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Real-time and in situ monitoring of mechanochemical milling reactions
by
Halasz, Ivan
, Dinnebier, Robert E.
, Adams, Frank
, Beldon, Patrick J.
, Belenguer, Ana M.
, Friščić, Tomislav
, Kimber, Simon A.J.
, Honkimäki, Veijo
in
639/638/298/921
/ 639/638/549
/ Additives
/ Analytical Chemistry
/ Biochemistry
/ Catalysis
/ Chemistry
/ Chemistry/Food Science
/ Imidazoles - chemistry
/ Inorganic Chemistry
/ Kinetics
/ Ligands
/ Materials Testing
/ Mechanical Phenomena
/ Metals
/ Models, Molecular
/ Organic Chemistry
/ Physical Chemistry
/ Porous materials
/ Radiation
/ X-Ray Diffraction
/ X-rays
/ Zinc Oxide - chemistry
2013
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Real-time and in situ monitoring of mechanochemical milling reactions
by
Halasz, Ivan
, Dinnebier, Robert E.
, Adams, Frank
, Beldon, Patrick J.
, Belenguer, Ana M.
, Friščić, Tomislav
, Kimber, Simon A.J.
, Honkimäki, Veijo
in
639/638/298/921
/ 639/638/549
/ Additives
/ Analytical Chemistry
/ Biochemistry
/ Catalysis
/ Chemistry
/ Chemistry/Food Science
/ Imidazoles - chemistry
/ Inorganic Chemistry
/ Kinetics
/ Ligands
/ Materials Testing
/ Mechanical Phenomena
/ Metals
/ Models, Molecular
/ Organic Chemistry
/ Physical Chemistry
/ Porous materials
/ Radiation
/ X-Ray Diffraction
/ X-rays
/ Zinc Oxide - chemistry
2013
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Real-time and in situ monitoring of mechanochemical milling reactions
by
Halasz, Ivan
, Dinnebier, Robert E.
, Adams, Frank
, Beldon, Patrick J.
, Belenguer, Ana M.
, Friščić, Tomislav
, Kimber, Simon A.J.
, Honkimäki, Veijo
in
639/638/298/921
/ 639/638/549
/ Additives
/ Analytical Chemistry
/ Biochemistry
/ Catalysis
/ Chemistry
/ Chemistry/Food Science
/ Imidazoles - chemistry
/ Inorganic Chemistry
/ Kinetics
/ Ligands
/ Materials Testing
/ Mechanical Phenomena
/ Metals
/ Models, Molecular
/ Organic Chemistry
/ Physical Chemistry
/ Porous materials
/ Radiation
/ X-Ray Diffraction
/ X-rays
/ Zinc Oxide - chemistry
2013
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Real-time and in situ monitoring of mechanochemical milling reactions
Journal Article
Real-time and in situ monitoring of mechanochemical milling reactions
2013
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Overview
Chemical and structural transformations have long been carried out by milling. Such mechanochemical steps are now ubiquitous in a number of industries (such as the pharmaceutical, chemical and metallurgical industries), and are emerging as excellent environmentally friendly alternatives to solution-based syntheses. However, mechanochemical transformations are typically difficult to monitor in real time, which leaves a large gap in the mechanistic understanding required for their development. We now report the real-time study of mechanochemical transformations in a ball mill by means of
in situ
diffraction of high-energy synchrotron X-rays. Focusing on the mechanosynthesis of metal–organic frameworks, we have directly monitored reaction profiles, the formation of intermediates, and interconversions of framework topologies. Our results reveal that mechanochemistry is highly dynamic, with reaction rates comparable to or greater than those in solution. The technique also enabled us to probe directly how catalytic additives recently introduced in the mechanosynthesis of metal–organic frameworks, such as organic liquids or ionic species, change the reactivity pathways and kinetics.
Milling and grinding, long used to alter the chemical and physical properties of materials, have recently garnered interest as alternatives to traditional solution-based syntheses — but these reactions remain difficult to monitor. High-energy synchrotron X-ray radiation has now enabled the
in situ
observation, in real time, of solid-state transformations occurring during the mechanochemical syntheses of metal–organic frameworks.
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