Research output: Contribution to journal › Article › peer-review
Challenges of Mechanochemistry : Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation. / Michalchuk, Adam A.L.; Tumanov, Ivan A.; Konar, Sumit et al.
In: Advanced Science, Vol. 4, No. 9, 1700132, 01.09.2017, p. 1700132.Research output: Contribution to journal › Article › peer-review
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TY - JOUR
T1 - Challenges of Mechanochemistry
T2 - Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation
AU - Michalchuk, Adam A.L.
AU - Tumanov, Ivan A.
AU - Konar, Sumit
AU - Kimber, Simon A.J.
AU - Pulham, Colin R.
AU - Boldyreva, Elena V.
N1 - Publisher Copyright: © 2017 The Authors. Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
PY - 2017/9/1
Y1 - 2017/9/1
N2 - 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.
AB - 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.
KW - kinetics
KW - mechanochemistry
KW - organic salts
KW - X-ray powder diffraction
KW - ACTIVATION
KW - ACID
KW - X-RAY-DIFFRACTION
KW - OPPORTUNITIES
UR - http://www.scopus.com/inward/record.url?scp=85019110441&partnerID=8YFLogxK
U2 - 10.1002/advs.201700132
DO - 10.1002/advs.201700132
M3 - Article
C2 - 28932677
AN - SCOPUS:85019110441
VL - 4
SP - 1700132
JO - Advanced Science
JF - Advanced Science
SN - 2198-3844
IS - 9
M1 - 1700132
ER -
ID: 9049343