CN105199709A - Electrochromic material and preparation method thereof - Google Patents
Electrochromic material and preparation method thereof Download PDFInfo
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- CN105199709A CN105199709A CN201510567911.7A CN201510567911A CN105199709A CN 105199709 A CN105199709 A CN 105199709A CN 201510567911 A CN201510567911 A CN 201510567911A CN 105199709 A CN105199709 A CN 105199709A
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- electrode
- indoles
- ethylenedioxy
- electrochromic material
- boron trifluoride
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- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- IUAUCKUPPITNHN-UHFFFAOYSA-N 3,7-dihydro-2h-[1,4]dioxino[2,3-e]indole Chemical class O1CCOC2=C1C=CC1=C2C=CN1 IUAUCKUPPITNHN-UHFFFAOYSA-N 0.000 claims description 30
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 229910015900 BF3 Inorganic materials 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- KZMGYPLQYOPHEL-UHFFFAOYSA-N Boron trifluoride etherate Chemical compound FB(F)F.CCOCC KZMGYPLQYOPHEL-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 9
- 238000005868 electrolysis reaction Methods 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 9
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 239000004576 sand Substances 0.000 claims description 8
- 230000004044 response Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 abstract 4
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 abstract 2
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 abstract 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 1
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 150000002475 indoles Chemical class 0.000 description 16
- 239000000126 substance Substances 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 229920001940 conductive polymer Polymers 0.000 description 5
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 4
- 239000002861 polymer material Substances 0.000 description 4
- HZKISDDUZHNOFH-UHFFFAOYSA-N 3,6-dihydro-2h-[1,4]dioxino[2,3-f]indole Chemical class C1=C2OCCOC2=CC2=C1C=CN2 HZKISDDUZHNOFH-UHFFFAOYSA-N 0.000 description 3
- 229940054051 antipsychotic indole derivative Drugs 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- -1 ethylenedioxy ring Chemical group 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000001041 indolyl group Chemical group 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003115 supporting electrolyte Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Abstract
The invention relates to an electrochromic material and a preparation method thereof. The electrochromic material is prepared from a monomer 4,5-dioxyethylene indole in a boron trifluoride-ether system by an electrochemical polymerization method. The poly(4,5-dioxyethylene indole) material prepared by the preparation method has excellent electrochromic property, good thermal stability, relatively high electric conductivity and good flexibility and self-supporting property, and the preparation process is small in energy consumption.
Description
Technical field
The present invention relates to the material and preparation method with excellent conductive performance, be specifically related to a kind of poly-(4,5-ethylenedioxy indoles) material with self-supporting character and electrochromic property and preparation method thereof, belong to electrochromic polymer Material Field.
Background technology
The research emphasis field of " state natural sciences fund " 12 " development program " comprises the Design & preparation of study emphasis photoelectric material, the preparation and property of photoelectricity antetype device characterizes, and electrochromic material and device development are also one of study hotspots of the outer photoelectric functional material of Present Domestic.Comprehensive literature is reported, the electrochromic material of present people's research and development mainly contains following several large class: inorganic electrochromic material, organic molecule electrochromic material and Polymer Electrochromic material, the latter, because have good use and processing characteristics, is the emphasis of research at present.In macromolecular material, thiofuran polymer and polyaniline chemical stability good, electrochromic property is excellent, is the off-color material be the most extensively concerned.In domestic and international association area, less to the applied research of indoles polymkeric substance in electrochromic material at present.
Indoles polymkeric substance belongs to the main chain conjugated type conductive polymers in macromolecular material, is a class potential electrochromism functional materials of good performance: indoles is made up of phenyl ring and pyrrole ring, shows that poly-indoles may have the performance of polyphenyl and polypyrrole concurrently; The indoles polymkeric substance of electrochemical synthesis has good thermostability, comparatively stable in the specific conductivity of doping state; And because phenyl ring participates in conjugated system, demonstrate unique character, the existence of phenyl ring allows quinoid and benzenoid structure resonance, experience the change of colored-colorless because of near infrared absorption when being oxidized, this colour-change is different from other conductive polymerss, therefore has good market outlook and business potential by indoles polymer application to electrochromic material.
According to prior art, mainly there is following shortcoming in the preparation of indoles conductive polymers: when 1, electrochemical polymerization method prepares indoles conductive polymers, oxidizing potential is higher, and energy consumption is larger.2, the poly-indoles conductive polymers prepared in neutral solution, mostly the polymkeric substance obtained is particle or Powdered, and mechanical property is poor, is difficult to carry out practical application.
Summary of the invention
The invention provides a kind of novel electrochromic polymer materials, adopt electrochemical process to be polymerized by monomer 4,5-ethylenedioxy indoles and generate, the structure of 4,5-ethylenedioxy indoles as shown in Figure 1.Preparation method's step of this polymer materials is as follows:
(1) Ag silk is put into the hydrochloric acid soln that concentration is 4-8mol/L, after electrolysis 50-150s under constant potential 1.4-1.7V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.(2) take solid 4,5-ethylenedioxy indoles 0.0170-0.0180g to be dissolved in 5mL boron trifluoride diethyl etherate (BFEE) solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.019-0.021mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.43-0.65V.vs.SCE, reaction certain hour.(3) working electrode in step (2) is taken out, to superincumbent poly-(4,5-ethylenedioxy indoles) the further subsequent disposal of material of attachment.
Adopt 4,5-ethylenedioxy indoles as the monomer preparing electrochromic polymer material in the present invention, it is a kind of new indole analog derivative, and its 4,5 introduce two Sauerstoffatoms.Compared with other indole derivatives, 4,5-ethylenedioxy indoles has the following advantages: 1) 4, the hydrogen of 5 is replaced by ethylenedioxy ring, reduce its energy level, thus can hinder α position that side reaction occurs in the process of electropolymerization, obtain high-quality polymeric film; 2) introducing of ethylenedioxy ring can reduce polymkeric substance oxidation (doping) state time current potential, make the polymkeric substance of doping state have more excellent stability and higher electroconductibility.
Adopt BFEE as the solution system of electrochemical polymerization in technical scheme of the present invention.BFEE itself is a kind of Lewis acid, and itself not only a kind of solution, also can be used as supporting electrolyte simultaneously, have higher ionic conductivity, therefore have electrocatalysis.Containing phenyl ring on indole derivatives, can interact with the boron trioxide in BFEE solution system, ether and generate π-complex compound, reduce the delocalized energy of phenyl ring, thus reduce the oxidizing potential of indoles, be conducive to the reduction of energy consumption.The total acidity adding the system of also enhancing of ether, also improves the ionic conductivity of solution simultaneously, and then accelerates indole derivatives and its cationic coupling speed, improves rate of polymerization.
Poly-(4,5-ethylenedioxy indoles) electrochromic material that the present invention prepares, have porous spherical structure, the aperture size of described polymkeric substance is micron order, after amplifying 10000 times under an electron microscope as shown in Figure 2.It has solid fluorescence character, is Yellow luminous thing, has excellent electrochromic property, can be reversible change between yellowish brown and deep green after adding voltage, and thiophene-based electrochromic polymer generally presents blueness.Its mechanical property and Heat stability is good, have higher specific conductivity, and there will not be safety problem under room temperature.It also has good snappiness and self-supporting character, can intactly take off from working electrode, can greatly expand the range of application in real life.Material oxidation current potential is low, energy consumption is little, is conducive to reducing costs in preparation poly-(4,5-ethylenedioxy indoles), possesses the potential quality that suitability for industrialized production is promoted.
Accompanying drawing explanation
Figure 14, the monomer structure of 5 ethylenedioxies-indoles
The stereoscan photograph of poly-(4, the 5-ethylenedioxy indoles) film of Fig. 2
The spectroelectrochemistry curve of poly-(4, the 5-ethylenedioxy indoles) film of Fig. 3
Fig. 4 gathers (4,5-ethylenedioxy indoles) transmitance-time curve at 675nm place
Figure 54,5-ethylenedioxy indoles (A) and going adulterates the infrared spectrogram of poly-(4, the 5-ethylenedioxy indoles) film (B) of state
Fig. 6 gathers (4,5-ethylenedioxy indoles) fluorescence spectrum figure
Fig. 7 gathers (4,5-ethylenedioxy indoles) thermogravimetric curve figure
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described, but technical scheme of the present invention implements the description that is not limited in embodiment.
Embodiment 1
(1) Ag silk is put into the hydrochloric acid soln that concentration is 4mol/L, after electrolysis 100s under constant potential 1.7V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.
(2) take solid 4,5-ethylenedioxy indoles 0.0175g to be dissolved in 5mL boron trifluoride ether solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.02mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.5V.vs.SCE, reaction 50s.
(3) working electrode in step (2) is taken out, to superincumbent poly-(4,5-ethylenedioxy indoles) the further subsequent disposal of material of attachment.
Embodiment 2
(1) Ag silk is put into the hydrochloric acid soln that concentration is 8mol/L, after electrolysis 60s under constant potential 1.4V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.
(2) take solid 4,5-ethylenedioxy indoles 0.0175g to be dissolved in 5mL boron trifluoride ether solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.02mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.5V.vs.SCE, reaction 50s.
(3) working electrode in step (2) is taken out, to superincumbent poly-(4,5-ethylenedioxy indoles) the further subsequent disposal of material of attachment.
Embodiment 3
(1) Ag silk is put into the hydrochloric acid soln that concentration is 6mol/L, after electrolysis 100s under constant potential 1.5V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.
(2) take solid 4,5-ethylenedioxy indoles 0.018g to be dissolved in 5mL boron trifluoride ether solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.021mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.5V.vs.SCE, reaction 45s.
(3) working electrode in step (2) is taken out, to superincumbent poly-(4,5-ethylenedioxy indoles) the further subsequent disposal of material of attachment.
Embodiment 4
(1) Ag silk is put into the hydrochloric acid soln that concentration is 6mol/L, after electrolysis 100s under constant potential 1.5V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.
(2) take solid 4,5-ethylenedioxy indoles 0.0175g to be dissolved in 5mL boron trifluoride ether solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.02mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.5V.vs.SCE, reaction 50s.
(3) described ITO electrode is taken out, be positioned over the logical light mouth place of ultraviolet spectrophotometer, the voltage applying-0.5 ~ 1.2V also adopts the method combined with spectral absorption, obtain the spectroelectrochemistry curve of polymeric film as shown in Figure 3, illustrate that the polymeric film of preparation has electrochromic property, and color change interval is between yellowish brown to deep green.
Embodiment 5
(1) Ag silk is put into the hydrochloric acid soln that concentration is 6mol/L, after electrolysis 100s under constant potential 1.5V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.
(2) take solid 4,5-ethylenedioxy indoles 0.0175g to be dissolved in 5mL boron trifluoride ether solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.02mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.5V.vs.SCE, reaction 50s.
(3) described ITO electrode is taken out, be positioned over the logical light mouth place of ultraviolet spectrophotometer, adopt the method that square wave current potential and spectral absorption combine, primary voltage is changed at interval of 5s, under the scanning of square-wave voltage-0.5V and 1.2V, poly-(4,5-ethylenedioxy indoles) the film optic response at 675nm place of record, as shown in Figure 4.Can draw at 675nm from figure, optical contrast ratio is 26%, and need 2.1s painted, 2.5s is reduced, and coloration efficiency is 108cm
2c
-1, this is far away higher than the value (50-70cm of the polypyrrole of document record
2c
-1).
Embodiment 6
(1) Ag silk is put into the hydrochloric acid soln that concentration is 6mol/L, after electrolysis 100s under constant potential 1.5V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.Ito glass electrode is clean by alcohol wipe, as working electrode.Stainless steel electrode 1200 object sand paperings, rinse successively with water, ethanol, acetone afterwards and dry up, as to electrode.
(2) take solid 4,5-ethylenedioxy indoles 0.0175g to be dissolved in 5mL boron trifluoride ether solution, be configured to the reaction soln of 4,5-ethylenedioxy indoles monomer concentration 0.02mol/L.By good for three combination of electrodes in step (1), put in the boron trifluoride ether solution containing 4,5-ethylenedioxy indoles monomer, apply the voltage of 0.5V.vs.SCE, reaction 10000s.
(3) polymeric film pocket knife is scraped, and be placed in distilled water soak 3 days, repeatedly use acetone and distilled water flushing afterwards, vacuum-drying 48h at 60 DEG C, the specific conductivity of resulting polymers film is 0.21Scm
-1, and there is self-supporting character and good snappiness.
(4) the present embodiment uses the Fourier transform infrared spectrogram of monomer to see Fig. 5-A, and the Fourier transform infrared spectrogram of resulting polymers is shown in Fig. 5-B.As seen from the figure, at 3394cm
-1strong and the narrow peak that place occurs is the charateristic avsorption band of N-H, at 1561cm
-1the absorption peak at place is stretching vibration and the formation vibration of N-H key respectively, at 725cm
-1with 762cm
-1the absorption peak at place is C
2with C
3the C-H out-of-plane deformation vibration characteristic peak of position.In fig. 2,3397cm
-1the peak that place occurs is the charateristic avsorption band of N-H, is positioned at 792cm
-1and 1084cm
-1the peak at place is 1,2,3,4, the out-of-plane vibration of phenyl ring c h bond of replacement and the peak of in plane vibration, C on indole ring
2with C
3the C-H stretching vibration peak of position disappears, and illustrates that monomer may there occurs polymerization at the prosposition of indoles.
(5) fluorescence spectrum of the present embodiment resulting polymers is shown in Fig. 6, and the peak being positioned at 468nm is the excitation spectrum peak of polymkeric substance, and the peak being positioned at 581nm is the emmission spectrum of described polymkeric substance, illustrates that described polymkeric substance is a kind of Yellow luminous material.
(6) thermogravimetric curve of the present embodiment resulting polymers is shown in Fig. 7, and when temperature rises to 1000K, the residual content of described polymkeric substance still has 62%, illustrates that described polymkeric substance has good thermostability.
Claims (10)
1. an electrochromic material, is characterized in that, the structural formula of described electrochromic material is as shown below:
2. electrochromic material as claimed in claim 1, is characterized in that: described electrochromic material is prepared from by electrochemical polymerization method in boron trifluoride diethyl etherate system by monomer 4,5-ethylenedioxy indoles.
3. electrochromic material as claimed in claim 2, is characterized in that: described polymerization adopts three-electrode system.
4. preparation is according to the method for the arbitrary described electrochromic material of claim 1-3, it is characterized in that: after three combination of electrodes, put into containing 4,5-ethylenedioxy indoles monomer concentration is in the boron trifluoride ether solution of 0.019-0.021mol/L, after applying the voltage response certain hour of 0.43-0.65V.vs.SCE, working electrode is removed, to superincumbent poly-(4,5-ethylenedioxy indoles) the further subsequent disposal of material of attachment.
5. method according to claim 4, is characterized in that, after three combination of electrodes are good, puts into the boron trifluoride ether solution of 0.02mol/L, applies the voltage of 0.5V.vs.SCE, reaction 50s.
6. the method as described in claim 4 or 5, is characterized in that: adopt AgCl as reference electrode, and ito glass electrode is as working electrode, and stainless steel electrode is as to electrode.
7. method as claimed in claim 6, it is characterized in that: Ag silk is put into the hydrochloric acid soln that concentration is 4-8mol/L, after electrolysis 50-150s under constant potential 1.4-1.7V, the AgCl adhesion layer of Surface Creation redness, as reference electrode.
8. method as claimed in claim 7, it is characterized in that: concentration of hydrochloric acid solution is 6mol/L, constant potential is 1.5V, electrolysis time 100s.
9. method as claimed in claim 6, is characterized in that: stainless steel electrode 1200 object sand paperings, rinses successively afterwards and dry up with water, ethanol, acetone, as to electrode.
10. method as claimed in claim 6, is characterized in that: ito glass electrode alcohol wipe is clean, as working electrode.
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| CN105623642A (en) * | 2016-02-24 | 2016-06-01 | 青岛科技大学 | Novel electrochromic material P(6NIIn-co-EDOT) and preparation method thereof |
| CN107267136A (en) * | 2017-06-28 | 2017-10-20 | 江西科技师范大学 | Novel electrochromic material and preparation method thereof |
| WO2018023883A1 (en) * | 2016-08-04 | 2018-02-08 | 北京工业大学 | Method for testing and analyzing cycling stability of electrochromic material based on multi-cycle double-step timing analysis technology |
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| CN105623642A (en) * | 2016-02-24 | 2016-06-01 | 青岛科技大学 | Novel electrochromic material P(6NIIn-co-EDOT) and preparation method thereof |
| WO2018023883A1 (en) * | 2016-08-04 | 2018-02-08 | 北京工业大学 | Method for testing and analyzing cycling stability of electrochromic material based on multi-cycle double-step timing analysis technology |
| CN107267136A (en) * | 2017-06-28 | 2017-10-20 | 江西科技师范大学 | Novel electrochromic material and preparation method thereof |
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