The detailed phase analysis using XRD coupled with SEM/EDS and metal composition data confirmed that the crystalline phases of NMC were well-preserved in the untreated BM, where BM1, BM2, and BM3 belong to NMC622, NMC111, and NMC901 chemistries. It was also determined that graphite in BM could either be a pure 2H phase or a mixture of 2H and 3R phases. These phases can be quantified using XRD. Furthermore, SEM/EDS analysis revealed the distribution of PVDF binder on NMC particles by detecting fluorine, which could hinder metal leaching efficiency and graphite recovery by flotation. These techniques also revealed that phase transformations of NMC caused by pyrolysis pre-treatment altered the surface morphology of NMC particles from needlelike structure to rough surface. TGA/MS under pyrolytic conditions showed that the decomposition of residual electrolytes and PVDF in BM gives rise to the evolution of carbonaceous (CO 2, CO, and CH4) and fluorinated (HF and fluorine) gases. It also provided direct evidence that complete PVDF decomposition under inert conditions can require temperatures above 600 °C while leaving behind carbonaceous char. Whereas, TGA/MS of pure PVDF under oxidative atmosphere showed 100 % mass loss and this finding can be used to estimate the amount of PVDF in BM. Quantification of carbon in NMC-based BM using a calibration curve developed with TGA/MS of pure graphite under an oxidative atmosphere is a novel finding of this study. This has established a fast and robust methodology for determining the carbon content in BM and provided a basis for optimizing graphite recovery by flotation. Furthermore, SEM/EDS analysis of graphite particles in BM samples showed deposition of metals on the surface of graphite while Raman spectroscopy enabled a detailed examination of carbonaceous species deposited on graphite. Ramana spectra showed that ID/IG ratios varied across different particles in the same BM sample due to differences in surface deposition and disorder. Overall, this study highlights the importance of linking various characterization approaches to guide the development of efficient BM pre-treatment and recycling workflows. The insights gained into particle size effects, phase transformations, binder removal, and carbon quantification provide a foundation for optimizing recycling strategies that maximize recovery of valuables while minimizing process inefficiencies.