This paper describes a totally electrochemical process for the fabrication and functionalization of high‐surface‐area, nanoporous gold films. The fabrication process involves the electrodeposition of a binary gold–zinc alloy at gold wires, followed by subsequent electrochemical dealloying of the less noble component zinc from the surface. Both the deposition and dealloying steps are conducted in a single low‐temperature bath of 40.0–60.0 mol‐% zinc chloride–1‐ethyl‐3‐methylimidazolium chloride ionic liquid at 120 °C without using any other corrosive acids or bases. The porous structure and morphology of the nanostructured gold film could be controlled by electrochemical variation of the composition of the Au–Zn surface alloy. It is demonstrated that the nanoporous gold surface can be successfully functionalized with self‐assembled monolayers of L‐cysteine. Such functionalization greatly improves the utility of the nanoporous gold, as is demonstrated in the sensitive and selective determination of Cu(II).

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The electrodeposition of aluminium is demonstrated using a eutectic mixture of aluminium chloride and urea. The mixture is shown to be conducting through the formation of both cationic ([AlCl2·urean](+)) and anionic (AlCl4(-)) species and electrodeposition is achieved through the cationic species. The use of a biphasic system with the ionic liquid and a protective hydrocarbon layer allows metal deposition to be carried out in an environment with ambient moisture without the need for a glove box. A direct comparison is made between the AlCl3:urea and imidazolium chloride:AlCl3 systems and the differences in speciation and mass transport manifest themselves in different deposit morphologies. Brighteners which work in the chloroaluminate system such as toluene and LiCl are shown to be ineffective in the urea based system and the reasons for these differences are ascribed to the mechanism of the anodic reaction which is rate limiting.

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