The escalating global demand for lithium‐ion batteries necessitates efficient and sustainable end‐of‐life management. Major recycling routes such as pyrometallurgy and hydrometallurgy offer promising paths for metal recovery, but their efficiency often depends on the pretreatment of spent batteries. However, optimizing low‐temperature pretreatment for complete organic removal while preserving active material integrity remains challenging. This study investigated thermal decomposition and surface changes of key battery components—lithium nickel manganese cobalt oxide (NMC622) cathode, graphite anode, and polymeric separator—from 100 to 800 °C, focusing on the 400–650 °C industrial interval. Material responses were characterized using thermo‐gravimetric analysis coupled with mass spectrometry, isothermal mass loss, and scanning electron microscopy with energy‐dispersive X‐ray spectroscopy. A 500 °C treatment was identified as optimal, enabling complete organic carbon removal within 1 h without compromising the NMC spinel structure or current collector degradation. This precise control reduces energy consumption and mitigates hazardous gas release, enhancing environmental sustainability and providing a practical, scalable, and cost‐effective strategy for improving battery recycling. These findings help to define the parameters for efficient electroactive material separation. This work advances the understanding of low‐temperature thermal pretreatment for battery recycling, supporting a circular economy for critical materials.