Photoelectrochemical Hydrogen Evolution and CO₂ Reduction over MoS₂/Si and MoSe₂/Si Nanostructures by Combined Photoelectrochemical Deposition and Rapid-Thermal Annealing Process

Diverse methods have been employed to synthesize MoS2 and MoSe2 catalyst systems. Herein, a combined photoelectrochemical (PEC) deposition and rapid-thermal annealing process has first been employed to fabricate MoS2 and MoSe2 thin films on Si substrates. The newly developed transition-metal dichalcogenides were characterized by scanning electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. PEC hydrogen evolution reaction (HER) was demonstrated in an acidic condition to show a PEC catalytic performance order of MoOx/Si < MoS2/Si << MoSe2/Si under the visible light-on condition. The HER activity (4.5 mA/cm2 at −1.0 V vs Ag/AgCl) of MoSe2/Si was increased by 4.8× compared with that under the dark condition. For CO2 reduction, the PEC activity was observed to be in the order of MoS2/Si < MoOx/Si << MoSe2/Si under the visible light-on condition. The reduction activity (0.127 mA/cm2) of MoSe2/Si was increased by 9.3× compared with that under the dark condition. The combined electrochemical deposition and rapid-thermal annealing method could be a very useful method for fabricating a thin film state catalytic system perusing hydrogen production and CO2 energy conversion