Electropolymerization of enhanced electrochromic (EC) polymer film

• US 7,450,290 B2
• Filed: 08/13/2004
• Issued: 11/11/2008
• Est. Priority Date: 06/25/2001
• Status: Active Grant

• Current Assignee: University of Washington, Washington University In St Louis
• Original Assignee: University of Washington
• Inventors: Taya, Minoru, Xu, Chunye, Liu, Lu
• Primary Examiner(s): Stultz; Jessica T
• Application Number:
  US10/917,954
• Publication Number:
  US 20070188845A1
• Time in Patent Office: 1,551 Days
• Field of Search: 359/265
• US Class Current: 359/265
• CPC Class Codes: C08G 61/123 derived from five-membered heterocyclic compounds
• CPC Class Codes: C08G 61/124 with a five-membered ring containing one nitrogen atom in the ring
• CPC Class Codes: C08G 61/126 with a five-membered ring containing one sulfur atom in the ring
• CPC Class Codes: C09K 2211/1029 containing one nitrogen atom as the heteroatom
• CPC Class Codes: C09K 2211/1096 containing other heteroatoms
• CPC Class Codes: C09K 2211/1458 containing sulfur as the only heteroatom
• CPC Class Codes: C09K 2211/1466 containing nitrogen as the only heteroatom
• CPC Class Codes: C09K 2211/1491 containing other combinations of heteroatoms
• CPC Class Codes: C09K 9/02 Organic tenebrescent materials
• CPC Class Codes: G01N 21/553 and using surface plasmons fluorescence excitation G01N21/648; enhanced Raman G01N21/658
• CPC Class Codes: G02F 1/15165 Polymers
• CPC Class Codes: G02F 1/155 Electrodes
• CPC Class Codes: G02F 2001/1555 Counter electrode

Abstract

Electropolymerization of EC monomers is employed to obtain an EC polymer film deposited on a substrate. A first embodiment of a method to produce the film employs cyclic voltammetry alone, while a second embodiment deposits a very thin homogeneous layer using chronoamperometry, and then cyclic voltammetry is employed to increase the density of the film. Another aspect of the present invention is directed to specific web like configurations for a grid of conductive material deposited onto a transparent substrate. The web like configuration is based either on concentric circles, or on concentric ellipses. Yet another aspect of the present invention is directed to an imaging system including a digital window that is disposed between a prism and a patterned analytic layer.

Claims

1. A method for producing a high quality electrochromic polymer film, comprising the steps of:

(a) providing an electrochromic monomer that when polymerized yields an electrochromic polymer; and

(b) using chronoamperometry to polymerize a first quantity of the electrochromic monomer, then using cyclic voltammetry to polymerize an additional quantity of the electrochromic monomer, thereby producing the high quality electrochromic polymer film.

2. The method of claim 1, wherein the step of using cyclic voltammetry to polymerize the electrochromic monomer comprises the step of depositing the polymer as a film on a substrate.

3. The method of claim 2, wherein the step of depositing the polymer as a film on a substrate comprises the step of depositing the film on a transparent electrode.

4. The method of claim 2, wherein the step of depositing the polymer as a film on a substrate comprises the step of depositing the film on a transparent substrate coated with indium tin oxide.

5. The method of claim 1, wherein the step of providing an electrochromic monomer comprises the step of providing [3,6-bis(2-(3,4ethylenedioxythiophene))-N-methylcarbazole].

6. The method of claim 1, wherein the step of providing an electrochromic monomer comprises the step of providing dimethyl propylenedioxythiophene.

7. The method of claim 1, wherein the step of providing an electrochromic monomer comprises the step of providing [3,3-dimethyl-3,4-dihydro-2H-thieno[3,4-b][1,4]dioxepine].

8. The method of claim 1, wherein the step of providing an electrochromic monomer comprises the step of providing the monomer as a solution in which the monomer is present at a concentration of about 0.01M.

9. The method of claim 1, wherein the step of providing an electrochromic monomer comprises the step of dissolving the monomer in a solvent to achieve a monomer solution.

10. The method of claim 9, wherein the step of dissolving the monomer in a solvent to achieve a monomer solution comprises the step of dissolving the monomer in propylene carbonate.

11. The method of claim 10, wherein the step of dissolving the monomer in propylene carbonate comprises the step of using propylene carbonate to which tetrabutyl ammonium perchlorate has been added.

12. The method of claim 10, wherein the step of dissolving the monomer in propylene carbonate comprises the step of using a solution of about 0.1M of tetrabutyl ammonium perchlorate in propylene carbonate.

13. The method of claim 1, wherein the step of using cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using multiple scan cyclic voltammetry.

14. The method of claim 13, wherein the step of using multiple scan cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using a voltage ranging from about +0.8 volts to about −

1.0 volts.

15. The method of claim 13, wherein the step of using multiple scan cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using a scanning rate of about 20 mV/second.

16. The method of claim 13, wherein the step of using multiple scan cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using about 10 cycles.

17. The method of claim 13, wherein the step of using multiple scan cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using:

(a) a voltage ranging from about +0.8 volts to about −

1.0 volts;

(b) a scanning rate of about 20 mV/second; and

(c) about 10 cycles.

18. The method of claim 1, wherein the step of using cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using a platinum wire is a counter electrode.

19. The method of claim 1, wherein the step of using cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using cyclic voltammetry in the absence of moisture.

20. The method of claim 1, wherein the step of using cyclic voltammetry to polymerize the electrochromic monomer comprises the step of using cyclic voltammetry in the absence of water.

21. The method of claim 1, wherein the step of using chronoamperometry to polymerize the first quantity of the monomer comprises the step of using chronoamperometry to deposit a thin film of the polymer on a substrate.

22. The method of claim 21, wherein the step of using cyclic voltammetry to polymerize an additional quantity of the monomer comprises the step of using cyclic voltammetry to deposit additional polymer onto the thin film of the polymer that was deposited using chronoamperometry.

23. The method of claim 1, wherein the step of using chronoamperometry to polymerize the first quantity of the monomer comprises the step of using chronoamperometry for about a hundred seconds at about 0.88 volts.

24. An electrochromic polymer structure comprising a relatively thin base layer generated using chronoamperometry, and a relatively thicker upper layer generated using cyclic voltammetry.

25. The electrochromic polymer of claim 24, wherein the electrochromic polymer in the base layer and the upper layer comprises poly[3,3-dimethyl-3,4-dihydro-2H-thieno[3,4-b][1,4]dioxepine].

26. The electrochromic polymer of claim 24, wherein the electrochromic polymer in the base layer and the upper layer comprises poly[3,6-bis(2-(3,4ethylenedioxythiophene))-N-methylcarbazole].

27. A method for producing a high quality electrochromic polymer film, comprising the steps of:

(a) providing an electrochromic monomer that when polymerized yields an electrochromic polymer, the electrochromic monomer comprising [3,3-dimethyl-3,4-dihydro-2H-thieno[3,4-b][1,4]dioxepine]; and

(b) using cyclic voltammetry to polymerize the electrochromic monomer, thereby producing the high quality electrochromic polymer film.