CN103123431B - A kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte and application thereof - Google Patents
A kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte and application thereof Download PDFInfo
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- CN103123431B CN103123431B CN201310048110.0A CN201310048110A CN103123431B CN 103123431 B CN103123431 B CN 103123431B CN 201310048110 A CN201310048110 A CN 201310048110A CN 103123431 B CN103123431 B CN 103123431B
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Abstract
The invention provides a kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte, it comprises: the first electrode, by electrically conducting transparent ito glass substrate and the polythiophene be deposited thereon and derivant PProDOT-Me thereof
2composition; And second electrode relative with this first electrode, by electrically conducting transparent ito glass substrate and the inorganic, metal oxide V that is deposited thereon
2o
5composition; Be arranged on the dielectric substrate between described first electrode and the second electrode.The present invention utilizes new matching process, by electrochromic material PProDOT-Me
2, vanadium pentoxide (V
2o
5) and ionic liquid electrolyte combination, solve the environment that electrochromic device assembling process needs exclusion of water oxygen, greatly reduce difficulty and the cost of device manufacture.Be assembled into the electrochromic device that matching is superior, have transmitance difference high, long working life, stable work in work under high temperature, technology of preparing can the advantage such as business promotion, is applicable to automobile, Aero-Space, and the application on the buildings in extreme climate area.
Description
Technical field
The invention belongs to electrochromic device technical field, be specifically related to a kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte and application thereof.
Background technology
Electrochromism phenomenon refers to that the phenomenon of stable, reversible chemical change occurs the optical properties (reflectivity, transmitance, absorptivity etc.) of material under the effect of extra electric field, shows as the reversible change of color or transparency in appearance.The material with electrochromic property is called electrochromic material, and the device with controllable color change function utilizing this material to be prepared into is called as intelligence or electrochromic device (electrochromicdevice, ECD).
Electrochromic optionally absorbs under electric field action or reflect ambient heat radiation is spread with prevention internal heat, therefore can reduce office building and the mass energy spent by private residence four seasons temperature control.Simultaneously, electrochromic can improve natural light illumination, peep-proof, the effects such as anti-dazzle, reduces indoor and outdoor shading facility.Along with the development of this technology, the Commercialization applications such as electrochromic, display, glareproof mirror gradually attract attention by market, in today that energy crisis is day by day deepened, this Research Significance is very great.
But, at present in electrochromic field, there is device and encapsulation is required that strict assembly cost is high; The device cycle life-span falls short of, and chemical property is stable not; Device inside electrolytic solution inflammable and contaminated environment time broken; At high temperature mission life such as to be obviously affected at the urgent technical barrier.
Compared with conventional solvent, the special performances such as the electrochemical window that ionic liquid has steam to force down, not volatile, conductivity is high, larger, stable chemical property and thermal behavior, reusable edible, environmental protection are the perfect electrolytes of the electrochromic device of exploitation function admirable.
Summary of the invention
In order to solve the problem, the object of this invention is to provide a kind of electrochromic device based on polythiophene and derivant and ionic liquid electrolyte and application thereof.
In order to realize object of the present invention, provide following solution:
Based on an electrochromic device for polythiophene and derivant and ionic liquid electrolyte, comprising:
First electrode, by electrically conducting transparent ito glass substrate and the polythiophene that is deposited thereon and derivant PProDOT-Me thereof
2composition;
And second electrode relative with this first electrode, by electrically conducting transparent ITO (indium tin oxide-coated glass) glass substrate and the inorganic, metal oxide V that is deposited thereon
2o
5composition;
Be arranged on the dielectric substrate between described 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]).
Present invention also offers the application of above-mentioned electrochromic device in the devices such as color-changing window, display, glareproof mirror or shadow shield make.
Beneficial effect of the present invention is as follows:
Electrolyte 1-ethyl-3-methylimidazole hexafluorophosphate ([the EMIM] [PF used in the present invention
6]), and 1-ethyl-3-methylimidazole fluoroform sulphonate ([EMIM] [OTF]) is ionic liquid.Relative to common lithium salts and carbonates electrolyte for the feature of the moisture in air, oxygen sensitive, the environmental stability of ionic liquid will exceed a lot.Assembling ionic liquid in the present invention does not all use glove box to assemble as electrolytical device, only need assemble the stability that can reach desirable and other chemical properties under common indoor environment.And ionic liquid is moderate, consumption is saved, and greatly can reduce the cost making electrochromic.
The present invention utilizes new matching process, by electrochromic material PProDOT-Me
2, vanadium pentoxide (V
2o
5) and ionic liquid electrolyte combination, solve the environment that electrochromic device assembling process needs exclusion of water oxygen, greatly reduce difficulty and the cost of device manufacture.Be assembled into the electrochromic device that matching is superior, have transmitance difference high, long working life, stable work in work under high temperature, technology of preparing can the advantage such as business promotion, is applicable to automobile, Aero-Space, and the application on the buildings in extreme climate area.
Accompanying drawing explanation
Fig. 1 is the structural representation of electrochromic device of the present invention;
Fig. 2 and Fig. 3 is 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 circulation 1,000 front and back in+PC;
Fig. 9 is typical electrochromic device WO
3/ V
2o
5device is at electrolyte LiClO
4circulate in+PC the discharge capability before 1,000 times;
Figure 10 is typical electrochromic device WO
3/ V
2o
5device is at electrolyte LiClO
4circulate in+PC the discharge capability after 1,000 times;
Figure 11 is be the optical property of electrolytical electrochromic device of the present invention repeatedly in cyclic process with 1-ethyl-3-methylimidazole hexafluorophosphate;
Figure 12 is be the optical property of electrolytical electrochromic device of the present invention repeatedly in cyclic process with 1-ethyl-3-methylimidazole fluoroform sulphonate;
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 ° 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 ° C environment;
The many potential step curve of Figure 19 using [BMIM] [OTF] as electrolytical device in 25oC environment;
The many potential step curve of Figure 20 using [BMIM] [OTF] as electrolytical device in 65 ° of C environment;
The cyclic voltammetry curve of Figure 21 using [BMIM] [OTF] as electrolytical device in 25 ° of C and 65 ° C environment.
Embodiment
Further describe the present invention by the following examples.
Ionic liquid 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]), 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) (the prompt ionic liquid company limited of upper marine origin);
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 to WardHill, MA, USA);
Electrochemical workstation 660D type (Shanghai Chen Hua company limited).
The preparation of embodiment 1 electrochromic device
The preparation process of the first electrode comprises: by bibliographical information (C.Kaneko, C.Xu, L.Liu, N.Dai, andM.Taya, Proc.ofSPIE, vol.5759, pp.518,2005) method, by the mode of the acetonitrile solution of PProDOT-Me2 monomer by plating, polymeric conductor films is deposited on leaching ito glass in the solution.Working electrode after film forming will carry out painted, test of fading in electrochemical workstation.
The preparation process of the second electrode comprises: by the method for bibliographical information (C.Kaneko, C.Xu, L.Liu, N.Dai, andM.Taya, Proc.ofSPIE, vol.5759, pp.518,2005), by V
2o
5colloidal sol, by the mode of plating, makes conductive film deposit to be immersed on ito glass wherein.Will heat-treat electrode after film forming, temperature preferable range is 80-150 ° of C, and the time, preferable range was at 10-20h.Painted, test of fading to be carried out in electrochemical workstation equally to electrode.
The encapsulation of electrochromic device: by working electrode with to the surrounding of electrode stress glue bond, after the clamping of two panels electrode, is full of ionic liquid, finally uses the gap of device in UV rubber seal, guarantee inner vacuum tightness under common laboratory condition between electrode.The present invention's preparation is using ionic liquid as electrolytical typical electrochromic device PProDOT-Me
2/ V
2o
5the structure of electrochromic device, as shown in Figure 1.
During use, both sides transparent conductive substrate is connected 1.5V battery.Its principle of work is as follows: power supply is connected with both sides electrode material by electric wire, and as cut-off switch A, during Closing Switch B, ion storage is in electrode, and electrochromic layer is in bleached state, device transparent colourless (as shown in Figure 2); As cut-off switch B, Closing Switch A, namely reverse voltage is applied to device and drive ion to pass ion conductive layer and electrolyte from ion storage, enter electrochromic layer, device color is deepened (as shown in Figure 3).Again during deenergization, ion leaves electrochromic layer, and device comes back to pellucidity.Like this, device just achieves control and the conversion (as shown in Figure 4) of painted, bleached state.
The Performance comparision of embodiment 2 electrochromic device of the present invention and other electrochromic devices
Comparative example one: use the condition of 2.0V direct supply in electrochemical workstation 660D under, with LiClO
4+ PC is as electrolytical typical electrochromic device WO
3/ V
2o
5, after circulation 1,000 times, its optical property just there occurs significant change.Solid line shown in Fig. 7 and dotted line are respectively this device and fade before circulation and the transmitance under colored state, reach transmitance difference maximal value 35% at 540nm place.Solid line shown in Fig. 8 and dotted line are respectively this device and fade after circulation 1,000 times and transmitance under colored state, reach transmitance difference maximal value 30% at 540nm place.Can be found out by contrast, the discoloration of this typical electrochromic device is very limited, and particularly after circulation 1,000 times, optical property obviously declines.
In addition, the charging and discharging capabilities before and after this device cycle shown in composition graphs 9 and Figure 10, can contrast after drawing circulation 1,000 times, the ability of its discharge and recharge obviously declines.
Comparative example two: use the condition of 1.5V direct supply in electrochemical workstation 660D under, with LiClO
4+ PC is as electrolytical typical electrochromic device PProDOT-Me
2/ V
2o
5, within the scope of 20-65 ° of C, raised temperature (5 °, interval C adjusts a temperature, measurement data after each temperature stabilization), adopts many potential step methods and cyclic voltammetry to device detection.As can be seen from 25 ° of C(as shown in figure 13) and 65 ° of C(as shown in figure 14) time many potential steps curve control, the chemical property of device changes significantly; Device cycle volt-ampere curve (as shown in figure 15) at two temperature also can be found out (sweep velocity: 100mV/s), and chemical property changes greatly.
Typical in LiClO
4+ PC is as electrolytical typical electrochromic device WO
3/ V
2o
5, after circulation 1,000 times, its optical property and chemical property just there occurs obvious decline, continue 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, raised temperature within the scope of 20-65 ° of C, its cycle performance can suffer irreversible destruction, can not continue normal work.
The present invention under the condition using 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)) within the scope of 300 ~ 1000nm, remain on more than 40%, 600nm place and obtain solid line in maximal value 81%(Fig. 5), and transmitance (T during colored state
d(λ)) dotted line in minimum value 4%(Fig. 5 is obtained at 580nm place), i.e. now working electrode transmitance difference (△ %T=T
t(λ)-T
d(λ)) reaching maximum at 580nm place, is 75%; Detect the device made, transmitance difference (△ %T) reaches curve in maximal value 57%(Figure 11 at 580nm place).This device has good optical property as can be seen here.
Using 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) as electrolytical working electrode, when being in bleached state, transmitance (T%) remains on more than 40% within the scope of 300 ~ 1000nm, about 400nm obtains maximal value 87%(Fig. 5 solid line), and transmitance (T%) obtains minimum value 3%(Fig. 5 dotted line at 580nm place during colored state), i.e. now working electrode transmitance difference (△ %T=T
t(λ)-T
d(λ)) reaching maximum at 580nm place, is 78%; Detect the device made, transmitance difference (△ %T) reaches maximal value 62%(Figure 12 curve at 580nm place).This device has good optical property equally as can be seen here.
The electrolytical contrast experiment of embodiment 3 electrochromic device
Example one: use the condition of 1.5V direct supply in electrochemical workstation 660D under, with 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]) as electrolytical electrochromic device, circulate after 50,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T within the scope of 200 ~ 1000nm obtains maximal value 54%(table 1 at 580nm place); Circulate after 100,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T within the scope of this obtains maximal value 45%(table 1 at 580nm place).Namely device is after 100,000 circulations, and optical property only have dropped 9%.
Example two: use the condition of 1.5V direct supply in electrochemical workstation 660D under, using 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) as electrolytical electrochromic device, circulate after 50,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T within the scope of 200 ~ 1000nm obtains maximal value 59%(table 1 at 580nm place); Circulate after 100,000 cyclic voltammetrics (sweep velocity: 100m/s), the transmitance difference △ %T within the scope of this obtains maximal value 52%(table 1 at 580nm place).Namely device is after 100,000 circulations, and optical property only have dropped 7%.
Table 1: be respectively the maximum transmission difference of electrolytical device in repeatedly cyclic process with two kinds of ionic liquids
| 5 circulations | 50000 circulations | 100000 circulations | |
| [BMIM][PF 6] | 57% | 54% | 45% |
| [BMIM][OTF] | 62% | 59% | 52% |
Example three: use the condition of 1.5V direct supply in electrochemical workstation 660D under, with 1-ethyl-3-methylimidazole hexafluorophosphate ([BMIM] [PF
6]) as electrolytical electrochromic device, within the scope of 20 ~ 65 ° of C, raised temperature (5 °, interval C adjusts a temperature, measurement data after each temperature stabilization), adopts many potential step methods and cyclic voltammetry to device detection.As can be seen from 25 ° of C(Figure 16) and 65 ° of C(Figure 17) time many potential steps curve control, the chemical property of device almost changes very little; Device cycle volt-ampere curve (Figure 18) at two temperature also can be found out (sweep velocity: 100m/s), and chemical property change is little.
Be not difficult to find out in conjunction with three examples, in from room temperature to the temperature range of 65 ° of C, the temperature stability of this device is better.
Example four: use the condition of 1.5V direct supply in electrochemical workstation 660D under, using 1-ethyl-3-methylimidazole fluoroform sulphonate ([BMIM] [OTF]) as electrolytical electrochromic device, within the scope of 20 ~ 65 ° of C, (5 °, interval C adjusts a temperature to raised temperature, measurement data after each temperature stabilization), adopt many potential step methods and cyclic voltammetry to device detection.As can be seen from 25 ° of C(Figure 19) and 65 ° of C(Figure 20) time many potential steps curve control, the chemical property of device almost changes very little; Device cycle volt-ampere curve (Figure 21) at two temperature also can be found out (sweep velocity: 100m/s), and chemical property change is little.This example is not difficult to find out in conjunction with example three, and in from room temperature to the temperature range of 65 ° of C, the temperature stability of this device is better.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing 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 (2)
1., based on an electrochromic device for polythiophene and derivant and ionic liquid electrolyte, it is characterized in that, comprising:
First electrode, by electrically conducting transparent ito glass substrate and the polythiophene that is deposited thereon and derivant PProDOT-Me thereof
2composition;
And second electrode relative with this first electrode, by electrically conducting transparent ito glass substrate and the inorganic, metal oxide V that is deposited thereon
2o
5composition; V
2o
5colloidal sol, by the mode of plating, makes conductive film deposit to be immersed on ito glass wherein; The second electrode after film forming will be heat-treated, and temperature preferable range is 80-150 DEG C, and the time, preferable range was at 10-20h;
Be arranged on the dielectric substrate between described first electrode and the second electrode; Described dielectric substrate is ionic liquid;
The temperature stabilization performance that described electrochromic device has had;
The preparation process of described electrochromic device is without the need to exclusion of water and oxygen;
Described ionic liquid is 1-ethyl-3-methylimidazole hexafluorophosphate or 1-ethyl-3-methylimidazole fluoroform sulphonate.
2. the device such as the color-changing window between floors of electrochromic device described in claim 1, display, glareproof mirror or shadow shield make in application.
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| 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 |
| 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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