期刊
NATURE PROTOCOLS
卷 8, 期 9, 页码 1718-1729出版社
NATURE PORTFOLIO
DOI: 10.1038/nprot.2013.100
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资金
- Herchel Smith Fund
- British Council/The German Academic Exchange Service (DAAD) [1377]
- ESRF
- NanoDTC, the University of Cambridge
- Ministry of Science, Education and Sports of the Republic of Croatia [098-0982904-2953]
- EPSRC
- Canadian Natural Sciences and Engineering Research Council (NSERC) Discovery grant
- Fonds Quebecois de la Recherche sur la Nature et les Technologies (FRQNT) Centre for Green Chemistry and Catalysis
- McGill University
- FRQNT Nouveaux Chercheurs grant
- EPSRC [EP/J01110X/1] Funding Source: UKRI
- Engineering and Physical Sciences Research Council [EP/J01110X/1] Funding Source: researchfish
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 (similar to 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).
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