CN108191257A - A kind of method that electrochomeric films are prepared using spray pyrolysis - Google Patents
A kind of method that electrochomeric films are prepared using spray pyrolysis Download PDFInfo
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- CN108191257A CN108191257A CN201810012211.5A CN201810012211A CN108191257A CN 108191257 A CN108191257 A CN 108191257A CN 201810012211 A CN201810012211 A CN 201810012211A CN 108191257 A CN108191257 A CN 108191257A
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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
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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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
- C03C2217/70—Properties of coatings
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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
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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
- C03C2218/112—Deposition methods from solutions or suspensions by spraying
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Abstract
The present invention relates to a kind of method that electrochomeric films are prepared using spray pyrolysis, including:AMT is dissolved in deionized water, stirs, obtains the aqueous solution of AMT hydrates;Polyethylene glycol PEG 400 is added in, continues to stir, obtains vitreosol;Ammonium molybdate is added in, stirring obtains precursor solution;FTO electro-conductive glass is sprayed at, it is in situ to thermally decompose, obtain tungsten oxide/molybdenum oxide compound electrochromic membrane.The method of the present invention preparation process is simple, at low cost;Electrochomeric films obtained discoloration is uniform, function admirable, available in electrochromic device, can effective electrochromic property, feasibility is provided for large area production, with larger application prospect.
Description
Technical field
The invention belongs to electrochomeric films technical fields, more particularly to a kind of to prepare electrochromism using spray pyrolysis
The method of film.
Background technology
Electrochromism refer to material stablize under DC Electric Field, reversible color change the phenomenon that.Electricity consumption mutagens
The device that color material is assembled into is known as electrochromic device.General electrochromic device achieves that light under the voltage of very little
Learn the reversible change of property.The reversible change of this optical property and the smaller particular advantages of required voltage, make it in intelligence
The fields such as window, display and visualization ultracapacitor are with a wide range of applications.Electrochromic device be usually by with
Under several parts composition:Conductive layer, electrochromic layer and the electrolyte layer being deposited in substrate, wherein electrochromic layer are outstanding
Its important part.Electrochromic material includes inorganic electrochromic material and organic electrochromic material.Inorganic electroluminescence becomes
Color material includes tungstic acid, nickel oxide, yttrium oxide, niobium pentaoxide etc.;Organic electrochromic material includes polyaniline, poly- thiophene
Fen etc..
Inorganic electrochromic material is most widely used, and preparation method includes vapour deposition method, magnetron sputtering method, chemical vapor deposition
Product, spray pyrolysis, sol-gal process, electro-deposition and anodizing etc..
In electrochromic material, tungsten oxide is most widely used.In recent years, with the development of doping techniques, research
Personnel wish to obtain the tungsten oxide electrochomeric films of function admirable by doping techniques.Zhang Xuping et al. exists《Photoelectron technology》
It has been delivered on Vol.17No.1Mar.1997 and has prepared the electrochromic of molybdenum oxide doped tungsten oxide using electron beam evaporation process
Method.Although the method can prepare the tungsten oxide electrochomeric films of the pretty good doping molybdenum oxide of performance, the method
In practical applications also there are it is many problem of, such as:(1) preparation process is complicated, higher to technique, preparation environmental requirement;(2) institute
The ultrahigh vacuum coater equipment used is expensive.
Invention content
The technical problems to be solved by the invention are to provide a kind of side that electrochomeric films are prepared using spray pyrolysis
Method, the method for the present invention preparation process are simple, at low cost;With the industry application possibility being film-made in glass surface.
A kind of method that electrochomeric films are prepared using spray pyrolysis of the present invention, including:
(1) ammonium metatungstate AMT is dissolved in deionized water, stirs to being completely dissolved, obtain the aqueous solution of AMT hydrates;
Polyethylene glycol PEG-400 is added in, continues to stir, obtains vitreosol;The mass ratio of wherein AMT and PEG-400 is 1:8~12;
(2) ammonium molybdate is added in into the vitreosol that step (1) obtains, stirs to clarify, obtain precursor solution;Wherein
The molar ratio of ammonium molybdate and AMT in step (1) are 0.1~12:1;
(3) precursor solution that step (2) obtains is sprayed at FTO electro-conductive glass, then thermal decomposition in situ, is aoxidized
Tungsten/molybdenum oxide compound electrochromic membrane.
A concentration of 0.008~0.012mol/L of the aqueous solution of AMT hydrates in the step (1).
The temperature stirred in the step (1) is 65~75 DEG C.
Continue in the step (1) stirring technological parameter be:It is 65~75 DEG C to continue whipping temp, continues mixing time
For 40~50min.
The temperature stirred in the step (2) is 75~85 DEG C.
The technological parameter thermally decomposed in situ in the step (3) is:Heat decomposition temperature in situ is 300~450 DEG C, in-situ heat
Resolving time is 20~30min.
The present invention prepares electrochomeric films in electro-conductive glass substrate by spray pyrolysis, breaches existing preparation
The technical bottleneck of electrochomeric films material, the extensive industrialization to realize electrochomeric glass are laid a solid foundation.
The unique structure of tungsten oxide/molybdenum oxide compound electrochromic membrane obtained by the present invention has more hole,
Larger electrochemical reaction active surface can be provided, significantly shorten reaction time (Coloring Time<15s), coloration efficiency
(40.1cm2/C cm2/ C) and the electrochromic properties such as cyclical stability (1000 times cycle electrochomeric films without significant change).
Advantageous effect
(1) present invention sprays liquid precursor by the FTO conductive glass surfaces in heating, and presoma is in FTO conduction glass
Glass surface forms electrochomeric films, method is simple, of low cost, has electroluminescent in glass surface system by in-situ thermal oxidation
The industry application feasibility of optically variable films.
(2) spray pyrolysis employed in the present invention can be used for extensive deposition, be prepared by spray pyrolysis thin
The crystal grain of film is superfine, and with special pattern, so as to be conducive to element doping, is effectively improved electrochromic property.
(3) tungsten oxide/molybdenum oxide compound electrochromic membrane of the invention has porous structure, and this porous structure both contracted
The short diffusion path of ion in the film, and its active surface is enable to be fully utilized, so as to effectively increase film
Electrochromic property, Coloring Time<15s, coloration efficiency is up to 40.1cm2/ C, and with cyclical stability.
(4) electrochomeric films produced by the present invention discoloration is uniform, function admirable, available in electrochromic device, and
The electrochromic property of device can be effectively improved, feasibility is provided, and electroluminescent for the production of electrochromic device large area
There is larger application prospect in Electrochromic device industrialization.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of tungsten oxide/molybdenum oxide compound electrochromic membrane in embodiment 1;
Fig. 2 is that electrochromic device applies negative pressure (left side) and applies the digital photograph figure of positive pressure (right side) in embodiment 1;
Fig. 3 is that electrochromic device is colouring and the light transmission rate curve under bleached state in embodiment 1;
Fig. 4 is the electrochromism time response curve of electrochromic device in embodiment 2;
Fig. 5 is optical density (OD) difference-charge density curve of electrochromic device in embodiment 2;
Fig. 6 is the scanning electron microscope (SEM) photograph of tungsten oxide electrochomeric films in comparative example 1;
Fig. 7 is that electrochromic device applies negative pressure (left side) and applies the digital photograph figure of positive pressure (right side) in comparative example 1;
Fig. 8 is that electrochromic device is colouring and the light transmission rate curve under bleached state in comparative example 1;
Fig. 9 is the electrochromism time response curve of electrochromic device in comparative example 1;
Figure 10 is optical density (OD) difference-charge density curve of electrochromic device in comparative example 1.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) 9.18g AMT are dissolved in 300mL deionized waters, are stirred at 70 DEG C to being completely dissolved, obtained a concentration of
The aqueous solution of the AMT hydrates of 0.01mol/L;91.8g PEG-400 are added in, continues 70 DEG C of stirring 45min, obtains clear
Bright colloidal sol.
(2) 1.18g ammonium molybdates are added in into the vitreosol that 100mL steps (1) obtain, 80 DEG C stir to clarify, and obtain
Precursor solution.
(3) precursor solution that 100mL steps (2) obtain is sprayed on 5 × 2.5cm in laboratory conditions2FTO lead
On electric glass, 20min is then thermally decomposed in situ at 450 DEG C, obtains tungsten oxide/molybdenum oxide compound electrochromic membrane.
The scanning electron microscope (SEM) photograph of tungsten oxide made from the present embodiment/molybdenum oxide compound electrochromic membrane, as shown in Figure 1, can
Know that tungsten oxide and molybdenum oxide are compound relatively good.
Tungsten oxide made from the present embodiment/molybdenum oxide compound electrochromic membrane is assembled into electrochromic device, device
The light transmission rate of obtained device is measured with two electrode system combination electrochemical workstations and solid ultraviolet-uisible spectrophotometer
Variation and electrochromism response speed, and coloration efficiency is calculated, test electrochromic property.The result shows that:As application negative pressure -3V
When, device becomes blue;When applying positive pressure+2V, device fades phenomenon, as shown in Figure 2;The light transmittance of the device 300~
800nm wave bands are without too apparent variation, and it is 32.08% to be reached at λ=632.8nm, as shown in Figure 3;The response time of the device
It can control within 15s, coloration efficiency reaches 40.1cm2/C.The device has non-in following electrochromic intelligent window field
Often good application prospect.
Embodiment 2
(1) 10.64g AMT are dissolved in 300mL deionized waters, are stirred at 70 DEG C to being completely dissolved, obtained a concentration of
The aqueous solution of the AMT hydrates of 0.012mol/L;127.73g PEG-400 are added in, continues 70 DEG C of stirring 45min, is clarified
Vitreosol.
(2) 1.37g ammonium molybdates are added in into the vitreosol that 100mL steps (1) obtain, 80 DEG C stir to clarify, and obtain
Precursor solution.
(3) precursor solution that 100mL steps (2) obtain is sprayed on 5 × 2.5cm in laboratory conditions2FTO lead
On electric glass, 25min is then thermally decomposed in situ at 400 DEG C, obtains tungsten oxide/molybdenum oxide compound electrochromic membrane.
Tungsten oxide made from the present embodiment/molybdenum oxide compound electrochromic membrane is assembled into electrochromic device, device
The light transmission rate of obtained device is measured with two electrode system combination electrochemical workstations and solid ultraviolet-uisible spectrophotometer
Variation and electrochromism response speed, and coloration efficiency is calculated, test electrochromic property.The result shows that:As application negative pressure -3V
When, device becomes blue;When applying positive pressure+2V, device fades phenomenon;The light transmittance of the device 300~800nm wave bands without
Too apparent variation, it is 30.29% to be reached at λ=632.8nm;The response time of the device can be controlled within 15s, such as schemed
Shown in 4;Coloration efficiency reaches 34.5cm2/ C, as shown in Figure 5.The device has very in following electrochromic intelligent window field
Good application prospect.
Comparative example 1
(1) 7.10g AMT are dissolved in 300mL deionized waters, are stirred at 70 DEG C to being completely dissolved, obtained a concentration of
The aqueous solution of the AMT hydrates of 0.008mol/L;56.8g PEG-400 are added in, continues 70 DEG C of stirring 45min, obtains clear
Vitreosol.
(2) vitreosol that 100mL steps (1) obtain is sprayed on 5 × 2.5cm in laboratory conditions2FTO it is conductive
On glass, 30min is then thermally decomposed in situ at 300 DEG C, obtains tungsten oxide electrochomeric films.
The scanning electron microscope (SEM) photograph of tungsten oxide electrochomeric films made from this comparative example, as shown in Figure 6, it is known that oxidation obtained
Tungsten electrochomeric films are porous and pattern is uniform.
Tungsten oxide electrochomeric films made from comparative example are assembled into electrochromic device, two electrode system knots of device
Electrochemical workstation and solid ultraviolet-uisible spectrophotometer are closed to measure the variation of the light transmission rate of obtained device and electrochromism
Response speed, and coloration efficiency is calculated, test electrochromic property.The result shows that:When applying negative pressure -3V, device can be slightly
Become blue;When applying positive pressure+2V, device fades phenomenon, as shown in Figure 7;The light transmittance of the device is in 300~800nm
Wave band is without too apparent variation, and it is 16.48% to be reached at λ=632.8nm, as shown in Figure 8;The response time of the device can be controlled
System is within 25s, as shown in Figure 9;Coloration efficiency reaches 21.4cm2/ C, as shown in Figure 10.
Claims (6)
1. a kind of method that electrochomeric films are prepared using spray pyrolysis, including:
(1) ammonium metatungstate AMT is dissolved in deionized water, stirs to being completely dissolved, obtain the aqueous solution of AMT hydrates;It adds in
Polyethylene glycol PEG-400 continues to stir, obtains vitreosol;The mass ratio of wherein AMT and PEG-400 is 1:8~12;
(2) ammonium molybdate is added in into the vitreosol that step (1) obtains, stirs to clarify, obtain precursor solution;Wherein molybdic acid
The molar ratio of ammonium and AMT in step (1) are 0.1~12:1;
(3) precursor solution that step (2) obtains is sprayed at FTO electro-conductive glass, then thermal decomposition in situ, obtain tungsten oxide/
Molybdenum oxide compound electrochromic membrane.
2. a kind of method that electrochomeric films are prepared using spray pyrolysis according to claim 1, it is characterised in that:
A concentration of 0.008~0.012mol/L of the aqueous solution of AMT hydrates in the step (1).
3. a kind of method that electrochomeric films are prepared using spray pyrolysis according to claim 1, it is characterised in that:
The temperature stirred in the step (1) is 65~75 DEG C.
4. a kind of method that electrochomeric films are prepared using spray pyrolysis according to claim 1, it is characterised in that:
Continue in the step (1) stirring technological parameter be:It is 65~75 DEG C to continue whipping temp, continue mixing time for 40~
50min。
5. a kind of method that electrochomeric films are prepared using spray pyrolysis according to claim 1, it is characterised in that:
The temperature stirred in the step (2) is 75~85 DEG C.
6. a kind of method that electrochomeric films are prepared using spray pyrolysis according to claim 1, it is characterised in that:
The technological parameter thermally decomposed in situ in the step (3) is:Heat decomposition temperature in situ is 300~450 DEG C, thermal decomposition time in situ
For 20~30min.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108663868A (en) * | 2018-07-05 | 2018-10-16 | 东华大学 | A kind of preparation method of tungsten oxide electrochromic electrode |
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2018
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WO2015163824A1 (en) * | 2014-04-24 | 2015-10-29 | Nanyang Technological University | Method for forming a transparent conducting polymeric film and its use as a transparent electrode |
CN107406985A (en) * | 2015-01-14 | 2017-11-28 | 列日大学 | Ultrasonic spray pyrolysis deposits the ameliorative way of one or more electrochromic films and/or dielectric film in substrate |
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