Abstract: A comprehensive experiment for the photocatalytic CO₂ reduction of brookite TiO₂ (B-TiO₂) has been designed. The pristine brookite TiO₂ (B-TiO₂), Cu₂O and their composites B-TiO₂-Cu₂O have been synthesized. The structure, morphology, and optic absorption properties of the material have been analyzed by X-ray diffractometer (XRD), UV-visible diffuse reflectance spectra (DRS), and scanning electron microscope (SEM), and the qualitative and quantitative analysis of the CO₂ reduction performance has been carried out by gas chromatography. The promotion effect of the formation of p-n heterojunction on the CO₂ reduction has also been discussed. This comprehensive experiment has exercised students’ literature research and hands-on practical ability. Meanwhile, it is helpful for students to understand the frontier of photocatalysis issue and stimulate students’ interest in learning. It is of great help to students’ innovative thinking, rigorous scientific research attitude, and ability to analyze and solve problems. This experiment can be used as a comprehensive experimental teaching content for undergraduate students of grade three in the applied chemistry class, which lays a foundation for the teaching of graduation thesis.