Electrochromic coating and method for making same

• US 4,959,247 A
• Filed: 12/14/1987
• Issued: 09/25/1990
• Est. Priority Date: 12/14/1987
• Status: Expired due to Fees

• Current Assignee: Donnelly Corporation 414 East Fortieth Street Holland
• Original Assignee: Donnelly Corporation (Magna International Incorporated)
• Inventors: Lynam, Niall R., Moser, Frank H.
• Primary Examiner(s): BELL, JANYCE A
• Application Number:
  US07/132,196
• Time in Patent Office: 1,016 Days
• Field of Search: 427/126.6, 427/126.5, 427/226, 427/230, 427/108, 427/165, 427/169, 427/110, 427/168
• US Class Current: 427/126.5
• CPC Class Codes: C03C 17/25 by deposition from the liquid phase
• CPC Class Codes: C03C 17/27 by oxidation of a coating previously applied
• CPC Class Codes: C03C 17/3417 all coatings being oxide coatings
• CPC Class Codes: C03C 2217/217 FeOx, CoOx, NiOx
• CPC Class Codes: C03C 2218/11 from solutions or suspensions
• CPC Class Codes: C03C 2218/322 Oxidation
• CPC Class Codes: C04B 35/00 Shaped ceramic products characterised by their composition porous ceramic products C04B38/00; ceramic articles characterised by particular shape, see the relevant classes, e.g. linings for casting ladles, tundishes, cups or the like B22D41/02; ceramic substrates for microelectronic semi-conductors H01L23/15; Ceramics compositions containing free metal bonded to carbides, diamond, oxides, borides, nitrides, silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides or sulfides other than as macroscopic reinforcing agents C22C; shaping of ceramics B28B; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products chemical preparation of powders of inorganic compounds C01; infiltration of sintered ceramic preforms with molten metal C04B41/51
• CPC Class Codes: C04B 41/0072 Heat treatment
• CPC Class Codes: C04B 41/009 characterised by the material treated
• CPC Class Codes: C04B 41/4535 applied as a solution, emulsion, dispersion or suspension
• CPC Class Codes: C04B 41/455 the coating or impregnating process including a chemical conversion or reaction
• CPC Class Codes: C04B 41/46 with organic materials
• CPC Class Codes: C04B 41/5072 with oxides or hydroxides not covered by C04B41/5025 C04B40/0236 takes precedence; boron oxide C04B41/5006
• CPC Class Codes: C04B 41/5089 Silica sols, alkyl, ammonium or alkali metal silicate cements
• CPC Class Codes: C04B 41/85 with inorganic materials
• CPC Class Codes: G02F 1/1524 Transition metal compounds

Abstract

Transition metal nitrates such as nickel nitrate are dissolved in monoalcohols having from 1 to 5 carbon atoms. The coatings are applied to a substrate material and fired to convert the coating to an electrochromically active state.

Claims

1. A method for preparing an electrochromic coating on a substrate, consisting essentially of:

forming a coating solution by contacting at least one transition metal nitrate compound with at least one monohydric alcohol having from 1 to 5 carbon atoms;

coating the surface of said substrate with said coating solution to provide a coating thereon of a desired thickness; and

firing said coating to an electrochromically active state.

2. A method in accordance with claim 1 wherein said coating solution comprises from 5 to 20 weight/volume percent of transition metal nitrate.

3. A method in accordance with claim 2 wherein said transition metal nitrate comprises nickel nitrate.

4. A method in accordance with claim 2 wherein said transition metal nitrate comprises an admixture of nickel nitrate and cobalt nitrate.

6. A method in accordance with claim 2 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

8. A method in accordance with claim 2 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent tetraethylorthosilicate.

10. A method in accordance with claim 1 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

12. A method in accordance with claim 2 wherein said firing is effected at a temperature in the range from 100°

to 400°

C.

13. A method in accordance with claim 12 wherein said transition metal nitrate comprises nickel nitrate.

14. A method in accordance with claim 12 wherein said transition metal nitrate comprises an admixture of nickel nitrate and cobalt nitrate.

15. A method in accordance with claim 12 wherein said coating solution contains from 5 to 60 weight/volume percent of ethyl acetate.

16. A method in accordance with claim 12 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

18. A method in accordance with claim 12 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent tetraethylorthosilicate.

20. A method in accordance with claim 18 wherein said coating composition contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

22. A method in accordance with claim 1 wherein said substrate has at least one electrically conductive surface.

23. A method in accordance with claim 22 wherein said coating solution comprises from 5 to 20 weight/volume percent transition metal nitrate.

24. A method in accordance with claim 23 wherein said transition metal nitrate comprises nickel nitrate.

25. A method in accordance with claim 23 wherein said transition metal nitrate comprises an admixture of nickel nitrate and cobalt nitrate.

27. A method in accordance with claim 23 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

29. A method in accordance with claim 23 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.

31. A method in accordance with claim 29 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

33. A method in accordance with claim 23 wherein said firing is effected at a temperature in the range from 100°

to 400°

C.

34. A method in accordance with claim 33 wherein said transition metal nitrate comprises nickel nitrate.

35. A method in accordance with claim 33 wherein said transition metal nitrate comprises an admixture of nickel nitrate and cobalt nitrate.

37. A method in accordance with claim 33 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

39. A method in accordance with claim 33 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.

41. A method in accordance with claim 39 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

5. A method for preparing an electrochromic coating on a substrate, comprising:

forming a coating solution comprising at least one monohydric alcohol having from 1 to 5 carbon atoms, from 5 to 20 weight/volume percent of at least one transition metal nitrate and from 5 to 60 weight/volume percent of ethyl acetate;

coating the surface of said substrate with said coating solution to provide a coating thereon of a desired thickness; and

firing said coating to an electrochromically active state.

7. A method in accordance with claim 5 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

9. A method in accordance with claim 5 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent tetraethylorthosilicate.

11. A method in accordance with claim 5 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one ;

nonionic wetting agent and from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.

17. A method in accordance with claim 5 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent and said firing is effected at a temperature in the range from 100°

to 400°

C.

19. A method in accordance with claim 5 wherein said coating solution contains 0.25 to 7.5 weight/volume percent tetraethylorthosilicate and said firing is effected at a temperature in the range from 100°

to 400°

C.

21. A method in accordance with claim 5 wherein said coating composition contains from 0.1 to 20 weight/volume percent of at least one wetting agent and from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate and said firing is effected at a temperature in the range from 100°

to 400°

C.

26. A method in accordance with claim 5 wherein said substrate has at least one electrically conductive surface.

28. A method in accordance with claim 26 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

30. A method in accordance with claim 26 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.

32. A method in accordance with claim 26 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent and from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.

36. A method in accordance with claim 26 wherein said firing is effected at a temperature in the range from 100°

to 400°

C.

38. A method in accordance with claim 36 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent.

40. A method in accordance with claim 36 wherein said coating solution contains from 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.

42. A method in accordance with claim 36 wherein said coating solution contains from 0.1 to 20 weight/volume percent of at least one nonionic wetting agent and 0.25 to 7.5 weight/volume percent of tetraethylorthosilicate.