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Developing high‐efficiency bifunctional electrocatalysts for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) to realize low‐cost water splitting is the premise for large‐scale production of hydrogen. The catalytic activity of an electrocatalysts greatly depends on its composition and structure. In this work, we report the preparation of hollow CoS2/MoS2 heterostructure using ZIF‐67 as the precursor. The ratio of Co and Mo are optimized to maximize the synergy of CoS2 and MoS2, due to their specific catalytic activity for OER and HER. The optimized CoS2/MoS2 exhibits good bifunctional catalytic activity in view of its low overpotentials for HER (170 mV) and OER (270 mV), as well as small cell voltage of 1.66 V for overall water splitting. This work provides a facile strategy to controllable fabrication of efficient bifunctional electrocatalysts for renewable energy applications. [ABSTRACT FROM AUTHOR]