Monitoring and quantifying morphological and structural changes in electrode materials under operando conditions

Marcus Fehse*, Matteo P. Hogan, Sally Hiu Tung Pang, Oliver Blackman, Erik M. Kelder, Alessandro Longo, Maria Alfredsson

*Corresponding author for this work

Research output: Contribution to journalArticleScientificpeer-review

2 Citations (Scopus)
13 Downloads (Pure)


X-ray absorption and small-angle x-ray scattering spectra were simultaneously acquired under operando conditions in a joined technique approach, for the first time applied in the field of energy storage materials. This approach allows one to closely follow the electronic and local structure evolution, as well as monitor and quantify the morphological and nanostructural changes occurring during electrochemical cycling. Here we demonstrate its potential on the example of doped and non-doped Fe2O3 anode material vs. Li. Our results reveal that upon discharge Fe3+ is gradually reduced to the metallic state and segregated as nanoparticles. For the relithiation reaction, upon subsequent charge, we observe improved reversibility for the Sr-doped compared to non-doped and Ca-doped Fe2O3. We highlight that this combined technique approach is a reliable, facile and powerful tool to investigate electrode materials under realistic cycling condition. It provides an unbiased and holistic picture of the morphological and structural changes occurring during operation, which allows for adequate material tailoring.

Original languageEnglish
Article number228685
Number of pages8
JournalJournal of Power Sources
Publication statusPublished - 2020


  • Conversion reaction
  • FeO
  • Operando characterization
  • Small-angle x-ray scattering
  • X-ray absorption spectroscopy


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