CN111471448A - Liquid bipolar color-changing particle, preparation method of electrochromic layer and electrochromic device - Google Patents
Liquid bipolar color-changing particle, preparation method of electrochromic layer and electrochromic device Download PDFInfo
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- CN111471448A CN111471448A CN202010390897.9A CN202010390897A CN111471448A CN 111471448 A CN111471448 A CN 111471448A CN 202010390897 A CN202010390897 A CN 202010390897A CN 111471448 A CN111471448 A CN 111471448A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
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Abstract
The application relates to a liquid bipolar color-changing particle, a preparation method of an electrochromic layer and an electrochromic device, wherein the preparation method of the liquid bipolar color-changing particle comprises the following steps: adding the bipolar color-changing particle solution into the nano dispersant, and stirring into uniformly dispersed liquid; carrying out first reduced pressure distillation on the liquid, and removing the solvent in the bipolar color changing particle solution to obtain a suspension; mixing the suspension with acrylic microspheres according to the mass fraction ratio of 10:1, and stirring until the suspension is uniformly dispersed to obtain a mixed solution; and carrying out reduced pressure distillation on the mixed solution to remove air bubbles in the mixed solution, thereby obtaining the liquid-state bipolar color-changing particles. Compared with the electrochromic layer in the existing electrochromic glass, the electrochromic layer prepared by the liquid-state bipolar color-changing particles and the preparation method of the electrochromic layer has obvious advantages in color-changing effect, and is lower in haze and voltage.
Description
Technical Field
The application relates to electrochromic glass, in particular to liquid bipolar color changing particles, a preparation method of an electrochromic layer and an electrochromic device.
Background
The electrochromic glass has the adjustability of light absorption and transmission under the action of an electric field, can selectively absorb or reflect external heat radiation and internal heat diffusion, and reduces a large amount of energy which is consumed for keeping office buildings and civil houses cool in summer and warm in winter. Meanwhile, the purposes of improving the natural illumination degree and preventing peeping are achieved. The problem of urban light pollution which is continuously worsened in modern times is solved, and the method is a development direction of energy-saving building materials.
In carrying out the present application, the applicant has found that: the prior electrochromic glass has the problems of high voltage, slow response speed, high haze, environmental protection and the like. Therefore, a scheme is urgently needed to solve the problems of high voltage, low response speed, high haze, environmental protection and the like in the electrochromic glass.
Disclosure of Invention
The embodiment of the application provides a liquid-state bipolar color-changing particle, a preparation method of an electrochromic layer and an electrochromic device, and solves the problems of high voltage, low response speed, high haze, environmental protection and the like of the conventional electrochromic glass.
In order to solve the above technical problem, the present application is implemented as follows:
in a first aspect, a method for preparing liquid-state bi-polar color-changing particles is provided, which is applied to an electrochromic layer process, and comprises the following steps:
adding the bipolar color-changing particle solution into the nano dispersant, and stirring into uniformly dispersed liquid;
carrying out first reduced pressure distillation on the liquid, and removing the solvent in the bipolar color changing particle solution to obtain a suspension;
mixing the suspension with acrylic microspheres according to the mass fraction ratio of 10:1, and stirring until the suspension is uniformly dispersed to obtain a mixed solution;
and carrying out reduced pressure distillation on the mixed solution to remove air bubbles in the mixed solution, thereby obtaining the liquid-state bipolar color-changing particles.
In a first possible implementation manner of the first aspect, the solvent in the bipolar color-changing particle solution is isoamyl acetate.
In a second possible implementation of the first aspect, the nanodispersant is dioctyl terephthalate.
In a third possible implementation manner of the first aspect, the temperature of the reduced pressure distillation is 58-62 degrees.
In a fourth possible implementation manner of the first aspect, the acrylic beads have a diameter of 10 micrometers.
In a second aspect, there is provided a method for preparing an electrochromic layer, comprising the steps of:
taking the liquid bipolar discoloration particles prepared by the liquid bipolar discoloration particle preparation method in any one of the first aspect;
compounding liquid bipolar color-changing particles between the two film layers, and sealing the peripheries of the two film layers;
and manufacturing electrodes on the two film layers.
In a first possible implementation manner of the second aspect, the film layer is a polyester film or an indium tin oxide semiconductor film.
In a second possible implementation manner of the second aspect, the liquid-state bipolar color-changing particles are compounded between two film layers by an extrusion device; the peripheries of the two film layers are sealed by glue.
In a third aspect, an electrochromic layer is provided, comprising: the liquid bipolar color-changing particles are arranged between the two film layers, the peripheries of the two film layers are sealed, and the two film layers are respectively provided with an electrode for driving the liquid bipolar color-changing particles to change color.
In a fourth aspect, there is provided an electrochromic device comprising two cover plates and an electrochromic layer of the third aspect, the electrochromic layer being disposed between the two cover plates.
Compared with the prior art, the application has the advantages that:
according to the liquid bipolar color changing particles, the preparation method of the electrochromic layer and the electrochromic device, compared with the existing electrochromic layer in electrochromic glass, the electrochromic layer has obvious advantages in color changing effect, and is lower in haze and voltage.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic flow chart of steps of a method for preparing liquid-state bipolar color-changing particles according to a first embodiment of the present application.
Fig. 2 is a schematic flow chart illustrating steps of a method for manufacturing an electrochromic layer according to a second embodiment of the present application.
Fig. 3 is a schematic structural view of an electrochromic layer of a third embodiment of the present application.
Fig. 4 is a schematic structural diagram of an electrochromic device according to a fourth embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In a first embodiment of the present application, the method for preparing liquid bichromal particles of the embodiment is mainly applied to a process of an electrochromic layer, and is used for preparing the liquid bichromal particles applied to the electrochromic layer.
The flow of the steps of the method for preparing the liquid bichromal particles is described below. Fig. 1 is a schematic flow chart of steps of a method for preparing liquid-state bipolar color-changing particles according to a first embodiment of the present application. As shown in fig. 1, the liquid-state bipolar color-changing particle preparation method 1 includes the following steps 101 to 104, wherein:
Specifically, the bipolar color changing particles are dissolved and dispersed in the acetic acid isoamyl ester to form a bipolar color changing particle solution, then the bipolar color changing particle solution is added into the dioctyl terephthalate, and the mixture is stirred uniformly by an ultrasonic stirring mode to form uniformly dispersed liquid. It should be understood that the solvent in the solution of the bi-polar color-changing particles is only illustrated by taking the isoamyl acetate as an example, but not limited thereto, and those skilled in the art can also select other materials capable of dissolving the bi-polar color-changing particles as the solvent in the solution of the bi-polar color-changing particles according to the teachings of the present embodiment. It should also be understood that the nano dispersant is described above by taking dioctyl terephthalate as an example, but the nano dispersant is not limited thereto.
102, carrying out first reduced pressure distillation. And carrying out first reduced pressure distillation on the liquid, and removing the solvent in the bipolar color changing particle solution to obtain a suspension.
Specifically, the liquid dispersed in the step 101 is placed in a vacuum distillation apparatus, the vacuum distillation temperature is set to be 58-62 ℃, and the first vacuum distillation is performed to remove isoamyl acetate to obtain a suspension, wherein the suspension refers to the color-changing dye, but the suspension is not limited thereto. In this example, there is no particular requirement for the selection of the vacuum distillation apparatus, and the conventional selection by those skilled in the art is referred to.
Specifically, the suspension prepared in the step 102 and the acrylic beads are mixed according to the mass fraction of 10:1, wherein the diameter of the acrylic micro-bead is 10 microns, and the stirring temperature is 58-62 ℃.
And 104, carrying out second reduced pressure distillation. And carrying out reduced pressure distillation on the mixed solution to remove air bubbles in the mixed solution, thereby obtaining the liquid-state bipolar color-changing particles.
Specifically, after the suspension and the acrylic beads are uniformly stirred, the suspension is placed in a reduced pressure distillation device, the mixed solution is subjected to a second reduced pressure distillation to remove air bubbles in the mixed solution, so as to obtain liquid-state bipolar color change particles, and the liquid-state bipolar color change particles can be used for preparing an electrochromic layer in a subsequent electrochromic layer manufacturing process, but not limited thereto.
In a second embodiment of the present application, fig. 2 is a schematic flow chart illustrating steps of a method for manufacturing an electrochromic layer according to the second embodiment of the present application. As shown in fig. 2, the electrochromic layer preparation method 2 includes the following steps 201 to 203, in which:
Specifically, the liquid-state bipolar color changing particles prepared according to the liquid-state bipolar color changing particle preparation method 1 shown in the first embodiment described above.
Specifically, the liquid bi-polar color-changing particles are compounded between two polyester films (PET)/indium tin oxide semiconductor films (ITO) by an extrusion device, and the periphery of the liquid bi-polar color-changing particles is sealed by glue, but not limited thereto. It should be understood that the above description is only for the example of PET/ITO, but not limited thereto.
Specifically, electrodes are formed on the two film layers to provide voltage for the liquid bi-polar color-changing particles between the two film layers to change color. It should be noted that the method for manufacturing the electrode is a conventional technical means in the art, and therefore, this embodiment is not described herein again.
In a third embodiment of the present application, fig. 3 is a schematic structural diagram of an electrochromic layer of the third embodiment of the present application. As shown in fig. 3, the electrochromic layer 3 includes two film layers 301 and the liquid bichromal particles 302 prepared in the first embodiment, the liquid bichromal particles 302 are disposed between the two film layers 301, the peripheries of the two film layers 301 are sealed, and the two film layers 301 are further respectively provided with electrodes 303 for driving the liquid bichromal particles 302 to change color. Preferably, the film 301 is a polyester film (PET) or an indium tin oxide semiconductor film (ITO), but not limited thereto.
Alternatively, the electrode 303 generally includes a first conductive layer 31, an electrolyte layer 32, an ion storage layer 33, and a second conductive layer 34. Specifically, as shown in fig. 3, the film layer 301 is a polyester film, the liquid-state bipolar color-changing particles 302 are compounded between two polyester films, and the periphery of the film layer is sealed by glue 304. The first conductive layer 31 is provided on one of the polyester films, and the electrolyte layer 32, the ion storage layer 33, and the second conductive layer 34 are laminated and sequentially provided on the other polyester film. It should be understood that the above description is only for the example of the polyester film, but not limited thereto. It should be further understood that the electrode 303 is described above by taking only the first conductive layer 31, the electrolyte layer 32, the ion storage layer 33, and the second conductive layer 34 as an example, but not limited thereto.
In a fourth embodiment of the present application, fig. 4 is a schematic structural diagram of an electrochromic device 4 according to the fourth embodiment of the present application. As shown in fig. 4, the electrochromic device 4 includes two cover plates 401 and the electrochromic layer 3 prepared by the above-described second embodiment electrochromic layer preparation method 2, with the electrochromic layer 3 being disposed between the two cover plates 401.
Optionally, the cover plate 401 is glass. In particular, as shown in fig. 4, the first conductive layer 31 is arranged on one of the glass cover plates, and the second conductive layer 34 is arranged on the other glass cover plate, so that the electrochromic layer 3 is arranged between the two glass cover plates. It should be understood that the cover 401 is described above by taking glass as an example, but not limited thereto.
The following will illustrate the beneficial effects of the liquid bicolor particle preparation method of the present application in combination with specific examples and test data.
Example 1
Dissolving and dispersing the bipolar discoloring particles in isoamyl acetate to form a bipolar discoloring particle solution, then adding the bipolar discoloring particle solution into dioctyl terephthalate, and uniformly stirring the solution in an ultrasonic stirring manner to form uniformly dispersed liquid.
And (3) placing the dispersed liquid into a reduced pressure distillation device, setting the temperature of reduced pressure distillation at 60 ℃, carrying out first reduced pressure distillation on the liquid, and removing isoamyl acetate to obtain a suspension, wherein the suspension refers to the color-changing dye.
The suspension and the acrylic microspheres are mixed according to the mass fraction of 10:1, wherein the diameter of the acrylic microspheres is 20 microns, the stirring temperature is set to be 60 ℃, and the solution is subjected to secondary reduced pressure distillation to remove bubbles in the solution, so that the liquid bipolar color-changing particles are obtained. The liquid bipolar color-changing particle obtained in the way has the light transmission and color change range of 5-65% and the haze of 2.5-0.9%.
Example 2
The difference between this example and the above example 1 is that the diameter of the acrylic bead in this example is 15 μm. The light-transmitting and color-changing range of the color-changing particles obtained in the mode is 5% -65%, and the haze is 2.0% -0.85%.
Example 3
The difference between this embodiment and the above embodiment 1 is that the diameter of the acrylic bead in this embodiment is 10 μm. The light-transmitting and color-changing range of the color-changing particles obtained in the mode is 5-65%, and the haze is 1.6-0.7%.
Example 4
The difference between this example and the above example 1 is that the diameter of the acrylic bead in this example is 5 μm. The light-transmitting and color-changing range of the color-changing particles obtained in the mode is 5-60%, and the haze is 1.5-0.7%.
As is obvious from the above embodiments 1 to 4, compared with the electrochromic particles in the existing electrochromic layer, the liquid bipolar color change particles prepared by the liquid bipolar color change particle preparation method 1 of the present application have obvious advantages in color change effect, and are lower in haze and voltage.
In addition, as can be seen from the test data of the above examples 1 to 4, the haze of the liquid bicolor particles obtained in examples 1 and 2 is higher; the discoloration effect of the liquid-state bipolar-discoloration particles obtained in example 4 was decreased; haze and discoloration effect of the liquid bichromal particles obtained in example 3. Therefore, the light-transmitting color-changing particles prepared by mixing acrylic micro-beads with the diameter of 10 microns and the suspension have better light transmission, color changing and haze.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of liquid bipolar color-changing particles is applied to the manufacture procedure of an electrochromic layer and is characterized by comprising the following steps:
adding the bipolar color-changing particle solution into the nano dispersant, and stirring into uniformly dispersed liquid;
carrying out first reduced pressure distillation on the liquid, and removing the solvent in the bipolar color changing particle solution to obtain a suspension;
mixing the suspension with acrylic microspheres according to the mass fraction ratio of 10:1, and stirring until the suspension is uniformly dispersed to obtain a mixed solution;
and carrying out reduced pressure distillation on the mixed solution, and removing bubbles in the mixed solution to obtain the liquid-state bipolar color-changing particles.
2. The method for preparing liquid bichromal particles according to claim 1, wherein the solvent in the solution of bichromal particles is isoamyl acetate.
3. The method for preparing liquid bichromatic particles according to claim 1 wherein the nano dispersant is dioctyl terephthalate.
4. The method for preparing liquid bichromal particles according to claim 1, wherein the temperature of the reduced pressure distillation is 58 to 62 ℃.
5. The method of preparing liquid bichromal particles according to claim 1, wherein the acrylic beads have a diameter of 10 μm.
6. A method for preparing an electrochromic layer is characterized by comprising the following steps:
taking the liquid bipolar color change particles prepared by the method for preparing the liquid bipolar color change particles according to any one of the claims 1 to 5;
compounding the liquid bipolar color-changing particles between the two film layers, and sealing the peripheries of the two film layers;
and manufacturing electrodes on the two film layers.
7. The method for producing an electrochromic layer according to claim 6, wherein the film layer is a polyester film or an indium tin oxide semiconductor film.
8. The method for preparing an electrochromic layer according to claim 6, wherein the liquid-state bipolar color-changing particles are compounded between two of the film layers by an extrusion apparatus; the peripheries of the two film layers are sealed by glue.
9. An electrochromic layer, comprising: two film layers and the liquid bipolar color changing particles prepared by the method for preparing liquid bipolar color changing particles according to any one of claims 1 to 5, wherein the liquid bipolar color changing particles are arranged between the two film layers, the peripheries of the two film layers are sealed, and electrodes are respectively arranged on the two film layers and used for driving the liquid bipolar color changing particles to change color.
10. An electrochromic device comprising two cover plates and an electrochromic layer according to claim 9, said electrochromic layer being arranged between said two cover plates.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113755805A (en) * | 2021-09-09 | 2021-12-07 | 宁波伯宇科技有限公司 | Curved surface coating process for electrochromic lens |
| CN115212779A (en) * | 2022-07-05 | 2022-10-21 | 江苏铁锚玻璃股份有限公司 | Iodine removing method for bipolar color-changing particles |
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| CN106707653A (en) * | 2017-03-28 | 2017-05-24 | 江苏铁锚玻璃股份有限公司 | Intelligent glass used for dimming and color changing |
| CN108363255A (en) * | 2018-03-27 | 2018-08-03 | 深圳市华科创智技术有限公司 | A kind of electrochromism membrane material and its electrochromism membrane module of preparation |
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2020
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| CN1308716A (en) * | 1998-07-09 | 2001-08-15 | 尖端研究公司 | Light-polarizing particles of improved particle size distribution |
| CN106479478A (en) * | 2015-08-24 | 2017-03-08 | 北京大学 | A kind of electrochromic material based on metal nanoparticle and device |
| CN106707653A (en) * | 2017-03-28 | 2017-05-24 | 江苏铁锚玻璃股份有限公司 | Intelligent glass used for dimming and color changing |
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| CN113755805A (en) * | 2021-09-09 | 2021-12-07 | 宁波伯宇科技有限公司 | Curved surface coating process for electrochromic lens |
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| CN115212779B (en) * | 2022-07-05 | 2023-05-26 | 江苏铁锚玻璃股份有限公司 | Iodine removal method for bipolar color-changing particles |
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