This article describes the synthesis of hydroxyapatite (HAp) flakes through a microwave-assisted hydrothermal method. These flakes are intended for use as substrates for depositing titanium dioxide (TiO2) films using chemical vapor deposition with metal–organic precursors (MOCVD). The results reveal the formation of crystalline hydroxyapatite characterized by a uniform mor-phology. Additionally, we demonstrated the successful deposition of TiO2 coatings on the hy-droxyapatite flakes, resulting in a distinctive faceted prism morphology. Our findings affirm the effective synthesis of the HAp/TiO2 composite material. To further explore the material’s practical applications, we recommend assessing the photocatalytic activity of these composite membranes in future research.