A comparison between lead and silver electrodeposition onto fluorine-doped tin oxide (FTO) electrodes from nitrate solution was investigated in this work. Chronoamperometry has been used as an in situ technique to track the dynamics of the electrodeposition during advanced nucleation phases. The experimental results are correlated with a theoretical evaluation. It has shown that they have a strong correlation with each other. After that, the obtained deposits are characterized and compared as well by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), scanning electron microscopy (SEM), and impedance spectroscopy. The data reflects the effect of the material under investigation on current density, deposition density, and dielectric properties. Additionally, the electrodeposition approach (a two-in-one technique) can be followed in order to make well-controlled thin films that can be used for various purposes in addition to recovering heavy metals from wastewater.