Abstract: CoNi/rGO microwave absorber was successfully prepared by a polar solvothermal method. The absorption intensity and bandwidth could be modulated effectively by morphology adjustment and in situ compositing with graphene. Finally, a new microwave absorbing material with ultra-thin thickness, light weight, wide frequency band and strong absorption was obtained. This comprehensive experiment covers the entire experimental workflow, including synthesis and preparation, characterization and analysis, as well as performance testing. It integrates multidisciplinary knowledge from fields such as solid state physics, electromagnetics, material analysis and testing methods, as well as chemical synthesis and preparation. The experiment focuses on research hotspots and aligns with practical applications. By integrating education with scientific research during the teaching process, it aims to stimulate students’ enthusiasm and interest in experimentation. The experiment proposes a multi-stage and multi-dimensional assessment model. Through comprehensive evaluation at every stage, it aims to refine students’ experimental literacy and develop their abilities in independent thinking and innovative practice.