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Although sheet-like materials have good electrochemical properties, they still suffer from agglomeration problems during the electrocatalytic process. Integrating two-dimensional building blocks into a hollow cage-like structure is considered as an effective way to prevent agglomeration. In this work, the hierarchical NiCo 2 O 4 nanocages were successfully synthesized via coordinated etching and precipitation method combined with a post-annealing process. The nanocages are constructed through the interaction of two-dimensional NiCo 2 O 4 nanosheets, forming a three-dimensional hollow hierarchical architecture. The three-dimensional supporting cavity effectively prevents the aggregation of NiCo 2 O 4 nanosheets and the hollow porous feature provides amounts of channels for mass transport and electron transfer. As an electrocatalytic electrode for methanol, the NiCo 2 O 4 nanocages-modified glassy carbon electrode exhibits a lower overpotential of 0.29 V than those of NiO nanocages (0.38 V) and Co 3 O 4 nanocages (0.34 V) modified glassy carbon electrodes. The low overpotential is attributed to the prominent electrocatalytic dynamic issued from the three-dimensional hollow porous architecture and two-dimensional hierarchical feature of NiCo 2 O 4 building blocks. Furthermore, the hollow porous structure provides sufficient interspace for accommodation of structural strain and volume change, leading to improved cycling stability. The NiCo 2 O 4 nanocages-modified glassy carbon electrode still maintains 80% of its original value after 1000 consecutive cycles. The results demonstrate that the NiCo 2 O 4 nanocages could have potential applications in the field of direct methanol fuel cells due to the synergy between two-dimensional hierarchical feature and three-dimensional hollow structure.

Design of Hierarchical NiCo2O4 Nanocages with Excellent Electrocatalytic Dynamic for Enhanced Methanol Oxidation