Abstract

Double optical monitoring is applied to determine the influence of main process parameters on the formation of sulfated zirconia and self-assembled mesoporous silica solgel films by dip coating. In addition, we analyze, for the first time to the best of our knowledge, the influence of withdrawal speed, temperature, and relative humidity on refractive-index and physical thickness variations (uncertainties of ±0.005 and ±7nm) during the process. Results provide insight into controlled production of single and multilayer films from complex fluids by dip coating.

© 2008 Optical Society of America

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  1. L. E. Scriven, "Physics and applications of dip coating and spin coating," Mater. Res. Soc. 121, 717-729 (1988).
    [CrossRef]
  2. P. R. Schunk, A. J. Hurd, and C. J. Brinker, "Free-meniscus coating processes," in Liquid Film Coating, S. F. Kistler and P. M. Schweizer, eds. (Chapman & Hall, 1997), pp. 673-708.
    [CrossRef]
  3. R. P. Spiers, C. V. Subabaraman, and W. L. Wilkinson, "Free coating of a Newtonian liquid onto a vertical surface," Chem. Eng. Sci. 29, 389-396 (1973).
  4. H. A. Macleod, Thin-Film Optical Filters, 2nd ed. (Macmillan, 1986).
    [CrossRef]
  5. F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).
  6. A. F. Michels, T. Menegotto, and F. Horowitz, "Interferometric monitoring of dip coating," Appl. Opt. 43, 820-823 (2004).
    [CrossRef] [PubMed]
  7. A. F. Michels, T. Menegotto, and F. Horowitz, "Optically monitored dip coating as a contactless viscometry method for liquid films," Appl. Opt. 44, 912-915 (2005).
    [CrossRef] [PubMed]
  8. A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
    [CrossRef] [PubMed]
  9. A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
    [CrossRef]
  10. L. A. Chiavacci, S. H. Pulcinelli, and C. V. Santilli, "Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid," Chem. Mater. 10, 986-993 (1998).
    [CrossRef]
  11. R. M. Grudzien, B. E. Grabicka, and M. Jaroniec, "Effective method for removal of polymeric template from SBA-16 silica combining extraction and temperature-controlled calcinations," J. Mater. Chem 16, 819-823 (2006).
    [CrossRef]

2006 (3)

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
[CrossRef]

R. M. Grudzien, B. E. Grabicka, and M. Jaroniec, "Effective method for removal of polymeric template from SBA-16 silica combining extraction and temperature-controlled calcinations," J. Mater. Chem 16, 819-823 (2006).
[CrossRef]

2005 (1)

2004 (1)

A. F. Michels, T. Menegotto, and F. Horowitz, "Interferometric monitoring of dip coating," Appl. Opt. 43, 820-823 (2004).
[CrossRef] [PubMed]

1998 (1)

L. A. Chiavacci, S. H. Pulcinelli, and C. V. Santilli, "Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid," Chem. Mater. 10, 986-993 (1998).
[CrossRef]

1997 (1)

P. R. Schunk, A. J. Hurd, and C. J. Brinker, "Free-meniscus coating processes," in Liquid Film Coating, S. F. Kistler and P. M. Schweizer, eds. (Chapman & Hall, 1997), pp. 673-708.
[CrossRef]

1993 (1)

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

1988 (1)

L. E. Scriven, "Physics and applications of dip coating and spin coating," Mater. Res. Soc. 121, 717-729 (1988).
[CrossRef]

1986 (1)

H. A. Macleod, Thin-Film Optical Filters, 2nd ed. (Macmillan, 1986).
[CrossRef]

1973 (1)

R. P. Spiers, C. V. Subabaraman, and W. L. Wilkinson, "Free coating of a Newtonian liquid onto a vertical surface," Chem. Eng. Sci. 29, 389-396 (1973).

Brinker, C. J.

P. R. Schunk, A. J. Hurd, and C. J. Brinker, "Free-meniscus coating processes," in Liquid Film Coating, S. F. Kistler and P. M. Schweizer, eds. (Chapman & Hall, 1997), pp. 673-708.
[CrossRef]

Chiavacci, L. A.

L. A. Chiavacci, S. H. Pulcinelli, and C. V. Santilli, "Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid," Chem. Mater. 10, 986-993 (1998).
[CrossRef]

Dawnay, E.

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

Fardad, A.

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

Grabicka, B. E.

R. M. Grudzien, B. E. Grabicka, and M. Jaroniec, "Effective method for removal of polymeric template from SBA-16 silica combining extraction and temperature-controlled calcinations," J. Mater. Chem 16, 819-823 (2006).
[CrossRef]

Green, M.

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

Grieneisen, H. P.

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

Grudzien, R. M.

R. M. Grudzien, B. E. Grabicka, and M. Jaroniec, "Effective method for removal of polymeric template from SBA-16 silica combining extraction and temperature-controlled calcinations," J. Mater. Chem 16, 819-823 (2006).
[CrossRef]

Horowitz, F.

A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
[CrossRef]

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, and F. Horowitz, "Optically monitored dip coating as a contactless viscometry method for liquid films," Appl. Opt. 44, 912-915 (2005).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, and F. Horowitz, "Interferometric monitoring of dip coating," Appl. Opt. 43, 820-823 (2004).
[CrossRef] [PubMed]

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

Hurd, A. J.

P. R. Schunk, A. J. Hurd, and C. J. Brinker, "Free-meniscus coating processes," in Liquid Film Coating, S. F. Kistler and P. M. Schweizer, eds. (Chapman & Hall, 1997), pp. 673-708.
[CrossRef]

Jaroniec, M.

R. M. Grudzien, B. E. Grabicka, and M. Jaroniec, "Effective method for removal of polymeric template from SBA-16 silica combining extraction and temperature-controlled calcinations," J. Mater. Chem 16, 819-823 (2006).
[CrossRef]

Macleod, H. A.

H. A. Macleod, Thin-Film Optical Filters, 2nd ed. (Macmillan, 1986).
[CrossRef]

Menegotto, T.

A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
[CrossRef]

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, and F. Horowitz, "Optically monitored dip coating as a contactless viscometry method for liquid films," Appl. Opt. 44, 912-915 (2005).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, and F. Horowitz, "Interferometric monitoring of dip coating," Appl. Opt. 43, 820-823 (2004).
[CrossRef] [PubMed]

Michels, A. F.

A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
[CrossRef]

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, and F. Horowitz, "Optically monitored dip coating as a contactless viscometry method for liquid films," Appl. Opt. 44, 912-915 (2005).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, and F. Horowitz, "Interferometric monitoring of dip coating," Appl. Opt. 43, 820-823 (2004).
[CrossRef] [PubMed]

Pulcinelli, S. H.

L. A. Chiavacci, S. H. Pulcinelli, and C. V. Santilli, "Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid," Chem. Mater. 10, 986-993 (1998).
[CrossRef]

Santilli, C. V.

A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
[CrossRef]

L. A. Chiavacci, S. H. Pulcinelli, and C. V. Santilli, "Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid," Chem. Mater. 10, 986-993 (1998).
[CrossRef]

Schunk, P. R.

P. R. Schunk, A. J. Hurd, and C. J. Brinker, "Free-meniscus coating processes," in Liquid Film Coating, S. F. Kistler and P. M. Schweizer, eds. (Chapman & Hall, 1997), pp. 673-708.
[CrossRef]

Scriven, L. E.

L. E. Scriven, "Physics and applications of dip coating and spin coating," Mater. Res. Soc. 121, 717-729 (1988).
[CrossRef]

Spiers, R. P.

R. P. Spiers, C. V. Subabaraman, and W. L. Wilkinson, "Free coating of a Newtonian liquid onto a vertical surface," Chem. Eng. Sci. 29, 389-396 (1973).

Subabaraman, C. V.

R. P. Spiers, C. V. Subabaraman, and W. L. Wilkinson, "Free coating of a Newtonian liquid onto a vertical surface," Chem. Eng. Sci. 29, 389-396 (1973).

Susin, M. B.

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

Wilkinson, W. L.

R. P. Spiers, C. V. Subabaraman, and W. L. Wilkinson, "Free coating of a Newtonian liquid onto a vertical surface," Chem. Eng. Sci. 29, 389-396 (1973).

Yeatman, E. M.

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

Appl. Opt. (2)

A. F. Michels, T. Menegotto, and F. Horowitz, "Interferometric monitoring of dip coating," Appl. Opt. 43, 820-823 (2004).
[CrossRef] [PubMed]

A. F. Michels, T. Menegotto, H. P. Grieneisen, M. B. Susin, and F. Horowitz, "Double optical monitoring of dip coating with a time-varying refractive index," Appl. Opt. 45, 1491-1494 (2006).
[CrossRef] [PubMed]

Appl. Opt. (1)

Chem. Eng. Sci. (1)

R. P. Spiers, C. V. Subabaraman, and W. L. Wilkinson, "Free coating of a Newtonian liquid onto a vertical surface," Chem. Eng. Sci. 29, 389-396 (1973).

Chem. Mater. (1)

L. A. Chiavacci, S. H. Pulcinelli, and C. V. Santilli, "Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid," Chem. Mater. 10, 986-993 (1998).
[CrossRef]

J. Mater. Chem (1)

R. M. Grudzien, B. E. Grabicka, and M. Jaroniec, "Effective method for removal of polymeric template from SBA-16 silica combining extraction and temperature-controlled calcinations," J. Mater. Chem 16, 819-823 (2006).
[CrossRef]

J. Non-Cryst. Solids (1)

A. F. Michels, T. Menegotto, C. V. Santilli, and F. Horowitz, "Temporal evolution of sulfated zirconia sol-gel during dip coating: analysis of mass drainage with time-varying refractive index," J. Non-Cryst. Solids 352, 5362-5367 (2006).
[CrossRef]

J. Phys (Paris) III (1)

F. Horowitz, E. M. Yeatman, E. Dawnay, A. Fardad, and M. Green, "Real-time optical monitoring of spin coating," J. Phys (Paris) III 3, 2059-2063 (1993).

Mater. Res. Soc. (1)

L. E. Scriven, "Physics and applications of dip coating and spin coating," Mater. Res. Soc. 121, 717-729 (1988).
[CrossRef]

Other (2)

P. R. Schunk, A. J. Hurd, and C. J. Brinker, "Free-meniscus coating processes," in Liquid Film Coating, S. F. Kistler and P. M. Schweizer, eds. (Chapman & Hall, 1997), pp. 673-708.
[CrossRef]

H. A. Macleod, Thin-Film Optical Filters, 2nd ed. (Macmillan, 1986).
[CrossRef]

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Figures (6)

Fig. 1
Fig. 1

Illustration of the dip coating batch process with laser probing.

Fig. 2
Fig. 2

Reflectance temporal evolution of SZC films during dip coating at different withdrawal speeds (U).

Fig. 3
Fig. 3

Temporal evolution of physical thickness and refractive index during dip coating of SZC at different withdrawal speeds.

Fig. 4
Fig. 4

Temporal evolution of physical thickness and refractive index during dip coating of SBA-15 solgel at different withdrawal speeds.

Fig. 5
Fig. 5

Temporal evolution of physical thickness and refractive index during dip coating of SZC at different temperatures.

Fig. 6
Fig. 6

Temporal evolution of physical thickness and refractive index during dip coating of SZC at different relative humidities.

Equations (1)

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h = C μ g ρ x t ,

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