In this investigation, nickel hydroxide Ni(OH) 2 based nanostructured materials were synthesized by simple and low cost free template hydrothermal method at two different growth temperatures with and without SDS surfactant. The X-ray diffraction, Raman spectroscopy and field emission scanning electron microscopy analysis confirmed the formation of β-Ni(OH) 2 pure brucite crystalline phase in spherical nanoparticle morphology with an average diameter ranging from 8 to 27 nm. In the second step, these nanospherical agglomerated hydroxide particles with activated carbon addition were performed as electroactive materials deposited on nickel foam current collector as working electrodes. The electrochemical tests in a three-electrode configuration using 6 MKOH electrolyte show that the best electroactive NPs (β bc-Ni(OH) 2 and β-Ni(OH) 2 obtained at optimized conditions, have a maximum specific capacitance (C s) of 4697 F g −1 and 3431 F g −1 at 5 mV s −1 scan rate with a specific capacity (Q s) of 744 mAh g −1 and 618 mAh g −1 at 1 A g −1 current density with an R s of about 0.24 and 0.28 Ω, respectively. At 30 A g −1 after 1700 cycles, the coulombic retention is around 99.06% (or capacity retention 109 mAh g −1), demonstrating remarkable cycling stability for Ni based hydroxide.