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Study of the Chemical Mechanism Involved in the Formation of Tungstite in Benzyl Alcohol by the Advanced QEXAFS Technique

  1. Inga Olliges-Stadler1,
  2. Jan Stötzel2,
  3. Dr. Dorota Koziej1,
  4. Dr. Marta D. Rossell1,
  5. Prof. Dr. Jan-Dierk Grunwaldt3,4,
  6. Dr. Maarten Nachtegaal5,
  7. Prof. Dr. Ronald Frahm2,
  8. Prof. Dr. Markus Niederberger1,*

Article first published online: 16 JAN 2012

DOI: 10.1002/chem.201101514

Issue

Chemistry - A European Journal

Chemistry - A European Journal

Volume 18, Issue 8, pages 2305–2312, February 20, 2012

Additional Information

How to Cite

Olliges-Stadler, I., Stötzel, J., Koziej, D., Rossell, M. D., Grunwaldt, J.-D., Nachtegaal, M., Frahm, R. and Niederberger, M. (2012), Study of the Chemical Mechanism Involved in the Formation of Tungstite in Benzyl Alcohol by the Advanced QEXAFS Technique. Chem. Eur. J., 18: 2305–2312. doi: 10.1002/chem.201101514

Author Information

  1. 1

    Laboratory for Multifunctional Materials, Department of Materials, ETH Zürich, Wolfgang-Pauli-Strasse 10, 8093 Zürich (Switzerland)

  2. 2

    Department of Physics, University of Wuppertal, Gaussstrasse 20, 42097 Wuppertal (Germany)

  3. 3

    Institute for Chemical Technology and Polymer Chemistry, Karlsruhe Institute of Technology (KIT), Engesserstrasse 20, 76131 Karlsruhe (Germany)

  4. 4

    Department of Chemical and Biochemical Engineering, Technical University of Denmark, 2800 Kgs. Lyngby (Denmark)

  5. 5

    Swiss Light Source, Paul Scherrer Institute, 5232 Villigen (Switzerland)

*Laboratory for Multifunctional Materials, Department of Materials, ETH Zürich, Wolfgang-Pauli-Strasse 10, 8093 Zürich (Switzerland)

Publication History

  1. Issue published online: 10 FEB 2012
  2. Article first published online: 16 JAN 2012
  3. Manuscript Received: 16 MAY 2011

Funded by

  • University of Wuppertal
  • Swiss National Science Foundation. Grant Number: 200021-119741
  • ETH Zürich
  • DANSCAT
  • Danish Strategic Research Council

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Keywords:

  • gas chromatography;
  • nanoparticles;
  • reaction mechanisms;
  • sol–gel processes;
  • tungsten;
  • X-ray absorption spectroscopy

Abstract

Insight into the complex chemical mechanism for the formation of tungstite nanoparticles obtained by the reaction of tungsten hexachloride with benzyl alcohol is presented herein. The organic and inorganic species involved in the formation of the nanoparticles were studied by time-dependent gas chromatography and X-ray diffraction as well as by time-resolved in situ X-ray absorption near-edge structure and extended X-ray absorption fine structure spectroscopy. Principal component analysis revealed two intermediates, which were identified as WCl4 and WOCl4 by using linear combination analysis. Quick-scanning extended X-ray absorption fine structure spectroscopy enabled the time-dependent evolution of the starting compound, the intermediates and the product to be monitored over the full reaction period. The reaction starts with fast chlorine substitution and partial reduction during the dissolution of the tungsten hexachloride in benzyl alcohol followed by the generation of intermediates with W[DOUBLE BOND]O double bonds and finally the construction of the W[BOND]O[BOND]W network of the tungstite structure.

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