Process for preparing multi-layer electrochromic stacks

• US 10,761,394 B2
• Filed: 08/27/2018
• Issued: 09/01/2020
• Est. Priority Date: 07/23/2014
• Status: Active Grant

• Current Assignee: Halio Incorporated
• Original Assignee: Kinestral Technologies, Inc.
• Inventors: Choi, Hye Jin, Bailey, Mark, Bass, John David, von Kugelgen, Stephen Winthrop, Lachman, Eric, Turner, Howard W., Giaquinta, Daniel Mark
• Primary Examiner(s): Gross, Carson
• Application Number:
  US16/113,317
• Publication Number:
  US 20190011795A1
• Time in Patent Office: 736 Days
• CPC Class Codes: B05D 1/005 Spin coating
• CPC Class Codes: B05D 3/0486 Operating the coating or treatment in a controlled atmosphere
• CPC Class Codes: B32B 17/10513 Electrochromic layer
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C03C 17/25 by deposition from the liquid phase
• CPC Class Codes: C03C 2217/21 Oxides
• CPC Class Codes: C23C 18/1254 Sol or sol-gel processing
• CPC Class Codes: G02F 1/1523 comprising inorganic material
• CPC Class Codes: G02F 1/1524 Transition metal compounds
• CPC Class Codes: G02F 1/155 Electrodes
• CPC Class Codes: G02F 2001/1555 Counter electrode

Abstract

Process for forming a multi-layer electrochromic structure, the process comprising depositing a film of a liquid mixture onto a surface of a substrate, and treating the deposited film to form an anodic electrochromic layer, the liquid mixture comprising a continuous phase and a dispersed phase, the dispersed phase comprising metal oxide particles, metal alkoxide particles, metal alkoxide oligomers, gels or particles, or a combination thereof having a number average size of at least 5 nm.

Claims

1. A process for preparing a multi-layer electrochromic structure, comprising:

(a) depositing a film of a first liquid mixture onto a first substrate to form a first deposited film and treating the first deposited film to form a cathodic electrochromic layer comprising a first exposed surface and a first electrochromic state;

(b) depositing a film of a second liquid mixture onto a second substrate to form a second deposited film and treating the second deposited film to form an anodic electrochromic layer comprising an inorganic electrochromic material on the second substrate, wherein the anodic electrochromic layer comprises a second exposed surface and a second electrochemical state, the second electrochemical state being matched to the first electrochemical state; and

(c) forming a laminate of the anodic electrochromic layer, the cathodic electrochromic layer and a polymeric ion conductor layer, the polymeric ion conductor layer being sandwiched between the first exposed surface and the second exposed surface.

2. The process of claim 1, wherein forming the polymeric ion conductor layer comprises crosslinking an ion conductor formulation.

3. The process of claim 1, wherein forming the polymeric ion conductor layer comprises placing a free-standing fully formulated ion-conducting film between the first exposed surface and the second exposed surface.

4. The process of claim 1, wherein the anodic electrochromic layer and the cathodic electrochromic layer are formed by a sol-gel process.

5. The process of claim 1, wherein the treating the second deposited film comprises annealing the second deposited film in a controlled atmosphere at a temperature of at least 200°

C. and at a relative humidity of about 5% RH to about 55% RH.

6. The process of claim 1, wherein the first electrochemical state and the second electrochemical state are matched to be in a bleached state.

7. The process of claim 6, wherein forming the anodic electrochromic layer in the bleached state comprises providing the second liquid mixture comprising a bleached state stabilizing element.

8. The process of claim 7, wherein providing the second liquid mixture comprises providing a bleached state stabilizing element selected from the group consisting of a group 4, a group 5, or a group 6 element.

9. The process of claim 1, wherein the anodic electrochromic layer is adapted to cycle between bleached states having a transmissivity of at least 70% and darkened states having a transmissivity less than 30%.

10. The process of claim 1, wherein the first substrate and the second substrate comprise a transparent conductive layer and a glass layer, and the surface of the substrate onto which the first or the second liquid mixture is deposited is a surface of the transparent conductive layer.

11. The process of claim 1, wherein the multi-layer electrochromic structure is formed using materials selected to provide a transparent multi-layer electrochromic structure when the anodic electrochromic layer and the cathodic electrochromic layer are in a bleached state.

12. A process of preparing a multi-layer electrochromic structure, comprising:

(a) depositing a film of a first liquid mixture onto a first substrate to form a first deposited film and treating the first deposited film to form a cathodic electrochromic layer comprising a first exposed surface and a first electrochromic state;

(b) depositing a film of a second liquid mixture onto a second substrate to form a second deposited film and treating the second deposited film to form an anodic electrochromic layer comprising a lithium nickel oxide and a bleached state stabilizing element on the second substrate, wherein the anodic electrochromic layer comprises a second exposed surface and a second electrochemical state, the second electrochemical state being matched to the first electrochemical state;

(c) forming a laminate of the anodic electrochromic layer, the cathodic electrochromic layer and an ion conductor layer, the ion conductor layer being sandwiched between the first exposed surface and the second exposed surface; and

(d) wherein the anodic electrochromic layer comprises a charge capacity of greater than 10 mC/cm² and cycles between a bleached state transmissivity of at least 70% and a darkened state transmissivity of less than 30%.

13. The process of claim 12, wherein the anodic electrochromic layer has a bleached state voltage of at least 2V.

14. The process of claim 12, wherein the anodic electrochromic layer comprises a charge capacity of greater than 15 mC/cm².

15. The process of claim 12, wherein the cathodic electrochromic layer is an optically passive electrochromic layer.

16. The process of claim 12, wherein depositing the anodic electrochromic layer comprises forming the anodic electrochromic layer to have an average thickness between about 100 nm and about 700 nm.

17. The process of claim 12, wherein the second liquid mixture is formed to provide the anodic electrochromic layer comprising between approximately 0.01 weight percent carbon to approximately 5 weight percent carbon.

18. The process of claim 12, wherein the bleached state stabilizing element is selected from the group consisting of a group 4, a group 5, or a group 6 element.

19. The process of claim 12, wherein the bleached state stabilizing element is selected from the group consisting of Ta, Ti, Zr, Hf, Sb, and V.

20. The process of claim 12, wherein the bleached state stabilizing element comprises Nb.