Abstract: As a fundamental component of physical chemistry and instrumental analysis, electrochemical theory finds practical application in supercapacitor performance evaluation. This study initially synthesized the (NH₄)₆[NiMo₉O₃₂]·6H₂O polyoxometalate precursor, followed by the hydrothermal synthesis of Ni(OH)₂-NiMoO₄/NF electrode material. The supercapacitor performance was subsequently evaluated using an electrochemical workstation. The experimental procedure integrates knowledge from inorganic chemistry, physical chemistry, and instrumental analysis, representing a comprehensive, interdisciplinary innovation experiment. This approach enhances students’ theoretical understanding, improves experimental skills, facilitates data processing, bridges theory with practical applications, stimulates research interest, and cultivates problem-solving abilities and innovative thinking.

Key words: Electrochemistry, Polyoxometalates, Supercapacitors, Electrode material, Comprehensive experiment