We report a scalable, solvent-lean electrospinning route to TiO2/Co3O4 core–shell fibers using a dual-bore needle, followed by low-temperature calcination (480°C). The coaxial architecture establishes a p–n junction (n-TiO2 core, p-Co3O4 shell) that generates an internal electric field across the heterointerface, accelerating charge transfer and ion transport. The fibers are phase-pure with Ti4+ and mixed Co2+/Co3+ states. The core–shell design more than doubles the surface area of TiO2 (81.2 vs 38.7 m2/g) and lowers interfacial resistance (RCT = 2.40 Ω), with a small IR drop (0.049 V at 5 A/g). In three-electrode tests, the core–shell fibers exhibit a specific capacitance of 1459 F/g at 10 mV/s, outperforming single-oxide fibers. An asymmetric supercapacitor assembled with TiO2/Co3O4/activated carbon in 1 M KOH achieves 196 F/g at 1 A/g, an energy density of 27.2 Wh/kg, and a power density of up to 1944 W/kg within a 0–1 V window, retaining 93 % of its capacitance after 10,000 cycles with a high Coulombic efficiency. These results demonstrate that a simple, mass-producible core–shell fiber electrode can achieve high energy and power while maintaining long life. The work highlights coaxial transition metal oxide heterostructures as a practical route to durable, high-performance asymmetric supercapacitors.
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