Heterostructure design and integration with conductive materials play a crucial role in enhancing the conversion kinetics of electrode materials for metal-ion batteries. However, integrating nanocrystal heterojunctions into a conductive layer to form a superstructure is a significant challenge, mainly due to the difficulty in maintaining the structural integrity. Here we report a unique glucose-induced heterogeneous nucleation method that enables the independent manipulation of nucleation and growth of Mo2C/MoC heterojunction nanocrystals within 2D layers. Our investigations reveal that the rGO-Mo2C/MoC-rGO superstructure is formed by a topological transformation induced by subsequent heat treatment of the initial hydrothermally prepared rGO-MoO2-rGO precursor. This novel structure embeds Mo2C/MoC heterojunction nanocrystals within a 2D graphene matrix, providing enhanced mechanical stability, accelerated Na+ transport, and improved electron conduction. Ex situ XRD and Raman spectroscopy analyses reveal that the rGO-Mo2C/MoC-rGO superstructure significantly enhances the stability and reversibility of anodes. Leveraging these unique characteristics, the newly developed superstructural anode exhibits remarkable long-term cycling stability and outstanding rate performance. As a result, superstructure anodes demonstrate superior electrochemical capabilities, delivering a specific capacity of 106mAh/g after enduring 5000 cycles at 1 A/g. Our study underscores the critical importance of superstructure design in propelling the advancement of battery materials.
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