Recent studies have
proven that newly emerging two-dimensional molybdenum diselenide (MoSe<sub>2</sub>) is a promising noble-metal-free electrocatalyst for hydrogen
evolution reaction (HER). Increasing the exposures of the active edges
of MoSe<sub>2</sub> nanostructures is a key issue to fully realize
the excellent electrochemical properties of MoSe<sub>2</sub>. In this
work, a few-layered MoSe<sub>2</sub>/carbon fiber aerogel (CFA) hybrids
have been facilely obtained through the combination of high-temperature
carbonization and one-pot solvothermal reaction. CFA derived from
cotton wool is used as a three-dimensional conductive network for
construction of hierarchical MoSe<sub>2</sub>/CFA hybrids, where few-layered
MoSe<sub>2</sub> nanosheets are uniformly and perpendicularly decorated
on the surfaces of CFA. In the designed and prepared hybrids, CFA
effectively increases the exposures of the active edges of MoSe<sub>2</sub> nanosheets as well as provides reduced lengths for both electron
transportation and ion diffusion. Therefore, the obtained optimal
MoSe<sub>2</sub>/CFA hybrid exhibits excellent electrochemical activity
as HER electrocatalyst with a small onset potential of −0.104
V vs reversible hydrogen electrode and a small Tafel slope of 62 mV
per decade, showing its great potential as a next-generation Pt-free
electrocatalyst for HER