To meet the requirements for cultivating students’ comprehensive practical and innovative abilities under the background of the Emerging Engineering Education, this paper designs an integrated comprehensive experiment for water electrolysis hydrogen production covering catalyst preparation, structural characterization and performance testing. Taking the development of NiFeOx electrocatalysts as the carrier, the experiment integrates three modules: combustion synthesis, electrochemical measurement and Raman spectroscopy characterization. Guided by the strategic background of hydrogen energy, students systematically master the methods of catalyst design, performance evaluation and structural analysis, and deeply understand the “structure-performance” relationship. The experiment content is closely integrated with cutting-edge scientific research and the regional characteristics of abundant renewable energy in Xinjiang, emphasizing the deep integration of theory and practice. Through task-driven and group cooperation, it is suitable for undergraduate comprehensive experimental teaching of materials, chemistry, energy and other related majors. It effectively improves students’ material design ability, instrument operation skills and data analysis literacy, and provides an operable teaching case for cultivating high-quality material talents with innovative thinking and the ability to solve complex engineering problems.