CN105130207A - Two-dimensional ordered quick response electrochromism composite film and production method thereof - Google Patents
Two-dimensional ordered quick response electrochromism composite film and production method thereof Download PDFInfo
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- CN105130207A CN105130207A CN201510400506.6A CN201510400506A CN105130207A CN 105130207 A CN105130207 A CN 105130207A CN 201510400506 A CN201510400506 A CN 201510400506A CN 105130207 A CN105130207 A CN 105130207A
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Abstract
The invention relates to a composite film and a production method thereof, and concretely relates to a two-dimensional ordered quick response electrochromism composite film and a production method thereof. The technical problems to be solved in the invention are long response time and slow color change of present electrochromism films. The structure of the composite film comprises ITO conductive glass as a substrate, two-dimensional ordered zinc oxide as an interface layer and an electrochromism film tungsten oxide material as a top layer. The method comprises the following steps: 1, carrying out ultrasonic cleaning on the ITO conductive glass substrate, and drying; 2, preparing a colloid solution; 3, preparing a membrane-shaped colloid crystal template; 4, preparing two-dimensional ordered zinc oxide; and 5, producing the film. The excellent electron conduction property of zinc oxide and the large specific surface area of the two-dimensional structure improve the properties of the electrochromism composite film, so the electrochromism response time is shortened to below 1s from several minutes. The method is used for producing the two-dimensional ordered quick response electrochromism composite film.
Description
Technical field
The present invention relates to laminated film and preparation method thereof.
Background technology
Under electrochromism refers to alive effect outside, the valence state of material and chemical composition occur reversible change, make the phenomenon of the emission characteristic generation modulation of material, show as the reversible change of material color and transparency in appearance.The material with electrochromism phenomenon is called electrochromic material.
Electrochromic material comprises section transitions metal oxide as nickel oxide, Tungsten oxide 99.999, tantalum oxide etc., and organism is as polyaniline, Polythiophene, purple sieve essence etc.The electrochromism Electrochromic device be assembled into by electrochromic material has had to be applied, widely as electrochromism Energy Saving Windows, anti-dazzle driving mirror, aircraft windows etc.And in display, space flight etc. on have very large application potential.
The current electrochromic material general time of response is long, and as in smart window, usual variable color needs just can complete for tens minutes.This is mainly thick due to electrochomeric films, and ion and the more difficult injection of electronics cause.
Summary of the invention
It is long that the present invention will solve the existing electrochomeric films time of response, and variable color is technical problem slowly, and provides a kind of sequential 2 D to respond electrochromism laminated film and preparation method thereof fast.
A kind of sequential 2 D responds electrochromism laminated film fast, and the structure of this laminated film is with ITO conductive glass for substrate, and sequential 2 D zinc oxide is middle layer, and electrochomeric films tungsten oxide material is the structure of top layer.
Described a kind of sequential 2 D responds the preparation method of electrochromism laminated film fast, specifically carries out according to following steps:
One, ITO conducting glass substrate is adopted acetone, methyl alcohol and ultrapure water ultrasonic cleaning successively, dry;
Two, prepare polystyrene microsphere solution, then ultrasonic disperse, obtains colloidal solution;
Three, the substrate processed through step one is put into the colloidal solution that step 2 obtains, solvent is evaporated, obtains membranaceous colloidal crystal template;
Four, the membranaceous colloidal crystal template that step 3 is obtained is put into zinc nitrate solution, zinc-oxide film is filled in galvanic deposit, controlling deposit thickness is the space filling up the bottom one deck of template, then adopts organic solvent dissolution polystyrene moulding, obtains sequential 2 D zinc oxide;
Five, the sequential 2 D zinc oxide adopting magnetron sputtering method to obtain in step 4 prepares Tungsten oxide 99.999 electrochomeric films, preparation technology: pressure is 3Pa, sputtering power is 40 ~ 100W, and depositing time is 0.5 ~ 2h, obtains sequential 2 D and responds electrochromism laminated film fast.
The invention has the beneficial effects as follows:
In the present invention, the electronic conduction character that zinc oxide is outstanding and the larger specific surface area of two-dirnentional structure promote the character of electrochomeric films, within 1 second that the electrochromic time of response is reduced from several minutes.
The present invention responds electrochromism laminated film fast for the preparation of sequential 2 D.
Accompanying drawing explanation
Fig. 1 be the Electronic Speculum figure of membranaceous colloidal crystal template prepared by embodiment one step 3 as shown; Fig. 2 is the Electronic Speculum figure of sequential 2 D zinc oxide prepared by embodiment one step 4; Fig. 3 is that sequential 2 D prepared by embodiment one responds the Electronic Speculum figure of electrochromism laminated film fast; Fig. 4 is that sequential 2 D prepared by embodiment one responds the variable color light spectrogram of electrochromism laminated film fast;
Fig. 5 is that sequential 2 D prepared by embodiment two responds the variable color light spectrogram of electrochromism laminated film fast;
Fig. 6 is that sequential 2 D prepared by embodiment three responds the variable color light spectrogram of electrochromism laminated film fast.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the structure that a kind of sequential 2 D of present embodiment responds electrochromism laminated film is fast with ITO conductive glass for substrate, and sequential 2 D zinc oxide is middle layer, and electrochomeric films tungsten oxide material is the structure of top layer.
Embodiment two: a kind of sequential 2 D described in embodiment one responds the preparation method of electrochromism laminated film fast, specifically carries out according to following steps:
One, ITO conducting glass substrate is adopted acetone, methyl alcohol and ultrapure water ultrasonic cleaning successively, dry;
Two, prepare polystyrene microsphere solution, then ultrasonic disperse, obtains colloidal solution;
Three, the substrate processed through step one is put into the colloidal solution that step 2 obtains, solvent is evaporated, obtains membranaceous colloidal crystal template;
Four, the membranaceous colloidal crystal template that step 3 is obtained is put into zinc nitrate solution, zinc-oxide film is filled in galvanic deposit, controlling deposit thickness is the space filling up the template lowest layer, then adopts organic solvent dissolution polystyrene moulding, obtains sequential 2 D zinc oxide;
Five, the sequential 2 D zinc oxide adopting magnetron sputtering method to obtain in step 4 prepares Tungsten oxide 99.999 electrochomeric films, preparation technology: pressure is 3Pa, sputtering power is 40 ~ 100W, and depositing time is 0.5 ~ 2h, obtains sequential 2 D and responds electrochromism laminated film fast.
Embodiment three: present embodiment and embodiment two unlike: prepare the polystyrene microsphere solution that mass concentration is 0.2% in step 2.Other is identical with embodiment two.
Embodiment four: present embodiment and embodiment two or three are unlike ultrasonic disperse 5min in step 2.Other is identical with embodiment two or three.
Embodiment five: one of present embodiment and embodiment two to four unlike: in step 3 under temperature is 60 DEG C of conditions evaporating solvent.Other is identical with one of embodiment two to four.
Embodiment six: one of present embodiment and embodiment two to five unlike: in step 4, the concentration of zinc nitrate solution is 0.2mol/L.Other is identical with one of embodiment two to five.
Embodiment seven: one of present embodiment and embodiment two to six unlike: in step 4 galvanic deposit adopt constant-voltage method, control deposition voltage is 0.9V, and the time is 200s.Other is identical with one of embodiment two to six.
Embodiment eight: one of present embodiment and embodiment two to seven unlike: in step 4, organic solvent is toluene.Other is identical with one of embodiment two to seven.
Embodiment nine: one of present embodiment and embodiment two to eight unlike: in step 5, sputtering power is 80W, and depositing time is 1h.Other is identical with one of embodiment two to eight.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The structure that a kind of sequential 2 D of the present embodiment responds electrochromism laminated film is fast with ITO conductive glass for substrate, and sequential 2 D zinc oxide is middle layer, and electrochomeric films tungsten oxide material is the structure of top layer.
Described a kind of sequential 2 D responds the preparation method of electrochromism laminated film fast, specifically carries out according to following steps:
One, ITO conducting glass substrate is adopted acetone, methyl alcohol and ultrapure water ultrasonic cleaning successively, dry;
Two, prepare the polystyrene microsphere solution that mass concentration is 0.2%, then ultrasonic disperse, obtains colloidal solution;
Three, the substrate processed through step one is put into the colloidal solution that step 2 obtains, evaporating solvent under temperature is 60 DEG C of conditions, obtains membranaceous colloidal crystal template;
Four, the membranaceous colloidal crystal template that step 3 is obtained is put into zinc nitrate solution, zinc-oxide film is filled in galvanic deposit, controlling deposit thickness is the space filling up the template lowest layer, then adopts organic solvent dissolution polystyrene moulding, obtains sequential 2 D zinc oxide; Wherein organic solvent is toluene; The concentration of zinc nitrate solution is 0.2mol/L; Galvanic deposit adopts constant-voltage method, and control deposition voltage is 0.9V, and the time is 200s;
Five, the sequential 2 D zinc oxide adopting magnetron sputtering method to obtain in step 4 prepares Tungsten oxide 99.999 electrochomeric films, preparation technology: pressure is 3Pa, and sputtering power is 40W, and depositing time is 0.5h, obtains sequential 2 D and responds electrochromism laminated film fast.
The Electronic Speculum figure of membranaceous colloidal crystal template prepared by the present embodiment step 3 as shown in Figure 1; The Electronic Speculum figure of sequential 2 D zinc oxide prepared by step 4 as shown in Figure 2; The sequential 2 D of preparation responds the Electronic Speculum figure of electrochromism laminated film as shown in Figure 3 fast; Sequential 2 D prepared by the present embodiment responds the variable color light spectrogram of electrochromism laminated film as shown in Figure 4 fast.
Embodiment two:
The structure that a kind of sequential 2 D of the present embodiment responds electrochromism laminated film is fast with ITO conductive glass for substrate, and sequential 2 D zinc oxide is middle layer, and electrochomeric films tungsten oxide material is the structure of top layer.
Described a kind of sequential 2 D responds the preparation method of electrochromism laminated film fast, specifically carries out according to following steps:
One, ITO conducting glass substrate is adopted acetone, methyl alcohol and ultrapure water ultrasonic cleaning successively, dry;
Two, prepare the polystyrene microsphere solution that mass concentration is 0.2%, then ultrasonic disperse, obtains colloidal solution;
Three, the substrate processed through step one is put into the colloidal solution that step 2 obtains, evaporating solvent under temperature is 60 DEG C of conditions, obtains membranaceous colloidal crystal template;
Four, the membranaceous colloidal crystal template that step 3 is obtained is put into zinc nitrate solution, zinc-oxide film is filled in galvanic deposit, controlling deposit thickness is the space filling up the template lowest layer, then adopts organic solvent dissolution polystyrene moulding, obtains sequential 2 D zinc oxide; Wherein organic solvent is toluene; The concentration of zinc nitrate solution is 0.2mol/L; Galvanic deposit adopts constant-voltage method, and control deposition voltage is 0.9V, and the time is 200s;
Five, the sequential 2 D zinc oxide adopting magnetron sputtering method to obtain in step 4 prepares Tungsten oxide 99.999 electrochomeric films, preparation technology: pressure is 3Pa, and sputtering power is 80W, and depositing time is 1h, obtains sequential 2 D and responds electrochromism laminated film fast.
Sequential 2 D prepared by the present embodiment responds the variable color light spectrogram of electrochromism laminated film as shown in Figure 5 fast.
Embodiment three:
The structure that a kind of sequential 2 D of the present embodiment responds electrochromism laminated film is fast with ITO conductive glass for substrate, and sequential 2 D zinc oxide is middle layer, and electrochomeric films tungsten oxide material is the structure of top layer.
Described a kind of sequential 2 D responds the preparation method of electrochromism laminated film fast, specifically carries out according to following steps:
One, ITO conducting glass substrate is adopted acetone, methyl alcohol and ultrapure water ultrasonic cleaning successively, dry;
Two, prepare the polystyrene microsphere solution that mass concentration is 0.2%, then ultrasonic disperse, obtains colloidal solution;
Three, the substrate processed through step one is put into the colloidal solution that step 2 obtains, evaporating solvent under temperature is 60 DEG C of conditions, obtains membranaceous colloidal crystal template;
Four, the membranaceous colloidal crystal template that step 3 is obtained is put into zinc nitrate solution, zinc-oxide film is filled in galvanic deposit, controlling deposit thickness is the space filling up the template lowest layer, then adopts organic solvent dissolution polystyrene moulding, obtains sequential 2 D zinc oxide; Wherein organic solvent is toluene; The concentration of zinc nitrate solution is 0.2mol/L; Galvanic deposit adopts constant-voltage method, and control deposition voltage is 0.9V, and the time is 200s;
Five, the sequential 2 D zinc oxide adopting magnetron sputtering method to obtain in step 4 prepares Tungsten oxide 99.999 electrochomeric films, preparation technology: pressure is 3Pa, and sputtering power is 100W, and depositing time is 2h, obtains sequential 2 D and responds electrochromism laminated film fast.
Sequential 2 D prepared by the present embodiment responds the variable color light spectrogram of electrochromism laminated film as shown in Figure 6 fast.
Claims (9)
1. sequential 2 D responds an electrochromism laminated film fast, and it is characterized in that the structure of this laminated film is with ITO conductive glass for substrate, sequential 2 D zinc oxide is middle layer, and electrochomeric films tungsten oxide material is the structure of top layer.
2. a kind of sequential 2 D as claimed in claim 1 responds the preparation method of electrochromism laminated film fast, it is characterized in that specifically carrying out according to following steps:
One, ITO conducting glass substrate is adopted acetone, methyl alcohol and ultrapure water ultrasonic cleaning successively, dry;
Two, prepare polystyrene microsphere solution, then ultrasonic disperse, obtains colloidal solution;
Three, the substrate processed through step one is put into the colloidal solution that step 2 obtains, solvent is evaporated, obtains membranaceous colloidal crystal template;
Four, the membranaceous colloidal crystal template that step 3 is obtained is put into zinc nitrate solution, zinc-oxide film is filled in galvanic deposit, controlling deposit thickness is the space filling up the template lowest layer, then adopts organic solvent dissolution polystyrene moulding, obtains sequential 2 D zinc oxide;
Five, the sequential 2 D zinc oxide adopting magnetron sputtering method to obtain in step 4 prepares Tungsten oxide 99.999 electrochomeric films, preparation technology: pressure is 3Pa, sputtering power is 40 ~ 100W, and depositing time is 0.5 ~ 2h, obtains sequential 2 D and responds electrochromism laminated film fast.
3. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, it is characterized in that preparing the polystyrene microsphere solution that mass concentration is 0.2% in step 2.
4. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, it is characterized in that ultrasonic disperse 5min in step 2.
5. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, to it is characterized in that in step 3 evaporating solvent under temperature is 60 DEG C of conditions.
6. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, it is characterized in that the concentration of zinc nitrate solution in step 4 is 0.2mol/L.
7. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, and it is characterized in that in step 4, galvanic deposit adopts constant-voltage method, control deposition voltage is 0.9V, and the time is 200s.
8. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, it is characterized in that in step 4, organic solvent is toluene.
9. a kind of sequential 2 D according to claim 2 responds the preparation method of electrochromism laminated film fast, and it is characterized in that in step 5, sputtering power is 80W, depositing time is 1h.
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Cited By (4)
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| CN109592910A (en) * | 2018-11-26 | 2019-04-09 | 哈尔滨工业大学 | A kind of preparation method of hollow ball-shape electrochomeric films |
| CN112319012A (en) * | 2020-10-21 | 2021-02-05 | 湖北大学 | Preparation method of sandwich-like structure membrane with ultraviolet stable superhydrophobic and fast response color change |
| CN112897575A (en) * | 2019-12-03 | 2021-06-04 | 中国科学院深圳先进技术研究院 | Method and structure for forming two-dimensional cadmium sulfide on substrate in large area |
| CN115629501A (en) * | 2022-09-28 | 2023-01-20 | 贵州大学 | In-situ self-assembly large-area multicolor electrochromic device and preparation method and application thereof |
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| CN101551569A (en) * | 2008-04-01 | 2009-10-07 | 中国科学院物理研究所 | Nonlinear optical material based on metal nanometer cluster array and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592910A (en) * | 2018-11-26 | 2019-04-09 | 哈尔滨工业大学 | A kind of preparation method of hollow ball-shape electrochomeric films |
| CN112897575A (en) * | 2019-12-03 | 2021-06-04 | 中国科学院深圳先进技术研究院 | Method and structure for forming two-dimensional cadmium sulfide on substrate in large area |
| CN112319012A (en) * | 2020-10-21 | 2021-02-05 | 湖北大学 | Preparation method of sandwich-like structure membrane with ultraviolet stable superhydrophobic and fast response color change |
| CN112319012B (en) * | 2020-10-21 | 2023-03-07 | 湖北大学 | Preparation method of sandwich structure-imitated membrane with ultraviolet stable super-hydrophobicity and quick response color change |
| CN115629501A (en) * | 2022-09-28 | 2023-01-20 | 贵州大学 | In-situ self-assembly large-area multicolor electrochromic device and preparation method and application thereof |
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