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To develop efficient visible light driven photocatalysts for air purification, we constructed a novel semimetal–semiconductor Bi–Bi₂MoO₆ (Bi–Mo) nanohybrid via the in situ deposition of Bi nanoparticles on the surface of Bi₂MoO₆ microspheres. In this strategy, the Bi³⁺ ions were in situ reduced to metallic Bi particles by glucose during in hydrothermal process. The XRD, XPS, SEM, TEM, UV–vis, DRS, PL spectra, and surface photovoltage were employed to explore the structural and optical properties. The as-synthesized Bi–Bi₂MoO₆ nanohybrid was applied in photocatalytic removal of NO in air. The results indicated that the amount of reductive glucose not only exerted a pivotal effect on the morphological structure but also affected the photocatalytic capability of the Bi–Bi₂MoO₆ nanohybrid. The optimized Bi–Mo-50 hybrids exhibited exceptionally high visible-light photocatalytic performance with a NO removal ratio …