08. June 2026

Radiation damage or intrinsic material change?

PTB study reveals dose limits for reliable X-ray analysis of battery materials

Diagram of the investigation with arrows and text blocks

Diagram of the systematic investigation into the influence of radiation on the results of X-ray analytical measurements. © PTB

X-ray radiation provides insight into the chemical changes in battery materials during battery operation ("operando"), but is also the cause of radiation-generated effects that can superimpose and falsify measurement results. In a case study on selected polymer-based solid-state electrolyte materials for lithium-sulphur batteries, a systematic strategy for avoiding radiation damage in X-ray analytical examination methods was demonstrated.

X-ray spectroscopy is widely used in materials science and provides valuable insights into the elemental composition, chemical state and structure of materials. Consideration of the effects of the X-rays used on the sample is crucial to distinguish between radiation-induced effects and material properties, to avoid misinterpretation and to improve the reliability of experimental results.

Using synchrotron radiation, Near Edge X-Ray Absorption Fine Structure (NEXAFS) spectroscopy was used to investigate the dose-dependent X-ray induced changes in the battery material. Structural changes could be correlated with the absolute radiation dose and thus limit values could be determined.

Measurement of the sulphur absorption edge in the polymer and sulphur-containing salt electrolyte layers under investigation revealed a two-step reduction of the sulphonyl groups to sulphides in the investigated electrolyte layers of polymer and sulphur-containing salt. At induced doses of approximately (200 ± 8) kGy, a reduction of (1,2 ± 0,1) % of the original sulphur species was detectable. An effect of the measurement on the polymer matrix was excluded.

Based on the calculated doses and the determined photon flux, the results could also be extrapolated to other experiments and material compositions. Interpretation of the induced structural changes allows to estimate the impact on functionality and the definition of real thresholds for induced doses to optimally plan operando experiments.

Publication:

ACS Energy Letters 2026: Facing X-ray Radiation Damage Systematically: A Quantitative Investigation on Solid-State Electrolytes for LiS Batteries
Lena K. Mathies, Katja Frenzel, Adrian Jonas, Sebastian Risse, and Burkhard Beckhoff
https://doi.org/10.1021/acsenergylett.6c00098