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It is still a great challenge to achieve high volumetric capacitance without losing gravimetric capacitance and cycling performances for carbon-based electrode materials to fulfill the demands for next-generation supercapacitors. In this work, we have fabricated carbon nanofiber (CNF) mats doped with tetraheteroatoms (N, P, O, and S) via a two-step process: electrospinning and carbonization. The surface porosity, mass density, and doping density of the as-prepared doped CNFs were optimized by varying the l-cysteine-to-potassium pentoxide mass ratio in the polyacrylonitrile (PAN) precursor solution. The structural evaluation of different heteroatom species in the carbon lattice of the as-prepared NPOS-CNFs was systematically studied by various spectroscopic techniques. The optimized NPOS-CNF 12 nanofibers, which were prepared from the PAN precursor containing an l-cysteine/P₂O₅ mass ratio of 1:2, have a …