A heterojunction structure between the UiO-66 metal–organic framework (MOF) and MoS₂ nanoflowers is produced using a straightforward hydrothermal process. The hybrid MoS₂@UiO-66 was then used as an electrode material for high-per formance supercapacitor applications. In this study, 10 and 20 wt.% of MoS₂ were anchored on the surface of UiO-66. The morphology and structure of UiO-66, MoS₂, and the hybrid MoS₂@UiO-66 were evaluated using XRD, FT-IR, HR-TEM, EDX, and BET analyses. The hybrid MoS₂@UiO-66 demonstrated a significant enhancement in electrochemical performance attributed to the synergistic combination of the structural characteristics of the UiO-66 and MoS₂. The basic flower-like construction of the MoS₂@UiO-66 composite remained unaffected, exhibiting an impressive specific capacitance of 1455 F g⁻¹ at a current density of 1.0 A g⁻¹ and exceptional cyclic stability with a retention rate of 95% after 5000 cycles at a 5.0 A g⁻¹ current. Due to its promising electrochemical performance, MoS₂@UiO-66 may applied in energy storage technology.