Non-Monotonic Structural Response of Co3O4 during Calcination
Calcination is widely applied to adjust crystallinity and defects in metal oxides. However, structural evolution is often assumed to follow a monotonic temperature dependence. Here, we demonstrate that the structural response of Co3O4 to calcination is significantly more complex. Using a multi-modal approach combining diffraction, microscopy, spectroscopy, and defect-sensitive analysis, we track the structural evolution across multiple scales from 300–600 °C. While average crystallographic descriptors evolve monotonically with temperature, defect-associated features exhibit pronounced non-monotonic behaviour, revealing asynchronous evolution across structural levels. A distinct structural turning emerges at 400 °C, where found the metastable Co3O4. This state is characterized by enhanced local disorder and a distinct combination of various defects within spinel matrix. The results reveal that calcination does not induce a monotonic ordering pathway but activates coupled asynchronous structural processes. Our work highlights the importance of multiscale structural characterization for understanding and controlling the complex structures of oxide nanomaterials.
Authors
- Malte Behrens (ORCID: https://orcid.org/0000-0003-3407-5011)
- Nicolas Cosanne (ORCID: https://orcid.org/0009-0003-0039-2593)
- Annette Trunschke (ORCID: https://orcid.org/0000-0003-2869-0181)
- Arno Bergmann (ORCID: https://orcid.org/0000-0001-5071-6806)
- Anna Rabe (ORCID: https://orcid.org/0000-0002-9049-4002)
- Wulyu Jiang (ORCID: https://orcid.org/0000-0003-2258-8688)
- Stephan Barcikowski (ORCID: https://orcid.org/0000-0002-9739-7272)
- Ahmed G. Attallah (ORCID: https://orcid.org/0000-0002-7759-0315)
- Thomas Lunkenbein (ORCID: https://orcid.org/0000-0002-8957-4216)
- Janis Timoshenko (ORCID: https://orcid.org/0000-0003-2963-3912)
- Sven Reichenberger (ORCID: https://orcid.org/0000-0002-7166-9428)
- Heiko Wende (ORCID: https://orcid.org/0000-0001-8395-3541)
- Maik Butterling (ORCID: https://orcid.org/0000-0003-3674-0767)
- Andreas Wagner (ORCID: https://orcid.org/0000-0001-7575-3961)
- Serena DeBeer (ORCID: https://orcid.org/0000-0002-5196-3400)
- Takuma Sato (ORCID: https://orcid.org/0000-0002-2213-3117)
- Beatriz Roldán Cuenya (ORCID: https://orcid.org/0000-0002-8025-307X)
- Frank Girgsdies (ORCID: https://orcid.org/0000-0002-0994-0686)
- Eric Hirschmann (ORCID: https://orcid.org/0000-0001-5782-9627)
- Alexander Schnegg (ORCID: https://orcid.org/0000-0002-2362-0638)
- Jihao Wang (ORCID: https://orcid.org/0000-0003-3473-5980)
- Timon Wagner (ORCID: https://orcid.org/0000-0002-6760-1797)
- Axel Knop‐Gericke (ORCID: https://orcid.org/0009-0008-1149-4102)
- Olaf Rüdiger (ORCID: https://orcid.org/0000-0002-5148-9083)
- Dana Schellenburg
- Joonbaek Jang
- Brian Wuille Bille
- Shan Jiang
Institutions
- Fritz Haber Institute of the Max Planck Society (DE)
- Helmholtz-Zentrum Dresden-Rossendorf (DE)
- Christian-Albrechts-Universität zu Kiel (DE)
- Max Planck Institute for Chemical Energy Conversion (DE)
- University of Bayreuth (DE)
- University of Duisburg-Essen (DE)
- Minia University (EG)
Publication Details
- Journal
- ChemRxiv
- Published
- 2026-10-28
- DOI
- https://doi.org/10.26434/chemrxiv.15011176/v1
- Primary Topic
- Chemical and Physical Properties of Materials
- Type
- preprint
Funders
- Deutsche Forschungsgemeinschaft
- European Synchrotron Radiation Facility
- Bundesministerium für Bildung und Forschung