Thermal stability of valuable metals in lithium-ion battery cathode materials: Temperature range 100–400 °C

Lithium is crucial in lithium-ion batteries (LIBs), serving as a main component of the electrolyte and cathode. Elements such as cobalt, nickel, and manganese are also vital for high performance, energy density, and stability. This study aimed to examine the behaviour of end-of-life cathode material (LiNi0.6Mn0.2Co0.2O2) and its valuable metals after exposure to temperatures between 100 and 400 °C, comparing it with untreated material. The lithium content cannot be reliably determined by conventional analytical methods, so inductively coupled plasma optical emission spectroscopy (ICP-OES) was chosen for this purpose. For ICP-OES measurements, samples were dissolved in different solvents for a specified time, and the concentrations of lithium, nickel, manganese, and cobalt were measured. From the measured values, their theoretical yields were calculated. Due to the annealing at given temperatures and subsequent dissolution, this step can be considered as the first stage of the pyrometallurgical-hydrometallurgical process used in battery recycling. The study was complemented by further analyses to monitor the effect of annealing temperatures on the properties of the material. Based on the results, it was found that the highest theoretical yield in this temperature range was for material annealed at 400 °C and dissolved in 20 % nitric acid for 4 h. •First step of pyro-hydrometallurgical process: heat treated cathode at 100–400 °C.•ICP-OES analysis of valuable metals (Li, Ni, Mn, Co).•Analysis of NMC spinel using XRF, XRD, TGA, SEM/EDS.•Leaching efficiency of NMC in demineralized water and nitric acid.•Comparison of yield with other recycling techniques.