CN116413965A - Laminated electrochromic glass based on PVB film and preparation method thereof - Google Patents
Laminated electrochromic glass based on PVB film and preparation method thereof Download PDFInfo
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- CN116413965A CN116413965A CN202210007681.9A CN202210007681A CN116413965A CN 116413965 A CN116413965 A CN 116413965A CN 202210007681 A CN202210007681 A CN 202210007681A CN 116413965 A CN116413965 A CN 116413965A
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- electrochromic
- laminated
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- gel
- glass
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- 239000011521 glass Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 6
- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002608 ionic liquid Substances 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- UYWQUFXKFGHYNT-UHFFFAOYSA-N Benzylformate Chemical compound O=COCC1=CC=CC=C1 UYWQUFXKFGHYNT-UHFFFAOYSA-N 0.000 claims description 4
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 claims description 4
- 229920000620 organic polymer Polymers 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229960002903 benzyl benzoate Drugs 0.000 claims description 3
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 3
- 229940093499 ethyl acetate Drugs 0.000 claims description 2
- 150000002460 imidazoles Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229940095102 methyl benzoate Drugs 0.000 claims description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical class N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920000123 polythiophene Polymers 0.000 claims description 2
- FHCPAXDKURNIOZ-UHFFFAOYSA-N tetrathiafulvalene Chemical compound S1C=CSC1=C1SC=CS1 FHCPAXDKURNIOZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005340 laminated glass Substances 0.000 abstract description 9
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 2
- TYOCDPIZUIQUSO-UHFFFAOYSA-N 1-butyl-2,3-dimethyl-2h-imidazole Chemical compound CCCCN1C=CN(C)C1C TYOCDPIZUIQUSO-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ANRHNWWPFJCPAZ-UHFFFAOYSA-M thionine Chemical compound [Cl-].C1=CC(N)=CC2=[S+]C3=CC(N)=CC=C3N=C21 ANRHNWWPFJCPAZ-UHFFFAOYSA-M 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- KYMNSBSWJPFUJH-UHFFFAOYSA-N iron;5-methylcyclopenta-1,3-diene;methylcyclopentane Chemical group [Fe].C[C-]1C=CC=C1.C[C-]1[CH-][CH-][CH-][CH-]1 KYMNSBSWJPFUJH-UHFFFAOYSA-N 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
- G02F1/153—Constructional details
- G02F1/1533—Constructional details structural features not otherwise provided for
Landscapes
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Joining Of Glass To Other Materials (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention provides a laminated electrochromic glass based on PVB film and a preparation method thereof, wherein the method comprises the following steps: (1) Coating electrochromic gel on the surface of the substrate, and performing heat treatment to obtain an electrochromic layer; (2) Covering the electrochromic layer obtained in the step (1) with another substrate to obtain a sandwich structure; (3) And (3) carrying out hot pressing (vacuum or normal pressure environment) on the sandwich structure obtained in the step (2) at a certain temperature to obtain the laminated electrochromic glass based on the PVB film. The color-changing laminated glass prepared by the preparation method is high in transparency, high in safety coefficient, simple in preparation process and environment-friendly.
Description
Technical Field
The invention belongs to the field of device structures, relates to a preparation method of laminated electrochromic glass, and particularly relates to a preparation method of a color-changing laminated glass based on an organic electrochromic material.
Background
The electrochromic device has the advantages of low working voltage, multistability, static state without power consumption, continuously adjustable transmittance, long service life and low cost, and is widely applied to the fields of dimming glass, displays and automobile rearview mirrors. Electrochromic devices currently being fabricated mainly employ electrochromic devices based on liquid electrolytes. This approach to preparation typically employs high-risk lithium perchlorate as the electrolyte, resulting in poor device safety and possibly even risk of leakage. The other is a semi-solid electrochromic device using a gel electrolyte, which has high safety but poor stability.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the laminated electrochromic glass based on the PVB film and the preparation method thereof, and the color-changing laminated glass prepared by the preparation method has high transparency, high safety coefficient, simple preparation process and environmental protection.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a PVB film-based laminated electrochromic glass and a preparation method thereof, and is characterized in that the method comprises the following steps:
(1) Coating electrochromic gel on the surface of the substrate, and performing heat treatment to obtain an electrochromic layer;
(2) Covering the electrochromic layer obtained in the step (1) with another substrate to obtain a sandwich structure;
(3) And (3) carrying out hot pressing (vacuum or normal pressure environment) on the sandwich structure obtained in the step (2) at a certain temperature to obtain the laminated electrochromic glass based on the PVB film.
Wherein the electrochromic gel comprises an organic electrochromic material, an ionic liquid, an ion pair, an organic polymer and an organic solvent.
2. The preparation method according to claim 1, wherein the electrochromic material in the electrochromic gel in step (1) comprises any one or more of polythiophenes and derivatives thereof, viologens, tetrathiafulvalene and metal phthalocyanine compounds.
3. The preparation method according to claim 1, wherein the ionic liquid in the electrochromic gel in step (1) comprises any one or more of imidazoles and derivatives thereof. The ion pair comprises any one or more of ferrocene and derivatives thereof.
4. The method of claim 1, wherein the organic polymer in the electrochromic gel of step (1) is PVB (polyvinyl butyral Ding Quanzhi).
5. The method of claim 1, wherein the organic solvent in the electrochromic gel of step (1) comprises any one or two of ethyl acetate, benzyl benzoate, methyl benzoate, or benzyl formate.
6. The method of claim 1, wherein the substrate in step (1) comprises any one or more of various types of glass substrates, coated glass, organic glass substrates, or polymeric substrates.
7. The method of claim 1, wherein the additional substrate in step (2) comprises any one or more of various glass substrates, coated glass, organic glass substrates, or polymeric substrates.
8. The method of any one of claims 1-7, wherein the annealing treatment in step (1) is performed at a temperature of 60-150 ℃;
preferably, the annealing treatment in the step (1) is performed for 5-15 min.
9. The method according to any one of claims 1 to 8, wherein the concentration of the lower electrochromic gel in step (1) is 0.1 to 2.5mol/L
Preferably, the electrochromic gel of step (1) has a thickness of 1 μm to 10mm;
10. the method of any one of claims 1-9, wherein the hot pressing temperature in step (3) is 80-180 ℃;
preferably, the lower hot pressing time in the step (3) is 5-30 min;
preferably, the pressure of the lower hot pressing in the step (3) is 0.1-1 MPa.
11. The method of any one of claims 1-10, wherein the laminated electrochromic glazing of step (3) is characterized by a color change material integrated with the laminated.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) The invention provides a laminated electrochromic glass based on PVB film and a preparation method thereof, wherein the laminated glass device prepared by the laminated electrochromic glass has a sandwich structure, and the inside of the sandwich structure is isolated from water and oxygen;
(2) The invention provides a laminated electrochromic glass based on PVB film and a preparation method thereof, wherein the middle of a laminated glass device prepared by the laminated electrochromic glass is made of polymer materials, broken glass cannot be generated after the device is broken, and personal safety is protected;
(3) The invention provides a PVB film-based laminated electrochromic glass and a preparation method thereof, wherein the transparent color-changing laminated glass prepared by the preparation method has average transmittance of more than 80% in the wavelength range of 400-780 nm.
Drawings
FIG. 1 is a schematic view of the structure of an optical waveguide laminated glass with a down-converting material according to the present invention
In the figure: 1-a substrate, 2-a color changing gel layer.
Fig. 2 is a color fading physical diagram of the laminated electrochromic glass provided by the invention
FIG. 3 is a colored physical image of the laminated electrochromic glass provided by the invention
The present invention will be described in further detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The present example provides a laminated electrochromic glass based on PVB film and a method for preparing the same, the method comprising:
(1) Coating a color-changing gel (the color-changing material is bis (trifluoromethylsulfonyl) imide heptyl purple cyanine, the ionic liquid is 1-butyl-3-methyl-methylimidazole bis (trifluoromethylsulfonyl) imide, the ion pair is dimethylferrocene, and the solvent is ethyl acetate), and annealing at 80 ℃ for 10min to obtain a color-changing film;
(2) And (3) covering the electrochromic layer obtained in the step (1) with another substrate to obtain a sandwich structure.
(3) And (3) carrying out hot pressing on the sandwich laminated glass obtained in the step (2) at 100 ℃ under the pressure of 1Mpa for 60min to obtain the laminated electrochromic glass of the PVB film.
Example 2
The present example provides a laminated electrochromic glass based on PVB film and a method for preparing the same, the method comprising:
(1) Coating a color-changing gel (the color-changing material is bis (trifluoromethylsulfonyl) imide heptyl purple cyanine, the ionic liquid is 1-butyl-3-methyl-methylimidazole bis (trifluoromethylsulfonyl) imide, the ion pair is ferrocene, and the solvent is benzyl benzoate), and annealing at 150 ℃ for 10min to obtain a color-changing film;
(2) And (3) covering the electrochromic layer obtained in the step (1) with another substrate to obtain a sandwich structure.
(3) And (3) carrying out hot pressing on the sandwich laminated glass obtained in the step (2) for 30min at 150 ℃ under the pressure of 1Mpa to obtain the laminated electrochromic glass of the PVB film.
Claims (11)
1. A laminated electrochromic glass based on a PVB film and a preparation method thereof, wherein the method comprises the following steps:
(1) Coating electrochromic gel on the surface of the substrate, and performing heat treatment to obtain an electrochromic layer;
(2) Covering the electrochromic layer obtained in the step (1) with another substrate to obtain a sandwich structure;
(3) And (3) carrying out hot pressing (vacuum or normal pressure environment) on the sandwich structure obtained in the step (2) at a certain temperature to obtain the laminated electrochromic glass based on the PVB film.
Wherein the electrochromic gel comprises an organic electrochromic material, an ionic liquid, an ion pair, an organic polymer and an organic solvent.
2. The preparation method according to claim 1, wherein the electrochromic material in the electrochromic gel in step (1) comprises any one or more of polythiophenes and derivatives thereof, viologens, tetrathiafulvalene and metal phthalocyanine compounds.
3. The preparation method according to claim 1, wherein the ionic liquid in the electrochromic gel in step (1) comprises any one or more of imidazoles and derivatives thereof. The ion pair comprises any one or more of ferrocene and derivatives thereof.
4. The method of claim 1, wherein the organic polymer in the electrochromic gel of step (1) is PVB (polyvinyl butyral Ding Quanzhi).
5. The method of claim 1, wherein the organic solvent in the electrochromic gel of step (1) comprises any one or two of ethyl acetate, benzyl benzoate, methyl benzoate, or benzyl formate.
6. The method of claim 1, wherein the substrate in step (1) comprises any one or more of various types of glass substrates, coated glass, organic glass substrates, or polymeric substrates.
7. The method of claim 1, wherein the additional substrate in step (2) comprises any one or more of various glass substrates, coated glass, organic glass substrates, or polymeric substrates.
8. The method of any one of claims 1-7, wherein the annealing treatment in step (1) is performed at a temperature of 60-150 ℃; preferably, the annealing treatment in the step (1) is performed for 5-15 min.
9. The method according to any one of claims 1 to 8, wherein the concentration of the lower electrochromic gel in step (1) is 0.1 to 2.5mol/L
Preferably, the electrochromic gel of step (1) has a thickness of 1 μm to 10mm.
10. The method of any one of claims 1-9, wherein the hot pressing temperature in step (3) is 80-180 ℃;
preferably, the lower hot pressing time in the step (3) is 5-30 min;
preferably, the pressure of the lower hot pressing in the step (3) is 0.1-1 MPa.
11. The method of any one of claims 1-10, wherein the laminated electrochromic glazing of step (3) is characterized by a color change material integrated with the laminated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210007681.9A CN116413965A (en) | 2022-01-05 | 2022-01-05 | Laminated electrochromic glass based on PVB film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210007681.9A CN116413965A (en) | 2022-01-05 | 2022-01-05 | Laminated electrochromic glass based on PVB film and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116413965A true CN116413965A (en) | 2023-07-11 |
Family
ID=87052030
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210007681.9A Pending CN116413965A (en) | 2022-01-05 | 2022-01-05 | Laminated electrochromic glass based on PVB film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116413965A (en) |
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2022
- 2022-01-05 CN CN202210007681.9A patent/CN116413965A/en active Pending
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