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In this study, amorphous zinc oxide incorporated with sulfur-doped carbon composite nanofiber (ZnO@S-CNF) was obtained through a facile electrospinning technique and calcination. The ZnO@S-CNF composite was characterized in detail in order to understand the structural features of the electrodes and applied for supercapacitors. As a self-supporting electrode, it achieved a high capacitance of 209 F/g at 1 A/g and sustained 158 F/g at 10 A/g. Also, an asymmetric supercapacitor (ASC) assembled by ZnO@S-CNF as the positive and carbon nanofiber as the negative electrode (−CNF//ZnO@S-CNF+) achieved a specific energy of 11.2 Wh/kg at a specific power of 900 W/kg in 0–1.8 V. The excellent electrochemical performance can be ascribed to the enhanced surface area, increased micropore volume, and heteroatom content. This study can provide a feasible way for the development of other carbon composite electrodes with remarkable performance. [Display omitted] • Modification of the electronic structure by heteroatom doping, thereby promoting the supercapacitive performance. • Increased surface area with the synergistic effect of amorphous zinc oxide and introduction of sulfur in the carbon skeleton. • ASC device with a specific energy of 11.2 Wh/kg at a specific power of 900 W/kg. [ABSTRACT FROM AUTHOR]