Abstract: By refining scientific research results, the nickel complex with electrocatalytic hydrogen production activity was introduced into the comprehensive innovative experimental teaching of undergraduate. An ionic nickel(II) complex (Ni(bpy)₃Ni(mnt)₂) was prepared using 2,2'-bipyridine (bpy), 1, 2-dicyano-1,2' -dithiolene (mnt) and nickel chloride as raw materials. The complex was characterized by single crystal X-ray diffraction, infrared spectrum, electrospray ionization mass spectrometry, and ultraviolet-visible spectrum. The properties of electrocatalytic hydrogen production in organic phase and aqueous phase are systematically investigated. The results show that in a phosphate buffer solution with a low potential of −1.15 V, the amount of electrocatalytic hydrogen production of the complex in 4 hours was 0.386 mmol, and the TON is 2922.13 and the complex remains very good stability. This experimental project has simple synthesis steps, cutting-edge and comprehensiveness, covers many knowledge points and experimental technologies, which helps to establish green and low-carbon idea and cultivate students' innovation ability and scientific research ability.