In Situ Electrochemical Cells to Study the Oxygen Evolution Reaction by Near Ambient Pressure X-ray Photoelectron Spectroscopy

Abstract

In this contribution, we report the development of in situ electrochemical cells based on proton exchange membranes suitable for studying interfacial structural dynamics of energy materials under operation by near ambient pressure X-ray photoelectron spectroscopy. We will present both the first design of a batch-type two-electrode cell prototype and the improvements attained with a continuous flow three-electrode cell. Examples of both sputtered metal films and carbon-supported metal nanostructures are included demonstrating the high flexibility of the cells to study energy materials. Our immediate focus was on the study of the oxygen evolution reaction, however, the methods described herein can be broadly applied to reactions relevant in energy conversion and storage devices.

The rise of electrochemical NAPXPS operated in the soft X-ray regime exemplified by the oxygen evolution reaction on IrOx electrocatalysts

“…Because of this fact, the electrified interfaces are inaccessible directly to the common surface sensitive techniques like photoelectron spectroscopy, requiring new experimental strategies for their operation under these conditions [12]. Recently different approaches were developed enabling the investigation of the electronic structure variation of electrodes under potentiostatic control using near ambient pressure X-ray photoelectron spectroscopy (NAPXPS) [13], from gas phase up to bulk aqueous electrolyte [11,12,[14][15][16][17][18]. Some of the most extensively used approaches entail the use of hard X-rays to allow the photoelectrons to escape through thick electrode membranes [19] (a few nanometers thick) or thin film electrolytes [20].…”

Stamping Nanoparticles onto the Electrode for Rapid Electrochemical Analysis in Microfluidics

“…Cyclic voltammetry (CV) is an electrochemical method that measures the current in an electrochemical cell while cycling the potential of the working electrode (WE) [ 6 ]. Microfluidic electrochemical cells enable similar CV studies of micro- and nanomaterials [ 7 , 8 , 9 ].…”

Essentials of High Performance Water Electrolyzers – From Catalyst Layer Materials to Electrode Engineering

“…[58] In order to decouple the contributors to performance losses, and provide a more realistic picture of the degradation phenomena involved, in situ and in operando studies are paramount as shown for OER model systems. [89][90][91] A recent study from Kang et al used gold ribbon sense wires to measure though-plane voltage losses under cell operation. [92] These confirmed that CCMs, specifically the CL/PTL interfacial contact resistance, have the highest contribution in high-frequency resistance losses: 100-fold than that of anode and cathode current collectors.…”