CN104932169B - A kind of flexible electro-chromic device of quick response and its application - Google Patents
A kind of flexible electro-chromic device of quick response and its application Download PDFInfo
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- CN104932169B CN104932169B CN201510427775.1A CN201510427775A CN104932169B CN 104932169 B CN104932169 B CN 104932169B CN 201510427775 A CN201510427775 A CN 201510427775A CN 104932169 B CN104932169 B CN 104932169B
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- 239000000758 substrate Substances 0.000 claims abstract description 45
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 53
- 229910001868 water Inorganic materials 0.000 claims description 34
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 32
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 32
- -1 allyl ester Chemical class 0.000 claims description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 238000000151 deposition Methods 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 17
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 14
- 229910003893 H2WO4 Inorganic materials 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 5
- 238000005478 sputtering type Methods 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- ITZGNPZZAICLKA-UHFFFAOYSA-N bis(oxiran-2-ylmethyl) 7-oxabicyclo[4.1.0]heptane-3,4-dicarboxylate Chemical compound C1C2OC2CC(C(=O)OCC2OC2)C1C(=O)OCC1CO1 ITZGNPZZAICLKA-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- WECMXZWEYLYREA-UHFFFAOYSA-I [C+4].Cl(=O)(=O)(=O)[O-].[Li+].Cl(=O)(=O)(=O)[O-].Cl(=O)(=O)(=O)[O-].Cl(=O)(=O)(=O)[O-].Cl(=O)(=O)(=O)[O-] Chemical compound [C+4].Cl(=O)(=O)(=O)[O-].[Li+].Cl(=O)(=O)(=O)[O-].Cl(=O)(=O)(=O)[O-].Cl(=O)(=O)(=O)[O-].Cl(=O)(=O)(=O)[O-] WECMXZWEYLYREA-UHFFFAOYSA-I 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims 5
- 238000005868 electrolysis reaction Methods 0.000 claims 3
- 229920002472 Starch Polymers 0.000 claims 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 claims 1
- 235000019698 starch Nutrition 0.000 claims 1
- 239000008107 starch Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 22
- 238000004061 bleaching Methods 0.000 abstract description 4
- 239000003792 electrolyte Substances 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000970 chrono-amperometry Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910000474 mercury oxide Inorganic materials 0.000 description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical group O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- CGNJOCXWRKNYRU-UHFFFAOYSA-M lithium;carbonic acid;perchlorate Chemical compound [Li+].OC(O)=O.[O-]Cl(=O)(=O)=O CGNJOCXWRKNYRU-UHFFFAOYSA-M 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000037303 wrinkles 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
- G02F1/153—Constructional details
- G02F1/155—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/155—Electrodes
- G02F2001/1552—Inner electrode, e.g. the electrochromic layer being sandwiched between the inner electrode and the support substrate
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/155—Electrodes
- G02F2001/1555—Counter electrode
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
A kind of flexible electro-chromic device of quick response and its application, it is related to a kind of electrochromic device and its application.The invention aims to solve the material preparation method and the jejune problem of flexible device package technique of existing flexible device.A kind of flexible electro-chromic device of quick response includes：Working electrode, to electrode and dielectric substrate, wherein working electrode is the flexible electrochomeric films of transparent quick response；It is PET ITO to electrode；Dielectric substrate is in working electrode and between electrode；The flexible electro-chromic device edge of quick response is packaged using resin.A kind of flexible electro-chromic device of quick response is as wearable electronic product in smart electronics product scope application.A kind of present invention flexible electro-chromic device response time of quick response is short, and bleaching time is 4s~6s, and coloration time is 8s~10s.The present invention can obtain a kind of flexible electro-chromic device of quick response.
Description
Technical field
The present invention relates to a kind of electrochromic device and its application.
Background technology
Electrochromism refers to that under certain electric field or the function of current light scattering or light absorbs can occur for material, so that
Cause its color to change, when polarity of electrode changes, the phenomenon faded occurs again.Since Deb.S.K. in 1969 first
It is found that WO3Since electrochromism phenomenon, people are found that much and WO in succession again3Equally with electrochromic property
Material, such as NiO, purple sieve essence, polyaniline etc. so that the species of electrochromic material gradually increases, wide using gradually change.
When redox reaction occurs for electrochromic material, its color can occur reversibly to change.As electroluminescent
The representative of off-color material, tungstic acid (WO3) because it has the advantages that contrast is high, transparency is high, stability is good and it is a large amount of
Research and extensive use, particularly its hydrate (WO3·H2O, H2WO4·H2O etc.), show more excellent electrochromism
Performance.But it differs greatly as inorganic electrochromic material in the performance of response time with organic electrochromic material.
Poly- 3,4-ethylene dioxythiophene (PEDOT) is paid close attention to because of its excellent coloration efficiency and electric conductivity, in electrochromism device
Both organic electrochromic material is may be used as in part, the slow shortcoming of inorganic electrochromic material response speed is made up, can use again
Make conducting polymer, strengthen the electric conductivity of device, further enhance the transmission of electronics and ion in colourshifting process, improve electroluminescent become
Color performance.
With the continuous progress of science and technology, people gradually have wearable demand to smart electronicses product.Wearable production
Product require that material has certain mechanical strength, can be stretched, distort, fold, wrinkle, without performance degradation.These productions
Product can adapt to the non-planar surfaces of complexity, the application field for having rigid mount not have.Wherein, electrochromic material because
It can realize color change under small voltage control and have very high application value.
In order to meet wearable demand, the rigid electrochromic device assembled by substrate of glass can not be met
It is required that, flexible electro-chromic device progressively turns into study hotspot.However, available for the material preparation method of flexible device and soft
Property device package technique it is immature, largely constrain the development and application of flexible electro-chromic device.Prepare soft
The conventional method of property electrochomeric films includes：Magnetron sputtering, plasma enhanced chemical vapor deposition and photoetching, it usually needs
Expensive equipment, strict experiment condition and multiple process steps.Further, since the adhesion between material and flexible substrates
Difference, conventional films can be strained after stress bending, are broken, or even be separated with substrate.Therefore, synthesizing new electrochromism material
Material, develops the package technique of flexible electro-chromic device, to the practical application of electrochromic material, there is highly important meaning
Justice.
The content of the invention
The invention aims to solve the material preparation method and flexible device assembling skill of existing flexible device
The jejune problem of art, and flexible electro-chromic device and its application of a kind of quick response are provided.
A kind of flexible electro-chromic device of quick response includes：Working electrode, to electrode and dielectric substrate, wherein working
Electrode is the flexible electrochomeric films of transparent quick response；It is PET-ITO to electrode；Dielectric substrate be in working electrode and
To between electrode；The flexible electro-chromic device edge of described quick response is packaged using resin.
A kind of flexible electro-chromic device of quick response should in smart electronics product scope as wearable electronic product
With.
Advantages of the present invention：
First, a kind of flexible electro-chromic device stability of quick response of the invention is good, and color change interval is wide, at 900nm
Light modulation scope is 50%；
2nd, a kind of flexible electro-chromic device response time of quick response of the invention is short, and bleaching time is 4s~6s,
The color time is 8s~10s；
3rd, the flexible electrochomeric films for the transparent quick response for preparing the present invention (will this by 360 ° of bendings
The head and the tail connection for inventing the flexible electrochomeric films of the transparent quick response prepared forms a ring) after, microscopic appearance is not
Change；
4th, the present invention is prepared for the flexible electrochomeric films of transparent quick response, the flexibility of transparent quick response
H containing flexible substrates and flaky nanometer structure in electrochomeric films2WO4·H2O, has taken into account cost, the transparency of conductive layer
And electric conductivity；Using the flexible electrochomeric films of the transparent quick response of preparation as working electrode, make in quick response
While there is the electrochromic properties such as fast-response, contrast height in flexible electro-chromic device, flexible electrochromism is solved
Adhesion between device material and substrate is poor, and strain, fracture occur after the bending of film stress and the technology bottle such as separates with substrate
Neck, expands the application field of electrochromic device；
5th, a kind of preparation method of the flexible electro-chromic device of quick response of the invention is simple, can be mass-produced, pushes away
Electrochromic industrialization is moved；Safely and effectively, energy-conserving and environment-protective make a kind of flexible electro-chromic device of quick response of the present invention
Use long lifespan.
The present invention can obtain a kind of flexible electro-chromic device of quick response.
Brief description of the drawings
Fig. 1 schemes for the SEM of the flexible electrochomeric films of the transparent quick response prepared in embodiment one；
Fig. 2 be embodiment one in a kind of quick response flexible electro-chromic device digital photograph figure；
Fig. 3 is a kind of structural representation of the flexible electro-chromic device of quick response in embodiment one, and 1 is in Fig. 3
The flexible electrochomeric films of transparent quick response, 2 be dielectric substrate, and 3 be that 4 be resin to electrode PET-ITO；
Fig. 4 uses chronoamperometry in 900nm for a kind of flexible electro-chromic device of quick response in embodiment one
Place, transmitance-time graph under+3V~-3V tests.
Embodiment
Embodiment one：Present embodiment is that a kind of flexible electro-chromic device of quick response includes：Work electricity
Pole, to electrode and dielectric substrate, wherein working electrode is the flexible electrochomeric films of transparent quick response；To electrode PET-
ITO；Dielectric substrate is in working electrode and between electrode；The flexible electro-chromic device edge of described quick response is used
Resin is packaged.
The advantage of present embodiment：
First, a kind of flexible electro-chromic device stability of quick response of present embodiment is good, and color change interval is wide,
Light modulation scope is 50% at 900nm；
2nd, a kind of flexible electro-chromic device response time of quick response of present embodiment is short, bleaching time be 4s~
6s, coloration time is 8s~10s；
3rd, the flexible electrochomeric films for the transparent quick response for preparing present embodiment are bent (i.e. by 360 °
The head and the tail connection of the flexible electrochomeric films of transparent quick response prepared by present embodiment forms a ring) after, it is micro-
Pattern is seen not change；
4th, present embodiment is prepared for the flexible electrochomeric films of transparent quick response, transparent quick response
H containing flexible substrates and flaky nanometer structure in flexible electrochomeric films2WO4·H2O, taken into account conductive layer cost, thoroughly
Lightness and electric conductivity；Using the flexible electrochomeric films of the transparent quick response of preparation as working electrode, make quickly ringing
While there is the electrochromic properties such as fast-response, contrast height in the flexible electro-chromic device answered, solve flexible electroluminescent
Adhesion between Electrochromic device material and substrate is poor, and strain, fracture occur after the bending of film stress and the skill such as separates with substrate
Art bottleneck, expands the application field of electrochromic device；
5th, a kind of preparation method of the flexible electro-chromic device of quick response of present embodiment is simple, can in high volume give birth to
Production, has promoted electrochromic industrialization；A kind of flexible electro-chromic device of quick response of present embodiment safely and effectively, is saved
Can be environmentally friendly, service life is long.
Present embodiment can obtain a kind of flexible electro-chromic device of quick response.
Embodiment two：The difference of present embodiment and embodiment one is：It is described transparent quick
The flexible electrochomeric films of response are prepared as follows：
First, flexible substrates are cleaned by ultrasonic 20min~30min in acetone, methanol and ultra-pure water successively respectively, placed into
Temperature is dry 10h~15h, the flexible substrates cleaned at 40 DEG C~60 DEG C；
Flexible substrates described in step one are the PET base that surface is covered with that thickness is 20nm~100nmEVA glue；
2nd, Ag layers are prepared：Use magnetically controlled sputter method EVA glue in the flexible substrates of cleaning surface sputter thickness for
10nm~50nm Ag sedimentaries, obtaining surface deposition has Ag layers of PET base；
The parameter of magnetically controlled sputter method described in step 2 is specific as follows：Target is Ag targets, and sputtering type is splashed for direct current
Penetrate, target-cardinal distance is 10cm~20cm, gas flow is argon gas 1sccm~10sccm, and depositing temperature is room temperature, and deposition pressure is
2Pa~4Pa, sputtering power is 10W~20W, and sedimentation time is 10s~40s；
3rd, mixed solution B is prepared：
1. the sodium tungstate that, sulfuric acid and concentration for being 0.01mol/L~1mol/L by concentration are 0.01mol/L~1mol/L is molten
Liquid is mixed, and is added the hydrogen peroxide that mass fraction is 30%, is added ultra-pure water, then low whipping speed be 500r/min~
5min~10min is stirred under 1000r/min, mixed solution A is obtained；Mixed solution A is stood to 5 days~7 days at room temperature, obtained
Yellow mercury oxide material, as H2WO4·H2O；
Step 3 1. described in concentration be 0.01mol/L~1mol/L sulfuric acid and concentration be 0.01mol/L~1mol/
The volume ratio of L sodium tungstate solution is 1:1；
Step 3 1. described in concentration be 0.01mol/L~1mol/L sulfuric acid and mass fraction be 30% hydrogen peroxide
Volume ratio be 1:(0.01~0.1)；
Step 3 1. described in concentration be 0.01mol/L~1mol/L sulfuric acid and the volume ratio of ultra-pure water be 1:(1~
10)；
2. the use of ultra-pure water is, solvent, by H2WO4·H2O is centrifuged in the case where centrifugal speed is 2000r/min~8000r/min
5min~10min, removes supernatant；
3., repeat step three 2. 3 times~5 times, the H after being cleaned2WO4·H2O；
4., by the H after cleaning2WO4·H2O is distributed in ultra-pure water, obtains the H that mass fraction is 5%~50%2WO4·
H2O solution；To the H that mass fraction is 5%~50%2WO4·H2It is 0.002%~0.01% that mass fraction is added in O solution
Cetyl trimethylammonium bromide solution, adds the PEDOT that mass fraction is 5%~30%:PSS solution, then in stirring speed
Spend to stir 10min~30min under 500r/min~1000r/min, obtain mixed solution B；
Step 3 4. described in mass fraction be 5%~50% H2WO4·H2O solution is 0.002% with mass fraction
The volume ratio of~0.01% cetyl trimethylammonium bromide solution is 1:(0.05~0.5)；
Step 3 4. described in mass fraction be 5%~50% H2WO4·H2O solution and mass fraction be 5%~
30% PEDOT:The volume ratio of PSS solution is 1:(0.05~0.5)；
4th, H is prepared2WO4·H2O/PEDOT films：
1. the PET base that, depositing surface has Ag layers is immersed in 1min~3min in mixed solution B, then surface is deposited
There is Ag layers of PET base to lift from mixed solution B with 200 μm/s~500 μm/s pull rate to come out, then do at room temperature
Dry 1min~5min；
2., repeat step four 1. 3 times~10 times, obtain the H using PET as substrate2WO4·H2O/PEDOT films；
3., by the H using PET as substrate2WO4·H2O/PEDOT films cross heat sealing machine, obtain the soft of transparent quick response
Property electrochomeric films；
Step 4 3. described in heat sealing machine temperature be 100 DEG C~200 DEG C, the heat-sealing time be 1s~5s, heat-sealing pressure
For 0.1MPa.Other are identical with embodiment one.
Embodiment three：The difference of present embodiment and embodiment one or two is：It is described to electrode
For PET-ITO；Described PET-ITO is that ITO conductive layer is covered on the pet substrate, is obtained to electrode.Other and specific embodiment party
Formula one or two is identical.
ITO conductive layer described in present embodiment is tin indium oxide.
Embodiment four：The difference of present embodiment and embodiment one to three is：Described electrolyte
Layer is the lithium perchlorate carbonic allyl ester solution that concentration is 0.1mol/L~1mol/L, the system of lithium perchlorate carbonic allyl ester solution
Preparation Method is：Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbon that concentration is 0.1mol/L~1mol/L is obtained
Acid propylene ester solution.Other are identical with embodiment one to three.
Embodiment five：The difference of present embodiment and embodiment one to four is：Described resin is
Epoxy resin；Described epoxy resin is TDE-85.Other are identical with embodiment one to four.
Embodiment six：The difference of present embodiment and embodiment one to five is：Described electrolyte
Layer is the lithium perchlorate carbonic allyl ester solution that concentration is 0.1mol/L, the preparation method of lithium perchlorate carbonic allyl ester solution
For：Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbonic allyl ester solution that concentration is 0.1mol/L is obtained.Its
He is identical with embodiment one to five.
Embodiment seven：The difference of present embodiment and embodiment one to six is：Described electrolyte
Layer is the lithium perchlorate carbonic allyl ester solution that concentration is 0.5mol/L, the preparation method of lithium perchlorate carbonic allyl ester solution
For：Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbonic allyl ester solution that concentration is 0.5mol/L is obtained.Its
He is identical with embodiment one to six.
Embodiment eight：The difference of present embodiment and embodiment one to seven is：Described electrolyte
Layer is the lithium perchlorate carbonic allyl ester solution that concentration is 1mol/L, and the preparation method of lithium perchlorate carbonic allyl ester solution is：
Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbonic allyl ester solution that concentration is 1mol/L is obtained.Other with
Embodiment one to seven is identical.
Embodiment nine：The difference of present embodiment and embodiment one to eight is：Described in step 2
Magnetically controlled sputter method parameter it is specific as follows：Target is Ag targets, and sputtering type is d.c. sputtering, and target-cardinal distance is 15cm, gas
Flow is argon gas 5sccm, and depositing temperature is room temperature, and deposition pressure is 3Pa, and sputtering power is 15W, and sedimentation time is 25s.Other
It is identical with embodiment one to eight.
Embodiment ten：Present embodiment is a kind of flexible electro-chromic device of quick response as wearable electricity
Sub- product is in smart electronics product scope application.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：A kind of flexible electro-chromic device of quick response includes：Working electrode, to electrode and electrolyte
Layer, wherein working electrode are the flexible electrochomeric films of transparent quick response；It is PET-ITO to electrode；At dielectric substrate
In working electrode and between electrode；The flexible electro-chromic device edge of described quick response is packaged using resin；
The flexible electrochomeric films of described transparent quick response are prepared as follows：
First, flexible substrates are cleaned by ultrasonic 25min respectively in acetone, methanol and ultra-pure water successively, placing into temperature is
12h, the flexible substrates cleaned are dried at 50 DEG C；
Flexible substrates described in step one are the PET base that surface is covered with that thickness is 60nmEVA glue；
2nd, Ag layers are prepared：Use magnetically controlled sputter method EVA glue in the flexible substrates of cleaning surface sputter thickness for
30nm Ag sedimentaries, obtaining surface deposition has Ag layers of PET base；
The parameter of magnetically controlled sputter method described in step 2 is specific as follows：Target is Ag targets, and sputtering type is splashed for direct current
Penetrate, target-cardinal distance is 15cm, gas flow is argon gas 5sccm, and depositing temperature is room temperature, and deposition pressure is 3Pa, and sputtering power is
15W, sedimentation time is 25s；
3rd, mixed solution B is prepared：
1. the sodium tungstate solution mixing that, sulfuric acid and concentration for being 0.01mol/L by concentration are 0.01mol/L, adds matter
The hydrogen peroxide that fraction is 30% is measured, adds ultra-pure water, then low whipping speed to stir 8min under 800r/min, obtains mixing molten
Liquid A；Mixed solution A is stood to 6 days at room temperature, yellow mercury oxide material, as H is obtained2WO4·H2O；
Step 3 1. described in concentration be 0.01mol/L sulfuric acid and concentration be 0.01mol/L sodium tungstate solution
Volume ratio is 1:1；
Step 3 1. described in concentration be 0.01mol/L sulfuric acid and mass fraction be 30% hydrogen peroxide volume ratio
For 1:0.05；
Step 3 1. described in concentration be 0.01mol/L sulfuric acid and the volume ratio of ultra-pure water be 1:5；
2. the use of ultra-pure water is, solvent, by H2WO4·H2O is centrifuged in 8min, removal in the case where centrifugal speed is 5000r/min
Clear liquid；
3., repeat step three 2. 4 times, the H after being cleaned2WO4·H2O；
4., by the H after cleaning2WO4·H2O is distributed in ultra-pure water, obtains the H that mass fraction is 5%2WO4·H2O is molten
Liquid；To the H that mass fraction is 5%2WO4·H2The cetyl trimethyl bromination that mass fraction is 0.002% is added in O solution
Ammonium salt solution, adds the PEDOT that mass fraction is 5%:PSS solution, then low whipping speed is stirs 20min under 800r/min,
Obtain mixed solution B；
Step 3 4. described in mass fraction be 5% H2WO4·H2O solution and mass fraction are the 16 of 0.002%
The volume ratio of alkyl trimethyl ammonium bromide solution is 1:0.2；
Step 3 4. described in mass fraction be 5% H2WO4·H2O solution and the PEDOT that mass fraction is 5%:
The volume ratio of PSS solution is 1:0.2；
4th, H is prepared2WO4·H2O/PEDOT films：
1. the PET base that, depositing surface has Ag layers is immersed in 2min in mixed solution B, then surface deposition is had into Ag layers
PET base lifted and come out from mixed solution B with 300 μm/s pull rate, then be dried at room temperature for 3min；
2., repeat step four 1. 3 times, obtain the H using PET as substrate2WO4·H2O/PEDOT films；
3., by the H using PET as substrate2WO4·H2O/PEDOT films cross heat sealing machine, obtain the soft of transparent quick response
Property electrochomeric films；
Step 4 3. described in heat sealing machine temperature be 100 DEG C, the heat-sealing time be 3s, heat-sealing pressure be 0.1MPa；
Described PET-ITO is that ITO conductive layer is covered on the pet substrate, is obtained to electrode；Described ITO conductions are oxygen
Change indium tin；
Described dielectric substrate is the lithium perchlorate carbonic allyl ester solution that concentration is 0.5mol/L, lithium perchlorate carbonic acid third
The preparation method of alkene ester solution is：Lithium perchlorate is dissolved into propene carbonate, the perchloric acid that concentration is 0.5mol/L is obtained
Lithium carbonic allyl ester solution；
Described resin is epoxy resin；Described epoxy resin is TDE-85.
Fig. 1 schemes for the SEM of the flexible electrochomeric films of the transparent quick response prepared in embodiment one；Can from Fig. 1
Know, the flexible electrochomeric films of the transparent quick response prepared in embodiment one are the tungstic acid of laminated structure, (wherein
The PEDOT being mixed into is less and showed in SEM figures unobvious due to content).
Fig. 2 be embodiment one in a kind of quick response flexible electro-chromic device digital photograph figure；Can from Fig. 2
Know, the flexibility of the flexible electro-chromic device for the transparent quick response that embodiment one is obtained is good.
Fig. 3 is a kind of structural representation of the flexible electro-chromic device of quick response in embodiment one, and 1 is in Fig. 3
The flexible electrochomeric films of transparent quick response, 2 be dielectric substrate, and 3 be that 4 be resin to electrode PET-ITO.Can from Fig. 3
Know, a kind of flexible electro-chromic device of quick response in embodiment one includes：Working electrode, to electrode and dielectric substrate,
Wherein working electrode is the flexible electrochomeric films of transparent quick response；It is PET-ITO to electrode；Dielectric substrate is in work
Make electrode and between electrode；The flexible electro-chromic device edge of described quick response is packaged using resin.
Fig. 4 uses chronoamperometry in 900nm for a kind of flexible electro-chromic device of quick response in embodiment one
Place, transmitance-time graph under+3V~-3V tests；As can be seen from Figure 4, the flexible electrical of a kind of quick response in embodiment one
Mutagens color device is at 900nm, and transmitance in+3V~-3V is stable, the response time it is short (needed for transmitance change 90% when
Between be the response time), bleaching time is 5s, and coloration time is 9s, excellent performance.
Claims (5)
1. a kind of a kind of flexible electro-chromic device of quick response, it is characterised in that flexible electro-chromic device of quick response
Including：Working electrode, to electrode and dielectric substrate, wherein working electrode is thin for the flexible electrochromism of transparent quick response
Film；It is PET-ITO to electrode；Dielectric substrate is in working electrode and between electrode；Described quick response it is flexible electroluminescent
Electrochromic device edge is packaged using resin；
The flexible electrochomeric films of described transparent quick response are prepared as follows：
First, flexible substrates are cleaned by ultrasonic 20min~30min in acetone, methanol and ultra-pure water successively respectively, place into temperature
To dry 10h~15h, the flexible substrates cleaned at 40 DEG C~60 DEG C；
Flexible substrates described in step one are the PET base that surface is covered with that thickness is 20nm~100nmEVA glue；
2nd, Ag layers are prepared：Use magnetically controlled sputter method EVA glue in the flexible substrates of cleaning surface sputter thickness for 10nm~
50nm Ag sedimentaries, obtaining surface deposition has Ag layers of PET base；
The parameter of magnetically controlled sputter method described in step 2 is specific as follows：Target is Ag targets, and sputtering type is d.c. sputtering,
Target-cardinal distance is 10cm~20cm, and gas flow is argon gas 1sccm~10sccm, and depositing temperature is room temperature, and deposition pressure is 2Pa
~4Pa, sputtering power is 10W~20W, and sedimentation time is 10s~40s；
3rd, mixed solution B is prepared：
1., the sodium tungstate solution that the sulfuric acid and concentration for being 0.01mol/L~1mol/L by concentration are 0.01mol/L~1mol/L is mixed
Close, add the hydrogen peroxide that mass fraction is 30%, add ultra-pure water, then low whipping speed is 500r/min~1000r/
5min~10min is stirred under min, mixed solution A is obtained；Mixed solution A is stood to 5 days~7 days at room temperature, yellow is obtained and sinks
Starch matter, as H2WO4·H2O；
Step 3 1. described in concentration be 0.01mol/L~1mol/L sulfuric acid and concentration be 0.01mol/L~1mol/L's
The volume ratio of sodium tungstate solution is 1:1；
Step 3 1. described in concentration be 0.01mol/L~1mol/L sulfuric acid and mass fraction be 30% hydrogen peroxide body
Product is than being 1:(0.01~0.1)；
Step 3 1. described in concentration be 0.01mol/L~1mol/L sulfuric acid and the volume ratio of ultra-pure water be 1:(1~10)；
2. the use of ultra-pure water is, solvent, by H2WO4·H2O centrifuges 5min in the case where centrifugal speed is 2000r/min~8000r/min
~10min, removes supernatant；
3., repeat step three 2. 3 times~5 times, the H after being cleaned2WO4·H2O；
4., by the H after cleaning2WO4·H2O is distributed in ultra-pure water, obtains the H that mass fraction is 5%~50%2WO4·H2O is molten
Liquid；To the H that mass fraction is 5%~50%2WO4·H2In O solution add mass fraction be 0.002%~0.01% 16
Alkyl trimethyl ammonium bromide solution, adds the PEDOT that mass fraction is 5%~30%:PSS solution, then low whipping speed is
10min~30min is stirred under 500r/min~1000r/min, mixed solution B is obtained；
Step 3 4. described in mass fraction be 5%~50% H2WO4·H2O solution and mass fraction be 0.002%~
The volume ratio of 0.01% cetyl trimethylammonium bromide solution is 1:(0.05~0.5)；
Step 3 4. described in mass fraction be 5%~50% H2WO4·H2O solution is 5%~30% with mass fraction
PEDOT:The volume ratio of PSS solution is 1:(0.05~0.5)；
4th, H is prepared2WO4·H2O/PEDOT films：
1. the PET base that, depositing surface has Ag layers is immersed in 1min~3min in mixed solution B, then surface deposition is had into Ag
The PET base of layer is lifted with 200 μm/s~500 μm/s pull rate from mixed solution B to be come out, then is dried at room temperature for
1min~5min；
2., repeat step four 1. 3 times~10 times, obtain the H using PET as substrate2WO4·H2O/PEDOT films；
3., by the H using PET as substrate2WO4·H2O/PEDOT films cross heat sealing machine, obtain the flexible electrical of transparent quick response
Cause optically variable films；
Step 4 3. described in heat sealing machine temperature be 100 DEG C~200 DEG C, the heat-sealing time be 1s~5s, seal pressure be
0.1MPa；
Described is PET-ITO to electrode；Described PET-ITO is that ITO conductive layer is covered on the pet substrate, is obtained to electrode；
Described dielectric substrate is the lithium perchlorate carbonic allyl ester solution that concentration is 0.1mol/L~1mol/L, lithium perchlorate carbon
The preparation method of acid propylene ester solution is：Lithium perchlorate is dissolved into propene carbonate, obtain concentration for 0.1mol/L~
1mol/L lithium perchlorate carbonic allyl ester solution；
Described resin is epoxy resin；Described epoxy resin is TDE-85.
2. a kind of flexible electro-chromic device of quick response according to claim 1, it is characterised in that described electrolysis
Matter layer is the lithium perchlorate carbonic allyl ester solution that concentration is 0.1mol/L, the preparation method of lithium perchlorate carbonic allyl ester solution
For：Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbonic allyl ester solution that concentration is 0.1mol/L is obtained.
3. a kind of flexible electro-chromic device of quick response according to claim 1, it is characterised in that described electrolysis
Matter layer is the lithium perchlorate carbonic allyl ester solution that concentration is 0.5mol/L, the preparation method of lithium perchlorate carbonic allyl ester solution
For：Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbonic allyl ester solution that concentration is 0.5mol/L is obtained.
4. a kind of flexible electro-chromic device of quick response according to claim 1, it is characterised in that described electrolysis
Matter layer is the lithium perchlorate carbonic allyl ester solution that concentration is 1mol/L, the preparation method of lithium perchlorate carbonic allyl ester solution
For：Lithium perchlorate is dissolved into propene carbonate, the lithium perchlorate carbonic allyl ester solution that concentration is 1mol/L is obtained.
5. a kind of flexible electro-chromic device of quick response according to claim 1, it is characterised in that institute in step 2
The parameter for the magnetically controlled sputter method stated is specific as follows：Target is Ag targets, and sputtering type is d.c. sputtering, and target-cardinal distance is 15cm,
Gas flow is argon gas 5sccm, and depositing temperature is room temperature, and deposition pressure is 3Pa, and sputtering power is 15W, and sedimentation time is 25s.
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| CN103966583A (en) * | 2014-05-07 | 2014-08-06 | 哈尔滨工业大学 | Preparation method for electrochromic polyaniline film on surface of flexible gold film |
| CN104216192A (en) * | 2014-09-16 | 2014-12-17 | 哈尔滨工业大学 | Preparation method of novel fast-response high-contrast electrochromic device |
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| CN103969904A (en) * | 2014-05-26 | 2014-08-06 | 电子科技大学 | Preparation method for flexible electrochromic layer and device |
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