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Mechanistic investigations of mechanosyntheses

  • Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms often remain unclear. In the last years, we have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. A further development is the in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. [5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. Based onMechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms often remain unclear. In the last years, we have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. A further development is the in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. [5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. Based on these data, metastable polymorphs of cocrystals and coordination polymorphs could be isolated and struc-turally characterized. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses.zeige mehrzeige weniger

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Metadaten
Autor*innen:Franziska EmmerlingORCiD
Dokumenttyp:Vortrag
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2018
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.3 Strukturanalytik
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:In situ; Mechanochemistry; Phosphonates
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
Chemie und Prozesstechnik / Chemische Charakterisierung und Spurenanalytik
Veranstaltung:Beilstein Symposium MECHANOCHEMISTRY: MICROSCOPIC AND MACROSCOPIC ASPECTS
Veranstaltungsort:Rüdesheim, Germany
Beginndatum der Veranstaltung:13.11.2018
Enddatum der Veranstaltung:15.11.2018
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:29.11.2018
Referierte Publikation:Nein
Eingeladener Vortrag:Nein
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