{
  "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.",
  "abstract_shown": true,
  "affiliations": [
    "Department of Inorganic Chemistry",
    "Fritz Haber Institute of the Max Planck Society",
    "Department of Interface Science",
    "Max Planck Institute for Chemical Energy Conversion",
    "Institute of Inorganic Chemistry",
    "Kiel University",
    "Faculty of Physics and Center for Nanointegration Duisburg-Essen (CENIDE",
    "University of Duisburg-Essen",
    "Technical Chemistry I and Center for Nanointegration Duisburg-Essen (CENIDE",
    "Institute of Radiation Physics",
    "Helmholtz-Zentrum Dresden-Rossendorf (HZDR",
    "Physics Department,",
    "Minia University",
    "University of Bayreuth, Universitätsstraße 30, Bayreuth, Germany, 95447"
  ],
  "article_type": null,
  "arxiv": null,
  "author_total": 28,
  "authors": [
    {
      "affs": [
        0,
        1
      ],
      "name": "Wulyu Jiang",
      "orcid": "0000-0003-2258-8688"
    },
    {
      "affs": [
        2,
        1
      ],
      "name": "Timon Wagner"
    },
    {
      "affs": [
        0,
        1
      ],
      "name": "Frank Girgsdies"
    },
    {
      "affs": [
        3
      ],
      "name": "Takuma Sato"
    },
    {
      "affs": [
        4,
        5,
        6,
        7
      ],
      "name": "Anna Rabe"
    },
    {
      "affs": [
        2,
        1
      ],
      "name": "Joonbaek Jang"
    },
    {
      "affs": [
        0,
        1
      ],
      "name": "Jihao Wang"
    },
    {
      "affs": [
        3
      ],
      "name": "Brian Wuille Bille"
    },
    {
      "affs": [
        8,
        7
      ],
      "name": "Dana Schellenburg"
    },
    {
      "affs": [
        8,
        7
      ],
      "name": "Sven Reichenberger"
    },
    {
      "affs": [
        9,
        10,
        11,
        12
      ],
      "name": "Ahmed Gamal Attallah"
    },
    {
      "affs": [
        4,
        5
      ],
      "name": "Nicolas Cosanne"
    },
    {
      "affs": [
        0,
        1
      ],
      "name": "Shan Jiang"
    },
    {
      "affs": [
        9,
        10
      ],
      "name": "Maik Butterling"
    },
    {
      "affs": [
        9,
        10
      ],
      "name": "Eric Hirschmann"
    },
    {
      "affs": [
        9,
        10
      ],
      "name": "Andreas Wagner"
    },
    {
      "affs": [
        0,
        1
      ],
      "name": "Annette Trunschke"
    },
    {
      "affs": [
        0,
        1,
        3
      ],
      "name": "Axel Knop-Gericke"
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    {
      "affs": [
        6,
        7
      ],
      "name": "Heiko Wende"
    },
    {
      "affs": [
        3
      ],
      "name": "Olaf Rüdiger"
    },
    {
      "affs": [
        3
      ],
      "name": "Alexander Schnegg"
    },
    {
      "affs": [
        2,
        1
      ],
      "name": "Janis Timoshenko"
    },
    {
      "affs": [
        8,
        7
      ],
      "name": "Stephan Barcikowski"
    },
    {
      "affs": [
        3
      ],
      "name": "Serena DeBeer"
    },
    {
      "affs": [
        4,
        5
      ],
      "name": "Malte Behrens"
    },
    {
      "affs": [
        2,
        1
      ],
      "name": "Arno Bergmann"
    },
    {
      "affs": [
        2,
        1
      ],
      "name": "Beatriz Roldan Cuenya"
    },
    {
      "affs": [
        0,
        1,
        13
      ],
      "name": "Thomas Lunkenbein"
    }
  ],
  "bibtex": "https://research.draconitic.com/paper/5m59qavsz2n6b.bib",
  "cited_by": 0,
  "doi": "10.26434/chemrxiv.15011176/v1",
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  "language": null,
  "licence": "CC-BY",
  "licence_label": "CC BY",
  "licence_source": "journal",
  "licence_url": "https://creativecommons.org/licenses/by/4.0/",
  "metadata_licence": null,
  "native_subjects": [
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      "openalex",
      "2505|Chemical and Physical Properties of Materials"
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  "openalex": "W7224122120",
  "pdf_url": null,
  "pmcid": null,
  "pmid": null,
  "published": "2026-10-28",
  "publisher": "American Chemical Society (ACS)",
  "ris": "https://research.draconitic.com/paper/5m59qavsz2n6b.ris",
  "sources": [
    {
      "first_seen": "2026-10-30T12:17:26Z",
      "native_id": "10.26434/chemrxiv.15011176",
      "source": "chemrxiv",
      "url": "https://chemrxiv.org/doi/full/10.26434/chemrxiv.15011176/v1"
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  "subjects": [
    {
      "field": "chemistry",
      "origin": "openalex:2505|Chemical and Physical Properties of Materials",
      "subfield": "materials-polymers"
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  ],
  "title": "Non-Monotonic Structural Response of Co3O4 during Calcination",
  "title_text": "Non-Monotonic Structural Response of Co3O4 during Calcination",
  "type": "preprint",
  "updated_at": "2026-10-30T12:17:26Z",
  "url": "https://research.draconitic.com/paper/5m59qavsz2n6b",
  "venue": "ChemRxiv",
  "versions": []
}