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The synthesis of cost-effective and high-performance electrocatalysts for water splitting is the main challenge in electrochemical hydrogen production. In this study, we adopted a high throughput method to prepare bi-metallic catalysts for oxygen/hydrogen evolution reactions (OER/HER). A series of Ni–Mo alloy electrocatalysts with tunable compositions were prepared by a simple co-sputtering method. Due to the synergistic effect between Ni and Mo, the intrinsic electrocatalytic activity of the Ni–Mo alloy electrocatalysts is improved, resulting in excellent HER and OER performances. The Ni 90 Mo 10 electrocatalyst shows the best HER performance, with an extremely low overpotential of 58 mV at 10 mA cm−2, while the Ni 40 Mo 60 electrocatalyst shows an overpotential of 258 mV at 10 mA cm−2 in OER. More significantly, the assembled Ni 40 Mo 60 //Ni 90 Mo 10 electrolyzer only needs a cell voltage of 1.57 V to reach 10 mA cm−2 for overall water splitting. [Display omitted] • A high throughput method was used to prepare Ni–Mo alloy catalysts. • Ni–Mo alloy catalysts exhibit remarkable activity and stability for HER and OER. • The Ni–Mo alloy acts as a bifunctional catalyst for overall water splitting. • The synergistic effect between Ni and Mo leads to the excellent performances. [ABSTRACT FROM AUTHOR]