CN107555810A - A kind of tungsten oxide electrochromism laminated film of Nanocrystals Embedded - Google Patents
A kind of tungsten oxide electrochromism laminated film of Nanocrystals Embedded Download PDFInfo
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- CN107555810A CN107555810A CN201710705116.9A CN201710705116A CN107555810A CN 107555810 A CN107555810 A CN 107555810A CN 201710705116 A CN201710705116 A CN 201710705116A CN 107555810 A CN107555810 A CN 107555810A
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- nanocrystalline
- laminated film
- tungsten
- tungsten oxide
- electrochromism
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Abstract
The present invention discloses a kind of tungsten oxide electrochromism laminated film of Nanocrystals Embedded, including aoxidizes tungsten basal body and be evenly distributed on nanocrystalline in oxidation tungsten basal body；It is described it is nanocrystalline be ZnO, TiO2, ITO, Al2O3Or SiO2In one kind.The present invention's meets in film, due to the nanocrystalline specific surface area with larger non-stoichiometric, with excellent electro-chemical activity, the hetero-junctions with nano combined effect is formed with amorphous tungsten, the laminated film of the structure shows excellent electrochromism spectral modulation performance and faster electrochromism response speed, can be applicable to electrochromic intelligent dimming glass field.
Description
Technical field
The present invention relates to a kind of nanocrystalline/tungsten oxide complex thin film structure, more particularly to a kind of oxidation of Nanocrystals Embedded
Tungsten electrochromism laminated film.
Background technology
So-called electrochromism refers in the presence of applied voltage or electric field, and material color or transmitance are stablized reversible
Change.The research of electrochromic effect will trace back to Deb in 1966 to amorphous state WO3The preparation of film, learn both at home and abroad since then
Person has carried out deeply extensive research around electrochomeric films and its application.At present, electrochromic material is considered as most to have
One of intellectual material of application prospect, in Intelligent energy-saving window (smart window), automobile anti-glazing rearview mirror, electrochromic display
The directions such as device have huge potential using value.
Nanocrystalline material is often with having superior chemical and photoelectric characteristic, such as high electrochemical activity surface, local surface plasma
Resonance body, electroluminescent etc., this mainly has benefited from the surface of its nano effect and high-specific surface area and non-stoichiometric
Structure.In numerous electrochromic materials, tungsten oxide has cheap nothing as most common inorganic cathode electrochromic material
The advantages that malicious superior performance is stable, is received significant attention.The preparation method of general tungsten oxide film includes chemical vapor deposition, penetrated
RF sputtering, collosol and gel etc., pure zirconia W film prepared by these methods often due to structure is dense, chemism compared with
Low, the migration of its intermediate ion or electronics is affected, and often spectral modulation amplitude is not high, and the response time is longer, becomes colour efficiency not
It is high.The nanocrystalline and amorphous tungsten of small size is compounded to form nanocrystalline/tungsten oxide bluk recombination film with mosaic texture,
It is nanocrystalline to form mosaic texture in tungsten basal body is aoxidized, hetero-junctions can be formed in the film, there is nano combined effect, strengthened
The electrochromic property of tungsten oxide.
The content of the invention
It is an object of the invention to propose a kind of tungsten oxide electrochromism laminated film of Nanocrystals Embedded, the composite
With excellent electrochromic property, suitable for electrochromic intelligent energy-saving field.
Concrete technical scheme of the present invention is as follows：
The tungsten oxide electrochromism laminated film of a kind of Nanocrystals Embedded, it is characterised in that including oxidation tungsten basal body and
It is even be distributed in oxidation tungsten basal body in it is nanocrystalline；
It is described it is nanocrystalline be ZnO, TiO2, ITO, Al2O3Or SiO2In one kind.
Need possess the good oxide nanocrystalline of crystallinity in the present invention, in complex thin film structure, it is nanocrystalline to be uniformly distributed
In amorphous tungsten basal body, and with oxidation tungsten basal body carried out on nanoscale it is compound.
Preferably, film thickness is 50~1000nm.
Preferably, the nanocrystalline crystallite dimension is in the range of 3nm~20nm.
Preferably, described oxidation tungsten basal body is amorphous state.
Preferably, it is described it is nanocrystalline with the compound yardstick of oxidation tungsten basal body in below 100nm, i.e., in any 100nm scopes
It is compound inside all to there is nanocrystalline and tungsten oxide two-phase.
It is further preferred that it is described it is nanocrystalline be ZnO.
The film of the Nanocrystals Embedded structure of the present invention can be assembled into tool as electrochromic material with combinations such as NiO
Have the electrochromic device of EO-1 hyperion modulation amplitude, optionally can absorb or reflect under electric field action the external world heat radiation and
Internal hot diffusion, reduce office block and residential houses and keep feeling nice and cool what is kept warm with winter and must consume in summer
Mass energy, it is a main direction of development of modern energy saving building material.
In the present invention, due to the nanocrystalline specific surface area with larger non-stoichiometric, there is excellent electrochemistry
Activity, and amorphous tungsten form the hetero-junctions with nano combined effect, and the laminated film of the structure shows excellent
Electrochromism spectral modulation performance and faster electrochromism response speed, it can be applicable to electrochromic intelligent dimming glass neck
Domain.
Brief description of the drawings
Fig. 1 is the structural representation of the tungsten oxide electrochromism laminated film of Nanocrystals Embedded；
Fig. 2 is ZnO nano crystalline substance/WO3The TEM photos of complex thin film structure；
Fig. 3 is ZnO nano crystalline substance/WO3Laminated film electrochromism spectral modulation performance；
Fig. 4 is ZnO nano crystalline substance/WO3The electrochromism response time of laminated film.
Embodiment
The present invention is described in detail with reference to embodiment and accompanying drawing, but the present invention is not limited to this.
Case study on implementation 1：
ZnO nano crystalline substance/WO in the present embodiment3Laminated film, using amorphous tungsten as matrix, zinc oxide (ZnO)
It is nanocrystalline to be evenly distributed in amorphous tungsten.
The implementation case is used as substrate using ito glass (30mm × 30mm), carries out following cleaning step before coating：
In acetone by ito glass be cleaned by ultrasonic 30min → deionized water rinsing 3 times then be put into ultrasonic 30min in deionized water → go from
Ultrasonic 30min → drying, standby is carried out after being rinsed 3 times in sub- water in ethanol.
Prepare comprising the following steps that for laminated film in the present embodiment：
Step (1)：0.5g solubility ZnO nano crystalline flours end ultrasonic disperse is dissolved in 10mL water, it is water-soluble to form ZnO nano crystalline substance
Liquid；
Step (2)：2g ammonium metatungstates are added in the foregoing gained ZnO nano crystalline substance aqueous solution, supersound process obtains compound molten
Liquid；
Step (3)：3mL ethanol and 2mL PEG600 are sequentially added in foregoing gained composite solution, is ultrasonically treated；
Step (4)：Using spin coating instrument by step (3) resulting solution spin coating ito substrate after cleaning；Spin coating rotating speed is
500r/min spin coating time 5s, then rotating speed 3000r/min spin coating times 20s；
Step (5)：Wet film made from step (4) is first heat-treated in air atmosphere, heat treatment temperature is 350 DEG C, is protected
The warm time is 60min, and ZnO/WO3 nano compound films are made.
ZnO nano crystalline substance/the WO being prepared3Its TEM photo of laminated film is as shown in Fig. 2 can be clearly seen that film
In Nanocrystals Embedded structure.The electrochromism spectral modulation performances of ZnO nano crystalline substance/WO3 laminated films as shown in figure 3,
Spectral modulation amplitude at 633nm is 54%.Electrochromism response times of ZnO nano crystalline substance/WO3 laminated films as shown in figure 4,
Coloration time is 10.8s, fading time 2.6s.
Case study on implementation 2：
TiO in the present embodiment2Nanocrystalline/WO3Laminated film, using amorphous tungsten as matrix, titanium oxide (TiO2)
It is nanocrystalline to be evenly distributed in amorphous tungsten.
The implementation case is used as substrate using ito glass (30mm × 30mm), carries out following cleaning step before coating：
In acetone by ito glass be cleaned by ultrasonic 30min → deionized water rinsing 3 times then be put into ultrasonic 30min in deionized water → go from
Ultrasonic 30min → drying, standby is carried out after being rinsed 3 times in sub- water in ethanol.
Prepare comprising the following steps that for laminated film in the present embodiment：
Step (1)：By 0.45g TiO2Manocrystalline powders ultrasonic disperse is dissolved in 6mL water, forms TiO2The nanocrystalline aqueous solution；
Step (2)：1.5g ammonium metatungstates are added in the foregoing nanocrystalline aqueous solution of gained TiO2, supersound process obtains compound
Solution；
Step (3)：Before state to sequentially add 2mL ethanol and 1mL PEG600 in composite solution, be ultrasonically treated；
Step (4)：Using spin coating instrument by step (3) resulting solution spin coating ito substrate after cleaning；Spin coating rotating speed is
500r/min spin coating time 5s, then rotating speed 3000r/min spin coating times 20s；
Step (5)：Wet film made from step (4) is first heat-treated in air atmosphere, heat treatment temperature is 350 DEG C, is protected
The warm time is 60min, and TiO is made2/WO3Nano compound film.
Laminated film obtained by this implementation example, the spectral modulation amplitude at 633nm are 46%, coloration time 7.9s,
Fading time is 2.8s.
Case study on implementation 3：
SiO in the present embodiment2Nanocrystalline/WO3Laminated film, using amorphous tungsten as matrix, silica (SiO2)
It is nanocrystalline to be evenly distributed in amorphous tungsten.
The implementation case is used as substrate using ito glass (30mm × 30mm), carries out following cleaning step before coating：
In acetone by ito glass be cleaned by ultrasonic 30min → deionized water rinsing 3 times then be put into ultrasonic 30min in deionized water → go from
Ultrasonic 30min → drying, standby is carried out after being rinsed 3 times in sub- water in ethanol.
Prepare comprising the following steps that for laminated film in the present embodiment：
Step (1)：By 0.3g SiO2Manocrystalline powders ultrasonic disperse is dissolved in 6mL dimethylformamides (DMF), forms TiO2
Nanocrystalline DMF solution；
Step (2)：1.5g ammonium metatungstates are added into foregoing gained SiO2In nanocrystalline DMF solution, supersound process obtains
Composite solution；
Step (3)：Before state to sequentially add 2mL ethanol in composite solution, be ultrasonically treated；
Step (4)：Using spin coating instrument by step (3) resulting solution spin coating ito substrate after cleaning；Spin coating rotating speed is
500r/min spin coating time 5s, then rotating speed 1000r/min spin coating times 20s；
Step (5)：Wet film made from step (4) is first heat-treated in air atmosphere, heat treatment temperature is 350 DEG C, is protected
The warm time is 60min, and SiO is made2Nanocrystalline/WO3Nano compound film.
Laminated film obtained by this implementation example, the spectral modulation amplitude at 633nm is 46%, coloration time 8s, is taken off
The color time is 4.3s.
The foregoing is only the preferable implementation example of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (6)
1. the tungsten oxide electrochromism laminated film of a kind of Nanocrystals Embedded, it is characterised in that including oxidation tungsten basal body and uniformly
It is distributed in nanocrystalline in oxidation tungsten basal body；
It is described it is nanocrystalline be ZnO, TiO2, ITO, Al2O3Or SiO2In one kind.
2. tungsten oxide electrochromism laminated film as claimed in claim 1, it is characterised in that film thickness be 50~
1000nm。
3. tungsten oxide electrochromism laminated film as claimed in claim 1, it is characterised in that the nanocrystalline crystallite dimension
In the range of 3nm~20nm.
4. tungsten oxide electrochromism laminated film as claimed in claim 1, it is characterised in that described oxidation tungsten basal body is nothing
Shape state.
5. tungsten oxide electrochromism laminated film as claimed in claim 1, it is characterised in that described nanocrystalline and tungsten oxide base
The compound yardstick of body is in below 100nm.
6. tungsten oxide electrochromism laminated film as claimed in claim 1, it is characterised in that it is described it is nanocrystalline be ZnO.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650741A (en) * | 2019-02-21 | 2019-04-19 | 合肥工业大学 | A kind of tungsten trioxide nano bowl electrochromic material and preparation method thereof |
| CN110391583A (en) * | 2019-07-03 | 2019-10-29 | 浙江大学 | Saturable absorber and preparation method thereof based on non-stoichiometric transition metal oxide film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036564A (en) * | 2015-06-25 | 2015-11-11 | 西安理工大学 | Nanocrystalline enhanced tungsten oxide electrochromic film and preparation method thereof |
-
2017
- 2017-08-17 CN CN201710705116.9A patent/CN107555810A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036564A (en) * | 2015-06-25 | 2015-11-11 | 西安理工大学 | Nanocrystalline enhanced tungsten oxide electrochromic film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 袁广中 等: "纳米晶增强TiO2@WO3复合薄膜电致变色性能及其电化学机理研究", 《硅酸盐通报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650741A (en) * | 2019-02-21 | 2019-04-19 | 合肥工业大学 | A kind of tungsten trioxide nano bowl electrochromic material and preparation method thereof |
| CN109650741B (en) * | 2019-02-21 | 2021-09-10 | 合肥工业大学 | Tungsten trioxide nanometer bowl electrochromic material and preparation method thereof |
| CN110391583A (en) * | 2019-07-03 | 2019-10-29 | 浙江大学 | Saturable absorber and preparation method thereof based on non-stoichiometric transition metal oxide film |
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