Water splitting is an area of research which is of pressing interest in addressing climate change. Water splitting provides oxygen and hydrogen as products, with hydrogen finding use as a potential high-density fuel to replace fossil fuels. Water splitting manifests as two half-cell reactions, namely the anodic oxygen evolution reaction and the cathodic hydrogen evolution reaction. The purpose of this project is to synthesise a bifunctional electrocatalyst to use in the water splitting reaction, replacing the rare and expensive transition metals catalysts currently in use such as platinum and ruthenium. The ideal material would exhibit strong performance for both the oxygen evolution reaction and the hydrogen evolution reaction.In this project, Layered Double Hydroxides (LDHs) have been synthesised for use in water splitting. LDHs are a group of ionic compounds characterised by their layered structure of positively charged sheets and an interlayer region consisting of the corresponding anions. LDHs typically contain a bivalent and a trivalent metal as part of the generic formula [M2+ 1–xM3+ x(OH)2][An–]x/n·zH2O. In this project the bivalent metal in use is typically cobalt and the trivalent metal is typically iron. The synthesis developed is a simple, one pot hydrothermal synthesis which can be seen in Figure 1. In this synthesis, the process begins with the precursor materials dissolved in solution. These solutions are mixed and stirred until homogenous. The resultant solution is then heated to form an impure product. Following washing steps and centrifugation a purified powder product is obtained. A variety of metallic salts have been tested for their use in these LDHs with the optimum LDHs selected for further study. The metallic salts used to provide the metals for the LDHs are typically hydrated transition metal nitrates.The LDHs have been characterised and their structure confirmed by a variety of analytical techniques including X-Ray Diffraction and Scanning Electron Microscopy. Simple qualitative analysis has been performed with FTIR spectroscopy. These LDHs have been immobilised on a variety of porous, high surface area materials, including nickel foam and copper foam, to enhance the properties seen in the screening study. These materials allow synthesis of high surface area, reactive electrocatalysts. To enhance the stability of the LDHs, carbon materials have been integrated with the LDHs. Examination of a variety of carbon materials involved post-synthesis mixing of the carbon material and the LDH product or inclusion of the carbon material in the LDH synthesis to form a composite. A variety of carbon materials have been analysed including graphene oxide, carbon black and carbon nanotubes. Figure 1