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Mechanochemistry is increasingly used for synthesizing various materials including metal organic compounds and cocrystals. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained in in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup enabling a combined in situ investigation of mechanochemical reactions using synchrotron XRD and 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. Besides well-known MOFs like ZIF-8, the formation process of new metal phosphonates and model cocrystals could be studied in detail. The syntheses pathway of the different compounds could be revealed. The results prove that the presented method combination is applicable for a wide range of materials and will provide the necessary understanding to tune and optimize mechanochemically synthesized compounds.
Mechanochemistry is increasingly used for synthesizing various materials. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained by in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup combining in situ synchrotron XRD and Raman spectroscopy. This combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. The formation process of MOFs, metal phosphonates and model cocrystals could be studied in detail. The results prove that the presented method combination is applicable for a wide range of materials and will provide the necessary understanding to tune and optimize mechanochemically synthesized compounds.
Mechanochemistry is a convenient way to form metal phosphonates with neutral and/or monodeprotonated phosphonates, controlled by the stoichiometric. In situ investigation of reactions helps understanding mechanisms and formation of intermediates. The knowledge of intermediates helps to find metastable structures.The diffusion mechanism is most probable for the mechanochemical synthesis of metal phosphonates.