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Water-repellent metal oxide film and method of forming same on glass substrate

Assignee: Central Glass Co Ltd
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Filing: 1993-01-29
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Granted: 1995-05-09
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Expires: 2013-01-29
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Abstract

Abstract The invention relates to a multilayered metal oxide film formed on a glass substrate by the sol-gel process. The film has a first metal oxide layer formed on the glass substrate and a second metal oxide layer formed on the first layer. To make the first layer minutely rough, at least two sols are respectively prepared from at least one compound selected from the group consisting of metal alkoxides and metal acetylacetonatos, such that polymers of the sols have different average molecular weights. Then, the at least two sols are mixed with a solvent so as to prepare a first coating solution. The first coating solution is applied to the glass substrate so as to form thereon a first sol film. The thus coated glass substrate is heated so as to transform the first sol film into the first metal oxide layer. To form a water-repellent metal oxide film on the first layer, a silane compound containing a fluorocarbon group is mixed with a solvent so as to prepare a second coating solution. After that, the second coating solution is applied to the first metal oxide layer so as to form thereon a second sol film. Then, the glass substrate is heated so as to transform the second sol film into the second metal oxide layer which is water-repellent.

Inventors

  • 👤 Ichiro Nakamura
  • 👤 Seiji Yamazaki
  • 👤 Osamu Takahashi
  • 👤 Hiroaki Arai
  • 👤 Shigeo Hamaguchi

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-08 07:02
CPC Classifications
C; C03; C03C; C03C17/00; C03C17/34; C03C2217/00; C03C2217/40; C03C2217/70; C03C2217/76

Claims Analysis

Total Claims: 18
Claim 1
Independent Claim 225 words
A multilayered film formed on a glass substrate, the film having a first layer of metal oxide having numerous micro-pits and a second layer of metal oxide which is water-repellent, the film being prepared by a method comprising the steps of: (a) preparing at least two sols respectively from at least one compound so as to disperse therein at least two polymers of said at least one compound, said at least one compound being selected from the group consisting of metal alkoxides and metal acetylacetonatos, said at least two polymers having different average molecular weights; (b) mixing said at least two sols with a solvent so as to prepare a first coating solution; (c) applying the first coating solution to the glass substrate so as to form thereon a first sol film; (d) heating the glass substrate so as to transform the first sol film into a first metal oxide layer which has a minutely rough surface having numerous micro-pits thereon; (e) mixing a silane compound containing a fluorocarbon group with a solvent so as to prepare a second coating solution; (f) applying the second coating solution to the first metal oxide layer so as to form thereon a second sol film; and (g) heating the glass substrate so as to transform the second sol film into a second metal oxide layer which is water-repellent.
Claim 2
Dependent Claim 225 words
A multilayered film formed on a glass substrate, the film having a first layer of metal oxide having numerous micro-pits and a second layer of metal oxide which is water-repellent, the film being prepared by a method comprising the steps of: (a) preparing at least two sols respectively from at least one compound so as to disperse therein at least two polymers of said at least one compound, said at least one compound being selected from the group consisting of metal alkoxides and metal acetylacetonatos, said at least two polymers having different average molecular weights; (b) mixing said at least two sols with a solvent so as to prepare a first coating solution; (c) applying the first coating solution to the glass substrate so as to form thereon a first sol film; (d) heating the glass substrate so as to transform the first sol film into a first metal oxide layer which has a minutely rough surface having numerous micro-pits thereon; (e) mixing a silane compound containing a fluorocarbon group with a solvent so as to prepare a second coating solution; (f) applying the second coating solution to the first metal oxide layer so as to form thereon a second sol film; and (g) heating the glass substrate so as to transform the second sol film into a second metal oxide layer which is water-repellent.
Claim 3
Dependent Claim 139 words
A metal oxide film formed on a glass substrate, the film having numerous micro-pits formed thereon, the film being prepared by a method comprising the steps of: (a) preparing at least two sols respectively from at least one compound so as to disperse therein at least two polymers of said at least one compound, said at least one compound being selected from the group consisting of metal alkoxides and metal acetylacetonatos said at least two polymers having different average molecular weights; (b) mixing said at least two sols with a solvent so as to prepare a coating solution; (c) applying the coating solution to the glass substrate so as to form thereon a sol film; and (d) heating the glass substrate so as to transform the sol film into a metal oxide film which has a minutely rough surface.
Claim 4
Dependent Claim 139 words
A metal oxide film formed on a glass substrate, the film having numerous micro-pits formed thereon, the film being prepared by a method comprising the steps of: (a) preparing at least two sols respectively from at least one compound so as to disperse therein at least two polymers of said at least one compound, said at least one compound being selected from the group consisting of metal alkoxides and metal acetylacetonatos said at least two polymers having different average molecular weights; (b) mixing said at least two sols with a solvent so as to prepare a coating solution; (c) applying the coating solution to the glass substrate so as to form thereon a sol film; and (d) heating the glass substrate so as to transform the sol film into a metal oxide film which has a minutely rough surface.
Claim 5
Dependent Claim 50 words
A multilayered film according to claim 1, wherein one polymer of said at least two polymers has an average molecular weight ranging from about 800 to about 10,000, and the other at least one polymer of said at least two polymers has an average molecular weight not lower than 10,000.
Claim 6
Dependent Claim 25 words
A multilayered film according to claim 3, wherein the other at least one polymer has an average molecular weight ranging from 10,000 to about 600,000.
Claim 7
Dependent Claim 26 words
A multilayered film according to claim 4, wherein the other at least one polymer has an average molecular weight ranging from about 50,000 to about 500,000.
Claim 8
Dependent Claim 23 words
A multilayered film according to claim 3, wherein the one polymer has an average molecular weight ranging from about 1,500 to about 8,000.
Claim 9
Dependent Claim 39 words
A multilayered film according to claim 1, wherein at step (b) said one polymer and the other at least one polymer are mixed in the ratio of 1:10 to 30:1 by the number of moles calculated as metal oxide.
Claim 10
Dependent Claim 14 words
A multilayered film according to claim 1, wherein said solvent is an alcohol solution.
Claim 11
Dependent Claim 26 words
A multilayered film according to claim 1, wherein the concentration of said silane compound in the second coating solution is not less than 0.1 wt. %.
Claim 12
Dependent Claim 24 words
A multilayered film according to claim 1, wherein the glass substrate is heated at step (d) at a temperature not lower than 100° C.
Claim 13
Dependent Claim 24 words
A multilayered film according to claim 1, wherein the glass substrate is heated at step (d) at a temperature not lower than 100° C.
Claim 14
Dependent Claim 33 words
A multilayered film according to claim 1, wherein said at least one compound is selected from the group consisting of alkoxides of Si, Ti and Zr and acetylacetonatos of Si, Ti and Zr.
Claim 15
Dependent Claim 22 words
A multilayered film according to claim 1, wherein at step (b) viscosity of the first coating solution is adjusted to 1-10 centipoises.
Claim 16
Dependent Claim 38 words
A multilayered film according to claim 1, wherein at step (b) the concentration of said at least two polymers in the first coating solution is in the range from 0.01 to 10 wt. % calculated as metal oxide.
Claim 17
Dependent Claim 33 words
A multilayered film according to claim 1, wherein at step (c) the first coating solution is applied to the glass substrate in an atmosphere having a relative humidity ranging from 20 to 80%.
Claim 18
Dependent Claim 28 words
A multilayered film according to claim 1, wherein the numerous micro-pits are stable on baking the first metal oxide layer at a temperature of at least 500° C.

References Cited (Backward Citations)

JPS60231442A Cited
JPH01246160A Cited
JPH0375243A Cited
JPH03247538A Cited
JPH03247537A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1998-05-08 1998-11-07 1999-05-09 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2002-05-08 2002-11-07 2003-05-09 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2006-05-08 2006-11-07 2007-05-09 $7700.00 Window Closed / Lapsed

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