Electrochemichromic solutions, process for preparing and using the same, and devices manufactured with the same

• US 6,143,209 A
• Filed: 06/04/1999
• Issued: 11/07/2000
• Est. Priority Date: 09/06/1991
• Status: Expired due to Fees

• Current Assignee: Donnelly Corporation (Magna International Incorporated)
• Original Assignee: Donnelly Corporation (Magna International Incorporated)
• Inventors: Lynam, Niall R.
• Primary Examiner(s): TUCKER, PHILIP C
• Application Number:
  US09/325,712
• Time in Patent Office: 522 Days
• Field of Search: 252/583, 359/265, 359/267, 359/270, 359/272, 359/275
• US Class Current: 252/583
• CPC Class Codes: C09K 9/02 Organic tenebrescent materials
• CPC Class Codes: E06B 2009/2464 featuring transparency control by applying voltage, e.g. LCD, electrochromic panels
• CPC Class Codes: E06B 9/24 Screens or other constructions affording protection against light, especially against sunshine; Similar screens for privacy or appearance; Slat blindsoperating, guiding or securing devices or arrangements for roll-type closures E06B9/56; free-hanging flexible screens A47H23/00
• CPC Class Codes: G02F 1/1503 caused by oxidation-reduction reactions in organic liquid solutions, e.g. viologen solutions
• CPC Class Codes: G02F 2001/1502 complementary cell
• CPC Class Codes: G02F 2001/15145 the electrochromic layer comprises a mixture of anodic and cathodic compounds

Abstract

The present invention relates to electrochromic solutions and devices manufactured therefrom. More precisely, the invention relates to electrochemichromic solutions, and those devices manufactured with the same, that demonstrate superior responsiveness to those solutions known heretofore when an applied potential is introduced thereto. That is, the responsiveness observed in terms of solution coloring is of a greater rapidity, intensity and uniformity than those electrochemichromic solutions of the prior art. Preparation of these solutions involve the novel process of pre-treating at least one of the electrochemichromic compounds with a redox agent prior to placing it in contact with the other electrochemichromic compound. Moreover, the present invention relates to methods of preparing such novel solutions and processes for using these solutions to provide devices that exhibit and benefit from the aforementioned superior characteristics.

Claims

1. An electrochromic window device, said device comprising:

(a) a first substantially transparent substrate coated with a substantially transparent conductive coating having a sheet resistance from about 1 to about 100 ohms per square;

(b) a second substantially transparent substrate coated with a substantially transparent conductive coating having a sheet resistance from about 1 to about 100 ohms per square, said substantially transparent conductive coating of said second substrate positioned in an opposing and spaced apart relationship with said substantially transparent conductive coating of said first substrate;

(c) a seal positioned toward the peripheral edge of each of said first substrate and said second substrate and sealingly forming a cell cavity therebetween, said seal formed of one of a thermoplastic material and a thermosetting material;

(d) an electrochromic medium capable of color change when an applied potential is introduced thereto disposed within said cell cavity, said electrochromic medium comprising;

(i) at least one anodic compound;

(ii) at least one cathodic compound; and

(iii) a solvent; and

(e) a means for introducing an applied potential to said electrochromic medium to controllably cause a variation in the amount of light transmitted through said device, wherein at least one of said first substrate and said second substrate comprises a float glass panel that is coated with a multilayered structure that increases the amount of reflected color inhibited and light transmitted therethrough, said multilayer structure comprising a layer of fluorine-doped tin oxide, and wherein said layer of fluorine-doped tin oxide is undercoated with an anti-iridescence means; and

wherein said electrochromic window device comprises one of an architectural glazing, an aeronautical glazing, a vehicular glazing, a privacy partition, a security partition and an optically attenuating contrast filter.

2. The device according to claim 1, wherein said anti-iridescence means comprises additional thin film layers which undercoat said layer of fluorine-doped tin oxide.

3. The device according to claim 1, wherein said anti-iridescence means comprises (i) a layer of silica-silicone and (ii) a layer of tin oxide, wherein said silica-silicone layer is disposed between said layer of fluorine-doped tin oxide and said layer of tin oxide.

4. The device according to claim 1, wherein said conductive coating of each of said first substrate and said second substrate is composed of a layer of fluorine-doped tin oxide.

5. The device according to claim 4, wherein each of said layers of fluorine-doped tin oxide is undercoated with an anti-iridescence means.

6. The device according to claim 5, wherein said anti-iridescence means comprises additional thin film layers which undercoat said layer of fluorine-doped tin oxide.

7. The device according to claim 5, wherein said anti-iridescence means comprises (i) a layer of silica-silicone and (ii) a layer of tin oxide, wherein said silica-silicone layer is disposed between said layer of fluorine-doped tin oxide and said layer of tin oxide.

8. The device according to claim 1, wherein said vehicular glazing is selected from the group consisting of sun roofs, sun visors and sun bands.

9. The device according to claim 1, wherein the sheet resistance of at least one of said first substrate or said second substrate is from about 6 ohms per square to about 15 ohms per square.

10. The device according to claim 1, wherein each of said first substrate and said second substrate is coated with a multilayered structure manufactured through on-line chemical vapor deposition.

11. The device according to claim 1, wherein each of said first substrate and said second substrate is constructed from float glass.

12. The device according to claim 11, wherein each of said float glass substrates is coated with a multilayered structure that increases the amount of reflected color inhibited and light transmitted therethrough, said multilayer structure comprising a layer of fluorine-doped tin oxide, and wherein said layer of fluorine-doped tin oxide is undercoated with an anti-iridescence means.

13. The device according to claim 12, wherein said anti-iridescence means comprises additional thin film layers which undercoat said layer of fluorine-doped tin oxide.

14. The device according to claim 12, wherein said anti-iridescence means comprises (i) a layer of silica-silicone and (ii) a layer of tin oxide, wherein said silica-silicone layer is disposed between said layer of fluorine-doped tin oxide and said layer of tin oxide.

15. The device according to claim 1, wherein said float glass panel coated with said multilayered structure has a daylight transmittance of about 77% to about 87%.

16. The device according to claim 1, wherein said float glass panel coated with said multilayered structure has a solar transmittance from about 64% to about 80%.

17. The device according to claim 1, wherein said float glass panel coated with said multilayered structure has an infrared reflectance from about 30% to about 87% at a wavelength of about 10 μ

m.

18. The device according to claim 11, wherein said thermoplastic material comprises a member selected from the group consisting of plasticized polyvinyl butyral, polyvinyl chloride, paraffin waxes, ionomer resins and combinations thereof.

19. The device according to claim 1, wherein said thermosetting material comprises a member selected from the group consisting of an epoxy resin and silicones.

20. The device according to claim 1, wherein the cell cavity has an interpane space between said first substrate and said second substrate of about 10 μ

m to about 1000 μ

m.

21. The device according to claim 20, wherein the cell cavity has an interpane space between said first substrate and said second substrate of about 50 μ

m to about 100 μ

m.

22. The device according to claim 1, wherein the anodic compound and the cathodic compound are present in said electrochromic medium in solution and in a ratio from about 5:

1 to about 1;

5.

23. The device according to claim 22, wherein the anodic compound and the cathodic compound are present in said electrochromic medium in a ratio of about 1:

1.

24. The device according to claim 22, wherein said solvent is a member selected from the group consisting of acetonitrile, 3-hydroxypropionitrile, methoxypropionitrile, 3-ethoxypropionitrile, 2-acetylbutyrolactone, propylene carbonate, cyanoethyl sucrose, γ

-butyrolactone, 2-methylglutaronitrile, N,N'"'"'-dimethylformamide, 3-methylsulfolane, glutaronitrile, 3,3'"'"'-oxydipropionitrile, methylethyl ketone, cyclopentanone, cyclohexanone, benzoyl acetone, 4-hydroxy-4-methyl-2-pentanone, acetophenone, 2-methoxyethyl ether, triethylene glycol dimethyl ether and combinations thereof.

25. The device according to claim 23, wherein said solvent is a member selected from the group consisting of acetonitrile, 3-hydroxypropionitrile, methoxypropionitrile, 3-ethoxypropionitrile, 2-acetylbutyrolactone, propylene carbonate, cyanoethyl sucrose, γ

-butyrolactone, 2-methylglutaronitrile, N,N'"'"'-dimethylformamide, 3-methylsulfolane, glutaronitrile, 3,3'"'"'-oxydipropionitrile, methylethyl ketone, cyclopentanone, cyclohexanone, benzoyl acetone, 4-hydroxy-4-methyl-2-pentanone, acetophenone, 2-methoxyethyl ether, triethylene glycol dimethyl ether and combinations thereof.

26. The device according to claim 1, wherein said electrochromic medium further comprises an ultraviolet stabilizing agent.

27. The device according to claim 26, wherein the ultraviolet stabilizing agent of said electrochromic medium is present in a concentration of at least about 5% (w/v).

28. The device according to claim 27, wherein the ultraviolet stabilizing agent is selected from the group consisting of a benzotriazole, a benzotriazole derivative, a benzophenone, a benzophenone derivative and a combination thereof.

29. The device according to claim 28, wherein said benzotriazole or benzotriazole derivative is selected from the group consisting of 2-(2'"'"'-hydroxy-5'"'"'-methylphenyl)-benzotriazole, 2-(3'"'"',5'"'"'-di-t-butyl-2'"'"'-hydroxyphenyl)-5-chlorobenzotriazole, 2-(3'"'"',5'"'"'-di-n-pentyl-2'"'"'-hydroxyphenyl)-benzotriazole, and 2,2'"'"'-dihydroxy-4-methoxybenzophenone.

30. The device according to claim 28, wherein said benzophenone or benzophenone derivative is selected from the group consisting of 2,4-dihydroxybenzophenone, 2,2'"'"'-dihydroxy-4,4'"'"'-dimethoxybenzophenone, and 2,2'"'"'-dihydroxy-4-methoxybenzophenone.

31. The device according to claim 1, wherein the applied potential introduced to said electrochromic medium is from about 0.001 volts to about 5 volts.

32. The device according to claim 31, wherein the applied potential introduced to said electrochromic medium is from about 0.2 volts to about 2 volts.

33. The device according to claim 1, wherein the first and second substantially transparent substrates each have a surface area of greater than 3000 square centimeters.

34. The device according to claim 1, wherein the device changes color uniformly and without substantial iris-effect.

35. The device according to claim 1, wherein the device has a range of visible light transmission variable from greater than about 70% to less than about 10%.

36. The device according to claim 1, wherein said at least one cathodic compound comprises a viologen.

37. An electrochromic window device, said device comprising:

(a) a first substantially transparent substrate coated with a substantially transparent conductive coating having a sheet resistance from about 1 to about 100 ohms per square;

(b) a second substantially transparent substrate coated with a substantially transparent conductive coating having a sheet resistance from about 1 to about 100 ohms per square, said substantially transparent conductive coating of said second substrate positioned in an opposing and spaced apart relationship with said substantially transparent conductive coating of said first substrate;

(c) a seal positioned toward the peripheral edge of each of said first substrate and said second substrate and sealingly forming a cell cavity therebetween;

(d) an electrochromic medium capable of color change when an applied potential is introduced thereto disposed within said cell cavity;

(e) a means for introducing an applied potential to said electrochromic medium to controllably cause a variation in the amount of light transmitted through said device, wherein at least one of said first substrate and said second substrate comprises a float glass panel that is coated with a multilayered structure that increases the amount of reflected color inhibited and light transmitted therethrough, said multilayer structure comprising a layer of fluorine-doped tin oxide, and wherein said layer of fluorine-doped tin oxide is undercoated with an anti-iridescence means; and

wherein at least one of said first substrate and said second substrate comprises at least one of tempered glass and laminated glass.

38. The device according to claim 37, wherein said anti-iridescence means comprises additional thin film layers which undercoat said layer of fluorine-doped tin oxide.

39. The device according to claim 37, wherein said anti-iridescence means comprises (i) a layer of silica-silicone and (ii) a layer of tin oxide, wherein said silica-silicone layer is disposed between said layer of fluorine-doped tin oxide and said layer of tin oxide.

40. The device according to claim 37, wherein the sheet resistance of at least one of said first substrate or said second substrate is from about 6 ohms per square to about 15 ohms per square.

41. The device according to claim 37, wherein each of said first substrate and said second substrate is coated with a multilayered structure manufactured through on-line chemical vapor deposition.

42. The device according to claim 37, wherein said float glass panel coated with said multilayered structure has a daylight transmittance of about 77% to about 87%.

43. The device according to claim 39, wherein said float glass panel coated with said multilayered structure has a solar transmittance from about 64% to about 80%.

44. The device according to claim 37, wherein the cell cavity has an interpane space between said first substrate and said second substrate of about 10 μ

m to about 1000 μ

m.

45. The device according to claim 44, wherein the cell cavity has an interpane space between said first substrate and said second substrate of about 50 μ

m to about 100 μ

m.

46. The device according to claim 37, wherein the first and second substantially transparent substrates each have a surface area of greater than 3000 square centimeters.

47. The device according to claim 37, wherein said electrochromic window device comprises a vehicular glazing selected from the group consisting of sun roofs, sun visors and sun bands.

48. The device according to claim 37, wherein said electrochromic medium comprises:

(i) at least one anodic compound;

(ii) at least one cathodic compound; and

(iii) a solvent.

49. The device according to claim 37, wherein said float glass panel coated with said multilayered structure has an infrared reflectance from about 30% to about 87% at a wavelength of about 10 μ

m.

50. The device according to claim 37, wherein said electrochromic window device comprises one of an architectural glazing, an aeronautical glazing, a vehicular glazing, a privacy partition, a security partition and an optically attenuating contrast filter.

51. The device according to claim 37, wherein the device has a range of visible light transmission variable from greater than about 70% to less than about 10%.

52. The device according to claim 48, wherein said at least one cathodic compound comprises a viologen.

53. The device according to claim 48, wherein the anodic compound and the cathodic compound are present in said electrochromic medium in solution and in a ratio from about 5:

1 to about 1;

5.

54. The device according to claim 37, wherein said electrochromic window device comprises a molded casing placed about its periphery.

55. The device according to claim 37, wherein said electrochromic medium further comprises an ultraviolet stabilizing agent.

56. The device according to claim 55, wherein the ultraviolet stabilizing agent of said electrochromic medium is present in a concentration of at least about 5% (w/v).

57. The device according to claim 55, wherein the ultraviolet stabilizing agent is selected from the group consisting of a benzotriazole, a benzotriazole derivative, a benzophenone, a benzophenone derivative and a combination thereof.