The use of a liquid injection delivery system to form composite films containing nanoparticles was investigated. Al2O3–TiO2 films were grown on silicon substrates by direct liquid injection MOCVD (DLI-MOCVD) at 400 °C. The α-Al2O3 nanoparticles (α-Al2O3NPs) dispersed in TiO2 films resulted from co-deposition using colloidal α-Al2O3 solution and titanium tetraisopropoxide as titanium precursor. Scanning electron microscopy coupled with EDS as well as Raman spectroscopy confirmed the presence of α-Al2O3NPs aggregates embedded in the TiO2 matrix. The liquid injection system coupled with CVD technique can be promising to form composite films containing preformed nanoparticles.