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Toward reliable probing of electrocatalysts: Identifying X-ray-induced artifacts in operando spectroscopy

Operando X-ray spectroscopy is a powerful tool for probing electrocatalyst dynamics—but 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 catalytic materials 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—sometimes 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–Cu and Cu–O 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 data integrity. 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 flux- and dose-dependent damage thresholds and provides practical strategies—including beamline selection and quick-scan modes—to ensure spectroscopic fidelity in electrochemical environments."