Skip to main content
Log in

Transmission infrared study of acid-catalyzed sol-gel silica coatings during room ambient drying

  • Articles
  • Published:
Journal of Materials Research Aims and scope Submit manuscript

Abstract

Sol-gel solutions prepared from tetraethylorthosilicate (TEOS) hydrolyzed in acidic conditions were used to make thin films on Si wafers via spin coating. Solutions with H2O/TEOS ratios of 2, 5, and 10 were prepared and aged at room temperature in sealed containers for times ranging from <2.5 h to 1 month. Transmission Fourier transform infrared spectra acquired around 1 min after spinning showed peaks characteristic of both SiO2 and SiOH. Additional features at ≍580, 1093, and 1130 cm−1 were observed and possible origins are discussed. Peaks at ≍580 and 1130 cm−1, which increased in intensity with solution age time, are attributed to cyclic Si–O, e.g., 4-member rings. When films were exposed to room air, ring concentration decreased significantly within 30 min. Rings were stable for hours, however, when films were kept in N2. The feature at 1093 cm−1, most sensitive to H2O/TEOS, is attributed to residual Si–O–C.

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

Access this article

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

Instant access to the full article PDF.

Similar content being viewed by others

References

  1. C. J. Brinker, K. D. Keefer, D. W. Schaefer, and C. S. Ashley, J. Non-Cryst. Solids 48, 47 (1982).

    Article  CAS  Google Scholar 

  2. C. J. Brinker, K. D. Keefer, D. W. Schaefer, R. A. Assink, B. D. Kay, and C. S. Ashley, J. Non-Cryst. Solids 63, 45 (1984).

    Article  CAS  Google Scholar 

  3. R. B. Pettit, C. S. Ashley, S. T. Reed, and C. J. Brinker, Sol-gel Technology for Thin films, Fibers, Preforms, Electronics, and Specialty Shapes, edited by L. Klein (Noyes Publications, Park Ridge, NJ, 1988), p. 80.

  4. R. A. Weimar, P. M. Lenahan, T. A. Marchione, and C. J. Brinker, Appl. Phys. Lett. 51, 1179 (1987).

    Article  Google Scholar 

  5. M. Kuisl, Thin Solid Films 157, 129 (1988).

    Article  CAS  Google Scholar 

  6. A. Boelle, J. A. Roger, B. Canut, J. Mugnier, and M. Pitaval, Appl. Surf. Sci. 46, 200 (1990).

    Article  CAS  Google Scholar 

  7. W. L. Warren, P. M. Lenahan, C. J. Brinker, C. S. Ashley, and S. T. Reed, J. Electronic Mater. 19, 425 (1990).

    Article  CAS  Google Scholar 

  8. G. V. Chandrashekhar and M. W. Schafer, Electronic Packaging Materials Science II, edited by K. A. Jackson, R. C. Pohanka, D. R. Uhlmann, and D. R. Ulrich (Mater. Res. Soc. Symp. Proc. 72, Pittsburgh, PA, 1986), p. 309.

  9. V. Comello, Semicond. International Nov. , 60 (1990).

  10. C. J. Brinker, A. J. Hurd, G. C. Frye, K. J. Ward, and C. S. Ashley, J. Non-Cryst. Solids 121, 294 (1990).

    Article  CAS  Google Scholar 

  11. W. A. Pliskin, J. Vac. Sci. Technol. 14, 1064 (1977).

    Article  CAS  Google Scholar 

  12. R. J. Bell, N. F. Bird, and P. Dean, J. Phys. C1, 299 (1968).

  13. R. J. Bell, P. Dean, and D. C. Hibbins-Butler, J. Phys. C3, 2111 (1970).

    Google Scholar 

  14. R. J. Bell, P. Dean, and D. C. Hibbins-Butler, J. Phys. C4, 1214 (1971).

    Google Scholar 

  15. P. N. Sen and M. F. Thorpe, Phys. Rev. B 15, 4030 (1977).

    Article  CAS  Google Scholar 

  16. F. L. Galeener, Phys. Rev. B 19, 4292 (1979).

    Article  CAS  Google Scholar 

  17. D. W. Berreman, Phys. Rev. 130, 2193 (1963).

    Article  CAS  Google Scholar 

  18. K. Hiibner, L. Schumann, A. Lehmann, H. H. Vajen, and G. Zuther, Phys. Status Solidi B104, K1 (1981).

  19. A. Bertoluzza, C. Fagnano, M. A. Morelli, V. Gottardi, and M. Gugliemi, J. Non-Cryst. Solids 48, 117 (1982).

    Article  CAS  Google Scholar 

  20. D. L. Wood and E. M. Rabinovich, J. Non-Cryst. Solids 107, 199 (1989).

    Article  CAS  Google Scholar 

  21. D. L. Wood and E. M. Rabinovich, Appl. Spec. 43, 263 (1989).

    Article  CAS  Google Scholar 

  22. J. W. Park and H. Chen, J. Non-Cryst. Solids 40, 515 (1980).

    Article  CAS  Google Scholar 

  23. J. A. Theil, D. V. Tsu, M. W. Watkins, S. S. Kim, and G. Lucov-sky, J. Vac. Sci. Technol. A8, 1374 (1990).

    Article  Google Scholar 

  24. H. A. Benesi and A. C. Jones, J. Phys. Chem. 63, 179 (1959).

    Article  CAS  Google Scholar 

  25. P. G. Pai, S. S. Chao, Y. Takagi, and G. Lucovsky, J. Vac. Sci. Technol. A4, 689 (1986).

    Article  Google Scholar 

  26. C. T. Kirk, Phys. Rev. B 38, 1255 (1988).

    Article  CAS  Google Scholar 

  27. F. L. Galeener, A. J. Leadbetter, and M. W. Stringfellow, Phys. Rev. B 27, 1052 (1983).

    Article  CAS  Google Scholar 

  28. C. J. Brinker and G. W. Scherer, Sol-gel Science: The Physics and Chemistry of Sol-gel Processing (Academic Press, San Diego, CA, 1990), p. 581.

    Google Scholar 

  29. A. L. Smith, Spectrochim. Acta 16, 87 (1960).

    Article  CAS  Google Scholar 

  30. G. Lucovsky, C. K. Wong, and W. B. Pollard, J. Non-Cryst. Solids 5960, 839 (1983).

    Google Scholar 

  31. P. Lange, J. Appl. Phys. 66, 201 (1989).

    Article  CAS  Google Scholar 

  32. P. Lange, U. Schnakenberg, S. Ullerich, and H-J. Schliwinski, J. Appl. Phys. 68, 3532 (1990).

    Article  CAS  Google Scholar 

  33. J. C. Phillips, Solid State Phys. 37, 93 (1982).

    Article  CAS  Google Scholar 

  34. K. A. Mauritz and R. M. Warren, Macromolecules 22, 1730 (1989).

    Article  CAS  Google Scholar 

  35. H. Yoshino, K. Kamiya, and H. Nasu, J. Non-Cryst. Solids 126, 68 (1990).

    Article  CAS  Google Scholar 

  36. K Kamiya, T. Yoko, K. Tanaka, and M. Takeuchi, J. Non-Cryst. Solids 121, 182 (1990).

    Article  CAS  Google Scholar 

  37. R. D. Husung and R. H. Doremus, J. Mater. Res. 5, 2209 (1990).

    Article  CAS  Google Scholar 

  38. R. M. Almeida and C. G. Pantano, J. Appl. Phys. 68, 4225 (1990).

    Article  CAS  Google Scholar 

  39. O. K. Johannson and C-L. Lee, Cyclic Monomers, edited by K. C. Frisch (Wiley Interscience, New York, 1972), p. 459.

  40. C. J. Brinker, J. Non-Cryst. Solids 100, 31 (1988).

    Article  CAS  Google Scholar 

  41. L. W. Kelts and N. J. Armstrong, J. Mater. Res. 4, 423 (1989).

    Article  CAS  Google Scholar 

  42. J. J. van Beek, D. Seykens, J. B. H. Jansen, and R. D. Schuiling, J. Non-Cryst. Solids 134, 14 (1991).

    Article  Google Scholar 

  43. J. K. West, B. F. Zhu, Y. C. Cheng, and L. L. Hench, J. Non-Cryst. Solids 121, 51 (1990).

    Article  CAS  Google Scholar 

  44. P. L. Pai, A. Chetty, R. Roat, N. Cox, and C. Ting, J. Electrochem. Soc. 134, 2829 (1987).

    Article  CAS  Google Scholar 

  45. M. P. Woo, J. L. Cain, and C-O. Lee, J. Electrochem. Soc. 137, 196 (1990).

    Article  CAS  Google Scholar 

  46. S. Ito, Y. Homma, E. Sasaki, S. Uchimura, and H. Morishima, J. Electrochem. Soc. 137, 1212 (1990).

    Article  CAS  Google Scholar 

  47. T. Mii and H. C. Casey, Jr. , J. Electronic Mater. 19, 1281 (1990).

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

About this article

Cite this article

Parrill, T.M. Transmission infrared study of acid-catalyzed sol-gel silica coatings during room ambient drying. Journal of Materials Research 7, 2230–2239 (1992). https://doi.org/10.1557/JMR.1992.2230

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1557/JMR.1992.2230

Navigation