Abstract: A self-supported electrode with NiSe2 hybrid nanostructure grown on carbon fiber paper (CFP) was synthesized, for the first time, by using a two-step method combining hydrothermal process with chemical vapor deposition. The morphology, composition and phases were characterized by SEM, XRD and XPS. Moreover, the HER performance of the as-grown electrode in 0.5 mol·L-1 H2SO4 was determined. The results showed that the nanowires of the precursor, Ni2(CO3)(OH)2, linked during the selenization reaction. The product exhibited hybrid structure of NiSe2 nanowires and nanoparticles (H-NiSe2/CFP), which uniformly covered the CFP. The H-NiSe2/CFP only required a low overpotential of 232 mV to deliver the current density of 100 mA·cm-2, which is lower than that of the NiSe2 nanoparticles grown on CFP (NiSe2 NPs/CFP). Accordingly, the H-NiSe2/CFP displayed lower Tafel slope (38.3 mV·dec-1) and charge transfer resistance (3.2 Ω) when compared with the NiSe2 NPs/CFP. Also, the H-NiSe2/CFP showed larger double-layer capacitance (11.81 mF·cm-2) and TOF value (0.284 H2·s-1) than those of the NiSe2 NPs/CFP. These indicated the excellent HER performance of H-NiSe2/CFP. Moreover, this electrode exhibited remarkable stability during 3 000 times cycles CV sweeps and 20 h testing at the fixed overpotentials.
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