Effect of total dose from X-ray irradiation on the coordination number (CN) of metallic Cu-Cu bonds. Credit: National Taiwan University

Operando X-ray spectroscopy is a powerful tool for probing electrocatalyst dynamics鈥攂ut intense X-ray exposure can distort structural insights. A recent article reveals flux- and dose-dependent artifact thresholds and proposes practical protocols to ensure accurate, artifact-free measurements.

What if the advanced techniques we rely on to study in action are, in some cases, distorting the phenomena we aim to observe?

Researchers at National Taiwan University and National Synchrotron Radiation Research Center have tackled this question head-on by revealing how intense X-ray beams used in operando studies can unintentionally alter catalyst structures鈥攕ometimes leading to misleading conclusions.

In a paper in Advanced Materials, the team systematically evaluated how photon flux, dose, and measurement conditions affect structural readings of copper-based electrocatalysts during CO2 reduction.

By comparing multiple synchrotron beamlines and carefully tracking coordination changes in Cu鈥揅u and Cu鈥揙 bonds, they uncovered critical thresholds beyond which X-ray-induced damage skews the data.

Their findings not only expose the hidden pitfalls of modern X-ray spectroscopy but also offer practical guidelines to preserve . This work sets a new standard for reliability in dynamic catalytic studies and provides a roadmap for ensuring operando measurements reflect chemistry, not artifacts.

"Operando X-ray spectroscopies are essential tools for probing electrocatalyst dynamics, yet intense X-ray exposure can introduce structural artifacts," said Prof. Hao Ming Chen.

"This study identifies - and dose-dependent damage thresholds and provides practical strategies鈥攊ncluding beamline selection and quick-scan modes鈥攖o ensure spectroscopic fidelity in electrochemical environments."

More information: Jiali Wang et al, Resolving Dynamic Behavior of Electrocatalysts via Advances of Operando X鈥怰ay Absorption Spectroscopies: Potential Artifacts and Practical Guidelines, Advanced Materials (2025).

Journal information: Advanced Materials