CN108873537A - A kind of electrochomeric films, preparation method and application and electrochromic device - Google Patents
A kind of electrochomeric films, preparation method and application and electrochromic device Download PDFInfo
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- CN108873537A CN108873537A CN201810659349.4A CN201810659349A CN108873537A CN 108873537 A CN108873537 A CN 108873537A CN 201810659349 A CN201810659349 A CN 201810659349A CN 108873537 A CN108873537 A CN 108873537A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 239000002253 acid Substances 0.000 claims abstract description 64
- 239000003792 electrolyte Substances 0.000 claims abstract description 42
- 239000004014 plasticizer Substances 0.000 claims abstract description 41
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 34
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 34
- 230000004044 response Effects 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000000975 dye Substances 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims description 48
- 238000003860 storage Methods 0.000 claims description 40
- 238000000576 coating method Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 23
- 239000003513 alkali Substances 0.000 claims description 19
- 150000004982 aromatic amines Chemical class 0.000 claims description 16
- 150000003672 ureas Chemical class 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 13
- -1 imidazole radicals benzoquinones Chemical class 0.000 claims description 12
- 150000004989 p-phenylenediamines Chemical class 0.000 claims description 12
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical class [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 12
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 8
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000004054 benzoquinones Chemical class 0.000 claims description 5
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 5
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 4
- 150000004056 anthraquinones Chemical class 0.000 claims description 4
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 4
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 4
- AMKRBKSZCGCEJK-UHFFFAOYSA-N 1,2-dimethoxyanthracene-9,10-dione Chemical compound C1=CC=C2C(=O)C3=C(OC)C(OC)=CC=C3C(=O)C2=C1 AMKRBKSZCGCEJK-UHFFFAOYSA-N 0.000 claims description 3
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 238000009825 accumulation Methods 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- MFZQGVIVNYZZGI-UHFFFAOYSA-N 1,2-diethoxyanthracene-9,10-dione Chemical compound C1=CC=C2C(=O)C3=C(OCC)C(OCC)=CC=C3C(=O)C2=C1 MFZQGVIVNYZZGI-UHFFFAOYSA-N 0.000 claims description 2
- 150000004057 1,4-benzoquinones Chemical class 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 2
- 241001597008 Nomeidae Species 0.000 claims description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 2
- 238000010422 painting Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- HMWVNKJRYWXJGS-UHFFFAOYSA-N C(C)(=O)OC=C.[C] Chemical compound C(C)(=O)OC=C.[C] HMWVNKJRYWXJGS-UHFFFAOYSA-N 0.000 claims 1
- 150000004985 diamines Chemical class 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 8
- 230000002441 reversible effect Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 230000005684 electric field Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 7
- 235000013877 carbamide Nutrition 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- 238000006467 substitution reaction Methods 0.000 description 5
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 4
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- YUSWFULMAAAFJQ-UHFFFAOYSA-N 1,3-oxazole quinoline Chemical compound C1=COC=N1.N1=CC=CC2=CC=CC=C21 YUSWFULMAAAFJQ-UHFFFAOYSA-N 0.000 description 1
- 125000000590 4-methylphenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)C([H])([H])[H] 0.000 description 1
- 229910003893 H2WO4 Inorganic materials 0.000 description 1
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 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 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 150000002518 isoindoles Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound 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 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000123 polythiophene Chemical class 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229960003351 prussian blue Drugs 0.000 description 1
- 239000013225 prussian blue Substances 0.000 description 1
- BBNQQADTFFCFGB-UHFFFAOYSA-N purpurin Chemical compound C1=CC=C2C(=O)C3=C(O)C(O)=CC(O)=C3C(=O)C2=C1 BBNQQADTFFCFGB-UHFFFAOYSA-N 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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
Abstract
The present invention provides a kind of electrochomeric films, preparation method and application and electrochromic device, the electrochomeric films include electrochromic layer, and the raw material of the electrochromic layer includes following component in parts by weight：Polymethyl methacrylate 30-50 parts by weight；Acid response dyestuff 18-22 parts by weight；Plasticizer 20-30 parts by weight；Electrolyte 10-20 parts by weight；Wherein, the acid response dyestuff is the combination of electroluminescent acid with sour responsive materials.Electrochomeric films provided by the invention can stablize in the effect of extra electric field, reversible color change, have electrochromic property.
Description
Technical field
The invention belongs to display device technical field, be related to a kind of electrochomeric films, preparation method and application and
Electrochromic device.
Background technique
Electrochromism is the optical properties of material, refer to stablize under external electric field or the function of current, reversible color becomes
Change, the process of reversible change occurs for the color and transparency that intuitively show as material.From foreign scholar's the 1960s
Since Plant is put forward for the first time electrochromism concept, electrochromism phenomenon, which causes, widely to be paid close attention to.It is existing using this electrochromism
As electrochromic device can be prepared.Electrochromic device have visual angle is wide, driving voltage is low, idle memory etc. it is unique excellent
Point herewith has extremely wide purposes in the rearview mirror etc. of sensitive window, display and automobile etc..Electrochromic material can divide
For inorganic and organic two class, inorganic electrochromic material has tungstic acid, Prussian blue etc., and organic electrochromic dyestuff is divided into again
Two class of small organic molecule and macromolecule, small molecular have purpurine, phthalocyanine etc., and macromolecule includes polyaniline compound, polythiophene class etc..
For electrochomeric films majority using ito glass as electrically-conductive backing plate, assemble method is broadly divided into two classes, Yi Zhongfang at present
Method is by electrochomeric films by being either physically or chemically deposited on electrically-conductive backing plate surface, and this method cost of manufacture is higher,
The difficulty for obtaining the uniform electrochomeric films of large scale is larger；Another method is that electrochromic material is dissolved in gel or liquid
It in body electrolyte, is filled among two panels electrically-conductive backing plate, although this technology cost of manufacture reduces, it can be difficult to producing big ruler
Very little, special shape optically variable films.CN101412588A discloses a kind of cathodic electrochromic film and electrochomeric glass
Preparation method, with H2WO4Powder or Ni (NO3) powder be raw material, using citric acid complex-polymerization liquid chemical method, immersion coating
Technique or spin coating coating processes obtain sol pellicle on ito glass substrate, obtain cathode electricity through dry polymerization, Low Temperature Heat Treatment
Optically variable films is caused, preparation method is complicated, and the electrochromism response time is longer and consumes energy more；" electroluminescent acid/base it is theoretical and its
It is mentioned in application in organic electrochromic material " and uses hydroquinone for electroluminescent alkali, novel oxazole quinoline molecule FXF is as soda acid
Response color indicator is prepared for electrochromic device, and the electrochromic device response time is short, but the stability of device is poor.
Currently, the electronical display huge energy consumption that the whole world is annual, year power consumption is more than 3.5 million degree of electricity, total close to whole world power consumption
The 19% of amount is equivalent to the year power generation total amount in 70 Yangtze River Gorges；And traditional electronic display screen is because of color flash and back
The stimulation of scape light, can cause irreversible injury to human eye.
Need a kind of low energy consumption, electrochromism response time short at present and the simple electrochomeric films of preparation method.
Summary of the invention
The purpose of the present invention is to provide a kind of electrochomeric films, preparation method and application and electrochromism devices
Part.
In order to achieve that object of the invention, the present invention uses following technical scheme：
On the one hand, the present invention provides a kind of electrochomeric films, the electrochomeric films include electrochromic layer, institute
The raw material for stating electrochromic layer includes following component in parts by weight：
Wherein, the acid response dyestuff is the combination of electroluminescent acid with sour responsive materials.
Electrochomeric films provided by the invention include electrochromic layer, and preparing for electrochromic layer includes acid in raw material
Dyestuff is responded, after applying voltage, electroluminescent acid occurs oxidation (or reduction) reaction and releases proton, sour responsive materials and proton knot
It closes, the variation of color occurs, and this state still can be continued for a period of time after voltage removes；And apply backward voltage
Afterwards, electroluminescent acid is reduced (or oxidation) and recaptures proton, and the color of sour responsive materials is restored to original state；Electricity provided by the invention
Causing optically variable films includes electrochromic layer, can be stablized in the effect of extra electric field, reversible color change, has electricity
Cause discoloration can be under the premise of not consuming energy after being stimulated by voltage, lasting display information, therefore there is energy consumption
Low feature.
In the present invention, the parts by weight of the polymethyl methacrylate be 30-50 parts by weight, such as 32 parts by weight,
35 parts by weight, 40 parts by weight, 42 parts by weight, 45 parts by weight, 47 parts by weight etc..
In the present invention, the parts by weight of the acid response dyestuff are 18-22 parts by weight, such as 19 parts by weight, 20 weight
Part, 21 parts by weight etc..
In the present invention, the parts by weight of the plasticizer are 20-30 parts by weight, such as 22 parts by weight, 24 parts by weight, 25
Parts by weight, 26 parts by weight, 28 parts by weight, 29 parts by weight etc..
In the present invention, the parts by weight of the electrolyte are 10-20 parts by weight, such as 12 parts by weight, 13 parts by weight, 15
Parts by weight, 17 parts by weight, 18 parts by weight, 19 parts by weight etc..
Preferably, the electroluminescent acid is in the carbamide derivative of p-phenylene diamine derivative, hydroquinone and aromatic amine substitution
Any one or at least two combination, preferably N- replace p-phenylene diamine derivative and/or aromatic amine replace ureas spread out
Biology.
When the electroluminescent acid that the present invention selects is that the p-phenylene diamine derivative that N- replaces and/or the ureas that aromatic amine replaces are derivative
When object, the electrochomeric films electrochromism response time of the invention is short, it is only necessary to 0.01-3s.
Preferably, the sour responsive materials are fluorane kind derivant, the preferably green derivative of rhodamine derivative, temperature-sensitive
With temperature-sensitive in black derivative any one or at least two combination, the rhodamine of further preferred spirolactams form spreads out
Biological and/or black temperature-sensitive derivative.
Preferably, the mass ratio of the electroluminescent acid and sour responsive materials is 1:(2-4), such as 1:2.5,1:3,1:3.5 waiting.
Preferably, the electroluminescent acid is the carbamide derivative of p-phenylene diamine derivative and/or aromatic amine substitution that N- replaces,
The sour responsive materials derivative black for the Rhodamine Derivatives and/or temperature-sensitive of spirolactams form, the electroluminescent acid are responded with acid
The mass ratio of material is 1:(2.5-3), such as 1:2.6,1:2.7,1:2.8,1:2.9 waiting.
In the present invention, conductive layer and ion storage are set gradually in the electrochromic layer side.
Preferably, the electrochromic layer with a thickness of 1-500 μm, such as 50 μm, 100 μm, 200 μm, 300 μm, 400 μm
Deng.
Preferably, the raw material of the conductive layer includes following component in parts by weight：
Polymethyl methacrylate 40-60 parts by weight；
Plasticizer 25-40 parts by weight；
Electrolyte 15-25 parts by weight.
In the present invention, the parts by weight of the polymethyl methacrylate be 40-60 parts by weight, such as 42 parts by weight,
45 parts by weight, 50 parts by weight, 52 parts by weight, 55 parts by weight, 57 parts by weight etc..
In the present invention, the parts by weight of the plasticizer are 25-40 parts by weight, such as 28 parts by weight, 30 parts by weight, 32
Parts by weight, 34 parts by weight, 36 parts by weight, 38 parts by weight etc..
In the present invention, the parts by weight of the electrolyte are 15-25 parts by weight, such as 17 parts by weight, 20 parts by weight, 21
Parts by weight, 22 parts by weight, 23 parts by weight, 24 parts by weight etc..
Preferably, the raw material of the ion storage includes following component in parts by weight：
The electroluminescent acid and electroluminescent alkali with electro-chemical activity are added in ion storage, can make far from electrochromic layer one
It is easier that redox reaction occurs on the electrode of side, when electrochomeric films two sides, encapsulated electrode obtains electrochromic device
Afterwards, after applying voltage, while oxidation (or reduction) reaction occurs for electrochromic layer, the ion far from electrochromic layer side
Reduction (or oxidation) reaction can occur in accumulation layer, can reduce the operating voltage of device in this way, reduce the generation of side reaction,
So as to increase the stability of device, and electrochromism response speed is also promoted.
In the present invention, the parts by weight of the polymethyl methacrylate be 40-60 parts by weight, such as 42 parts by weight,
45 parts by weight, 50 parts by weight, 52 parts by weight, 55 parts by weight, 57 parts by weight etc..
In the present invention, the parts by weight of the plasticizer are 20-40 parts by weight, such as 22 parts by weight, 25 parts by weight, 30
Parts by weight, 34 parts by weight, 36 parts by weight, 38 parts by weight etc..
In the present invention, the parts by weight of the electrolyte are 10-20 parts by weight, such as 12 parts by weight, 15 parts by weight, 16
Parts by weight, 17 parts by weight, 18 parts by weight, 19 parts by weight etc..
In the present invention, the parts by weight of the electroluminescent acid are 5-20 parts by weight, such as 7 parts by weight, 10 parts by weight, 15 weights
Measure part, 17 parts by weight, 18 parts by weight, 19 parts by weight etc..
In the present invention, the parts by weight of the electroluminescent alkali are 5-20 parts by weight, such as 7 parts by weight, 10 parts by weight, 15 weights
Measure part, 17 parts by weight, 18 parts by weight, 19 parts by weight etc..
Preferably, in the ion storage, the electroluminescent alkali is that 1,4-benzoquinone analog derivative and/or Anthraquinones are derivative
Benzoquinones, imidazole radicals benzoquinones, anthraquinone, dimethoxy anthraquinone and the diethyl of benzoquinones, phenyl substitution that object, preferably dimethyl amido replace
In oxygroup anthraquinone any one or at least two combination.
Preferably, the plasticizer includes ethylene carbonate and/or propene carbonate.
The electrolyte includes tetrabutyl ammonium hexafluorophosphate, lithium perchlorate, bis-trifluoromethylsulfoandimide lithium, 1- ethyl -3-
Any one in methylimidazole hexafluorophosphate and 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt or at least two
Combination.
In the present invention, the unit mass of so-called each parts by weight is the same, such as in electrochromic layer, each
Parts by weight are 10g, then each parts by weight in conductive layer and ion storage are 10g.
Second aspect, the present invention provides the preparation method of electrochomeric films as described in relation to the first aspect, the preparation
Method includes the following steps：
(1) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, coating
Film forming, obtains electrochomeric films.
In the present invention, the coating film forming means to be handled solution to obtain film, either spraying, drop coating, rotation
The technological means that solution can be become film by painting, blade coating etc. can use, also, those skilled in the art know, are applying
It is that be painted on solution arbitrarily can be to form a film on the substrate of coating during dressing up film.
Preferably, the preparation method includes the following steps：
(A) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, are applied
Film is dressed up, ion storage is obtained；
(B) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, are obtained in step (A)
Coating film forming in ion storage obtains ion storage-conductive layer；
(C) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step
Suddenly coating film forming on the conductive layer that (B) is obtained, obtains the electrochomeric films.
The third aspect, the present invention provides a kind of electrochromic device, the electrochromic device includes first aspect institute
The electrochomeric films stated.
Preferably, electrochromic device electrochomeric films as described in first aspect and be located at electrochromism it is thin
The electrically-conductive backing plate of film two sides forms.
Preferably, the electrically-conductive backing plate is ITO electro-conductive glass.
Preferably, the preparation method of the electrochromic device includes the following steps：It successively will be from ITO electro-conductive glass
Then sub- accumulation layer, conductive layer and electrochromic layer coating film forming encapsulate another ITO electro-conductive glass, obtain the electroluminescent change
Color device.
Fourth aspect, the present invention provides the answering in electronic display screen of electrochomeric films as described in relation to the first aspect
With.
Being not required to continued power using the electronic display screen that electrochomeric films provided by the invention obtain can be realized electricity
Mutagens color, and the electrochromic response time is short, can save electric power resource.
Compared with the existing technology, the invention has the advantages that：
(1) electrochomeric films provided by the invention can stablize in the effect of extra electric field, reversible color
Variation has electrochromic property, and the electrochromism response time is short, only 0.01-3s；
(2) when the electroluminescent acid that the present invention selects is the p-phenylene diamine derivative that N- replaces and/or the ureas that aromatic amine replaces
Derivative, sour responsive materials are the black derivative of the Rhodamine Derivatives and/or temperature-sensitive of spirolactams form and electroluminescent acid and acid
The mass ratio of responsive materials is 1:When (2.5-3), electrochomeric films provided by the invention have the electrochromism response time compared with
It is short, only 0.01-1s；
(3) provided by the invention preparation method is simple, need to only be simply mixed, coating film forming can be obtained by electroluminescent change
Color film, without passing through either physically or chemically the methods of deposition；
(4) electrochomeric films provided by the invention, which are not required to continued power, can be realized electrochromism, be mentioned using the present invention
The electronic display screen that the electrochomeric films of confession obtain can save a large amount of electric power resource.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the electrochomeric films that preparation example provides.
Wherein, 101- ion storage；102- conductive layer；103- electrochromic layer.
Fig. 2 be embodiment provide electrochromism during structural schematic diagram.
Wherein, 201- ion storage；202- conductive layer；203- electrochromic layer；204- electrically-conductive backing plate.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Preparation example 1
Fig. 1 is the structural schematic diagram of electrochomeric films provided in this embodiment, wherein from bottom to top includes ion storage
Layer 101, conductive layer 102 and electrochromic layer 103.
Wherein, electrochromic layer includes following component in parts by weight：
Conductive layer includes following component in parts by weight：
50 parts by weight of polymethyl methacrylate；
30 parts by weight of plasticizer；
20 parts by weight of electrolyte.
Ion storage includes following component in parts by weight：
Acid response dyestuff is the p-phenylene diamine derivative that N- replaces and the black derivative of temperature-sensitive is 1 in mass ratio:3 compositions
Mixture；Plasticizer is ethylene carbonate；Electrolyte is lithium perchlorate.
In ion storage, electroluminescent acid is the p-phenylene diamine derivative that N- replaces, and electroluminescent alkali is the benzoquinones that phenyl replaces.
Preparation method includes the following steps：
(1) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, are applied
Film is dressed up, ion storage is obtained；
(2) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, are obtained in step (1)
Coating film forming in ion storage obtains ion storage-conductive layer；
(3) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step
Suddenly coating film forming on the conductive layer that (2) obtain, obtains electrochomeric films.
Preparation example 2
Difference with preparation example 1 is only that in acid response dyestuff, the p-phenylene diamine derivative and temperature-sensitive that N- replaces are black
Derivative mass ratio is 1:2.5 (preparation examples 2), 1:1 (preparation example 3), 1:5 (preparation examples 4).
Preparation example 5
A kind of electrochomeric films are followed successively by ion storage, conductive layer and electrochromic layer from top to bottom.
Wherein, electrochromic layer includes following component in parts by weight：
Conductive layer includes following component in parts by weight：
40 parts by weight of polymethyl methacrylate；
40 parts by weight of plasticizer；
15 parts by weight of electrolyte.
Ion storage includes following component in parts by weight：
Acid response dyestuff is that the carbamide derivative of aromatic amine substitution and the Rhodamine Derivatives of spirolactams form press quality
Than being 1:The mixture of 2 compositions；Plasticizer is propene carbonate；Electrolyte is bis-trifluoromethylsulfoandimide lithium.
In ion storage, electroluminescent acid is the carbamide derivative that aromatic amine replaces, and electroluminescent alkali is imidazole radicals benzoquinones.
Preparation method includes the following steps：
(1) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, are applied
Film is dressed up, ion storage is obtained；
(2) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, are obtained in step (1)
Coating film forming in ion storage obtains ion storage-conductive layer；
(3) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step
Suddenly coating film forming on the conductive layer that (2) obtain, obtains electrochomeric films.
Preparation example 6
A kind of electrochomeric films are followed successively by ion storage, conductive layer and electrochromic layer from top to bottom.
Wherein, electrochromic layer includes following component in parts by weight：
Conductive layer includes following component in parts by weight：
60 parts by weight of polymethyl methacrylate；
25 parts by weight of plasticizer；
25 parts by weight of electrolyte.
Ion storage includes following component in parts by weight：
Acid response dyestuff is the carbamide derivative that aromatic amine replaces and the black derivative of temperature-sensitive is 1 in mass ratio:4 compositions
Mixture；Plasticizer is ethylene carbonate；Electrolyte is lithium perchlorate.
In ion storage, electroluminescent acid is the carbamide derivative that aromatic amine replaces, and electroluminescent alkali is imidazole radicals benzoquinones.
Preparation method includes the following steps：
(1) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, are applied
Film is dressed up, ion storage is obtained；
(2) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, are obtained in step (1)
Coating film forming in ion storage obtains ion storage-conductive layer；
(3) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step
Suddenly coating film forming on the conductive layer that (2) obtain, obtains electrochomeric films.
Preparation example 7
A kind of electrochomeric films are followed successively by ion storage, conductive layer and electrochromic layer from top to bottom.
Wherein, electrochromic layer includes following component in parts by weight：
Conductive layer includes following component in parts by weight：
55 parts by weight of polymethyl methacrylate；
35 parts by weight of plasticizer；
25 parts by weight of electrolyte.
Ion storage includes following component in parts by weight：
Acid response dyestuff is the p-phenylene diamine derivative that N- replaces and the black derivative of temperature-sensitive is 1 in mass ratio:2 compositions
Mixture；Plasticizer is propene carbonate；Electrolyte is 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt.
In ion storage, electroluminescent acid is the p-phenylene diamine derivative that N- replaces, and electroluminescent alkali is diethoxy anthraquinone.
Preparation method includes the following steps：
(1) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, are applied
Film is dressed up, ion storage is obtained；
(2) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, are obtained in step (1)
Coating film forming in ion storage obtains ion storage-conductive layer；
(3) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step
Suddenly coating film forming on the conductive layer that (2) obtain, obtains electrochomeric films.
Preparation example 8
A kind of electrochomeric films are followed successively by ion storage, conductive layer and electrochromic layer from top to bottom.
Wherein, electrochromic layer includes following component in parts by weight：
Conductive layer includes following component in parts by weight：
45 parts by weight of polymethyl methacrylate；
25 parts by weight of plasticizer；
15 parts by weight of electrolyte.
Ion storage includes following component in parts by weight：
Acid response dyestuff is that the carbamide derivative of aromatic amine substitution and the Rhodamine Derivatives of spirolactams form press quality
Than being 1:The mixture of 3 compositions；Plasticizer is ethylene carbonate and propene carbonate；Electrolyte is 1- ethyl-3-methylimidazole
Hexafluorophosphate.
In ion storage, electroluminescent acid is the carbamide derivative that aromatic amine replaces, and electroluminescent alkali is dimethoxy anthraquinone.
Preparation method includes the following steps：
(1) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, are applied
Film is dressed up, ion storage is obtained；
(2) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, are obtained in step (1)
Coating film forming in ion storage obtains ion storage-conductive layer；
(3) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step
Suddenly coating film forming on the conductive layer that (2) obtain, obtains electrochomeric films.
Compare preparation example 1
Difference with preparation example 1 is only that, in electrochromic layer, acid response dyestuff is 1- (4- (dimethylamino) benzene
Base) -3-) p-methylphenyl) urea (Urea-N) and Rhodamine Derivatives 3', bis- (the diethylamino) -3- oxo spiral shell [iso-indoles of 6'-
- 1,9'-ant tons of quinoline] 2- base ester (Rh-M) combination.
Compare preparation example 2-4
Difference with preparation example 1 is only that, in ion storage, is not included electroluminescent acid (comparison preparation example 2), is not included
Electroluminescent alkali (comparison preparation example 3) does not include electroluminescent acid and electroluminescent alkali (comparison preparation example 4).
Embodiment 1-8
A kind of electrochromic device by the electrochomeric films provided in preparation example 1-8 and is located at electrochomeric films
The ITO electro-conductive glass of two sides forms.
Wherein, Fig. 2 is the structural schematic diagram of electrochromic device, from bottom to top includes ITO electrode 204, ion storage
201, conductive layer 202, electrochromic layer 203 and ITO electrode 204.
Preparation method includes the following steps：Any one two side packing of electrochomeric films provided in preparation example 1-8
ITO electro-conductive glass, obtains electrochromic device.
Comparative example 1-4
A kind of electrochromic device by the electrochomeric films provided in comparison preparation example 1-4 and is located at electrochromism
The ITO electro-conductive glass of film two sides forms.
Preparation method includes the following steps：Any one the electrochomeric films two sides provided in comparison preparation example 1-4
ITO electro-conductive glass is encapsulated, electrochromic device is obtained.
Performance test
The embodiment 1-8 and comparative example 1-4 electrochromic device provided is tested for the property：
(1) 1V voltage is applied to electrochromic device, record is applied the alive time when having color change, and record result is shown in
Table 1；
(2) test method being used in conjunction using uv-vis spectra and electrochemistry：1V voltage is applied to electrochromic device, is made
It is measured when its absorbance value changes a lot and is applied the alive time with UV, visible light spectrophotometer, and recorded as a result, seeing
Table 2；
Table 1
By the comparison of embodiment and comparative example it is found that the electrochomeric films electrochromism response time provided by the invention
It is short, electrochromism can be occurred within 0.10-0.25s after applying voltage, and the colour stable time up to 500s or more, by
Embodiment 1-2,8 it is found that when it is electroluminescent acid be N- replace p-phenylene diamine derivative and/or aromatic amine replace carbamide derivative,
Sour responsive materials are the black derivative of the Rhodamine Derivatives and/or temperature-sensitive of spirolactams form and electroluminescent acid and sour responsive materials
Mass ratio be 1:When (2.5-3), the electrochromism response time of electrochomeric films provided by the invention is shorter, in 0.10-
Electrochromism can occur in 0.12s, and the colour stable time is in 1000s or more.
Table 2
Table 2 is the time of voltage applied when detecting absorbance change by ultraviolet-uisible spectrophotometer and extinction
Spend the retention time.By embodiment and comparative example it is found that electrochomeric films absorbance provided by the invention changes the used time compared with
It is short, the variation of absorbance can occur within 50ms after applying voltage, and the absorbance retention time is long, up to 500s with
On, by embodiment 1-2,8 it is found that when electroluminescent acid is that the p-phenylene diamine derivative that N- replaces and/or the ureas that aromatic amine replaces spread out
Biology, sour responsive materials is the black derivatives of the Rhodamine Derivatives and/or temperature-sensitive of spirolactams form and electroluminescent acid is rung with acid
The mass ratio for answering material is 1:When (2.5-3), the absorbance of electrochomeric films provided by the invention used time that changes is shorter,
Within 25ms, and the absorbance retention time is in 1100s or more.
The Applicant declares that the present invention is explained by the above embodiments electrochomeric films of the invention, preparation method
With application and electrochromic device, but the present invention is not limited to the above embodiments, that is, does not mean that the present invention must rely on
Above-described embodiment could be implemented.It should be clear to those skilled in the art, any improvement in the present invention, to the present invention
The equivalence replacement of selected raw material and addition, the selection of concrete mode of auxiliary element etc., all fall within protection scope of the present invention
Within the open scope.
Claims (10)
1. a kind of electrochomeric films, which is characterized in that the electrochomeric films include electrochromic layer, the electrochromism
The raw material of layer includes following component in parts by weight：
Wherein, the acid response dyestuff is the combination of electroluminescent acid with sour responsive materials.
2. electrochomeric films according to claim 1, which is characterized in that it is described it is electroluminescent acid be p-phenylene diamine derivative,
In the carbamide derivative that hydroquinone and aromatic amine replace any one or at least two combination, preferably N- replace to benzene
The carbamide derivative that diamine derivative and/or aromatic amine replace；
Preferably, the sour responsive materials are fluorane kind derivant, the preferably green derivative of rhodamine derivative, temperature-sensitive and heat
In quick black derivative any one or at least two combination, the Rhodamine Derivatives of further preferred spirolactams form
And/or the derivative that temperature-sensitive is black.
3. electrochomeric films according to claim 1 or 2, which is characterized in that the electroluminescent acid and sour responsive materials
Mass ratio is 1:(2-4)；
Preferably, the electroluminescent acid is that the p-phenylene diamine derivative that N- replaces and/or the carbamide derivative that aromatic amine replaces, acid are rung
Answer the derivative that material is black for the Rhodamine Derivatives and/or temperature-sensitive of spirolactams form, the electroluminescent acid and sour responsive materials
Mass ratio be 1:(2.5-3).
4. electrochomeric films described in any one of -3 according to claim 1, which is characterized in that in the electrochromic layer
Side sets gradually conductive layer and ion storage；
Preferably, the electrochromic layer with a thickness of 1-500 μm.
5. electrochomeric films according to claim 4, which is characterized in that the raw material of the conductive layer wraps in parts by weight
Include following component：
Polymethyl methacrylate 40-60 parts by weight；
Plasticizer 25-40 parts by weight；
Electrolyte 15-25 parts by weight；
Preferably, the raw material of the ion storage includes following component in parts by weight：
6. electrochomeric films according to claim 5, which is characterized in that described electroluminescent in the ion storage
Alkali be 1,4-benzoquinone analog derivative and/or anthraquinone derivatives, preferably dimethyl amido replace benzoquinones, phenyl replace benzoquinones,
In imidazole radicals benzoquinones, anthraquinone, dimethoxy anthraquinone and diethoxy anthraquinone any one or at least two combination.
7. electrochomeric films described in any one of -6 according to claim 1, which is characterized in that the plasticizer includes carbon
Vinyl acetate and/or propene carbonate；
The electrolyte includes tetrabutyl ammonium hexafluorophosphate, lithium perchlorate, bis-trifluoromethylsulfoandimide lithium, 1- ethyl -3- methyl
In limidazolium hexafluorophosphate and 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimide salt any one or at least two group
It closes.
8. the preparation method of electrochomeric films described in any one of -7 according to claim 1, which is characterized in that the system
Preparation Method includes the following steps：
(1) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, coating film forming,
Obtain electrochomeric films；
Preferably, the preparation method includes the following steps：
(A) polymethyl methacrylate of formula ratio, plasticizer, electrolyte, electroluminescent acid and electroluminescent alkali are uniformly mixed, painting is dressed up
Film obtains ion storage；
(B) polymethyl methacrylate of formula ratio, plasticizer and electrolyte are uniformly mixed, in the ion that step (A) obtains
Coating film forming in accumulation layer obtains ion storage-conductive layer；
(C) polymethyl methacrylate of formula ratio, acid response dyestuff, plasticizer and electrolyte are uniformly mixed, in step (B)
Coating film forming on obtained conductive layer obtains the electrochomeric films.
9. a kind of electrochromic device, which is characterized in that the electrochromic device includes any one of claim 1-7 institute
The electrochomeric films stated；
Preferably, electrochromic device electrochomeric films as described in any one of claim 1-7 and it is located at
The electrically-conductive backing plate of electrochomeric films two sides forms；
Preferably, the electrically-conductive backing plate is ITO electro-conductive glass；
Preferably, the preparation method of the electrochromic device includes the following steps：Successively ion is deposited on ITO electro-conductive glass
Then reservoir, conductive layer and electrochromic layer coating film forming encapsulate another ITO electro-conductive glass, obtain the electrochromism device
Part.
10. application of the electrochomeric films described in any one of -7 in electronic display screen according to claim 1.
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| CN110330809A (en) * | 2019-07-18 | 2019-10-15 | 江南大学 | A kind of electric, temperature double-cotrolled type chromotropic dye and its microcapsules preparation method |
| CN111948863A (en) * | 2020-08-21 | 2020-11-17 | 中国人民解放军96901部队25分队 | Multi-band adjustable electrochromic device and preparation method and application thereof |
| CN112300309A (en) * | 2020-10-30 | 2021-02-02 | 江南大学 | Preparation method of stretchable flexible electrochromic film |
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| CN109696785A (en) * | 2019-01-08 | 2019-04-30 | 辽宁大学 | A kind of high-performance electrochromism capacitor double-function device and preparation method thereof |
| CN109696785B (en) * | 2019-01-08 | 2021-06-01 | 辽宁大学 | High-performance electrochromic capacitor dual-function device and manufacturing method thereof |
| CN109856882A (en) * | 2019-03-25 | 2019-06-07 | 华南理工大学 | A kind of electrochomeric glass and its packaging method |
| CN110330809A (en) * | 2019-07-18 | 2019-10-15 | 江南大学 | A kind of electric, temperature double-cotrolled type chromotropic dye and its microcapsules preparation method |
| CN110330809B (en) * | 2019-07-18 | 2020-07-07 | 江南大学 | Electricity and temperature dual-control type color-changing dye and preparation method of microcapsule thereof |
| WO2021008346A1 (en) * | 2019-07-18 | 2021-01-21 | 江南大学 | Method for preparing electrical/temperature dual control bistable color-changing dye and microcapsule |
| US11655373B2 (en) | 2019-07-18 | 2023-05-23 | Jiangnan University | Method of preparing electric and temperature dual-control bi-stable color-changing dyes and microcapsules |
| CN111948863A (en) * | 2020-08-21 | 2020-11-17 | 中国人民解放军96901部队25分队 | Multi-band adjustable electrochromic device and preparation method and application thereof |
| CN112300309A (en) * | 2020-10-30 | 2021-02-02 | 江南大学 | Preparation method of stretchable flexible electrochromic film |
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