Abstract

To prepare abrasion-resistant antireflective (AR) films for inertial confinement fusion, four solgel routes have been investigated on polysiloxane-modified and polyvinylalcohol- (PVA-) modified SiO2 sols. As confirmed with a transmissive electron microscope, different fractal structure characteristics of the modified SiO2 particles are disclosed by small-angle x-ray scattering technology. And it is these special fractal characteristics that determine the performance of AR films on the level of internal microstructure. A Si29 magic angle spinning and nuclear magnetic resonance study has been successfully applied in explaining the fractal microstructure and its relation to the laser-induced damage threshold (LIDT) of AR films. The films modified by PVA120000 or acetic acid-catalyzed polysiloxane have higher LIDTs than those films modified by PVA16000 or hydrochloride acid-catalyzed polysiloxane. The films from PVA-modified SiO2 sols have a stronger abrasion resistance but lower antireflection than those films from polysiloxane-modified SiO2 sols. In addition, the films from polysiloxane-modified SiO2 sols can possess high transmittance and high LIDT if the polysiloxane synthesis condition is appropriately chosen, but the abrasion resistance is not as good as that from PVA modification. If strong abrasion resistance is necessary, a possible resolution may be to choose a more appropriate hydrophilic polymer than PVA. If not, polysiloxane-modified silica sol can also work when polysiloxane is synthesized under acetic acid catalysis.

© 2005 Optical Society of America

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    [Crossref]
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    [Crossref]
  21. Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
    [Crossref]
  22. R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
    [Crossref]
  23. Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).
  24. K. D. Keefer and D. W. Schaefer, "Growth of fractally rough colloids," Phys. Rev. Lett. 56, 2376-2379 (1986).
    [Crossref] [PubMed]
  25. A. F. Craievich, "SAXS study of the porous fractal structure of tricalcuim silicate dry gels," J. Appl. Crystallogr. 20, 327-329 (1987).
    [Crossref]
  26. C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
    [Crossref]
  27. D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
    [Crossref]

2004 (2)

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

2003 (1)

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

2001 (1)

C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
[Crossref]

1997 (1)

J. C. Panitz and A. Wokaun, "Characterization of the sol-gel process using Raman spectroscopy organically modified silica gels prepared via the formic acid-alkoxide route," J. Sol-Gel Sci. Technol. 9, 251-263 (1997).
[Crossref]

1996 (1)

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

1995 (1)

H. G. Floch, P. F. Belleville, and P. M. Pegon, "Sol-gel optical coatings for lasers II," Am. Ceram. Soc. Bull. 74, 84-89 (1995).

1992 (1)

1987 (1)

A. F. Craievich, "SAXS study of the porous fractal structure of tricalcuim silicate dry gels," J. Appl. Crystallogr. 20, 327-329 (1987).
[Crossref]

1986 (1)

K. D. Keefer and D. W. Schaefer, "Growth of fractally rough colloids," Phys. Rev. Lett. 56, 2376-2379 (1986).
[Crossref] [PubMed]

1984 (1)

D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
[Crossref]

1968 (1)

W. Stöber, A. Fink, and E. Bohn, "Controlled growth of monodisperse silica spheres on the micro size range," J. Colloid Interface Sci. 26, 62-66 (1968).
[Crossref]

Adachi, K.

H. Hirashima, K. Adachi, and H. Imai, "Modification of sol-gel thin films by ion implantation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 33-40 (1994).

Andrew, J. E.

H. A. Mcinnes, J. E. Andrew, N. J. Bazin, A. J. Morris, and K. J. Porter, "Ultra violet laser damage and optical properties of high refractive index single layers, multiple layers and high/low index multilayer stacks," in Laser-Induced Damage in Optical Materials, G.J.Exarhos, A.H.Guenther, M.R.Kozlowski, and M.J.Soilean, eds., Proc. SPIE 3244, 500-508 (1998).

Awazu, K.

H. Imai, H. Hirashima, K. Awazu, and H. Onuki, "Modification and densification of sol-gel derived silica films at low temperatures," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 144-149 (1997).

Bazin, N. J.

H. A. Mcinnes, J. E. Andrew, N. J. Bazin, A. J. Morris, and K. J. Porter, "Ultra violet laser damage and optical properties of high refractive index single layers, multiple layers and high/low index multilayer stacks," in Laser-Induced Damage in Optical Materials, G.J.Exarhos, A.H.Guenther, M.R.Kozlowski, and M.J.Soilean, eds., Proc. SPIE 3244, 500-508 (1998).

Belleville, P. F.

H. G. Floch, P. F. Belleville, and P. M. Pegon, "Sol-gel optical coatings for lasers II," Am. Ceram. Soc. Bull. 74, 84-89 (1995).

H. G. Floch and P. F. Belleville, "Optical thin films from the sol-gel process," in Optical Interference Coatings, F.Abeles, ed., Proc. SPIE 2253, 764-790 (1994).

H. G. Floch and P. F. Belleville, "A scratch-resistant single-layer antireflective coating by a low temperature sol-gel route," in Sol-Gel Optics II, J.D.MacKenzie, ed., Proc. SPIE 1758, 135-149 (1992).

P. F. Belleville and P. Prene, "A sol-gel broad band antireflective and scratch-resistant coating for megajoule-class laser amplifer blastshields," in Third International Conference on Solid State Lasers for Application to Inertial Confinement Fusion, W.H.Lowdermilk, ed., Proc. SPIE 3492, 230-237 (1999).

P. F. Belleville, P. Prene, and B. Lambert, "A UV-cured sol-gel broadband antireflective and scratch-resistant coating for CRT," in Sol-Gel Optics V, B.S.Dunn. E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3943, 67-71 (2000).

P. F. Belleville and H. G. Floch, "Ammonia hardening of porous silica antireflective coatings," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 25-32 (1994).

Bernards, T. N.

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

Bohmer, M. R.

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

Bohn, E.

W. Stöber, A. Fink, and E. Bohn, "Controlled growth of monodisperse silica spheres on the micro size range," J. Colloid Interface Sci. 26, 62-66 (1968).
[Crossref]

Boulton, J. M.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, and B. J. J. Zelinski, "Sol-gel synthesis of optical thin films and coatings," in Sol-Gel Optics, J.D.MacKenzie, ed., Proc. SPIE 1328, 270-294 (1990).

Brinker, C. J.

C. J. Brinker and G. W. Scherer, Sol-Gel Science: the Physics and Chemistry of Sol-Gel Processing (Academic, 1990), pp. 160-173.

Cannel, D. S.

D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
[Crossref]

Craievich, A. F.

A. F. Craievich, "SAXS study of the porous fractal structure of tricalcuim silicate dry gels," J. Appl. Crystallogr. 20, 327-329 (1987).
[Crossref]

Despetis, F.

C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
[Crossref]

Dong, B. Z.

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Ehlers, H.

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

Etienne, P.

C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
[Crossref]

Fan, W. H.

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Fink, A.

W. Stöber, A. Fink, and E. Bohn, "Controlled growth of monodisperse silica spheres on the micro size range," J. Colloid Interface Sci. 26, 62-66 (1968).
[Crossref]

Floch, H. G.

H. G. Floch, P. F. Belleville, and P. M. Pegon, "Sol-gel optical coatings for lasers II," Am. Ceram. Soc. Bull. 74, 84-89 (1995).

H. G. Floch and P. F. Belleville, "Optical thin films from the sol-gel process," in Optical Interference Coatings, F.Abeles, ed., Proc. SPIE 2253, 764-790 (1994).

H. G. Floch and P. F. Belleville, "A scratch-resistant single-layer antireflective coating by a low temperature sol-gel route," in Sol-Gel Optics II, J.D.MacKenzie, ed., Proc. SPIE 1758, 135-149 (1992).

P. F. Belleville and H. G. Floch, "Ammonia hardening of porous silica antireflective coatings," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 25-32 (1994).

Frantzen, A.

P. W. Oliveira, H. Krug, A. Frantzen, M. Mennig, and H. Schmidt, "Generation of wet-chemical AR-coating on plastic substrates by use of polymerizable nanoparticles," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 452-461 (1997).

Hirashima, H.

H. Imai, H. Hirashima, K. Awazu, and H. Onuki, "Modification and densification of sol-gel derived silica films at low temperatures," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 144-149 (1997).

H. Imai and H. Hirashima, "Structural change in sol-gel derived SiO2 films using ultraviolet irradiation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 71-76 (1994).

H. Hirashima, K. Adachi, and H. Imai, "Modification of sol-gel thin films by ion implantation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 33-40 (1994).

Imai, H.

H. Hirashima, K. Adachi, and H. Imai, "Modification of sol-gel thin films by ion implantation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 33-40 (1994).

H. Imai and H. Hirashima, "Structural change in sol-gel derived SiO2 films using ultraviolet irradiation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 71-76 (1994).

H. Imai, H. Hirashima, K. Awazu, and H. Onuki, "Modification and densification of sol-gel derived silica films at low temperatures," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 144-149 (1997).

Kaiser, N.

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

Keefer, K. D.

K. D. Keefer and D. W. Schaefer, "Growth of fractally rough colloids," Phys. Rev. Lett. 56, 2376-2379 (1986).
[Crossref] [PubMed]

Krug, H.

P. W. Oliveira, H. Krug, A. Frantzen, M. Mennig, and H. Schmidt, "Generation of wet-chemical AR-coating on plastic substrates by use of polymerizable nanoparticles," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 452-461 (1997).

Lambert, B.

P. F. Belleville, P. Prene, and B. Lambert, "A UV-cured sol-gel broadband antireflective and scratch-resistant coating for CRT," in Sol-Gel Optics V, B.S.Dunn. E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3943, 67-71 (2000).

Lammers, J. H.

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

Lanux, S.

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

Li, Z. H.

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Marliere, C.

C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
[Crossref]

Martin, J. E.

D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
[Crossref]

Mcinnes, H. A.

H. A. Mcinnes, J. E. Andrew, N. J. Bazin, A. J. Morris, and K. J. Porter, "Ultra violet laser damage and optical properties of high refractive index single layers, multiple layers and high/low index multilayer stacks," in Laser-Induced Damage in Optical Materials, G.J.Exarhos, A.H.Guenther, M.R.Kozlowski, and M.J.Soilean, eds., Proc. SPIE 3244, 500-508 (1998).

Meng, Q. H.

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

Mennig, M.

P. W. Oliveira, H. Krug, A. Frantzen, M. Mennig, and H. Schmidt, "Generation of wet-chemical AR-coating on plastic substrates by use of polymerizable nanoparticles," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 452-461 (1997).

Mertin, M.

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

Morris, A. J.

H. A. Mcinnes, J. E. Andrew, N. J. Bazin, A. J. Morris, and K. J. Porter, "Ultra violet laser damage and optical properties of high refractive index single layers, multiple layers and high/low index multilayer stacks," in Laser-Induced Damage in Optical Materials, G.J.Exarhos, A.H.Guenther, M.R.Kozlowski, and M.J.Soilean, eds., Proc. SPIE 3244, 500-508 (1998).

Mutter, C.

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

Niederwald, H.

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

Oliveira, P. W.

P. W. Oliveira, H. Krug, A. Frantzen, M. Mennig, and H. Schmidt, "Generation of wet-chemical AR-coating on plastic substrates by use of polymerizable nanoparticles," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 452-461 (1997).

Onuki, H.

H. Imai, H. Hirashima, K. Awazu, and H. Onuki, "Modification and densification of sol-gel derived silica films at low temperatures," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 144-149 (1997).

Panitz, J. C.

J. C. Panitz and A. Wokaun, "Characterization of the sol-gel process using Raman spectroscopy organically modified silica gels prepared via the formic acid-alkoxide route," J. Sol-Gel Sci. Technol. 9, 251-263 (1997).
[Crossref]

Peeters, M. P.

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

Pegon, P. M.

H. G. Floch, P. F. Belleville, and P. M. Pegon, "Sol-gel optical coatings for lasers II," Am. Ceram. Soc. Bull. 74, 84-89 (1995).

Phalippou, J.

C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
[Crossref]

Porter, K. J.

H. A. Mcinnes, J. E. Andrew, N. J. Bazin, A. J. Morris, and K. J. Porter, "Ultra violet laser damage and optical properties of high refractive index single layers, multiple layers and high/low index multilayer stacks," in Laser-Induced Damage in Optical Materials, G.J.Exarhos, A.H.Guenther, M.R.Kozlowski, and M.J.Soilean, eds., Proc. SPIE 3244, 500-508 (1998).

Prene, P.

P. F. Belleville, P. Prene, and B. Lambert, "A UV-cured sol-gel broadband antireflective and scratch-resistant coating for CRT," in Sol-Gel Optics V, B.S.Dunn. E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3943, 67-71 (2000).

P. F. Belleville and P. Prene, "A sol-gel broad band antireflective and scratch-resistant coating for megajoule-class laser amplifer blastshields," in Third International Conference on Solid State Lasers for Application to Inertial Confinement Fusion, W.H.Lowdermilk, ed., Proc. SPIE 3492, 230-237 (1999).

Ristau, D.

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

Rong, L. X.

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Schaefer, D. W.

K. D. Keefer and D. W. Schaefer, "Growth of fractally rough colloids," Phys. Rev. Lett. 56, 2376-2379 (1986).
[Crossref] [PubMed]

D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
[Crossref]

Scherer, G. W.

C. J. Brinker and G. W. Scherer, Sol-Gel Science: the Physics and Chemistry of Sol-Gel Processing (Academic, 1990), pp. 160-173.

Schmidt, H.

P. W. Oliveira, H. Krug, A. Frantzen, M. Mennig, and H. Schmidt, "Generation of wet-chemical AR-coating on plastic substrates by use of polymerizable nanoparticles," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 452-461 (1997).

Shen, J.

G. M. Wu, J. Wang, and J. Shen, "Preparation and properties of scratch-resistant nano porous broadband AR silica films derived by a two-step catalytic sol-gel process," in Fourth International Conference on Thin Film Physics and Applications, J.Chu, P.Lin, and Y.Chang, eds., Proc. SPIE 4086, 807-810 (2000).

Stöber, W.

W. Stöber, A. Fink, and E. Bohn, "Controlled growth of monodisperse silica spheres on the micro size range," J. Colloid Interface Sci. 26, 62-66 (1968).
[Crossref]

Sun, Y. H.

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Teowee, G.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, and B. J. J. Zelinski, "Sol-gel synthesis of optical thin films and coatings," in Sol-Gel Optics, J.D.MacKenzie, ed., Proc. SPIE 1328, 270-294 (1990).

Thomas, I. M.

Uhlmann, D. R.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, and B. J. J. Zelinski, "Sol-gel synthesis of optical thin films and coatings," in Sol-Gel Optics, J.D.MacKenzie, ed., Proc. SPIE 1328, 270-294 (1990).

Wang, J.

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

G. M. Wu, J. Wang, and J. Shen, "Preparation and properties of scratch-resistant nano porous broadband AR silica films derived by a two-step catalytic sol-gel process," in Fourth International Conference on Thin Film Physics and Applications, J.Chu, P.Lin, and Y.Chang, eds., Proc. SPIE 4086, 807-810 (2000).

Weisenbach, L.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, and B. J. J. Zelinski, "Sol-gel synthesis of optical thin films and coatings," in Sol-Gel Optics, J.D.MacKenzie, ed., Proc. SPIE 1328, 270-294 (1990).

Wiltzius, P.

D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
[Crossref]

Wokaun, A.

J. C. Panitz and A. Wokaun, "Characterization of the sol-gel process using Raman spectroscopy organically modified silica gels prepared via the formic acid-alkoxide route," J. Sol-Gel Sci. Technol. 9, 251-263 (1997).
[Crossref]

Wu, D.

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Wu, G. M.

G. M. Wu, J. Wang, and J. Shen, "Preparation and properties of scratch-resistant nano porous broadband AR silica films derived by a two-step catalytic sol-gel process," in Fourth International Conference on Thin Film Physics and Applications, J.Chu, P.Lin, and Y.Chang, eds., Proc. SPIE 4086, 807-810 (2000).

Xu, Y.

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Xü, Y.

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

Zelinski, B. J.

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, and B. J. J. Zelinski, "Sol-gel synthesis of optical thin films and coatings," in Sol-Gel Optics, J.D.MacKenzie, ed., Proc. SPIE 1328, 270-294 (1990).

Zhang, R.

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

Zhao, H.

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

Acta Phys. Sin. (1)

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Two fractal structures of methyl-modified silica gels by SAXS," Acta Phys. Sin. 52, 442-447 (2003).

Am. Ceram. Soc. Bull. (1)

H. G. Floch, P. F. Belleville, and P. M. Pegon, "Sol-gel optical coatings for lasers II," Am. Ceram. Soc. Bull. 74, 84-89 (1995).

Appl. Opt. (1)

Appl. Surf. Sci. (1)

Y. Xu, Z. H. Li, W. H. Fan, D. Wu, Y. H. Sun, L. X. Rong, and B. Z. Dong, "Density fluctuation in silica-PVA hybrid gels determined by small-angle X-ray scattering," Appl. Surf. Sci. 225, 116-123 (2004).
[Crossref]

J. Appl. Crystallogr. (1)

A. F. Craievich, "SAXS study of the porous fractal structure of tricalcuim silicate dry gels," J. Appl. Crystallogr. 20, 327-329 (1987).
[Crossref]

J. Colloid Interface Sci. (1)

W. Stöber, A. Fink, and E. Bohn, "Controlled growth of monodisperse silica spheres on the micro size range," J. Colloid Interface Sci. 26, 62-66 (1968).
[Crossref]

J. Non-Cryst. Solids (1)

C. Marliere, F. Despetis, P. Etienne, and J. Phalippou, "Two fractal structures in aerogel," J. Non-Cryst. Solids 285, 175-180 (2001).
[Crossref]

J. Sol-Gel Sci. Technol. (1)

J. C. Panitz and A. Wokaun, "Characterization of the sol-gel process using Raman spectroscopy organically modified silica gels prepared via the formic acid-alkoxide route," J. Sol-Gel Sci. Technol. 9, 251-263 (1997).
[Crossref]

J. Supercrit. Fluids (1)

R. Zhang, Y. Xü, Q. H. Meng, J. Wang, H. Zhao, and B. Z. Dong, "Small angle x-ray scattering study of microstructure changes of organic hydrogels from supercritical carbon dioxide drying," J. Supercrit. Fluids 28, 263-276 (2004).
[Crossref]

Phys. Rev. Lett. (2)

K. D. Keefer and D. W. Schaefer, "Growth of fractally rough colloids," Phys. Rev. Lett. 56, 2376-2379 (1986).
[Crossref] [PubMed]

D. W. Schaefer, J. E. Martin, P. Wiltzius, and D. S. Cannel, "Fractal geometry of colloidal aggregates," Phys. Rev. Lett. 52, 2371-2374 (1984).
[Crossref]

Thin Solid Films (1)

C. Mutter, T. N. M. Bernards, M. P. J. Peeters, J. H. Lammers, and M. R. Bohmer, "The effect of the solvent on the cross-link density of SuO2 coatings," Thin Solid Films 351, 95-98 (1996).
[Crossref]

Other (15)

Ref. , pp. 212-215.

C. J. Brinker and G. W. Scherer, Sol-Gel Science: the Physics and Chemistry of Sol-Gel Processing (Academic, 1990), pp. 160-173.

H. A. Mcinnes, J. E. Andrew, N. J. Bazin, A. J. Morris, and K. J. Porter, "Ultra violet laser damage and optical properties of high refractive index single layers, multiple layers and high/low index multilayer stacks," in Laser-Induced Damage in Optical Materials, G.J.Exarhos, A.H.Guenther, M.R.Kozlowski, and M.J.Soilean, eds., Proc. SPIE 3244, 500-508 (1998).

H. G. Floch and P. F. Belleville, "Optical thin films from the sol-gel process," in Optical Interference Coatings, F.Abeles, ed., Proc. SPIE 2253, 764-790 (1994).

D. R. Uhlmann, J. M. Boulton, G. Teowee, L. Weisenbach, and B. J. J. Zelinski, "Sol-gel synthesis of optical thin films and coatings," in Sol-Gel Optics, J.D.MacKenzie, ed., Proc. SPIE 1328, 270-294 (1990).

H. G. Floch and P. F. Belleville, "A scratch-resistant single-layer antireflective coating by a low temperature sol-gel route," in Sol-Gel Optics II, J.D.MacKenzie, ed., Proc. SPIE 1758, 135-149 (1992).

P. F. Belleville and P. Prene, "A sol-gel broad band antireflective and scratch-resistant coating for megajoule-class laser amplifer blastshields," in Third International Conference on Solid State Lasers for Application to Inertial Confinement Fusion, W.H.Lowdermilk, ed., Proc. SPIE 3492, 230-237 (1999).

P. F. Belleville, P. Prene, and B. Lambert, "A UV-cured sol-gel broadband antireflective and scratch-resistant coating for CRT," in Sol-Gel Optics V, B.S.Dunn. E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3943, 67-71 (2000).

G. M. Wu, J. Wang, and J. Shen, "Preparation and properties of scratch-resistant nano porous broadband AR silica films derived by a two-step catalytic sol-gel process," in Fourth International Conference on Thin Film Physics and Applications, J.Chu, P.Lin, and Y.Chang, eds., Proc. SPIE 4086, 807-810 (2000).

P. W. Oliveira, H. Krug, A. Frantzen, M. Mennig, and H. Schmidt, "Generation of wet-chemical AR-coating on plastic substrates by use of polymerizable nanoparticles," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 452-461 (1997).

P. F. Belleville and H. G. Floch, "Ammonia hardening of porous silica antireflective coatings," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 25-32 (1994).

H. Imai, H. Hirashima, K. Awazu, and H. Onuki, "Modification and densification of sol-gel derived silica films at low temperatures," in Sol-Gel Optics IV, B.S.Dunn. J.D.MacKenzie, E.J. A.Pope, H.K.Schmidt, and M.Yamane, eds., Proc. SPIE 3136, 144-149 (1997).

H. Imai and H. Hirashima, "Structural change in sol-gel derived SiO2 films using ultraviolet irradiation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 71-76 (1994).

H. Hirashima, K. Adachi, and H. Imai, "Modification of sol-gel thin films by ion implantation," in Sol-Gel Optics III, J.D.MacKenzie, ed., Proc. SPIE 2288, 33-40 (1994).

S. Lanux, N. Kaiser, H. Niederwald, M. Mertin, H. Ehlers, and D. Ristau, "Broadband antireflection coatings deposited with ion-assisted evaporation," in Advances in Optical Interference Coatings, C.Amra and H.A.Macleod, eds., Proc. SPIE 3738, 76-80 (1999).

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Figures (10)

Fig. 1
Fig. 1

AFM morphology of a glass substrate: R q = 0.814 nm .

Fig. 2
Fig. 2

Schematic of the testing optics for LIDT. B and C are the calorimeter and the photodiode.

Fig. 3
Fig. 3

Transmittance of abrasion-resistant AR film. X C or X A is the volume percentage of polisiloxane C or A. C PVA is the weight percentage of PVA.

Fig. 4
Fig. 4

Abrasion-resistance testing results of AR film. X C or X A is the volume percentage of polisiloxane C or A. C PVA is the weight percentage of PVA.

Fig. 5
Fig. 5

AFM morphologies of abrasion-resistant AR films: (a) SC2, R q = 6.391 nm ; (b) SC5, R q = 17.542 nm ; (c) SA2, R q = 4.788 nm ; (d) SA5, R q = 6.414 nm ; (e) SPL2, R q = 1.302 nm ; (f) SPL5, R q = 2.767 nm ; (g) SPH2, R q = 1.657 nm ; (h) SPH5, R q = 7.272 nm .

Fig. 6
Fig. 6

Laser-induced damage morphologies of AR films: (a) USiO, (b) SC2, (c) SA2, (d) SPL2, (e) SPL5, (f) SPH2, (g) SPH5.

Fig. 7
Fig. 7

Si 29 MAS–NMR results of gels.

Fig. 8
Fig. 8

Fractal curves of polymer-modified SiO 2 sols from SAXS.

Fig. 9
Fig. 9

TEM photographs of unmodified SiO 2 sol (a) USiO and modified SiO 2 sols (b) SC4, (c) SA4, (d) SPH5.

Fig. 10
Fig. 10

Schematic presentation of the linkage among SiO 2 particles by (a) polysiloxane C (b) polysiloxane A, (c) PVA.

Tables (3)

Tables Icon

Table 1 Detailed Components of Sols a

Tables Icon

Table 2 LIDT ( J cm 2 , 1064 nm, 1 ns) of Films

Tables Icon

Table 3 Fractal Structure Parameters Calculated from SAXS Results a

Equations (3)

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

A F Q = n = 1 4 n S n n = 1 4 S n ,
Si ( OC 2 H 5 ) 4 + 4 H 2 O hydrolysis fast HO Si ( OH ) 3 + 4 C 2 H 5 OH ,
Si ( OC 2 H 5 ) 4 + 4 CH 3 COOH SiO 2 + 2 H 2 O + 4 CH 3 COOC 2 H 5 .

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