Real-Time in Situ Monitoring of Particle and Structure Evolution in the Mechanochemical Synthesis of UiO-66 Metal–Organic Frameworks

While in situ synchrotron X-ray powder diffraction has revolutionized mechanistic studies of mechanochemistry and inspired the development of other real-time monitoring approaches, the full potential of such data remains unexploited, with most applications addressing only reaction kinetics. Focusing on UiO-type metal–organic frameworks (MOFs) as models, we now show how in-depth analysis of real-time diffraction data can provide insight into the evolution of both crystallographic structure and crystallite size, including the direct relation to the particle size of mechanochemically formed MOFs.