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Developing an in situ EXAFS experiment of microwave-induced gelation

Abstract

Internal gelation is an advanced route to produce small spheres of metal from a nitrate solution. In this work, microwave heating is used to trigger the gelation of the solution. X-ray absorption spectroscopy is a powerful tool to follow the gelation advancement and verify the completeness of a reaction, but in order to use it on falling nitrate droplets, the study is split into two experiments. First, a fluorescence measurement has been carried out on a trickle of small falling cerium nitrate droplets generated at high frequency to verify that capturing a discontinuous signal would not generate too much noise. Then, a measurement of silver nitrate undergoing gelation in a microwave cavity has been performed in transmission mode, which proved that a fast recording method is suitable for following the evolution of chemicals during such a reaction. The combination of both analyses confirms that it is possible to study microwave gelation of falling droplets using X-ray absorption spectroscopy at the SuperXAS beamline.

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Acknowledgments

S. Valance is acknowledged for his assistance during the analysis of the results. This work was part of the PINE project and its follow-up MeAWaT and was partially financed by the Swiss Competence Center for Energy and Mobility. The authors greatly appreciate the financial support of the European Commission through Contract No. 295664 regarding the FP7 PELGRIMM project, as well as Contract No. 295825 regarding the FP7-ASGARD project.

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Correspondence to C. Cozzo.

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Cozzo, C., Ishizaki, K., Pouchon, M.A. et al. Developing an in situ EXAFS experiment of microwave-induced gelation. J Sol-Gel Sci Technol 78, 507–513 (2016) doi:10.1007/s10971-016-3992-5

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Keywords

  • EXAFS
  • Internal gelation
  • Microwave
  • Reaction advancement