A comprehensive laboratory-style teaching activity involving the synthesis, characterization, and analysis of structure-activity relationships of metal-organic framework (MOF) nanozymes was developed specifically for undergraduates at Tianjin University. The students acquired familiarity with the general approach in synthesizing MOFs by solvothermal method using substituted MIL-101­(Fe)-X (MIL is an acronym for Materials of Institute Lavoisier). Several modern characterization methods were taught, including powder X-ray diffraction and fluorescence spectroscopy for assessing MIL-101­(Fe)-X crystal structures and superoxide dismutase (SOD)-like activities. In particular, students were guided by the instructor to investigate the relationship between structural differences in MOFs caused by ligand changes and their SOD-like activities. The Hammett relationships were later demonstrated to be an accurate method of quantifying structure-activity relationships of MIL-101­(Fe)-Xnanozymes. By participating in this laboratory experience, students are able to improve their scientific thinking, practical abilities, and teamwork. Additionally, a fundamental principle of material design can be conveyed to undergraduates based on the structure-activity relationship, thereby deepening their understanding of nanozymes and the course's content.