Abstract
An electrochemical three-electrode flow-cell is presented for in situ small-angle X-ray scattering (SAXS) and X-ray absorption spectroscopy (XAS) experiments in transmission mode at synchrotron X-ray sources. The cell also allows for in situ XAS performed in fluorescence mode. Constant experimental conditions, even under moderate gas evolution, are provided by the electrolyte flow with controlled gas saturation. A special configuration of working and counter electrode, respectively, yields low residual ohmic resistance in three-electrode measurements that enables the study of thick porous electrodes of active high surface area materials. The cell proved its functionality and reliability in two studies: First, an in situ anomalous SAXS experiment for the high-potential degradation properties of a Pt/IrO2-TiO2 catalyst for the oxygen reduction reaction at polymer electrolyte fuel cell cathodes; and second, an in situ XAS study of the electronic state of Ir centers inside an IrO2-TiO2 catalyst under oxygen evolution conditions.
Highlights
Modern research in electrocatalysis makes extensive use of in situ X-ray techniques that provide information about the structure and the electronic state of catalyst materials under electrochemical potential control
The most common technique applied for this purpose is transmission electron microscopy (TEM), which has the convenient advantage that changes of the Pt nanoparticle structure can be directly visualized, especially with the use of identical location TEM (IL-TEM).[5]
In situ anomalous small-angle X-ray scattering (SAXS) results: Pt/IrO2-TiO2 degradation.—In situ SAXS curves of the bare IrO2-TiO2 support material without Pt nanoparticles are shown in Figure 5 at an early stage and at the end of the degradation protocol
Summary
Modern research in electrocatalysis makes extensive use of in situ X-ray techniques that provide information about the structure and the electronic state of catalyst materials under electrochemical potential control. In this publication (Part I.), we present in detail the design of an electrochemical three-electrode flow-cell for in situ SAXS and XAS experiments in liquid electrolytes at synchrotron X-ray sources.
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