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Potential-dependent surface structures of Au(111) and Au(100) single-crystal electrodes in a 50 mM H2SO4 solution were investigated at an atomic level using in situ surface X-ray scattering (SXS) techniques. It was confirmed that both the Au(111) and Au(100) surfaces were reconstructed with an attached submonolayer of an oxygen species, most probably water, at 0 V (vs Ag/AgCl). Results at +0.95 V supported a previously suggested model for both the Au(111) and the Au(100) electrodes that, based on infrared and scanning tunneling microscopy measurements, the surfaces were a (1 x 1) structure with the coadsorbed sulfate anion and hydronium cation (H3O+). At +1.05 V, where a small amount of an anodic current flowed, adsorption of a monolayer of oxygen species was observed on both surfaces. When the single-crystal gold electrodes were electrochemically oxidized at +1.40 V, the expansion of the gold surface by about one monolayer of Au atoms was observed, suggesting the penetration of oxygen into the surface gold layers (i.e., the formation of two layers of surface oxide). When the surface oxide was reduced at +0.65 V, the surface structure returned back to the structure observed at +0.95 V before the oxide formation (i.e., a (1 x 1) structure with coadsorbed sulfate anion and H3O+). When the potential was reduced to 0 V, the surfaces were reconstructed again but with slightly more random structures than those before the potential cycle

the journal of physical chemistry c

Structure of Au(111) and Au(100) Single-Crystal Electrode Surfaces at Various Potentials in Sulfuric Acid Solution Determined by In Situ Surface X-ray Scattering