CN116931329A - Electrochromic device - Google Patents
Electrochromic device Download PDFInfo
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- CN116931329A CN116931329A CN202210337709.5A CN202210337709A CN116931329A CN 116931329 A CN116931329 A CN 116931329A CN 202210337709 A CN202210337709 A CN 202210337709A CN 116931329 A CN116931329 A CN 116931329A
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- Prior art keywords
- layer
- electrochromic
- porous
- electrochromic device
- ion conducting
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- 229920000642 polymer Polymers 0.000 claims abstract description 43
- 238000003860 storage Methods 0.000 claims abstract description 41
- 239000011244 liquid electrolyte Substances 0.000 claims abstract description 33
- 239000011148 porous material Substances 0.000 claims abstract description 16
- 150000002500 ions Chemical class 0.000 claims description 73
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- 239000000758 substrate Substances 0.000 claims description 25
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- 230000000996 additive effect Effects 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 6
- 229910003002 lithium salt Inorganic materials 0.000 claims description 6
- 159000000002 lithium salts Chemical class 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 6
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 6
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims description 5
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 5
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 5
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 5
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- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 239000000565 sealant Substances 0.000 claims description 4
- AVBJHQDHVYGQLS-AWEZNQCLSA-N (2s)-2-(dodecanoylamino)pentanedioic acid Chemical compound CCCCCCCCCCCC(=O)N[C@H](C(O)=O)CCC(O)=O AVBJHQDHVYGQLS-AWEZNQCLSA-N 0.000 claims description 3
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 claims description 3
- FHMRWRBNAIDRAP-UHFFFAOYSA-N 5,7-dibromo-2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=C(Br)SC(Br)=C21 FHMRWRBNAIDRAP-UHFFFAOYSA-N 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 235000003704 aspartic acid Nutrition 0.000 claims description 3
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- ILRSCQWREDREME-UHFFFAOYSA-N dodecanamide Chemical compound CCCCCCCCCCCC(N)=O ILRSCQWREDREME-UHFFFAOYSA-N 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 claims description 3
- 229910001416 lithium ion Inorganic materials 0.000 claims description 3
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims description 3
- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 claims description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 3
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 3
- 229920000767 polyaniline Polymers 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229920000128 polypyrrole Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229960003351 prussian blue Drugs 0.000 claims description 3
- 239000013225 prussian blue Substances 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910001887 tin oxide Inorganic materials 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
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- 238000001723 curing Methods 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 4
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- GIVZWHXTULQQAZ-UHFFFAOYSA-N 3,4-bis(2-ethylhexoxy)thiophene Chemical compound CCCCC(CC)COC1=CSC=C1OCC(CC)CCCC GIVZWHXTULQQAZ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 238000009413 insulation Methods 0.000 description 2
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 2
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- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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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
- G02F1/153—Constructional details
-
- 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
Landscapes
- 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 application provides an electrochromic device, wherein a porous ion conducting layer is arranged between an electrochromic layer and an ion storage layer, the porous ion conducting layer is soaked by liquid electrolyte, the porous ion conducting layer is a porous polymer layer, the porosity of the porous polymer layer is 20% -60%, and the average pore size of the porous polymer layer is more than 0nm and less than 1000nm. The electrochromic device has the advantages that the structure of the electrochromic device is changed due to the porous ion conducting layer, the liquid leakage rate is greatly reduced, and the mass production of liquid-based electrochromic devices is facilitated.
Description
Technical Field
The present application relates to an electrochromic device.
Background
Electrochromic (eletrochromic) refers to a material that can undergo a redox reaction and is highly reversible when a voltage is applied, thereby causing a reversible change in its optical properties (reflection or absorption) in the visible wavelength range, and thus exhibiting a characteristic that the color of the material changes reversibly with an applied voltage. Therefore, electrochromic materials are paid attention to different fields, and mainly comprise an energy-saving intelligent window for buildings, an intelligent dimming skylight for automobiles, a rearview mirror, a rear shell of a smart phone and the like. A typical electrochromic device is a stacked structure consisting of a transparent conductive layer-an electrochromic layer-an ion conducting layer-an ion storage layer-a transparent conductive layer. The ion conducting layer is of vital importance, has the performances of electronic insulation and ion conduction, and plays a role in compensating charge imbalance in the electrochromic process, so that the running stability of the device is ensured. The electrolyte in the ion conductive layer is classified into a solid electrolyte, a gel electrolyte and a liquid electrolyte. The solid electrolyte has high stability after encapsulation, but has higher processing cost, low ionic conductivity and poor interface compatibility; the gel electrolyte can effectively solve the problem of poor ion conductivity in the solid electrolyte, but has the problems of high purity requirement on raw materials in the preparation process, difficult control of large-area uniformity, low color change response speed and the like. However, the liquid electrolyte has the advantages of complete dissociation, small viscosity and high ion transfer speed, and can obviously enhance the response speed and the preparation cost of the electrochromic device, but the traditional liquid device structure has the defects of easy liquid leakage and adverse mass production of liquid-based electrochromic devices.
Disclosure of Invention
In view of the above, the application provides an electrochromic device, wherein the electrolyte in the ion conducting layer is liquid electrolyte, the structure of the electrochromic device is changed, the liquid leakage rate is greatly reduced, and the preparation process is simple, thereby being beneficial to the mass production of liquid-based electrochromic devices.
The application provides an electrochromic device, wherein a porous ion conducting layer is arranged between an electrochromic layer and an ion storage layer, the porous ion conducting layer is soaked by liquid electrolyte, the porous ion conducting layer is a porous polymer layer, the porosity of the porous polymer layer is 20% -60%, and the average pore diameter of the porous polymer layer is more than 0nm and less than 1000nm.
Through a great deal of experiments, the inventor of the application discovers that when the pore size is in the nanometer level, the pore has capillary force to further fix the liquid electrolyte; further has a limiting effect on the fluidity of the liquid, the porosity is 20% -60%, the electrolyte can be adsorbed and fixed, and the requirement of the electrochromic device on ion conductivity can be met, compared with the prior art, the usage amount of the electrolyte is reduced (as low as 0.5mg/cm 2 -1.6mg/cm 2 ) The liquid leakage phenomenon of the liquid-state base electrochromic device is greatly reduced.
Optionally, the porous polymer layer is one of a polyethylene film, a polypropylene film, a polyvinylidene fluoride film, a polyimide film and a polyaramid film. The preparation methods of the polyethylene film, the polypropylene film, the polyvinylidene fluoride film, the polyimide film and the polyaramid film are mature, and can be commercially available polymer films meeting the requirements of the porosity and the average pore diameter, and can also be prepared by themselves, and the preparation methods are well known in the art and are not repeated herein. The electrochromic device prepared by the method is simple in preparation method, suitable for large-scale industrial production, greatly reduced in cost and suitable for commercial popularization because the porous polymer layer can be a commercially available polymer film.
Optionally, the porous ion conducting layer area is greater than 0.1% -30% of the electrochromic layer or ion storage layer area.
Optionally, sealant is arranged around the electrochromic layer, the porous ion conducting layer and the ion storage layer.
Optionally, the porous ion conducting layer has a thickness of 2um to 25um.
Optionally, the electrochromic layer comprises a transparent substrate, a conductive layer, an electrochromic layer, an ion conducting layer, an ion storage layer, a conductive layer and a transparent substrate from top to bottom.
Optionally, the transparent substrate is one or more of glass, polyethylene terephthalate, polycarbonate and polymethyl methacrylate; the conductive layer is one or more of indium tin oxide, antimony doped with tin oxide, zinc oxide and zinc doped with aluminum, and the electrochromic layer is one or more of poly (3, 4-ethylenedioxythiophene), poly (2, 5-dibromo-3, 4-ethylenedioxythiophene), poly (3, 4-bis (2-ethylhexyloxy) thiophene), polyaniline, polypyrrole, 1' -dimethyl-4, 4' -bipyridine, di- (2-phosphonoethyl) -4,4' -bipyridine, tungsten oxide, molybdenum oxide and titanium oxide; the ion storage layer is one or more of nickel oxide, niobium pentoxide, vanadium pentoxide, prussian blue and cerium oxide.
Optionally, the liquid electrolyte contains lithium salt, a solvent and an additive, wherein the lithium salt is one or more of lithium bis (trifluoromethanesulfonyl) imide, lithium trifluoromethanesulfonate, lithium perchlorate, lithium tetrafluoroborate and lithium hexafluorophosphate, the solvent is one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, 1, 2-dimethoxyethane, N-dimethylformamide and water, and the additive is one or more of vinylene carbonate, fluoroethylene carbonate, polyethylene glycol, polyvinyl alcohol, ethylene glycol, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, N-lauroyl glutamic acid and N-lauroyl amid aspartic acid.
Optionally, the liquid electrolyte contains: the concentration of the lithium ions is 0.8mol/L-63mol/L, the additive is 1wt% -30wt% and the balance is solvent.
Drawings
Fig. 1 is a schematic structural view of the present application.
The reference numerals are explained as follows: 1-a porous ion conducting layer; 2-electrochromic layer; a 3-ion conducting layer; 4-a conductive layer; a 5-transparent substrate; and 6, packaging glue.
Detailed Description
The technical scheme of the application is described in detail below with reference to the accompanying drawings.
The embodiment of the application provides an electrochromic device, wherein a porous ion conducting layer is arranged between an electrochromic layer and an ion storage layer, the porous ion conducting layer is soaked by liquid electrolyte, the porous ion conducting layer is a porous polymer layer, the porosity of the porous polymer layer is 20% -60%, and the average pore diameter of the porous polymer layer is larger than 0nm and smaller than 1000nm. The porous ion conducting layer separates the electrochromic layer from the ion storage layer, and preferably the porous ion conducting layer has an area that is 0.1% -30% greater than the area of the electrochromic layer or ion storage layer, such that the porous ion conducting layer completely separates the electrochromic layer from the ion storage layer.
In some embodiments, the electrochromic layer 2, the porous ion conducting layer 1 and the ion storage layer 3 are provided with a sealant 6 around, so that the functional layers are assembled into a whole and are used for sealing liquid electrolyte from leakage of the electrolyte.
As shown in fig. 1, the electrochromic layer sequentially comprises a transparent substrate 5, a conductive layer 4, an electrochromic layer 2, a porous ion conductive layer 1, an ion storage layer 3, a conductive layer 4 and a transparent substrate 5 from top to bottom.
In order to make the technical problems, technical schemes and beneficial effects solved by the application more clear, the application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The transparent base 5 may be a base material commonly used in electrochromic devices, and may be any base material that has good light transmittance, good insulation, and easy formation of an electrode on the surface of a substrate. For example, it may be one or more of glass, polyethylene terephthalate (PET), polycarbonate (PC), and polymethyl methacrylate (PMMA).
As a specific embodiment, the transparent substrate is polyethylene terephthalate and is a polymer, the substrate is an electrochromic device formed by the material flexibly, the transparent substrate has impact resistance and is not easy to break, and the porous ion conducting layer is spongy, so that the stress can be better released, the situation of pollution caused by leakage of liquid electrolyte can not occur, and the transparent substrate has good stability.
The conductive layer is made of various conductive materials, such as metal, metal alloy or metal oxide, preferably metal oxide. As a specific embodiment, the metal oxide may be one or more of Indium Tin Oxide (ITO), tin oxide doped antimony, zinc oxide doped aluminum; preferably, the first transparent conductive layer and the second transparent conductive layer are made of Indium Tin Oxide (ITO) material. The transparent conductive layer can be formed on the surface of the transparent substrate by one of physical vapor deposition, vacuum evaporation, chemical vapor deposition, coating or electroplating; preferably, the transparent conductive layer is made of ITO and is formed by physical vapor deposition.
The liquid electrolyte contains lithium salt, a solvent and an additive, wherein the lithium salt is one or more of lithium bis (trifluoromethanesulfonyl) imide, lithium trifluoromethanesulfonate, lithium perchlorate, lithium tetrafluoroborate and lithium hexafluorophosphate, the solvent is one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methylethyl carbonate, 1, 2-dimethoxyethane, N-dimethylformamide and water, and the additive is one or more of vinylene carbonate, fluoroethylene carbonate, polyethylene glycol, polyvinyl alcohol, ethylene glycol, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, N-lauroyl glutamic acid and N-lauroyl amide aspartic acid.
The liquid electrolyte contains: the concentration of the lithium ions is 0.8mol/L-63mol/L, the additive is 1wt% -30wt% and the balance is solvent.
The electrochromic layer is one or more of poly 3, 4-ethylenedioxythiophene, poly 2, 5-dibromo-3, 4-ethylenedioxythiophene, poly 3, 4-bis (2-ethylhexyl oxy) thiophene, polyaniline, polypyrrole, 1' -dimethyl-4, 4' -bipyridine, di- (2-phosphonoethyl) -4,4' -bipyridine, tungsten oxide, molybdenum oxide and titanium oxide; preferably, the electrochromic layer is made of poly 3, 4-ethylenedioxythiophene.
The electrochromic device provided by the application adopts a sandwich structure, the transparent state transmittance at 650nm can reach more than 70%, the transparent state transmittance and the coloring state transmittance can reach about 35%, and the electrochromic device has wide application prospects in the fields of automobile components such as glass, skylights, electrochromic windows and the like.
The application also provides a preparation method of the electrochromic device, which comprises the following steps:
s1, preparing a component with an electrochromic layer and a component with an ion storage layer, and placing a porous polymer layer between the electrochromic layer and the ion storage layer;
s2, dripping a proper amount of prepared liquid electrolyte onto the porous polymer layer to enable the porous polymer layer to be completely infiltrated;
s3, sealing the periphery of the electrochromic device by using packaging glue, and thus the electrochromic device can be assembled.
Optionally, the component with the electrochromic layer is a component with an electrochromic layer obtained by sequentially arranging a conductive layer and an electrochromic layer on a transparent substrate, where the transparent substrate, the conductive layer and the electrochromic layer are transparent substrates, conductive layers and electrochromic layers commonly used in the art, and are not described herein. The component with the ion storage layer is a component with the ion storage layer, which is obtained by sequentially arranging a conductive layer and an ion storage layer on a transparent substrate, wherein the transparent substrate, the conductive layer and the ion storage layer are common transparent substrates, conductive layers and ion storage layers in the field, and the details are not repeated here.
Optionally, the porous polymer is surface treated for 5-10 seconds with nitrogen purge to the porous polymer surface to allow good interfacial compatibility with the liquid electrolyte used.
The ion storage layer is one or more of nickel oxide, niobium pentoxide, vanadium pentoxide, prussian blue and cerium oxide, and has good ion storage performance.
According to the preparation method provided by the application, in the step S3, the material of the encapsulation adhesive can be selected from adhesive materials such as epoxy resin or UV curing adhesive.
Hereinafter, the electrochromic device of the present application will be described in detail with reference to specific examples.
Example 1:
two pieces of transparent substrate PET were cut out, the transparent substrate being 12cm long and 10cm wide. Performing physical vapor deposition on one of the conductive layers, namely ITO and silk-screen electrochromic layer poly-3, 4-ethylenedioxythiophene to obtain a component with an electrochromic layer;
the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a porous polymer polyethylene film with the thickness of 9um to a length of 12.2cm and a width of 10.2cm, fixing the film on a clamp, and using N 2 Air purging for 5s, wherein the porosity of the air purging is 25%, and the average pore size of the porous polymer layer is 20nm;
s2, the prepared liquid electrolyte is used in an amount of 0.5mg/c per unit aream 2 Dripping the porous polymer layer to make the porous polymer layer completely soaked;
s3, sealing the periphery of the electrochromic device by using ultraviolet curing glue of the packaging glue, and curing by ultraviolet light to obtain the electrochromic device;
the liquid electrolyte composition: the concentration of lithium perchlorate is 1mol/L, the content of vinylene carbonate as an additive is 1wt%, and propylene carbonate organic solvent is used as a solvent to obtain 1L of liquid electrolyte.
Example 2
200 electrochromic devices were prepared according to the method of example 1. After the high-temperature high-humidity test for 192 hours at the temperature of 85 ℃ and the humidity of 85%, no liquid leakage phenomenon is found in the sample.
Example 3:
the difference from example 1 is that:
the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a porous polymer polypropylene film to a length of 12.8cm and a width of 10.8cm, fixing the film on a clamp, and using N 2 Air purging for 5s, wherein the porosity of the air purging is 35%, and the average pore size of the porous polymer layer is 100nm;
s2, the prepared liquid electrolyte has a capacity of 0.8mg/cm per unit area 2 Drop-wise addition to the porous polymer layer is carried out so that it is completely impregnated.
Example 4:
the difference from example 1 is that:
the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a porous polymer polypropylene film to a length of 13cm and a width of 12cm, fixing the film on a clamp, and using N 2 Air purging for 5s, wherein the porosity of the air purging is 45%, and the average pore size of the porous polymer layer is 250nm;
s2, the prepared liquid electrolyte has a capacity of 1.0mg/cm per unit area 2 Dripping onto the porous polymer layer to makeIt is completely infiltrated.
Example 5:
the difference from example 1 is that:
the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a porous polymer polyaramid film to a length of 14cm and a width of 13cm, fixing the film on a clamp, and using N 2 A gas sweep for 5 seconds, the porosity of which is 50%, the average pore size of the porous polymer layer being 500nm;
s2, the prepared liquid electrolyte has a capacity of 1.2mg/cm per unit area 2 Drop-wise addition to the porous polymer layer is carried out so that it is completely impregnated.
Example 6:
the difference from example 1 is that:
the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a polyethylene film with a thickness of 20um with multiple holes to a length of 14cm and a width of 13cm, fixing the polyethylene film on a fixture, and using N 2 Air purging for 5s, wherein the porosity of the air purging is 60%, and the average pore size of the porous polymer layer is 650nm;
s2, the prepared liquid electrolyte has a capacity of 1.4mg/cm per unit area 2 Drop-wise addition to the porous polymer layer is carried out so that it is completely impregnated.
Example 7:
the difference from example 1 is that:
the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a porous polymer polyvinylidene fluoride film to a length of 12.2cm and a width of 10.2cm, fixing the film on a clamp, and using N 2 Air blowing for 5s, wherein the porosity of the air blowing agent is 60%, and the average pore size of the porous polymer layer is 900nm;
s2, the prepared liquid electrolyte has a capacity of 1.6mg/cm per unit area 2 Dripping is carried outOnto the porous polymer layer so that it is completely wetted.
Comparative example 1
The difference from example 1 is that:
no porous polymer layer is present. The addition amount of the liquid electrolyte was 5.0mg/cm 2 The amount of the liquid electrolyte can ensure the normal operation of the electrochromic device.
Comparative example 2
The difference from example 1 is that:
no porous polymer layer is present. The addition amount of the liquid electrolyte was 8.0mg/cm 2 The amount of the liquid electrolyte can ensure the normal operation of the electrochromic device.
Comparative example 3
A polyvinyl butyral porous electrolyte membrane was produced according to an electrospinning method as described in example 2 of CN107422564A publication.
Two transparent substrates were cut out, the transparent substrates were 12cm long and 10cm wide. Carrying out physical vapor deposition on one of the conductive layers, wherein the ITO and the electrochromic layer are poly 3, 4-ethylenedioxythiophene to obtain a component with the electrochromic layer; the other piece is subjected to physical vapor deposition of a conducting layer ITO and an ion storage layer which are nickel oxide to obtain a component with the ion storage layer;
s1, cutting a polyvinyl butyral porous electrolyte membrane with a thickness of 12um to a length of 12.2cm and a width of 10.2cm, fixing the membrane on a clamp, and using N 2 A gas sweep for 5 seconds, wherein the porosity of the gas sweep is 70 percent, and the average pore size of the porous polyvinyl butyral porous electrolyte membrane is 3um;
s2, the prepared liquid electrolyte is used according to the unit area dosage of 2.8mg/cm 2 Dripping the porous polymer layer to make the porous polymer layer completely soaked;
s3, sealing the periphery of the electrochromic device by using ultraviolet curing glue of the packaging glue, and curing by ultraviolet light to obtain the electrochromic device;
the liquid electrolyte composition: the concentration of lithium perchlorate is 1mol/L, the content of vinylene carbonate as an additive is 1wt%, and propylene carbonate organic solvent is used as a solvent to obtain 1L of liquid electrolyte.
The test method is as follows:
transmittance test:
the transmittance of the samples was measured in experiments using an ultraviolet-visible spectrophotometer. The device step size was set to 2nm and the wavelength range was variable from 380nm to 1100 nm. The device can perform spectrum scanning, can also select any wavelength between 380nm and 1100nm to perform time scanning, and can obtain the full spectrum transmittance. The inventive examples and comparative examples were chosen for transmittance testing at 650 nm.
Electrochromic performance test:
the application adopts a spectral test system self-made in a laboratory to record electrochromic behaviors of materials in situ, one side of the device is connected with a light source (the model of light source equipment is DT-mini-2-GS, ocean Optics) through optical fibers, and the other side of the device is connected with an optical fiber spectrometer (the model of optical fiber spectrometer equipment is MAYA 2000-Pro, ocean Optics) of American Ocean company. The electrochemical workstation uses Shanghai Chenhua CHI 660D electrochemical workstation. The electrochromic performance test of all samples was performed in synchronization with the corresponding chronoamperometric test.
High temperature and high humidity test:
setting the environmental condition of the sealing equipment as 85 ℃ and 85% humidity, directly placing the electrochromic device in the sealing equipment under the test condition, continuously operating for 8 days (192 h), and visually observing the surrounding phenomenon of the encapsulation glue of the electrochromic device.
Table 1 summary of test results of electrochromic devices prepared in each example and comparative example
As can be seen from the data in table 1, the electrochromic devices provided in examples 1 to 7 of the present application have no electrolyte leakage even after the high temperature and high humidity test (i.e., under severe test environment conditions), and in particular, example 2, 200 electrochromic devices identical to example 1 were prepared, and the electrochromic devices of the present application were further illustrated to be suitable for mass production. In addition, the transmittance of the electrochromic devices prepared in the examples 1 and 3-7 of the application is tested under the condition of 650nm, and the difference between the transparent state transmittance and the coloring state transmittance is about 35%, which shows that the electrochromic device of the application has better performance. The electrochromic devices prepared in examples 1 and 3 to 7 of the present application have small change in transmittance in the colored state after high temperature and high humidity from that in the initial state even if subjected to severe conditions such as high temperature and high humidity, and further demonstrate that the electrochromic device of the present application has stable performance.
And the high-temperature and high-humidity test results of the electrochromic devices prepared in the comparative examples 1-2 show that the occurrence of white edges around the electrochromic devices indicates that the sealant is corroded and aged, and leakage exists.
Comparative example 3 the polyvinyl butyral porous electrolyte membrane was prepared according to the electrostatic spinning method, and first, the electrostatic spinning method was complicated, which was not conducive to large-scale industrial production. Secondly, the porosity of the film layer prepared by the electrostatic spinning method is up to 70%, the average pore size is 3 microns, which indicates that the pores are large and sparse and are unfavorable for stably adsorbing electrolyte, so that the electrochromic device prepared by the method has white edges around and electrolyte leakage after high-temperature and high-humidity testing.
Moreover, the electrochromic properties of comparative examples 1 to 3 after high temperature and high humidity were 10% or less, and the use requirements of electrochromic devices could not be satisfied.
The inventors of the present application found through a number of experiments that the electrolyte content of the electrochromic device provided with the porous ion conducting layer was 0.5mg/cm as shown in the examples of the present application 2 -1.6mg/cm 2 The normal operation of the electrochromic device can be achieved with relatively little electrolyte. While the electrolyte content of comparative examples 1-2 was 5mg/cm 2 -8mg/cm 2 Can realize the normal operation of the electrochromic deviceThe electrolyte content is required. Thus, the examples of the present application show that the electrolyte dosage of the present application is reduced and more environmentally friendly than the prior art, such as the comparative examples of the present application.
While the foregoing is directed to exemplary embodiments of the present application, it will be appreciated by those skilled in the art that various modifications and adaptations can be made thereto without departing from the principles of the present application, and such modifications and adaptations are intended to be comprehended within the scope of the present application.
Claims (9)
1. An electrochromic device is characterized in that a porous ion conducting layer is arranged between an electrochromic layer and an ion storage layer, the porous ion conducting layer is soaked by liquid electrolyte, the porous ion conducting layer is a porous polymer layer, the porosity of the porous polymer layer is 20% -60%, and the average pore size of the porous polymer layer is larger than 0nm and smaller than 1000nm.
2. The electrochromic device according to claim 1, wherein the porous ion conducting layer area is greater than 0.1% -30% of the area of the electrochromic layer or ion storage layer.
3. The electrochromic device according to claim 1, wherein a sealant is provided around the electrochromic layer, the porous ion conducting layer, the ion storage layer.
4. The electrochromic device according to claim 1, wherein the porous ion conducting layer has a thickness of 2um-25um.
5. The electrochromic device according to claim 1, wherein the porous polymer layer is one of a polyethylene film, a polypropylene film, a polyvinylidene fluoride film, a polyimide film, a polyaramid film.
6. The electrochromic device according to claim 1, wherein the electrochromic layer comprises, in order from top to bottom, a transparent substrate, a conductive layer, the electrochromic layer, the porous ion conducting layer, the ion storage layer, a conductive layer, a transparent substrate.
7. The electrochromic device according to claim 6, wherein the transparent substrate is one or more of glass, polyethylene terephthalate, polycarbonate, polymethyl methacrylate, the conductive layer is one or more of indium tin oxide, tin oxide doped antimony, zinc oxide doped aluminum, the electrochromic layer is one or more of poly 3, 4-ethylenedioxythiophene, poly 2, 5-dibromo-3, 4-ethylenedioxythiophene, poly 3, 4-bis (4-ethylhexyloxy) thiophene, polyaniline, polypyrrole, 1' -dimethyl-4, 4' -bipyridine, di- (2-phosphonoethyl) -4,4' -bipyridine, tungsten oxide, molybdenum oxide, titanium oxide; the ion storage layer is one or more of nickel oxide, niobium pentoxide, vanadium pentoxide, prussian blue and cerium oxide.
8. The electrochromic device according to claim 1, wherein the liquid electrolyte contains a lithium salt, a solvent and an additive; the lithium salt is one or more of lithium bistrifluoromethane sulfonyl imide, lithium trifluoromethane sulfonate, lithium perchlorate, lithium tetrafluoroborate and lithium hexafluorophosphate, the solvent is one or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, 1, 2-dimethoxyethane, N-dimethylformamide and water, and the additive is one or more of vinylene carbonate, fluoroethylene carbonate, polyethylene glycol, polyvinyl alcohol, ethylene glycol, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, N-lauroyl glutamic acid and N-lauroyl amid aspartic acid.
9. The electrochromic device according to claim 8, wherein the liquid electrolyte comprises: the concentration of lithium ions is 0.8mol/L-63mol/L, the additive is 1wt% -30wt% and the rest is solvent.
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| CN118393788A (en) * | 2024-06-27 | 2024-07-26 | 比亚迪股份有限公司 | Ion conducting layer for electrochromic device, preparation method of ion conducting layer, electrochromic device and application of ion conducting layer |
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| JPH06279610A (en) * | 1993-03-29 | 1994-10-04 | Tonen Corp | Polymer porous membrane and solid electrolyte membrane |
| JPH06313903A (en) * | 1993-04-30 | 1994-11-08 | Tonen Corp | Electrochromic electrode and its production |
| EP0628848A1 (en) * | 1992-12-28 | 1994-12-14 | Tonen Corporation | Electrochromic device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0628848A1 (en) * | 1992-12-28 | 1994-12-14 | Tonen Corporation | Electrochromic device |
| JPH06279610A (en) * | 1993-03-29 | 1994-10-04 | Tonen Corp | Polymer porous membrane and solid electrolyte membrane |
| JPH06313903A (en) * | 1993-04-30 | 1994-11-08 | Tonen Corp | Electrochromic electrode and its production |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118393788A (en) * | 2024-06-27 | 2024-07-26 | 比亚迪股份有限公司 | Ion conducting layer for electrochromic device, preparation method of ion conducting layer, electrochromic device and application of ion conducting layer |
| CN118393788B (en) * | 2024-06-27 | 2024-10-11 | 比亚迪股份有限公司 | Ion conducting layer for electrochromic device, preparation method of ion conducting layer, electrochromic device and application of ion conducting layer |
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