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In this research, we report a simple hydrothermal synthesis to prepare rhenium (Re)- doped MoS 2 flower-like microspheres and the tuning of their structural, electronic, and electrocatalytic properties by modulating the insertion of Re. The obtained compounds were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Structural, morphological, and chemical analyses confirmed the synthesis of poorly crystalline Re-doped MoS 2 flower-like microspheres composed of few stacked layers. They exhibit enhanced hydrogen evolution reaction (HER) performance with low overpotential of 210 mV at current density of 10 mA/cm 2 , with a small Tafel slope of 78 mV/dec. The enhanced catalytic HER performance can be ascribed to activation of MoS 2 basal planes and by reduction in charge transfer resistance during HER upon doping.

Electrochemical Hydrogen Evolution over Hydrothermally Synthesized Re-Doped MoS2 Flower-Like Microspheres