A research-style laboratory experiment composed of the synthesis of MOF-74 materials, related structural characterization, and the cutting-edge application of electrocatalytic oxygen evolution reaction (OER) has been designed toward advanced undergraduates at East China University of Technology (ECUT). The desired monometallic MOF-74 (Ni-MOF-74 and Co-MOF-74) and bimetallic NiCo-MOF-74 were synthesized by students using cheap raw materials under mild reaction conditions. Students operated the modern instruments to perform powder X-ray diffraction (PXRD), Fourier transform infrared (FT-IR) spectroscopy, and thermogravimetric analysis (TGA) applied extensively in chemical research to explore whether the materials were successfully synthesized and the thermal stability under the guidance of the instructor. The electrocatalytic OER activity of bimetallic NiCo-MOF-74 was compared with monometallic Ni-MOF-74 and Co-MOF-74 to explore and understand the bimetallic synergy effect in MOFs materials. This experiment not only enabled students to master the solvothermal method for MOFs synthesis but also provided students the chance to operate several common chemical instruments and master their functions, realizing the application of theoretical knowledge to practice. Most importantly, this experiment helped students realize the importance of MOFs in the electrochemical energy fields and established a sense of teamwork by analyzing and discussing the bimetallic synergy effect in NiCo-MOF-74 for OER catalysis.