Investigating the chemical nature of the adsorbed intermediate species on well-defined Cu single crystal substrates is crucial in understanding many electrocatalytic reactions. Herein, we systemati...

Early Stages of Electrochemical Oxidation of Cu(111) and Polycrystalline Cu Surfaces Revealed by in Situ Raman Spectroscopy.

Surface-enhanced infrared absorption spectroscopy is used to examine the co-adsorption of a selection of polyethers with Cl– under conditions relevant to superconformal Cu electrodeposition in CuSO...

SEIRAS Study of Chloride-Mediated Polyether Adsorption on Cu.

Copper (Cu) is a unique electrocatalyst, which is able to efficiently oxidize CO at very low overpotentials and reduce CO2 to valuable fuels with reasonable Faradaic efficiencies. Yet, knowledge of its electrochemical properties at the solid/liquid interface is still scarce. Here, we present the first two-stranded correlation of the potential of zero free charge (pzfc) of Cu(111) in alkaline electrolyte at different pH values through application of nanosecond laser pulses and the corresponding interfacial structure changes by in situ electrochemical scanning tunneling microscopy imaging. The pzfc of Cu(111) at pH 13 is identified at -0.73 VSHE in the apparent double layer region, prior to the onset of hydroxide adsorption. It shifts by (88 ± 4) mV to more positive potentials per decreasing pH unit. At the pzfc, Cu(111) shows structural dynamics at both pH 13 and pH 11, which can be understood as the onset of surface restructuring. At higher potentials, full reconstruction and electric field dependent OH adsorption occurs, which causes a remarkable decrease in the atomic density of the first Cu layer. The expansion of the Cu-Cu distance to 0.3 nm generates a hexagonal Moire pattern, on which the adsorbed OH forms a commensurate (1 × 2) adlayer structure with a steady state coverage of 0.5 monolayers at pH 13. Our experimental findings shed light on the true charge distribution and its interrelation with the atomic structure of the electrochemical interface of Cu.

The Potential of Zero Charge and the Electrochemical Interface Structure of Cu(111) in Alkaline Solutions.

Modelling the butterfly: (3×7) ordering on fcc(1 1 1) surfaces

The hydrogen evolution reaction (HER) has been crucial for the development of fundamental knowledge on electrocatalysis and electrochemistry, in general. In alkaline media, many key questions concerning pH-dependent structure-activity relations and the underlying activity descriptors remain unclear. While the presence of Ni(OH)2 deposited on Pt(111) has been shown to highly improve the rate of the HER through the electrode's bifunctionality, no studies exist on how low coverages of Ni(OH)2 influence the electrocatalytic behavior of Cu surfaces, which is a low-cost alternative to Pt. Here, we demonstrate that Cu(111) modified with 0.1 and 0.2 monolayers (ML) of Ni(OH)2 exhibits an unusual non-linear activity trend with increasing coverage. By combining in situ structural investigations with studies on the interfacial water orientation using electrochemical scanning tunneling microscopy and laser-induced temperature jump experiments, we find a correlation between a particular threshold of surface roughness and the decrease in the ordering of the water network at the interface. The highly disordered water ad-layer close to the onset of the HER, which is only present for 0.2 ML of Ni(OH)2, facilitates the reorganization of the interfacial water molecules to accommodate for charge transfer, thus enhancing the rate of the reaction. These findings strongly suggest a general validity of the interfacial water reorganization as an activity descriptor for the HER in alkaline media.

Interfacial Water Structure as a Descriptor for Its Electro-Reduction on Ni(OH)2-Modified Cu(111).

As a prototypical example of a metal-electrolyte interface the adsorption of sulfate on well defined Cu(111) single crystal electrodes from a 5 mM H 2 SO 4 solution has been studied by means of in-situ electrochemical scanning tunneling microscopy (EC-STM) and infrared reflection absorption spectroscopy (IRAS). The EC-STM images show the formation of the well-known Moire-like structure upon adsorption of sulfate on the Cu(111) surface. While IR frequency data fail to provide information about the anion adsorption site high-resolution STM images taken under specific tunneling conditions also clearly reveal the C 2v symmetry and the twofold bridging coordination of the sulfate adsorption complex. Analysis of the IR intensities, however, does show that the sulfate adsorption starts at a potential noticeably lower (less anodic) than the potential of first Moire formation. In this potential region the adsorbed sulfate is very mobile on the surface and difficult to image by STM. Adsorption rate and sulfate coverage are strongly dependent on the electrode potential. The slow adsorption process leading to a well ordered Moire structure is compared to a fast adsorption process by applying potential steps. Under the latter conditions no or only barely ordered sulfate adlayers are observed with STM. As shown by the IR measurements, however, the saturation coverage is hardly affected by the adsorption rate.

In‐situ Characterization of Metal/Electrolyte Interfaces: Sulfate Adsorption on Cu(111)

In situ and ex situ FTIR characterization of a cyanate adlayer on Cu(111)

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In‐situ Characterization of Metal/Electrolyte Interfaces: Sulfate Adsorption on Cu(111)

In situ and ex situ FTIR characterization of a cyanate adlayer on Cu(111)