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- MakaleAçık Erişim2026Scopus SJRQ2Investigation of the Effects of Low-Temperature Thermal Treatment Applied to Graphite in Spent Lithium-Ion Anode Recycling
Kara, Adem; Temur, Hakan
As the use of lithium-ion batteries (LIB) increases rapidly, recovery of graphite, the main component of the anode, from spent batteries has become important from environmental and economic perspectives. In this study, an acid leaching step followed by thermal treatment under partial atmosphere at a relatively low calcination temperature was investigated to recover graphite from spent lithium-ion batteries. The molecular and chemical structures of the recovered graphite in all spent anode samples were investigated using FTIR, ICP-MS, XRD, SEM–EDX and TEM–EDX. It was observed that organic impurities and volatile components were largely removed after acid leaching and thermal treatment at 750 °C. In addition, it was observed that graphite layers were rearranged and the distance between the layers decreased under the effect of thermal treatment. Partial atmosphere calcination at 750 °C can be considered as a feasible method for graphite recovery, offering energy efficiency and scalability. However, in an efficient calcination, it is necessary to maintain controlled oxygen levels to prevent excessive graphite loss and to perform preliminary acid leaching to reduce metal impurities. In order to best recycle graphite in waste lithium-ion anode recovery, a balance must be achieved between temperature, energy efficiency and material recovery. Considering this balance, a calcination temperature of 750 °C appears to be preferable for recycling.
AtıfScopus2WoS2İncele
- MakaleYalnız künye2026Scopus SJRQ1Multidimensional characterization of graphite anode degradation in used lithium-ion batteries under real-life conditions
Temur, Hakan; Kara, Adem
The degradation of graphite anodes in lithium-ion batteries remains a critical barrier to extending cycle life and enabling efficient recycling. This study employs a multi-technique approach combining XRD, FTIR, SEM-EDS, ICP-MS, and XPS to investigate degradation mechanisms in graphite anodes recovered from commercial spent mobile phone batteries. While unused reference anodes show no significant degradation, spent anodes exhibit surface cracks, porous networks, heterogeneous SEI growth, and pronounced oxygen/fluorine accumulation. FTIR and XRD confirm increased LiF and Li2CO3 formation, indicating electrolyte decomposition and structural breakdown. ICP-MS reveals transition metal migration (Co, Ni, Mn) and current collector corrosion (Cu, Al), which correlate with degradation severity. Surface-sensitive XPS analysis further resolves a progressive degradation pathway: from limited SEI formation in low-degradation samples, through concurrent corrosion and metal crossover in medium-degradation samples, to extensive LiF-rich SEI accumulation in the most degraded samples. These findings are consistent with a self-accelerating chain-reaction mechanism wherein electrolyte decomposition, metal migration, and corrosion synergistically accelerate capacity fade. This study proposes a mechanistic framework for understanding heterogeneous degradation in real-world spent batteries and offers a practical, multi-technique diagnostic tool for recycling and second-life applications.


