Note: Fixture for characterizing electrochemical devices in-operando in traditional vacuum systems

Whaley, Josh A.; McDaniel, Anthony H.; Gabaly, Farid El; Farrow, Roger L.; Graß, Michael; Hussain, Zahid; Li, Zhi; Linne, Mark; Bluhm, Hendrik; McCarty, K. F.

doi:10.1063/1.3479384

Cited by 41 publications

(51 citation statements)

References 15 publications

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“…41.4c, the real component of the device impedance is plotted versus temperature measured with a pyrometer, and the relative resistance is also shown during heating. These plots show that good contact is being made over the temperature range studied and the temperature dependence of the resistance measured is consistent with that of a Ni film used in the device as the upper electrode, indicating that most of the impedance is in the film [16]. …”

Section: Electrochemical Device Working In Uhvsupporting

confidence: 69%

Electrochemical Sources and Devices

Yates

2015

Experimental Innovations in Surface Science

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Section: Electrochemical Device Working In Uhvsupporting

confidence: 69%

Electrochemical Sources and Devices

Yates

2015

Experimental Innovations in Surface Science

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“…28). Our homebuilt sample holder provides both heating and electrical contacts 57 . The sample was mounted onto the heater with a wound Pt wire sandwiched in-between for electrical connection with the bottom (counter) electrode.…”

Section: Methodsmentioning

confidence: 99%

Fast vacancy-mediated oxygen ion incorporation across the ceria–gas electrochemical interface

et al. 2014

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Electrochemical incorporation reactions are ubiquitous in energy storage and conversion devices based on mixed ionic and electronic conductors, such as lithium-ion batteries, solidoxide fuel cells and water-splitting membranes. The two-way traffic of ions and electrons across the electrochemical interface, coupled with the bulk transport of mass and charge, has been challenging to understand. Here we report an investigation of the oxygen-ion incorporation pathway in CeO 2-d (ceria), one of the most recognized oxygen-deficient compounds, during hydrogen oxidation and water splitting. We probe the response of surface oxygen vacancies, electrons and adsorbates to the electrochemical polarization at the ceria-gas interface. We show that surface oxygen-ion transfer, mediated by oxygen vacancies, is fast. Furthermore, we infer that the electron transfer between cerium cations and hydroxyl ions is the rate-determining step. Our in operando observations reveal the precise roles of surface oxygen vacancy and electron defects in determining the rate of surface incorporation reactions.

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“…The characteristic information depth is estimated to be B1 nm as elaborated in the Supplementary Methods. The electrochemical cell was placed on a custom sample holder 51 equipped with a ceramic heater and Pt-Ir electrical probes, which contacted the microelectrode. For the cross-plane electrochemical cell, a wound Pt coil, placed between the heater and the cell, contacted the counter electrode.…”

Section: Electrochemicalmentioning

confidence: 99%

Redox activity of surface oxygen anions in oxygen-deficient perovskite oxides during electrochemical reactions

et al. 2015

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Surface redox-active centres in transition-metal oxides play a key role in determining the efficacy of electrocatalysts. The extreme sensitivity of surface redox states to temperatures, to gas pressures and to electrochemical reaction conditions renders them difficult to investigate by conventional surface-science techniques. Here we report the direct observation of surface redox processes by surface-sensitive, operando X-ray absorption spectroscopy using thin-film iron and cobalt perovskite oxides as model electrodes for elevated-temperature oxygen incorporation and evolution reactions. In contrast to the conventional view that the transition metal cations are the dominant redox-active centres, we find that the oxygen anions near the surface are a significant redox partner to molecular oxygen due to the strong hybridization between oxygen 2p and transition metal 3d electronic states. We propose that a narrow electronic state of significant oxygen 2p character near the Fermi level exchanges electrons with the oxygen adsorbates. This result highlights the importance of surface anion-redox chemistry in oxygen-deficient transition-metal oxides.

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Note: Fixture for characterizing electrochemical devices in-operando in traditional vacuum systems

Cited by 41 publications

References 15 publications

Electrochemical Sources and Devices

Electrochemical Sources and Devices

Fast vacancy-mediated oxygen ion incorporation across the ceria–gas electrochemical interface

Redox activity of surface oxygen anions in oxygen-deficient perovskite oxides during electrochemical reactions

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