阅读说明：本技术 一种透明基底单层水平电致变色器件的制备方法 (Preparation method of transparent substrate single-layer horizontal electrochromic device ) 是由 简凌锋 闵永刚 刘屹东 于 2020-05-27 设计创作，主要内容包括：本发明提供一种透明基底单层水平电致变色器件的制备方法,主要包括两片单独分离的电致变色器件基底的合成、器件组成,上层极性连接材料以及电致变色材料合成方法等。(The invention provides a preparation method of a transparent substrate single-layer horizontal electrochromic device, which mainly comprises synthesis of two independently separated electrochromic device substrates, device composition, an upper-layer polar connecting material, an electrochromic material synthesis method and the like.)

1. A preparation method of a transparent substrate single-layer horizontal electrochromic device comprises the following steps: the method comprises the following steps of taking a water-blocking and oxygen-blocking conductive material/transparent substrate as two disconnected transparent conductive layers/electrodes at the lower layer, taking a three-dimensional thiophene polymer as an electrochromic material, taking a solid electrolyte as an electrolyte layer, and connecting two independent electrochromic devices at the top by using a polar material.

2. The single-layer horizontal electrochromic device as claimed in claim 1, wherein the electrochromic material is synthesized by adding 5,5' - (3,5-didecylthiophene-2,4-diyl) bis (2,3-dihydrothieno [3,4-b ] [1,4] dioxine) and EDOT tin reagent into dry THF respectively, introducing N2 for about 20-40 min, adding PdCl2(PPh3)2 catalyst at room temperature, refluxing for 18-24 h at 100 ℃, washing with water, diluting, drying, filtering and spin-drying; and (3) spin-drying the obtained mixture by using dichloromethane and three times of silica gel, eluting by using a mixed eluent, washing by using methanol and dichloromethane, and drying at normal temperature to obtain the t-EDOT-TH-like liquid crystal phase electrochromic material.

3. A single-layer horizontal electrochromic device as claimed in claim 2, wherein 5,5' - (3, 5-dicylchitophene-2, 4-diyl) bis (2,3-dihydrothieno [3,4-b ] [1,4] dioxine): EDOT tin reagent is 1: 5-8 (molar ratio), 5,5' - (3,5-didecylthiophene-2,4-diyl) bis (2,3-dihydrothieno [3,4-b ] [1,4] dioxine): PdCl2(PPh3)2 catalyst 2-5: 1 (molar ratio).

4. Single-layer horizontal electrochromic device according to claim 2, wherein the mixed eluent of electrochromic materials can be DCM: PE ═ 1: 1-2 (volume ratio).

5. The single-layered horizontal electrochromic device according to claim 1, wherein the water-and oxygen-blocking transparent substrate may be a PC/PMMA composite, PTFE/PVDF composite, CPI, or the like.

6. A single-layer horizontal electrochromic device according to claim 1, wherein the water-and oxygen-blocking conductive material/transparent substrate is made by coextrusion of three layers, the upper and lower layers incorporating one or more of fillers such as MMT, graphene oxide, mica platelets.

7. Single level electrochromic device as claimed in claim 1, wherein the conductive material and process material of the transparent substrate may be a metallized mesh, a surface layer carbonized/graphitized, etc.

8. The single-layered horizontal electrochromic device as set forth in claim 1, wherein the electrolyte layer is a solid electrolyte solvent of polymethylmethacrylate, polystyrene pyrrolidone, or the like.

Technical Field

The invention relates to a preparation method of a transparent substrate single-layer horizontal electrochromic device, belonging to the field of organic photoelectric materials. In particular to a transparent base substrate, an associated electrode layer, an electrochromic layer and an electrolyte layer, all of which are coextruded using three layers. Has the characteristics of flexibility, good stability, high color change response speed and wide application.

Background

The trend of non-renewable energy sources and the increasing severity of environmental pollution lead us to be aware of the necessity of developing new energy sources, the development of new energy sources is a development direction which must be adhered to by people besides the main development direction of developing solar energy, wind energy and geothermal energy to the greatest extent, and the development of new energy-saving and environment-friendly materials is also a development direction which is adhered to by people, and the electrochromic material is used as a new energy source material, so that a large amount of energy sources can be saved in the aspects of adjusting light, temperature, electric quantity storage and the like. The material is mainly applied to materials such as color-changing windows, intelligent color-changing textile guides, stealth, display screens, sunglasses, rear mirrors, super capacitor clothes, electronic tags and the like, and has small pollution and flexible display, so that the material has great potential in later development.

Disclosure of Invention

Aiming at the prior art, the invention provides a preparation method of a transparent substrate single-layer horizontal electrochromic device, which mainly comprises the synthesis of an electrochromic device substrate, the device composition, an upper-layer polar connecting material, an electrochromic material synthesis method and the like.

In order to achieve the purpose, the technical scheme of the invention is as follows:

a preparation method of a transparent substrate single-layer horizontal electrochromic device comprises the following steps:

the method comprises the following steps of taking a water-blocking and oxygen-blocking conductive material/transparent substrate as two disconnected transparent conductive layers/electrodes at the lower layer, taking a three-dimensional thiophene polymer as an electrochromic material, taking a solid electrolyte as an electrolyte layer, and connecting two independent electrochromic devices at the top by using a polar material.

As a further improvement of the invention, the synthesis method of the electrochromic material comprises the steps of respectively adding 5,5' - (3,5-didecylthiophene-2,4-diyl) bis (2,3-dihydrothieno [3,4-b ] [1,4] dioxine) and EDOT tin reagent into dry THF, introducing N2 for about 20-40 min, adding a PdCl2(PPh3)2 catalyst at room temperature, refluxing for 18-24 h at 100 ℃, cooling, washing with water, diluting, drying, filtering and spin-drying; and (3) spin-drying the obtained mixture by using dichloromethane and three times of silica gel, eluting by using a mixed eluent, washing by using methanol and dichloromethane, and drying at normal temperature to obtain the liquid crystal phase electrochromic material of the liquid crystal phase polymer similar to the t-EDOT-TH.

As shown in fig. 2:

as a further improvement of the invention, the electrochromic material is 5,5' - (3,5-didecylthiophene-2,4-diyl) bis (2,3-dihydrothieno [3, 4-b)][1,4]dioxine): EDOT tin reagent is 1: 5-8 (molar ratio), 5,5' - (3,5-didecylthiophene-2,4-diyl) bis (2,3-dihydrothieno [3,4-b ]][1,4]dioxine)： PdCl₂(PPh₃)₂And (3) the catalyst is 2-5: 1 (molar ratio).

As a further improvement of the present invention, the mixed eluent of the electrochromic material may be DCM: PE ═ 1: 1-2 (volume ratio).

As a further improvement of the invention, the water-blocking and oxygen-blocking transparent substrate can be a PC/PMMA composite, a PTFE/PVDF composite, a CPI material and the like.

As a further improvement of the invention, the manufacturing method of the water-blocking and oxygen-blocking conductive material/transparent substrate is three-layer coextrusion, and one or more of fillers such as MMT, graphene oxide and mica sheets are added into the upper layer and the lower layer.

As a further improvement of the invention, the conductive material and the method material of the middle transparent substrate can be metal-plated grids, surface carbonization/graphitization and the like.

As a further improvement of the present invention, the electrolyte layer is a solid electrolyte solvent such as polymethyl methacrylate, polystyrene pyrrolidone, or the like.

Drawings

FIG. 1 is a schematic diagram of a transparent substrate single-layer horizontal electrochromic device;

FIG. 2 is a schematic molecular structure diagram of a liquid crystal phase electrochromic material of a t-EDOT-TH-like liquid crystal phase polymer;

Detailed Description

The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.