Abstract
Mechanochemical methods offer unprecedented academic and industrial opportunities for solvent‐free synthesis of novel materials. The need to study mechanochemical mechanisms is growing, and has led to the development of real‐time in situ X‐ray powder diffraction techniques (RI‐XRPD). However, despite the power of RI‐XRPD methods, there remain immense challenges. In the present contribution, many of these challenges are highlighted, and their effect on the interpretation of RI‐XRPD data considered. A novel data processing technique is introduced for RI‐XRPD, through which the solvent‐free mechanochemical synthesis of an organic salt is followed as a case study. These are compared to ex situ studies, where notable differences are observed. The process is monitored over a range of milling frequencies, and a nonlinear correlation between milling parameters and reaction rate is observed. Kinetic analysis of RI‐XRPD allows, for the first time, observation of a mechanistic shift over the course of mechanical treatment, resulting from time evolving conditions within the mechanoreactor.
Highlights
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This field has developed widely,[1,2,3] and numerous applications to the generation and processing of processing technique is introduced for real-time in situ X-ray powder diffraction techniques (RI-X-ray powder diffraction (XRPD)), through which the solventadvanced organic, inorganic, and hybrid free mechanochemical synthesis of an organic salt is followed as a case materials are known.[4]
Kinetic analysis of real-time in situ (RI)-XRPD allows, for the first time, observation of mechanochemical technologies have been successfully employed in the preparation of novel electronic and magnetic materials, the assembly of porous and nanomaterials, and the time evolving conditions within the mechanoreactor
Summary
Both are known to enhance the dehydration rate of OAD.[31] It is known that solvate liquid is important in driving organic mechanochemical processes[23,32] and desolvation is believed to be responsible for formation of a fluidized (truly fluid or strongly disordered solid) intermediate state In such a case, one would expect to see two stages of a reaction: one for the consumption of reactant material (fluidization), and a second corresponding to the nucleation/growth kinetics of the product. This novel technique, based on a combination of Rietveld refinement and peak integration, has proved very promising for the processing of RI-XRPD data This has led to the first identification of time-evolving kinetics in a mechanochemical cocrystallization, it remains unclear whether this evolution is due to changes in the free flowing powder, temperature, or particle size. In this way can true insights into the fundamental mechanisms leading to the mechanochemical production of advanced materials be achieved
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