Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation

Adam A.L. Michalchuk, Ivan A. Tumanov, Sumit Konar, Simon A.J. Kimber, Colin R. Pulham, Elena V. Boldyreva

Результат исследования: Научные публикации в периодических изданияхстатья

20 Цитирования (Scopus)

Аннотация

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.

Язык оригиналаанглийский
Номер статьи1700132
Страницы (с-по)1700132
Число страниц7
ЖурналAdvanced Science
Том4
Номер выпуска9
DOI
СостояниеОпубликовано - 1 сен 2017

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