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In this paper, catalyst precursor fibers were prepared by a sol gel method combined with an electrospinning method using tetrabutyl titanate as a titanium source, cobalt acetylacetonate as a cobalt source, and iron acetylacetonate as an iron source. CoFe@TiO 2 nanofibers (NFs) with a bimetallic spinel structure were formed after thermal annealing, which have dual-functional catalytic activity. With the molar ratio of Co and Fe coming to 1:1, a typical spinel CoFe 2 O 4 structure was generated in Co 1 Fe 1 @TiO 2 NFs. At a load of only 28.7 μg•cm −2 , Co 1 Fe 1 @TiO 2 NFs not only have a low overpotential (284 mV) and Tafel slope (54 mV•dec −1 ) in the oxygen evolution reaction but also show a high initial potential (0.88 V) and limiting current density (6.40 mA•cm −2 ) in the oxygen reduction reaction. Meanwhile, Co 1 Fe 1 @TiO 2 NFs exhibit good durability, cycle stability, and dual-function catalysis.

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