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<p>Direct regeneration of spent cathode materials offers a promising alternative to conventional lithium-ion battery recycling routes that rely on metal separation and re-synthesis. In this work, a precipitation-free direct regeneration strategy based on a citric acid/ethylene glycol (CA/EG) deep eutectic solvent (DES) is developed for recovering LiCoO<sub>2</sub> (LCO) cathodes from spent lithium-ion batteries. The DES system enables efficient leaching, stoichiometric replenishment, and structural reconstruction of LCO in a single process, eliminating the need for lithium-cobalt separation. Structural and surface analyses using XRD, Rietveld refinement, SEM, and XPS confirm that the regenerated LCO exhibits a well-restored layered structure, reduced Co²⁺ content, suppressed cation mixing, and refined nanoscale particle morphology. Electrochemical evaluations under a high cutoff voltage of 4.6&#xa0;V demonstrate significantly improved performance, with regenerated LCO delivering an initial discharge capacity of 199.4 mAh·g<sup>− 1</sup> at 0.1&#xa0;C and enhanced rate capability compared to spent material. Mg-assisted regeneration further enhances structural stability, achieving an initial capacity of 179.5 mAh·g<sup>− 1</sup> and suppressing irreversible phase transitions during prolonged cycling. After 100 cycles at 1&#xa0;C, capacity retentions of 87.6% and 83.2% are obtained for regenerated LCO with and without Mg doping, respectively. Compared with conventional inorganic acid-based recycling processes, the proposed DES-based approach is environmentally benign, precipitation-free, and process-efficient. This work demonstrates a sustainable and scalable pathway for the direct regeneration and upcycling of spent LiCoO<sub>2</sub> cathodes, providing a viable solution for next-generation lithium-ion battery recycling.</p>

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Precipitation-free direct regeneration of LiCoO2 cathodes from spent lithium-ion batteries via a deep eutectic solvent process

  • 期刊论文

  • 发表日期：

    2026年5月20日

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  • Hao-Jie Zhang,
  • Ki-Tae Lee

摘要

Direct regeneration of spent cathode materials offers a promising alternative to conventional lithium-ion battery recycling routes that rely on metal separation and re-synthesis. In this work, a precipitation-free direct regeneration strategy based on a citric acid/ethylene glycol (CA/EG) deep eutectic solvent (DES) is developed for recovering LiCoO2 (LCO) cathodes from spent lithium-ion batteries. The DES system enables efficient leaching, stoichiometric replenishment, and structural reconstruction of LCO in a single process, eliminating the need for lithium-cobalt separation. Structural and surface analyses using XRD, Rietveld refinement, SEM, and XPS confirm that the regenerated LCO exhibits a well-restored layered structure, reduced Co²⁺ content, suppressed cation mixing, and refined nanoscale particle morphology. Electrochemical evaluations under a high cutoff voltage of 4.6 V demonstrate significantly improved performance, with regenerated LCO delivering an initial discharge capacity of 199.4 mAh·g− 1 at 0.1 C and enhanced rate capability compared to spent material. Mg-assisted regeneration further enhances structural stability, achieving an initial capacity of 179.5 mAh·g− 1 and suppressing irreversible phase transitions during prolonged cycling. After 100 cycles at 1 C, capacity retentions of 87.6% and 83.2% are obtained for regenerated LCO with and without Mg doping, respectively. Compared with conventional inorganic acid-based recycling processes, the proposed DES-based approach is environmentally benign, precipitation-free, and process-efficient. This work demonstrates a sustainable and scalable pathway for the direct regeneration and upcycling of spent LiCoO2 cathodes, providing a viable solution for next-generation lithium-ion battery recycling.