Open AccessOn the Mechanism of Cocrystal Mechanochemical Reaction via Low Melting Eutectic: A Time-Resolved In Situ Monitoring Investigation
Author(s) -
Paolo Pio Mazzeo,
Michele Prencipe,
Torvid Feiler,
Franziska Emmerling,
Alessia Bacchi
Publication year - 2022
Publication title -
crystal growth and design
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.966
H-Index - 155
eISSN - 1528-7505
pISSN - 1528-7483
DOI - 10.1021/acs.cgd.2c00262
Subject(s) - mechanochemistry , eutectic system , cocrystal , materials science , powder diffraction , metastability , synchrotron , crystallography , chemical engineering , nanotechnology , chemistry , metallurgy , alloy , molecule , organic chemistry , optics , hydrogen bond , physics , engineering
Mechanochemistry has become a sustainable and attractive cost-effective synthetic technique, largely used within the frame of crystal engineering. Cocrystals, namely, crystalline compounds made of different chemical entities within the same crystal structure, are typically synthesized in bulk via mechanochemistry; however, whereas the macroscopic aspects of grinding are becoming clear, the fundamental principles that underlie mechanochemical cocrystallization at the microscopic level remain poorly understood. Time-resolved in situ (TRIS) monitoring approaches have opened the door to exceptional detail regarding mechanochemical reactions. We here report a clear example of cocrystallization between two solid coformers that proceeds through the formation of a metastable low melting binary eutectic phase. The overall cocrystallization process has been monitored by time-resolved in situ (TRIS) synchrotron X-ray powder diffraction with a customized ball milling setup, currently available at μSpot beamline at BESSY-II, Helmholtz-Zentrum Berlin. The binary system and the low melting eutectic phase were further characterized via DSC, HSM, and VT-XRPD.