Transition metal phosphides are emerging non-noble metal electrocatalysts for hydrogen evolution reaction (HER) in water splitting. Herein, porous nickel cobalt phosphide nanosheet arrays with hierarchical structure were synthesized on carbon cloth (NiCoxPy-P/CC) as a robust and stable HER electrocatalyst by a facile approach involving electrodeposition and an effective PH3 plasma-assisted phosphorization. Owing to the unique structure with porous nanosheets composed of defect-abundant fine nanocrystals, the as-synthesized NiCoxPy/CC electrocatalyst demonstrates superior catalytic activity for HER to its thermally-phosphorized counterpart. Only at the overpotential as low as 70 (in 0.5?M?H2SO4) and 42?mV (in 1?M KOH), the current density of 10?mA/cm2 is achieved for the NiCoxPy/CC, which is among the best reported values for metal phosphide electrocatalysts. Moreover, the catalyst shows satisfying long-term durability up to 24?h in both the acidic and alkaline media. The outstanding HER performance and efficient synthesis strategy for the NiCoxP-P/CC makes it a promising electrocatalyst for hydrogen production.

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