Method for deposition of electrochromic layers

• US 4,855,161 A
• Filed: 02/19/1987
• Issued: 08/08/1989
• Est. Priority Date: 02/19/1987
• Status: Expired due to Fees

• Current Assignee: Donnelly Corporation (Magna International Incorporated)
• Original Assignee: Donnelly Corporation (Magna International Incorporated)
• Inventors: Lynam, Niall R., Moser, Frank H.
• Primary Examiner(s): Silverberg, Sam
• Application Number:
  US07/016,663
• Time in Patent Office: 901 Days
• Field of Search: 427/108, 427/110, 350/357
• US Class Current: 427/108
• CPC Class Codes: C03C 17/25 by deposition from the liquid phase
• CPC Class Codes: C03C 17/3417 all coatings being oxide coatings
• CPC Class Codes: C03C 2217/229 Non-specific enumeration
• CPC Class Codes: C03C 2217/23 Mixtures
• CPC Class Codes: C03C 2218/111 by dipping, immersion
• CPC Class Codes: C03C 2218/112 by spraying
• CPC Class Codes: C03C 2218/116 by spin-coating, centrifugation
• CPC Class Codes: C09K 9/00 Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
• CPC Class Codes: G02F 1/1524 Transition metal compounds
• CPC Class Codes: Y10S 359/90 Methods

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 C₁ to C₅ 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.

Claims

1. A method for preparing an electrochromic coating on a substrate having an electrically conductive surface, comprising:

preparing a coating solution by reacting an anhydrous halide of an electrochromically active transition metal with a C₁ to C₅ anhydrous alcohol, wherein the ratio of transition metal halid to alcohol is from about 5 to 20 weight/volume percent, at 0 to 80 degrees C. while simultaneously passing a stream of 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.

2. The method of claim 1 which includes filtering said solution after the reaction has completed.

3. The method of claim 1 in which said gas is an inert gas.

4. 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.

5. The method of claim 4 in which from 10 to 15% of said wetting agent is added to said coating solution.

6. The method of claim 2 in which said reaction is allowed to continue for several hours.

7. The method of claim 6 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.

8. The method of claim 7 in which said transition metal is tungsten.

9. The method of claim 2 which includes mixing two or more of said solutions, each being formed from a different transition metal halide.

11. The method of claim 1 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.

12. The method of claim 1 in which said transition metal is tungsten.

13. The method of claim 1 which includes mixing two or more of said solutions each being formed from a different transition metal halide.

14. The method of claim 1 which includes using a mixture of two or more of said C₁ to C₅ alcohols .

15. The method of claim 1 in which said gas is an inert gas.

16. The method of claim 1 in which from 5 to 20% of a wetting agent is added to said coating solution to facilitate good cosmetic appearance in thicker coatings.

17. The method of claim 16 in which from 10 to 15% of said wetting agent is added to said coating solution.

18. The method of claim 1, in which said substrate is coated with a conductive coating having a specific resistivity of less than about 4×

10^-4 ohm centimeters and a sheet resistance less than about 10 ohms per square prior to applying said electrochromic coating.

19. The method of claim 18 which said conductive coating is an indium tin oxide coating.

21. The method of any of the preceding claims 1,2,3-8, 9-12, 13, 14, 15-19 and 20 in which said halide is a chloride.

22. The method of any of claims 1, 2, 3-8, 9-12, 13, 14 and 15-19 in which said coating is applied by dipping said glass substrate into said solution and removing it at a rate necessary to give said desired coating thickness.

10. The method of claim 10 which includes using a mixture of two or more of said C₁ to C₅ alcohols.

20. 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 of an electrochromically active transition metal with a C₁ to C₅ anhydrous alcohol, wherein the ratio of transition metal halide to alcohol is from about 5 to 20 weight/volume percent, at 0 to 80 degrees C. while simultaneously passing a stream of gas over said first solution during said reaction;

forming a second solution by reacting anhydrous halide of a different electrochemically active transition metal with a C₁ to C₅ anhydrous alcohol, wherein the ratio of said different electrochemically active transition metal halide to alcohol is from about 5 to 20 weight/volume percent, at 0 to 80 degrees C. while simultaneously passing a stream of gas over said second solution during said reaction; and

blending said two solutions together to form a transition metal dip coating solution.