Abstract This paper introduced the preparation of high ordered lamellar Ti/Si composite materials by sol-gel method using cationic surfactant CTAB as template, TEOS as silicon source, and TiCl3 as titanium source in hydrothermal system. The structure and morphology of the samples were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that the products possessed high ordered microporous structure and homogeneous lamellar morphology with a dimension of around 10 nm, which provides favorable condition for its catalytic oxidation and establishes the theoretical foundation for the preparation of Ti/Si composite materials in the experiment teaching materials.