Patent US5851674A successfully refreshed from Google Patents.
US5851674A
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Antisoiling coatings for antireflective surfaces and methods of preparation
Assignee: 3M Co
•
Filing: 1997-07-30
•
Granted: 1998-12-22
•
Expires: 2017-07-30
Abstract
Abstract An antisoiling coating for an antireflective surface, particularly the outer surface of an antireflective film stack, wherein the antisoiling coating includes a fluorinated siloxane, preferably prepared by applying a coating composition of a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Inventors
- 👤 Mark J. Pellerite
- 👤 Judith M. Invie
- 👤 Dong-Wei Zhu
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 20:16
CPC Classifications
C; C09; C09D; C09D5/00; C09D5/006; G; G02; G02B; G02B1/00; G02B1/10; G02B1/11; G02B1/111; B; B05; B05D; B05D1/00; B05D1/18; B82; B82Y; B82Y30/00; C09D183/00; C09D183/02; C09D4/00; C09D7/00; C09D7/20; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/3154; Y10T428/31544; Y10T428/31652; Y10T428/31663
Claims Analysis
Total Claims: 48
Claim 1
Independent Claim
116 words
An antireflective article comprising a substrate having an antireflective surface and an antisoiling coating of less than about 100 Angstroms thick deposited thereon; wherein the antisoiling coating comprises a fluorinated siloxane prepared by applying a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 2
Dependent Claim
116 words
An antireflective article comprising a substrate having an antireflective surface and an antisoiling coating of less than about 100 Angstroms thick deposited thereon; wherein the antisoiling coating comprises a fluorinated siloxane prepared by applying a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 3
Dependent Claim
21 words
The antireflective article of claim 1 wherein the antireflective surface comprises a metal oxide film having one or more metal oxides.
Claim 4
Dependent Claim
17 words
The antireflective article of claim 2 wherein the antireflective surface comprises a sputter coated metal oxide film.
Claim 5
Dependent Claim
17 words
The antireflective article of claim 3 wherein the antisoiling coating is at least about 20 Angstroms thick.
Claim 6
Dependent Claim
44 words
The antireflective article of claim 1 wherein the antisoiling coating comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not significantly reduce the antireflective characteristics of the antireflective article.
Claim 7
Dependent Claim
30 words
The antireflective article of claim 1 which has a first surface antireflectivity that is less than about 0.2 percent different than that of the same article without the antisoiling coating.
Claim 8
Dependent Claim
26 words
The antireflective article of claim 1 wherein the coating is prepared by applying a coating composition comprising a fluorinated silane wherein each X is a halide.
Claim 9
Dependent Claim
44 words
The antireflective article of claim 1 wherein the coating is prepared by applying a coating composition comprising a fluorinated silane wherein R f is a perfluoroalkyl group of the formula C n F 2n .sbsb.+ 1 wherein n is about 4 to about 20.
Claim 10
Dependent Claim
44 words
The antireflective article of claim 8 wherein the coating is prepared by applying a coating composition comprising a fluorinated silane wherein R f is a perfluoroalkyl group of the formula C n F 2n .sbsb.+ 1 wherein n is about 7 to about 10.
Claim 11
Dependent Claim
144 words
The antireflective article of claim 1 wherein the coating is prepared by applying a coating composition comprising a fluorinated silane selected from the group of C 7 F 15 CH 2 OCH 2 CH 2 CH 2 SiCl 3 , C 7 F 15 CH 2 OCH 2 CH 2 CH 2 Si(CH 3 )Cl 2 , C 7 F 15 CH 2 OCH 2 CH 2 CH 2 SiCl(OCH 3 ) 2 , C 7 F 15 CH 2 OCH 2 CH 2 CH 2 SiCl 2 (OC 2 H 5 ), C 8 F 17 SO 2 N(Et)CH 2 CH 2 CH 2 SiCl 3 , C 8 F 17 SO 2 N(Me)CH 2 CH 2 CH 2 Si(CH 3 )Cl 2 , and C 7 F 15 CH 2 OCH 2 CH 2 CH 2 Si(OAc) 3 , and mixtures thereof.
Claim 12
Dependent Claim
144 words
An antireflective article comprising a substrate having an antireflective surface and an antisoiling coating deposited thereon; wherein the antisoiling coating comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not substantially change the antireflective characteristics of the antireflective article; wherein the fluorinated siloxane is prepared by applying a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 13
Dependent Claim
144 words
An antireflective article comprising a substrate having an antireflective surface and an antisoiling coating deposited thereon; wherein the antisoiling coating comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not substantially change the antireflective characteristics of the antireflective article; wherein the fluorinated siloxane is prepared by applying a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 14
Dependent Claim
21 words
The antireflective article of claim 11 wherein the antireflective surface comprises a metal oxide film having one or more metal oxides.
Claim 15
Dependent Claim
17 words
The antireflective article of claim 12 wherein the antireflective surface comprises a sputter coated metal oxide film.
Claim 16
Dependent Claim
30 words
The antireflective article of claim 11 which has a first surface antireflectivity that is less than about 0.2 percent different than that of the same article without the antisoiling coating.
Claim 17
Dependent Claim
62 words
An antireflective article comprising a substrate having an antireflective surface and an antisoiling coating deposited thereon; wherein the antisoiling coating is less than about 100 Angstroms thick and comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not significantly reduce the antireflective characteristics of the antireflective article.
Claim 18
Dependent Claim
62 words
An antireflective article comprising a substrate having an antireflective surface and an antisoiling coating deposited thereon; wherein the antisoiling coating is less than about 100 Angstroms thick and comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not significantly reduce the antireflective characteristics of the antireflective article.
Claim 19
Independent Claim
111 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising treating the antireflective surface with a coating composition comprising a fluorinated silane without subsequent processing; wherein the fluorinated silane has the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 20
Independent Claim
111 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising treating the antireflective surface with a coating composition comprising a fluorinated silane without subsequent processing; wherein the fluorinated silane has the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 21
Dependent Claim
143 words
The method of claim 16 wherein the coating is prepared by applying a coating composition comprising a fluorinated silane selected from the group of C 7 F 15 CH 2 OCH 2 CH 2 CH 2 SiCl 3 , C 7 F 15 CH 2 OCH 2 CH 2 CH 2 Si(CH 3 )Cl 2 , C 7 F 15 CH 2 OCH 2 CH 2 CH 2 SiCl(OCH 3 ) 2 , C 7 F 15 CH 2 OCH 2 CH 2 CH 2 SiCl 2 (OC 2 H 5 ), C 8 F 17 SO 2 N(Et)CH 2 CH 2 CH 2 SiCl 3 , C 8 F 17 SO 2 N(Me)CH 2 CH 2 CH 2 Si(CH 3 )Cl 2 , and C 7 F 15 CH 2 OCH 2 CH 2 CH 2 Si(OAc) 3 , and mixtures thereof.
Claim 22
Dependent Claim
29 words
The method of claim 16 wherein the antisoiling coating formed comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material.
Claim 23
Dependent Claim
17 words
The method of claim 16 wherein the antisoiling coating formed is less than about 100 Angstroms thick.
Claim 24
Dependent Claim
17 words
The method of claim 19 wherein the antisoiling coating formed is at least about 20 Angstroms thick.
Claim 25
Dependent Claim
16 words
The method of claim 16 wherein the step of treating is carried out at room temperature.
Claim 26
Dependent Claim
24 words
The method of claim 16 wherein the coating composition comprising the fluorinated silane comprises less than about 2.0 weight percent of the fluorinated silane.
Claim 27
Dependent Claim
24 words
The method of claim 16 wherein the antireflective substrate is treated with a coating composition comprising a fluorinated silane for less than 30 minutes.
Claim 28
Dependent Claim
25 words
The method of claim 23 wherein the antireflective substrate is treated with a coating composition comprising a fluorinated silane for less than about 10 minutes.
Claim 29
Dependent Claim
37 words
The method of claim 16 wherein the step of treating comprises immersing the substrate in the coating composition comprising the fluorinated silane and removing the coated antireflective substrate, wherein upon removal the coated substrate emerges substantially autophobic.
Claim 30
Dependent Claim
18 words
The method of claim 16 wherein the coating composition comprising the fluorinated silane further comprises a nonchlorinated solvent.
Claim 31
Dependent Claim
26 words
The method of claim 26 wherein the solvent is selected from the group of an alkane, a fluorinated alkane, an alkyl perfluoroalkyl ether, and mixtures thereof.
Claim 32
Dependent Claim
20 words
The method of claim 27 wherein the solvent is a mixture of a paraffinic solvent and an alkyl perfluoroalkyl ether.
Claim 33
Independent Claim
122 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method consisting essentially of treating the antireflective surface with a coating composition comprising less than about 0.5 weight percent of a fluorinated silane for less than 30 minutes; wherein the fluorinated silane has the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 34
Independent Claim
122 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method consisting essentially of treating the antireflective surface with a coating composition comprising less than about 0.5 weight percent of a fluorinated silane for less than 30 minutes; wherein the fluorinated silane has the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1.
Claim 35
Dependent Claim
37 words
The method of claim 29 wherein the step of treating comprises immersing the substrate in the coating composition comprising the fluorinated silane and removing the coated antireflective substrate, wherein upon removal the coated substrate emerges substantially autophobic.
Claim 36
Independent Claim
56 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising immersing the substrate in a coating composition comprising less than about 0.5 weight percent of a fluorinated silane for less than about 20 minutes and removing the coated antireflective substrate, wherein upon removal the coated substrate emerges substantially autophobic.
Claim 37
Independent Claim
56 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising immersing the substrate in a coating composition comprising less than about 0.5 weight percent of a fluorinated silane for less than about 20 minutes and removing the coated antireflective substrate, wherein upon removal the coated substrate emerges substantially autophobic.
Claim 38
Independent Claim
117 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising immersing the substrate in a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1; wherein the antisoiling coating formed has a thickness of less than about 100 Angstroms.
Claim 39
Independent Claim
117 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising immersing the substrate in a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1; wherein the antisoiling coating formed has a thickness of less than about 100 Angstroms.
Claim 40
Dependent Claim
20 words
The method of claim 32 wherein the antireflective surface comprises a metal oxide film having one or more metal oxides.
Claim 41
Dependent Claim
16 words
The method of claim 33 wherein the antireflective surface comprises a sputter coated metal oxide film.
Claim 42
Dependent Claim
10 words
An antireflective article made by the method of claim 32.
Claim 43
Independent Claim
141 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising immersing the substrate in a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1; wherein the antisoiling coating comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not substantially change the antireflective characteristics of the antireflective article.
Claim 44
Independent Claim
141 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprising immersing the substrate in a coating composition comprising a fluorinated silane of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1; wherein the antisoiling coating comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not substantially change the antireflective characteristics of the antireflective article.
Claim 45
Dependent Claim
10 words
An antireflective article made by the method of claim 36.
Claim 46
Independent Claim
173 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprises immersing the substrate in a coating composition comprising less than about 0.5 weight percent of a fluorinated silane for less than about 5 minutes without subsequent processing; wherein the fluorinated silane is of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1; wherein the antisoiling coating formed has a thickness of less than about 100 Angstroms and comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not substantially change the antireflective characteristics of the antireflective article.
Claim 47
Independent Claim
173 words
A method of applying an antisoiling coating to a substrate having an antireflective surface, the method comprises immersing the substrate in a coating composition comprising less than about 0.5 weight percent of a fluorinated silane for less than about 5 minutes without subsequent processing; wherein the fluorinated silane is of the following formula: R.sub.f --R.sup.1 --SiX.sub.3-x R.sup.2.sub.x wherein: R f is a perfluorinated group optionally containing one or more heteroatoms; R 1 is a divalent alkylene group, arylene group, or mixture thereof, substituted with one or more heteroatoms or functional groups, containing about 2 to about 16 carbon atoms; R 2 is a lower alkyl group; X is a halide, a lower alkoxy group, or an acyloxy group; and x is 0 or 1; wherein the antisoiling coating formed has a thickness of less than about 100 Angstroms and comprises a fluorinated siloxane base film of an approximately monolayer thickness on which is adsorbed oligomeric fluorinated siloxane material in an amount that does not substantially change the antireflective characteristics of the antireflective article.
Claim 48
Dependent Claim
10 words
An antireflective article made by the method of claim 38.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 2001-12-21 | 2002-06-22 | 2002-12-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2005-12-21 | 2006-06-22 | 2006-12-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2009-12-21 | 2010-06-22 | 2010-12-22 | $7700.00 | Window Closed / Lapsed |