In this study, the nickel phosphate hydrate (NiPh) microplates are deposited on 3D Ni-foam by a facile hydrothermal method. The microstructures of NiPh electrodes vary with hydrothermal reaction time (2, 4 and 6 h) at the constant reaction temperature. The structural, morphological and electrochemical characterizations of the NiPh electrodes were systematically studied. X-ray diffraction (XRD) study reveals a monoclinic crystal system of NiPh material with an I2/m space group. The scanning electron microscopy (SEM) analysis shows plates like microstructures. The electrochemical measurements of NiPh electrodes were carried out in 1 M KOH electrolyte in −0.2 to 0.55 V vs SCE potential window. NiPh (deposited at 2 h reaction time) electrode shows the specific capacitance of 855.11 F/g (178.18 mAh/g) at 10 mA/cm2 current density. It is speculated that NiPh deposited on Ni-foam can be an efficient electrode material for energy storage applications.