Electrochemistry is a study of the correlation between applied or measured electrical potential and corresponding chemical changes, or vice versa. Different voltammetry techniques have been developed to measure the potential, charge or current of electrochemical systems for analytical and characterization purposes. I have been employed several voltammetry techniques such as cyclic voltammetry, square wave voltammetry, chronopotentiometry as well as electrochemical impedance spectroscopy (EIS) to obtain a clear insight into the interfacial electrochemical behavior between the designed electrode and electrolytes. Particularly, I use cyclic square wave voltammetry method to study the mechanism of electron transfer of electroactive materials in different electrode/electrolyte interfaces.