Porous carbon materials are widely used in supercapacitors, CO₂ capture, and rapid absorption applications, owing to their high surface area and tunable functionality. In our previous work, we demonstrated that a commercially available blend of butadiene-acrylonitrile (BAN) and styrene-acrylonitrile (SAN) random copolymers can be directly pyrolyzed to form porous carbon structures. Compared to traditional hard/soft templating methods and block copolymer-based pyrolysis, our approach offers a low-cost, time-efficient strategy for producing structure-controlled porous carbon without the need for complex block copolymer synthesis. In this study, we report the use of electrospinning for fabricating porous carbon fibers from the BAN/SAN blend. To our knowledge, this is the first report to establish processing–structure relationships for electrospun porous carbon derived from this commercially available random copolymer system. We employed rapid thermal annealing (RTA) with heating rates up to 10 °C/s—approximately six times faster than conventional methods—to effectively quench the phase-separated morphology and preserve nanoscale pores averaging ~750 nm. To further tailor the structure, we introduced 1,4-benzenediboronic acid (BDBA) as a dopant, which reduced pore size to ~85 nm while simultaneously incorporated boron heteroatoms into the carbon matrix. The resulting carbon fibers, treated with both RTA and BDBA, retained their morphology and displayed well-defined hierarchical porosity. Our method provides a cost-effective, scalable route to functional porous carbon fibers and expands the design space for heteroatom-doped materials in energy storage, catalysis, and environmental applications.
