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The growing demand for lithium-ion batteries (LIBs) has led to an urgent need for sustainable recycling strategies for spent cathode materials. In this study, a mechanochemical approach was developed for the recovery of lithium and cobalt from end-of-life LiCoO2 cathodes using high-energy ball milling. For the first time, aluminum and carbon were employed as internal reducing agents, facilitating the in situ decomposition of LiCoO2 into CoO, Li2O, and metallic Co. X-ray diffraction analysis confirmed significant structural disorder, phase transitions, and the formation of CoO, AlCo, and spinel-like CoAl2O4. The Taguchi method was applied to optimize milling parameters, identifying 800 rpm, 60 min, and a ball-to-powder ratio of 50:1 as the most effective conditions for structural activation. Subsequent ammonia leaching under fixed conditions (3.0 M NH3·H2O, 1.0 M (NH4)2CO3, 60 °C, 25 mL/g, 6 h) demonstrated high recovery efficiencies: up to 94.6% for lithium and 83.7% for cobalt in the best-performing samples. These results highlight the synergistic benefits of mechanical activation and reductant-assisted phase engineering for enhancing metal recovery. The proposed method offers a simple, scalable, and eco-friendly route for the hydrometallurgical recycling of LIB cathodes without requiring extensive chemical pretreatment.

The advancement and implementation of silicon anode materials are significantly impeded by the considerable volume effect. In this work, lithium oxide (Li 2 O) was deposited in conjunction with silicon by magnetron co-sputtering, with the objective of optimizing the electrochemical performance of the Si anode. During the deposition process, a portion of the silicon is oxidized to SiO x with a lower volume effect. Furthermore, irreversible products, including lithium silicates and lithium oxide, are formed on the surface of the material during the lithiation process, which serve as a protective layer to mitigate the volume effect of the Si anode. Concurrently, the pre-lithiation effect of Li 2 O can also enhance its cycling stability. The composite anode prepared by co-sputtering exhibited an initial specific capacity of 2357 mAh g −1 and a capacity retention of 88.41% after 100 cycles at 0.5 C (significantly higher than the capacity retention of 60.68% for the pure Si anode). Moreover, the material showed a rate capacity of 1300 mAh g −1 at 5 C with a good capacity recovery. This study demonstrates that the advanced incorporation of Li 2 O into the Si anode by magnetron co-sputtering can effectively enhance its cycling stability while simultaneously providing an effective and feasible method for mitigating the volume effect of Si-based materials.

The change in the composition of the electrolyte after life cycle testing (cycling) of lithium-ion batteries (LIBs) was studied. The cell with a nominal capacity of 22 A h was composed of a cathode based on nickel-rich layered lithium oxide LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) and an anode based on graphite. NMR and high-resolution mass spectrometry demonstrated the continuous decomposition of dimethyl carbonate and ethyl methyl carbonate, related to the disruption of the formation of protective surface layers on the graphite electrode. The degradation of the LIB is related to the formation of polyethylene oxide oligomers of various compositions as a result of the decomposition of the electrolyte components and the precipitation of the salt MeOCO 2 Li, which is poorly soluble in carbonate solvents, on the separator. A water content of more than 20 ppm in the electrolyte leads to the hydrolysis of the salt LiPF 6 with the formation of HPO 2 F 2 and HF. The presence of HF facilitates the dissolution of the components of the surface film at the graphite/electrolyte interface with the regeneration of H 2 O and the formation of a “fresh” surface on the graphite, which participates in the electrochemical decomposition of the carbonate solvents. Organophosphate C 2 H 5 O 4 P is formed upon the interaction of the electrolyte components with HF.

This paper reports on a new approach to chlorinating molten salts using vaporized NH 4 Cl. In separate experiments, chlorination of dissolved Li 2 O and submerged U metal was demonstrated. Ammonium chloride was thermally decomposed in a quartz glass vaporization chamber with an internal temperature ranging from 295 to 384 °C. These decomposition products were then bubbled into eutectic LiCl–KCl salt via argon carrier gas. The vapor appears to absorb as NH 4 + /Cl − into the molten LiCl–KCl based on the high dissolved concentration of acid compared literature reported solubility of HCl. In Li 2 O chlorination experiments, complete reaction was achieved starting with 1 wt% Li 2 O for reaction times of 24.8 h or less. In U metal chlorination experiments, dissolved U concentrations ranged from 1.75 to 4.17 wt% for reaction times ranging from 3.5 to 21.6 h. The rate limiting step is mass transfer and reaction between the molten salt and U metal pellet. Cyclic voltammetry peak heights were correlated with dissolved U concentration with overall scan results consistent with UCl 3 being the dominant form of dissolved U.

A novel process to recover lithium and manganese oxides from a cathode material (LiMn2O4) of spent lithium-ion battery was attempted using thermal reaction with hydrogen gas at elevated temperatures. A hydrogen gas as a reducing agent was used with LiMn2O4 powder and it was found that separation of Li2O and MnO was taken place at 1050°C. The powder after thermal process was washed away with distilled water and only lithium was dissolved in the water and manganese oxide powder left behind. It was noted that manganese oxide powder was found to be 98.20 wt.% and the lithium content in the solution was 1,928 ppm, respectively.

The literature indicates that utilizing pyrometallurgical methods for processing spent LiCoO2 (LCO) batteries can lead to cobalt recovery in the forms of Co3O4, CoO, and Co, while lithium can be retrieved as Li2O or Li2CO3. However, the technology’s high energy consumption has also been noted as a challenge in this recovery process. Recently, an innovative and sustainable approach using microwave (MW) radiation has been proposed as an alternative to traditional pyrometallurgical methods for treating used lithium-ion batteries (LiBs). This method aims to address the shortcomings of the conventional approach. In this study, the treatment of the black mass (BM) from spent LCO batteries is explored for the first time using MW–materials interaction under an air atmosphere. The research reveals that the process can trigger carbothermic reactions. However, MW makes the BM so reactive that it causes rapid heating of the sample in a few minutes, also posing a fire risk. This paper presents and discusses the benefits and potential hazards associated with this novel technology for the recovery of spent LCO batteries and gives information about real samples of BM. The work opens the possibility of using a microwave for raw material recovery in spent LIBs, allowing to obtain rapid and more efficient reactions.

Li2ZrO3-coated and Al-doped micro-sized monocrystalline LiMn2O4 powder is synthesized through solid-state reaction, and the electrochemical performance is investigated as cathode materials for lithium-ion batteries. It is found that Li2ZrO3-coated LiAl0.06Mn1.94O4 delivers a discharge capacity of 110.90 mAhg−1 with 94% capacity retention after 200 cycles at room temperature and a discharge capacity of 104.4 mAhg−1 with a capacity retention of 87.8% after 100 cycles at 55 °C. Moreover, Li2ZrO3-coated LiAl0.06Mn1.94O4 could retain 87.5% of its initial capacity at 5C rate. This superior cycling and rate performance can be greatly contributed to the synergistic effect of Al-doping and Li2ZrO3-coating.

The effect of lithium Oxide content on the characteristics and mechanical property of willemite (2ZnO.SiO2) under a heating condition in Na2O-K2O-Li2O-CaO-(ZnO)-Al2O3-SiO2 glazing system used in stoneware, sintered at a maximum at temperature 1250 °C by a heating rate of 2.6 °C/min for 8 hours is the firing process of the glazes and clay to melt. After 15 minutes, the temperature dropped to 1100 °C for 40 minutes was stimulated crystallization and soaked in kiln at 1100 °C for 4 hours. This result was consistent with the chemical compositions from the XRF technique indicated that the glaze comprised ZnO and SiO2 were the main compositions and compared to the mineral composition after sintering of the glazed crystal which revealed 2ZnO.SiO2 as the main component and the result from the XRD technique. The microstructure of the glazed crystals after sintering was needle shaped and had spherical growth. The analytical results from Vickers hardness technique showed that microhardness by adding 3-5 % of Li2O of the glazes S1, S2, S3, S4 and S5 as 105.96 ± 4.58, 112.30 ± 9.95, 153.90 ± 7.29, 244.80 ± 5.42 and 382.62 ± 9.20, respectively. More willemite crystals in the glaze results in more strength of the glaze as well.

Open circuit voltage (OCV) of lithium batteries has been of interest since the battery management system (BMS) requires an accurate knowledge of the voltage characteristics of any Li-ion batteries. This article presents an OCV characteristic for lithium manganese oxide (LMO) batteries under several experimental operating conditions, and discusses factors for accurate OCV determination. A test system is developed for OCV characterization based on the OCV pulse test method. Various factors for the OCV behavior, such as resting period, step-size of the pulse test, testing current amplitude, hysteresis phenomena, and terminal voltage relationship, are investigated and evaluated. To this end, a general OCV model based on state of charge (SOC) tracking is developed and validated with satisfactory results.

Ordered layered structures serve as essential components in lithium (Li)-ion cathodes 1 – 3 . However, on charging, the inherently delicate Li-deficient frameworks become vulnerable to lattice strain and structural and/or chemo-mechanical degradation, resulting in rapid capacity deterioration and thus short battery life 2 , 4 . Here we report an approach that addresses these issues using the integration of chemical short-range disorder (CSRD) into oxide cathodes, which involves the localized distribution of elements in a crystalline lattice over spatial dimensions, spanning a few nearest-neighbour spacings. This is guided by fundamental principles of structural chemistry and achieved through an improved ceramic synthesis process. To demonstrate its viability, we showcase how the introduction of CSRD substantially affects the crystal structure of layered Li cobalt oxide cathodes. This is manifested in the transition metal environment and its interactions with oxygen, effectively preventing detrimental sliding of crystal slabs and structural deterioration during Li removal. Meanwhile, it affects the electronic structure, leading to improved electronic conductivity. These attributes are highly beneficial for Li-ion storage capabilities, markedly improving cycle life and rate capability. Moreover, we find that CSRD can be introduced in additional layered oxide materials through improved chemical co-doping, further illustrating its potential to enhance structural and electrochemical stability. These findings open up new avenues for the design of oxide cathodes, offering insights into the effects of CSRD on the crystal and electronic structure of advanced functional materials. The introduction of chemical short-range disorder substantially affects the crystal structure of layered lithium oxide cathodes, leading to improved charge transfer and structural stability.