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CN-117311046-B - Thermosetting type viologen electrochromic solution and electrochromic device

CN117311046BCN 117311046 BCN117311046 BCN 117311046BCN-117311046-B

Abstract

The invention provides a thermosetting type viologen electrochromic solution and an electrochromic device, wherein the thermosetting type viologen electrochromic solution comprises 1.5-4.5 g/mL of di-epoxy functional group molecules, 0.5-0.8 g/mL of anhydride curing agent, 0.1-0.4 g/mL of viologen compound and 0.05-0.3 g/mL of counter electrode material, and the di-epoxy functional group molecules are selected from at least one of bisphenol f diglycidyl ether, bisphenol a diglycidyl ether and bisphenol s diglycidyl ether. The electrochromic device includes a solid electrochromic layer formed by curing the thermoset electrochromic solution. According to the invention, through optimization of the formula, the electrochromic solution can realize heat curing and ensure good electrochromic performance, so that the problems of easy leakage and poor safety of the viologen electrochromic device are solved, and the ultraviolet electrochromic solution can be formed by heat curing, thereby avoiding potential adverse effects of an ultraviolet curing mode on the performance of the device.

Inventors

  • LING HUAN
  • ZENG XIPING
  • YU DONGXU

Assignees

  • 深圳市华科创智技术有限公司

Dates

Publication Date
20260508
Application Date
20230905

Claims (9)

  1. 1. A thermosetting viologen electrochromic solution is characterized by comprising 1.5-4.5 g/mL of di-epoxy functional group molecules, 0.5-0.8 g/mL of anhydride curing agent, 0.1-0.4 g/mL of viologen compound and 0.05-0.3 g/mL of counter electrode material; The diglycidyl functional group molecule is selected from at least one of bisphenol f diglycidyl ether, bisphenol a diglycidyl ether, bisphenol s diglycidyl ether; the anhydride curing agent is at least one selected from pyromellitic dianhydride, phthalic anhydride and hexahydrophthalic anhydride.
  2. 2. The thermoset viologen electrochromic solution of claim 1, comprising 2.5-4 g/mL of di-epoxy functional molecules, 0.55-0.7 g/mL of anhydride curing agent, 0.15-0.35 g/mL of viologen compound, 0.05-0.2 g/mL of counter electrode material.
  3. 3. The thermoset viologen electrochromic solution of claim 1, wherein the viologen compound is selected from at least one of methyl viologen, ethyl viologen, heptyl viologen, phenyl viologen, para-trifluoromethylphenyl viologen.
  4. 4. The thermoset viologen electrochromic solution of claim 1, wherein the counter electrode material is selected from at least one of 10-methylphenothiazine, ferrocene, benzoquinone-based small molecule compounds.
  5. 5. The thermoset viologen electrochromic solution of claim 1, wherein the solvent of the thermoset viologen electrochromic solution is selected from at least one of N, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, methanol, acetonitrile, acetone, chlorobenzene, ethyl acetate, isopropyl acetate.
  6. 6. An electrochromic device, wherein the electrochromic device comprises a solid electrochromic layer formed by curing the thermosetting viologen electrochromic solution of any one of claims 1-5.
  7. 7. The electrochromic device according to claim 6, wherein said solid state electrochromic layer has a thickness of 20 μm to 200 μm.
  8. 8. The electrochromic device of claim 6, wherein said electrochromic device comprises a first FTO electrically conductive glass and a second FTO electrically conductive glass, said solid electrochromic layer disposed between said first FTO electrically conductive glass and said second FTO electrically conductive glass.
  9. 9. The method for manufacturing the electrochromic device according to any one of claims 6 to 8, comprising the steps of (1) thermally curing the thermosetting electrochromic solution at 60-120 ℃ for 20-40 min to obtain the solid electrochromic layer, and (2) placing the solid electrochromic layer between a first FTO conductive glass and a second FTO conductive glass, and sealing to obtain the electrochromic device.

Description

Thermosetting type viologen electrochromic solution and electrochromic device Technical Field The invention belongs to the technical field of electrochromic, and particularly relates to a thermosetting viologen electrochromic solution and an electrochromic device. Background Electrochromic refers to a phenomenon that optical properties (reflectivity, transmittance, absorptivity, etc.) of a material undergo a stable and reversible color change under the action of an applied electric field, and is represented by a reversible change in color and transparency in appearance. Materials having electrochromic properties are referred to as electrochromic materials, and devices made from electrochromic materials are referred to as electrochromic devices. The purple refined compound is one of electrochromic materials widely used at present due to the advantages of easily available raw materials, rich color change types and the like. However, electrochromic devices based on viologen are generally based on liquid and gel states, resulting in the disadvantages of easy leakage and solvent evaporation. The existing electrochromic device based on the viologen is of a sandwich structure of an electrochromic layer, a counter electrode material layer and an electrolyte layer, and cannot be integrated. In addition, it is typically cured by ultraviolet radiation, which can have a potentially detrimental effect on the performance of the device. Disclosure of Invention Based on this, the present invention aims to provide a thermosetting type viologen electrochromic solution, which can prepare and obtain an integrated thermosetting type electrochromic device by adopting a thermosetting mode. In order to achieve the above purpose, the present invention adopts the following technical scheme. A thermosetting viologen electrochromic solution comprises the following components with the concentration of 1.5-4.5 g/mL of di-epoxy functional group molecules, 0.5-0.8 g/mL of anhydride curing agent, 0.1-0.4 g/mL of viologen compound and 0.05-0.3 g/mL of counter electrode material; The diglycidyl functional group molecule is selected from at least one of bisphenol f diglycidyl ether, bisphenol a diglycidyl ether, bisphenol s diglycidyl ether. In some embodiments, the thermoset viologen electrochromic solution is characterized by comprising the following components in concentration of 2.5-4 g/mL of a di-epoxy functional group molecule, 0.55-0.7 g/mL of an anhydride curing agent, 0.15-0.35 g/mL of a viologen compound, and 0.05-0.2 g/mL of a counter electrode material. In some embodiments, the anhydride curing agent is selected from at least one of pyromellitic dianhydride, phthalic anhydride, hexahydrophthalic anhydride. In some embodiments, the viologen compound is selected from at least one of methyl viologen, ethyl viologen, heptyl viologen, phenyl viologen, para-trifluoromethyl phenyl viologen. In some embodiments, the counter electrode material is selected from at least one of 10-methylphenothiazine, ferrocene, benzoquinone-based small molecule compounds. In some embodiments, the solvent of the thermoset viologen electrochromic solution is selected from at least one of N, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, methanol, acetonitrile, acetone, chlorobenzene, ethyl acetate, isopropyl acetate. The invention also provides an electrochromic device which comprises a solid electrochromic layer formed by curing the thermosetting electrochromic solution. In some embodiments, the solid state electrochromic layer has a thickness of 20 μm to 200 μm. In some embodiments, the electrochromic device includes a first FTO conductive glass and a second FTO conductive glass with the solid electrochromic layer disposed therebetween. The invention also provides a preparation method of the electrochromic device, which comprises the following steps of (1) thermally curing the thermosetting electrochromic solution at 60-120 ℃ for 20-40 min to obtain the solid electrochromic layer, and (2) placing the solid electrochromic layer between the first FTO conductive glass and the second FTO conductive glass, and sealing to obtain the electrochromic device. The invention provides a thermosetting electrochromic solution, which can realize thermosetting and ensure good electrochromic performance through the optimization of a formula. The epoxy functional group molecules in the formula can enable the polymer to have proper network crosslinking degree, so that electrochromic molecules can be diffused, the surface adhesion is enhanced due to the existence of polyhydroxy, the problem that interlayer shrinkage and tension of an electrochromic layer and a base material are not matched is solved, and a proper curing agent and a solvent are compounded to enable all raw materials to form a homogeneous system, so that a purple refined compound and counter electrode material molecules can be transferred and diffused between a polymer network and the surface of an