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Raman spectroscopy for real-time and in situ monitoring of mechanochemical milling reactions

We describe the protocol for real-time and in situ monitoring of mechanochemical milling reactions conducted on vibratory ball mills by Raman spectroscopy. Recently, solid-state milling reactions became an attractive and sustainable alternative for the preparation of almost all classes of compounds and materials. Raman spectroscopy monitoring comes complementary to already established in situ monitoring based on powder X-rays diffraction, which requires a synchrotron X-ray source and therefore has a limited accessibility to a wide research community. Raman spectroscopy milling setup exploits the modular nature of Raman instrumentation, and consists of portable and small spectrometer, a laser source, and a Raman probe. As such, it is readily implemented in a laboratory environment. Translucent reaction jars made of plastic enable interaction of the laser beam with the milled solid sample inside the closed reaction vessel and subsequent collection of Raman–scattered photons. Acquired Raman spectra are analysed using commercial, or open-source software for data analysis (Matlab, Octave, Python, R, etc.) Simply plotting the Raman spectra versus time enables a quallitative analysis of reaction paths, as well as phase identification. We demonstrate here, derivations of the reaction profile from intensities of selected Raman peaks. Alternatively, more rigorous approach should include the use of multivariate analysis.

Raman spectroscopy ; in situ ; monitoring ; mechanochemistry ; milling

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