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Thermoplasticity of sol–gel-derived titanoxanes chemically modified with benzoylacetone

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Abstract

Titanium tetra-n-butoxide was hydrolyzed in the presence of benzoylacetone (BzAc), and the solution obtained was concentrated and served for spin-coating or dropping on substrates, followed by successive drying at 120, 200 and 250 °C. The dried products were transparent and amorphous, and the infrared absorption and Raman spectroscopic studies showed that BzAc forms chelate rings. Thermomechanical analysis showed that the 120 and 200 °C-dried products showed steep, thermoplastic shrinkage at around 30 and 70–85 °C, respectively, whereas the 250 °C-dried product did not show thermoplasticity. Thus as the drying temperature was increased, the thermoplasticity appeared at a higher temperature and finally disappeared. These changes in thermoplasticity with drying temperature were concluded to result from the progress of condensation between titanoxane polymers and/or clusters, which was evidenced in gel permeation chromatographic analysis.

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Acknowledgments

The authors thank Dr. Naoyuki Kitamura and Dr. Kohei Fukumi, the National Institute of Advanced Industrial Science and Technology (AIST), for their help on the Raman spectra measurement.

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Authors and Affiliations

  1. Graduate School of Science and Engineering, Kansai University, 3-3-35 Yamate-cho, Suita, 564-8680, Japan

    Shinya Oda

  2. Faculty of Chemistry and Bioengineering, Kansai University, 3-3-35 Yamate-cho, Suita, 564-8680, Japan

    Hiroaki Uchiyama & Hiromitsu Kozuka

Authors
  1. Shinya Oda
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  2. Hiroaki Uchiyama
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  3. Hiromitsu Kozuka
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Correspondence to Hiromitsu Kozuka.

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Oda, S., Uchiyama, H. & Kozuka, H. Thermoplasticity of sol–gel-derived titanoxanes chemically modified with benzoylacetone. J Sol-Gel Sci Technol 70, 441–450 (2014). https://doi.org/10.1007/s10971-014-3304-x

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  • DOI: https://doi.org/10.1007/s10971-014-3304-x

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