US4996083A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method for deposition of electrochromic layers
Assignee: Magna Donnelly Corp
•
Filing: 1989-06-12
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Granted: 1991-02-26
•
Expires: 2009-06-12
Abstract
Abstract The specification discloses a method for coating a substrate with electrochromic coatings by dipping a substrate having a conductive surface into, or spraying, or spin coating with, a solution prepared by reacting an anhydrous halide of an electrochromically active transition metal with a C 1 to C 5 anhydrous alcohol, most preferably under a stream of inert gas, at 0 to 80 degrees C. The dipped substrate is removed at a rate necessary to give a desired thickness, and the resulting coating is dried and hydrolyzed and further condensed to create an electrochromically active coating.
Inventors
- 👤 Frank H. Moser
- 👤 Niall R. Lynam
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 18:33
CPC Classifications
C; C03; C03C; C03C17/00; C03C17/34; C03C17/3411; C03C17/3417; C03C17/22; C03C17/23; C03C17/25; C09; C09K; C09K9/00; G; G02; G02F; G02F1/00; G02F1/01; G02F1/15; G02F1/1514; G02F1/1523; G02F1/1524; C03C2217/00; C03C2217/20; C03C2217/21; C03C2217/229; C03C2217/23; C03C2218/00; C03C2218/10; C03C2218/11; C03C2218/111; C03C2218/112; C03C2218/116
Claims Analysis
Total Claims: 50
Claim 1
Independent Claim
82 words
A method for preparing transition metal coating solutions which are suitable for preparing electrochromic layers and the like, comprising: forming a first solution by reacting an anhydrous halide for an electrochromically active transition metal with a C 1 to C 5 carbon anhydrous at 0 to 80 degrees C., and blending in a coating solution, in alcohol, comprising about 5% to about 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate coating solution to said solution being about 10:90 to about 75:25.
Claim 2
Independent Claim
82 words
A method for preparing transition metal coating solutions which are suitable for preparing electrochromic layers and the like, comprising: forming a first solution by reacting an anhydrous halide for an electrochromically active transition metal with a C 1 to C 5 carbon anhydrous at 0 to 80 degrees C., and blending in a coating solution, in alcohol, comprising about 5% to about 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate coating solution to said solution being about 10:90 to about 75:25.
Claim 3
Independent Claim
99 words
The method of claim for preparing transition metal coating solutions which are suitable for preparing electrochromic layers and the like, comprising: forming a first solution by reacting an anhydrous halide for an electrochromically active transition metal with a C 1 to C 5 carbon anhydrous at 0 to 80 degrees C. while simultaneously passing a stream comprising at least one inert gas over said first solution during said reaction; and blending in a coating solution, in alcohol, comprising about 5% to about 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate coating solution being about 10:90 to about 75:25.
Claim 4
Dependent Claim
23 words
The method of claim 2 in which the ratio of transition metal halide to alcohol is from about 5 to 20 weight/volume percent.
Claim 5
Dependent Claim
17 words
The method of claim 3 in which includes filtering said first solution after the reaction has completed.
Claim 6
Dependent Claim
21 words
The method of claim 4 in which a stream of inert gas is passed over said coating solution during said reaction.
Claim 7
Dependent Claim
29 words
The method of claim 4 in which from 5 to 20% of a wetting agent is added to said coating solution to facilitate good cosmetic appearance in thicker coatings.
Claim 8
Dependent Claim
21 words
The method of claim 6 in which from 10 to 15% of said wetting agent is added to said coating solution.
Claim 9
Dependent Claim
18 words
The method of claim 4 in which said first solution reaction is allowed to continue for several hours.
Claim 10
Dependent Claim
32 words
The method of claim 8 in which said transition metals used ar selected from the group consisting of vanadium, chromium, molybdenum, tungsten, iridium, manganese and nickel whereby electrochromic coatings can be obtained.
Claim 11
Dependent Claim
12 words
The method of claim 9 in which said transition metal is tungsten.
Claim 12
Dependent Claim
41 words
The method of claim 10 in which said transition metal is nickel and an alkali metal alkoxy compound is added to the reaction mixture in a ratio of from about 10% to about 100% by weight of said transition metal halide.
Claim 13
Dependent Claim
31 words
The method of claim 11 in which said alkali metal alkoxy includes an alkoxy group which corresponds to at least one of the alcohols being reacted with said transition metal halide.
Claim 14
Dependent Claim
25 words
The method of claim 4 in which includes mixing two or more of said first solutions each being formed from a different transition metal halide.
Claim 15
Dependent Claim
23 words
The method of claim 4 in which includes using a mixture of two or more of said C 1 to C 5 alcohols.
Claim 16
Dependent Claim
32 words
The method of claim 2 in which said transition metals used are selected from the group consisting of vanadium, chromium, molybdenum, tungsten, iridium, manganese and nickel whereby electrochromic coatings can be obtained.
Claim 17
Dependent Claim
12 words
The method of claim 2 in which said transition metal is tungsten.
Claim 18
Dependent Claim
41 words
The method of claim 2 in which said transition metal is nickel and an alkali metal alkoxy compound is added to the reaction mixture in a ratio of from about 10% to about 100% by weight of said transition metal halide.
Claim 19
Dependent Claim
25 words
The method of claim 2 in which includes mixing 2 or more of said first solutions each being formed from a different transition metal halide.
Claim 20
Dependent Claim
23 words
The method of claim 2 in which includes using a mixture of two or more of said C 1 to C 5 alcohols.
Claim 21
Dependent Claim
21 words
The method of claim 1 in which a stream of inert gas is passed over said coating solution during said reaction.
Claim 22
Dependent Claim
29 words
The method of claim 2 in which from 5 to 20% of a wetting agent is added to said coating solution to facilitate good cosmetic appearance in thicker coatings.
Claim 23
Dependent Claim
21 words
The method of claim 21 in which from 10 to 15% of said wetting agent is added to said coating solution.
Claim 24
Independent Claim
84 words
A method for preparing an electrochromic coating on a substrate having an electrically conductive surface comprising: preparing a coating solution by reacting at least one nickel halide compound, at least one C 1 to C 5 anhydrous alcohol and at least one alkali metal alkoxide at 0 to 80 degrees C.; coating the conductive surface of said substrate with the resulting solution to give a coating of a desired thickness; and drying and hydrolyzing and further condensing said coating to an electrochromically active coating.
Claim 25
Independent Claim
84 words
A method for preparing an electrochromic coating on a substrate having an electrically conductive surface comprising: preparing a coating solution by reacting at least one nickel halide compound, at least one C 1 to C 5 anhydrous alcohol and at least one alkali metal alkoxide at 0 to 80 degrees C.; coating the conductive surface of said substrate with the resulting solution to give a coating of a desired thickness; and drying and hydrolyzing and further condensing said coating to an electrochromically active coating.
Claim 26
Dependent Claim
40 words
The method of claim 23 wherein said coating solution is blended with a coating solution, in alcohol, comprising from 5 to 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate solution to said solution being about 10:90 to about 75:25.
Claim 27
Dependent Claim
20 words
The method of claim 23 in which from 5 to 20% of the wetting agent is added to said blend.
Claim 28
Dependent Claim
20 words
The method of claim 24 in which from 5 to 20% of the wetting agent is added to said blend.
Claim 29
Dependent Claim
12 words
The method of claim 23 wherein said nickel halide comprises nickel chloride.
Claim 30
Dependent Claim
13 words
The method of claim 23 wherein said alkali metal alkoxide comprises sodium ethylate.
Claim 31
Dependent Claim
15 words
The method of claim 24 wherein said tetraethyl orthosilicate coating solution comprises partially hydrolyzed tetraethylorthosilicate.
Claim 32
Dependent Claim
40 words
The method of claim 27 wherein said coating solution is blended with a coating solution, in alcohol, comprising from 5 to 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate coating to said solution being about 10:90 to about 75:25.
Claim 33
Dependent Claim
20 words
The method of claim 27 wherein said coating solution contains from 5 to 20% of at least one wetting agent.
Claim 34
Dependent Claim
12 words
The method of claim 30 wherein said silica coating comprises nickel chloride.
Claim 35
Dependent Claim
12 words
The method of claim 28 wherein said nickel halide comprises nickel chloride.
Claim 36
Dependent Claim
41 words
The method of claim 33 wherein said coating solution is blended with a silica coating solution, in alcohol, comprising from 5 to 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate coating to said solution being about 10:90 to about 75:25.
Claim 37
Dependent Claim
20 words
The method of claim 33 wherein said coating solution contains from 5 to 20% of at least one wetting agent.
Claim 38
Independent Claim
143 words
A method for preparing an electrochromic coating on a substrate having an electrically conductive surface comprising: preparing a coating solution by reacting at least one anhydrous halide of an electrochromically active transition metal, at least one C 1 to C 5 anhydrous alcohol and at least one alkali metal alkoxy compound, wherein the ratio of transition metal halide to alcohol is from about 5 to 20 weight/volume percent and the ratio of alkali metal alkoxy compound to transition metal halide is from about 0 to 100 weight/volume weight percent, at 0 to 80 degrees C. while simultaneously passing a stream of inert gas over said coating solution during said reaction; coating the conductive surface of said substrate with the resulting solution to give a coating of a desired thickness; and drying and hydrolyzing and further condensing said coating to an electrochromically active coating.
Claim 39
Independent Claim
143 words
A method for preparing an electrochromic coating on a substrate having an electrically conductive surface comprising: preparing a coating solution by reacting at least one anhydrous halide of an electrochromically active transition metal, at least one C 1 to C 5 anhydrous alcohol and at least one alkali metal alkoxy compound, wherein the ratio of transition metal halide to alcohol is from about 5 to 20 weight/volume percent and the ratio of alkali metal alkoxy compound to transition metal halide is from about 0 to 100 weight/volume weight percent, at 0 to 80 degrees C. while simultaneously passing a stream of inert gas over said coating solution during said reaction; coating the conductive surface of said substrate with the resulting solution to give a coating of a desired thickness; and drying and hydrolyzing and further condensing said coating to an electrochromically active coating.
Claim 40
Dependent Claim
16 words
The method of claim 36 which includes filtering said solution after the reaction has been completed.
Claim 41
Dependent Claim
22 words
The method of claim 37 wherein said coating solution contains from 5 to 20% by weight of at least one wetting agent.
Claim 42
Dependent Claim
19 words
The method of claim 38 wherein the amount of said wetting agent is from 10 to 15% by weight.
Claim 43
Dependent Claim
15 words
The method of claim 37 wherein said reaction is allowed to continue for several hours.
Claim 44
Dependent Claim
32 words
The method of claim 40 in which said transition metals used are selected from the group consisting of vanadium, chromium, molybdenum, tungsten, iridium, manganese and nickel whereby electrochromic coatings can be obtained.
Claim 45
Dependent Claim
12 words
The method of claim 41 in which said transition metal is tungsten.
Claim 46
Dependent Claim
12 words
The method of claim 41 in which said transition metal is nickel.
Claim 47
Dependent Claim
32 words
The method of claim 43 in which said alkali metal alkoxy compound includes an alkoxy group which corresponds to at least one of the alcohols being reacted with said transition metal halide.
Claim 48
Dependent Claim
42 words
The method of claim 43 in which said solution is blended with a coating solution, in alcohol, comprising about 5% to about 10% tetraethyl orthosilicate, the ratio of said tetraethyl orthosilicate coating solution to said solution being about 10:90 to about 75:25.
Claim 49
Dependent Claim
12 words
The method of claim 36 in which said transition metal is nickel.
Claim 50
Dependent Claim
40 words
The method of claim 46 in which said solution is blended with a coating solution, in alcohol, comprising about 5% to about 10% tetraethyl/orthosilicate the ratio of said tetraethyl/orthos coating solution to said solution being about 10:90 to about 75:25.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1994-02-25 | 1994-08-27 | 1995-02-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-02-25 | 1998-08-27 | 1999-02-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-02-25 | 2002-08-27 | 2003-02-26 | $7700.00 | Window Closed / Lapsed |