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Quantitative in situ and real-time monitoring of mechanochemical reactions

An experimental technique for in situ and real- time monitoring of mechanochemical reactions in a shaker ball mill was recently described, which utilises highly penetrating X-ray radiation available at the ID15B beamline of the European Synchrotron Radiation Facility. Herein, we describe the first attempts to perform such reaction monitoring in a quantitative fashion, by introducing an internal X-ray diffraction standard. The use of silicon as an internal standard resolved the issue with variations of the amount of the sample in the X-ray beam due to non- uniform distribution of the sample in the reaction jar and allowed, via Rietveld analysis, the first quantitative estimate of amorphous phase content in mechanochemical reaction as it is being milled. We also highlight problems associated with non- ideal mixing of the reaction mixture.

in situ X-ray diffraction; powder diffraction; quantutative Rietvld analysis; mechanochemistry; amorphous

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