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Nowadays, materials that possess high activity and natural oxygen vacancy have garnered significant attention as potential electrode materials for supercapacitors. In this study, we successfully prepared the Hf 6 Ta 2 O 17 (HTO) nanofibres (NFs) with an orthorhombic superlattice structure using the electrospinning technique and sintering process. The characterization results indicate that the HTO NFs synthesized at 750 °C show good micro nanostructures and outstanding electrochemical properties. To enhance its energy storage performance, additional oxygen vacancies (OVs) were introduced through a carbothermal treatment under an Ar atmosphere. Although longer reduction reaction times can produce more OVs, the integration of grain boundaries and the growth of grain size caused by large annealing times may limit its electrochemical performance. Therefore, the HTO NFs treated for 1 h (HTO/C-1) exhibited the maximum C s of 925 F·g−1 at 1 A·g−1 with a larger voltage window of 2.1 V. Furthermore, a symmetric supercapacitor fabricated by two reduced HTO NFs electrodes and 1 M Na 2 SO 4 solution, recorded as r-HTO NFs//r-HTO NFs. The device demonstrated excellent energy density of 73.3 Wh·kg−1 (at power density of 1050 W·kg−1) and a long cycling life (81.8% retained after 5000 cycles). These results suggest that the optimized reduction process can provide appropriate oxygen vacancies in HTO NFs, thereby effectively enhancing its performance. [Display omitted] • The Hf 6 Ta 2 O 17 (HTO) nanofibres (NFs) are synthesized by electrospinning method. • The micro nanostructures and electrochemical property of HTO NFs can be designed by controlling the synthesis temperature. • The carbothermal treatment carried under Ar atmosphere is used to improve the amount of oxygen vacancies of HTO NFs. • The HTO NFs treated of 1 h (HTO/C-1) presents excellent capacitance of 925 F·g−1 at 1 A·g−1. • The r-HTO NFs//r-HTO NFs device shows high energy density of 73.3 Wh·kg−1 at power density of 1050 W·kg−1. [ABSTRACT FROM AUTHOR]