CN105036564B - A kind of nanocrystalline enhancing tungsten oxide electrochomeric films and preparation method thereof - Google Patents
A kind of nanocrystalline enhancing tungsten oxide electrochomeric films and preparation method thereof Download PDFInfo
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- CN105036564B CN105036564B CN201510358853.7A CN201510358853A CN105036564B CN 105036564 B CN105036564 B CN 105036564B CN 201510358853 A CN201510358853 A CN 201510358853A CN 105036564 B CN105036564 B CN 105036564B
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Abstract
It is using transparent conductive oxide (TCO) is nanocrystalline, amorphous tungsten oxide is prepared as matrix " nanocrystalline WO of TCO the invention discloses a kind of nanocrystalline enhancing tungsten oxide electrochomeric films3Amorphous " two-phase laminated film；The invention also discloses the preparation method of the nanocrystalline enhancing tungsten oxide electrochomeric films.The present invention uses nanocrystalline enhancing technology, improve electrochromic property of the conventional oxidation W film in visible light wave range, utilize the nanocrystalline modulating characteristics near infrared band of TCO simultaneously, modulation of the tungsten oxide film near infrared band is realized, solves the problems, such as that tungsten oxide film cycle life falls short of in the prior art, the large scale materials Electrochromic speed of response is slow and lacks near-infrared modulation capability.
Description
Technical field
The invention belongs to inorganic functional material technical field, and in particular to a kind of nanocrystalline enhancing tungsten oxide electrochromism is thin
Film；The invention further relates to the preparation method of the nanocrystalline enhancing tungsten oxide electrochomeric films.
Background technology
Tungsten oxide electrochomeric films because with can adjust indoor lighting and function of heat insulation in real time and in building energy conservation
Glass art possesses huge application value, it is considered to be substitutes the energy-conservation window material of future generation of Low-e coated glasses.
Tungsten oxide system electrochromism glass windows mainly by transparency electrode, tungsten oxide electrochomeric films, lithium-ion electrolyte,
Five layers of composition such as ion storage film, transparency electrode, an additional low-tension supply provide driving voltage, realize the electricity of the sandwich
Mutagens color；And existing tungsten oxide system electrochromism glass windows are present that cycle life is long, large-size glass electrochromism response speed
The shortcomings that rate is slow and lacks near-infrared modulation capability, have impact on the material widely using in building energy conservation glass art.Shadow
The critical material for ringing the window electrochromic property is tungsten oxide electrochomeric films, therefore, how to prepare electrochromic material
Have extended cycle life, large scale material discoloration the speed of response be provided simultaneously with soon near-infrared modulation capability tungsten oxide electrochromism it is thin
The problem of film is urgent need to resolve.
The content of the invention
It is an object of the invention to provide a kind of nanocrystalline enhancing tungsten oxide electrochomeric films, solves existing tungsten oxide system electricity
The problem of mutagens color material circulation short life, the large scale material discoloration speed of response are slow and lack near-infrared modulation capability.
It is a further object of the present invention to provide the preparation method of the nanocrystalline enhancing tungsten oxide electrochomeric films, work is prepared
Skill is easy.
The technical solution adopted in the present invention is that a kind of nanocrystalline enhancing tungsten oxide electrochomeric films, are with amorphous state
Tungsten oxide be matrix, crystalline state nanometer transparent conductive oxide (TCO) is embedded into matrix, the " nanocrystalline-WO of TCO of preparation3
Amorphous " two-phase laminated film.
It is of the invention to be further characterized in that,
Crystalline state nanometer TCO is heavily-doped semiconductor, to mix the indium oxide of tin (ITO), mixing the tin oxide (ATO) of antimony or mixing aluminium
Zinc oxide (AZO) in any one.
Crystalline state nanometer TCO particle diameter is 5~20nm, carrier concentration 1018~1021Individual/cm3。
Another technical scheme of the present invention is a kind of preparation side of nanocrystalline enhancing tungsten oxide electrochomeric films
Method, comprise the following steps that：
Step 1, after tungsten chloride and TCO being mixed with metal nitrate, it is dissolved in organic solvent, obtains mixed solution；Xiang Qi
Middle addition deionized water, stirs 2h at normal temperatures, fully after dissolving, obtains complex sol；
Step 2, using Best-Effort request or spin coating technique, by step 1 gained complex sol even application in electrically conducting transparent oxygen
On compound glass substrate, gel mould is formed；
Step 3, step 2 gained gel mould is placed in 150 DEG C of environment after 10min, be put into heat-treatment furnace in 200~
1 hour is incubated under 300 DEG C of oxygen atmosphere, is then drawn off, is air-cooled to room temperature, produce electrochomeric films.
It is of the invention to be further characterized in that,
In step 1, TCO metal nitrates, for nitric acid tin and the mixture of indium nitrate；Or nitric acid tin and antimony trichloride
Mixture；Or the mixture of zinc nitrate and aluminum nitrate.
In step 1, the mol ratio of nitric acid tin, indium nitrate and tungsten chloride is 0.1:1:5~20；Or antimony trichloride, nitric acid tin
Mol ratio with tungsten chloride is 0.04:1:10~100；Or aluminum nitrate:Zinc nitrate:The mol ratio of tungsten chloride is 0.06:1:5~
20。
In step 1, organic solvent is methanol, ethanol and one kind in ethylene glycol monomethyl ether or any several with arbitrary proportion institute
Mixture, the molar concentration of tungsten chloride is 0.05~0.15mol/L in gained mixed solution.
In step 1, the volume ratio of deionized water and organic solvent is 1：100.
The invention has the advantages that using nanocrystalline enhancing technology, conventional oxidation W film is improved in visible light wave
The electrochromic property of section, while the nanocrystalline modulating characteristics near infrared band of TCO are utilized, tungsten oxide film is realized near
The modulation of infrared band, solve tungsten oxide film cycle life in the prior art fall short of, large scale materials Electrochromic ring
The problem of answering speed slow and lacking near-infrared modulation capability.
Brief description of the drawings
Fig. 1 is the gained of the embodiment 1 " nanocrystalline-WO of ITO3" WO obtained by amorphous " laminated film and comparative example3Amorphous " film
The transmittance curve of color state and colour fading state；
Fig. 2 is the gained of the embodiment 1 " nanocrystalline-WO of ITO3" WO obtained by amorphous " laminated film and comparative example3The electricity of amorphous " film
The mutagens colour response time.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Embodiment 1
Prepare " nanocrystalline-the WO of ITO3Amorphous " electrochomeric films：
0.9914g tungsten chlorides, 0.0477g indium nitrates, 0.0046g nitric acid tin are taken, is dissolved in 49.5mL methanol, thereto
0.5mL deionized waters are added, are stirred at normal temperatures 2 hours after fully dissolving, obtain the complex sol of tungstenic, indium, tin；Using dipping
Lifting or spin coating technique, by gained complex sol even application on transparent conductive oxide substrate, gel mould is formed,
After drying 10min at a temperature of 150 DEG C, it is put into heat-treatment furnace and 1h is incubated under 200~300 DEG C of oxygen atmosphere, then by it
Take out, be air-cooled to room temperature and obtain " nanocrystalline-the WO of ITO3Amorphous " two-phase laminated film.
The coloured state of film obtained by the present embodiment and the transmittance curve of colour fading state are as shown in figure 1, in visible light wave range
Optical modulation contrast △ T% are 70%；Optical modulation contrast △ T% at 1200nm wave bands are 50%；100×100mm2
Film discoloration response time 1s, the electrochromism response time figure of film is shown in Fig. 2 obtained by the present embodiment；Fade treatment 2000 times
Afterwards, film magnitude of the stored charge declines only 3%.
Embodiment 2
Prepare " nanocrystalline-the WO of ITO3Amorphous " electrochomeric films：
3g tungsten chlorides, 0.5777g indium nitrates, 0.055g nitric acid tin are taken, is dissolved in 49.5mL ethanol, adds thereto
0.5mL deionized waters, stir at normal temperatures 2 hours after fully dissolving, obtain the complex sol of tungstenic, indium, tin；Using Best-Effort request
Or spin coating technique, by gained complex sol even application on transparent conductive oxide substrate, gel mould is formed, 150
After drying 10min at a temperature of DEG C, it is put into heat-treatment furnace and is incubated 1h under 200~300 DEG C of oxygen atmosphere, then taken
Go out, be air-cooled to room temperature and obtain " nanocrystalline-the WO of ITO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is 65% in the optical modulation contrast △ T% of visible light wave range；At 1200nm wave bands
Optical modulation contrast △ T% be 53%；100×100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 2%.
Embodiment 3
Prepare " nanocrystalline-the WO of ITO3Amorphous " electrochomeric films：
2g tungsten chlorides, 0.1527g indium nitrates, 0.0147g nitric acid tin are taken, is dissolved in 49.5mL ethylene glycol monomethyl ethers, Xiang Qi
Middle addition 0.5mL deionized waters, stir at normal temperatures 2 hours after fully dissolving, obtain the complex sol of tungstenic, indium, tin；Using leaching
Stain lifts or spin coating technique, by gained complex sol even application on transparent conductive oxide substrate, forms gel mould,
After drying 10min at a temperature of 150 DEG C, it is put into heat-treatment furnace and is incubated 1h under 200~300 DEG C of oxygen atmosphere, then will
It takes out, and is air-cooled to room temperature and obtains " nanocrystalline-the WO of ITO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is at 72%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 55%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 2%.
Embodiment 4
Prepare " nanocrystalline-the WO of ATO3Amorphous " electrochomeric films：
Take 300g tungsten chlorides, 2.787g nitric acid tin, 0.0693g antimony trichloride, be dissolved in 500mL methanol, 513mL ethanol
In mixed solution, 10mL deionized waters are added thereto, are stirred 2 hours at normal temperatures fully after dissolving, are obtained tungstenic, indium, tin
Complex sol；Using Best-Effort request or spin coating technique, by gained complex sol even application in transparent conductive oxide base
On plate, gel mould is formed, after drying 10min at a temperature of 150 DEG C, is put into heat-treatment furnace in 200~300 DEG C of oxygen atmosphere
Lower insulation 1h, is then drawn off, and is air-cooled to room temperature and obtains " nanocrystalline-the WO of ATO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is at 63%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 50%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 4%.
Embodiment 5
Prepare " nanocrystalline-the WO of ATO3Amorphous " electrochomeric films：
10g tungsten chlorides, 0.929g nitric acid tin, 0.0231g antimony trichloride are taken, is dissolved in 400mL methanol and 107mL second
In glycol methyl ether mixed solution, thereto add 5mL deionized waters, at normal temperatures stir 2 hours fully dissolving after, obtain tungstenic,
The complex sol of indium, tin；Using Best-Effort request or spin coating technique, by gained complex sol even application in transparent conductive oxide
On glass substrate, gel mould is formed, after drying 10min at a temperature of 150 DEG C, is put into heat-treatment furnace in 200~300 DEG C of oxygen
1h is incubated under gas atmosphere, is then drawn off, room temperature is air-cooled to and obtains " nanocrystalline-the WO of ATO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is at 65%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 48%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 3%.
Embodiment 6
Prepare " nanocrystalline-the WO of ATO3Amorphous " electrochomeric films：
Take 12g tungsten chlorides, 0.929g nitric acid tin, 0.0231g antimony trichloride, be dissolved in 150mL methanol, 50mL ethanol,
In the mixed solution of 53mL ethylene glycol monomethyl ethers, 2.5mL deionized waters are added thereto, stir fully dissolving in 2 hours at normal temperatures
Afterwards, the complex sol of tungstenic, indium, tin is obtained；Using Best-Effort request or spin coating technique, by gained complex sol even application in transparent
On conductive oxide glass substrate, gel mould is formed, after drying 10min at a temperature of 150 DEG C, is put into heat-treatment furnace in 200
1h is incubated under~300 DEG C of oxygen atmosphere, is then drawn off, room temperature is air-cooled to and obtains " nanocrystalline-the WO of ATO3Amorphous " two-phase
Laminated film.
Film obtained by the present embodiment, it is at 70%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 51%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 2%.
Embodiment 7
Prepare " nanocrystalline-the WO of AZO3Amorphous " electrochomeric films：
39.66g tungsten chlorides, 1.4875g zinc nitrates, 0.1125g aluminum nitrate are taken, is dissolved in 667mL ethanol, is added thereto
Enter 6.7mL deionized waters, stir at normal temperatures 2 hours after fully dissolving, obtain the complex sol of tungstenic, indium, tin；Carried using dipping
Drawing or spin coating technique, by gained complex sol even application on transparent conductive oxide substrate, gel mould is formed,
After drying 10min at a temperature of 150 DEG C, it is put into heat-treatment furnace and 1h is incubated under 200~300 DEG C of oxygen atmosphere, then by it
Take out, be air-cooled to room temperature and obtain " nanocrystalline-the WO of AZO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is at 64%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 45%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 3%.
Embodiment 8
Prepare " nanocrystalline-the WO of AZO3Amorphous " electrochomeric films：
19.83g tungsten chlorides, 2.9749g zinc nitrates, 0.2251g aluminum nitrate are taken, is dissolved in 1000mL ethylene glycol monomethyl ethers,
10mL deionized waters are added thereto, are stirred at normal temperatures 2 hours after fully dissolving, and obtain the complex sol of tungstenic, indium, tin；Adopt
It is with Best-Effort request or spin coating technique, gained complex sol even application is solidifying on transparent conductive oxide substrate, being formed
Glued membrane, after drying 10min at a temperature of 150 DEG C, it is put into heat-treatment furnace and is incubated 1h under 200~300 DEG C of oxygen atmosphere, with
After be drawn off, be air-cooled to room temperature and obtain " nanocrystalline-the WO of AZO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is at 72%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 56%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 4%.
Embodiment 9
Prepare " nanocrystalline-the WO of AZO3Amorphous " electrochomeric films：
9.91g tungsten chlorides, 0.7437g zinc nitrates, 0.0563g aluminum nitrate are taken, is dissolved in 250mL methanol, is added thereto
Enter 2.5mL deionized waters, stir at normal temperatures 2 hours after fully dissolving, obtain the complex sol of tungstenic, indium, tin；Carried using dipping
Drawing or spin coating technique, by gained complex sol even application on transparent conductive oxide substrate, gel mould is formed,
After drying 10min at a temperature of 150 DEG C, it is put into heat-treatment furnace and 1h is incubated under 200~300 DEG C of oxygen atmosphere, then by it
Take out, be air-cooled to room temperature and obtain " nanocrystalline-the WO of AZO3Amorphous " two-phase laminated film.
Film obtained by the present embodiment, it is at 74%, 1200nm wave bands in the optical modulation contrast △ T% of visible light wave range
Optical modulation contrast △ T% be 50%, 100 × 100mm2Film changes colour response time 1s, after fade treatment 2000 times,
Film magnitude of the stored charge declines only 3%.
Comparative example
Prepare amorphous WO3Electrochomeric films：
0.9914g tungsten chlorides are taken, are dissolved in 50mL methanol, fully dissolving in 2 hours is stirred at normal temperatures, obtains tungsten oxide forerunner
Colloidal sol；Using Best-Effort request or spin coating technique, by gained complex sol even application on transparent conductive oxide substrate,
Gel mould is formed, after drying 10min at a temperature of 150 DEG C, is put into heat-treatment furnace and is protected under 200~300 DEG C of oxygen atmosphere
Warm 1h, is then drawn off, and is air-cooled to room temperature and obtains amorphous WO3Film.
The coloured state of contrast film obtained by the present embodiment and the transmittance curve of colour fading state are as shown in figure 1, in visible light wave
The optical modulation contrast △ T% of section are 40%；Optical modulation contrast △ T% at 1200nm wave bands are 3%；100×
100mm2Film discoloration response time 6s, the electrochromism response time figure of film is shown in Fig. 2 obtained by the present embodiment；Fade treatment
After 2000 times, film magnitude of the stored charge declines 60%.
Tungsten oxide film is prepared into noncrystal membrane by the present invention, because the heterogeneous microstructure of non-crystalline material is that short distance is unordered
, therefore the nanochannel for being advantageous to lithium ion disengaging is easily produced in amorphous oxide tungsten, and in the oxidation tungsten basal body of amorphous
Middle incorporation TCO is nanocrystalline, can increase the disordered structure of material internal, produce more Nanoscale channels, in addition, TCO is nanocrystalline
Itself there is near-infrared electrochromic property, by the nanocrystalline incorporation tungsten oxide non-crystalline materials of TCO, form " nanocrystalline-the WO of TCO3
Amorphous " laminated film, it can not only improve tungsten oxide film visible spectrum modulation capability, increase the service life, and can also improve
It makes that tungsten oxide system electrochomeric glass spectral tuning is higher, heat-proof quality is more preferable in the modulation capability of near infrared band.
Claims (3)
1. a kind of preparation method of nanocrystalline enhancing tungsten oxide electrochomeric films, it is characterised in that comprise the following steps that：
Step 1, after tungsten chloride and TCO being mixed with metal nitrate, it is dissolved in organic solvent, obtains mixed solution；Thereto plus
Enter deionized water, stir 2h at normal temperatures, fully after dissolving, obtain complex sol；
The TCO metal nitrates, it is the mixture of nitric acid tin and indium nitrate；Or the mixture of nitric acid tin and antimony trichloride；
Or the mixture of zinc nitrate and aluminum nitrate；The mol ratio of nitric acid tin, indium nitrate and tungsten chloride is 0.1:1:5~20；Or tri-chlorination
The mol ratio of antimony, nitric acid tin and tungsten chloride is 0.04:1:10~100；Or aluminum nitrate:Zinc nitrate:The mol ratio of tungsten chloride is
0.06:1:5~20；
Step 2, using Best-Effort request or spin coating technique, by step 1 gained complex sol even application in transparent conductive oxide
On glass substrate, gel mould is formed；
Step 3, step 2 gained gel mould is placed in 150 DEG C of environment after 10min, be put into heat-treatment furnace in 200~300 DEG C
Oxygen atmosphere under be incubated 1 hour, be then drawn off, be air-cooled to room temperature, produce electrochomeric films.
2. a kind of preparation method of nanocrystalline enhancing tungsten oxide electrochomeric films according to claim 1, its feature exist
In in step 1, organic solvent is one kind or any several with obtained by arbitrary proportion in methanol, ethanol and ethylene glycol monomethyl ether
Mixture, the molar concentration of tungsten chloride is 0.05~0.15mol/L in gained mixed solution.
3. a kind of preparation method of nanocrystalline enhancing tungsten oxide electrochomeric films according to claim 1, its feature exist
In in step 1, the volume ratio of deionized water and organic solvent is 1：100.
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| WO2017137396A1 (en) * | 2016-02-11 | 2017-08-17 | Basf Se | Electrochromic devices |
| CN107098596B (en) * | 2017-04-24 | 2020-06-23 | 揭阳市宏光镀膜玻璃有限公司 | Preparation method of silk-screen printing molybdenum-doped tungsten oxide nanostructure electrochromic film |
| CN107512853B (en) * | 2017-08-17 | 2020-07-24 | 浙江大学 | Al with mosaic structure 2O3/WO3Nano composite electrochromic film and preparation method thereof |
| CN107512854B (en) * | 2017-08-17 | 2020-05-08 | 浙江大学 | ITO/WO with nano mosaic structure3Composite electrochromic film and preparation method thereof |
| CN107382092A (en) * | 2017-08-17 | 2017-11-24 | 浙江大学 | TiO with Nanoparticles Embedded structure2 /WO3Compound electrochromic membrane and preparation method thereof |
| CN107555810A (en) * | 2017-08-17 | 2018-01-09 | 浙江大学 | A kind of tungsten oxide electrochromism laminated film of Nanocrystals Embedded |
| CN107986637B (en) * | 2017-11-23 | 2020-08-18 | 西安理工大学 | Preparation method of in-situ crystallized tin-doped indium oxide nanocrystalline thin film |
| CN107935405B (en) * | 2017-11-23 | 2020-09-25 | 西安理工大学 | Preparation method of antimony-doped tin oxide electrochromic film |
| CN107935408B (en) * | 2017-12-16 | 2020-08-18 | 西安理工大学 | Multilayer electrochromic film and preparation method thereof |
| CN108439821B (en) * | 2018-02-05 | 2020-11-17 | 西安理工大学 | High-performance dual-frequency independent modulation electrochromic film and preparation method thereof |
| CN108465465A (en) * | 2018-04-04 | 2018-08-31 | 广东工业大学 | A kind of semiconductive thin film and preparation method thereof |
| CN108483939B (en) * | 2018-04-17 | 2021-04-06 | 西安理工大学 | Electrochromic film capable of effectively modulating sunlight transmittance and preparation method thereof |
| CN108585539B (en) * | 2018-04-17 | 2021-01-15 | 西安理工大学 | Long-life electrochromic film capable of selectively regulating light and heat and preparation method thereof |
| CN108828868B (en) * | 2018-05-02 | 2021-06-04 | 上海大学 | Preparation method of electrochromic film |
| CN109704591B (en) * | 2019-01-29 | 2021-10-22 | 西安理工大学 | Visible-near infrared double-frequency modulated single-phase electrochromic film and preparation method thereof |
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| CN103999251A (en) * | 2011-07-25 | 2014-08-20 | 加州大学校务委员会 | Electrochromic nanocomposite films |
| CN102646759B (en) * | 2012-05-04 | 2015-05-27 | 深圳市科聚新材料有限公司 | Preparing method for transparent conductive oxide film |
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