Non-Monotonic Structural Response of Co3O4 during Calcination
14 affiliations
- 1Department of Inorganic Chemistry
- 2Fritz Haber Institute of the Max Planck Society
- 3Department of Interface Science
- 4Max Planck Institute for Chemical Energy Conversion
- 5Institute of Inorganic Chemistry
- 6Kiel University
- 7Faculty of Physics and Center for Nanointegration Duisburg-Essen (CENIDE
- 8University of Duisburg-Essen
- 9Technical Chemistry I and Center for Nanointegration Duisburg-Essen (CENIDE
- 10Institute of Radiation Physics
- 11Helmholtz-Zentrum Dresden-Rossendorf (HZDR
- 12Physics Department,
- 13Minia University
- 14University of Bayreuth, Universitätsstraße 30, Bayreuth, Germany, 95447
Abstract
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.
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BibTeX
@misc{jiang2026nonmonotonic,
title = {{Non-Monotonic Structural Response of Co3O4 during Calcination}},
author = {Wulyu Jiang and Timon Wagner and Frank Girgsdies and Takuma Sato and Anna Rabe and Joonbaek Jang and Jihao Wang and Brian Wuille Bille and Dana Schellenburg and Sven Reichenberger and Ahmed Gamal Attallah and Nicolas Cosanne and Shan Jiang and Maik Butterling and Eric Hirschmann and Andreas Wagner and Annette Trunschke and Axel Knop-Gericke and Heiko Wende and Olaf Rüdiger and Alexander Schnegg and Janis Timoshenko and Stephan Barcikowski and Serena DeBeer and Malte Behrens and Arno Bergmann and Beatriz Roldan Cuenya and Thomas Lunkenbein},
howpublished = {ChemRxiv},
year = {2026},
month = oct,
doi = {10.26434/chemrxiv.15011176/v1},
url = {https://chemrxiv.org/doi/full/10.26434/chemrxiv.15011176/v1},
note = {CC BY},
}
RIS
TY - UNPB
TI - Non-Monotonic Structural Response of Co3O4 during Calcination
AU - Wulyu Jiang
AU - Timon Wagner
AU - Frank Girgsdies
AU - Takuma Sato
AU - Anna Rabe
AU - Joonbaek Jang
AU - Jihao Wang
AU - Brian Wuille Bille
AU - Dana Schellenburg
AU - Sven Reichenberger
AU - Ahmed Gamal Attallah
AU - Nicolas Cosanne
AU - Shan Jiang
AU - Maik Butterling
AU - Eric Hirschmann
AU - Andreas Wagner
AU - Annette Trunschke
AU - Axel Knop-Gericke
AU - Heiko Wende
AU - Olaf Rüdiger
AU - Alexander Schnegg
AU - Janis Timoshenko
AU - Stephan Barcikowski
AU - Serena DeBeer
AU - Malte Behrens
AU - Arno Bergmann
AU - Beatriz Roldan Cuenya
AU - Thomas Lunkenbein
PY - 2026
DA - 2026/10/28
PB - ChemRxiv
DO - 10.26434/chemrxiv.15011176/v1
UR - https://chemrxiv.org/doi/full/10.26434/chemrxiv.15011176/v1
AB - 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.
ER -