Publication date: 6th November 2020
Developing new materials with improved catalytic properties is one of the most critical challenges facing the sustainable production of clean and renewable energy sources. In order to achieve this long-standing goal, an atomistic understanding of the processes that place at the electrode-electrolyte interface is required. Here we introduce our customized experimental set-up, Fig. 1 (a), which enables structural, chemical and electrochemical characterization on exactly the same sample, by allowing the transfer of the catalyst from ultra-high vacuum (UHV) –compatible with surface science techniques- to an electrochemical cell in a controlled argon gas atmosphere. This optimized approach enables the direct correlation between the surface composition (X-Ray photoemission spectroscopy, XPS) and structure (Low energy electron diffraction, LEED, and Scanning tunneling microscopy, STM) at the atomic scale, and the macroscopic response of the catalyst (Cyclic Voltammetry, CV, Linear Sweep Voltammetry, LSV, and Chronoamperometry, CA.).
We applied experimental approach to study the potential induced structure changes during the electrochemical oxidation of Au(111) in 0.05M H2SO4, which results in the formation of an oxide film that influences the catalytic performance of the material. Surface electrooxidation of gold on acidic media is a widely discussed problem, involving different processes such as adsorption of (bi)sulfatesurface ions, competitive hydroxile adsorption, formation of gold surface (hydr)oxides by OH or O exchange with metal atoms and subsequent growth of a bulk oxide1–3. Combining ex-situ XPS and LEED characterization before and after potential steps we have monitored the surface changes within electrochemical window, Fig. 1 (b) up to oxide formation near the Oxygen Evolution Reaction (OER) potential.