There has been considerable research to engineer composites of transition metal dichalcogenides with other materials to improve their catalytic performance. In this work, we present a modified solution-processed method for the formation of molybdenum selenide (MoSe2) nanosheets and a facile method of structuring composites with graphene oxide (GO) or reduced graphene oxide (rGO) at different ratios to prevent aggregation of the MoSe2 nanosheets and hence improve their electrocatalytic hydrogen evolution reaction performance. The prepared GO, rGO, and MoSe2 nanosheets were characterized by X-ray powder diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, and scanning electron microscopy. The electrocatalytic performance results showed that the pure MoSe2 nanosheets exhibited a somewhat high Tafel slope of 80 mV/dec, whereas the MoSe2-GO and MoSe2-rGO composites showed lower Tafel slopes of 57 and 67 mV/dec at ratios of 6:4 and 4:6, respectively. We attribute the improved catalytic effects to the better contact and faster carrier transfer between the edge of MoSe2 and the electrode due to the addition of GO or rGO.

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Summary The development of an efficient water electrolyser is essential for sustainable hydrogen production; however, its application remains limited by the insufficient performance of the electrode. Herein, we report a rapid, simple, and cost‐effective fabrication of an Ni‐Co‐S cathode for the hydrogen evolution reaction (HER), which is directly usable for an anion exchange membrane water electrolyser (AEMWE). The Ni‐Co‐S electrocatalysts are prepared on a carbon paper (CP) substrate by a one‐step electrodeposition method by controlling deposition parameters such as the deposition potential, time, and electrolyte composition. The optimized Ni‐Co‐S/CP electrode demonstrates a high HER activity with an overpotential of 91 mV at −10 mA/cm2 in 1.0 M KOH. An AEMWE single cell employing the Ni‐Co‐S/CP cathode coupled with a commercial IrO2/CP anode exhibits a current density of 1.7 A/cm2 at 2.4 Vcell, which is higher than that of an AEMWE single cell with a commercial Pt/C/CP cathode; this is attributable to the enhancement of the electron and reactant/product transfer via appropriate cathode design.

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Transition metal dichalcogenides (TMDs) have been considered as one of the most promising electrocatalysts for the hydrogen evolution reaction (HER). Many studies have demonstrated the feasibility of significant HER performance improvement of TMDs by constructing composite materials with Ni-based compounds. In this work, we prepared Ni3Se4@MoSe2 composites as electrocatalysts for the HER by growing in situ MoSe2 on the surface of Ni3Se4 nanosheets. Electrochemical measurements revealed that Ni3Se4@MoSe2 nanohybrids are highly active and durable during the HER process, which exhibits a low onset overpotential (145 mV) and Tafel slope (65 mV/dec), resulting in enhanced HER performance compared to pristine MoSe2 nanosheets. The enhanced HER catalytic activity is ascribed to the high surface area of Ni3Se4 nanosheets, which can both efficiently prevent the agglomeration issue of MoSe2 nanosheets and create more catalytic edge sites, hence accelerate electron transfer between MoSe2 and the working electrode in the HER. This approach provides an effective pathway for catalytic enhancement of MoSe2 electrocatalysts and can be applied for other TMD electrocatalysts.