Microwave‐Induced Structural Engineering and Pt Trapping in 6R‐TaS₂ for the Hydrogen Evolution Reaction

Abstract The nanoengineering of the structure of transition metal dichalcogenides (TMDs) is widely pursued to develop viable catalysts for the hydrogen evolution reaction (HER) alternative to the precious metallic ones. Metallic group‐5 TMDs have been demonstrated to be effective catalysts for the HER in acidic media, making affordable real proton exchange membrane water electrolysers. Their key‐plus relies on the fact that both their basal planes and edges are catalytically active for the HER. In this work, the 6R phase of TaS₂ is “rediscovered” and engineered. A liquid‐phase microwave treatment is used to modify the structural properties of the 6R‐TaS₂ nanoflakes produced by liquid‐phase exfoliation. The fragmentation of the nanoflakes and their evolution from monocrystalline to partly polycrystalline structures improve the HER‐activity, lowering the overpotential at cathodic current of 10 mA cm⁻² from 0.377 to 0.119 V. Furthermore, 6R‐TaS₂ nanoflakes act as ideal support to firmly trap Pt species, which achieve a mass activity (MA) up 10 000 A g_Pt⁻¹ at overpotential of 50 mV (20 000 A g_Pt⁻¹ at overpotentials of 72 mV), representing a 20‐fold increase of the MA of Pt measured for the Pt/C reference, and approaching the state‐of‐the‐art of the Pt mass activity.