A versatile electrochemical cell for the preparation and characterisation of model electrocatalytic systems

Abstract

An electrochemical cell for the controllable modification and comprehensive electrochemical characterisation of model electro-catalytic surfaces has been developed. In-depth electrochemical characterisation of stationary electrodes as well as rotating disc electrode (RDE) measurements in hanging meniscus configuration becomes possible. Additionally, the temperature of the electrodes in contact with electrolytes can be accurately controlled between room temperature and 70–80 °C. It is of particular importance for model electro-catalytic studies that in one experimental set-up (i) electrochemical metal and non-metal deposition to adjust the amount of the foreign atoms at the surface, (ii) controllable thermal treatment to vary the position of these atoms at the surface and subsurface regions, and (iii) state-of-the-art techniques common in electrocatalysis to characterise the resulting samples are possible. The deposition and annealing procedures under various atmospheres allow accurate control over the position of the foreign atoms at the electrode surface as overlayers, surface alloys and sub-surface (or near-surface) alloys, where the solute element is preferentially located in the second atomic layer of the host metal. The cell enables us to perform all operations without exposing the samples to the laboratory atmosphere at any of the experimental stages. To demonstrate the performance and advantages of the developed cell, we use model experiments with Pt(111) single crystal electrodes and Pt(111) surfaces modified with (sub)monolayer amounts of copper.