This study is the first attempt to examine the electrochemical properties of TiO2 composite with Fe3O4 thin film. In our analysis, X-Ray diffraction (XRD) confirms the formation of Fe3O4 on TiO2. Fourier Transform Infrared Spectroscopy (FT-IR) and Raman spectroscopy confirmed the functional groups. The UV–Vis spectroscopy analysis shows that the addition of Fe3O4 results in decrease in optical band gap. Our Cyclic Voltammetry (CV) results demonstrate that, under steady state conditions, the behaviors of TiO2 and Fe3O4/TiO2 electrodes regarding ion adsorption and charge transmission vary. Pseudocapacitive effects and charge transfer affects the functionality of the TiO2 electrode, whereas two-layer capacitance effects primarily control the response of the Fe3O4/TiO2 electrode. Numerous factors, including ion diffusion, rate capability, charge transfer, and series resistance, can be directly determined using electrochemical impedance spectroscopy (EIS). The experimental results and analysis presented in this work brings to light the significance of Fe3O4 in the electrochemical response of an electrode-electrolyte interface.