Electrochromic polymeric solid films, manufacturing electrochromic devices using such solid films, and processes for making such films and devices

• US 6,245,262 B1
• Filed: 02/18/1999
• Issued: 06/12/2001
• Est. Priority Date: 02/26/1993
• Status: Expired due to Fees

• Current Assignee: Donnelly Corporation (Magna International Incorporated)
• Original Assignee: Donnelly Corporation (Magna International Incorporated)
• Inventors: Allemand, Pierre-Marc, Agrawal, Anoop, Dornan, Craig Allen, Varaprasad, Desaraju V., Zhao, Mingtang, Lynam, Niall R.
• Primary Examiner(s): Vargot, Mathieu D.
• Application Number:
  US09/251,937
• Time in Patent Office: 845 Days
• Field of Search: 264/1.31, 264/1.34, 264/1.7, 264/1.9, 264/1.38, 264/571, 264/1.36, 359/267, 359/270, 359/273
• US Class Current: 264/1.31
• CPC Class Codes: B32B 17/06 comprising glass as the main or only constituent of a layer, next to another layer of a specific material
• CPC Class Codes: B32B 17/10036 comprising two outer glass sheets
• CPC Class Codes: B32B 17/10697 being cross-linked
• CPC Class Codes: B60Q 1/2665 on rear-view mirrors lighting devices for vehicle interior on or for rear-view mirrors B60Q3/258
• CPC Class Codes: B60Q 2900/40 Several lamps activated in sequence, e.g. sweep effect, progressive activation
• CPC Class Codes: B60R 1/088 using a cell of electrically changeable optical characteristic, e.g. liquid-crystal or electrochromic mirrors
• CPC Class Codes: B60R 1/1207 with lamps; with turn indicators
• CPC Class Codes: C09K 2211/1007 Non-condensed systems
• CPC Class Codes: C09K 2211/1011 Condensed systems
• CPC Class Codes: C09K 2211/1014 bridged by heteroatoms, e.g. N, P, Si or B
• CPC Class Codes: C09K 2211/1029 containing one nitrogen atom as the heteroatom
• CPC Class Codes: C09K 2211/1033 with oxygen
• CPC Class Codes: C09K 2211/1037 with sulfur
• CPC Class Codes: C09K 9/02 Organic tenebrescent materials
• CPC Class Codes: G02F 1/1503 caused by oxidation-reduction reactions in organic liquid solutions, e.g. viologen solutions
• CPC Class Codes: G02F 1/1516 comprising organic material
• CPC Class Codes: G02F 1/15165 Polymers
• CPC Class Codes: G02F 1/155 Electrodes
• 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
• CPC Class Codes: G02F 2001/1518 : Ferrocene compounds
• CPC Class Codes: G02F 2201/58 : Arrangements comprising a monitoring photodetector
• CPC Class Codes: G02F 2202/022 : polymeric
• CPC Class Codes: Y10T 428/24785 : including layer embodying mechanically interengaged strands, strand portions or strand-like strips [e.g., weave, knit, etc.]
• CPC Class Codes: Y10T 428/26 : Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
• CPC Class Codes: Y10T 428/31551 : Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
• CPC Class Codes: Y10T 428/31649 : Ester, halide or nitrile of addition polymer
• CPC Class Codes: Y10T 428/31678 : Of metal
• CPC Class Codes: Y10T 428/31935 : Ester, halide or nitrile of addition polymer
• CPC Class Codes: Y10T 83/0419 : By distorting within elastic limit

Abstract

The present invention relates to electrochromic polymeric solid films, manufacturing electrochromic devices using such solid films and processes for making such solid films and devices. The electrochromic polymeric solid films of the present invention exhibit beneficial properties and characteristics, especially when compared to known electrochromic media. The electrochromic polymeric solid films are transformed in situ from a low viscosity electrochromic monomer composition by exposure to electromagnetic radiation, and in so doing minimum shrinkage occurs. The electrochromic polymeric solid films of the present invention also perform well under prolonged coloration, outdoor weathering and all-climate exposure, and provide an inherent safety aspect not known to electrochromic media heretofore.

Claims

1. A method of disposing a solid polymer film between two opposing, spaced substrates of an electrochromic device, said method including the steps of:

providing a first substrate of the electrochromic device, said first substrate comprising a first substantially transparent element having a first transparent conductive surface;

providing a second substrate of the electrochromic device, said second substrate comprising a second element having a second conductive surface;

opposing the conductive surface of said first substrate with the conductive surface of said second substrate and spacing said substrates apart with a solid spacer, said spacer and said substrates forming an interpane cavity between said first and second substrates;

providing a low viscosity monomer composition that includes at least one of (A) a monofunctional monomer and a cross-linking agent and (B) a polyfunctional component capable of cross-linking, said monomer composition further including a plasticizer;

causing said low viscosity monomer composition to flow into said interpane cavity; and

with the monomer composition disposed within said interpane cavity, in-situ curing said monomer composition to form a cross-linked solid polymer film.

2. The method of claim 1 wherein said monomer composition includes a component selected from the group consisting of urethane forming material, acrylate forming material, derivatized urethane forming material, acrylate forming material, epoxy forming material, and vinyl forming material.

3. The method of claim 1 wherein said monomer composition includes a component selected from the group consisting of a monofunctional monomer, a difunctional monomer, a trifunctional monomer, a polyfunctional monomer or mixtures thereof.

4. The method of claim 1 wherein said spacing of said substrates apart by said solid spacer is in the range from about 1000 microns to about 10 microns.

5. The method of claim 1 wherein said spacing of said substrates apart by said solid spacer is in the range from about. 325 microns to about 20 microns.

6. The method of claim 1 wherein said solid spacer comprises a boundary seal.

7. The method of claim 6 wherein said boundary seal is made from a polymeric material.

8. The method of claim 1 wherein said plasticizer comprises triglyme, tetraglyme, acetonitrile, benzylacletone, 3-hydroxypropionitrile, methoxypropionitrile, 3-ethoxypropionitrile, butylene carbonate, propylene carbonate, ethylene carbonate, glycerine carbonate, 2-acetylbutyrolactone, cyanoethyl sucrose, γ

-butyrolactone, 2-methylglutaronitrile, N,N′

-dimethylformamide, 3-methylsulfolane, methylethyl ketone, cyclopentanone, cyclohexanone, 4-hydroxy-4-methyl-2-pentanone, acetophenone, glutaronitrile, 3,31-oxydipropionitrile, 2-methoxyethyl ether, triethylene glycol dimethyl ether, or combinations thereof.

9. The method of claim 1 wherein said first transparent conductive surface comprises a transparent conductor selected from the group consisting of indium tin oxide, doped tin oxide and doped zinc oxide.

10. The method of claim 9 wherein said second conductive surface comprises a transparent conductor selected from the group consisting of indium tin oxide, doped tin oxide and doped zinc oxide.

11. The method of claim 10 wherein said electrochromic device is an electrochromic glazing.

12. The method of claim 1 wherein said electrochromic device comprises one of an electrochromic vehicular glazing and an electrochromic architectural glazing.

13. The method of claim 1 wherein said polyfunctional component comprises a polyfunctional hydroxy compound.

14. The method of claim 13 wherein said polyfunctional hydroxy compound comprises a glycol or a glycerol.

15. The method of claim 13 wherein said polyfunctional hydroxy compound comprises a triol.

16. The method of claim 1 wherein said polyfunctional component comprises a polyfunctional amino compound or a polyfunctional mercapto compound.

17. The method of claim 1 wherein said polyfunctional component has a functionality of 2 or greater.

18. The method of claim 1 wherein said monomer composition comprises at least one of an ultraviolet stabilizer, a humectant, a coloring agent, an antioxidizing agent, an electrochromic compound, a lubricating agent, an electrolytic material, a spacer bead, a compatibilizing agent, a polymerization initiator, an adhesion promoting agent and a coupling agent.

19. The method of claim 11 wherein said electrochromic glazing is a large area glazing of an area of at least 99 square inches.

20. The method of claim 1 wherein at least one of said first substrate and said second substrate comprises a specialized glass with reduced ultraviolet radiation transmission.

21. The method of claim 1 wherein at least one of said first substrate and said second substrate comprises a tinted glass.

22. The method of claim 1 wherein said flow of said monomer composition into said interpane cavity is by vacuum backfilling.

23. The method of claim 1 wherein said flow of said monomer composition into said interpane cavity is by dispensing into said cavity.

24. The method of claim 1 wherein said first and second substrates are curved glass substrates.

25. The method of claim 1 wherein the temperature of at least one of said first substrate, said second substrate and said monomer composition is elevated to decrease the viscosity of said monomer composition to enhance flow into said cavity.