Carbon nanofibers (CNFs) incorporating NiS nanoparticles (NPs), namely NiS@CNFs were prepared by one-step electrospinning and successfully employed as a catalyst for hydrogen production from hydrolytic dehydrogenation of sodium borohydride (SBH). As-prepared NiS@CNFs, composed of polyacrylonitrile (PAN), nickel acetate, and ammonium sulfide, was calcined at 900 degrees C in argon atmosphere, and characterized using standard surface science techniques. The combined results revealed the growth of NiS NPs inside the CNFs, hence confirmed the presence of elemental Ni, S, and C. The as-prepared NiS@CNFs catalyst has a significantly higher surface area (650.92 m(2)/g) than the reported value of 376 m(2)/g. Importantly, this catalyst exhibited a much higher catalytic performance, for H-2 production from SBH, than that of Ni@CNFs, as evidenced by its low activation energy (similar to 25.11576 kJ/mol) and their R-max values of 2962 vs. 1770 mL/g.min. Recyclability tests on using NiS@CNFs catalyst showed quantitatively production (similar to 100% conversion) of H-2 from SBH and retained up to 70% of its initial catalytic activity after five successive cycles. The low cost and high catalytic performance of the designed NiS@CNFs catalyst enable facile H-2 production from readily available hydrogen storage materials. (C) 2019 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.