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An aqueous solution–gel citratoperoxo–Ti(IV) precursor: synthesis, gelation, thermo-oxidative decomposition and oxide crystallization

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Abstract

A watersoluble citratoperoxo–Ti(IV) complex was synthesized and the chemical reactions that occur during the different synthesis steps were studied. A crystalline complex could be obtained by slow evaporation of highly concentrated precursor solutions, while fast evaporation led to the preparation of a homogeneous, amorphous glassy solid, the gel. The chemical structure of the crystallized complex ion and of the gel were shown to be related, but differed due to the presence of a crosslinked ammonium citrate network in the gel, which prevents crystallization. The thermo-oxidative decomposition pathway of the crystalline complex and the gel to the metal oxide is described based on in-situ thermal analysis techniques combined with Fourier transform infrared and mass spectrometry, diffuse reflection infrared by Fourier transform as well as high-temperature X-ray diffraction. The study offers a fundamental understanding of the behavior of the aqueous solution gel Ti(IV) precursor which is applicable in the preparation of all kinds of multimetal oxide systems containing Ti(IV) ions.

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Acknowledgements

A Hardy and M.K. Van Bael are postdoctoral research fellows of the Research Foundation—Flanders (FWO Vlaanderen). The authors thank dr. G. Vanhoyland for the (HT-)XRD work and would like to express their gratitude towards late prof. dr. em. L.C. Van Poucke for many fruitful discussions of the results presented here.

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Authors and Affiliations

  1. Laboratory of Inorganic and Physical Chemistry—Institute for Materials Research, Hasselt University, Diepenbeek, Belgium

    A. Hardy, M. K. Van Bael & J. Mullens

  2. Department IWT, XIOS Hogeschool Limburg, Diepenbeek, Belgium

    A. Hardy

  3. Institute for Materials Research, Materials Physics, Hasselt University, Diepenbeek, Belgium

    J. D’Haen

  4. Division IMOMEC, IMEC, Diepenbeek, Belgium

    J. D’Haen & M. K. Van Bael

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  1. A. Hardy
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  2. J. D’Haen
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  3. M. K. Van Bael
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  4. J. Mullens
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Correspondence to M. K. Van Bael.

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Hardy, A., D’Haen, J., Van Bael, M.K. et al. An aqueous solution–gel citratoperoxo–Ti(IV) precursor: synthesis, gelation, thermo-oxidative decomposition and oxide crystallization. J Sol-Gel Sci Technol 44, 65–74 (2007). https://doi.org/10.1007/s10971-007-1601-3

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  • DOI: https://doi.org/10.1007/s10971-007-1601-3

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