CN104698715A - All-solid electrochromic device - Google Patents
All-solid electrochromic device Download PDFInfo
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- CN104698715A CN104698715A CN201310640917.3A CN201310640917A CN104698715A CN 104698715 A CN104698715 A CN 104698715A CN 201310640917 A CN201310640917 A CN 201310640917A CN 104698715 A CN104698715 A CN 104698715A
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- electrochromic device
- full
- solid electrochromic
- acrylate
- solid
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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
- G02F1/1506—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
- G02F1/1508—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode using a solid electrolyte
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Nonlinear Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention discloses an all-solid electrochromic device which can change color with the variations of the polarity and the strength of an external electric field. The all-solid electrochromic device sequentially comprises a transparent non-conducting base, a transparent conducting electrode layer, an electrochromic material layer, a polymer electrolyte layer, an ion storage layer, another conducting electrode layer and another non-conducting base, wherein the polymer electrolyte layer is a material layer composed of lithium salt, an organic solvent, a high-molecular polymer material, a prepolymer, a monomer, a photoinitiator and glass beads which are mixed according to a certain proportion, and then solidified through UV-irradiation. Finally, the device is sealed through non-conducting glue. Therefore, the all-solid electrochromic device is formed.
Description
Technical field
The present invention relates to a kind of electrochromic device, particularly a kind of full-solid electrochromic device adopting polymer dielectric.
Background technology
Electrochromic device (Electrochromic Devices) refers to the change along with extra electric field polarity and intensity, the color of electrochromic material and reversible change is occurred to the reflection of incident ray or intensity in transmission, thus a kind of device through intensity of solar radiation can be controlled.Because electrochromic device only uses lower DC voltage (being generally no more than ± 5V) to change color, and there is memory effect, namely, after extra electric field is cancelled, (generally more than 8 hours) can also keep current painted or bleached state for a long time, therefore the energy consumption of device is considerably less.If this device is applied to the wall face of buildings, people can according to the change of season and time, ACTIVE CONTROL through intensity of solar radiation, greatly save the energy consumption of buildings.Other application also comprise: sunglasses, vehicle dormer window and side window, anti-dazzle driving mirror and side-view mirror, the porthole, electronic display etc. of aircraft.
Electrochromic device is generally 5 Rotating fields: transparency conductive electrode layer, electrochromic material layer, dielectric substrate, ion storage and another conductive electrode layer.Electrochromic device can be divided into liquid electrolyte and the large class of solid electrolyte two according to the electrolyte used.Disclosed in patent CN203012308U and CN101493625B, electrochromic device all adopts liquid electrolyte, and implement fairly simple, cost is lower.But also there is many problems, comprise corrosion and the leakage of electrolyte solution, encapsulation difficulty, easily produces bubble, and the thickness of detector made is larger etc.Patent CN100498493 adopts the method for low temperature magnetic sputtering to make all retes of the device of the film electrolyte layer comprised containing lithium, although thickness of detector reduces greatly, require very high to coating quality, easily occur the situation of short circuit, yield rate is low, and cost is also higher.In addition, the method that then polymer dielectric containing lithium solidifies is used also can to prepare full-solid electrochromic device.As disclosed the thermal curing methods preparing full-solid electrochromic device with the polymer dielectric containing lithium in patent US8218225B2 and CN101510038B, this method is when preparing dielectric substrate, lithium salts is first dissolved among organic solvent, and then and the mixing of two or more organic monomer after add initiating agent, then improve temperature and impel oligomer monomer polymerization and crosslinked with the object reaching solidification.But slower, the consuming time length of this mode curing rate, energy consumption is high, and technique is also complicated.
Summary of the invention
For above problem, the present invention adopts the mode of ultra-violet curing, lithium salts is first dissolved among organic solvent, add a certain amount of macromolecule polymer material to regulate the viscosity of solution and to strengthen the conductivity of lithium ion, then prepolymer is added, monomer, the glass microballoon of light trigger and control device thickness of interlayer fully after mixing, this potpourri is coated between the electrochromic material layer of electrochromic device and ion storage, the energy of recycling ultraviolet light at room temperature carries out the solidification of polymer dielectric, finally utilize transparent non-conductive encapsulation glue by device environmental seal, make all solid state electrochromic device.This mode efficiency is high, energy consumption is low, repeatability is high, simplify the packaging technology of device, is applicable to high-speed automated coating and produces, can greatly enhance productivity.
As shown in Figure 1, full-solid electrochromic device of the present invention comprises transparent non-conductive substrate, transparency conductive electrode layer, electrochromic material layer, at the bottom of another nonconductive matrix, conductive electrode layer, ion storage, and be in the polyelectrolyte floor between electrochromic material layer and ion storage.
In one embodiment of the present invention, the transparent non-conductive substrate of described device, it can be inorganic material, as glass, also can be organic material, as: polyethylene terephthalate (Polythylene terephthalate), polycarbonate (Polycarbonate), polymethylmethacrylate (PMMA) etc.
Above-mentioned transparent non-conductive substrate forms transparency conductive electrode layer, as: In
2o
3: Sn (ITO), SnO
2: F (FTO), ZnO:Al (AZO).
In one embodiment of the present invention, can be the material to visible transparent at the bottom of another nonconductive matrix described, also can be to the opaque material of visible ray.The conductive electrode layer formed at the bottom of above-mentioned nonconductive matrix can be the conductive material to visible transparent, as: In
2o
3: Sn (ITO), SnO
2: F (FTO), ZnO:Al (AZO) they also can be the metal materials higher to visible reflectance, as: silver, aluminium, titanium, chromium, nickel, molybdenum etc.
In one embodiment of the present invention, described electrochromic material layer can be cathodic coloration electrochromic material, comprise organic electrochromic material, transition metal oxide or Prussian blue, Ke Yishi: Vilogen, Pyrazoline, Poly (aniline), Tetrathiafulvalene, WO
3, MoO
3, Nb
2o
5, TiO
2, V
2o
5, Fe
4[Fe (CN)
6]
3.
In one embodiment of the present invention, described ion storage can be weak cathodic coloration electrochromic material or anodic coloration electrochromic material.Comprise: NiO, TiO
2, V
2o
5, Co
2o
3, Rh
2o
3, IrO
2deng.
In one embodiment of the present invention, described polyelectrolyte floor is by lithium salts, organic solvent, macromolecule polymer material, prepolymer, monomer and light trigger, and the glass microballoon of control device thickness of interlayer, mix according to a certain percentage, then through the material layer of UV-irradiation Post RDBMS formation.
Above-mentioned lithium salts can be: lithium perchlorate (LiClO
4), LiBF4 (LiBF
4), lithium hexafluoro phosphate (LiPF
6), trifluoromethyl sulfonic acid lithium (LiCF
3sO
3), two (trifluoromethane sulfonic acid) imine lithium (LiN (CF
3sO
2)
2) etc.
Above-mentioned organic solvent can be the potpourri of a kind of solvent or several solvent, comprising: carbonic allyl ester (Propylene carbonate), dimethyl carbonate (Dimethyl carbonate), ethylene carbonate (Ethylene carbonate), dimethyl formamide (Dimethyl formamide), acetamide (Acetamide), dimethyl acetamide (Dimethyl acetamide) etc.
Above-mentioned high molecular polymer can be: polymethylmethacrylate (Poly (methyl meth-acrylate)), polyoxyethylene (Poly (ethylene oxide)), PEF ethylene glycol Poly (ethylene glycole)), polypropyleneoxide (Poly (propylene oxide)) etc.
Above-mentioned prepolymer is the low polymer with reactivity, Ke Yishi: polyester acrylate, epoxy acrylate, urethane acrylate, unsaturated polyester (UP), polyolefin/mercaptan etc.
Above-mentioned monomer is reactive diluent again, its Main Function is adjusting viscosity and participates in polyreaction, can be that the potpourri of one or more monomers is as styrene, butyl acrylate, Isooctyl acrylate monomer, isobornyl acrylate, tri (propylene glycol) diacrylate, hexanediyl ester, trimethylolpropane triacrylate and NVP etc.
The effect of above-mentioned light trigger is after absorption ultraviolet light (wavelength 250 ~ 400nm) energy, decomposes and produces free radical, and then the polyreaction of trigger monomer and prepolymer, makes potpourri be solid by liquid state.Light trigger can be: dibenzoyl, benzophenone, styrax and ether compound thereof are as dimethoxybenzoin, benzoin ethyl ether, benzoin isobutyl ether etc.
Like this, when device runs, electric field is added at device two ends by conductive electrode, by changing polarity and the intensity of extra electric field, lithium ion in polyelectrolyte floor can reversibly pass in and out electrochromic material layer, and the color change of electrochromic material causes device to realize the adjustment of continuous print gradual change type to the transmitance of visible ray or reflectivity.
The electrochromic device made in this way is made to have following beneficial effect:
1, use polymer dielectric to prepare full-solid electrochromic device, the leakage problem of liquid electrolyte can be avoided;
2, add the viscosity that high molecular polymer can increase electrolyte solution, the production efficiency of coating process can be improved; The conductivity of lithium ion can also be improved, reduce the reaction time of device;
3, adopt the thickness of interlayer of glass microballoon control device, thickness of detector is greatly reduced, and the film defects that causes of the dust during can avoiding due to plated film and the shorted devices phenomenon that causes;
4, utilize the energy of ultraviolet light to realize the solidification of polymer dielectric, compare the method for heat curing, energy consumption is low, technique is simple, be applicable to robotization coating production, can greatly enhance productivity.
Accompanying drawing explanation
Below in conjunction with accompanying drawing and embodiment, the present invention is further described:
Accompanying drawing 1 is the basic block diagram of full-solid electrochromic device.In figure, 101 are transparent non-conductive substrates, 102 are transparency conductive electrode layers, 103 is electrochromic material layers, 201 is at the bottom of another nonconductive matrix, 202 are conductive electrode layers, 203 are ion storage, 300 are polyelectrolyte floors, 401 and 402 is the transparent non-conductive adhesive glues of device package.
Embodiment
Embodiment 1: concrete implementation step is as follows:
(1) as shown in Figure 1, magnetron sputtering method is adopted to make transparency conductive electrode layer 102 in transparent non-conductive substrate 101, as: ITO(In
2o
3: Sn), FTO(SnO:F) or AZO (ZnO:Al), its thickness is between 100nm-200nm, and square resistance is less than 20W/, and transmittance is greater than 80%;
(2) magnetron sputtering method or vacuum vapour deposition is adopted to make electrochromic material layer 103, as: WO
3, MoO
3, its thickness is between 100nm-500nm;
(3) magnetron sputtering method is adopted to make transparency conductive electrode layer 202 in another transparent non-conductive substrate 201, as: ITO(In
2o
3: Sn), FTO(SnO:F) or AZO (ZnO:Al), its thickness is between 100nm-200nm, and square resistance is less than 20W/, and transmittance is greater than 80%;
(4) magnetron sputtering method or vacuum vapour deposition is adopted to make ion storage 203, as: NiO, TiO
2, V
2o
5, its thickness is between 50nm-300nm;
(5) prepolymer epoxy acrylate, monomer trimethylol-propane trimethacrylate and NVP are made into mixed solution according to the ratio of 3:1:2;
(6) dimethoxybenzoin and benzophenone are made into mixed light initiating agent according to the ratio of 2:1;
(7) in the mixed solution of above-mentioned prepolymer and monomer, add above-mentioned mixed light initiating agent, the weight ratio of light trigger is between 3%-5%;
(8) by lithium salts lithium perchlorate, be dissolved among organic solvent carbonic allyl ester, magnetic agitation makes it dissolve completely, and lithium salt is between 0.1M/L to 1M/L.Add the macromolecule polymer material polymethylmethacrylate that weight ratio is 5% to 30% again, if desired solution is heated to 40-70
oc makes solution mix;
(9) in the mixed solution of above-mentioned lithium salts and high molecular polymer, add the above-mentioned mixed solution be made up of prepolymer, monomer and light trigger according to the weight ratio of 3:1, magnetic agitation makes it mix;
(10) add the glass microballoon (diameter is between 10 microns to 100 microns) that weight ratio is 3/1000ths, magnetic agitation makes it mix;
(11) mixed solution be equipped with in step 10 is coated on the substrate 101 being coated with rete 102 and 103, the substrate 201 another being coated with rete 202 and 203 is placed on it, use certain pressure, two substrates are combined closely, does not have among bubble interlayer.And this thickness of interlayer is by the diameter control of glass microballoon;
(12) adopt ultraviolet light to irradiate device, after the mixed solution solidification be equipped with in step 10, form solid polymer electrolyte layer 300;
(13) and then utilize transparent non-conductive bonding glue, by device sealing, all solid state electrochromic device is made.
These device both sides all adopt transparent substrates and transparency conductive electrode, are transmission type electrochromic device.
Embodiment 2: when needs make reflective electrochromic device, only need change the transparency conductive electrode layer 202 at the bottom of another nonconductive matrix on 201 in example 1 metal material with high reflectance into, as: silver, aluminium, titanium, chromium, nickel, molybdenum etc.Other steps are with identical in example 1.
Claims (10)
1. a full-solid electrochromic device, is characterized in that, comprising: transparent non-conductive substrate; Transparency conductive electrode layer, it is formed on described transparent non-conductive substrate; Electrochromic material layer, it is formed on transparency conductive electrode; At the bottom of another nonconductive matrix; Conductive electrode layer, it is formed at the bottom of another nonconductive matrix described; Ion storage, it is formed on conductive electrode layer; Polyelectrolyte floor, it is formed between electrochromic material layer and ion storage, it is characterized in that: comprise lithium salts, organic solvent, macromolecule polymer material, prepolymer, monomer and light trigger, and the glass microballoon of control device thickness of interlayer, mix according to a certain percentage, then through the material layer of UV-irradiation Post RDBMS formation.
2. full-solid electrochromic device according to claim 1, is characterized in that, described lithium salts comprises: lithium perchlorate (LiClO
4), LiBF4 (LiBF
4), lithium hexafluoro phosphate (LiPF
6), trifluoromethyl sulfonic acid lithium (LiCF
3sO
3), two (trifluoromethane sulfonic acid) imine lithium (LiN (CF
3sO
2)
2).
3. full-solid electrochromic device according to claim 1, it is characterized in that, described organic solvent can be the potpourri of a kind of solvent or several solvent, comprising: carbonic allyl ester (Propylene carbonate), dimethyl carbonate (Dimethyl carbonate), ethylene carbonate (Ethylene carbonate), dimethyl formamide (Dimethyl formamide), acetamide (Acetamide), dimethyl acetamide (Dimethyl acetamide).
4. full-solid electrochromic device according to claim 1, it is characterized in that, described high molecular polymer comprises: polymethylmethacrylate (Poly (methyl meth-acrylate)), polyoxyethylene (Poly (ethylene oxide)), PEF ethylene glycol Poly (ethylene glycole)), polypropyleneoxide (Poly (propylene oxide)).
5. full-solid electrochromic device according to claim 1, is characterized in that, described prepolymer comprises: polyester acrylate, epoxy acrylate, urethane acrylate.
6. full-solid electrochromic device according to claim 1, it is characterized in that, described monomer can be the potpourri of one or more monomers, comprising: styrene, butyl acrylate, Isooctyl acrylate monomer, isobornyl acrylate, tri (propylene glycol) diacrylate, hexanediyl ester, trimethylolpropane triacrylate and NVP.
7. full-solid electrochromic device according to claim 1, is characterized in that, described light trigger comprises: dibenzoyl, benzophenone, dimethoxybenzoin, benzoin ethyl ether, benzoin isobutyl ether.
8. full-solid electrochromic device according to claim 1, it is characterized in that, described transparent non-conductive substrate, comprise: glass, polyethylene terephthalate (Polythylene terephthalate), polycarbonate (Polycarbonate), polymethylmethacrylate (PMMA).
9. full-solid electrochromic device according to claim 1, is characterized in that, described electrochromic material layer comprises: Vilogen, Pyrazoline, Poly (aniline), Tetrathiafulvalene, WO
3, MoO
3, Nb
2o
5, TiO
2, V
2o
5, Fe
4[Fe (CN)
6]
3.
10. full-solid electrochromic device according to claim 1, is characterized in that, described ion storage comprises: NiO, TiO
2, V
2o
5, Co
2o
3, Rh
2o
3, IrO
2.
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|---|---|---|---|
| CN201310640917.3A CN104698715A (en) | 2013-12-04 | 2013-12-04 | All-solid electrochromic device |
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|---|---|---|---|
| CN201310640917.3A CN104698715A (en) | 2013-12-04 | 2013-12-04 | All-solid electrochromic device |
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| CN107621737A (en) * | 2016-07-13 | 2018-01-23 | 武利铭 | Full-solid electrochromic glass |
| CN108089388A (en) * | 2017-12-29 | 2018-05-29 | 山东大学 | A kind of method of selected control electricity light modulation device operating voltage |
| CN108319088A (en) * | 2018-02-26 | 2018-07-24 | 江苏天贯碳纳米材料有限公司 | A kind of electrochromic device and its manufacturing method |
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