A novel galvanostatic electrochemical technique has been employed to synthesize a cobalt-nickel mixed oxide, a binary metal oxide, via a two-step route involving electrodeposition followed by calcination. A diaphragm cell was used for the electro-deposition of the binary hydroxide at room temperature in which the electrolyte comprises a nitrate and/or sulphate bath of the corresponding metal ions at pH 4. The electrodeposited product was calcined at 300 °C to obtain the desired oxide material. The formation of the binary metal oxide has been confirmed by X-ray diffraction analysis. The scanning electron microscopy images associated with energy dispersive analysis (EDS) suggest the formation of a nanoporous sea sponge architecture consisting of an interconnected array of nanosheets aligned perpendicular to each other. The elemental mapping analysis of the binary oxide illustrated the uniformity in the distribution of Co and Ni in the composite material. The TEM image shows that binary oxides are nanocrystalline materials. A nitrogen adsorption-desorption study supports the pore size distribution behaviour of the synthesized material. The hybrid capacitor based on the binary metal oxide cathode and activated carbon anode displayed a capacitive behaviour with a capacitance of 76 F g-1 at a current rate of 2 mA with 98% efficiency after 1000 cycles. Due to the unique interconnected porous network and the role of binary cations, Co-Ni oxide exhibits superior electrochemical behaviour. The synthesis of binary oxides forming various morphologies, such as hexagonal, flower-shape, and sea sponge has been discussed.
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