An all-in-one liquid electrochromic device and preparation method thereof

Abstract

The present invention relates to a preparation method and application of an all-in-one liquid electrochromic device, belonging to the field of electrochromic technology. The all-in-one liquid electrochromic device is composed of two layers of transparent indium tin oxide conductive glass and an all-in-one liquid electrochromic electrolyte filled between the two layers. The preparation method includes the preparation of the all-in-one liquid electrochromic device and the preparation of the all-in-one liquid electrochromic device electrolyte. The present invention uses a sarling film and a press to prepare an all-in-one liquid electrochromic device, which not only effectively simplifies the structure of the electrochromic device and reduces the manufacturing cost, but also the prepared device has a short production cycle, is easy to prepare, and has an excellent packaging effect. The prepared all-in-one liquid electrochromic device can achieve obvious color changes under the action of an external electric field, has high stability, and has broad application prospects in the fields of smart windows, energy-saving glass, etc.

Description

Technical Field

[0001] The present invention relates to a preparation method and application of an electrochromic device, and in particular to a preparation method and application of an all-in-one liquid electrochromic device, belonging to the technical field of electrochromic devices. Background Art

[0002] Electrochromism is defined as a phenomenon in which the optical properties of materials in the ultraviolet, visible and near-infrared regions change in a controllable, reversible and lasting manner due to the injection / extraction of electrons or ions caused by the application of current or electric field. In the electrochromic process, it is generally clearly observed that the color and transmittance of the material change significantly with the change of voltage. Electrochromic materials are widely used in many fields such as smart windows, energy-saving buildings, glare-free reflectors and smart displays.

[0003] The traditional electrochromic device consists of five layers: a transparent conductive layer, an electrochromic layer, an electrolyte layer, a counter electrode layer, and a transparent conductive layer. It can be regarded as a sandwich structure similar to a "sandwich". Under the action of an external electric field, electrons are injected (or extracted) from the transparent conductive layer into the electrochromic layer, causing the electrochromic device to change color (color or fade). For electrical balance, counterions are provided by the electrolyte layer and are kept electrically neutral by the counter electrode. For various reasons, how to prepare high-performance, long-life electrochromic devices remains an important research challenge. First, traditional electrochromic devices are usually formed by stacking five layers together to form a "sandwich" structure, and the interface blocking of different functional layers is an important factor that is not conducive to electron capture and thus limits the performance of the device. In addition, the multi-layer sandwich structure also increases the complexity of the package, and will also increase the difficulty of making large-area devices and increase production costs. At the same time, the all-in-one liquid electrochromic devices prepared in the literature are all simply heated at high temperature to dissolve the hot melt adhesive. The prepared devices have the disadvantages of long production cycle and uneven dissolution of the hot melt adhesive, resulting in poor device performance. Therefore, in order to reduce costs, reduce technical complexity and improve efficiency, simplification and improvement of the electrochromic device structure is an important aspect of studying the development of electrochromic devices. Summary of the invention

[0004] In order to overcome the deficiencies of the prior art, the present invention provides a method for preparing an all-in-one liquid electrochromic device. The prepared liquid electrochromic device has a simple preparation method, simple operation steps, and excellent device performance.

[0005] The purpose of the present invention can be achieved by the following technical solutions:

[0006] The invention discloses an all-in-one liquid electrochromic device, which is composed of two sheets of transparent conductive indium tin oxide glass and an all-in-one liquid electrochromic electrolyte filled between the two sheets of transparent conductive indium tin oxide glass.

[0007] A method for preparing an all-in-one liquid electrochromic device comprises the following steps:

[0008] (1) Preparation of the cavity of the all-in-one liquid electrochromic device:

[0009] Place the cleaned indium tin oxide conductive glass with the conductive surface facing up, and place a piece of Surlyn film with a hollow middle and a small hole on the right side on it, ensuring that three sides of the Surlyn film are in contact with the edges of the indium tin oxide conductive glass, and the side with the small hole is separated from the edge of the indium tin oxide conductive glass by a certain distance. Then place another piece of cleaned indium tin oxide conductive glass with the conductive surface facing down on the Surlyn film, and finally use a press to encapsulate the device.

[0010] (2) Preparation of all-in-one liquid electrochromic device electrolyte:

[0011] Weigh 0.05 M heptyl viologen tetrafluoroborate, 0.05 M anode electrochromic material and 0.5 M tetrabutylammonium tetrafluoroborate and dissolve them in a solvent.

[0012] (3) Fabrication of all-in-one liquid electrochromic devices:

[0013] A piece of foam is placed in a single-mouth round-bottom flask as a substrate for placing the device, and the cavity of the all-in-one liquid electrochromic device prepared in step (1) is placed on the foam substrate in the single-mouth round-bottom flask. Then, the cavity of the all-in-one liquid electrochromic device is replaced with nitrogen, and then the all-in-one liquid electrochromic device electrolyte prepared in step (2) is dripped onto the small hole reserved in the sarling film, and the all-in-one liquid electrochromic device electrolyte is injected into the device using a pressure difference, and finally the reserved small hole is sealed using ultraviolet light curing glue.

[0014] The method for cleaning the indium tin oxide conductive glass in step (1) is: first, ultrasonically clean the indium tin oxide conductive glass with deionized water, acetone and isopropanol for 15 minutes respectively, and then blow dry with nitrogen.

[0015] The size of the indium tin oxide conductive glass in step (1) is 1.5×2.5 cm 2 .

[0016] The size of the cavity of the sarin membrane in step (1) is 1.4×1.7 cm 2 .

[0017] In step (1), the press is pressed at 0.1 MPa and 130° C. for 50 seconds.

[0018] In step (2), the anode electrochromic material ferrocene is dissolved in a propylene carbonate solution, and N,N,N',N'-tetrakis(4-methoxyphenyl)benzidine is dissolved in a nitrogen methyl pyrrolidone solution.

[0019] The volume of the all-in-one liquid electrochromic device electrolyte prepared in step (2) is 0.05 mL.

[0020] The present invention has the following advantages:

[0021] The present invention prepares an all-in-one liquid electrochromic device by means of a hot press. The prepared device not only effectively simplifies the structure of the electrochromic device and reduces the manufacturing cost, but also the present invention uses a sarin film and a hot press to encapsulate the device. The prepared device has a short production cycle, and only needs 50 seconds to prepare a device. The preparation is simple, the packaging effect is excellent, and the electrochromic performance is improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a color change diagram of the all-in-one liquid electrochromic device of Example 1 under an external electric field.

[0023] Figure 2 : is the ultraviolet absorption spectrum of the all-in-one liquid electrochromic device of Example 1 at room temperature; as can be seen from the figure, the maximum absorption wavelength in the visible light region is at 604nm.

[0024] Figure 3 The cyclic stability of the all-in-one liquid electrochromic device of Example 1 at room temperature is shown; the results show that at the maximum absorption wavelength of 604nm, the transmittance difference of the electrochromic device can still maintain 92.1% of the initial state after 3000 cycles.

[0025] Figure 4 The response time diagram of the all-in-one liquid electrochromic device of Example 1 at room temperature; the results show that at the maximum absorption wavelength of 604nm, the coloring time of the electrochromic device is 0.28s and the fading time is 0.34s. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments.

[0027] Example 1

[0028] (1) Preparation of the cavity of the all-in-one liquid electrochromic device:

[0029] The cleaned 2.5×1.5cm 2 The indium tin oxide conductive glass is placed with the conductive surface facing up, and a piece of Surlyn film with a hollow middle and a small hole on the right is placed on it. Then, another piece of cleaned indium tin oxide conductive glass is placed on the Surlyn film with the conductive surface facing down. Finally, a press is used to press at 0.1MPa and 130℃ for 50s, and then the device is cooled and put into use.

[0030] (2) Preparation of all-in-one liquid electrochromic device electrolyte:

[0031] 1.3 mg of heptyl viologen tetrafluoroborate, 0.5 mg of ferrocene and 3.3 mg of tetrabutylammonium tetrafluoroborate were weighed and dissolved in 0.05 mL of propylene carbonate solution, followed by ultrasonication for 15 min to completely dissolve them.

[0032] (3) Preparation of all-in-one liquid electrochromic devices:

[0033] The side of the all-in-one liquid electrochromic device prepared in step (1) with the small hole in the cavity is vertically inserted upward into the foam base in the single-mouth round-bottom flask. Then, the cavity of the all-in-one liquid electrochromic device is replaced with nitrogen using a vacuum pump, and then the all-in-one liquid electrochromic device electrolyte prepared in step (2) is dripped onto the small hole reserved in the sarin membrane, and the single-mouth round-bottom flask is evacuated again, and then the single-mouth round-bottom flask is connected to the atmosphere, and the all-in-one liquid electrochromic device electrolyte is injected into the device using the pressure difference, and finally the reserved small hole is sealed using ultraviolet light curing glue.

[0034] Example 2

[0035] (1) The preparation method of the all-in-one liquid electrochromic device cavity is the same as that in Example 1.

[0036] (2) Preparation of all-in-one liquid electrochromic device electrolyte:

[0037] 1.3 mg of heptyl viologen tetrafluoroborate, 1.5 mg of N,N,N',N'-tetrakis(4-methoxyphenyl)benzidine and 3.3 mg of tetrabutylammonium tetrafluoroborate were weighed and dissolved in 0.05 mL of nitrogen methyl pyrrolidone solution, followed by ultrasonication for 15 min to completely dissolve them.

[0038] (3) The preparation method of the all-in-one liquid electrochromic device is the same as that in Example 1.

[0039] The above description is only a preferred example of the present invention and cannot be used to limit the protection scope of the present invention. Any modifications and improvements made within the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing an all-in-one liquid electrochromic device, comprising the following steps: (1) Preparation of the cavity of the all-in-one liquid electrochromic device: Place the cleaned indium tin oxide conductive glass with the conductive surface facing upwards, and place a piece of sarling film with a hollow middle and a small hole on the right side on it, ensuring that three sides of the sarling film are in contact with the edge of the indium tin oxide conductive glass, and the side with the small hole is at a certain distance from the edge of the indium tin oxide conductive glass, then place another cleaned indium tin oxide conductive glass with the conductive surface facing downwards on the sarling film, and finally use a press to encapsulate the device; (2) Preparation of all-in-one liquid electrochromic device electrolyte: 0.05 M heptyl viologen tetrafluoroborate, 0.05 M anode electrochromic material and 0.5 M tetrabutylammonium tetrafluoroborate were dissolved in a solvent. (3) Fabrication of all-in-one liquid electrochromic devices: A piece of foam is placed in a single-mouth round-bottom flask as a substrate for placing the device, and the cavity of the all-in-one liquid electrochromic device prepared in step (1) is placed on the foam substrate in the single-mouth round-bottom flask. Then, the cavity of the all-in-one liquid electrochromic device is replaced with nitrogen, and then the all-in-one liquid electrochromic device electrolyte prepared in step (2) is dripped onto the small hole reserved in the sarling film, and the all-in-one liquid electrochromic device electrolyte is injected into the device using a pressure difference, and finally the reserved small hole is sealed using ultraviolet light curing glue.

2. The method for preparing an all-in-one liquid electrochromic device according to claim 1, characterized in that: The method for cleaning the indium tin oxide conductive glass in step (1) is: first, ultrasonically clean the indium tin oxide conductive glass with deionized water, acetone and isopropanol for 15 minutes respectively, and then blow dry with nitrogen.

3. The method for preparing an all-in-one liquid electrochromic device according to claim 1, characterized in that: The size of the indium tin oxide conductive glass in step (1) is 1.5×2.5 cm 2 .

4. The method for preparing an all-in-one liquid electrochromic device according to claim 1, characterized in that: The size of the cavity of the sarin membrane in step (1) is 1.4×1.7 cm 2 .

5. The method for preparing an all-in-one liquid electrochromic device according to claim 1, characterized in that: In step (1), the press is pressed at 0.1 MPa and 130° C. for 50 seconds.

6. The method for preparing an all-in-one liquid electrochromic device according to claim 1, characterized in that: In step (2), the anode electrochromic material is ferrocene dissolved in a propylene carbonate solution, or N,N,N',N'-tetrakis(4-methoxyphenyl)benzidine dissolved in an N-methylpyrrolidone solution.

7. The method for preparing an all-in-one liquid electrochromic device according to claim 1, characterized in that: The volume of the all-in-one liquid electrochromic device electrolyte prepared in step (2) is 0.05 mL.

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