CN106371258A - Method for preparing electrochromic film and an electrochromic device - Google Patents
Method for preparing electrochromic film and an electrochromic device Download PDFInfo
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- CN106371258A CN106371258A CN201610921863.1A CN201610921863A CN106371258A CN 106371258 A CN106371258 A CN 106371258A CN 201610921863 A CN201610921863 A CN 201610921863A CN 106371258 A CN106371258 A CN 106371258A
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- electrochromic
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- electrochomeric films
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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
-
- 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
- G02F2001/164—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 the electrolyte is made of polymers
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- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a method for preparing an electrochromic film and an electrochromic device. The method for preparing the electrochromic film comprises the steps that an electrochromic material is dissolved in a polymer solution of 50-200 g/L to obtain a macromolecular composite electrochromic solution with the electrochromic material concentration of 0.05-0.2 mol/L, the macromolecular composite electrochromic solution forms a solution layer with the thickness of 50-500 microns, and after the solvent in the solution layer is removed, the electrochromic film is obtained. The technical problems of high preparation cost, difficult processing, difficult preparation due to large size and the like of an existing electrochromic film are solved. Compared with a magnetron sputtering technology of an existing electrochromic film preparation technology, the method has the advantages of being low in cost and simple in manufacturing process, needing simple required devices and the like. Compared with a filling technology, the method has the advantages that later processing is easy, a device assembly process is simple, special-shaped devices are easy to assemble and the like.
Description
Technical field
The present invention relates to electrochromic metallated polymer field and in particular to the preparation method of electrochomeric films and
Electrochromic device.
Background technology
Electrochromic material can change the color of itself under certain voltage, thus changing to the absorption of light or anti-
Penetrate, reach the purpose of light regulating, temperature.1961, deb found that WO 3 film can be no under electric field action first
Change, based on this discovery, Sweden scientist c.g.granqvist and American scientist c.m.lampert between normal complexion blueness
Etc. proposing a kind of new energy-conservation electrochromic concept.Numerous researchs are attracted from this electrochromic material and device preparation
The sight of person.
Electrochromic material can be divided into inorganic and organic two classes from structure, inorganic electrochromic material have Tungstic anhydride.,
Prussian blue etc., organic electrochromic material is divided into organic molecule and macromolecule two class again, wherein organic molecule have purpurine,
Phthalocyanine etc., macromolecule includes polyaniline compound, polythiophene class etc..
The assemble method of electrochomeric films is broadly divided into two kinds at present.A kind of method is to pass through electrochomeric films
Either physically or chemically it is deposited on electrically-conductive backing plate surface, this method cost of manufacture is higher, obtain the homogeneous electrochromism of large scale
The difficulty of thin film is larger；Another kind of method is that electrochromic material is dissolved in gel or liquid electrolyte, is filled to two panels
In the middle of conductive substrates, although this technology cost of manufacture reduces, it is difficult to produce large scale, the color-changing window of special shape.
Content of the invention
For the deficiency preparing electrochromic device in prior art, the present invention proposes and a kind of new cuts out electroluminescent change
The preparation method of color thin film, profit can obtain that a kind of film property is high, easy to process, be easily assembled to the electroluminescent of device in this way
Optically variable films, can not only greatly simplify the production technology of electrochromic device, and it can be used for preparing large scale and spy
The electrochromic device of different shape.
The invention provides a kind of method preparing electrochomeric films, comprising:
Electrochromic material is dissolved in the polymer solution that concentration is 50-200g/l, obtains electrochromic material concentration
Macromolecule composite electrochromic solution for 0.05-0.2mol/l, described macromolecule composite electrochromic solution shape in substrate
The solution layer becoming thickness to be 50-500 micron, after the solvent in solution layer is removed, obtains electrochomeric films.
The thin film of thickness 20-250 micron can be obtained according to the method described above, a thin film possessing better application value is thick
Degree is in 50-200 micron.
Preferably, described polymer solution is that polymer dissolving is obtained in a solvent, and described polymer includes poly- methyl
Acrylic acid methyl ester., polyvinyl alcohol, polrvinyl chloride, polyvinyl butyral resin, ethylene-vinyl acetate copolymer or polyurethanes
One or more of, described solvent includes methanol, acetone, acetonitrile, oxolane, chloroform, ethanol, Allyl carbonate, carbonic acid
Vinyl acetate, ethanol and n, one or more of n- dimethylformamide.
Preferably, described electrochromic material is 1,1- dimethyl -4,4'- bipyridinium dichloride, n, n salt two
Benzyl-benzyl salt second bipyridine dichloride, 1,1'- diethyl -4,4'- bipyridinium dibromide or 1,1'- diethyl -
4,4'- bipyridyl hexafluorophosphoric acid compound, dichloride -1,1'- two (4- carboxyl benzylidene) -4,4'- bipyridyl and/or chlorination -
1- (4- carboxyl benzylidene) -4,4'- bipyridyl.Because the change normal complexion electric current of thin-film material is related, therefore using other materials
Material can also play similar effect.
Preferably, the surface of described substrate and macromolecular material not bonding.Using the non-caked high molecular substrate in surface, make
The electrochomeric films obtaining can be obtained by simple stripping.
It is furthermore preferred that the surface of described substrate is Teflon, polypropylene, polystyrene or polyethylene terephthalate.
In embodiments of the invention, employ the surface plate that Teflon is obtained, electrochromism is obtained with by easy stripping
Thin film.
Preferably, the solution of described electrochromic polymeric compounds degassed process before forming solution layer and being formed.One very allusion quotation
The degassing process method of type is to use supersound process, and supersound process 30 minutes in ultrasonic washing instrument are put in such as round-bottomed flask sealing
Remove the bubble in liquid.
Preferably, the solution of described electrochromic polymeric compounds is through deoxidation treatment.Material for oxidation-sensitive, it is possible to use
The mode of deoxidation removes the oxygen in solution, and specific mode can be to be passed through dry nitrogen into solution.In order to prevent rousing
The gas for deoxygenation entering impacts to subsequent process, and this step is suitable in degasification process advance behavior.
Preferably, the described process removing solvent is to carry out under protective atmosphere.Because macromolecule composite electrochromic is molten
Component in liquid is sensitive for oxygen, and evaporation process should reduce the impact of oxygen, and in embodiments of the invention, evaporation process is in handss
Carry out in casing, the protective gas of employing is nitrogen.Those skilled in the art can also select suitable evaporitic environment and protection
Gas (as selected argon).
Preferably, described macromolecule composite electrochromic solution is prepared as follows:
Polyvinyl alcohol and polymethyl methacrylate are dissolved in ethanol/n, in n- dimethylformamide mixed solvent, heat up
Heating, until forming clear solution, stopping heating and being cooled to room temperature；Gamma-butyrolacton, ethanol, carbonic acid is added in previous solu
One or more of propylene and ethylene carbonate solvent, continues stirring to obtaining limpid viscous solution；Limpid to obtain
Add electrochromism part in viscous solution, stir under room temperature to being completely dissolved, add purpurine afterwards, stir under room temperature to completely molten
Add 4- butyl ammonium perchlorate after solution, be heated to being completely dissolved, obtain electrochromic polymeric compounds solution.
In above-mentioned preparation process, those skilled in the art can be adjusted flexibly heating-up temperature, material ratio as needed
Example and response time.
The film property of the electrochomeric films preparing according to the method described above is high, can be cut into arbitrary shape, subsequently
Assembly device mode is simple to operation.
Present invention also offers a kind of electrochromic device, described electrochromic device include the first conductive substrates, second
The electrochomeric films of conductive substrates and more than one layer, described electrochomeric films are located at first conductive substrates core the second conductive base
Between bottom.
Preferably, the thickness of described electrochomeric films is 20-200 micron, more preferably 50-200 micron.
Preferably, described conductive substrates are the substrate of flexible substrate or rigidity.
Described rigid base clear electro-conductive glass, such as indium oxide tin glass, fluorine-doped tin oxide glass etc.；Described flexibility
Substrate can be flexible conducting substrate, such as pet/ito, pet/go etc..
Preferably, described first conductive substrates and the second conductive substrates are ito glass, the conducting surface of ito glass and electricity
Optically variable films is caused to connect.
Preferably, also include fixture during described electrochromism, described fixture and the first conductive substrates and the second conductive base
Bottom connects, and realizes the close contact of the first conductive substrates and the second conductive substrates and electrochomeric films.
The present invention solves existing electrochomeric films preparation cost height, is not easy to processing, is difficult to prepare the skills such as large scale
Art problem, for the magnetron sputtering technique in existing electrochomeric films technology of preparing, has low cost, makes work
The advantages of skill is simple, equipment needed thereby is simple, for Canning Technique, has and is easy to post-production, the letter of assembly device technique
Singly, the advantages of be easily assembled to special shape device.
Brief description
Fig. 1, electrochromic device structural representation；
Fig. 2, electrochromic device transmitance figure in the clear state；
Fig. 3, electrochromic device transmitance figure in the energized state
Specific embodiment
As follows the specific embodiment with reference to the present invention to be illustrated technical scheme, it is only used as to the present invention
Illustrate rather than restriction.
A kind of electrochomeric films of the present invention are produced by following proposal:
Polyvinyl alcohol 2g, polymethyl methacrylate 0.5g, put into ethanol/n, in n- dimethylformamide mixed solvent
(wherein ethanol consumption is 20ml, and n, n- dimethylformamide consumption is 4ml), together pours in round-bottomed flask and adds magnetic force to stir
Mix son.Round-bottomed flask is placed in heat collecting type agitator, opens agitating function and design temperature begins to warm up for 80 DEG C.Until it is solid
Body material is completely dissolved in after forming sticky clear solution a in liquid, stops heating and is cooled to room temperature.
Gamma-butyrolacton (or ethanol, Allyl carbonate, ethylene carbonate or the above liquid of above two is added in a
Mixed solvent) 5ml, continues stirring, obtains limpid viscous solution b after system is homogeneous.
Weigh electrochromism part 0.071g, add in solution b, stir under room temperature to be completely dissolved to part and obtain solution c.
Subsequently weigh purpurine 0.1134g, add in solution c, stirring under room temperature, until purpurine is completely dissolved, obtains solution d.Weigh 4- fourth
Base ammonium perchlorate 0.205g, adds in solution d, and stirring under room temperature, until 4- butyl ammonium perchlorate is completely dissolved, obtains bottle green
Viscous solution e.
It is passed through the oxygen that dry nitrogen removes in liquid for 30 minutes in solution e, subsequently round-bottomed flask sealing is put into
The bubble that in ultrasonic washing instrument, supersound process removes in liquid for 30 minutes.
After ultrasonic end, solution e is equably poured in politef groove, put in the glove box of nitrogen protection,
Natural solvent flashing (ethanol and n, n- dimethylformamide) under room temperature.After solvent volatilizees completely, in politef groove
Obtain uniform thin film, thin film is torn and obtains tailorable electrochomeric films.
In above-mentioned preparation process, polymethyl methacrylate, polyvinyl alcohol, polrvinyl chloride, polyvinyl butyral resin, second
Alkene-acetate ethylene copolymer or polyurethanes, spendable solvent include methanol, acetone, acetonitrile, oxolane, chloroform,
Ethanol, Allyl carbonate, ethylene carbonate, ethanol and n, one or more of n- dimethylformamide, described electrochromism
Material is 1,1- dimethyl -4,4'- bipyridinium dichloride, n, n salt dibenzyl-benzyl salt second bipyridine dichloro
Compound, 1,1'- diethyl -4,4'- bipyridinium dibromide or 1,1'- diethyl -4,4'- bipyridyl hexafluorophosphoric acid compound, two
Chlorination -1,1'- bis- (4- carboxyl benzylidene) -4,4'- bipyridyl, chlorination -1- (4- carboxyl benzylidene) -4,4'- bipyridyl,
Those skilled in the art can surprisingly select other combinations in the present embodiment.
Referring to Fig. 1, the electrochromic device of the present invention is produced by following proposal:
The electrochomeric films obtaining are cut into required shape, are placed between the conducting surface of two panels conductive substrates, non-
Conducting surface fixture steps up, and is subsequently placed in vacuum drying oven.Close chamber door and start evacuation, design temperature is 90 DEG C and opens
Begin to heat.Keep vacuum state 5 minutes after temperature rises to 90 DEG C, close heating and slowly into vacuum drying oven, put into sky
Gas, until air and extraneous balance in case.After being cooled to room temperature, take out device and take off fixture, that is, obtain all solid state electricity
Mutagens color device.
Conductive substrates can be replaced by rigid transparent conducting glass, such as indium oxide tin glass, Fluorin doped oxidation herein
Stannum glass etc. or flexible conducting substrate, such as pet/ito, pet/go etc., it can play identical technique effect.
Electrochomeric films obtained above are cut into a size of 10cm x 10cm size, are clipped in two panels 11cm x 11cm
The ito glass conducting surface middle of size, nonconducting two sides clamp, put in vacuum drying oven.Close chamber door simultaneously
Start evacuation, design temperature is 90 DEG C and begins to warm up.Keep vacuum state 5 minutes after temperature rises to 90 DEG C, close and add
Heat simultaneously slowly puts into air into vacuum drying oven, until air and extraneous balance in case.After being cooled to room temperature, take out device
And take off fixture, and surrounding double-component fluid sealant edge sealing, that is, obtain all solid state electrochromic device.As shown in Figures 2 and 3.
Clear state to the device and coloured state transmitance in visible region tested it can be seen that energising in the case of, this
The electrochromic device of application has stronger absorption in visible light wave range.
In above-mentioned preparation process, vacuum compression can have a direct impact for performance, vacuum compression be make centre electroluminescent
Optically variable films is tight with baseplate-laminating, because laminating closely can not directly affect change color uniformity and the speed of resulting devices.
Claims (12)
1. a kind of method preparing electrochomeric films, comprising:
Electrochromic material is dissolved in the polymer solution that concentration is 50-200g/l, and obtaining electrochromic material concentration is
The macromolecule composite electrochromic solution of 0.05-0.2mol/l, described macromolecule composite electrochromic solution is formed in substrate
Thickness is the solution layer of 50-500 micron, after the solvent in solution layer is removed, obtains electrochomeric films.
2. the method preparing electrochomeric films according to claim 1 it is characterised in that described polymer solution be by
Polymer dissolving is obtained in a solvent, and described polymer includes polymethyl methacrylate, polyvinyl alcohol, polrvinyl chloride, poly- second
One or more of enol butyral, ethylene-vinyl acetate copolymer or polyurethanes, described solvent include methanol,
Acetone, acetonitrile, oxolane, chloroform, ethanol, Allyl carbonate, ethylene carbonate, ethanol and n, in n- dimethylformamide
One or more.
3. the method preparing electrochomeric films according to claim 1 is it is characterised in that described electrochromic material is
1,1- dimethyl -4,4'- bipyridinium dichloride, n, n salt dibenzyl-benzyl salt second bipyridine dichloride,
1,1'- diethyl -4,4'- bipyridinium dibromide or 1,1'- diethyl -4,4'- bipyridyl hexafluorophosphoric acid compound, dichloride -
1,1'- bis- (4- carboxyl benzylidene) -4,4'- bipyridyl and/or chlorination -1- (4- carboxyl benzylidene) -4,4'- bipyridyl.
4. the method preparing electrochomeric films according to claim 1 is it is characterised in that the surface of described substrate and height
Molecular material not bonding.
5. the method preparing electrochomeric films according to claim 4 is it is characterised in that the surface of described substrate is spy
Fluorine dragon, polypropylene, polystyrene or polyethylene terephthalate.
6. the method preparing electrochomeric films according to claim 1 is it is characterised in that described electrochromic polymeric compounds
Solution formed solution layer before degassed process.
7. the method preparing electrochomeric films according to claim 1 is it is characterised in that described electrochromic polymeric compounds
Solution through deoxidation treatment.
8. the method preparing electrochomeric films according to claim 1 it is characterised in that remove solvent process be
Carry out under protective atmosphere.
9. the method preparing electrochomeric films according to claim 1 it is characterised in that described macromolecule be combined electroluminescent
Electrochromic solution is prepared as follows:
Polyvinyl alcohol and polymethyl methacrylate are dissolved in ethanol/n, and in n- dimethylformamide mixed solvent, heat up heating,
Until forming clear solution, stopping heating and being cooled to room temperature；Gamma-butyrolacton, ethanol, Allyl carbonate is added in previous solu
With one or more of ethylene carbonate solvent, continue stirring to obtaining limpid viscous solution；Limpid sticky molten to obtain
Add electrochromism part in liquid, stir under room temperature to being completely dissolved, add purpurine afterwards, stir under room temperature to after be completely dissolved and add
Enter 4- butyl ammonium perchlorate, be heated to being completely dissolved, obtain macromolecule composite electrochromic solution.
10. a kind of electrochromic device, described electrochromic device include the first conductive substrates, the second conductive substrates and one layer with
On the arbitrary described electrochomeric films of claim 1-9, described electrochomeric films be located at the first conductive substrates and second
Between conductive substrates.
11. electrochromic devices according to claim 10 are it is characterised in that the thickness of described electrochomeric films is
20-200 micron.
12. electrochromic devices according to claim 10 it is characterised in that described conductive substrates be flexible substrate or
The substrate of rigidity.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106959564A (en) * | 2017-03-31 | 2017-07-18 | 上海凯密科实业有限公司 | A kind of glass pane with electrochromic property |
| CN108383981A (en) * | 2018-04-16 | 2018-08-10 | 西安电子科技大学 | The preparation method of conducting polymer copolymer nano pipe and its electrochromic layer and electrochromic device |
| CN112965311A (en) * | 2021-02-03 | 2021-06-15 | 畅的新材料科技（上海）有限公司 | Electrochromic film and preparation method thereof |
| WO2022134900A1 (en) * | 2020-12-24 | 2022-06-30 | 清华大学深圳国际研究生院 | Freely cuttable electrochromic device and application |
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Effective date of registration: 20220721 Address after: 100085 01, floor 1, building 2, yard 9, anningzhuang West Road, Haidian District, Beijing Patentee after: Yilaichuang (Beijing) Intelligent Material Technology Co.,Ltd. Address before: 235000 No. 99, Renmin Road, Xiangnan street, Xiangshan District, Huaibei City, Anhui Province Patentee before: Shanghai Moyi Biotechnology Co.,Ltd. Huaibei branch |