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ical hydrogen evolution reaction (HER) is an effective method to turn intermittent electric energy into renewable hydrogen energy. [2] However, the HER performance is dramatically limited by high overpotential energy barriers and kinetic sluggishness. [3] To address this problem, lots of effective and low-cost non-noble metalbased materials have been explored as efficient electrocatalysts for HER to decline the overpotential and accelerate reaction kinetics. [4] Among them, molybdenum diselenide (MoSe 2 ) is extensively investigated as a cathodic material for HER due to suitable hydrogen adsorption energy and electrical conductivity. [5] Note that these important research advances are basing on an assumption that MoSe 2 is stable in HER. However, currently, some researchers have found the dissolution of Mo in Mo-based electrocatalysts during HER process, [6][7][8][9][10] but the influence of Mo dissolution on chalcogenide under reduction condition and the promotion activity mechanism and leaching of chalcogen are still unclear. Exploring the surface structural transformation and the origin of active species are beneficial to the rational design of highly efficient electrocatalysts. The activation process of many catalysts under their operating conditions directly indicated a negative catalytic stability of themselves, [11][12][13] due to

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