Abstract: Binary metal oxides with porous structure were prepared by rapid, template-free solution combustion method, and characterized by XRD, SEM, BET and other analytical methods. The results show that the type and dosage of combustion agent have great influence on the phase and structure of binary metal oxide. The rapid and simple advantages of solution combustion method make it a suitable project of material synthesis and preparation experiment for senior undergraduates. As such, the experimental content is novel and innovative, and can be completed within the prescribed experimental course period. This experiment enables students to master new and simple material preparation methods, expands students’ knowledge and lays a good foundation for their future research.