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Coupling of two active semiconductors can easily lead to a deterioration of their intrinsic properties. In this work, tiny MoO3 nanocrystals were deposited on 3D MoS2 frameworks via a hydrothermal reaction, with heterostructures forming by oxygen-bonding interactions at their interface. When tested as a supercapacitor electrode, the MoS2/MoO3 heterostructure exhibited a high specific capacitance of 287.7 F g−1 at a current density of 1 A g−1, and a remarkable cycling stability after 1000 cycles at 1 A g−1 in an aqueous solution compared to pristine MoS2. The results thus reveal the superior properties of the MoS2/MoO3 heterostructure for supercapacitor electrode.