Binary metal hydroxides have tailored to quantum size in situ by manipulating the solvent medium in the co-precipitation process. Bimetallic cobalt-nickel hydroxide dots reveal hydrotalcite structure, and the mean hydrodynamic diameter is restricted to 2.5 nm when Co:Ni molar ratio 1:1. The bandgap values obtain around 2.64 eV using Tauc relation, which is within the quantum confinement region. The fitting results of X-ray photoelectron spectroscopy suggested the presence of redox couple Co 2+ , Co 3+ , Ni 2+ , and Ni 3+ in the hydroxides dots, which facilitates more electroactive sites. Again, excellent stability of hydroxide dots in solvent medium obtained by measuring T2 relaxation time. The binary dots electrode exhibits excellent pseudocapacitance performance with specific capacitance of 1926 F g À1 (221 mAh g À1 ) at 1 A g À1 with outstanding cycling retention of ~96% up to 20 000 cycles. Parallelly, an asymmetric supercapacitor device has been assembled by monitoring different mass loading of active material as +Ve and carbon black as ÀVe electrode cells. The ASC device utilizes to brighten a commercial LED to validate the electrode. Also, the specific capacitance of the ASC device has been calculated about 250 F g À1 (353 mAh g À1 ) with a holding energy density of 85 W h kg À1 .