In this study, 2D Co-B nanosheet-decorated 1D TiO2 nanofibers (2D Co-B NS-decorated 1D TiO2 NFs) are synthesized via electrospinning and an in situ chemical reduction technique. The as-prepared catalyst showed excellent catalytic performance in H2 generation from sodium borohydride (SBH). When compared to naked Co-B nanoparticles, the catalytic activity of the 2D Co-B NS-decorated 1D TiO2 NFs catalyst for the hydrolysis of SBH is significantly enhanced, as demonstrated by the high hydrogen generation rate (HGR) of 6020 mL min−1 g−1 at 25 °C. The activation energy of hydrolysis was measured to be 30.87 kJ mol−1, which agreed with the reported values. The catalyst also showed good stability. Moreover, the effects of SBH, catalyst concentration, and temperature on the catalytic performance of 2D Co-B NS-decorated 1D TiO2 NFs were studied to gain a comprehensive understanding of the dehydrogenation mechanism of SBH. Based on these findings, we conclude that 2D Co-B NS-decorated 1D TiO2 NFs are effective catalytic materials for the dehydrogenation of SBH.
