring high surface area, permanent porosity, high nitrogen content (23.49 wt %), extended π-conjugated architecture, layered structure, and bipolar combination of benzene and tricycloquinazoline. Synergy among these unique properties leads to a good performance as a cathode source for lithium-ion batteries (LIBs) in terms of high capacity (250 mA h g –1 at 0.1 A g –1 ), high rate capability (105 mA h g –1 at 5.0 A g –1 ), and impressive cycling stability (95.8% retention rate after 2000 cycles at 2.0 A g –1 together with a high Coulombic efficiency of 99.95%), surpassing most of the previous organic cathode counterparts.
25 ENERGY STORAGE↗
Controlling MoO 2 and MoO 3 phases in MoO x /CNTs nanocomposites and their application to anode materials for lithium-ion batteries and capacitors
Molybdenum oxides (MoO 2 and MoO 3 ) are attractive anode materials for Li- and Na- ion batteries. Although there have been extensive studies on them individually, systematic and comparative studies are still lacking. Here, we demonstrate a facile and straightforward synthesis method to control the phase and oxidation state in the MoO x /CNTs nanocomposites via hydrothermal reaction followed by heat-treatment. By changing the gas atmosphere during the annealing process, well-dispersed MoO 2 /CNTs and MoO 3 /CNTs nanocomposites are formed without altering their overall morphology. This strategy enables us to investigate the true structure-property correlation of MoO x /CNTs nanocomposites by comparing the structure and electrochemical properties of MoO 2 /CNTs and MoO 3 /CNTs. When tested as anode materials for lithium-ion batteries, both HT-MoO 2&3 /CNTs electrodes show much-improved cycling stability and rate performance compared to the rod-shaped bulk MoO 3 electrode. In situ Mo K-edge x-ray absorption spectroscopy (XAS) has been further employed to compare and elucidate Li + storage mechanisms of both electrodes. When employed to the negative electrode of a high-power lithium-ion capacitor (LIC), the LIC full-cell composed of HT-MoO 3 /CNTs negative and activated carbon positive electrodes demonstrates impressive energy and power densities (~ 90 Wh kg –1 with 2000 W kg –1 ) and excellent cycling stability (96.8 % capacity retention after 300 cycles), revealing the versatility of the MoO x /CNTs electrodes in energy applications.
25 ENERGY STORAGE↗