To improve the specific capacitance, power and energy of electrical energy storage devices, in particular hybrid capacitors, various methods of cathode material modification are used. One of the methods of modifying nanostructured materials without applying high temperatures, pressures and long reaction times is ultrasonic treatment. Although the interaction of ultrasound with the structure and surface of electrode materials is well enough studied, there are few works that investigate the optimal duration of ultrasonic treatment and its relationship with the capacitive characteristics of these materials. Therefore, we investigated the efficiency of ultrasonic dispersion of nanocrystalline nickel molybdate hydrate for 15, 60 and 90 minutes. The appearance of two cathodic peaks on cyclic voltammetry patterns was analyzed and the charge / discharge mechanism of the electrode based on nanocrystalline NiMoO4 hydrate was presented. Based on the results of potentiodynamic and galvanostatic studies the specific capacitances of the initial NiMoO4 and the material modified by ultrasound for 15, 60 and 90 minutes were calculated. The proton diffusion coefficients of nickel molybdate hydrate were determined on the basis of the Randles–Sevcik equation. NiMoO4 subjected to ultrasonic dispersion for 60 min as a cathode material in a hybrid electrochemical system was tested.