Recent advancements in 2D graphene materials highlight their versatile applications in electronics, clean energy, medicine, and other fields due to their exceptional properties and ease of fabrication. The current study investigates the preparation of reduced graphene oxide (RGO) through the thermal exfoliation of graphite oxide under an air atmosphere at varying temperatures (200–500 °C) and further examines its suitability as an anode for lithium-ion (Li-ion) batteries. The extent of reduction of functional groups, exfoliation, and other physical changes is analyzed by XRD, SEM, XPS, BET, and Raman studies, which show that the reduction of functional groups and surface area increases with increasing exfoliation temperature. The RGO electrodes are subjected to electrochemical studies, including cyclic voltammetry and charge–discharge cycling at various current densities, which demonstrate varying discharge capacities for RGO samples prepared at different temperatures. The RGO exfoliated at 400 °C delivered the maximum capacity, indicating that this temperature is optimal for the thermal preparation of RGO. This material shows potential for use as an anode in Li-ion batteries.