Skip to main content
Log in

Time-resolved light scattering studies of Spin-coated titanium dioxide

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

Abstract

Spin coating of titanium alkoxides is a fast and straightforward method of forming compact and durable titanium dioxide thin films. In this report, an optical interference technique is used to understand the dynamics of titanium dioxide thin film formation during the spin coating process of titanium (IV) ethoxide sols, and a 4-stage thinning model is proposed. Optical monitoring of interference fringes as a function of time enables determination of the time-dependent film thickness through measurement of the interference fringe separation while the sol to gel transition can be monitored by analyzing the fringe visibility. For films that are spun at 2,000 rpm or faster, a spin duration of 5 s is sufficient for the film to reach its final thickness. At a given spin speed, spin times longer than 5 s do not affect the final film thickness. However, thinner final film thicknesses can be achieved by increasing the spin speed. All films were found to densify on annealing with an annealed thickness approximately 0.4 times that of the pre-anneal thickness regardless of spin speed. Spin-coated titanium dioxide films are expected to play an important role in low-cost and scalable next generation solar cells employing dyes and quantum dots as the light harvesting agents.

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.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6

Similar content being viewed by others

Notes

  1. The solution gradually degrades over time, with the formation of a milky white gel becoming evident. The process is slowed by refrigeration, and the solution can be stored and used for about a month if refrigerated.

References

  1. Partlow DP, O’Keeffe TW (1990) Thirty-seven layer optical filter from polymerized solgel solutions. Appl Opt 29(10):1526–1529

    Article  CAS  Google Scholar 

  2. Hinczewski DS, Hinczewski M, Tepehan F, Tepehan G (2005) Optical filters from SiO2 and TiO2 multi-layers using sol-gel spin coating method. Sol. Energ. Mat. Sol. Cells 87:181–196

    Article  CAS  Google Scholar 

  3. Su C, Hong B-Y, Tseng C-M (2004) Sol-gel preparation and photocatalysis of titanium dioxide. Catal Today 96(3):119–126

    Article  CAS  Google Scholar 

  4. Lai C-H, Liu C-Y, Hsu C-H, Lee Y-M, Lin J-S, Yang H (2013) Effect of firing atmosphere and bottom electrode on resistive switching mode in TiO2 thin films. Thin Solid Films 529:430–434

    Article  CAS  Google Scholar 

  5. Burke A, Ito S, Snaith H, Bach U, Kwiatkowski J, Grätzel M (2008) The function of a TiO2 compact layer in dye-sensitized solar cells incorporating “Planar” organic dyes. Nano Lett 8(4):977–981

    Article  CAS  Google Scholar 

  6. Yu H, Zhang S, Zhao H, Will G, Liu P (2009) An efficient and low-cost TiO2 compact layer for performance improvement of dye-sensitized solar cells. Electrochim Acta 54(4):1319–1324

    Article  CAS  Google Scholar 

  7. Kim J-K, Seo H, Son M-K, Shin I, Choi J-H, Choi S-W, Kim H-J (2011) The optimization of TiO2 compact layer in dye-sensitized solar cell by the analysis of performance and internal impedance. Phys Status Solidi C 8(2):634–636

    Article  CAS  Google Scholar 

  8. Goh C, Coakley KM, McGehee MD (2005) Nanostructuring titania by embossing with polymer molds made from anodic alumina templates. Nano Lett 5(8):1545–1549

    Article  CAS  Google Scholar 

  9. Smith NJ, Emmett KJ, Rosenthal SJ (2008) Photovoltaic cells fabricated by electrophoretic deposition of CdSe nanocrystals. Appl Phys Lett 93:043504

    Article  Google Scholar 

  10. Hashizume M, Kunitake T (2003) Preparation of self-supporting ultrathin films of titania by spin coating. Langmuir 19:10172–10178

    Article  CAS  Google Scholar 

  11. Horowitz F (1994) Optical monitoring of the sol to gel transition in spinning silica films. SPIE 2288:67–70

    Article  CAS  Google Scholar 

  12. Birnie DP III, Manley M (1997) Combined flow and evaporation of fluid on a spinning disk. Phys Fluids 9(4):870

    Article  CAS  Google Scholar 

  13. Heriot SY, Jones RAL (2005) An interfacial instability in a transient wetting layer leads to lateral phase separation in thin spin-cast polymer-blend films. Nat Mater 4:782–786

    Article  CAS  Google Scholar 

  14. Emslie AG, Bonner FT, Peck LG (1958) Flow of a viscous liquid on a rotating disk. J Appl Phys 29:858–862

    Article  CAS  Google Scholar 

  15. Meyerhofer D (1978) Characteristics of resist films produced by spinning. J Appl Phys 49(7):3993–3997

    Article  Google Scholar 

  16. Birnie DP, Hau SK, Kamber DS (2005) Effect of ramping-up rate on film thickness for spin-on processing. J Mater Sci Mater Electron 16(11/12):715–720

    Article  CAS  Google Scholar 

  17. Hecht E, Optics, 4th ed. (Addison Wesley)

  18. Sakka S (1994) Preparation and properties of sol-gel coating films. J Solgel Sci Technol 2(1-3):451–455

    Article  CAS  Google Scholar 

  19. Burgos M, Langlet M (1999) Condensation and densification mechanism of sol–gel TiO2 layers at low temperature. J Solgel Sci Technol 16(3):267–276

    Article  CAS  Google Scholar 

  20. Scriven LE (1988) Physics and applications of dip coating and spin coating. Mater Res Soc Symp Proc 121:717–729

    Article  CAS  Google Scholar 

  21. Keddie JL, Braun PV, Giannelis EP (1994) Interrelationship between densification, crystallization, and chemical evolution in sol-gel titania thin films. J Am Ceram Soc 77(6):1592–1596

    Article  CAS  Google Scholar 

  22. Lide, DR (eds) (2008) Handbook of chemistry and physics, 89th edn. CRC Press, Boca Raton

    Google Scholar 

Download references

Acknowledgments

This work was partially funded by National Science Foundation EPS-1004083. We also gratefully acknowledge student support for Mr. Ben Bunnell provided by TNSCORE (Tennessee EPSCORE).

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Nathanael J. Smith.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Smith, N.J., Bunnell, B. Time-resolved light scattering studies of Spin-coated titanium dioxide. J Sol-Gel Sci Technol 67, 429–435 (2013). https://doi.org/10.1007/s10971-013-3095-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10971-013-3095-5

Keywords

Navigation