The aim of this thesis is to demonstrate the feasibility of a new technology developed in MNT group consisting on fabrication Metal-Insulator-Metal (MiM) capacitor by using electrospray technique. First an overview of the electrospray technique is introduced, and how 3D self assembled structures and colloidal crystals are attained by using the mentioned technique. Electrical Double Layer Capacitance (EDLC) theory is also explained. Once the previous is clarified, the fabrication procedure of MiM capacitor is detailed. Two alternatives have been tested: In the first capacitor Polystiene nanoparticles are deposited as insulator, on the contrary SiO2 nanoparticles are deposited in the second MiM capacitor. The Polystirene and SiO2 nanoparticles capacitors are measured by using impedance spectroscopy. The measurement setup is also exposed, and finally, results showing the supercapacitor behavior are exposed and discussed by comparing them with previous published works.