The electrolysis of water to produce hydrogen is a critical step in many green chemistry processes. The key to the efficiency of water electrolysis is the synthesis of an appropriate electrocatalyst. Three-dimensional (3D) printing is an increasingly important part of many industrial processes. In this study, we propose an efficient laboratory experiment to synthesize a 3D-printed, hydrophilic, conductive, and monolithic electrocatalyst for the hydrogen evolution reaction (HER). Students learn to assemble an electrochemical cell, conduct electrodeposition, and evaluate HERs on both a 3D-printed electrode and traditional nickel foam. In this experiment, students learn to understand fundamental electrochemical principles and test techniques, including cyclic voltammetry and linear-sweep voltammetry, and analyze the relation between the catalytic performance and electrocatalyst compositions. This study also broadens the utilization of 3D printing in catalysis, energy production, organic chemistry, and chemical reaction engineering courses by leveraging the unique properties of 3D-printed materials.