In this study, a series of nano-TiO 2 composite materials, including nano-TiO 2 , nano-SnO 2 /TiO 2 , nano-SiO 2 /TiO 2 , and nano-Fe 2 O 3 /TiO 2 , were successfully synthesized via the gaseous detonation method. Comprehensive characterization of the synthesized samples was carried out through X-ray diffraction (XRD), transmission electron microscopy/high-resolution TEM (TEM/HRTEM), scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS), Brunauer−Emmett− Teller (BET) method, and Fourier transform infrared (FTIR) analysis, which unveiled the significant influence of precursor types on the microstructure of the composite materials. Specifically, the incorporation of Sn 4+ promoted the transformation of TiO 2 to the rutile phase, reducing particle sizes from 25 to 19 nm and increasing the specific surface area from 44 to 86 m 2 /g. In contrast, the introduction of SiO 2 impeded the rutile phase formation, leading to a marked reduction in particle size to 14 nm and an enhancement of the specific surface area to 104 m 2 /g. Furthermore, the presence of Fe 3+ promoted the formation of the rutile phase and enabled particle growth to 44 nm. These findings not only deepen the understanding of structural control in the synthesis of nano-TiO 2 composite materials via the gaseous detonation method but also highlight the critical role of precursor selection in determining the properties of the resulting materials.