Unveiling amorphous intermediates in mechanochemical metal–organic synthesis through in situ PXRD and THz-Raman coupling

Macchietti, Laura;Casali, Lucia;Contini, Laura;Jiang, Yihua;Grepioni, Fabrizia;et.al.
(2026) RSC Mechanochemistry — (2026)

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Authors
  • Macchietti, Lauraorcid-logoDipartimento di Chimica “Giacomo Ciamician”, Università di Bologna, Via P. Gobetti 85, 40129 Bologna, Italy
    Author
  • Casali, Luciaorcid-logoBAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Strasse 11, 12489 Berlin, Germany
    Author
  • Contini, LauraDipartimento di Chimica “Giacomo Ciamician”, Università di Bologna, Via P. Gobetti 85, 40129 Bologna, Italy
    Author
  • Jiang, YihuaUCLouvain
    Author
  • Leyssens, TomUCLouvain
    Author
  • Grepioni, Fabriziaorcid-logoDipartimento di Chimica “Giacomo Ciamician”, Università di Bologna, Via P. Gobetti 85, 40129 Bologna, Italy
    Author
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Abstract
Decoding structural transitions during mechanochemical reactions remains challenging due to the transient and disordered nature of intermediate phases. In this study, we use a combination of in situ powder X-ray diffraction (PXRD) and terahertz (THz) Raman spectroscopy to investigate the amorphous-to-crystalline transformation that occurs during the formation of a metal–organic complex. The two probes complementary sensitivity reveals an amorphous intermediate preceding crystallisation, with water playing a pivotal role in activating the complexation process. Multivariate curve resolution (MCR) analysis enables the simultaneous interpretation of PXRD and Raman data, enhancing the detection of amorphous species and mapping their structural evolution in real time. This integrated approach provides a general framework for identifying disordered intermediates in mechanochemical synthesis.
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Macchietti, L., Casali, L., Contini, L., Jiang, Y., Leyssens, T., Emmerling, F., & Grepioni, F. (2026). Unveiling amorphous intermediates in mechanochemical metal–organic synthesis through in situ PXRD and THz-Raman coupling. RSC Mechanochemistry. Published. https://doi.org/10.1039/d6mr00045b (Original work published 2026)