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Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this contribution, I will discuss our recent results investigating the formation of (polymorphic) cocrystals and metal phosphonates. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented. Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat.5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds.
Chemie kann so einfach sein: Zwei Pulver in eine Kugelmühle geben, kräftig schütteln und schon entsteht eine neue Verbindung. Dr. Franziska Fischer konnte durch Echtzeitüberwachung die Reaktionswege solcher mechanochemischen Synthesen aufdecken. Ihre Dissertation am Institut für Chemie der Humboldt-Universität und an der Bundesanstalt für Materialforschung und -prüfung leistet einen entscheidenden Beitrag zur Entwicklung umweltverträglicher und kosteneffizienter Synthesemethoden.
Mechanochemie
(2018)