Graphite recovery from waste Li-ion battery black mass for direct re-use

Alexander Chernyaev*, Anna Kobets, Kerli Liivand, Fiseha Tesfaye, Pyry-Mikko Hannula, Tanja Kallio, Leena Hupa, Mari Lundström

*Corresponding author for this work

Research output: Contribution to journalArticleScientificpeer-review

4 Citations (Scopus)
15 Downloads (Pure)

Abstract

Graphite was recovered from two leached (H2SO4 = 2 M, 60 °C, t = 3 h, Fe3+ = 2 g/L) Li-ion battery black mass concentrates with minimized energy consumption. One black mass originated from a mixture of mobile device and power tool batteries, and another from a single electric vehicle battery. The leach residues were pyrolyzed (800 °C, t = 1 h, Ar atmosphere) to remove the polyvinylidene fluoride (PVDF) binder and other non-metallic fractions. The black mass, its leach residue, and pyrolyzed residue were characterized using inductively coupled plasma-optical emission spectrometry (ICP-OES), ion chromatography (IC), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Raman spectroscopy, and N2 adsorption/desorption. After hydrometallurgical recycling and pyrolysis, the main post-metallurgical black mass impurities were cobalt oxide, iron, acid-resistant boehmite (AlO(OH)), and silicon dioxide. The pyrolysis resulted in electrolyte and binder removal, affected the crystallinity of the remaining boehmite. The recovered graphite-rich residue with impurities identified was tested as an anode in half-cells vs. metal Li. The average specific capacities of recovered graphite-rich residues from both sources were 350 and 250 mAh g-1 at 0.1C and their capacity retention after 100 cycles was high (80%) suggesting rather slow deterioration and hence the proposed recycling route being promising for the graphite reuse in new
Li-ion batteries.
Original languageEnglish
Article number108587
Pages (from-to)1-12
Number of pages12
JournalMinerals Engineering
Volume208
DOIs
Publication statusPublished - Mar 2024
MoE publication typeA1 Journal article-refereed

Keywords

  • Graphite
  • residue
  • leaching
  • Li-ion battery
  • recycling

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