CN108828868B - Preparation method of electrochromic film - Google Patents
Preparation method of electrochromic film Download PDFInfo
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- CN108828868B CN108828868B CN201810410696.3A CN201810410696A CN108828868B CN 108828868 B CN108828868 B CN 108828868B CN 201810410696 A CN201810410696 A CN 201810410696A CN 108828868 B CN108828868 B CN 108828868B
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- G—PHYSICS
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- 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
- G02F1/153—Constructional details
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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
- G02F1/13—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 liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
Abstract
The invention discloses a preparation method of an electrochromic film. The prepared electrochromic film is formed by compounding metal oxide, Transparent Conductive Oxide (TCO) and a transparent conductive substrate. The invention adopts a blending method to prepare the coating liquid of the metal oxide and the TCO, and then adopts a wet coating method to prepare the electrochromic oxide nano film. The invention has the advantages that: the preparation method of the film is simple and convenient, and is suitable for large-scale production. The electrochromic film has the characteristics of short coloring and fading time, large optical modulation range, good cycle performance and low cost, and is suitable for manufacturing large-area electrochromic films.
Description
Technical Field
The invention relates to a preparation method of an optical film, in particular to a preparation method of an electrochromic functional film, which is applied to the technical field of preparation processes of nano inorganic functional material films.
Background
Electrochromism refers to reversible and stable change of transmittance, absorptivity or reflectivity of optical properties of a material in an ultraviolet, visible or near-infrared light region under the drive of an external electric field or current, and the appearance of the material shows change of color and transparency. Devices fabricated using this characteristic are referred to as electrochromic devices. Research on electrochromism dates back to 60s of the 19 th century, where WO was first discovered by s.k3The film has electrochromic performance, an electrochromic device is prepared by using the film, the color change mechanism of an oxygen vacancy color center is provided, the research enthusiasm of numerous scientists is attracted, and the electrochromic film is further widely applied to the fields of automobiles, airplanes, train embedded glass, building embedded glass, instrument display, optical elements, electronic paper and the like. Chinese patent No. CN104111568A discloses an intelligent glass capable of electrochromic, electrochemical energy storage and driving electronic devices, which has the functions of electrochromic, storing electrical energy and driving electronic devices, and can be used for light regulation and power supply.
Electrochromic materials are used as a novel energy-saving material and are divided into inorganic electrochromic materials and organic electrochromic materials according to the types of the materials. The inorganic electrochromic materials can be classified into cathode electrochromic materials and anode electrochromic materials according to different coloring modes. Representative of cathodic electrochromic materials are WO3、MoO3、TiO2、Nb2O5、V2O5Etc.; of anodically electrochromic materialsRepresentative is NiO and Co2O3、IrOx、Rh2O3、V2O5And the like. Representative organic electrochromic materials are: viologen, polyaniline, polypyrrole, polythiophene compounds and derivatives thereof and the like. However, the high cost and complexity of the technology for preparing the thin film still limit the development and application. The preparation method of the inorganic electrochromic film mainly comprises a sputtering method, a sol-gel method, an electrodeposition method, an anodic oxidation method, a hydrothermal/solvothermal method, an ink-jet printing method and the like. Chinese patent No. CN105366954A discloses a method for preparing a nano tungsten oxide electrochromic film, which combines liquid-phase laser ablation with electrophoretic deposition to obtain a tungsten oxide film with high activity and high hybridization degree, but the method requires expensive equipment. Chinese patent No. 201510824861.6 discloses a method for preparing a NiO nanocrystalline electrochromic film, which adopts an injection method and a pulling method to prepare a NiO nanocrystalline electrochromic film, wherein the obtained film has high uniformity and can be prepared in a large area. Therefore, it is always the direction of efforts of scientists to find a new method for preparing electrochromic thin film with low cost and simplicity, and the method is a technical problem to be solved urgently.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art and provide a preparation method of an electrochromic film, the electrochromic film is formed by compounding a metal oxide, a Transparent Conductive Oxide (TCO) and a transparent conductive substrate, large-scale continuous production is facilitated to prepare large-area electrochromic film devices, and the prepared electrochromic film has the advantages of large optical modulation, short color change time, good cycle stability, low manufacturing cost, simple process and easy realization.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an electrochromic film comprises the following steps:
a. mixing metal oxide nanoparticles and TCO nanoparticles to prepare a nano dispersion liquid, wherein the nano dispersion liquid is used as a coating liquid of metal oxide and TCO for later use; the metal oxide is an electrochromic material;
as a preferable technical scheme of the invention, the nano dispersion liquid comprises 100 parts by weight of metal oxide nanoparticles, 0.1-1000 parts by weight of TCO nanoparticles, 0.01-1000 parts by weight of dispersing agent, 100-20000 parts by weight of solvent, 0-1000 parts by weight of resin and 0-500 parts by weight of curing agent;
the metal oxide nanoparticles preferably adopt any one or any mixture of nanoparticles, nanorods, nanowires, nanotubes and nano-porous materials with electrochromic characteristics;
the TCO nano particles preferably adopt any one nano material or a mixture of any several nano materials of antimony-doped tin oxide, tin-doped indium oxide, gallium-doped zinc oxide, indium-doped gallium oxide and aluminum-doped zinc oxide;
when the nano dispersion liquid is prepared, the used solvent preferably adopts any one solvent or a mixture of any two solvents of alcohol, ether, ketone, ester, aromatic hydrocarbon and water;
when the nano dispersion liquid is prepared, the resin preferably adopts any one or a mixture of any more of epoxy resin, polyamide resin and dicyandiamide;
when the nano dispersion liquid is prepared, the curing agent is preferably any one or a mixture of any more of toluene diisocyanate, isophorone diisocyanate and polyamide;
b. after the transparent conductive substrate is pretreated, coating the nano dispersion liquid prepared in the step a on a conductive surface of the transparent conductive substrate by adopting a wet coating method to form a uniform nano particle thin layer;
the pretreatment method preferably adopts any one treatment method or any mixture of a plurality of treatment methods of Plasma treatment, physical cleaning, chemical cleaning, ultraviolet ozone treatment, heat treatment, corona discharge treatment and pressure treatment;
the wet coating method is preferably any one of spin coating, roll coating, bar coating, casting, dip coating, blade coating, spray coating, flow coating, micro gravure coating, slot coating, lip film extrusion coating, nozzle coating, comma coating, capillary coating and screen printing, flexography, offset printing, reverse printing, inkjet printing or any combination of several methods;
the transparent conductive substrate preferably adopts any one substrate or any mixed conductive material substrate of conductive glass of FTO, ITO, silver nanowires, graphene and conductive polymer films or conductive plastic films, sheets and plates based on FTO, ITO, silver nanowires, graphene and conductive polymer films;
c. b, performing heat treatment on the device formed by the transparent conductive substrate which is prepared in the step b and is used for forming the uniform nano-particle film, so as to obtain an electrochromic film formed by compounding the electrochromic metal oxide, the nano-film of the transparent conductive oxide and the transparent conductive substrate; the heat treatment temperature is preferably 30-450 ℃, and the heat treatment time is preferably 1-300 min; the heat treatment temperature is more preferably 50 to 400 ℃, and the heat treatment time is more preferably 5 to 300 min. Electrochromic metal oxide nanoparticles and transparent conductive oxide nanoparticles with the average particle size of 1-5000 nm are preferably adopted, and the thickness of a thin film layer with uniformly distributed nanoparticles formed on the conductive surface of the transparent conductive substrate is preferably 50-2000 nm.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method adopts the nano material as the raw material to directly obtain the electrochromic film with high uniformity, and is suitable for various nano particle materials;
2. the method adopts a method of mixing metal oxide nanoparticles and TCO nanoparticles, and solves the problems of short cycle life of an electrochromic device, uneven color change of large-area materials, low color change speed and poor optical modulation in the prior art;
3. the method adopts a method of coating the nano dispersion liquid by a wet method, can be used for a wide range of different substrates, has simple equipment and simple and convenient operation, and is convenient for large-scale production;
4. the nanometer electrochromic particle film obtained by the method has high coloring/fading contrast ratio, high response speed and good cycle performance, and the prepared nanometer films of the electrochromic metal oxide and the transparent conductive oxide have uniform distribution of nanometer particles, high film quality, simple process and low cost.
Drawings
FIG. 1 shows a method for preparing "WO" according to an embodiment of the present invention3nanoparticle-ITO nanoparticle electrochromic film and WO prepared in comparative example I3Contrast plot of transmittance curve of nano-particle electrochromic film in colored/faded state.
FIG. 2 is a comparison graph of transmittance curves of the electrochromic film of "NiO nanoparticles-AZO nanoparticles" prepared by the second method of the embodiment of the present invention and the electrochromic film of "NiO nanoparticles" prepared by the second comparative example in the colored/faded state.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example one
In this example, a method for preparing an electrochromic film, WO3The method for uniformly distributing the nano-particles and the ITO nano-particles in the electrochromic film comprises the following steps:
a. 5.6240g of WO3Dissolving the nano-particles, 0.5539g of ITO nano-particles and 0.3089g of dispersing agent in 70mL of ethanol, pouring the solution into a planetary rapid dispersion machine filled with zirconia balls with the diameter of 0.3mm, carrying out ball milling at the rotating speed of 10000r/min, and continuously dispersing for 13h to obtain nano-particle dispersion liquid serving as coating liquid of metal oxide and TCO for later use;
b. adopting ITO conductive glass as a transparent conductive substrate, pretreating the transparent conductive substrate, and cutting the ITO conductive glass with the surface resistance of 10 omega/□ into 3 multiplied by 4cm2The size of the gas is put into an Ar Plasma workstation for processing, the set parameters are 60W and 60s, the Ar gas flow is 30sccm, and the pressure is 75 mTorr; b, injecting the nano dispersion liquid prepared in the step a into a containing cavity containing coating liquid by adopting a slit extrusion coating method, and forming a uniform film on the conductive surface of the ITO conductive glass by using a slit extrusion coater;
c. performing heat treatment on the film formed on the transparent conductive substrate for forming the uniform nano-particle film prepared in the step b at 230 ℃ for 5min to obtain WO on the transparent conductive substrate3nanoparticle-ITO nanoparticle electrochromic films.
The transmittance curve of the electrochromic film obtained in the example in the colored state and the faded state is shown in fig. 1, and the optical modulation Δ T% at 630nm is 70%; the fading time of the electrochromic film is 8 s; after 1000 times of cycle processing, the film charge storage capacity is reduced by only 8%.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for preparing an electrochromic film, in which NiO nanoparticles and AZO nanoparticles are uniformly distributed in an electrochromic film, includes the following steps:
a. 4.8788g of NiO nano-particles, 0.9423g of AZO nano-particles and 0.2910g of dispersing agent are dissolved in 100mL of toluene, poured into a planetary rapid dispersion machine with zirconia balls with the diameter of 0.3mm, ball-milled at the rotating speed of 10000r/min, and continuously dispersed for 15 hours to obtain nano-particle dispersion liquid which is used as coating liquid of metal oxide and TCO for standby;
b. adopting ITO conductive glass as a transparent conductive substrate, pretreating the transparent conductive substrate, and cutting the ITO conductive glass with the surface resistance of 10 omega/□ into 3 multiplied by 4cm2B, drying the nano dispersion liquid after ultrasonic oscillation for 30min by using ethanol, acetone and water respectively, then pouring the nano dispersion liquid prepared in the step a into an ink box of a gravure coating machine by adopting a micro gravure coating preparation method, setting the rotating speed of a roller shaft to be 40rpm, adjusting the positions of a scraper and the micro gravure roller shaft, and adjusting the angle and the compression degree of the scraper so as to uniformly coat the nano particle dispersion liquidForming a uniform thin film on the ITO conductive glass and the conductive surface of the ITO conductive glass;
c. and c, carrying out heat treatment on the film formed by the transparent conductive substrate which is prepared in the step b and forms the uniform nano-particle film, carrying out heat treatment at 250 ℃ for 5min, and obtaining the NiO nano-particle-AZO nano-particle electrochromic film on the transparent conductive substrate.
The transmittance curve of the electrochromic film obtained in this example in the colored state and the discolored state is shown in fig. 2, and the optical modulation Δ T% at 550nm is 37%; the fading time of the electrochromic film was 7 s; after 1000 times of cyclic processing, the storage capacity of the thin film charge is reduced by only 9%.
EXAMPLE III
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this example, a method for preparing an electrochromic film, WO3The method for uniformly distributing the nano-particles and the ATO nano-particles in the electrochromic film comprises the following steps:
a. 4.8788g of WO3Dissolving nanoparticles, 0.9423g of ATO nanoparticles and 0.2910g of dispersing agent in 100mL of toluene, adding an epoxy resin polymer and a polyamide curing agent in a mass ratio of 2:1, pouring into a planetary rapid dispersion machine filled with zirconia balls with the diameter of 0.3mm, carrying out ball milling at a rotating speed of 10000r/min, and continuously dispersing for 13 hours to obtain a nanoparticle dispersion liquid which is used as a coating liquid of metal oxide and TCO for later use;
b. the ITO-PET film is adopted as a transparent conductive substrate, the transparent conductive substrate is pretreated, and the ITO-PET film with the surface resistance of 18 omega/□ is cut into 3 multiplied by 4cm2The size of the gas is put into an Ar Plasma workstation for processing, the set parameters are 20W and 60s, the Ar gas flow is 30sccm, and the pressure is 75 mTorr; coating the nano dispersion liquid prepared in the step a on an ITO-PET substrate by using a unfilled corner wheel coating preparation method, adjusting the rolling speed to be 0.5m/min, and forming a uniform film on the conductive surface of the ITO-PET;
c. performing a heat treatment on the thin film formed on the transparent conductive substrate formed with the uniform nanoparticle thin film prepared in the step b,heat treating at 80 deg.C for 5min to obtain WO on transparent conductive substrate3nanoparticle-ATO nanoparticle electrochromic films.
The electrochromic film obtained in the example had an optical modulation Δ T% at 630nm of 67%; the fading time of the electrochromic film was 9 s; after 1000 times of cyclic processing, the storage capacity of the thin film charge is reduced by 16%.
Example four
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this example, a method for preparing an electrochromic film, WO3The method for uniformly distributing the nano-particles and the ITO nano-particles in the large-area electrochromic film comprises the following steps:
a. 80.7620g of WO3Dissolving nanoparticles, 8.8798g of ITO nanoparticles and 4.4526g of dispersing agent in 1000mL of N-methylpyrrolidone, pouring the mixture into a planetary rapid dispersion machine filled with zirconia balls with the diameter of 0.3mm, carrying out ball milling at the rotating speed of 10000r/min, and continuously dispersing for 13 hours to obtain a nanoparticle dispersion liquid serving as a coating liquid of metal oxide and TCO for later use;
b. adopting ITO conductive glass as a transparent conductive substrate, pretreating the transparent conductive substrate, and cutting the ITO conductive glass with the surface resistance of 10 omega/□ into 60 x 80cm2The size of the gas is put into an Ar Plasma workstation for processing, the set parameters are 60W and 60s, the Ar gas flow is 30sccm, and the pressure is 75 mTorr; injecting the obtained nanoparticle dispersion liquid into a containing cavity containing coating liquid by adopting a slit extrusion coating method, and forming a uniform film on the conductive surface of the ITO conductive glass by using a slit extrusion coating machine;
c. performing heat treatment on the film formed on the transparent conductive substrate for forming the uniform nano-particle film prepared in the step b at 230 ℃ for 5min to obtain WO on the transparent conductive substrate3Nanoparticle-large area electrochromic films of ITO nanoparticles.
The large-area electrochromic film obtained in the embodiment has an optical modulation Delta T% at 630nm of 70%; the fading time of the electrochromic film was 50 s; after 1000 times of cycle processing, the storage capacity of the thin film charge is reduced by 18 percent.
Comparative example 1
This comparative example is substantially the same as the first example described above, with the particularity that:
in this comparative example, a method for producing an electrochromic film, WO3The method for uniformly distributing the nano particles in the electrochromic film comprises the following steps:
a. 6.1779g of WO3Dissolving nanoparticles and 0.3089g of dispersing agent in 70mL of ethanol, pouring into a planetary rapid dispersion machine filled with zirconia balls with the diameter of 0.3mm, carrying out ball milling at the rotating speed of 10000r/min, and continuously dispersing for 13h to obtain a nanoparticle dispersion liquid serving as a coating liquid of metal oxides for later use;
b. adopting ITO conductive glass as a transparent conductive substrate, pretreating the transparent conductive substrate, and cutting the ITO conductive glass with the surface resistance of 10 omega/□ into 3 multiplied by 4cm2The size of the gas is put into an Ar Plasma workstation for processing, the set parameters are 60W and 60s, the Ar gas flow is 30sccm, and the pressure is 75 mTorr; b, injecting the nano dispersion liquid prepared in the step a into a containing cavity containing coating liquid by adopting a slit extrusion coating method, and forming a uniform film on the conductive surface of the ITO conductive glass by using a slit extrusion coater;
c. performing heat treatment on the film formed on the transparent conductive substrate for forming the uniform nano-particle film prepared in the step b at 230 ℃ for 5min to obtain WO on the transparent conductive substrate3Nanoparticle electrochromic films.
The transmittance curves of the comparative electrochromic film obtained in the comparative example in the colored state and the faded state are shown in FIG. 1, and the optical modulation Δ T% at 630nm is 56%; the fading time of the electrochromic film was 20 s; after 1000 times of cycle processing, the storage capacity of the thin film charge is reduced by 62%.
Comparative example No. two
This comparative example is substantially the same as the second example described above, with the particularity that:
in this comparative example, a method for preparing an electrochromic film, in which NiO nanoparticles are uniformly distributed in an electrochromic film, includes the steps of:
a. 4.5660g of NiO nano-particles and 0.1178g of dispersing agent are dissolved in 100mL of toluene, poured into a planetary rapid dispersion machine with zirconia balls with the diameter of 0.3mm, ball-milled at the rotating speed of 10000r/min, and continuously dispersed for 15 hours to obtain nano-particle dispersion liquid which is used as coating liquid of metal oxide for later use;
b. adopting ITO conductive glass as a transparent conductive substrate, pretreating the transparent conductive substrate, and cutting the ITO conductive glass with the surface resistance of 10 omega/□ into 3 multiplied by 4cm2Drying after ultrasonic oscillation for 30min by using ethanol, acetone and water respectively; pouring the nano dispersion liquid prepared in the step a into an ink box of a gravure coater by adopting a micro-gravure coating preparation method, setting the rotating speed of a roller shaft to be 40rpm, adjusting the positions of a scraper and the micro-gravure roller shaft, and adjusting the angle and the compression degree of the scraper, so that the nano particle dispersion liquid is uniformly coated on the conductive surface of the ITO conductive glass to form a uniform film;
c. and c, carrying out heat treatment on the film formed by the transparent conductive substrate which is prepared in the step b and forms the uniform nano-particle film, and carrying out heat treatment at 250 ℃ for 5min to obtain the NiO nano-particle electrochromic film on the transparent conductive substrate.
The transmittance curves of the comparative electrochromic film obtained in the comparative example in the colored state and the faded state are shown in FIG. 2, and the optical modulation Δ T% at 550nm is 16%; the fading time of the electrochromic film was 18 s; after 1000 times of cycle processing, the storage capacity of the thin film charge is reduced by 55%.
In summary, in the embodiments of the present invention, the metal oxide nanoparticles and the TCO nanoparticles are used as the substrate to prepare the nanocomposite electrochromic film by the wet coating method, which has excellent coating performance and electrochromic performance, is suitable for large-area preparation of the electrochromic film, and is beneficial to large-scale industrial production. The porous nano structure in the electrochromic film has a larger specific surface area, so that ions can be conveniently embedded and removed, and the electrochromic performance of an electrochromic device is improved.
The embodiments of the present invention have been described above with reference to the drawings of the specification, but the present invention is not limited to the above embodiments, and various changes can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitution ways, so long as the invention is in accordance with the purpose of the present invention, and the invention shall fall within the protection scope of the present invention as long as the technical principle and the inventive concept of the method for preparing the electrochromic film of the present invention are not departed from the technical principle and the inventive concept.
Claims (11)
1. The preparation method of the electrochromic film is characterized by comprising the following steps of:
a. mixing metal oxide nano particles and transparent conductive oxide nano particles to prepare nano dispersion liquid serving as coating liquid of the metal oxide and the transparent conductive oxide for later use; the metal oxide is an electrochromic material;
b. after the transparent conductive substrate is pretreated, coating the nano dispersion liquid prepared in the step a on a conductive surface of the transparent conductive substrate by adopting a wet coating method to form a uniform nano particle thin layer;
c. performing heat treatment on the film formed on the transparent conductive substrate which is prepared in the step b and is used for forming the uniform nano-particle film, wherein the heat treatment temperature is 50-400 ℃, and the heat treatment time is 5-300 min; thereby obtaining the electrochromic film compounded by the nanometer film of the electrochromic metal oxide and the transparent conductive substrate.
2. The method for preparing an electrochromic film according to claim 1, characterized in that: in the step a, the nano dispersion liquid comprises 100 parts by weight of metal oxide nanoparticles, 0.1-1000 parts by weight of transparent conductive oxide nanoparticles, 0.01-1000 parts by weight of a dispersant, 100-20000 parts by weight of a solvent, 0-1000 parts by weight of a resin and 0-500 parts by weight of a curing agent.
3. The method for producing an electrochromic film according to claim 2, characterized in that: the metal oxide nano particles adopt any one nano material or any mixed nano material of nano particles, nano rods, nano wires, nano tubes and nano porous materials with electrochromic characteristics.
4. The method for producing an electrochromic film according to claim 2, characterized in that: the transparent conductive oxide nano particles are made of any one nano material or a mixture of any several nano materials of antimony-doped tin oxide, tin-doped indium oxide, gallium-doped zinc oxide, indium-doped gallium-doped zinc oxide and aluminum-doped zinc oxide.
5. The method for producing an electrochromic film according to claim 2, characterized in that: the solvent is any one or a mixture of any more of alcohol, ether, ketone, ester, aromatic hydrocarbon and water.
6. The method for producing an electrochromic film according to claim 2, characterized in that: the resin is any one or a mixture of any more of epoxy resin, polyamide resin and dicyandiamide.
7. The method for producing an electrochromic film according to claim 2, characterized in that: the curing agent is any one or a mixture of any more of toluene diisocyanate, isophorone diisocyanate and polyamide.
8. The method for preparing an electrochromic film according to claim 1, characterized in that: in the step b, the pretreatment mode is any one of Plasma treatment, physical cleaning, chemical cleaning, ultraviolet ozone treatment, heat treatment, corona discharge treatment and pressure treatment or a mode of carrying out mixed treatment on any plurality of materials.
9. The method for preparing an electrochromic film according to claim 1, characterized in that: in the step b, the wet coating method is any one of spin coating, roll coating, bar coating, casting, dip coating, knife coating, spray coating, flow coating, micro gravure coating, slit coating, lip film extrusion coating, nozzle coating, comma coating, capillary coating and screen printing, flexography, offset printing, reverse printing, inkjet printing or any mixture of a plurality of methods.
10. The method for preparing an electrochromic film according to claim 1, characterized in that: in the step b, the transparent conductive substrate is made of any one substrate of conductive glass of FTO, ITO, silver nanowires, graphene and conductive polymer films or a substrate of a conductive surface formed by any mixture of conductive materials based on conductive plastic films, sheets and plates of FTO, ITO, silver nanowires, graphene and conductive polymer films.
11. The method for preparing an electrochromic film according to claim 1, characterized in that: in the step c, electrochromic metal oxide nanoparticles and transparent conductive oxide nanoparticles with the average particle size of 1-5000 nm are adopted, and the thickness of a thin film layer with uniformly distributed nanoparticles is 50-2000 nm.
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| CN111477382A (en) * | 2020-04-17 | 2020-07-31 | 中国航发北京航空材料研究院 | Porous metal composite transparent conductive film and preparation method thereof |
| CN113655668A (en) * | 2021-08-25 | 2021-11-16 | 浙江理工大学绍兴柯桥研究院有限公司 | Planar flexible energy storage color change integrated device and preparation method thereof |
| EP4219649A1 (en) * | 2022-01-27 | 2023-08-02 | Friedrich-Alexander-Universität Erlangen-Nürnberg | Composition and method for forming an electrochromic layer |
| CN114721198B (en) * | 2022-04-21 | 2024-04-09 | 合肥工业大学 | Quick-response flexible NiOx@AgNWs electrochromic film and preparation method thereof |
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| CN105382268A (en) * | 2015-09-15 | 2016-03-09 | 海南大学 | Silver-doped vanadium pentoxide nanowire, preparing method of silver-doped vanadium pentoxide nanowire and preparing method of electrochromic device |
| CN105261423A (en) * | 2015-10-30 | 2016-01-20 | 中山大学 | Roll-to-roll preparation device and method for high-performance flexible transparent conductive film |
| CN106782769A (en) * | 2016-11-22 | 2017-05-31 | 华中科技大学 | Flexible and transparent conductive laminated film of low roughness low square resistance and preparation method thereof |
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