CN108298832B - Tungsten oxide electrochomeric films and preparation method thereof with EO-1 hyperion adjustable range - Google Patents
Tungsten oxide electrochomeric films and preparation method thereof with EO-1 hyperion adjustable range Download PDFInfo
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- CN108298832B CN108298832B CN201711478200.8A CN201711478200A CN108298832B CN 108298832 B CN108298832 B CN 108298832B CN 201711478200 A CN201711478200 A CN 201711478200A CN 108298832 B CN108298832 B CN 108298832B
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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
- C03C2217/00—Coatings on glass
- C03C2217/90—Other aspects of coatings
- C03C2217/94—Transparent conductive oxide layers [TCO] being part of a multilayer coating
-
- 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]
-
- 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
Abstract
The invention discloses a kind of preparation methods of tungsten oxide electrochomeric films with EO-1 hyperion adjustable range, configure precursor solution using tungsten hexachloride and oxalic acid as raw material, then be prepared through solvent thermal reaction；In the precursor solution, the concentration of tungsten hexachloride is 1~15g/L.The invention discloses a kind of preparation methods of tungsten oxide electrochomeric films with EO-1 hyperion adjustable range, by introducing oxalic acid as structural adjustment agent, adhesion amount of the tungsten oxide electrochomeric films in conductive substrates is improved under the concentration of the low source W, spectrum adjustable range is effectively improved, raw material availability is increased.The preparation method is simple, low in cost, securely and reliably.
Description
Technical field
The present invention relates to electrochromic material and its preparation fields, and in particular to a kind of oxygen with EO-1 hyperion adjustable range
Change tungsten electrochomeric films and preparation method thereof.
Background technique
Electrochromism refers to material, and there is a phenomenon where reversible changes for its optical property under DC Electric Field, can be applied to
The fields such as building intelligence window, automobile anti-dazzle back vision mirror, display equipment.W18O49It can be stabilized as one kind non-chemical
The oxidation tungsten compound of metering, by a variety of a variety of microstructures of wet-chemical mode controlledly synthesis, in electrochromism, sensor etc.
It is multi-field to show excellent performance, obtain the favor of researchers.
With WCl6The W of various structures is prepared for the source W18O49There are many reports, in 103818964 A of Publication No. CN
A kind of W is disclosed in state's patent document18O49The preparation method of superfine nanowire, comprising: a) by WCl6It is dissolved in triethylene glycol, is formed
WCl6Solution is transferred in reaction kettle, the product after hydro-thermal reaction is centrifuged, washs, dry after obtain W18O49It is ultra-fine to receive
Rice noodles.
For another example, a kind of multidimensional pure phase W is disclosed in the Chinese patent literature of 105036196 A of Publication No. CN18O49's
Preparation method, by WCl6It is added in alcohol, prepares solution, it is sonicated to obtain uniformly mixed solution, then to pour into high pressure anti-
It answers in kettle, in a nitrogen atmosphere, obtains the pure phase W of different morphologies through hydro-thermal reaction18O49。
For another example, it is disclosed in the Chinese patent literature of 105271420 A of Publication No. CN and a kind of prepares nano-scale particle shape
W18O49The method of material, by WCl6It is added in dehydrated alcohol, is configured to solution A；Oxalic acid is added into solution A, so that oxalic acid
And WCl6The ratio between the amount of substance be 5~10:1, obtain solution B；Solution B is sealed, stirring is ultrasonically treated, and solution is obtained
C；Solution C is reacted in homogeneous reactor, after reaction, obtains nano-scale particle shape W18O49Material.
Compared to above a variety of microstructures, with WCl6For the source W, W is prepared through hydro-thermal reaction18O49Film is to electrochromism
Material, light anode etc. have many reports, but known, which generally improves product by improving the initial source W concentration
W18O49The film thickness and compactness extent of film, but a large amount of Precipitations are had in solution, cause the significant wastage of raw material, and WCl6
Costly, this certainly will also lead to greatly improving for production cost.
Therefore, how to efficiently use raw material to increase W18O49Film is in the load capacity of the electrically conducting transparents substrate such as FTO, ITO
A problem to be solved.
Summary of the invention
The invention discloses a kind of preparation methods of tungsten oxide electrochomeric films with EO-1 hyperion adjustable range, pass through
Oxalic acid is introduced as structural adjustment agent, attachment of the tungsten oxide electrochomeric films in conductive substrates is improved under the concentration of the low source W
Amount effectively improves spectrum adjustable range, increases raw material availability.The preparation method is simple, low in cost, securely and reliably.
Specific technical solution is as follows:
A kind of preparation method of the tungsten oxide electrochomeric films with EO-1 hyperion adjustable range, with tungsten hexachloride and oxalic acid
Precursor solution is prepared for raw material, then is prepared through solvent thermal reaction；
In the precursor solution, the concentration of tungsten hexachloride is 1~15g/L.
It is known in the art that with WCl6W is prepared using solvent thermal reaction for the source W18O49Film, by increasing in precursor solution
The source W concentration, the thickness of adjustable electrochomeric films layer improve electrochromism adjustable range.But with W in precursor solution
The increase of source concentration certainly will have a large amount of precipitatings and be precipitated from solution, cause the significant wastage of raw material.And it tests and sends out through inventor
It is existing, oxalic acid is added as structural adjustment agent, further adjusts oxalic acid and the addition sequence in the source W and the amount ratio of the two, it can
With under lower tungsten source concentration (1~15g/L), obtained on substrate with the comparable film adhesion amount of higher tungsten source concentration, from
And it realizes and improves W18O49The purpose of electrochomeric films spectrum adjustable range.
Preferably, the preparation method, specifically includes:
(1) oxalic acid is mixed with organic solvent, adds tungsten hexachloride after mixing evenly, obtain precursor solution:
(2) transparent conduction base sheet after cleaning is immersed in the precursor solution of step (1) preparation, after solvent thermal reaction
Obtain the tungsten oxide electrochomeric films；
In the precursor solution, the mass ratio of tungsten hexachloride and oxalic acid is 1~4:1~10.
It is found through experiment that the additional amount of oxalic acid is to the W being prepared18O49Film has larger impact, and oxalic acid content increases meeting
Thicken film, while reducing transparent state transmitance, coloured state transmitance also can be reduced accordingly, go out spectrum adjustable range
The rule of reduction after now first increasing.
The addition sequence of oxalic acid and tungsten hexachloride can be to being prepared W18O49The spectrum adjustable range of film generates significant shadow
It rings.It is found through experiment that oxalic acid and organic solvent are added chlordene after mixing in the case where each raw material dosage is all the same
Change tungsten, the W of deposition can be significantly improved18O49The spectrum adjustable range of film.
WCl6It easily hydrolyzes in a humid environment, preferably, the oxalic acid is anhydrous oxalic acid, does not have moisture absorption
Property, additive amount, which increases, can't excessively introduce secondary water, lead to WCl6Hydrolysis.
Preferably, the organic solvent is selected from least one of methanol, ethyl alcohol, isopropanol in step (1).Through trying
Issue after examination and approval it is existing, using different solvents, the W that is prepared18O49The diameter of nano wire can change, and then influence the electrochromism
The response time of device.Consider solvent cost and safety issue, further preferred organic solvent is selected from ethyl alcohol.
Preferably, the concentration of tungsten hexachloride is 1~10g/L in the precursor solution.
Further preferably, the mass ratio of tungsten hexachloride and oxalic acid is 1:2.5~10, tungsten hexachloride in the precursor solution
Concentration be 3.3~6.7g/L.It is found through experiment that the W prepared under above-mentioned optimum condition18O49The spectrum adjustable range of film is most
It is good.
Preferably, the transparent conduction base sheet is selected from FTO transparent conduction base sheet or transparent is conductive in step (2)
Substrate.
Preferably, the solvent thermal reaction temperature is 150~200 DEG C in step (2), the time is 8~15h.Reaction
Temperature is too low or the reaction time is too short cannot form W18O49Nano wire film.
Preferably, the load obtained after solvent thermal reaction has W18O49The substrate of film also successively through ethyl alcohol, water washing,
And heat treatment process.Only being cleaned with ethyl alcohol will increase the electrochromism response time, is only washed with water and is easy to make film being heat-treated
It falls off in the process.
It after heat treatment can further improve W18O49Binding force between film and transparent conduction base sheet.Further preferably, institute
The heat treatment temperature stated is 150~200 DEG C, and the time is 0.5~1h.
The invention also discloses the tungsten oxide electrochromism with EO-1 hyperion adjustable range prepared according to the above method is thin
Film, spectrum adjustable range are 0~80%.Spectrum adjustable range in the present invention refers to that the tungsten oxide electrochomeric films colour
The difference of the transmitance of the transmitance and colour fading state of state.
Compared with prior art, the present invention has the advantage that
Preparation method of the invention is used as structural adjustment agent by introducing oxalic acid, and go forward side by side a successive step oxalic acid and the source W add
The amount ratio for entering sequence and the two, improves W under the concentration of the low source W18O49Adhesion amount of the film on substrate, is greatly improved original
Expect utilization rate.And preparation process is simple, it is low in cost, securely and reliably.
The spectrum adjustable range for the tungsten oxide electrochomeric films being prepared by the above method is very big, can adjust from 0%
It saves to 80%.A kind of completely new thinking is provided to prepare the tungsten oxide electrochomeric films of EO-1 hyperion adjustable range.
Detailed description of the invention
The W that Fig. 1 is comparative example 1 (a figure) and embodiment 2 (b figure) is prepared respectively18O49Electrochomeric films layer scanning electron microscope
Cross-section photographs；
Fig. 2 is W prepared by embodiment 218O49Electrochomeric films layer X ray diffracting spectrum；
Fig. 3 is the W that Examples 1 to 2 and comparative example 1~2 are prepared respectively18O49Electrochomeric films layer transmittance curve figure；
Fig. 4 is the W that embodiment 1 and comparative example 2 are prepared respectively18O49Electrochomeric films layer cyclic voltammetry curve.
Specific embodiment
Embodiment 1
Prepare W18O49Method, steps are as follows:
(1) FTO sheet glass is cleaned with acetone, isopropanol, ethyl alcohol；
(2) 0.5g oxalic acid is dissolved in 30ml ethyl alcohol, stirs 10min, obtain clear solution；
(3) by 0.1g WCl6It is dissolved in clear solution, stirs 20min, obtain glassy yelloe precursor solution；
(4) the FTO sheet glass of cleaning is vertically put into reaction kettle, the presoma for passing through 0.22 μm of organic membrane filter is added
Solution does not cross sheet glass, obtains W after solvent thermal reaction 10 hours through 180 DEG C18O49- FTO glass sample；
(5) by W18O49- FTO glass sample is successively cleaned with ethyl alcohol, water, and 60 DEG C of drying, 200 DEG C of heat treatment 1h are to enhance
W18O49With the contact of FTO substrate.
Electrochromism test is enterprising in CHI 600D electrochemical workstation and 5000 ultraviolet-visible spectrophotometer of Cary
Row, W18O49Film is used as working electrode, Pt to electrode, and Ag/AgCl is as reference electrode, 1M AlCl3As electrolyte,
Using timing coulometry test loop performance, coloured state application -0.75V voltage, colour fading state applies 0.25V voltage.Potential window
It is arranged between -0.75V-0.25V, sweep speed 10mV/s, carries out cyclic voltammetric (CV) test.
Embodiment 2
Prepare W18O49Method, steps are as follows:
(1) FTO sheet glass is cleaned with acetone, isopropanol, ethyl alcohol；
(2) 1.0g oxalic acid is dissolved in 30ml ethyl alcohol, stirs 10min, obtain clear solution；
(3) by 0.1g WCl6It is dissolved in clear solution, stirs 20min, obtain glassy yelloe precursor solution；
(4) the FTO sheet glass of cleaning is vertically put into reaction kettle, the presoma for passing through 0.22 μm of organic membrane filter is added
Solution does not cross sheet glass, obtains W after solvent thermal reaction 10 hours through 180 DEG C18O49- FTO glass sample；
(5) by W18O49- FTO glass sample is successively cleaned with ethyl alcohol, water, and 60 DEG C of drying, 200 DEG C of heat treatment 1h are to enhance
W18O49With the contact of FTO substrate.
A small amount of W is scraped from substrate18O49Powder, after tested after, X ray diffracting spectrum is as shown in Figure 2.
Embodiment 3
Prepare W18O49Method, steps are as follows:
(1) FTO sheet glass is cleaned with acetone, isopropanol, ethyl alcohol；
(2) 0.5g oxalic acid is dissolved in 30ml ethyl alcohol, stirs 10min, obtain clear solution；
(3) by 0.2gWCl6It is dissolved in clear solution, stirs 20min, obtain glassy yelloe precursor solution；
(4) the FTO sheet glass of cleaning is vertically put into reaction kettle, the presoma for passing through 0.22 μm of organic membrane filter is added
Solution does not cross sheet glass, obtains W after solvent thermal reaction 10 hours through 180 DEG C18O49- FTO glass sample；
(5) by W18O49- FTO glass sample is successively cleaned with ethyl alcohol, water, and 60 DEG C of drying, 200 DEG C of heat treatment 1h are to enhance
W18O49With the contact of FTO substrate.
Comparative example 1
Prepare W18O49Method, steps are as follows:
(1) FTO sheet glass is cleaned with acetone, isopropanol, ethyl alcohol；
(2) by 0.1g WCl6It is dissolved in 30ml ethanol solution, stirs 20min, obtain glassy yelloe precursor solution；
(3) the FTO sheet glass of cleaning is vertically put into reaction kettle, the presoma for passing through 0.22 μm of organic membrane filter is added
Solution does not cross sheet glass, obtains W after solvent thermal reaction 10 hours through 180 DEG C18O49- FTO glass sample；
(4) by W18O49- FTO glass sample is successively cleaned with ethyl alcohol, water, and 60 DEG C of drying, 200 DEG C of heat treatment 1h are to enhance
W18O49With the contact of FTO substrate.
Comparative example 2
Prepare W18O49Method, steps are as follows:
(1) FTO sheet glass is cleaned with acetone, isopropanol, ethyl alcohol；
(2) by 0.1gWCl6It is dissolved in 30ml ethyl alcohol, stirs 20min, obtain clear solution；
(3) 0.5g oxalic acid is dissolved in clear solution, stirs 10min, obtain glassy yelloe precursor solution；
(4) the FTO sheet glass of cleaning is vertically put into reaction kettle, the presoma for passing through 0.22 μm of organic membrane filter is added
Solution does not cross sheet glass, obtains W after solvent thermal reaction 10 hours through 180 DEG C18O49- FTO glass sample；
(5) by W18O49- FTO glass sample is successively cleaned with ethyl alcohol, water, and 60 DEG C of drying, 200 DEG C of heat treatment 1h are to enhance
W18O49With the contact of FTO substrate.
A, b in Fig. 1 are corresponding in turn to the W that comparative example 1 and embodiment 2 are prepared respectively18O49The SEM cross-section photographs of film.It is logical
Comparison diagram 1 is crossed it is found that when oxalic acid (comparative example 1) not being added, the film of preparation is grass-like nanowire structure (a figure), can by Fig. 3
Know, is at 633nm in wavelength, spectrum adjustable range is only 39%.After oxalic acid (embodiment 2) is added, as shown in Figure 1, in identical W
The membrane structure (b figure) that bottom is compacted zone, top is grass-like nano wire is prepared under the concentration of source, film adhesion amount increases.Knot
Close Fig. 3, spectrum adjustable range be in wavelength be 77% at 633nm, noticeably greater than the 39% of the 1 identical source W concentration of comparative example is shown
The tungsten oxide electrochomeric films that prepare after oxalic acid is added are shown to improve the remarkable effect of spectrum adjustable range.But continue to increase
Film thickness can also reduce the transmitance of transparent state, be reduced to 85% by 88%.
In addition, the W that comparative example 1 and comparative example 2 are prepared respectively18O49Film layer transmittance curve figure (Fig. 3) is implemented
W prepared by example 118O49Film layer shows bigger spectrum adjustable range, and coloured state is reduced to 20% by 28% at 633nm,
Spectrum adjustable range is increased to 66% by 59%.
The W that embodiment 1 and comparative example 2 are prepared respectively is given in Fig. 418O49Electrochomeric films layer cyclic voltammetric (CV)
Only there are a pair of of redox peaks in curve, CV curve test, and current potential is respectively in -0.5V and -0.6V or so, the electricity occurred
Chemical reaction equation can be described by following formula (1):
The closing area of CV curve can be used to characterize the capacitance of unit area storage, and area is bigger, and unit plane accumulates
The capacitance of storage is bigger.The W prepared compared to comparative example 2, embodiment 118O49Electrochomeric films layer generates more faraday
The closing area of electric current, CV curve gradually increases, with Al3+Deintercalation reaction increase, that is, participate in electrochemical reaction active material
Increase, forms more coloured state AlxW18O49, therefore show bigger spectrum adjustable range.
Claims (6)
1. a kind of preparation method of the tungsten oxide electrochomeric films with EO-1 hyperion adjustable range, which is characterized in that with chlordene
Change tungsten and oxalic acid is that raw material prepares precursor solution, then is prepared through solvent thermal reaction；It specifically includes:
(1) oxalic acid is mixed with organic solvent, adds tungsten hexachloride after mixing evenly, obtain precursor solution: the forerunner
In liquid solution, the concentration of tungsten hexachloride is 1~15g/L, and the mass ratio of tungsten hexachloride and oxalic acid is 1~4:1~10；
(2) transparent conduction base sheet after cleaning is immersed in the precursor solution of step (1) preparation, is obtained after solvent thermal reaction
W18O49Electrochomeric films；The solvent thermal reaction temperature is 150~200 DEG C, and the time is 8~15h.
2. the preparation method of the tungsten oxide electrochomeric films according to claim 1 with EO-1 hyperion adjustable range,
It is characterized in that, in step (1), the organic solvent is selected from least one of methanol, ethyl alcohol, isopropanol.
3. the preparation method of the tungsten oxide electrochomeric films according to claim 1 with EO-1 hyperion adjustable range,
It is characterized in that, in step (1), the concentration of tungsten hexachloride is 1~10g/L in the precursor solution.
4. the preparation method of the tungsten oxide electrochomeric films according to claim 1 with EO-1 hyperion adjustable range,
It is characterized in that, in step (2), the transparent conduction base sheet is selected from FTO transparent conduction base sheet or transparent conductive substrate.
5. the preparation method of the tungsten oxide electrochomeric films according to claim 1 with EO-1 hyperion adjustable range,
It is characterized in that, the tungsten oxide electrochomeric films also need to be heat-treated；
The heat treatment temperature is 150~200 DEG C, and the time is 0.5~1h.
6. the oxygen with EO-1 hyperion adjustable range of method preparation described in a kind of any claim according to claim 1~5
Change tungsten electrochomeric films, which is characterized in that the spectrum adjustable range of the tungsten oxide electrochomeric films is 0~80%.
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| CN109180017A (en) * | 2018-08-27 | 2019-01-11 | 华南理工大学 | A kind of solwution method low temperature preparation WO3The method of electrochomeric films |
| CN110967887B (en) * | 2018-09-30 | 2022-09-16 | 马亮 | Electrochromic film and preparation method thereof |
| CN109240014A (en) * | 2018-10-23 | 2019-01-18 | 南京邮电大学 | A kind of flexible electrochromic film and its preparation method and application based on tungsten oxide |
| FR3089969B1 (en) * | 2018-12-13 | 2023-02-24 | Genesink | Synthesis method of tungsten oxide nanoparticles |
| CN109455946B (en) * | 2019-01-04 | 2020-06-19 | 西安交通大学 | W with electrochromic property18O49/WO3Composite film and preparation method thereof |
| CN115745420B (en) * | 2022-11-28 | 2024-03-22 | 上海第二工业大学 | Preparation method of broadband optical modulation tungsten oxide electrochromic film, product and application thereof |
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| CN102352109B (en) * | 2011-07-05 | 2012-11-21 | 浙江大学 | Organic-inorganic composite electrochromic film and preparation method thereof |
| CN103818964A (en) * | 2014-02-27 | 2014-05-28 | 盐城工学院 | Preparation method for W18O49 ultrafine nanowire |
| CN105036196A (en) * | 2015-08-27 | 2015-11-11 | 陕西科技大学 | Preparation method of multi-dimensional pure-phase W18O49 |
| CN105271420B (en) * | 2015-10-27 | 2017-03-22 | 陕西科技大学 | Method for preparing nanoscale granular W18O49 material |
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