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Regeneration of LiNi1/3Co1/3Mn1/3O2 Cathode Active Materials from End-of-Life Lithium-Ion Batteries through Ascorbic Acid Leaching and Oxalic Acid Coprecipitation Processes

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    Research Article

    Regeneration of LiNi1/3Co1/3Mn1/3O2 Cathode Active Materials from End-of-Life Lithium-Ion Batteries through Ascorbic Acid Leaching and Oxalic Acid Coprecipitation Processes
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    • Septia Refly
      Septia Refly
      Department of Physics, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      More by Septia Refly
    • Octia Floweri
      Octia Floweri
      Research Center for Nanosciences and Nanotechnology, Institut Teknologi Bandung, Jl. Ganesha 10 Bandung 40132, Indonesia
      More by Octia Floweri
    • Tirta R. Mayangsari
      Tirta R. Mayangsari
      Department of Chemistry, Universitas Pertamina, Jl. Teuku Nyak Arief, Simprug, Jakarta 12220, Indonesia
      More by Tirta R. Mayangsari
    • Afriyanti Sumboja
      Afriyanti Sumboja
      Material Science and Engineering Research Group, Faculty of Mechanical and Aerospace Engineering, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      National Center for Sustainable Transportation Technology, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      More by Afriyanti Sumboja
      Orcidhttp://orcid.org/0000-0002-7389-4442
    • Sigit Puji Santosa
      Sigit Puji Santosa
      National Center for Sustainable Transportation Technology, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      Light-weight Structures Research Group, Faculty of Mechanical and Aerospace Engineering, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      More by Sigit Puji Santosa
    • Takashi Ogi
      Takashi Ogi
      Chemical Engineering Program, Graduate School of Advanced Science and Engineering, Hiroshima University, Hiroshima 739-8527, Japan
      More by Takashi Ogi
      Orcidhttp://orcid.org/0000-0003-3982-857X
    • Ferry Iskandar*
      Ferry Iskandar
      Department of Physics, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      Research Center for Nanosciences and Nanotechnology, Institut Teknologi Bandung, Jl. Ganesha 10 Bandung 40132, Indonesia
      National Center for Sustainable Transportation Technology, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
      *Email: [email protected]
      More by Ferry Iskandar
      Orcidhttp://orcid.org/0000-0002-0464-0035
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    ACS Sustainable Chemistry & Engineering

    Cite this: ACS Sustainable Chem. Eng. 2020, 8, 43, 16104–16114
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    https://doi.org/10.1021/acssuschemeng.0c01006
    Published October 22, 2020
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    Abstract

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    One of the emerging issues in solving the electronic waste problem is to address the growing amount of end-of-life Li-ion battery (LIB) waste. In this work, the regeneration of LiNi1/3Co1/3Mn1/3O2 (NCM 111) cathode active materials from end-of-life LIBs was successfully carried out via an easy, fast, and environmentally friendly recycling process that comprised three main stages, i.e., ascorbic acid leaching, oxalate coprecipitation process, and heat treatment. Ascorbic acid was able to leach Li, Ni, Co, and Mn ions from the spent NCM 111 cathode material with a relatively high leaching efficiency up to 90%. The following oxalic acid coprecipitation method has effectively recovered the transition metal ions in the leachate in the form of the metal oxalates MC2O4·2H2O (M = Ni, Mn, and Co), as confirmed by the result of X-ray diffraction characterization. The quantitative analysis of metal ions using X-ray fluorescence revealed that the ratio of Ni, Co, and Mn in the precipitate was approximately 1:1:1, with a slightly lower amount of Mn. Regeneration of NCM 111 via the heat treatment of metal oxalates at temperatures of 800–950 °C successfully reproduced the material (R-NCM) with an R3m hexagonal-layered structure, which could be reemployed as the cathode in LIBs. Charge–discharge characterization of the as-fabricated LIB at 2.5–4.3 V revealed that the battery with the R-NCM cathode synthesized at 900 °C exhibited a slightly higher initial specific discharge capacity (164.9 mAh/g at 0.2 C) than that of commercial NCM (157.4 mAh/g at 0.2 C). Moreover, the Li-ion battery also showed a very stable performance with a capacity retention of 91.3% after 100 cycles at 0.2 C.

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    • Pretreatment and characterization of spent LIBs (S1). X-ray diffraction pattern of the cathode samples before regeneration (Figure S1). The relation between the discharge capacity with I(003)/I(104) and Rct in R-NCM cathode materials synthesized at 800–950 °C (Figure S2). Linear fitting of Z′ vs ω-1/2 for R-NCM cathode materials synthesized at 800–950 °C (Figure S3). SEM image and X-ray diffraction pattern of the regenerated NCM with adjusted composition (aR-NCM 900) (Figure S4). Quantitative analysis results of metal elements in the S-NCM cathodes in atomic percent (Table S1). Warburg coefficient of R-NCM cathode materials prepared by heat treatment at 800–950 °C (Table S2). Lattice parameter of regenerated NCM with adjusted composition (aR-NCM 900) (Table S3). Mass balance analysis of Ni, Co, and Mn recoveries in the regeneration process of NCM cathode materials (Table S4). The equation for calculation of ionic diffusivity (Equation S1) (PDF)

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    Cite this: ACS Sustainable Chem. Eng. 2020, 8, 43, 16104–16114
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