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In situ and real-time monitoring of mechanochemical milling reactions using synchrotron X-ray diffraction
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In situ and real-time monitoring of mechanochemical milling reactions using synchrotron X-ray diffraction
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Journal Article
In situ and real-time monitoring of mechanochemical milling reactions using synchrotron X-ray diffraction
2013
Overview
We describe the only currently available protocol for
in situ
, real-time monitoring of mechanochemical reactions and intermediates by X-ray powder diffraction. Although mechanochemical reactions (inducing transformations by mechanical forces such as grinding and milling) are normally performed in commercially available milling assemblies, such equipment does not permit direct reaction monitoring. We now describe the design and in-house modification of milling equipment that allows the reaction jars of the operating mill to be placed in the path of a high-energy (∼90 keV) synchrotron X-ray beam while the reaction is taking place. Resulting data are analyzed using conventional software, such as TOPAS. Reaction intermediates and products are identified using the Cambridge Structural Database or Inorganic Crystal Structure Database. Reactions are analyzed by fitting the time-resolved diffractograms using structureless Pawley refinement for crystalline phases that are not fully structurally characterized (such as porous frameworks with disordered guests), or the Rietveld method for solids with fully determined crystal structures (metal oxides, coordination polymers).
Publisher
Nature Publishing Group UK,Nature Publishing Group
