Classification of spent Li-ion batteries based on ICP-OES/X-ray characterization of the cathode materials

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Dragana V. Medić
Snežana S. Milić
Slađana Č. Alagić
Ivan N. Đorđević
Silvana B. Dimitrijević


Development of lithium-ion batteries (LIBs) during the latest decades resulted in improved performances of the new integrated cathode materials and in their wide applications. This rapid expansion of new materials led to the intensive replacement of the old-fashioned, traditional materials and increased a simultaneous accumulation of both kinds of materials at extremely hazardous electronic waste sites, which additionally increased an urgent need for their recycling. Most importantly, in this way, spent LIBs may further serve as a significant source of valuable metals such as Li and cobalt. However, one of the key problems in LIBs recycling is the absence of a precise battery classification/sorting based on the chemical composition of the used cathode material. In this paper, characterization of the cathode material was performed regarding chemical composition of 40 samples of spent LIBs using inductively coupled plasma - optical emission spectrometry and X-ray diffraction. Preparation of the samples, (pretreatment) included: discharging, dismantling, separation of the main components (cathode, anode and the separator), and detachment of the cathode material from the aluminium foil. The obtained results showed that, in the investigated commercially available LIBs, lithium cobalt oxide was the most frequently used (cathode) material.


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Medić, D. V., Milić, S. S., Alagić, S. Č., Đorđević, I. N., & Dimitrijević, S. B. (2020). Classification of spent Li-ion batteries based on ICP-OES/X-ray characterization of the cathode materials. HEMIJSKA INDUSTRIJA (Chemical Industry), 74(3), 221–230.
Environmental Engineering - Solid Waste Treatment


Yoshio M, Kozawa A, Brodd RJ. Intoduction: Development of Lithium-Ion Batteries. In: Yoshio M, Brodd RJ, Kozawa A, ed. Lithium-Ion Batteries. 1sted. New York, NY: Springer Science+Business Media; 2009: 15–24.

Pegorettia VCB, Dixinia PVM, Smecellatoc PC, Biaggioc SR, Freitasa MBJG. Thermal synthesis, characterization and electrochemical study of high-temperature (HT) LiCoO2 obtained from Co(OH)2 recycled of spent lithium ion batteries. Mater Res Bull. 2017; 86: 5−8.

Park YM, Lim H, Moon J-H, Lee H-N, Son SH, Kim H, Kim H-J. High-Yield One-Pot Recovery and Characterization of Nanostructured Cobalt Oxalate from Spent Lithium-Ion Batteries and Successive Re-Synthesis of LiCoO2. Metals 2017; 7: 303.

Li L, Bian Y, Zhang X, Guan Y, Fan E, Wu F, Chen R. Process for recycling mixed-cathode materials from spent lithium-ion batteries and kinetics of leaching. Waste Manage. 2018; 71: 362−371.

Meshram P, Abhilash, Pandey BD, Mankhand TR, Deveci H. Comparision of Different Reductants in Leaching of Spent Lithium Ion Batteries. JOM US 2016; 68: 2613−2623.

Chen X, Ma H, Luo C, Zhou T. Recovery of valuable metals from waste cathode materials of spent lithium-ion batteries using mild phosphoric acid. J Hazard Mater. 2017; 326: 77–86.

Guo Y, Li Y, Lou X, Guan J, Li Y, Mai X, Liu H, Zhao CX, Wang N, Yan C, Gao G, Yuan H, Dai J, Su R, Guo Z. Improved extraction of cobalt and lithium by reductive acid from spent lithium-ion batteries via mechanical activation process. J Mate Sci. 2018; 53: 13790–13800.

Takacova Z, Havlik T, Kukurugya F, Orac D. Cobalt and lithium recovery from active mass of spent Li-ion batteries: Theoretical and experimental approach. Hydrometallurgy 2016; 163: 9–17.

Zhou H, Zhao X, Yin C, Li J. Regeneration of LiNi0.5Co0.2Mn0.3O2 cathode material from spent lithium-ion batteries. Electrochim Acta 2018; 291: 142–150.

Meng Q., Zhang Y, Dong P. Use of electrochemical cathode-reduction method for leaching of cobalt from spent lithium-ion batteries. J Clean Prod. 2018; 180: 64–70.

Shih Y-J, Chien S-K, Jhang S-R, Lin Y-C. Chemical leaching, precipitation and solvent extraction for sequential separation of valuable metals in cathode material of spent lithium ion batteries. J Taiwan Inst Chem E. 2019; 100: 151–159.

Pinna EG, Ruiz MC, Ojeda MW, Rodriguez MH. Cathodes of spent Li-ion batteries: Dissolution with phosphoric acid and recovery of lithium and cobalt from leach liquors. Hydrometallurgy 2017; 167: 66–71.

dos Santos CS, Alves JC, da Silva SP, Evangelista Sita L, da Silva PRC, de Almeida LC, Scarminio J. A closed-loop process to recover Li and Co compounds and to resynthesize LiCoO2 from spent mobile phone batteries. J Hazard Mater. 2019; 362: 458–466.

Li L, Fan E, Guan Y, Zhang X, Xue Q, Wei L, Wu F, Chen R. Sustainable Recovery of Cathode Materials from Spent Lithium-Ion Batteries Using Lactic Acid Leaching System. ACS Sustain Chem Eng. 2017; 5: 5224–5233.

Chen X, Guo C, Ma H, Li J, Zhou T, Cao L, Kang D. Organic reductants based leaching: A sustainable process for the recovery of valuable metals from spent lithium ion batteries. Waste Manage. 2018; 75: 459–468.

Santana IL, Moreira TFM, Lelis MFF, Freitas MBJG. Photocatalytic properties of Co3O4/LiCoO2 recycled from spent lithium-ion batteries using citric acid as leaching agent. Mater Chem and Phys. 2017; 190: 38–44.

He L-P, Sun S-Y, Song X-F, Yu J-G. Leaching process for recovering valuable metals from the LiNi1/3Co1/3Mn1/3O2 cathode of lithium-ion batteries. Waste Manage. 2017; 64: 171–181.

Jiang F, Chen Y, Ju S, Zhu Q, Zhang L, Peng J, Wang X, Miller JD. Ultrasound-assisted leaching of cobalt and lithium from spent lithium-ion batteries. Ultrason Sonochem. 2018; 48: 88–95.

Bernardes AM, Espinosa DCR, Tenório JAS. Recycling of batteries: a review of current processes and technologies. J Power Sources 2004; 130: 291–298.

Li X, Wang T, Pei L, Zhu C, Xu B. Conference Proceeding. In: Proceedings of IEEE Transportation Electrification Conference and Expo (ITEC) Asia-Pacific 2014. Beijing, China, 2014, pp. 1–6.

Lyu C, Song Y, Wang L, Li J, Zhang B, Liu E. A new method for lithium-ion battery uniformity sorting based on internal criteria. J Energy Storage 2019; 25: 100885.

Chen H, Shen J. A degradation-based sorting method for lithium-ion battery reuse. PLoS One 2017; 12: 1–15.

Yoon S, Hwang I, Lee CW, Ko HS, Han KH. Power capability analysis in lithium ion batteries using electrochemical impedance spectroscopy. J Electroanal Chem. 2011; 655: 32–38.

Pei L, Wang T, Lu R, Zhu C. Development of a voltage relaxation model for rapid open-circuit voltage prediction in lithium-ion batteries. J Power Sources 2014; 253: 412–418.

Kim J, Cho BH. Screening process-based modeling of the multi-cell battery string in series and parallel connections for high accuracy state-of-charge estimation. Energy 2013; 57: 581–599.

Ohshima T, Nakayama M, Fukuda K, Araki T, Onda K. Thermal Behavior of Small Lithium-Ion Secondary Battery During Rapid Charge and Discharge Cycles. Electrical Engineering in Japan 2006; 3: 17–25.

Li L, Lu J, Ren Y, Zhang XX, Chen RJ, Wu F, Amine K. Ascorbic-acid-assisted recovery of cobalt and lithium from spent Li-ion batteries. J Power Sources 2012; 218: 21–27.

Veluchamy A, Doha C-H, Kim D-H, Lee J-H, Shin H-M, Jin B-S, Kim H-S, Moon S-I. Thermal analysis of LixCoO2 cathode material of lithium ion battery. J Power Sources 2009; 189: 855–858.

Hanisch C, Loellhoeffel T, Diekmann J, Markley KJ, Haselrieder W, Kwade A. Recycling of lithium-ion batteries: a novel method to separate coating and foil of electrodes. J Clean Prod. 2015; 108: 301–311.

Fu Y, He Y, Qu L, Feng Y, Li J, Liu J, Zhang G, Xie W. Enhancement in leaching process of lithium and cobalt from spent lithium-ion batteries using benzenesulfonic acid system. Waste Manage. 2019; 88: 191–199.

Zheng Y, Long HL, Zhou L, Wu ZS, Zhou X, You L, Yang Y, Liu JW. Leaching Procedure and Kinetic Studies of Cobalt in Cathode Materials from Spent Lithium Ion Batteries Using Organic Citric Acid as Leachant. Int J Environ Res. 2016; 10: 159–168.

Li L, Dunn JB, Zhang XX, Gaines L, Chen RJ, Wu F, Amine K. Recovery of metals from spent lithium-ion batteries with organic acids as leaching reagents and environmental assessment. J Power Sources 2013; 233: 180–189.

Sun L, Qiu K. Vacuum pyrolysis and hydrometallurgical process for the recovery of valuable metals from spent lithium-ion batteries. J Hazard Mater. 2011; 194: 378–384.

Golmohammadzadeh R, Rashchi F, Vahidi E. Recovery of lithium and cobalt from spent lithium-ion batteries using organic acids: Process optimization and kinetic aspects. Waste Manage. 2017; 64: 244–254.

Daniel C, Mohanty D, Li J, Wood DL. Cathode Materials Review. AIP Conference Proceedings 1597 2014; 26: 26–43.

Jiang Y, Qin C, Yan P, Sui M. Origins of capacity and voltage fading of LiCoO2 upon high voltage cycling. J Mater Chem A 2019; 7: 20824–20831.