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Direct In Situ Investigation of Milling Reactions Using Combined X‐ray Diffraction and Raman Spectroscopy
Author(s) -
Batzdorf Lisa,
Fischer Franziska,
Wilke Manuel,
Wenzel KlausJürgen,
Emmerling Franziska
Publication year - 2015
Publication title -
angewandte chemie
Language(s) - English
Resource type - Journals
eISSN - 1521-3757
pISSN - 0044-8249
DOI - 10.1002/ange.201409834
Subject(s) - raman spectroscopy , in situ , diffraction , spectroscopy , materials science , x ray crystallography , chemistry , nanotechnology , analytical chemistry (journal) , organic chemistry , optics , physics , quantum mechanics
The combination of two analytical methods including time‐resolved in situ X‐ray diffraction (XRD) and Raman spectroscopy provides a new opportunity for a detailed analysis of the key mechanisms of milling reactions. To prove the general applicability of our setup, we investigated the mechanochemical synthesis of four archetypical model compounds, ranging from 3D frameworks through layered structures to organic molecular compounds. The reaction mechanism for each model compound could be elucidated. The results clearly show the unique advantage of the combination of XRD and Raman spectroscopy because of the different information content and dynamic range of both individual methods. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structures and thus obtaining reliable data for mechanistic studies.