Electrochemical characterization techniques are essential for studying and developing advanced materials across various fields, from corrosion science to energy storage, photovoltaics, and bioelectrochemistry. However, these techniques are often under-represented in educational curricula. This practical guide with a hands-on laboratory experiment introduces the Mott-Schottky technique to analyze the semiconductor properties of electrode surface. Through this experiment, students engage with core concepts such as the formation of the electrical double layer (EDL), the space charge region, and the relationship between capacitance and charge carrier density. They also learn the significance of the flat-band potential, gaining skills in calculating charge carrier density, identifying p-type or n-type behaviors, and assessing passive layer density, all of which are critical factors in evaluating the properties of semiconductor materials. Designed for senior undergraduate students, this experiment bridges theoretical knowledge and practical applications, preparing students for advanced research and industrial work in semiconductor electrochemistry and related fields.