Hydrogen production from electrochemical water splitting via hydrogen evolution reaction (HER) powered by sustainable energy has been recognized as one of the most promising alternatives to traditional fossil fuels. To integrate the fundamental knowledge of chemistry, electrochemistry, and materials science with practical application and scientific frontier, we propose an experiment design to prepare the HER electrodes and evaluate their electrochemical performance for materials science undergraduate students. The experiment has been carried out in a materials science comprehensive laboratory with conventional equipment and nontoxic chemicals. The experimental design covers the mechanism of water splitting, reaction routes in HER, the crystal structure of electrocatalyst, preparation protocol of electrode, electrochemical evaluation methods as well as the relationship between them, which would offer a new idea to deliver cutting-edge concepts related to new energy materials and devices to the students and design electrocatalysts with outstanding comprehensive properties for future green hydrogen production.