Binary skeletal metal catalysts were made by starting with a ternary alloy. The precursor alloys and catalysts were characterised using Optical Microscopy, X-ray Diffractometer, Scanning Electron Microscopy, Inductively Coupled Plasma (ICP) and BET surface area in term of morphologies, phase identification, surface area and pore structure. Skeletal copper catalyst presented high surface areas and consisted primarily of CuAl2 grains, with small well-dispersed areas of the Al-CuAl2 eutectic. The CuAl2 phase, which represented a tetragonal structure, showed large cell volumes resulted in a fine skeleton structure. Binary nickel-copper catalyst composed of three majority phases including Ni2Al3, Cu4NiAl7 and Al. The Cu4NiAl7 was found to be a caustic resistant phase which led to low surface area in the nickel-copper catalyst In terms of the selective removal of aluminium from the copper-cobalt-aluminium alloy to create the binary copper-cobalt catalyst, 11 alloy samples with various compositions were produced following the ternary phase diagram. The surface area and pore size of these catalysts was dependant on the crystal structure of the phases present and the amount of remaining Al. Electrochemical glucose oxidation and carbon dioxide reduction activity have been used for testing the catalyst performance. The electrochemical oxidation of glucose experiment using 11 samples of skeletal Cu-Co catalyst as an electrode showed the results that the significant oxidation peaks were observed in sample 1, 4, 8, 9 and the small oxidation humps were observed in other sample except sample 2. These small peaks resulted from that the glucose molecule had difficulty to absorb on the surface area of the skeletal Cu-Co catalysts electrode. The difficulty may results from very fine pore volume and pore size of the catalysts. In term of assessing the skeletal Cu-Co catalyst with electrochemical reduction of carbon dioxide experiment, the skeletal Cu-Co catalyst sample 7 which presented the highest surface area was selected as an electrode to compare with Cu foil electrode. The result of using skeletal Cu-Co as an electrode indicated significantly higher current. This results from that a skeletal Cu-Co catalyst electrode presented an actual high surface area which leads to more adsorbed regions.