In situ electrochemical STM imaging of roughened gold and platinum electrode surfaces

Breuer, N.; Funtikov, A.M.; Stimming, Ulrich; Vogel, R.

doi:10.1016/0039-6028(95)00460-2

Cited by 22 publications

(16 citation statements)

References 13 publications

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“…Unfortunately it was not possible to derive direct structural information rom SEM imaging and Pb underpotential deposition (Figure S1, Supporting Information). Our conclusion of a preferential (100)‐type orientation of the annealed film would be consistent also with a report of Breuer et al., who based on STM observations arrived at similar conclusions for an annealed Au foil …”

Section: Resultssupporting

confidence: 93%

“…This indicates a reaction mechanism where OH ad is involved in the reaction, which at higher potentials/high OH ad coverages results in the 4‐electron pathway, while at lower potentials/lower OH ad coverages the 2‐electron pathway contributes increasingly. This reaction behavior closely resembles previous findings for Au(100) electrodes, which would be consistent also with the report of Breuer et al., who based on STM observations concluded on a preferential (100) orientation of their annealed Au film . The difference in reaction mechanism compared to the ORR in acidic electrolyte is documented also by the absence of a kinetic H/D isotope effect in alkaline electrolyte at potentials close to the onset of the reaction, meaning that under these conditions there is no coupled proton‐electron transfer acting as rate limiting step …”

Section: Resultssupporting

confidence: 92%

See 1 more Smart Citation

The Effect of Anions and pH on the Activity and Selectivity of an Annealed Polycrystalline Au Film Electrode in the Oxygen Reduction Reaction‐Revisited

Jusys

Behm

2019

ChemPhysChem

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Aiming at a better understanding of correlations between the activity and selectivity of Au electrodes in the oxygen reduction reaction (ORR) under controlled transport conditions, we have investigated this reaction by combined electrochemical and in situ FTIR measurements, performed in a flow cell set‐up in an attenuated total reflection (ATR) configuration in acid and alkaline electrolytes. The formation of incomplete reduction products (hydrogen peroxyde/peroxyls) was detected by a collector electrode, the onset of OHad formation was probed by bulk CO oxidation. Using an electroless‐deposited, annealed Au film on a Si prism as working electrode and three different electrolytes for comparison (sulfuric acid, perchloric acid, sodium hydroxide solution), we could derive detailed information on the anion adsorption behavior, and could correlate this with the ORR characteristics. The data reveal pronounced effects of the anions and the pH on the ORR characteristics, indicated e. g., by a grossly different activity and selectivity for the 4‐electron pathway to water/hydroxyls, with the onset ranging from ca. 1.0 V in alkaline electrolyte to 0.6 V in sulfuric acid electrolyte, and the selectivity for the 4‐electron pathway ranging from 100 % (alkaline electrolyte, low overpotentials) to 40 % (acidic electrolytes, alkaline electrolyte at high overpotentials). In contrast, the effect of the ORR on the anion adsorption characteristics is small. Anion effects as well as correlations between anion adsorption and ORR are discussed.

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Section: Resultssupporting

confidence: 93%

Section: Resultssupporting

confidence: 92%

The Effect of Anions and pH on the Activity and Selectivity of an Annealed Polycrystalline Au Film Electrode in the Oxygen Reduction Reaction‐Revisited

Jusys

Behm

2019

ChemPhysChem

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“…It shows 200 nm wide terraces and multiple steps of 6 nm height, which are partly pinned by a few impurities. Similar structures containing multiple step edges have already been identified for similarly treated samples by STM [8].…”

Section: Resultsmentioning

confidence: 81%

A scanning force microscope for in situ observation of electrochemical processes

Siebel¹,

Memmert²,

Vogel

et al. 1998

Applied Physics A: Materials Science & Processing

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A scanning force microscope (SFM) for electrochemical applications, based on an optical fiber interferometer for force detection, is developed. Cu bulk deposition and dissolution on polycrystalline Au samples were used to demonstrate the performance of the instrument. The time dependence of the nucleation and deposition of Cu grains and their dissolution was monitored by one-dimensional scanning during the reaction. The data show that SFM in an electrochemical environment can be used to investigate inhomogeneous processes in situ on the micron scale. Problems due to electrochemical processes occurring on the SFM cantilevers are, however, of significance and require special attention.

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“…However, LEED and AES require ultra‐high vacuum (UHV) conditions to operate and involve sample transfer from liquid electrolyte to UHV, which increases the chance of contamination and induces changes in the sample environment. Additionally, potential dependent changes on the surface (such as formation of intermediates or new layers) can be only recorded in‐situ under electrochemical conditions by means of e. g. EC‐STM, Raman and infrared spectroscopy, or ellipsometry . All above‐mentioned techniques yield insight into one structural or compositional (chemical) property at the time.…”

Section: Introductionmentioning

confidence: 99%

“…Unlike ellipsometry, XRR does not require preliminary information of the sample, such as refractive indices, and retains the signal intensity even in presence of electrolyte as an advantage of using hard X‐rays. GISAXS (Grazing Incidence Small Angle Scattering) measurements can be utilized for following surface morphological changes such as island formation . As GISAXS probes very small wave vector transfer ( Q ) values both perpendicular and parallel to the surface, it is sensitive to structures with periodicity between a few nm and a few hundreds of nm.…”

Section: Introductionmentioning

confidence: 99%

Synchrotron based operando surface X‐ray scattering study towards structure–activity relationships of model electrocatalysts

et al. 2016

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A novel combination of Surface X-ray Scattering techniques (SXS), i. e. GISAXS (Grazing-Incidence Small-Angle X-Ray Scattering), XRR (X-Ray Reflectivity) and SXRD (Surface X-Ray Diffraction) alongside with simultaneous detection of gaseous products by OLEMS (On-Line Electrochemical Mass Spectrometry) has been applied to study under operando conditions structure-activity relationships of a Pt model electrocatalyst.The SXS-OLEMS combination is able to follow dynamic changes in surface morphology and crystallography during water electrolysis. To showcase the combined SXS-OLEMS setup for operando studies of electrode transformations, H 2 and O 2 evolution reactions (HER and OER) on a Pt model electrocatalyst and their dependence on type and degree of surface roughening have been investigated.

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In situ electrochemical STM imaging of roughened gold and platinum electrode surfaces

Cited by 22 publications

References 13 publications

The Effect of Anions and pH on the Activity and Selectivity of an Annealed Polycrystalline Au Film Electrode in the Oxygen Reduction Reaction‐Revisited

The Effect of Anions and pH on the Activity and Selectivity of an Annealed Polycrystalline Au Film Electrode in the Oxygen Reduction Reaction‐Revisited

A scanning force microscope for in situ observation of electrochemical processes

Synchrotron based operando surface X‐ray scattering study towards structure–activity relationships of model electrocatalysts

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