An integrated inorganic chemistry laboratory experience focusing on heterogeneous electrocatalysis with nickel (Ni)- and cobalt (Co)-based electrocatalysts is designed for upper-division, major-level chemistry students. In this laboratory, students will be guided through the fabrication of an indium tin oxide (ITO)-coated glass working electrode, electrodeposition of the nickel hydroxide (Ni(OH)[subscript 2]) and cobalt hydroxide (Co(OH)[subscript 2]) electrocatalysts on the ITO working electrodes, and the electrochemical characterization of the electrocatalysts. Students will investigate the electrocatalytic oxygen evolution reaction (OER) with electrocatalysts Ni(OH)[subscript 2] and Co(OH)[subscript 2] in an alkaline electrolyte. Cyclic voltammetry (CV) is the major experimental technique students will apply to measure the performances of different electrocatalysts on the OER activities. Additionally, a Python-based simulation of the cyclic voltammograms will be applied to help students gain more insights about the interpretation of the cyclic voltammograms of reversible one-electron redox reactions.