The exploration of transition metal based electrocatalyst for overall water splitting is becoming important as hydrogen becomes integral part of energy landscape. Recently, a new class of compounds i.e. layered double-hydroxides (LDHs), also known as anionic clays, are have shown tremendous promise for use as electrocatalyst. The lamellar morphology of LDHs accommodates higher active sites, that contributes to the facile electron transfer and thus attracts a great deal of interest in catalysis application. Moreover, the high catalytic activity of LDHs are also linked to their facile anion exchange, specific electronic structures, and versatile chemical compositions.

Herein, we have developed a series of ternary layered double hydroxide (LDH) using pH-adjusted co-precipitation method with varying ratio of Cu, Ni and Co, which are used as an electrocatalyst for overall water splitting. (Cu_3-xNi_x)Co₂-LDHs (x = 0, 1, 2, and 3) were systematically characterized using XRD, XPS, SEM, FTIR, TEM and BET techniques. The synergistic contributions from the electrocatalytically active metals and lamellar morphology of LDHs promotes water dissociation, facilitates faster release of H₂-O₂ gas bubbles, ameliorate electrolyte ion diffusion and improves electron transfer rate. It is further observed that the (Cu₂Ni)Co₂-LDH showed excellent electrocatalytic activity for both hydrogen evolution (HER) and oxygen evolution reaction (OER) with an overpotential of 147 and 218 mV for HER and OER, respectively at 10 mA cm^-2. Tafel slope was found to be lowest for (Cu₂Ni)Co₂-LDH. Further, the durability of the materials was also analysed by performing chronoampherometry for over 12 h. The overall water electrolytic cell using (Cu₂Ni)Co₂-LDH as both electrodes can reach 100 mA cm⁻² at 1.65 V with outstanding durability.