Carbonization‐Controlled Porosity and Electron Transport in Molybdenum Oxide‐Carbide/Carbon Nanoflower Anodes

ABSTRACT To design high‐performance Mo‐based composite electrodes for advanced energy‐storage devices, such as lithium‐ion batteries (LIBs), the relationship between pore structure and electron transport and its influence on the electrochemical behavior must be clarified, particularly in scenarios where these effects are strongly coupled. In this study, MoO 2 /Mo 2 C‐C nanoflower composites were synthesized via temperature‐controlled carbonization to regulate the structural characteristics of the active materials. By systematically varying the carbonization temperature, samples with distinct pore volumes and particle assembly configurations were obtained, and their electrochemical behavior as LIB anodes was comprehensively analyzed. Results revealed that although pore structure is an intrinsic property of the active material, electron transport is governed primarily by electrode‐level characteristics and depends strongly on interparticle contact within the composite electrode. At the same time, other temperature‐dependent structural changes may also influence the overall electrochemical response. The structure‐performance‐balanced sample exhibited enhanced charge transfer kinetics, as evidenced by the lowest charge transfer resistance, indicating the formation of more efficient electron transport pathways. In addition, a balanced structural configuration promoted the effective utilization of both diffusion‐ and surface‐controlled processes. Consequently, the optimized electrode delivered a high reversible capacity of 600 mAh/g at 100 mA/g after 400 cycles. These results demonstrate that electrochemical performance is determined by the coupling between material‐level structural behavior and electrode‐level transport properties, providing valuable design insights for high‐performance Mo‐based composite anodes.