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Studying an acetone sensor with prominent sensitivity and selectivity is of great significance for the development of portable diabetes monitoring system. In this paper, cubic-like NiO/ZnO composites with different contents of Ni²⁺ were successfully synthesized by modifying MOF-5 with Ni²⁺-doped. The structure and morphology of the prepared composites were characterized by XRD, XPS, and SEM. The experimental results show that the NiO/ZnO composite showed an enhanced gas sensing property to acetone compared to pure ZnO, and the composites showed the maximum response value when Ni²⁺ loading amount was 5 at%. The response value of the 5% NiO/ZnO composite to acetone (500 ppm) at the optimum operating temperature (340 °C) is 7.3 times as that of pure ZnO. At the same time, the 5% NiO/ZnO composite has excellent selectivity and reproducibility for acetone. The gas sensing mechanism of the heterojunction sensor was described.