CN103123431A - Electrochromism device and application thereof based on polythiophene and ramification thereof and ionic liquid electrolyte - Google Patents
Electrochromism device and application thereof based on polythiophene and ramification thereof and ionic liquid electrolyte Download PDFInfo
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- CN103123431A CN103123431A CN2013100481100A CN201310048110A CN103123431A CN 103123431 A CN103123431 A CN 103123431A CN 2013100481100 A CN2013100481100 A CN 2013100481100A CN 201310048110 A CN201310048110 A CN 201310048110A CN 103123431 A CN103123431 A CN 103123431A
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Abstract
The invention provides an electrochromism device based on polythiophene and ramification thereof and ionic liquid electrolyte. The electrochromism device comprises a first electrode, a second electrode opposite to the first electrode and an electrolyte layer arranged between the first electrode and the second electrode. The first electrode is composed of a transparent conductive ITO glass substrate and the polythiophene and the ramification PProDOT-Me2 of the polythiophene which are deposited on the glass substrate. The second electrode is composed of a transparent conductive ITO glass substrate and inorganic metallic oxide vanadium pentoxide (V2O5) which are deposited on the glass substrate. Due to adoption of a new matching method, the electrochromism material PProDOT-Me2, the V2O5 and the ionic liquid electrolyte are organically combined so that the problem that the environment of water and oxygen insulation is needed in the process of assembly of the electrochromism device is solved and difficulty and cost of manufacturing the device are greatly reduced. The electrochromism device has the advantages that matching performance is outstanding, transmittance difference is high, service life is long, working performance is stable under high temperature and manufacture technology can be commercially popularized and the like. The electrochromism device is applicable to a car, aerospace and a building in an area in extreme climate.
Description
Technical field
The invention belongs to the electrochromic device technical field, be specifically related to a kind of electrochromic device and application thereof based on polythiophene and derivant and ionic liquid electrolyte.
Background technology
The electrochromism phenomenon refers to that the phenomenon of stable, reversible chemical change occurs the optical properties (reflectivity, transmitance, absorptivity etc.) of material, shows as the reversible variation of color or transparency in appearance under the effect of extra electric field.Material with electrochromic property is called electrochromic material, utilizes the device with controllable color change function that this material is prepared into to be called as intelligence or electrochromic device (electrochromic device, ECD).
Electrochromic optionally absorbs under electric field action or reflection External Heat Flux and the diffusion of prevention internal heat, therefore can reduce office building and the spent mass energy of private residence four seasons temperature control.In this simultaneously, electrochromic can be improved natural light illumination, peep-proof, and the effects such as anti-dazzle reduce indoor and outdoor shading facility.Along with the development of this technology, the Commercialization applications such as electrochromic, display, glareproof mirror are attracted attention by market gradually, and in today that energy crisis is day by day deepened, this Research Significance is very great.
Yet, in the electrochromic field, exist device high to encapsulating strict assembly cost at present; Device cycle life falls short of, and chemical property is stable not; Inflammable and the contaminated environment of device inside electrolytic solution when broken; The mission life urgent technical barrier such as obviously be affected at high temperature.
Compare with conventional solvent, ionic liquid has the special performances such as steam forces down, not volatile, conductivity is high, larger electrochemical window, stable chemical property and thermal behavior, reusable edible, environmental protection, is the perfect electrolyte of the electrochromic device of exploitation function admirable.
Summary of the invention
In order to address the above problem, the purpose of this invention is to provide a kind of electrochromic device and application thereof based on polythiophene and derivant and ionic liquid electrolyte.
In order to realize purpose of the present invention, provide following solution:
A kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte comprises:
The first electrode is by on the electrically conducting transparent ito glass substrate and the polythiophene and the derivant PProDOT-Me thereof that are deposited thereon
2Form;
With second electrode relative with this first electrode, by on electrically conducting transparent ITO (indium tin oxide-coated glass) glass substrate and the inorganic, metal oxide V that is deposited thereon
2O
5Form;
Be arranged on the dielectric substrate between described the first electrode and the second electrode.
Preferably, described dielectric substrate is ionic liquid.
Preferred, described ionic liquid is 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]), or 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]).
The present invention also provides the application of above-mentioned electrochromic device in the devices such as color-changing window, display, glareproof mirror or shadow shield are made.
Beneficial effect of the present invention is as follows:
Electrolyte 1-ethyl-3-methylimidazole hexafluorophosphate ([the EMIM] [PF that uses in the present invention
6]), and 1-ethyl-3-methylimidazole fluoroform sulphonate ([EMIM] [OTF]) is ionic liquid.With respect to common lithium salts and the carbonates electrolyte characteristics for airborne moisture, oxygen sensitive, the environmental stability of ionic liquid will exceed a lot.Assemble in the present invention ionic liquid and all do not use the glove box assembling as electrolytical device, only need to assemble stability and other chemical properties that can reach desirable under common indoor environment.And ionic liquid is moderate, and consumption is saved, and can greatly reduce the cost of making electrochromic.
The present invention utilizes new matching process, with electrochromic material PProDOT-Me
2, vanadium pentoxide (V
2O
5) and ionic liquid electrolyte organically combine, solved the environment that the electrochromic device assembling process needs exclusion of water oxygen, greatly reduce difficulty and cost that device is made.Be assembled into the superior electrochromic device of matching, have the transmitance difference high, long working life, stable work in work under high temperature, technology of preparing can business promotion etc. advantage, be applicable to automobile, Aero-Space, and the application on the buildings in extreme climate area.
Description of drawings
Fig. 1 is the structural representation of electrochromic device of the present invention;
Fig. 2 and Fig. 3 are electrochromic device fundamental diagram of the present invention;
Fig. 4 is electrochromic device pictorial diagram of the present invention;
Fig. 5 is the optical property of working electrode of the present invention in 1-ethyl-3-methylimidazole hexafluorophosphate;
Fig. 6 is the optical property of working electrode of the present invention in 1-ethyl-3-methylimidazole fluoroform sulphonate;
Fig. 7 is typical electrochromic device WO
3/ V
2O
5At electrolyte LiClO
4Optical property in+PC before circulation;
Fig. 8 is typical electrochromic device WO
3/ V
2O
5At electrolyte LiClO
4The optical property of 1,000 front and back of circulation in+PC;
Fig. 9 is typical electrochromic device WO
3/ V
2O
5Device is at electrolyte LiClO
4The discharge capability of circulation before 1,000 times in+PC;
Figure 10 is typical electrochromic device WO
3/ V
2O
5Device is at electrolyte LiClO
4The discharge capability of circulation after 1,000 times in+PC;
Figure 11 is the optical property in cyclic process repeatedly take 1-ethyl-3-methylimidazole hexafluorophosphate as electrolytical electrochromic device of the present invention;
Figure 12 is the optical property in cyclic process repeatedly take 1-ethyl-3-methylimidazole fluoroform sulphonate as electrolytical electrochromic device of the present invention;
Figure 13 is with LiClO
4+ PC is as electrolytical device PProDOT-Me
2/ V
2O
5Many potential steps curve in 25 ° of C environment;
Figure 14 is with LiClO
4+ PC is as electrolytical device PProDOT-Me
2/ V
2O
5Many potential steps curve in 65 ° of C environment;
Figure 15 is with LiClO
4+ PC is as electrolytical device PProDOT-Me
2/ V
2O
5Cyclic voltammetry curve in 25 ° of C and 65 ° of C environment;
Figure 16 is with [BMIM] [PF
6] as the many potential step curve of electrolytical device in 25 ° of C environment;
Figure 17 is with [BMIM] [PF
6] as the many potential step curve of electrolytical device in 65 ° of C environment;
Figure 18 is with [BMIM] [PF
6] as the cyclic voltammetry curve of electrolytical device in 25 ° of C and 65 ° of C environment;
Figure 19 with [BMIM] [OTF] as electrolytical device the many potential steps curve in the 25oC environment;
Figure 20 with [BMIM] [OTF] as the many potential step curve of electrolytical device in 65 ° of C environment;
Figure 21 with [BMIM] [OTF] as the cyclic voltammetry curve of electrolytical device in 25 ° of C and 65 ° of C environment.
Embodiment
Further describe by the following examples the present invention.
Ionic liquid 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]), 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) (the prompt ionic liquid of upper marine origin company limited);
Acetonitrile ACN, propene carbonate (PC), acetonitrile and propene carbonate carry out purifying before use;
Lithium perchlorate (LiClO
4) (purity 99%, anhydrous), polythiophene and derivant PProDOT-Me thereof
2(above medicine is purchased the Hill to Ward, MA, USA);
Electrochemical workstation 660D type (Shanghai China in morning company limited).
The preparation of embodiment 1 electrochromic device
The preparation process of the first electrode comprises: press bibliographical information (C.Kaneko, C.Xu, L.Liu, N.Dai, and M.Taya, Proc.of SPIE, vol.5759, pp.518,2005) method, the mode of acetonitrile solution by electroplating with the PProDOT-Me2 monomer makes the conducting polymer thin film deposition to the ito glass that is immersed in solution.Working electrode after film forming will carry out painted, the test of fading in electrochemical workstation.
The preparation process of the second electrode comprises: press the method for bibliographical information (C.Kaneko, C.Xu, L.Liu, N.Dai, and M.Taya, Proc.of SPIE, vol.5759, pp.518,2005), with V
2O
5The mode of colloidal sol by electroplating deposits to conductive film to be immersed on ito glass wherein.Electrode will be heat-treated after film forming, temperature preferable range are 80-150 ° of C, and the time, preferable range was at 10-20h.To carry out painted, the test of fading to electrode in electrochemical workstation equally.
The encapsulation of electrochromic device: with working electrode with to the surrounding of electrode stress glue bond, two plate electrodes are being full of ionic liquid between electrode under common laboratory condition after clamping, and use at last the gap of device on the UV rubber seal, guarantee inner vacuum tightness.The present invention prepares with ionic liquid as electrolytical typical electrochromic device PProDOT-Me
2/ V
2O
5The structure of electrochromic device, as shown in Figure 1.
During use, the both sides transparent conductive substrate is connected the 1.5V battery.Its principle of work is as follows: power supply is connected with the both sides electrode material by electric wire, and as cut-off switch A, during Closing Switch B, ion storage is in to electrode, and electrochromic layer is in bleached state, and device is clear, colorless (as shown in Figure 2); As cut-off switch B, Closing Switch A namely applies reverse voltage to device and drives ion to pass ion conductive layer from ion storage be electrolyte, enters electrochromic layer, and device is darkened (as shown in Figure 3).During deenergization, ion leaves electrochromic layer again, and device comes back to pellucidity.Like this, device has just been realized control and conversion (as shown in Figure 4) painted, bleached state.
The Performance Ratio of embodiment 2 electrochromic device of the present invention and other electrochromic devices
Comparative Examples one: use in electrochemical workstation 660D under the condition of 2.0V direct supply, with LiClO
4+ PC is as electrolytical typical electrochromic device WO
3/ V
2O
5, after circulation 1,000 times, significant change has just occured in its optical property.Solid line shown in Figure 7 and dotted line be respectively that this device fades before circulation and colored state under transmitance, reach transmitance difference maximal value 35% at the 540nm place.Solid line shown in Figure 8 and dotted line be respectively this device circulation fade after 1,000 times and colored state under transmitance, reach transmitance difference maximal value 30% at the 540nm place.Can find out by contrast, the discoloration of this typical electrochromic device is very limited, and particularly after circulation 1,000 times, optical property obviously descends.
In addition, in conjunction with the charging and discharging capabilities before and after Fig. 9 and this device circulation shown in Figure 10, can contrast draw circulation 1,000 times after, its ability that discharges and recharges obviously descends.
Comparative Examples two: use in electrochemical workstation 660D under the condition of 1.5V direct supply, with LiClO
4+ PC is as electrolytical typical electrochromic device PProDOT-Me
2/ V
2O
5, the temperature that raises in 20-65 ° of C scope (5 °, interval C adjusts a temperature, measurement data after each temperature stabilization) adopts many potential step methods and cyclic voltammetry to device detection.From 25 ° of C(as shown in figure 13) and 65 ° of C(as shown in figure 14) time many potential steps curve contrast can find out, the chemical property of device changes significantly; Device cyclic voltammetry curve (as shown in figure 15) at two temperature can find out that also (sweep velocity: 100mV/s), chemical property changes greatly.
Typically with LiClO
4+ PC is as electrolytical typical electrochromic device WO
3/ V
2O
5, after circulation 1,000 times, obvious decline has just occured in its optical property and chemical property, continues the normal use that circulation even can affect device.In addition, existing with LiClO
4+ PC is as electrolytical typical electrochromic device PProDOT-Me
2/ V
2O
5, the temperature that raises in 20-65 ° of C scope, its cycle performance can suffer irreversible destruction, can not continue normal operation.
The present invention is under the condition of using the 1.5V direct supply, with 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]) as electrolytical working electrode, transmitance (T when being in bleached state
t(λ)) remain on more than 40% in 300～1000nm scope, 600nm obtains at the place solid line in maximal value 81%(Fig. 5), and transmitance (T during colored state
d(λ)) dotted line in the 580nm place obtains minimum value 4%(Fig. 5), namely this moment working electrode transmitance difference (△ %T=T
t(λ)-T
d(λ)) reaching maximum at the 580nm place, is 75%; The device of making is detected, and transmitance difference (△ %T) is curve in the 580nm place reaches maximal value 57%(Figure 11).This shows that this device has good optical property.
With 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) as electrolytical working electrode, transmitance when being in bleached state (T%) remains on more than 40% in 300～1000nm scope, 400nm obtains maximal value 87%(Fig. 5 solid line in the left and right), and transmitance (T%) obtains minimum value 3%(Fig. 5 dotted line at the 580nm place during colored state), namely this moment working electrode transmitance difference (△ %T=T
t(λ)-T
d(λ)) reaching maximum at the 580nm place, is 78%; The device of making is detected, and transmitance difference (△ %T) reaches maximal value 62%(Figure 12 curve at the 580nm place).This shows that this device has good optical property equally.
The electrolytical contrast experiment of embodiment 3 electrochromic devices
Example one: use in electrochemical workstation 660D under the condition of 1.5V direct supply, with 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]) as electrolytical electrochromic device, 50,000 cyclic voltammetrics of circulating (sweep velocity: 100m/s), the transmitance difference △ %T in 200～1000nm scope obtains maximal value 54%(table 1 at the 580nm place); 100,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T in this scope obtains maximal value 45%(table 1 at the 580nm place) circulate.Be that after device circulates through 100,000 times, optical property has only descended 9%.
Example two: use in electrochemical workstation 660D under the condition of 1.5V direct supply, with 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) as electrolytical electrochromic device, 50,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T in 200～1000nm scope obtains maximal value 59%(table 1 at the 580nm place) circulate; 100,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T in this scope obtains maximal value 52%(table 1 at the 580nm place) circulate.Be that after device circulates through 100,000 times, optical property has only descended 7%.
Table 1: be respectively electrolytical device in the maximum transmission difference of repeatedly cyclic process with two kinds of ionic liquids
| ? | 5 circulations | 50,000 circulations | 100,000 circulations |
| [BMIM][PF 6] | 57% | 54% | 45% |
| [BMIM][OTF] | 62% | 59% | 52% |
Example three: use in electrochemical workstation 660D under the condition of 1.5V direct supply, with 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]) as electrolytical electrochromic device, the temperature that raises in 20～65 ° of C scopes (5 °, interval C adjusts a temperature, measurement data after each temperature stabilization) adopts many potential step methods and cyclic voltammetry to device detection.From 25 ° of C(Figure 16) and 65 ° of C(Figure 17) time many potential steps curve contrast can find out, the chemical property of device almost changes very little; Device cyclic voltammetry curve (Figure 18) at two temperature can find out that also (sweep velocity: 100m/s), chemical property changes little.
Be not difficult to find out in conjunction with three examples, in the temperature range of room temperature to 65 ° C, the temperature stability of this device is better.
Example four: use in electrochemical workstation 660D under the condition of 1.5V direct supply, with 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) as electrolytical electrochromic device, (5 °, interval C adjusts a temperature to the temperature that raises in 20～65 ° of C scopes, measurement data after each temperature stabilization), adopt many potential step methods and cyclic voltammetry to device detection.From 25 ° of C(Figure 19) and 65 ° of C(Figure 20) time many potential steps curve contrast can find out, the chemical property of device almost changes very little; Device cyclic voltammetry curve (Figure 21) at two temperature can find out that also (sweep velocity: 100m/s), chemical property changes little.This example is not difficult to find out in conjunction with example three, and in the temperature range of room temperature to 65 ° C, the temperature stability of this device is better.
The above is only the preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. the electrochromic device based on polythiophene and derivant and ionic liquid electrolyte, is characterized in that, comprising:
The first electrode is by on the electrically conducting transparent ito glass substrate and the polythiophene and the derivant PProDOT-Me thereof that are deposited thereon
2Form;
With second electrode relative with this first electrode, by on the electrically conducting transparent ito glass substrate and the inorganic, metal oxide V that is deposited thereon
2O
5Form;
Be arranged on the dielectric substrate between described the first electrode and the second electrode.
2. electrochromic device according to claim 1, is characterized in that, described dielectric substrate is ionic liquid.
3. electrochromic device according to claim 2, is characterized in that, described ionic liquid is 1-ethyl-3-methylimidazole hexafluorophosphate or 1-ethyl-3-methylimidazole fluoroform sulphonate.
4. the application during the device such as color-changing window, display, glareproof mirror or the shadow shield of the described electrochromic device of claim 1～3 any one in buildings is made.
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|---|---|---|---|
| CN201310048110.0A CN103123431B (en) | 2013-02-06 | 2013-02-06 | A kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte and application thereof |
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Cited By (8)
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| CN104280982A (en) * | 2013-07-11 | 2015-01-14 | 文霞 | Imaging device and filtering switching module thereof |
| CN104375350A (en) * | 2014-10-31 | 2015-02-25 | 合肥博一环保科技有限公司 | Multifunctional controllable electrochromic device and manufacturing method thereof |
| CN105093770A (en) * | 2015-09-28 | 2015-11-25 | 张健敏 | Display screen shell capable of adjusting light transmittance and manufacturing method of display screen shell |
| CN105925246A (en) * | 2016-04-16 | 2016-09-07 | 吉林大学 | Electricity generated acid produced by blending substances with changeable oxidation state and electrolyte and applications thereof |
| CN106711778A (en) * | 2016-12-13 | 2017-05-24 | 深圳明创自控技术有限公司 | Visual switch cabinet |
| CN109651602A (en) * | 2018-12-12 | 2019-04-19 | 浙江工业大学 | A kind of preparation method of quick response electrochromism PTBTPA film |
| CZ309645B6 (en) * | 2022-04-12 | 2023-06-07 | Novák Marek Ing. | Electrochromic display |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104280982A (en) * | 2013-07-11 | 2015-01-14 | 文霞 | Imaging device and filtering switching module thereof |
| CN104199228A (en) * | 2014-09-26 | 2014-12-10 | 哈尔滨工业大学 | Electrochromic device (ECD) taking poly 3, 4-ethylenedioxy thiophene and vanadium pentoxide as electrochromism electrode materials and application thereof |
| CN104375350A (en) * | 2014-10-31 | 2015-02-25 | 合肥博一环保科技有限公司 | Multifunctional controllable electrochromic device and manufacturing method thereof |
| CN104375350B (en) * | 2014-10-31 | 2017-04-19 | 合肥博一环保科技有限公司 | Multifunctional controllable electrochromic device and manufacturing method thereof |
| CN105093770A (en) * | 2015-09-28 | 2015-11-25 | 张健敏 | Display screen shell capable of adjusting light transmittance and manufacturing method of display screen shell |
| CN105925246A (en) * | 2016-04-16 | 2016-09-07 | 吉林大学 | Electricity generated acid produced by blending substances with changeable oxidation state and electrolyte and applications thereof |
| CN106711778A (en) * | 2016-12-13 | 2017-05-24 | 深圳明创自控技术有限公司 | Visual switch cabinet |
| CN109651602A (en) * | 2018-12-12 | 2019-04-19 | 浙江工业大学 | A kind of preparation method of quick response electrochromism PTBTPA film |
| CZ309645B6 (en) * | 2022-04-12 | 2023-06-07 | Novák Marek Ing. | Electrochromic display |
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