Skip to main content
SpringerLink
Log in

Preparation of phenylsilsesquioxane thick films using thermal softening behavior

  • Original Paper
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

Transparent films with a thickness of more than 100 μm of phenylsilsesquioxane (PhSiO3/2) were prepared via thermal softening of PhSiO3/2 gel, which was obtained by a two-step acid-base catalyzed sol–gel process. The gel was applied to a substrate and subjected to a heat treatment at 200 °C, which resulted in the thermal softening of the gel and the attainment of fluidity. Upon cooling to ambient temperature, transparent films were obtained. The hardness of the films was slightly increased through the addition of colloidal silica in the preparation of PhSiO3/2 gel, which was also synthesized via a two-step acid-base catalyzed sol–gel process. The resulting gel containing colloidal silica also displayed fluidity upon heating, and crack-free films were obtained in a larger-thickness region with the addition of SiO2 filler.

Graphical Abstract

Highlights

  • Transparent films with a thickness of more than 100 μm of phenylsilsesquioxane (PhSiO3/2) were prepared via thermal softening of PhSiO3/2 gel.

  • PhSiO3/2 gel was obtained by a two-step acid-base catalyzed sol–gel process.

  • The formation process of the thick films is basically the same as that of the ceramic glazes.

  • The hardness of the films was increased through the addition of colloidal silica.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. Pradell T, Molera J (2020) Ceramic technology. How to characterize ceramic glazes. Archaeol Anthropol Sci 12:189. https://doi.org/10.1007/s12520-020-01136-9

    Article  Google Scholar 

  2. Toide T, Rosero-Navarro NC, Miura A, Kozuka H, Tadanaga K (2022) Preparation of transparent and mechanically hard inorganic-organic hybrid thick films from 3-glycidoxypropyltrimethoxysilane and zirconium propoxide. J Sol Gel Sci Technol 104:478–483. https://doi.org/10.1007/s10971-022-05836-7

    Article  CAS  Google Scholar 

  3. Baney RH, Itoh M, Sakakibara A, Suzuki T (1995) Silsesquioxanes. Chem Rev 95:1409–1430. https://doi.org/10.1021/cr00037a012

    Article  CAS  Google Scholar 

  4. Loy DA, Baugher BM, Baugher CR, Schneider DA, Rahimian K (2000) Substituent effects on the sol–gel chemistry of organotrialkoxysilanes. Chem Mater 12:3624–3632

    Article  CAS  Google Scholar 

  5. Cordes DB, Lickiss PD, Rataboul F (2010) Recent developments in the chemistry of cubic polyhedral oligosilsesquioxanes. Chem Rev 110:2081–2173. https://doi.org/10.1021/cr900201r

    Article  CAS  PubMed  Google Scholar 

  6. Choi JY, Kim CH, Kim DK (1998) Formation and characterization of monodisperse, spherical organo-silica powders from organo-alkoxysilane-water system. J Am Ceram Soc 81:1184–1188. https://doi.org/10.1111/j.1151-2916.1998.tb02466.x

    Article  CAS  Google Scholar 

  7. Ma C, Kimura Y (2002) Preparation of nanoparticles of poly(phenylsilsesquioxane)s by emulsion polycondensation of phenylsilanetriol formed in aqueous solution. Polym J 34:709–713. https://doi.org/10.1295/polymj.34.709

    Article  CAS  Google Scholar 

  8. Arkhireeva A, Hay JN (2003) Synthesis of sub-200 nm silsesquioxane particles using a modified Stöber sol–gel route. J Mater Chem 13:3122–3127. https://doi.org/10.1039/B306994J

    Article  CAS  Google Scholar 

  9. Choi SS, Lee AS, Hwang SS, Baek KY (2015) Structural control of fully condensed polysilsesquioxanes: ladderlike vs cage structured polyphenylsilsesquioxanes. Macromolecules 48:6063–6070. https://doi.org/10.1021/acs.macromol.5b01539

    Article  ADS  CAS  Google Scholar 

  10. Lee AS, Choi SS, Baek KY, Hwang SS (2016) Hydrolysis kinetics of a sol-gel equilibrium yielding ladder-like polysilsesquioxanes. Inorg Chem Commun 73:7–11. https://doi.org/10.1016/j.inoche.2016.09.004

    Article  ADS  CAS  Google Scholar 

  11. Matsuda A, Sasaki T, Hasegawa K, Tatsumisago M, Mianmi T (2000) Thermal softening behavior of poly (phenylsilsesquioxane) and poly (benzylsilsesquioxane) particles. J Ceram Soc Jpn 108:830–835. https://doi.org/10.2109/jcersj.108.1261_830

    Article  CAS  Google Scholar 

  12. Katagiri K, Hasegawa K, Matsuda A, Tatsumisago M, Minami T (1998) Preparation of transparent thick films by electrophoretic sol-gel deposition using phenyltriethoxysilane-derived particles. J Am Ceram Soc 81:2501–2503. https://doi.org/10.1111/j.1151-2916.1998.tb02653.x

    Article  CAS  Google Scholar 

  13. Takahashi K, Tadanaga K, Hayashi A, Matsuda A, Tatsumisago M (2008) Glass transition and thermal softening of poly(phenylsilsesquioxane) particles prepared using two-step acid-base catalyzed sol-gel process. J Non Cryst Solids 354:700–704. https://doi.org/10.1016/j.jnoncrysol.2007.07.073

    Article  ADS  CAS  Google Scholar 

  14. Macan J, Tadanaga K, Tatsumisago M (2010) Influence of copolymerization with alkyltrialkoxysilanes on condensation and thermal behaviour of poly(phenylsilsesquioxane) particles. J Sol Gel Sci Technol 53:31–37. https://doi.org/10.1007/s10971-009-2051-x

    Article  CAS  Google Scholar 

  15. Aparicio M, Jitianu A, Rodriguez G, Degnah A, Al-Marzoki K, Mosa J, Klein LC (2016) Corrosion protection of AISI 304 stainless steel with melting gel coatings. Electrochim Acta 202:325–332. https://doi.org/10.1016/j.electacta.2015.12.142

    Article  CAS  Google Scholar 

  16. Klein LC, Kallontzi S, Fabris L, Jitianu A, Ryan C, Aparicio M, Lei L, Singer JP (2019) Applications of melting gels. J Sol Gel Sci Technol 89:66–77. https://doi.org/10.1007/s10971-018-4599-9

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The present study was partly supported by JST A-STEP Grant Number JPMJTM19AH.

Author information

Authors and Affiliations

  1. Faculty of Engineering, Hokkaido University, Sapporo, Hokkaido, Japan

    Kiyoharu Tadanaga, Nataly Carolina Rosero-Navarro & Akira Miura

  2. Graduate School of Chemical Sciences and Engineering, Hokkaido University, Sapporo, Hokkaido, Japan

    Yuta Inoue

Authors
  1. Kiyoharu Tadanaga
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Yuta Inoue
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Nataly Carolina Rosero-Navarro
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Akira Miura
    View author publications

    You can also search for this author in PubMed Google Scholar

Contributions

KT wrote the main manuscript. YI carried out the experiments and prepared all figures. NCR-N and AM supported the experimental work, and discussed with KT and YI through this research. All authors reviewed the manuscript.

Corresponding author

Correspondence to Kiyoharu Tadanaga.

Ethics declarations

Conflict of interest

The authors declare no competing interests.

Additional information

Publisher’s note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Tadanaga, K., Inoue, Y., Rosero-Navarro, N.C. et al. Preparation of phenylsilsesquioxane thick films using thermal softening behavior. J Sol-Gel Sci Technol (2024). https://doi.org/10.1007/s10971-024-06332-w

Download citation

  • Received:

  • Accepted:

  • Published:

  • DOI: https://doi.org/10.1007/s10971-024-06332-w

Keywords

Search

Navigation