Design and Application of a Gas Diffusion Electrode (GDE) Cell for Operando and In Situ Studies

Area of Science:

• Electrochemistry
• Materials Science
• Spectroscopy

Background:

• Understanding electrocatalytic processes under working conditions is crucial for developing efficient energy conversion technologies.
• Existing methods often lack the resolution or operando capabilities needed for detailed mechanistic studies.
• X-ray scattering techniques offer powerful insights into structural changes during catalysis.

Purpose of the Study:

• To present a novel electrochemical three-electrode Gas Diffusion Electrode (GDE) cell designed for operando and in situ X-ray scattering investigations.
• To optimize the cell design for minimal sample-detector distances required for comprehensive X-ray total scattering.
• To demonstrate the cell's capability in studying electrocatalytic reactions, such as the oxygen evolution reaction (OER), under high current densities.

Main Methods:

• Development and characterization of a specialized electrochemical flow-cell.
• Integration of the cell with X-ray scattering techniques, including Small Angle X-ray Scattering (SAXS), X-ray Diffraction (XRD), and Pair Distribution Function (PDF) analysis.
• Operando studies of electrocatalytic processes, specifically focusing on gas evolution phenomena.

Main Results:

• The optimized GDE cell facilitates minimal sample-detector distances essential for high-resolution X-ray total scattering.
• The cell's transparency aids in alignment, troubleshooting, and background correction during experiments.
• Successful demonstration of SAXS, XRD, and PDF analyses on electrocatalysts under reaction conditions.

Conclusions:

• The developed electrochemical GDE cell is a versatile tool for in situ and operando investigations of electrocatalytic processes.
• This setup enables detailed structural and mechanistic studies of catalysts during operation, particularly for reactions involving gas evolution.
• The cell design advances the capability to perform advanced X-ray scattering analyses on working electrodes.