Graphene Oxide‐Directed Tunable Assembly of MoS 2 Ultrathin Nanosheets for Electrocatalytic Hydrogen Evolution

Three dimensional (3D) hierarchical architectures based on molybdenum disulfide (MoS 2 ) and reduced graphene oxide (rGO) are synthesized through a mixed solvothermal method. By simply increasing the amount of graphene oxide (GO) during the synthesis, the 3D assembly of MoS 2 can be tuned from nanoflowers to cross‐linked nanosheets firmly attached to rGO. The structural and compositional analysis show that MoS 2 nanostructures in the hybrids are constituted by ultrathin nanosheets with single or a few layers, and the GO precursor is reduced as rGO simultaneously. Due to the synergetic effects of rGO nanosheets and controllable assembly in MoS 2 ultrathin nanostructures, the resulting nanohybrids show optimized electrocatalytic hydrogen evolution properties in 0.5 M H 2 SO 4 solution. This work provides a facile method to increase the efficiency of hydrogen production for MoS 2 based materials and their analogues via a tunable bottom‐up assembly strategy.