AbstractHerein, we report the synthesis of TiO₂–SnO₂–C/carbide hybrid electrode materials for Li‐ion batteries (LIBs) via two different methods of controlled oxidation of layered Ti₂SnC. The material was partially oxidized in an open‐air furnace (OAF) or using a rapid thermal annealing (RTA) approach to obtain the desired TiO₂–SnO₂–C/carbide hybrid material; the carbide phase encompassed both residual Ti₂SnC and TiC as a reaction product. We tested the oxidized materials as an anode in a half cell to investigate their electrochemical performance in LIBs. Analysis of the various oxidation conditions indicated the highest initial lithiation capacity of 838 mAh/g at 100 mA/g for the sample oxidized in the OAF at 700°C for 1 h. Still, the delithiation capacity dropped to 427 mAh/g and faded over cycling. Long‐term cycling demonstrated that the RTA sample treated at 800°C for 30 s was the most efficient, as it demonstrated a reversible capacity of around 270 mAh/g after 150 cycles, as well as a specific capacity of about 150 mAh/g under high cycling rate (2000 mA/g). Given the materials’ promising performance, this processing method could likely be applied to many other members of the MAX family, with a wide range of energy storage applications.