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

摘要

Mechanistic understanding of mechanochemical reactions is sparse and has been acquired mostly by stepwise ex situ analysis. We describe here an unprecedented laboratory technique to monitor the course of mechanochemical transformations at the molecular level in situ and in real time by using Raman spectroscopy. The technique, which employs translucent milling vessels that allow collecting a Raman scattering signal from the sample as it is being milled, was validated on mechanochemical reactions forming coordination polymers and organic cocrystals. The technique enabled assessing reaction dynamics and course under different reaction conditions as well as, for the first time, direct insight in the behaviour of liquid additives during liquid-assisted grinding.