CN112965311B - Electrochromic film and preparation method thereof - Google Patents
Electrochromic film and preparation method thereof Download PDFInfo
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- CN112965311B CN112965311B CN202110147632.0A CN202110147632A CN112965311B CN 112965311 B CN112965311 B CN 112965311B CN 202110147632 A CN202110147632 A CN 202110147632A CN 112965311 B CN112965311 B CN 112965311B
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- -1 1-ethyl-3-methylimidazolium tetrafluoroborate Chemical compound 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- 239000002608 ionic liquid Substances 0.000 claims description 11
- 229920002799 BoPET Polymers 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
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- 238000013007 heat curing Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 4
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 4
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- MJSWUFPARNWKRE-UHFFFAOYSA-N B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC Chemical compound B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.B([O-])([O-])F.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC.C[N+]1=CN(C=C1)CC MJSWUFPARNWKRE-UHFFFAOYSA-N 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- KBLZDCFTQSIIOH-UHFFFAOYSA-M tetrabutylazanium;perchlorate Chemical compound [O-]Cl(=O)(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC KBLZDCFTQSIIOH-UHFFFAOYSA-M 0.000 claims description 3
- BMQZYMYBQZGEEY-UHFFFAOYSA-M 1-ethyl-3-methylimidazolium chloride Chemical compound [Cl-].CCN1C=C[N+](C)=C1 BMQZYMYBQZGEEY-UHFFFAOYSA-M 0.000 claims description 2
- LRESCJAINPKJTO-UHFFFAOYSA-N bis(trifluoromethylsulfonyl)azanide;1-ethyl-3-methylimidazol-3-ium Chemical compound CCN1C=C[N+](C)=C1.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F LRESCJAINPKJTO-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 5
- 238000004513 sizing Methods 0.000 claims 5
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- 230000008023 solidification Effects 0.000 claims 2
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- 238000002834 transmittance Methods 0.000 abstract description 7
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- FQERWQCDIIMLHB-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CC[NH+]1CN(C)C=C1 FQERWQCDIIMLHB-UHFFFAOYSA-N 0.000 description 1
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- 238000004134 energy conservation Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000002120 nanofilm Substances 0.000 description 1
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- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
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- 229920002635 polyurethane Polymers 0.000 description 1
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- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 230000007704 transition Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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Classifications
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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
- G02F1/15165—Polymers
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention discloses an electrochromic film and a preparation method thereof, and belongs to the technical field of optical film materials. The electrochromic film is composed of a composite material, wherein the composite material comprises thermosetting resin, electrochromic molecules and electrolyte; the thermosetting resin and the electrochromic molecules are dissolved in an organic solution; the electrolyte is dissolved in the thermosetting resin and the electrochromic molecule solution. According to the invention, the electrochromic molecules in the composite material have different driving voltages, and the prepared electrochromic film has different transmittances when different voltages are applied, and has the advantages of high stability, adjustable change depth, good weather resistance and the like. The core of the invention is that the traditional complex electrochromic production processes such as printing, evaporation and the like are changed, and the traditional coating process is used, so that the production cost is greatly reduced, and the yield is greatly improved.
Description
Technical Field
The invention relates to an electrochromic film and a preparation method thereof, belonging to the technical field of optical film materials.
Background
Electrochromic refers to a property in which the absorption or reflection spectrum of a material changes when an electric field is applied, and a substance having electrochromic characteristics is called an electrochromic material.
After the development of over ten years, the electrochromic material is widely applied, and plays an important role in military industry and daily life. In military field, one of the color change techniques in modern war is to use reversible color change material to make the color of the protected target surface change with the color of the background and mix with the background to achieve the purpose of visual invisibility. For example, if the surface of a barracks of the military is covered with a layer of electrochromic film material, the color of the barracks can be changed arbitrarily according to the requirement, so that the barracks have the same color as the surrounding environment.
The electrochromic material has wide application in daily life of people, and can be used in the fields of buildings, doors and windows of automobiles and airplanes and the like. People can change the color of the door and the window according to the needs, adjust the transmittance of the window glass of the door and the window, and achieve the aim of energy conservation; can also be used as controllable optical thin film materials such as a narrow visual angle conversion film of a liquid crystal display, an HDR light transmittance regulation film and the like.
At present, in the research of electrochromic materials at home and abroad, the research hot spots are mainly focused on the following materials.
The inorganic metal oxide is prepared with transition metal oxide and through transition of the metal ion in certain valence state to generate tungsten ion in high valence state and blue ion in low valence state. However, the material is difficult to realize the conversion of multiple colors, the response time of the electrochromism is long, and the color is changed due to the ionic charge after the material is used for a long time. Among them, WO is the most representative material3The accumulation of compensation ions in the electrochromic device degrades the color-changing performance.
Organic electrochromic materials such as polypyrrole, polythiophene, polyaniline, and the like. This kind of material is mainly used to change its color by the energy difference between its valence band and conduction band, so its color is limited by the electronic band of conducting molecule and it is unable to realize the switching of multiple colors. Moreover, the materials are difficult to realize the preparation of thin films and large areas.
In summary, electrochromic materials have a wide range of uses in the military and civilian fields. However, the existing electrochromic material has the defects that the service life and the color change can not be set arbitrarily. The defects greatly restrict the functions of the color-changing material in national defense construction and economy in China.
Disclosure of Invention
The invention aims to solve the problem that the electrochromic film can show different colors under different driving voltages by changing the driving voltage through the conductive ionic liquid, the electrolyte and the electrochromic molecule proportion, the electrochromic molecular film can be gradually changed from colorless to black under 1-20V, and the electrochromic film is realized by adopting the following technical scheme:
an electrochromic film is composed of a composite material and comprises the following components in parts by mass: 50.0% of a thermosetting resin, 0.1% of electrochromic molecules, 49.0% of an ionic liquid and 0.9% of an electrolyte;
the electrochromic molecules are as follows:
as a preferred example, the thermosetting resin and electrochromic molecules are dissolved in an ionic liquid solution; electrolyte is dissolved in the thermosetting resin and the electrochromic molecule solution, and the visible light transmittance range presented by applying a driving voltage of 1-20V to the electrochromic molecules in the composite material is 3-91%.
As a preferred example, the thermosetting resin is one of amino-modified acrylic thermosetting resin, epoxy-modified acrylic thermosetting resin, and urethane-modified acrylic thermosetting resin.
As a preferred example, the ionic liquid is one of 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium hexafluoroborate, 1-propyl-3-methylimidazolium tetrafluoroborate, and 1-ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide.
As a preferred example, the electrolyte is one of lithium perchlorate, lithium hexafluorophosphate, tetrabutylammonium perchlorate, tetrabutyllithium hexafluorophosphate.
As preferred examples, the organic solvent is: ethylene glycol monobutyl ether, dimethyl carbonate, ethyl acetate, butyl acetate, acetone, butanone and isophorone.
The preparation method of the electrochromic film comprises the following steps:
s1, preparation of a heat-curing coating: electrochromic molecules, ionic liquid and electrolyte are mixed according to the proportion of 0.1: 49: mixing according to the mass ratio of 0.9, adding thermosetting resin and slurry with the mass being 1 time that of the slurry into a mixed solution formed by a solvent, fully stirring until electrochromic molecules are completely dissolved, and the whole system becomes light yellow with the viscosity of 32-103 cp, and then sealing and storing to form a film;
s2, thermal curing: and (3) uniformly coating the thermosetting coating obtained in the step (S1) by using a wet coater, then putting the coating in an environment at 120 ℃ for thermal drying and curing for 120S, and obtaining the electrochromic film after thermal drying and curing.
As a preferred example, in S2, the specification of the wet coater is one of 5 μm, 10 μm, 15 μm, 20 μm, and 50 μm; the basic transparent film is an ITO-PET film.
The invention has the beneficial effects that: by regulating the weight ratio of electrochromic molecules to ionic liquid and electrolyte: the proportion of electrochromic molecules, thermosetting resin and electrolyte in the raw materials for preparing the composite material is as follows: (1) 50.0% of a thermosetting resin; (2) 49.0% of an ionic liquid; (3) 0.9% of an electrolyte; (4) 0.1% of electrochromic molecules. Uniformly mixing the electrochromic film with 2 times of organic solvent by mass, and thermally curing at 120 ℃ for 120S to obtain the electrochromic film, wherein the electrochromic proportion is the key for adjusting the magnitude of the driving voltage.
Drawings
FIG. 1 is a graph of 560nm transmittance spectra obtained with different driving voltages in the present invention;
fig. 2 is a sectional SEM image of the photochromic film according to the present invention.
It should be noted that: in fig. 2, the electrochromic film is divided into three regions, a left region, a middle region, and a right region, wherein the ITO-PET film is located in the left region and the right region, and the electrochromic layer is the middle region.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purpose and the efficacy of the invention easily understood, the invention is further described with reference to the following embodiments.
Example one
S1, preparation of a heat-curing coating: uniformly mixing 1-ethyl-3-methylimidazolium tetrafluoroborate, 0.1g of electrochromic molecules, 0.9g of lithium perchlorate electrolyte and 50.0g of polyurethane modified acrylic resin, adding the mixture into 200g of butanone, fully stirring until the system is completely and uniformly dissolved and the whole system becomes light yellow with 45cp viscosity, and then sealing and storing to form a film;
s2, coating: the heat-curable coating obtained in S1 was uniformly coated on the base transparent ITO-PET film by a wet coater (specification: 20 μm);
s3, thermal curing: and then, placing the film in an environment of 120 ℃ for 120S thermal drying and curing, and obtaining the electrochromic film with the driving voltage of 1-20V after curing.
Example two
S1, preparation of a heat-curing coating: uniformly mixing 1-ethyl-3-methylimidazolium hexafluoroborate, 0.1g of electrochromic molecules, 0.9g of tetrabutylammonium perchlorate electrolyte and 50.0g of epoxy modified acrylic resin, adding the mixture into 200g of dimethyl carbonate, fully stirring until the system is completely and uniformly dissolved, and the whole system becomes light yellow with the viscosity of 85cp, and is sealed and stored to form a film;
s2, coating: the heat-curable coating obtained in S1 was uniformly coated on the base transparent ITO-PET film by a wet coater (specification: 20 μm);
s3, thermal curing: and then, placing the film in an environment of 120 ℃ for 120S thermal drying and curing, and obtaining the electrochromic film with the driving voltage of 1-20V after curing.
EXAMPLE III
S1, preparation of a heat-curing coating: uniformly mixing 1-ethyl-3-methylimidazole chloride salt 49.0g, electrochromic molecules 0.1g, lithium hexafluorophosphate electrolyte 0.9g and amino modified acrylic resin 50.0g, adding the mixture into ethyl acetate 200g, fully stirring until the system is completely and uniformly dissolved, and the whole system becomes light yellow with the viscosity of 62cp, and then sealing and storing to form a film;
s2, coating: the heat-curable coating obtained in S1 was uniformly coated on the base transparent ITO-PET film using a wet coater (10 μm gauge);
s3, thermal curing: and then, placing the film in an environment of 120 ℃ for 120S thermal drying and curing, and obtaining the electrochromic film with the driving voltage of 1-20V after curing.
Example four
S1, preparation of a heat-curing coating: uniformly mixing 49.0g of 1-propyl-3-methylimidazolium tetrafluoroborate, 0.1g of electrochromic molecules, 0.9g of tetrabutylhexafluorophosphate electrolyte and 50.0g of epoxy modified acrylic resin, adding the mixture into 200g of ethylene glycol monobutyl ether, fully stirring until the system is completely and uniformly dissolved, and the whole system becomes light yellow with the viscosity of 103cp, and is sealed and stored to form a film;
s2, coating: coating on the base transparent film ITO-PET film using a wet coater (10 μm gauge);
s3, thermal curing: uniformly coating the prepared thermosetting coating on a basic transparent film by using a wet coater, then putting the basic transparent film into an environment of 120 ℃ for thermal drying and curing for 120 seconds, and curing to obtain the electrochromic film with the driving voltage of 1-20V.
EXAMPLE five
S1, preparation of a heat-curing coating: 1g of ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt, 0.1g of electrochromic molecules, 0.9g of hexafluorophosphoric acid, 50g of epoxy modified acrylic resin are mixed uniformly and then added into 200g of butyl acetate, the mixture is stirred fully until the system is dissolved uniformly and the whole system becomes light yellow with 32cp viscosity, and then the mixture is stored in a sealed manner to form a film;
s2, coating: the heat-curable coating obtained in S1 was uniformly coated on the base transparent ITO-PET film using a wet coater (50 μm gauge);
s3, thermal curing: uniformly coating the prepared thermosetting coating on a basic transparent film by using a wet coater, then putting the basic transparent film into an environment of 120 ℃ for thermal drying and curing for 120 seconds, and curing to obtain the electrochromic film with the driving voltage of 1-20V.
EXAMPLE six
S1, preparation of a heat-curing coating: uniformly mixing 1g of ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt, 0.1g of electrochromic molecules, 0.9g of lithium perchlorate electrolyte and 50.0g of amino modified acrylic resin, adding the mixture into 200g of isophorone, fully stirring until the system is completely and uniformly dissolved, and the whole system becomes light yellow with the viscosity of 43cp, and then sealing and storing the light yellow to form a film;
s2, coating: the heat-curable coating obtained in S1 was uniformly coated on the base transparent ITO-PET film using a wet coater (gauge: 20 μm);
s3, thermal curing: uniformly coating the prepared thermosetting coating on a basic transparent film by using a wet coater, then placing the film in an environment of 120 ℃ for 120S thermal drying and curing, and obtaining the electrochromic film with the driving voltage of 1-20V after curing.
EXAMPLE seven
S1, preparation of a heat-curing coating: uniformly mixing 1g of ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt, 0.1g of electrochromic molecules, 0.9g of lithium hexafluorophosphate electrolyte and 50.0g of amino modified acrylic resin, adding the mixture into 200g of acetone, fully stirring until the system is completely and uniformly dissolved, and the whole system becomes light yellow with the viscosity of 45cp, and then sealing and storing the light yellow to form a film;
s2, coating: the heat-curable coating obtained in S1 was uniformly coated on the base transparent ITO-PET film using a wet coater (gauge: 20 μm);
s3, thermal curing: and then, placing the film in an environment of 120 ℃ for 120S thermal drying and curing, and obtaining the electrochromic film with the driving voltage of 1-20V after curing.
To sum up, different visible light transmittance products were obtained according to the different driving voltages obtained in examples one to seven, as shown in table 1 below.
As can be seen from table 1, as the applied voltage increases, the transmittance at 560nm of visible light gradually decreases, and privacy protection can be increased according to the product requirements.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. An electrochromic film is characterized in that the raw materials comprise the following components in percentage by mass: 50.0% of thermosetting resin, 0.1% of electrochromic molecules, 49.0% of ionic liquid and 0.9% of electrolyte, and also an organic solvent with the mass fraction of 2 times of the total mass fraction of the thermosetting resin, the electrochromic molecules, the ionic liquid and the electrolyte;
the electrochromic molecules are as follows:
2. the electrochromic film according to claim 1, wherein the thermosetting resin is one of amino-modified acrylic thermosetting resin, epoxy-modified acrylic thermosetting resin, and urethane-modified acrylic thermosetting resin.
3. The electrochromic film according to claim 1, wherein said ionic liquid is one of 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium hexafluoroborate, 1-propyl-3-methylimidazolium tetrafluoroborate, and 1-ethyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide.
4. The electrochromic film of claim 1, wherein said electrolyte is one of lithium perchlorate, lithium hexafluorophosphate, tetrabutylammonium perchlorate, and tetrabutyllithium hexafluorophosphate.
5. The electrochromic film according to claim 1, wherein the organic solvent is: ethylene glycol monobutyl ether, dimethyl carbonate, ethyl acetate, butyl acetate, acetone, butanone and isophorone.
6. The method for preparing an electrochromic film according to any one of claims 1 to 5, comprising the steps of:
s1, preparation of a heat-curing coating: electrochromic molecules, ionic liquid and electrolyte are mixed according to the proportion of 0.1: 49: mixing the thermosetting resin and the sizing agent in a mass ratio of 0.9 to form sizing agent, adding the thermosetting resin and the sizing agent which are 1 time of the mass of the sizing agent into an organic solvent, fully stirring until the sizing agent and the thermosetting resin are completely dissolved in the organic solvent, and sealing and storing the whole system which is light yellow and has the viscosity of 32-103 cp to form a film;
s2, coating: uniformly coating the thermosetting coating obtained in the step S1 on a basic transparent ITO-PET film by using a wet coater;
s3, thermal curing: and then the film is placed in an environment with the temperature of 120 ℃ for thermal drying and solidification for 120S, and the electrochromic film can be obtained after the thermal drying and solidification.
7. The method for preparing an electrochromic film according to claim 6, wherein: in S2, the specification of the wet coater is one of 5 μm, 10 μm, 15 μm, 20 μm and 50 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110147632.0A CN112965311B (en) | 2021-02-03 | 2021-02-03 | Electrochromic film and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110147632.0A CN112965311B (en) | 2021-02-03 | 2021-02-03 | Electrochromic film and preparation method thereof |
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| CN112965311A CN112965311A (en) | 2021-06-15 |
| CN112965311B true CN112965311B (en) | 2022-07-19 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6203154B1 (en) * | 1997-12-19 | 2001-03-20 | Nippon Mitsubishi Oil Corporation | Electrochromic element |
| US6285486B1 (en) * | 1997-07-15 | 2001-09-04 | Nippon Oil Co., Ltd. | Electrochromic mirror and electrochromic devices |
| CN104610132A (en) * | 2014-11-26 | 2015-05-13 | 北京服装学院 | Viologen compound, and preparation method and application thereof |
| CN105579549A (en) * | 2013-09-17 | 2016-05-11 | 埃西勒国际通用光学公司 | Electrochromic composition |
| CN106371258A (en) * | 2016-10-21 | 2017-02-01 | 北京华逸高科科技有限公司 | Method for preparing electrochromic film and an electrochromic device |
| US9810962B1 (en) * | 2016-08-24 | 2017-11-07 | E-Chem Enterprise Corp. | Electrochromic material and anti-dazzle mirror having the same |
| CN108779113A (en) * | 2016-03-10 | 2018-11-09 | 佳能株式会社 | Organic compound, electrochromic device, electrochromic device, optical filter, image pick-up device, lens unit and window member |
| CN109557740A (en) * | 2018-12-21 | 2019-04-02 | 东华大学 | A kind of preparation method of purple Luo Jingji flexible color changing piece |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997035227A2 (en) * | 1996-03-15 | 1997-09-25 | Ecole Polytechnique Federale De Lausanne | Electrochromic or photoelectrochromic device |
| JP2005314377A (en) * | 2004-04-02 | 2005-11-10 | Fuji Photo Film Co Ltd | Method for producing bipyridinium compound |
| KR101735570B1 (en) * | 2010-03-26 | 2017-05-15 | 삼성전자주식회사 | Electrochromic material and electrochromic device including the same |
| CN101852960A (en) * | 2010-05-14 | 2010-10-06 | 马鞍山市盛宁高分子材料科技有限公司 | Full-solid state macromolecule controllable electrochromism flexible film device and manufacturing method thereof |
-
2021
- 2021-02-03 CN CN202110147632.0A patent/CN112965311B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6285486B1 (en) * | 1997-07-15 | 2001-09-04 | Nippon Oil Co., Ltd. | Electrochromic mirror and electrochromic devices |
| US6203154B1 (en) * | 1997-12-19 | 2001-03-20 | Nippon Mitsubishi Oil Corporation | Electrochromic element |
| CN105579549A (en) * | 2013-09-17 | 2016-05-11 | 埃西勒国际通用光学公司 | Electrochromic composition |
| CN104610132A (en) * | 2014-11-26 | 2015-05-13 | 北京服装学院 | Viologen compound, and preparation method and application thereof |
| CN108779113A (en) * | 2016-03-10 | 2018-11-09 | 佳能株式会社 | Organic compound, electrochromic device, electrochromic device, optical filter, image pick-up device, lens unit and window member |
| US9810962B1 (en) * | 2016-08-24 | 2017-11-07 | E-Chem Enterprise Corp. | Electrochromic material and anti-dazzle mirror having the same |
| CN106371258A (en) * | 2016-10-21 | 2017-02-01 | 北京华逸高科科技有限公司 | Method for preparing electrochromic film and an electrochromic device |
| CN109557740A (en) * | 2018-12-21 | 2019-04-02 | 东华大学 | A kind of preparation method of purple Luo Jingji flexible color changing piece |
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Denomination of invention: A electrochromic thin film and its preparation method Granted publication date: 20220719 Pledgee: The Bank of Shanghai branch Caohejing Limited by Share Ltd. Pledgor: CHANGDI NEW MATERIAL TECHNOLOGY (SHANGHAI) CO.,LTD. Registration number: Y2024980007123 |