We demonstrate a simple, efficient, yet versatile strategy for the synthesis of novel hierarchical heterostructures composed of TiO₂ nanofiber stem and various metal oxides (MOs) secondary nanostructures, including Co₃O₄, Fe₂O₃, Fe₃O₄, and CuO, by advantageously combining the versatility of the electrospinning technique and hydrothermal growth method, for which the controllable formation process and possible formation mechanism are also investigated. Moreover, as a proof-of-concept demonstration of the functional properties of these hierarchical heterostructures, the Co₃O₄/TiO₂ hierarchical heterostructures are investigated as the lithium-ion batteries (LIBs) anode materials for the first time, which not only delivers a high reversible capacity of 632.5 mAh g-1 and 95.3% capacity retention over 480 cycles, but also shows excellent rate capability with respect to the pristine TiO₂ nanofibers. The synergetic effect between Co₃O₄ and TiO₂ as well as the unique feature of hierarchical heterostructures are probably responsible for the enhanced electrochemical performance.

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