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CN-121995676-A - Single-component black electrochromic device and preparation method thereof

CN121995676ACN 121995676 ACN121995676 ACN 121995676ACN-121995676-A

Abstract

The invention provides a single-component black electrochromic device and a preparation method thereof, the single-component black electrochromic device sequentially comprises first ITO conductive glass, a single-component black electrochromic layer, an electrolyte layer and second ITO conductive glass from top to bottom, wherein the single-component black electrochromic layer comprises poly (benzodifurandione) and polyether modified polydimethylsiloxane containing aromatic groups, the poly (benzodifurandione) realizes reversible conversion from black to transparent through oxidation-reduction reaction of the poly (benzodifurandione), the material has good purity blackness, an ion storage layer is not needed, the preparation is simple, the production cost can be reduced, meanwhile, the problem of low lamination complementary matching efficiency is avoided through a single-component structure, and the cycle stability of the device can be remarkably improved. In addition, the synergistic effect of the poly (benzodifurandione) and the polyether modified polydimethylsiloxane containing the aromatic groups can further improve the cycling stability of the device and enable the preparation process to be more controllable.

Inventors

  • JIN WEIWEI
  • HUANG FEI

Assignees

  • 华南理工大学

Dates

Publication Date
20260508
Application Date
20260123

Claims (10)

  1. 1. The single-component black electrochromic device is characterized by comprising a first ITO conductive glass, a single-component black electrochromic layer, an electrolyte layer and a second ITO conductive glass from top to bottom in sequence; the single-component black electrochromic layer comprises an electrochromic material and a surfactant, wherein the electrochromic material is poly (benzodifurandione) and has the following structural formula: the surfactant is polyether modified polydimethylsiloxane containing aromatic groups.
  2. 2. The one-component black electrochromic device according to claim 1, wherein the method for preparing the aromatic group-containing polyether-modified polydimethylsiloxane comprises the steps of: S1, blending 4- (diphenylamino) phenol, bromopropene, potassium carbonate and potassium iodide, heating for reaction, and purifying to obtain 4-allyloxy triphenylamine; S2, under the protection of inert gas, blending the 4-allyloxy triphenylamine, the polymethylhydrosiloxane, the allyl polyether and the hexahydrated chloroplatinic acid, heating for reaction, and purifying to obtain the polyether modified polydimethylsiloxane containing the aromatic group.
  3. 3. The one-component black electrochromic device according to claim 2, wherein in step S1, the mass ratio of 4- (diphenylamino) phenol, bromopropene, potassium carbonate, potassium iodide is (20-100): 20-60): 20-100): 1.
  4. 4. The one-component black electrochromic device according to claim 2, wherein in step S2, the heating temperature is 70-90 ℃.
  5. 5. The one-component black electrochromic device according to claim 2, wherein in step S2, the mass ratio of 4-allyloxy triphenylamine, polymethylhydrosiloxane, allyl polyether, chloroplatinic acid hexahydrate is (1-10): 30-70): 10-20): 0.001-0.005.
  6. 6. The one-component black electrochromic device according to claim 1, wherein the electrolyte layer comprises an electrolyte, a polymer monomer, a photoinitiator, a solvent, and a tackifier; Wherein the electrolyte is selected from one or more of lithium perchlorate, lithium bis (trifluoromethyl) sulfonyl imide, tetrabutylammonium hexafluorophosphate, potassium hexafluorophosphate, 1-butyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium bis (trifluoromethyl) sulfonyl imide salt, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-hexyl-3-methylimidazolium tetrafluoroborate and 1-vinyl-3-methylimidazolium acetate; The polymer monomer is selected from one or more of polyethylene glycol diacrylate, methyl methacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate and ethoxylated trimethylolpropane triacrylate.
  7. 7. A method of manufacturing a one-component black electrochromic device according to any one of claims 1 to 6, characterized in that the method of manufacturing a one-component black electrochromic device comprises the steps of: s1, blending a black electrochromic material and a surfactant, coating the mixture on the surface of first ITO conductive glass, and heating and drying to obtain a black electrochromic layer; S2, blending the electrolyte, the polymer monomer, the photoinitiator, the solvent and the tackifier to obtain an electrolyte mixed solution; s3, controlling the interval between the black electrochromic layer and the second ITO conductive glass by using a polyimide adhesive tape, injecting the electrolyte mixed solution between the black electrochromic layer and the second ITO conductive glass, and performing ultraviolet curing to obtain the single-component black electrochromic device.
  8. 8. The method for manufacturing a one-component black electrochromic device according to claim 7, wherein in step S1, the mass ratio of the black electrochromic material to the surfactant is (90-99.9): (0.1-10).
  9. 9. The method of manufacturing a one-component black electrochromic device according to claim 7, wherein in step S1, the thickness of the black electrochromic layer is 50-250 μm.
  10. 10. The method for preparing the single-component black electrochromic device according to claim 7, wherein in the step S2, the mass ratio of the electrolyte, the polymer monomer, the photoinitiator, the solvent and the tackifier is (1-3): (35-42): (1-8): (40-46): (10-15).

Description

Single-component black electrochromic device and preparation method thereof Technical Field The invention relates to the technical field of electrochromic, in particular to a single-component black electrochromic device and a preparation method thereof. Background The electrochromic device is used as an intelligent material with dynamic regulation and control optical performance, and has wide application prospect in the fields of consumer electronics, building energy conservation, national defense science and technology and the like. In the prior art, electrochromic devices generally adopt a multi-layer stacked structure (typically seven layers of structures: supporting layer-ITO conductive layer-electrochromic layer-electrolyte layer-ion storage layer-ITO conductive layer-supporting layer), and optical state transition is realized through the synergistic effect of all functional layers. However, the structure has the problems of complex manufacturing procedures, higher process precision requirements, obvious equipment dependence and the like, so that the production cost is high, and the commercialization process of the structure is severely restricted. The black electrochromic device can realize the reversible switching characteristic of black-transparent, so that the black electrochromic device can effectively meet the diversified requirements of privacy protection, energy conservation, consumption reduction, camouflage stealth and the like, and becomes a research hot spot in the field. However, the prior art has the remarkable limitations that the mode of realizing black presentation by laminating and complementing multicolor materials inevitably leads to complicated device structure, increased manufacturing procedures and increased cost, the problem of poor complementary matching efficiency among different color development materials and easy degradation of cyclical stability, and the problem that single materials capable of independently realizing reversible conversion between black and transparent states are not discovered so far, still a multi-material compounding or doping process is needed, and the miniaturization and scale application potential of the device is greatly limited. Therefore, developing a black electrochromic device with simplified structure, high purity blackness and excellent cycle stability has become a key technical bottleneck to be broken through in the current urgent need. In view of the foregoing, a new solution is needed to solve the problems of the prior art. Disclosure of Invention In view of the above-described drawbacks and deficiencies of the prior art, the present invention provides a single component black electrochromic device and method of making the same. The invention can realize the black-to-transparent reversible conversion of the electrochromic device by using a single material, and has the advantages of simple process, simple structure and high pure blackness, and simultaneously, the invention maintains better cycling stability. An object of the present invention is to provide a single-component black electrochromic device comprising, in order from top to bottom, a first ITO conductive glass, a single-component black electrochromic layer, an electrolyte layer, and a second ITO conductive glass; the single-component black electrochromic layer comprises an electrochromic material and a surfactant, wherein the electrochromic material is poly (benzodifurandione) and has the following structural formula: ; the surfactant is polyether modified polydimethylsiloxane containing aromatic groups. Further, the preparation method of the polyether modified polydimethylsiloxane containing the aromatic group comprises the following steps: S1, blending 4- (diphenylamino) phenol, bromopropene, potassium carbonate and potassium iodide, heating for reaction, and purifying to obtain 4-allyloxy triphenylamine; S2, under the protection of inert gas, blending the 4-allyloxy triphenylamine, the polymethylhydrosiloxane, the allyl polyether and the hexahydrated chloroplatinic acid, heating for reaction, and purifying to obtain the polyether modified polydimethylsiloxane containing the aromatic group. Further, in the step S1, the mass ratio of the 4- (diphenylamino) phenol, the bromopropene, the potassium carbonate and the potassium iodide is (20-100): 20-60): 20-100): 1. Further, in step S2, the temperature is 70-90 DEG C Further, in the step S2, the mass ratio of the 4-allyloxy triphenylamine, the polymethylhydrosiloxane, the allyl polyether and the chloroplatinic acid hexahydrate is (1-10): (30-70): (10-20): (0.001-0.005). Further, the sheet resistances of the first ITO conductive glass and the second ITO conductive glass are 10-80 ohm/sq. Further, the electrolyte layer includes an electrolyte, a polymer monomer, a photoinitiator, a solvent, and a tackifier; Wherein the electrolyte is selected from one or more of lithium perchlorate, lithium bis (trifluoromethyl) sulfonyl imide, tetrabu