Abstract

A solgel process was developed, through which silica films possessing both high antireflection and super water repellence were obtained. In this process, methyl-modified SiO2 sols synthesized by colloidal suspension of SiO2 particles and hexamethyldisilazane (HMDS) were used to deposit spinning-coating films on optical glass substrates. On the resultant films the contact angle for water increased with the increasing amount of HMDS in the reaction mixture. The biggest contact angle was 165°, and the lowest reflectivity on one-sided film reached 0.03%. The antireflections were high all the while. One advantage of this process is that neither a roughened surface nor fluoroalkyltrialkoxylsilane (FAS) is needed to obtained super water repellence.

© 2003 Optical Society of America

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References

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  1. H. G. Floch, P. F. Belleville, “Optical thin films from the sol-gel process,” in Optical Interference Coatings, F. Abeles, ed., Proc. SPIE2253, 764–790 (1994).
  2. D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).
  3. H. G. Floch, P. F. Belleville, P. M. Peġon, “Sol-gel optical coatings for lasers II,” Am. Ceram. Soc. Bull. 74, 84–89 (1995).
  4. K. Tadanaga, N. Katata, T. Minami, “Formation process of super-water-repellent Al2O3 coating films with high transparency by the sol-gel method,” J. Am. Ceram. Soc. 80, 3213–3216 (1997).
    [CrossRef]
  5. T. Minami, N. Katata, K. Tadanaga, “Preparation and characterization of super-water-repellent Al2O3 coating films with high transparency,” in Sol-Gel Optics IV, B. S. Dunn, J. D. Mackenzie, E. J. Pope, H. K. Schmidt, M. Yanane, eds., Proc. SPIE3136, 168–175 (1997).
  6. T. Nakagawa, M. Soga, “A new method for fabricating water repellent silica films having high heat-resistance using the sol-gel method,” J. Non-Cryst. Solids 260, 167–174 (1999).
    [CrossRef]
  7. B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
    [CrossRef]
  8. A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
    [CrossRef]
  9. K. Tadanaga, J. Morinaga, T. Minami, “Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method,” Chem. Mater. 12, 590–592 (2000).
    [CrossRef]
  10. K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
    [CrossRef]
  11. Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
    [CrossRef]
  12. M. Morra, E. Occhiehho, F. Garbassi, “Contact angle hysteresis in oxygen plasma treated poly(tetrafluoroethylene),” Langmuir 5, 872–876 (1989).
    [CrossRef]
  13. W. Stöber, A. Fink, E. Bohn, “Controlled growth of monodisperse silica spheres on the micron size range,” J. Colloid Interface Sci. 26, 62–66 (1968).
    [CrossRef]
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    [CrossRef] [PubMed]
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    [CrossRef] [PubMed]
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    [CrossRef]
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    [CrossRef] [PubMed]
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    [CrossRef]
  20. F. M. Fowkes, “Dispersion force contributions to surface and interfacial tensions, contact angles, and heats of immersion,” Adv. Chem. Ser. 43, 99–111 (1964).

2001 (1)

Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
[CrossRef]

2000 (2)

A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
[CrossRef]

K. Tadanaga, J. Morinaga, T. Minami, “Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method,” Chem. Mater. 12, 590–592 (2000).
[CrossRef]

1999 (2)

T. Nakagawa, M. Soga, “A new method for fabricating water repellent silica films having high heat-resistance using the sol-gel method,” J. Non-Cryst. Solids 260, 167–174 (1999).
[CrossRef]

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

1997 (1)

K. Tadanaga, N. Katata, T. Minami, “Formation process of super-water-repellent Al2O3 coating films with high transparency by the sol-gel method,” J. Am. Ceram. Soc. 80, 3213–3216 (1997).
[CrossRef]

1996 (1)

B. M. De Witte, D. Commers, J. B. Uytterhoeven, “Distribution of organic groups in silica gels prepared from organo-alkyoxysilane,” J. Non-Cryst. Solids 202, 35–41 (1996).
[CrossRef]

1995 (1)

H. G. Floch, P. F. Belleville, P. M. Peġon, “Sol-gel optical coatings for lasers II,” Am. Ceram. Soc. Bull. 74, 84–89 (1995).

1993 (1)

K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
[CrossRef]

1989 (1)

M. Morra, E. Occhiehho, F. Garbassi, “Contact angle hysteresis in oxygen plasma treated poly(tetrafluoroethylene),” Langmuir 5, 872–876 (1989).
[CrossRef]

1984 (1)

1980 (1)

1979 (1)

1968 (1)

W. Stöber, A. Fink, E. Bohn, “Controlled growth of monodisperse silica spheres on the micron size range,” J. Colloid Interface Sci. 26, 62–66 (1968).
[CrossRef]

1964 (1)

F. M. Fowkes, “Dispersion force contributions to surface and interfacial tensions, contact angles, and heats of immersion,” Adv. Chem. Ser. 43, 99–111 (1964).

1963 (1)

Abe, K.

A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
[CrossRef]

Aksmatsu, Y.

Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
[CrossRef]

Belleville, P. F.

H. G. Floch, P. F. Belleville, P. M. Peġon, “Sol-gel optical coatings for lasers II,” Am. Ceram. Soc. Bull. 74, 84–89 (1995).

H. G. Floch, P. F. Belleville, “Optical thin films from the sol-gel process,” in Optical Interference Coatings, F. Abeles, ed., Proc. SPIE2253, 764–790 (1994).

Bohn, E.

W. Stöber, A. Fink, E. Bohn, “Controlled growth of monodisperse silica spheres on the micron size range,” J. Colloid Interface Sci. 26, 62–66 (1968).
[CrossRef]

Boulton, J. M.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).

Commers, D.

B. M. De Witte, D. Commers, J. B. Uytterhoeven, “Distribution of organic groups in silica gels prepared from organo-alkyoxysilane,” J. Non-Cryst. Solids 202, 35–41 (1996).
[CrossRef]

De Witte, B. M.

B. M. De Witte, D. Commers, J. B. Uytterhoeven, “Distribution of organic groups in silica gels prepared from organo-alkyoxysilane,” J. Non-Cryst. Solids 202, 35–41 (1996).
[CrossRef]

Dolukhanyan, T.

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

Ebert, J.

Fink, A.

W. Stöber, A. Fink, E. Bohn, “Controlled growth of monodisperse silica spheres on the micron size range,” J. Colloid Interface Sci. 26, 62–66 (1968).
[CrossRef]

Floch, H. G.

H. G. Floch, P. F. Belleville, P. M. Peġon, “Sol-gel optical coatings for lasers II,” Am. Ceram. Soc. Bull. 74, 84–89 (1995).

H. G. Floch, P. F. Belleville, “Optical thin films from the sol-gel process,” in Optical Interference Coatings, F. Abeles, ed., Proc. SPIE2253, 764–790 (1994).

Fowkes, F. M.

F. M. Fowkes, “Dispersion force contributions to surface and interfacial tensions, contact angles, and heats of immersion,” Adv. Chem. Ser. 43, 99–111 (1964).

Garbassi, F.

M. Morra, E. Occhiehho, F. Garbassi, “Contact angle hysteresis in oxygen plasma treated poly(tetrafluoroethylene),” Langmuir 5, 872–876 (1989).
[CrossRef]

Han, J. H.

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

Hashimoto, K.

A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
[CrossRef]

Hong, B. S.

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

Inaba, H.

Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
[CrossRef]

Katata, N.

K. Tadanaga, N. Katata, T. Minami, “Formation process of super-water-repellent Al2O3 coating films with high transparency by the sol-gel method,” J. Am. Ceram. Soc. 80, 3213–3216 (1997).
[CrossRef]

T. Minami, N. Katata, K. Tadanaga, “Preparation and characterization of super-water-repellent Al2O3 coating films with high transparency,” in Sol-Gel Optics IV, B. S. Dunn, J. D. Mackenzie, E. J. Pope, H. K. Schmidt, M. Yanane, eds., Proc. SPIE3136, 168–175 (1997).

Kim, S. T.

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

Makita, K.

Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
[CrossRef]

Minami, T.

Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
[CrossRef]

K. Tadanaga, J. Morinaga, T. Minami, “Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method,” Chem. Mater. 12, 590–592 (2000).
[CrossRef]

K. Tadanaga, N. Katata, T. Minami, “Formation process of super-water-repellent Al2O3 coating films with high transparency by the sol-gel method,” J. Am. Ceram. Soc. 80, 3213–3216 (1997).
[CrossRef]

T. Minami, N. Katata, K. Tadanaga, “Preparation and characterization of super-water-repellent Al2O3 coating films with high transparency,” in Sol-Gel Optics IV, B. S. Dunn, J. D. Mackenzie, E. J. Pope, H. K. Schmidt, M. Yanane, eds., Proc. SPIE3136, 168–175 (1997).

Morinaga, J.

K. Tadanaga, J. Morinaga, T. Minami, “Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method,” Chem. Mater. 12, 590–592 (2000).
[CrossRef]

Morra, M.

M. Morra, E. Occhiehho, F. Garbassi, “Contact angle hysteresis in oxygen plasma treated poly(tetrafluoroethylene),” Langmuir 5, 872–876 (1989).
[CrossRef]

Nakagawa, T.

T. Nakagawa, M. Soga, “A new method for fabricating water repellent silica films having high heat-resistance using the sol-gel method,” J. Non-Cryst. Solids 260, 167–174 (1999).
[CrossRef]

Nakajima, A.

A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
[CrossRef]

Nakayama, I.

K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
[CrossRef]

Occhiehho, E.

M. Morra, E. Occhiehho, F. Garbassi, “Contact angle hysteresis in oxygen plasma treated poly(tetrafluoroethylene),” Langmuir 5, 872–876 (1989).
[CrossRef]

Ogawa, K.

K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
[CrossRef]

Park, M. S.

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

Partlow, D. B.

Pegon, P. M.

H. G. Floch, P. F. Belleville, P. M. Peġon, “Sol-gel optical coatings for lasers II,” Am. Ceram. Soc. Bull. 74, 84–89 (1995).

Portens, J. O.

Soga, M.

T. Nakagawa, M. Soga, “A new method for fabricating water repellent silica films having high heat-resistance using the sol-gel method,” J. Non-Cryst. Solids 260, 167–174 (1999).
[CrossRef]

K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
[CrossRef]

Stöber, W.

W. Stöber, A. Fink, E. Bohn, “Controlled growth of monodisperse silica spheres on the micron size range,” J. Colloid Interface Sci. 26, 62–66 (1968).
[CrossRef]

Sung, C.

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

Tadanaga, K.

K. Tadanaga, J. Morinaga, T. Minami, “Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method,” Chem. Mater. 12, 590–592 (2000).
[CrossRef]

K. Tadanaga, N. Katata, T. Minami, “Formation process of super-water-repellent Al2O3 coating films with high transparency by the sol-gel method,” J. Am. Ceram. Soc. 80, 3213–3216 (1997).
[CrossRef]

T. Minami, N. Katata, K. Tadanaga, “Preparation and characterization of super-water-repellent Al2O3 coating films with high transparency,” in Sol-Gel Optics IV, B. S. Dunn, J. D. Mackenzie, E. J. Pope, H. K. Schmidt, M. Yanane, eds., Proc. SPIE3136, 168–175 (1997).

Takada, Y.

K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
[CrossRef]

Tang, J. F.

J. F. Tang, Theory of Thin Film Optics (National Defence Industry Press, Beijing, China, 1990), pp. 197–199.

Teowee, G.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).

Uhlmann, D. R.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).

Uytterhoeven, J. B.

B. M. De Witte, D. Commers, J. B. Uytterhoeven, “Distribution of organic groups in silica gels prepared from organo-alkyoxysilane,” J. Non-Cryst. Solids 202, 35–41 (1996).
[CrossRef]

Watanabe, T.

A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
[CrossRef]

Weisenbach, L.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).

Yoldas, B. E.

Zelinski, B. J. J.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).

Adv. Chem. Ser. (1)

F. M. Fowkes, “Dispersion force contributions to surface and interfacial tensions, contact angles, and heats of immersion,” Adv. Chem. Ser. 43, 99–111 (1964).

Am. Ceram. Soc. Bull. (1)

H. G. Floch, P. F. Belleville, P. M. Peġon, “Sol-gel optical coatings for lasers II,” Am. Ceram. Soc. Bull. 74, 84–89 (1995).

Appl. Opt. (3)

Chem. Mater. (1)

K. Tadanaga, J. Morinaga, T. Minami, “Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method,” Chem. Mater. 12, 590–592 (2000).
[CrossRef]

J. Am. Ceram. Soc. (1)

K. Tadanaga, N. Katata, T. Minami, “Formation process of super-water-repellent Al2O3 coating films with high transparency by the sol-gel method,” J. Am. Ceram. Soc. 80, 3213–3216 (1997).
[CrossRef]

J. Colloid Interface Sci. (1)

W. Stöber, A. Fink, E. Bohn, “Controlled growth of monodisperse silica spheres on the micron size range,” J. Colloid Interface Sci. 26, 62–66 (1968).
[CrossRef]

J. Non-Cryst. Solids (2)

B. M. De Witte, D. Commers, J. B. Uytterhoeven, “Distribution of organic groups in silica gels prepared from organo-alkyoxysilane,” J. Non-Cryst. Solids 202, 35–41 (1996).
[CrossRef]

T. Nakagawa, M. Soga, “A new method for fabricating water repellent silica films having high heat-resistance using the sol-gel method,” J. Non-Cryst. Solids 260, 167–174 (1999).
[CrossRef]

J. Opt. Soc. Am. (1)

Jpn. J. Appl. Phys. (1)

K. Ogawa, M. Soga, Y. Takada, I. Nakayama, “Development of a transparent and ultrahydrophobic glass plate,” Jpn. J. Appl. Phys. 32, 614–615 (1993).
[CrossRef]

Langmuir (1)

M. Morra, E. Occhiehho, F. Garbassi, “Contact angle hysteresis in oxygen plasma treated poly(tetrafluoroethylene),” Langmuir 5, 872–876 (1989).
[CrossRef]

Thin Solid Films (3)

Y. Aksmatsu, K. Makita, H. Inaba, T. Minami, “Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane,” Thin Solid Films 389, 138–145 (2001).
[CrossRef]

B. S. Hong, J. H. Han, S. T. Kim, M. S. Park, T. Dolukhanyan, C. Sung, “Endurable water-repellent glass for automobiles,” Thin Solid Films 351, 274–278 (1999).
[CrossRef]

A. Nakajima, K. Abe, K. Hashimoto, T. Watanabe, “Preparation of hard super-hydrophobic films with visible light transmission,” Thin Solid Films 376, 140–143 (2000).
[CrossRef]

Other (4)

T. Minami, N. Katata, K. Tadanaga, “Preparation and characterization of super-water-repellent Al2O3 coating films with high transparency,” in Sol-Gel Optics IV, B. S. Dunn, J. D. Mackenzie, E. J. Pope, H. K. Schmidt, M. Yanane, eds., Proc. SPIE3136, 168–175 (1997).

H. G. Floch, P. F. Belleville, “Optical thin films from the sol-gel process,” in Optical Interference Coatings, F. Abeles, ed., Proc. SPIE2253, 764–790 (1994).

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, B. J. J. Zelinski, “Sol-gel synthesis of optical thin films and coatings,” in Sol-Gel Optics, J. D. Mackenzie, D. K. Ulrich, eds., Proc. SPIE1328, 270–294 (1990).

J. F. Tang, Theory of Thin Film Optics (National Defence Industry Press, Beijing, China, 1990), pp. 197–199.

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Figures (5)

Fig. 1
Fig. 1

Schematic representation of the modification of methyl groups to SiO2 particle surface and the formation of water repellent film.

Fig. 2
Fig. 2

AFM graphs of (a) N1, (b) N3, and (c) N5 with average roughness R q of 1.155, 11.061, and 16.131 nm, respectively.

Fig. 3
Fig. 3

Photograph of water drop on the super-water-repellent AR film prepared from sol N5. The drop is approximately 1 mm in diameter.

Fig. 4
Fig. 4

Contact angle for water with respect to films after heat treatment at different temperatures.

Fig. 5
Fig. 5

DTA plot of gel derived from sol N4.

Tables (1)

Tables Icon

Table 1 Data List of Physical and Chemical Properties of Methyl-Modified Sols and the Filmsa

Equations (3)

Equations on this page are rendered with MathJax. Learn more.

SiOC2H54+2H2OSiO2+4C2H5OH.
2 OH+CH33SiNHSiCH332 O-SiCH33+NH3.
cos θ=2GFGWd½/GW-1,

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