CN108424006A - A kind of preparation method of nanometer of organic composite molybdenum oxide electrochomeric films - Google Patents
A kind of preparation method of nanometer of organic composite molybdenum oxide electrochomeric films Download PDFInfo
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- CN108424006A CN108424006A CN201810344404.0A CN201810344404A CN108424006A CN 108424006 A CN108424006 A CN 108424006A CN 201810344404 A CN201810344404 A CN 201810344404A CN 108424006 A CN108424006 A CN 108424006A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/425—Coatings comprising at least one inhomogeneous layer consisting of a porous layer
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/90—Other aspects of coatings
- C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
- C03C2217/948—Layers comprising indium tin oxide [ITO]
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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Abstract
The invention discloses the preparation methods of a kind of nanometer of organic composite molybdenum oxide electrochomeric films, include the following steps:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;Prepare the precursor solution A of the raw material containing molybdenum oxide;A certain amount of nanometer-sized monodisperse polystyrene colloid ball particle is added in precursor solution A and obtains composite suspension liquid;Ito glass is dipped vertically into composite suspension liquid and grows one layer of composite film;Furnace cooling can be obtained nanoscale molybdenum oxide electrochomeric films after composite film is heat-treated in air atmosphere;Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, Ammonium Persulfate 98.5 is added to obtain solution B, nanoscale molybdenum electrochomeric films are dipped vertically into solution B, it is final to obtain nanometer organic composite molybdenum oxide electrochomeric films, the present invention preparation so that organic material and inorganic material is equably combined with each other in nanoscale, effectively improve pure organic electrochromic material and inorganic electrochromic material there are the problem of.
Description
Technical field
The present invention relates to electrochomeric films preparing technical fields, the specially a kind of nanometer of electroluminescent change of organic composite molybdenum oxide
The preparation method of color film.
Background technology
Service life of the inorganic electrochromic material with high chemical stability, good weatherability and length, MoO3As one
Kind inorganic electrochromic material, is presented gray discoloration characteristic, color is soft, but as other inorganic electrochromic materials,
There is a problem of that color is single, response time length, and organic electrochromic material is just with rich in color, the response time is short
Advantage, on the other hand, nanostructure inorganic electrochromic film have higher specific surface area, high surface activity, with organic material
Material combines rear interface can be higher, while can solve the uniform Complex Problem between inorganic and organic materials, how to synthesize uniformly
Compound nanometer organic/inorganic compound electrochromic material is to solve that inorganic electrochromic material color is single, the response time is grown
One of effective way.
Invention content
The problem of for background technology, the present invention provides a kind of nanometer of organic composite molybdenum oxide electrochromism is thin
The preparation method of film.
To achieve the above object, the present invention provides the following technical solutions:A kind of nanometer of organic composite molybdenum oxide electrochromism
The preparation method of film, includes the following steps:
S10:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;
S20:Molybdenum oxide raw material is dissolved in nitric acid, the dosage of nitric acid is that can dissolve molybdenum oxide, and citric acid is molten
In 25~28% ammonium hydroxide, the amount of ammonium hydroxide can dissolve citric acid, then mix two kinds of solution, wherein molybdenum oxide:Lemon
The molar ratio of lemon acid is 1:1~1.5, ethylene glycol, absolute ethyl alcohol and water are added, the wherein volume ratio of absolute ethyl alcohol and water is 1
~3:1, the total amount of the two is 2~4 times of ammonia volume, finally uses nitric acid or ammonium hydroxide to adjust pH value and obtains precursor solution A;
S30:Mass fraction according to polystyrene colloid ball particle is 2.5%~5% a certain amount of nanoscale list of weighing
Rnonodisperse polystyrene colloid ball particle is added in precursor solution A, and 2~3h of ultrasonic disperse obtains composite suspension liquid;
S40:The spare ito glass of cleaning, drying is dipped vertically into composite suspension liquid, is stood at 40 DEG C~60 DEG C straight
To composite suspension liquid evaporating completely, one layer of composite film is grown in ITO substrate;
S50:Composite film is heat-treated in air atmosphere, keeps the temperature 1h at 100 DEG C respectively, at 350 DEG C~450 DEG C
2~4h is kept the temperature, medium velocity heating is 3 DEG C/min~4 DEG C/min, and it is thin that furnace cooling can be obtained nanoscale molybdenum oxide electrochromism
Film;
S60:Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, wherein nAniline:nO-phenylenediamine=1:1~0.8, over cure is then added
Nanoscale molybdenum electrochomeric films are dipped vertically into solution B by acid amide with obtaining solution B, at 40 DEG C~80 DEG C react 5~
For 24 hours, pulling film forming, with the organic matter of filter paper adsorption surface surplus, be placed under room temperature it is dry in vacuum drying chamber after received
Rice organic composite molybdenum oxide electrochomeric films.
As a kind of preferred technical solution of the present invention, the molar ratio of the ethylene glycol and shown citric acid is 1:1~2.
As a kind of preferred technical solution of the present invention, a concentration of 0.15~0.3mol/L of the aniline.
As a kind of preferred technical solution of the present invention, the ammonium persulfate concentrations are 0.2~0.25mol/L.
Compared with prior art, the beneficial effects of the invention are as follows:Present invention combination polystyrene colloid ball interaction force
And the preparation of composite suspension liquid, one-step synthesis combined oxidation molybdenum film layer can be obtained the hole of nanoscale using heat treatment
The Electrochromic Molybdenum Oxide Coatings being evenly distributed, then organic electrochromic material is compound with Electrochromic Molybdenum Oxide Coatings, so that organic material is filled in
In the hole of film, to reach compound uniform nano composite oxides molybdenum electrochomeric films.Compared with prior art, this hair
Organic electrochromic material is filled up completely in molybdenum oxide in the nano composite oxides molybdenum electrochomeric films structure of bright preparation
In nanoaperture, to make organic material and inorganic material equably be combined with each other in nanoscale, learns from other's strong points to offset one's weaknesses, have
Effect improve pure organic electrochromic material and inorganic electrochromic material there are the problem of.
Specific implementation mode
The technical solution in the present invention is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
Embodiment 1:
The preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films, including following step are provided in the present embodiment
Suddenly:
S10:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;
S20:Molybdenum oxide raw material is dissolved in nitric acid, the dosage of nitric acid is that can dissolve molybdenum oxide, and citric acid is molten
In 25% ammonium hydroxide, the amount of ammonium hydroxide can dissolve citric acid, then mix two kinds of solution, wherein molybdenum oxide:Citric acid
Molar ratio be 1:1, ethylene glycol, absolute ethyl alcohol and water are added, the wherein molar ratio of ethylene glycol and shown citric acid is 1:1,
The volume ratio of absolute ethyl alcohol and water is 1:1, the total amount of the two is 2 times of ammonia volume, and nitric acid or ammonium hydroxide is finally used to adjust pH value
Obtain precursor solution A;
S30:Mass fraction according to polystyrene colloid ball particle is that 2.5% a certain amount of nanometer-sized monodisperse of weighing is poly-
Styrene colloid ball particle is added in precursor solution A, and ultrasonic disperse 2h obtains composite suspension liquid;
S40:The spare ito glass of cleaning, drying is dipped vertically into composite suspension liquid, is stood until compound at 40 DEG C
After suspension evaporating completely, one layer of composite film is grown in ITO substrate;
S50:Composite film is heat-treated in air atmosphere, 1h is kept the temperature at 100 DEG C respectively, is kept the temperature at 350 DEG C DEG C
2h, medium velocity heating is 3 DEG C/min, and furnace cooling can be obtained nanoscale molybdenum oxide electrochomeric films;
S60:Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, wherein nAniline:nO-phenylenediamine=1:1, aniline it is a concentration of
Then Ammonium Persulfate 98.5 is added to obtain solution B, ammonium persulfate concentrations 0.2mol/L, by nanoscale molybdenum electricity in 0.15mol/L
Mutagens color film normal immerses in solution B, reacts 5h at 40 DEG C, pulling film forming, with the organic matter of filter paper adsorption surface surplus, often
It is placed under temperature in vacuum drying chamber and obtains nanometer organic composite molybdenum oxide electrochomeric films after drying.
Embodiment 2:
The preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films, including following step are provided in the present embodiment
Suddenly:
S10:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;
S20:Molybdenum oxide raw material is dissolved in nitric acid, the dosage of nitric acid is that can dissolve molybdenum oxide, and citric acid is molten
In 28% ammonium hydroxide, the amount of ammonium hydroxide can dissolve citric acid, then mix two kinds of solution, wherein molybdenum oxide:Citric acid
Molar ratio be 1:1.5, ethylene glycol, absolute ethyl alcohol and water are added, the wherein molar ratio of ethylene glycol and shown citric acid is 1:
2, the volume ratio of absolute ethyl alcohol and water is 3:1, the total amount of the two is 4 times of ammonia volume, and nitric acid or ammonium hydroxide is finally used to adjust pH
Value obtains precursor solution A;
S30:Mass fraction according to polystyrene colloid ball particle is 5% a certain amount of nanometer-sized monodisperse polyphenyl of weighing
Ethylene colloid ball particle is added in precursor solution A, and ultrasonic disperse 3h obtains composite suspension liquid;
S40:The spare ito glass of cleaning, drying is dipped vertically into composite suspension liquid, is stood until compound at 60 DEG C
After suspension evaporating completely, one layer of composite film is grown in ITO substrate;
S50:Composite film is heat-treated in air atmosphere, respectively at 100 DEG C keep the temperature 1h, at 450 DEG C heat preservation 2~
4h, medium velocity heating is 4 DEG C/min, and furnace cooling can be obtained nanoscale molybdenum oxide electrochomeric films;
S60:Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, wherein nAniline:nO-phenylenediamine=1:0.8, aniline it is a concentration of
Then Ammonium Persulfate 98.5 is added to obtain solution B, ammonium persulfate concentrations 0.25mol/L, by nanoscale molybdenum electricity in 0.3mol/L
Mutagens color film normal immerses in solution B, at 80 DEG C reaction for 24 hours, pulling film forming, with the organic matter of filter paper adsorption surface surplus,
It is placed under room temperature in vacuum drying chamber and obtains nanometer organic composite molybdenum oxide electrochomeric films after drying.
Embodiment 3:
The preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films, including following step are provided in the present embodiment
Suddenly:
S10:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;
S20:Molybdenum oxide raw material is dissolved in nitric acid, the dosage of nitric acid is that can dissolve molybdenum oxide, and citric acid is molten
In 26% ammonium hydroxide, the amount of ammonium hydroxide can dissolve citric acid, then mix two kinds of solution, wherein molybdenum oxide:Citric acid
Molar ratio be 1:1, ethylene glycol, absolute ethyl alcohol and water are added, the wherein molar ratio of ethylene glycol and shown citric acid is 1:1,
The volume ratio of absolute ethyl alcohol and water is 2:1, the total amount of the two is 3 times of ammonia volume, and nitric acid or ammonium hydroxide is finally used to adjust pH value
Obtain precursor solution A;
S30:Mass fraction according to polystyrene colloid ball particle is 4% a certain amount of nanometer-sized monodisperse polyphenyl of weighing
Ethylene colloid ball particle is added in precursor solution A, and ultrasonic disperse 3h obtains composite suspension liquid;
S40:The spare ito glass of cleaning, drying is dipped vertically into composite suspension liquid, is stood until compound at 50 DEG C
After suspension evaporating completely, one layer of composite film is grown in ITO substrate;
S50:Composite film is heat-treated in air atmosphere, respectively at 100 DEG C keep the temperature 1h, at 400 DEG C heat preservation 2~
4h, medium velocity heating is 4 DEG C/min, and furnace cooling can be obtained nanoscale molybdenum oxide electrochomeric films;
S60:Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, wherein nAniline:nO-phenylenediamine=1:0.9, aniline it is a concentration of
Then Ammonium Persulfate 98.5 is added to obtain solution B, ammonium persulfate concentrations 0.25mol/L, by nanoscale molybdenum electricity in 0.2mol/L
Mutagens color film normal immerses in solution B, reacts 12h at 60 DEG C, pulling film forming, with the organic matter of filter paper adsorption surface surplus,
It is placed under room temperature in vacuum drying chamber and obtains nanometer organic composite molybdenum oxide electrochomeric films after drying.
Embodiment 4:
The preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films, including following step are provided in the present embodiment
Suddenly:
S10:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;
S20:Molybdenum oxide raw material is dissolved in nitric acid, the dosage of nitric acid is that can dissolve molybdenum oxide, and citric acid is molten
In 27% ammonium hydroxide, the amount of ammonium hydroxide can dissolve citric acid, then mix two kinds of solution, wherein molybdenum oxide:Citric acid
Molar ratio be 1:1.3, ethylene glycol, absolute ethyl alcohol and water are added, the wherein molar ratio of ethylene glycol and shown citric acid is 1:
1.5, the volume ratio of absolute ethyl alcohol and water is 2.5:1, the total amount of the two is 3 times of ammonia volume, finally uses nitric acid or ammonium hydroxide tune
It saves pH value and obtains precursor solution A;
S30:Mass fraction according to polystyrene colloid ball particle is 3% a certain amount of nanometer-sized monodisperse polyphenyl of weighing
Ethylene colloid ball particle is added in precursor solution A, and ultrasonic disperse 2.5h obtains composite suspension liquid;
S40:The spare ito glass of cleaning, drying is dipped vertically into composite suspension liquid, is stood until compound at 55 DEG C
After suspension evaporating completely, one layer of composite film is grown in ITO substrate;
S50:Composite film is heat-treated in air atmosphere, 1h is kept the temperature at 100 DEG C respectively, keeps the temperature 3h at 420 DEG C,
The heating of its medium velocity is 3.5 DEG C/min, and furnace cooling can be obtained nanoscale molybdenum oxide electrochomeric films;
S60:Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, wherein nAniline:nO-phenylenediamine=1:1, aniline it is a concentration of
Then Ammonium Persulfate 98.5 is added to obtain solution B, ammonium persulfate concentrations 0.22mol/L, by nanoscale molybdenum electricity in 0.2mol/L
Mutagens color film normal immerses in solution B, reacts 18h at 50 DEG C, pulling film forming, with the organic matter of filter paper adsorption surface surplus,
It is placed under room temperature in vacuum drying chamber and obtains nanometer organic composite molybdenum oxide electrochomeric films after drying.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (4)
1. the preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films, which is characterized in that include the following steps:
S10:Prepare nanometer-sized monodisperse polystyrene colloid ball particle;
S20:Molybdenum oxide raw material is dissolved in nitric acid, the dosage of nitric acid is that can dissolve molybdenum oxide, and citric acid is dissolved in 25
In~28% ammonium hydroxide, the amount of ammonium hydroxide can dissolve citric acid, then mix two kinds of solution, wherein molybdenum oxide:Citric acid
Molar ratio be 1:1~1.5, ethylene glycol, absolute ethyl alcohol and water are added, the wherein volume ratio of absolute ethyl alcohol and water is 1~3:
1, the total amount of the two is 2~4 times of ammonia volume, finally uses nitric acid or ammonium hydroxide to adjust pH value and obtains precursor solution A;
S30:Mass fraction according to polystyrene colloid ball particle is 2.5%~5% a certain amount of nanometer-sized monodisperse of weighing
Polystyrene colloid ball particle is added in precursor solution A, and 2~3h of ultrasonic disperse obtains composite suspension liquid;
S40:The spare ito glass of cleaning, drying is dipped vertically into composite suspension liquid, is stood at 40 DEG C~60 DEG C until multiple
After closing suspension evaporating completely, one layer of composite film is grown in ITO substrate;
S50:Composite film is heat-treated in air atmosphere, 1h is kept the temperature at 100 DEG C respectively, is kept the temperature at 350 DEG C~450 DEG C
2~4h, medium velocity heating is 3 DEG C/min~4 DEG C/min, and furnace cooling can be obtained nanoscale molybdenum oxide electrochomeric films;
S60:Prepare the hydrochloric acid solution of aniline and o-phenylenediamine, wherein nAniline:nO-phenylenediamine=1:1~0.8, Ammonium Persulfate 98.5 is then added
To obtain solution B, nanoscale molybdenum electrochomeric films are dipped vertically into solution B, at 40 DEG C~80 DEG C react 5~for 24 hours,
Pulling film forming, with the organic matter of filter paper adsorption surface surplus, be placed under room temperature it is dry in vacuum drying chamber after i.e. acquisition nanometer have
Machine combined oxidation molybdenum electrochomeric films.
2. the preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films according to claim 1, feature
It is:The molar ratio of the ethylene glycol and shown citric acid is 1:1~2.
3. the preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films according to claim 1, feature
It is:A concentration of 0.15~0.3mol/L of the aniline.
4. the preparation method of a kind of nanometer of organic composite molybdenum oxide electrochomeric films according to claim 1, feature
It is:The ammonium persulfate concentrations are 0.2~0.25mol/L.
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CN105839084A (en) * | 2015-07-08 | 2016-08-10 | 北京工业大学 | Method for preparation of porous WO3/rGO composite film by Sol-Gel |
CN106746724A (en) * | 2017-02-21 | 2017-05-31 | 上海第二工业大学 | A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof |
CN107010843A (en) * | 2017-04-28 | 2017-08-04 | 江苏大学 | A kind of electrochromism WO3The sol-gel process for preparing of film |
CN107814493A (en) * | 2017-10-30 | 2018-03-20 | 上海艾谡新材料有限公司 | A kind of preparation method of nanometer of organic composite tungsten oxide electrochomeric films |
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2018
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CN1560185A (en) * | 2004-03-10 | 2005-01-05 | 复旦大学 | Metal oxide pore material with excellent electrochromism performance and its preparation process |
US20080030837A1 (en) * | 2006-08-01 | 2008-02-07 | Universite De Moncton | Chromogenically tunable photonic crystals |
CN102432192A (en) * | 2011-08-23 | 2012-05-02 | 陕西科技大学 | Method for preparing organic/inorganic electrochromic composite film |
CN105839084A (en) * | 2015-07-08 | 2016-08-10 | 北京工业大学 | Method for preparation of porous WO3/rGO composite film by Sol-Gel |
CN106746724A (en) * | 2017-02-21 | 2017-05-31 | 上海第二工业大学 | A kind of molybdenum oxide electrochromism nano thin-film and preparation method thereof |
CN107010843A (en) * | 2017-04-28 | 2017-08-04 | 江苏大学 | A kind of electrochromism WO3The sol-gel process for preparing of film |
CN107814493A (en) * | 2017-10-30 | 2018-03-20 | 上海艾谡新材料有限公司 | A kind of preparation method of nanometer of organic composite tungsten oxide electrochomeric films |
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Application publication date: 20180821 |