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Electrochemical IR Spectroscopy Apparatus with Liquid/Solid-Interface-Preparation

Subject Area Chemical Solid State and Surface Research
Term Funded in 2014
Project identifier Deutsche Forschungsgemeinschaft (DFG) - Project number 259673620
 
Final Report Year 2019

Final Report Abstract

As part of the project, a novel large-scale instrument was developed that combines the preparation of ultra-clean, atomically well-defined model surfaces under ultrahigh vacuum (UHV) conditions with a direct, contamination-free transfer into an electrochemical measurement environment. This setup enables, for the first time, in situ IR spectroscopic investigations under electrochemical control on electrodes that have been prepared using surface-science methods in UHV. In addition, procedures were developed that couple UHV preparation with further electrochemical characterization techniques, thereby opening up experimental access to well-defined model electrocatalysts. A key advance lies in the fabrication of complex, atomically defined model electrodes that are not accessible by conventional methods. Following commissioning, the system was initially used to investigate oxide-stabilized electrocatalysts, which allow a reduction in the use of noble metals by stabilizing very small metal particles. Using a model system (Pt nanoparticles on a cobalt oxide film), it was demonstrated that both the oxide support and the metal particles retain their atomic structure during transfer between UHV and the electrochemical environment. This was made possible by the newly developed transfer infrastructure as well as specifically adapted experimental protocols for contamination-free, structure-preserving transfer. The achieved instrumental and methodological advances enable, for the first time, systematic kinetic and mechanistic studies on such model surfaces. Pronounced particle size effects were identified, which can be attributed to the precisely adjustable particle size under UHV conditions. Furthermore, the combination of investigations under UHV and electrochemical conditions led to qualitatively new mechanistic insights. In particular, a novel reaction mechanism at oxide-stabilized electrode interfaces was demonstrated, in which the oxide support not only provides structural stability but also actively participates in the reaction, for example through the activation of oxygen species. Such metal–support interaction effects were previously known only from heterogeneous catalysis and were observed here for the first time under electrochemical conditions. The results led to high-impact publications and formed the basis for a wide range of subsequent studies, all of which relied on the UHV-based preparation developed in this project. In addition, the instrument was successfully employed in collaborative projects, for example for in situ investigations of alloy catalysts for fuel cells as well as of molecular systems for the electrochemical storage of solar energy. Overall, the developed system represents a versatile and powerful platform that enables new experimental approaches in fundamental research.

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