CN105130207B - A kind of sequential 2 D quick response electrochromism laminated film and preparation method thereof - Google Patents
A kind of sequential 2 D quick response electrochromism laminated film and preparation method thereof Download PDFInfo
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- CN105130207B CN105130207B CN201510400506.6A CN201510400506A CN105130207B CN 105130207 B CN105130207 B CN 105130207B CN 201510400506 A CN201510400506 A CN 201510400506A CN 105130207 B CN105130207 B CN 105130207B
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Abstract
A kind of sequential 2 D quick response electrochromism laminated film and preparation method thereof, the present invention relates to laminated film and preparation method thereof.The invention solves the problems that the existing electrochomeric films response time is long, change colour slow technical problem.The structure of laminated film of the present invention is that, with ITO electro-conductive glass as substrate, sequential 2 D zinc oxide is intermediate layer, and electrochomeric films tungsten oxide material is the structure of top layer;Method:First, it is cleaned by ultrasonic ITO conducting glass substrates, drying;2nd, colloidal solution is prepared;3rd, membranaceous colloidal crystal template is prepared;4th, sequential 2 D zinc oxide is prepared;5th, film is prepared.In the present invention, the outstanding electronic conductivity matter of zinc oxide and the larger specific surface area of two-dimensional structure lift the property of electrochomeric films, within make that electrochromic response time from a few minutes reduce 1 second.The present invention is for preparing sequential 2 D quick response electrochromism laminated film.
Description
Technical field
The present invention relates to laminated film and preparation method thereof.
Background technology
Electrochromism refers to that in the presence of outer making alive, valence state and the chemical constituent of material occur reversible change so that
The phenomenon that the emission characteristics of material is reversibly changed, shows as the reversible change of material color and transparency in appearance.Tool
There is the material referred to as electrochromic material of electrochromism phenomenon.
Electrochromic material includes section transitions metal oxide such as nickel oxide, tungsten oxide, tantalum oxide, organic matter
Such as polyaniline, polythiophene, purple sieve essence etc..The electrochromism Electrochromic device being assembled into by electrochromic material has had widely
Using such as electrochromism Energy Saving Windows, anti-dazzle driving mirror, aircraft windows.And have in the aspects such as display, space flight it is very big should
Use potentiality.
The current electrochromic material universal response time is long, and such as in smart window, generally discoloration needs more than ten minutes
Could complete.This is thick mainly due to electrochomeric films, and caused by ion and the more difficult injection of electronics.
The content of the invention
The invention solves the problems that the existing electrochomeric films response time is long, change colour slow technical problem, and provides a kind of
Sequential 2 D quick response electrochromism laminated film and preparation method thereof.
A kind of sequential 2 D quick response electrochromism laminated film, the structure of the laminated film is with ITO electro-conductive glass
It is substrate, sequential 2 D zinc oxide is intermediate layer, and electrochomeric films tungsten oxide material is the structure of top layer.
The preparation method of described a kind of sequential 2 D quick response electrochromism laminated film, specifically according to following step
Suddenly carry out:
First, ITO conducting glass substrates are cleaned by ultrasonic using acetone, methyl alcohol and ultra-pure water successively, drying;
2nd, polystyrene microsphere solution is prepared, then ultrasonic disperse, obtains colloidal solution;
3rd, the substrate processed through step one is put into the colloidal solution that step 2 is obtained, solvent is evaporated, obtain membranaceous
Colloidal crystal template;
4th, membranaceous colloidal crystal template obtained in step 3 is put into zinc nitrate solution, electro-deposition filling zinc oxide films
Film, it is to fill up the bottom one layer space of template to control deposit thickness, then using organic solvent dissolved polystyrene template, is obtained
To sequential 2 D zinc oxide;
5th, on the sequential 2 D zinc oxide that step 4 is obtained to prepare tungsten oxide electrochromism using magnetron sputtering method thin
Film, preparation technology:Pressure is 3Pa, and sputtering power is 40~100W, and sedimentation time is 0.5~2h, obtains sequential 2 D and quickly rings
Answer electrochromism laminated film.
The beneficial effects of the invention are as follows:
In the present invention, the outstanding electronic conductivity matter of zinc oxide and the larger specific surface area of two-dimensional structure lift electroluminescent change
The property of color film, within make that electrochromic response time from a few minutes reduce 1 second.
The present invention is for preparing sequential 2 D quick response electrochromism laminated film.
Brief description of the drawings
The electron microscope of the membranaceous colloidal crystal template that Fig. 1 is prepared for the step 3 of embodiment one is as shown;Fig. 2 is embodiment one
The electron microscope of sequential 2 D zinc oxide prepared by step 4;Fig. 3 is the electroluminescent change of sequential 2 D quick response prepared by embodiment one
The electron microscope of color laminated film;Fig. 4 is the discoloration of sequential 2 D quick response electrochromism laminated film prepared by embodiment one
Spectrogram;
Fig. 5 is the discoloration spectrogram of sequential 2 D quick response electrochromism laminated film prepared by embodiment two;
Fig. 6 is the discoloration spectrogram of sequential 2 D quick response electrochromism laminated film prepared by embodiment three.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also including each specific embodiment it
Between any combination.
Specific embodiment one:A kind of structure of sequential 2 D quick response electrochromism laminated film of present embodiment is
With ITO electro-conductive glass as substrate, sequential 2 D zinc oxide is intermediate layer, and electrochomeric films tungsten oxide material is the knot of top layer
Structure.
Specific embodiment two:A kind of sequential 2 D quick response electrochromism THIN COMPOSITE described in specific embodiment one
The preparation method of film, specifically follows the steps below:
First, ITO conducting glass substrates are cleaned by ultrasonic using acetone, methyl alcohol and ultra-pure water successively, drying;
2nd, polystyrene microsphere solution is prepared, then ultrasonic disperse, obtains colloidal solution;
3rd, the substrate processed through step one is put into the colloidal solution that step 2 is obtained, solvent is evaporated, obtain membranaceous
Colloidal crystal template;
4th, membranaceous colloidal crystal template obtained in step 3 is put into zinc nitrate solution, electro-deposition filling zinc oxide films
Film, it is the space for filling up the template bottom to control deposit thickness, then using organic solvent dissolved polystyrene template, obtains two
Tie up orderly zinc oxide;
5th, on the sequential 2 D zinc oxide that step 4 is obtained to prepare tungsten oxide electrochromism using magnetron sputtering method thin
Film, preparation technology:Pressure is 3Pa, and sputtering power is 40~100W, and sedimentation time is 0.5~2h, obtains sequential 2 D and quickly rings
Answer electrochromism laminated film.
Specific embodiment three:Present embodiment from unlike specific embodiment two:Quality is prepared in step 2 dense
Spend the polystyrene microsphere solution for 0.2%.Other are identical with specific embodiment two.
Specific embodiment four:Present embodiment from unlike specific embodiment two or three:Ultrasound point in step 2
Dissipate 5min.Other are identical with specific embodiment two or three.
Specific embodiment five:Unlike one of present embodiment and specific embodiment two to four:In step 3
Temperature is evaporation solvent under the conditions of 60 DEG C.Other are identical with one of specific embodiment two to four.
Specific embodiment six:Unlike one of present embodiment and specific embodiment two to five:Nitre in step 4
The concentration of sour zinc solution is 0.2mol/L.Other are identical with one of specific embodiment two to five.
Specific embodiment seven:Unlike one of present embodiment and specific embodiment two to six:Electricity in step 4
Deposition uses constant-voltage method, controls deposition voltage for 0.9V, and the time is 200s.Other phases one of with specific embodiment two to six
Together.
Specific embodiment eight:Unlike one of present embodiment and specific embodiment two to seven:Have in step 4
Machine solvent is toluene.Other are identical with one of specific embodiment two to seven.
Specific embodiment nine:Unlike one of present embodiment and specific embodiment two to eight:Splashed in step 5
Power is penetrated for 80W, sedimentation time is 1h.Other are identical with one of specific embodiment two to eight.
Beneficial effects of the present invention are verified using following examples:
Embodiment one:
A kind of structure of sequential 2 D quick response electrochromism laminated film of the present embodiment is with ITO electro-conductive glass as base
Bottom, sequential 2 D zinc oxide is intermediate layer, and electrochomeric films tungsten oxide material is the structure of top layer.
The preparation method of described a kind of sequential 2 D quick response electrochromism laminated film, specifically according to following step
Suddenly carry out:
First, ITO conducting glass substrates are cleaned by ultrasonic using acetone, methyl alcohol and ultra-pure water successively, drying;
2nd, the polystyrene microsphere solution that mass concentration is 0.2% is prepared, then ultrasonic disperse, obtains colloidal solution;
3rd, the substrate processed through step one is put into the colloidal solution that step 2 is obtained, under the conditions of being 60 DEG C in temperature
Evaporation solvent, obtains membranaceous colloidal crystal template;
4th, membranaceous colloidal crystal template obtained in step 3 is put into zinc nitrate solution, electro-deposition filling zinc oxide films
Film, it is the space for filling up the template bottom to control deposit thickness, then using organic solvent dissolved polystyrene template, obtains two
Tie up orderly zinc oxide;Wherein organic solvent is toluene;The concentration of zinc nitrate solution is 0.2mol/L;Electro-deposition uses constant-voltage method,
Control deposition voltage for 0.9V, the time is 200s;
5th, on the sequential 2 D zinc oxide that step 4 is obtained to prepare tungsten oxide electrochromism using magnetron sputtering method thin
Film, preparation technology:Pressure is 3Pa, and sputtering power is 40W, and sedimentation time is 0.5h, obtains the electroluminescent change of sequential 2 D quick response
Color laminated film.
The electron microscope of membranaceous colloidal crystal template prepared by the present embodiment step 3 is as shown in Figure 1;The two of step 4 preparation
The electron microscope for tieing up orderly zinc oxide is as shown in Figure 2;The electron microscope of the sequential 2 D quick response electrochromism laminated film of preparation
As shown in Figure 3;Discoloration spectrogram such as Fig. 4 institutes of sequential 2 D quick response electrochromism laminated film manufactured in the present embodiment
Show.
Embodiment two:
A kind of structure of sequential 2 D quick response electrochromism laminated film of the present embodiment is with ITO electro-conductive glass as base
Bottom, sequential 2 D zinc oxide is intermediate layer, and electrochomeric films tungsten oxide material is the structure of top layer.
The preparation method of described a kind of sequential 2 D quick response electrochromism laminated film, specifically according to following step
Suddenly carry out:
First, ITO conducting glass substrates are cleaned by ultrasonic using acetone, methyl alcohol and ultra-pure water successively, drying;
2nd, the polystyrene microsphere solution that mass concentration is 0.2% is prepared, then ultrasonic disperse, obtains colloidal solution;
3rd, the substrate processed through step one is put into the colloidal solution that step 2 is obtained, under the conditions of being 60 DEG C in temperature
Evaporation solvent, obtains membranaceous colloidal crystal template;
4th, membranaceous colloidal crystal template obtained in step 3 is put into zinc nitrate solution, electro-deposition filling zinc oxide films
Film, it is the space for filling up the template bottom to control deposit thickness, then using organic solvent dissolved polystyrene template, obtains two
Tie up orderly zinc oxide;Wherein organic solvent is toluene;The concentration of zinc nitrate solution is 0.2mol/L;Electro-deposition uses constant-voltage method,
Control deposition voltage for 0.9V, the time is 200s;
5th, on the sequential 2 D zinc oxide that step 4 is obtained to prepare tungsten oxide electrochromism using magnetron sputtering method thin
Film, preparation technology:Pressure is 3Pa, and sputtering power is 80W, and sedimentation time is 1h, obtains sequential 2 D quick response electrochromism
Laminated film.
The discoloration spectrogram of sequential 2 D quick response electrochromism laminated film manufactured in the present embodiment is as shown in Figure 5.
Embodiment three:
A kind of structure of sequential 2 D quick response electrochromism laminated film of the present embodiment is with ITO electro-conductive glass as base
Bottom, sequential 2 D zinc oxide is intermediate layer, and electrochomeric films tungsten oxide material is the structure of top layer.
The preparation method of described a kind of sequential 2 D quick response electrochromism laminated film, specifically according to following step
Suddenly carry out:
First, ITO conducting glass substrates are cleaned by ultrasonic using acetone, methyl alcohol and ultra-pure water successively, drying;
2nd, the polystyrene microsphere solution that mass concentration is 0.2% is prepared, then ultrasonic disperse, obtains colloidal solution;
3rd, the substrate processed through step one is put into the colloidal solution that step 2 is obtained, under the conditions of being 60 DEG C in temperature
Evaporation solvent, obtains membranaceous colloidal crystal template;
4th, membranaceous colloidal crystal template obtained in step 3 is put into zinc nitrate solution, electro-deposition filling zinc oxide films
Film, it is the space for filling up the template bottom to control deposit thickness, then using organic solvent dissolved polystyrene template, obtains two
Tie up orderly zinc oxide;Wherein organic solvent is toluene;The concentration of zinc nitrate solution is 0.2mol/L;Electro-deposition uses constant-voltage method,
Control deposition voltage for 0.9V, the time is 200s;
5th, on the sequential 2 D zinc oxide that step 4 is obtained to prepare tungsten oxide electrochromism using magnetron sputtering method thin
Film, preparation technology:Pressure is 3Pa, and sputtering power is 100W, and sedimentation time is 2h, obtains the electroluminescent change of sequential 2 D quick response
Color laminated film.
The discoloration spectrogram of sequential 2 D quick response electrochromism laminated film manufactured in the present embodiment is as shown in Figure 6.
Claims (4)
1. a kind of preparation method of sequential 2 D quick response electrochromism laminated film, it is characterised in that the method is specifically to press
Carried out according to following steps:
First, ITO conducting glass substrates are cleaned by ultrasonic using acetone, methyl alcohol and ultra-pure water successively, drying;
2nd, polystyrene microsphere solution is prepared, then ultrasonic disperse, obtains colloidal solution;
The polystyrene microsphere solution that mass concentration is 0.2% is prepared in step 2;
Ultrasonic disperse 5min in step 2;
3rd, the substrate processed through step one is put into the colloidal solution that step 2 is obtained, solvent is evaporated, obtain membranaceous colloid
Crystal template;
Evaporation solvent under the conditions of being 60 DEG C in temperature in step 3;
4th, membranaceous colloidal crystal template obtained in step 3 is put into zinc nitrate solution, electro-deposition filling zinc-oxide film, control
Deposit thickness processed is the space for filling up the template bottom, and then using organic solvent dissolved polystyrene template, obtaining two dimension has
Sequence zinc oxide;
The concentration of zinc nitrate solution is 0.2mol/L in step 4;
5th, tungsten oxide electrochomeric films are prepared on the sequential 2 D zinc oxide that step 4 is obtained using magnetron sputtering method, is made
Standby technique:Pressure is 3Pa, and sputtering power is 40~100W, and sedimentation time is 0.5~2h, obtains sequential 2 D quick response electricity
Mutagens color laminated film;
The response time of the sequential 2 D quick response electrochromism laminated film described in step 5 is within 1 second.
2. the preparation method of a kind of sequential 2 D quick response electrochromism laminated film according to claim 1, it is special
It is that electro-deposition uses constant-voltage method in step 4 to levy, and controls deposition voltage for 0.9V, and the time is 200s.
3. the preparation method of a kind of sequential 2 D quick response electrochromism laminated film according to claim 1, it is special
Levy is that organic solvent is toluene in step 4.
4. the preparation method of a kind of sequential 2 D quick response electrochromism laminated film according to claim 1, it is special
It is that sputtering power is 80W in step 5 to levy, and sedimentation time is 1h.
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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 |
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 |
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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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 |
CN102898038A (en) * | 2012-10-19 | 2013-01-30 | 东华大学 | Method for preparing vertically aligned tungsten oxide nano structural electrochromic film |
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