CN108363256A - A kind of electrochromic device and preparation method thereof - Google Patents
A kind of electrochromic device and preparation method thereof Download PDFInfo
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- CN108363256A CN108363256A CN201810384944.1A CN201810384944A CN108363256A CN 108363256 A CN108363256 A CN 108363256A CN 201810384944 A CN201810384944 A CN 201810384944A CN 108363256 A CN108363256 A CN 108363256A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/155—Electrodes
Abstract
The invention discloses a kind of electrochromic devices and preparation method thereof, and wherein the preparation method includes：Tungsten oxide film precursor liquid is prepared using sol-gal process, tungsten oxide film precursor liquid is deposited on the first layer at transparent layer, and anneal, to obtain tungsten oxide electrochromic layer；Electrolyte is prepared using sol-gal process, by electrolyte deposition on tungsten oxide electrochromic layer surface, to obtain electrolyte layer；Electrolyte layer and the second transparency conducting layer are bonded, and is dried and is cured, to obtain electrochromic device.Above-mentioned technical proposal disclosed in the present application, prepare tungsten oxide film precursor liquid and electrolyte respectively using sol-gal process, and it is deposited onto in corresponding film layer, to prepare electrochromic device, prepare that the equipment needed for electrochromic device is simple, easy to operate using the above method, and the technical process for preparing corresponding solution is fairly simple, therefore, the preparation process that electrochromic device can be simplified reduces its manufacturing cost.
Description
Technical field
The present invention relates to technical field of electronic devices, more specifically to a kind of electrochromic device and its preparation side
Method.
Background technology
Electrochromism refers to the optical properties (reflectivity, transmitance, absorptivity etc.) of material under the action of extra electric field
Color change there is a phenomenon where stablizing, reversible shows as the reversible change of color and transparency in appearance.With electroluminescent change
The material of color performance is known as electrochromic material, is known as electrochromic device with the device that electrochromic material is made.
Electrochromic device can be widely applied in building, the vehicles, have light absorption saturating under electric field action
The controllability crossed optionally absorbs or reflects extraneous heat radiation and internal thermal diffusion, reduces office block and the people
It keeps nice and cool in summer with house and winter keeps mass energy that is warm and must consuming.Due to reaching the sun of earth surface
The light for having 53% or so in light is near infrared light, and this part of light has the function of regulating and controlling temperature, therefore can pass through research
The electrochromic device of transmitance with regulation and control near infrared light reaches energy-efficient purpose.
Using tungsten oxide as the electrochromic device of electrochromic layer after coloring near infrared light have higher reflectivity,
Color is more soft and relatively good every optical property, can reach the heat insulation and preservation effect similar with low emissivity glass, helps to reduce
Indoor energy consumption.Currently, often passing through magnetron sputtering method, CVD (Chemical Vapor Deposition, chemical vapour deposition technique)
Prepare the tungsten oxide electrochromic layer and electrolyte layer in electrochromic device.But the technics comparing of both preparation methods
It is cumbersome, equipment price is more expensive.
In conclusion how to simplify the preparation process of electrochromic device, the manufacturing cost of reduction electrochromic device is
Those skilled in the art's technical problem urgently to be resolved hurrily.
Invention content
In view of this, the object of the present invention is to provide a kind of electrochromic device and preparation method thereof, with the electroluminescent change of simplification
The preparation process of color device, the manufacturing cost for reducing electrochromic device.
To achieve the goals above, the present invention provides the following technical solutions：
A kind of electrochromic device preparation method, including：
Tungsten oxide film precursor liquid is prepared using sol-gal process, the tungsten oxide film precursor liquid is deposited on first thoroughly
Bright conductive layer surface, and anneal, to obtain tungsten oxide electrochromic layer；
Electrolyte is prepared using sol-gal process, by the electrolyte deposition on the tungsten oxide electrochromic layer surface,
To obtain electrolyte layer；
The electrolyte layer and the second transparency conducting layer are bonded, and is dried and is cured, to obtain electroluminescent change
Color device.
Preferably, annealing temperature is 250 DEG C, annealing time 2h.
Preferably, the tungsten oxide film precursor liquid is deposited on the first layer at transparent layer, including：
The tungsten oxide film precursor liquid is spin-coated to first layer at transparent layer using spin-coating method.
Preferably, the tungsten oxide film precursor liquid is being spin-coated to first layer at transparent layer using spin-coating method
When, drop glue rate is 1200r/min, and the drop glue time is 10s, and spin coating rate is 3500r/min, spin coating time 25s.
Preferably, the tungsten oxide film precursor liquid is being spin-coated to first layer at transparent layer using spin-coating method
When, spin coating number is 5 times.
A kind of electrochromic device, the electrochromic device are to utilize electrochromic device system described in any one of the above embodiments
What Preparation Method was prepared into, the electrochromic device includes successively：First transparency conducting layer, tungsten oxide electrochromic layer, electrolysis
Matter layer, the second transparency conducting layer.
Preferably, the tungsten oxide electrochromic layer is amorphous state tungsten oxide film.
Preferably, the thickness of the amorphous state tungsten oxide film is 71nm.
Preferably, first transparency conducting layer, second transparency conducting layer are ITO electro-conductive glass.
Preferably, first transparency conducting layer, second transparency conducting layer are FTO electro-conductive glass.
The present invention provides a kind of electrochromic devices and preparation method thereof, and wherein the preparation method includes：Utilize colloidal sol
Gel method prepares tungsten oxide film precursor liquid, tungsten oxide film precursor liquid is deposited on the first layer at transparent layer, and carry out
Annealing, to obtain tungsten oxide electrochromic layer；Electrolyte is prepared using sol-gal process, electrolyte deposition is electroluminescent in tungsten oxide
Change colour layer surface, to obtain electrolyte layer；Electrolyte layer and the second transparency conducting layer are bonded, and is dried and is consolidated
Change, to obtain electrochromic device.It is thin to prepare tungsten oxide using sol-gal process respectively for above-mentioned technical proposal disclosed in the present application
Membrane precursor liquid and electrolyte, and be deposited onto in corresponding film layer, to prepare electrochromic device, prepared using the above method
Equipment needed for electrochromic device is simple, easy to operate, and the technical process for preparing corresponding solution is fairly simple, therefore, can
To simplify the preparation process of electrochromic device, its manufacturing cost is reduced.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is a kind of flow chart of electrochromic device preparation method provided in an embodiment of the present invention；
Fig. 2 is a kind of structural schematic diagram of electrochromic device provided in an embodiment of the present invention；
Fig. 3 is electrochromic device provided in an embodiment of the present invention in visible-near-infrared area's coloured state and colour fading state
Transmittance curve figure；
Fig. 4 be it is provided in an embodiment of the present invention with 100 obtained electrochromic devices of driving voltage scan round
The current peak distribution map of color state and colour fading state；
Fig. 5 is the change of the electric current provided in an embodiment of the present invention obtained with driving voltage scanning electrochromic device at any time
Change curve graph.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Fig. 1 is referred to, it illustrates a kind of flow chart of electrochromic device preparation method provided in an embodiment of the present invention,
May include：
S11：Tungsten oxide film precursor liquid is prepared using sol-gal process, tungsten oxide film precursor liquid is deposited on first thoroughly
Bright conductive layer surface, and anneal, to obtain tungsten oxide electrochromic layer.
The principle of sol-gal process is that will contain the compound of high chemical active ingredient as presoma, by these under liquid phase
Raw material uniformly mixes, and is hydrolyzed, is condensed chemical reaction, forms stable vitreosol system in the solution, colloidal sol is through old
Change, slowly polymerize between micelle, form the gel of three-dimensional space grid structure, be filled between gel network lose flowability it is molten
Agent forms gel.
The detailed process of tungsten oxide film precursor liquid is prepared using sol-gal process to be：Precompute required gold
The desired amount of metal tungsten powder is added in hydrogen peroxide the amount for belonging to tungsten powder and hydrogen peroxide.After waiting for that the reaction was complete, it is slowly added to ice
Acetic acid and absolute ethyl alcohol, to form tungsten peroxy acid.2h is stirred at room temperature in mixed solution after hybrid reaction, then in room temperature
Lower standing 70h by its filtered several times, generally 3 times, finally obtains faint yellow colloidal sol later, namely before obtaining tungsten oxide film
Drive liquid.Preparing tungsten oxide film precursor liquid using sol-gal process need not utilize complicated, expensive equipment can be realized, and
The technical process that tungsten oxide film precursor liquid is prepared using this method is fairly simple.
It should be noted that when configuring solution, the concentration of solution can be controlled by controlling the amount of each component
System.
It, can be by its uniform deposition in the first layer at transparent layer after having prepared tungsten oxide film precursor liquid.It is heavy
After product, the first transparency conducting layer can be placed in drying box and be dried, wherein drying temperature can generally be set as 60
DEG C, drying time can generally be set as 30min, finally obtain tungsten oxide electrochromic layer, and technical process is fairly simple, and
It need not be can be realized by expensive equipment.
It should be noted that before tungsten oxide film precursor liquid is deposited on the first transparency conducting layer, need to first
Transparency conducting layer is cleaned and is dried, and cleaning and drying process are specifically as follows：Distinguished using ethyl alcohol, acetone, distilled water
It is cleaned by ultrasonic the first transparency conducting layer, and utilizes N2It is dried up, to obtain the first dry transparency conducting layer of cleaning, to subtract
Less to the influence caused by electrochromic device performance.
S12：Electrolyte is prepared using sol-gal process, by electrolyte deposition on tungsten oxide electrochromic layer surface, to obtain
To electrolyte layer.
Equally, electrolyte can also be prepared using sol-gal process, by polymer, lithium salts or ionic liquid and plasticizer
Deng at being grouped as.Specifically, can be lithium salts using tetraethyl orthosilicate as polymer, lithium acetate, ethyl alcohol is plasticizer, pass through control
The ratio of reaction temperature and each component, to form the high polymer mixed electrolyte for being easy to charge transmission.Its preparation process specifically may be used
Think：CA (Citric Acid, citric acid) is added in absolute ethyl alcohol, is stirred at room temperature to dissolving.Then, silicon is added
Sour tetra-ethyl ester, lithium acetate so that the molar ratio of Si and CA is 1:2, ethylene glycol is added, 60 DEG C of stirring 1h is warming up to, obtains institute
The mixed polymer needed.
By the electrolyte uniform deposition of gained on tungsten oxide electrochromic layer surface, to obtain electrolyte layer.Wherein, it is electrolysed
Matter layer is ion conducting layer, typically refers to polymer dielectric, and most representative polymer electrolyte matrix material has poly-
Ether system, polyacrylonitrile, Kynoar system, polymethacrylates system etc., wherein polyether system is mainly PEO (Plasma
Electrolytic Oxidation, polyethylene glycol oxide).
S13：Electrolyte layer and the second transparency conducting layer are bonded, and is dried and is cured, to obtain electroluminescent change
Color device.
By the electrolyte layer of gained and through cleaning-drying the second transparency conducting layer bond, then carry out drying and
Solidification, to prepare electrochromic device, wherein drying temperature is generally 60 DEG C, and hardening time is generally for 24 hours.
It should be noted that the mode being cleaned and dried to the second transparency conducting layer is carried out with to the first transparency conducting layer
The mode of cleaning-drying is identical, and details are not described herein.
Above-mentioned technical proposal disclosed in the present application prepares tungsten oxide film precursor liquid and electrolysis using sol-gal process respectively
Matter, and be deposited onto in corresponding film layer, to prepare electrochromic device, electrochromic device institute is prepared using the above method
The equipment needed is simple, easy to operate, and the technical process for preparing corresponding solution is fairly simple, therefore, can simplify electrochromism
The preparation process of device reduces its manufacturing cost.
A kind of electrochromic device preparation method provided in an embodiment of the present invention, annealing temperature can be 250 DEG C, when annealing
Between can be 2h.
When tungsten oxide film precursor liquid is deposited on the first transparency conducting layer, and is annealed to it, control can be passed through
It makes the temperature of annealing and the crystalline state of tungsten oxide film is controlled.By experiment it is found that when annealing temperature is 250 DEG C, annealing
When time is 2h, what is obtained is amorphous state tungsten oxide film.Amorphous state tungsten oxide in corresponding electrochromic device is colouring
The reaction time of state and colour fading state is shorter, and electrochromism efficiency is relatively high, and the design parameter of electrochromic device can
With referring to obtained occurrence when subsequently testing electrochromic device.
Tungsten oxide film precursor liquid is deposited on by a kind of electrochromic device preparation method provided in an embodiment of the present invention
One layer at transparent layer may include：
Tungsten oxide film precursor liquid is spin-coated to the first layer at transparent layer using spin-coating method.
It can utilize spin-coating method that prepared tungsten oxide film precursor liquid is spin-coated to the surface of the first transparency conducting layer,
Spin-coating method, which is used in the preparation of electrochromic device, can prepare the bigger electrochromic layer of density, and acquired
Electrochromic layer film thickness it is relatively uniform, be conducive to improve electrochromic device performance.
It is of course also possible to which prepared tungsten oxide film precursor liquid is deposited on first by the methods of impregnating, spraying
Layer at transparent layer, these specific deposition methods within protection scope of the present invention, and can by spin-coating method,
Infusion process, spray coating method etc. by electrolyte deposition on the surface of electrochromic layer, to obtain electrolyte layer.
A kind of electrochromic device preparation method provided in an embodiment of the present invention, before using spin-coating method by tungsten oxide film
When drive liquid is spin-coated to the first layer at transparent layer, drop glue rate can be 1200r/min, and the drop glue time can be 10s, spin coating
Rate can be 3500r/min, and spin coating time can be 25s.
When tungsten oxide film precursor liquid is spin-coated to the first layer at transparent layer using spin-coating method, the rate of glue is dripped
Can be 1200r/min, the drop glue time can be 10s, in order to preferably transparent lead tungsten oxide film precursor liquid first
The surface of electric layer is even to open.After dropping in tungsten oxide film precursor liquid on the first transparency conducting layer, in order to preferably will be extra
Solution throw away, to obtain the more uniform tungsten oxide film of Film Thickness Ratio, then the rate of its spin coating can be 3500r/min, spin coating
Time can be 25s.
A kind of electrochromic device preparation method provided in an embodiment of the present invention, before using spin-coating method by tungsten oxide film
When drive liquid is spin-coated to the first layer at transparent layer, spin coating number is 5 times.
When preparing tungsten oxide film under the above parameters, when spin coating number is 5 times namely electrochromic layer is non-by 5 layers
When crystalline state tungsten oxide film is constituted, the thickness of corresponding amorphous state tungsten oxide film is proper, corresponding electrochromism device
The performance of part is better than the performance of the obtained electrochromic device under other spin coating numbers, and performance parameter can equally join
It sees below to continue and it is carried out to test obtained occurrence.
The embodiment of the present invention additionally provides a kind of electrochromic device, which is to utilize any of the above-described electricity
Mutagens color device preparation method is prepared into, and refers to Fig. 2, and it illustrates a kind of electrochromism devices provided in an embodiment of the present invention
The structural schematic diagram of part, electrochromic device may include successively：First transparency conducting layer 1, tungsten oxide electrochromic layer 2, electricity
Solve matter layer 3, the second transparency conducting layer 4.
A kind of electrochromic device provided in an embodiment of the present invention, tungsten oxide electrochromic layer 2 are that amorphous state tungsten oxide is thin
Film.
When annealing temperature is 250 DEG C, and annealing time is 2h, obtained tungsten oxide electrochromic layer 2 is amorphous state oxygen
Change W film, when being used in electrochromic device, regulation and control energy of the obtained electrochromic device in near-infrared region
Power is relatively good, so as to greatly reduce indoor energy consumption, to reach energy-efficient purpose.
The thickness of a kind of electrochromic device provided in an embodiment of the present invention, amorphous state tungsten oxide film is 71nm.
When utilizing the spin coating parameters spin coating tungsten oxide film precursor liquid in above-mentioned electrochromic device preparation method, every time
The thickness of obtained amorphous state tungsten oxide film is certain.When spin coating number is 5 times, obtained amorphous state tungsten oxide
The thickness of film is 71nm, corresponding tungsten oxide coloured state and colour fading state reaction time is shorter, electrochromism efficiency ratio
It is higher, stability is relatively good.
A kind of electrochromic device provided in an embodiment of the present invention, the first transparency conducting layer 1, the second transparency conducting layer 4 are
It can be ITO electro-conductive glass.
It can utilize that transmitance is high, conductive capability is strong, high-transmission rate ITO electro-conductive glass (i.e. lead by the indium oxide of doped tin
Electric glass) the first transparency conducting layer 1 and the second transparency conducting layer 4 as electrochromic device.
A kind of electrochromic device provided in an embodiment of the present invention, the first transparency conducting layer 1, the second transparency conducting layer 4 are
It can be FTO electro-conductive glass.
In addition to using ITO electro-conductive glass as the first transparency conducting layer 1 of electrochromic device and the second transparency conducting layer 4
Except, it can also utilize that resistivity is low, stable chemical performance, the stronger FTO electro-conductive glass of antiacid alkali ability is (i.e. at room temperature
Adulterate the fin oxide condutire glass of fluorine) the first transparency conducting layer 1 and the second transparency conducting layer 4 as electrochromic device.
It is of course also possible to use first electrically conducting transparent as electrochromic device such as zinc oxide electro-conductive glass of adulterated al
Layer 1 and the second transparency conducting layer 4.
In a kind of electrochromic device provided in an embodiment of the present invention relevant portion illustrate be referred to it is above-mentioned right
The detailed description of corresponding part in a kind of electrochromic device preparation method that the embodiment of the present invention is provided, it is no longer superfluous herein
It states.
In order to be 250 DEG C to above-mentioned annealing temperature namely electrochromic layer is amorphous state tungsten oxide film, and amorphous state oxygen
The performance of corresponding electrochromic device illustrates when the number of plies for changing W film is 5 layers, then can be joined with 2400 semiconductors
Number analyzers and ultraviolet-visible spectrophotometer assembling system testing electrochromic device different driving voltages effect under
The performances such as visible region and coloring/fading time of near-infrared region, transmitance, electrochromism efficiency, specifically may refer to Fig. 3
To Fig. 5.
Fig. 3 is electrochromic device provided in an embodiment of the present invention in visible-near-infrared area's coloured state and colour fading state
Transmittance curve figure, wherein the wavelength (Wavelength) that abscissa represents, what ordinate represented is transmitance
(Transmittance), that Δ T is represented is coloured state (Colored state) and colour fading state (Bleached under current wavelength
State the transmitance difference between).As seen from the figure, when wavelength is at 900nm, the corresponding transmitance of coloured state is 62.2%,
Coloration time is 15.8s, and the corresponding transmitance of colour fading state is 83%, fading time 2.5s, amorphous in the electrochromic device
The fading time of state tungsten oxide film is (more normal than the fading time of the amorphous state tungsten oxide film in existing electrochromic device
For 20s) reaction time of electrochromic device corresponding to the short namely present invention is than very fast.
The calculation formula of CE (Coloration Efficiency, electrochromism efficiency)：
CE=Δ OD/ Δs Q
Δ OD=log (Tb/Tc)
Wherein, TbFor the corresponding transmitance of colour fading state, TcFor the corresponding transmitance of coloured state, Δ OD indicates electrochromism device
The variation of part optical density under coloured state, colour fading state, Δ Q indicate the charge of unit area injection/extraction during coloring/colour fading
Amount.Measure Δ OD, and by Δ OD, TbAnd TcAbove-mentioned formula is substituted into, obtaining corresponding CE under 900nm wavelength is
78.8cm2/ C, and the CE that the electrochromic device prepared by existing amorphous state tungsten oxide film is corresponding under 900nm wavelength
For 40-50cm2/ C, namely it is relatively high using the electrochromism efficiency of the electrochromic device prepared by method of the invention.
Fig. 4 be it is provided in an embodiment of the present invention with 100 obtained electrochromic devices of driving voltage scan round
The current peak distribution map of color state and colour fading state, wherein abscissa is the time (Time), and ordinate is electric current (Current).Profit
It is+2.5V, -2.5V with scan amplitude, sweep time is the driving pulse scan round 100 times (100cycles) of 30s, wherein
+ 2.5V corresponds to colour fading voltage, and -2.5V corresponds to coloration voltage.When scanning, the first transparency conducting layer, the second transparency conducting layer difference
As anode, cathode, namely only it is tested by opposite polarity driving voltage, can not only reduce peripheral circuit
Complexity, the power consumption of electrochromic device can also be reduced.As can be seen from the figure electrochromic device is continuously recycling
When scanning 100 times, the transition process between coloured state, colour fading state, and the electric current of coloured state and colour fading state are shown every time
Peak value is sufficiently stable, this illustrate the electrochromic device with this condition cycle operation when, electrochromic property is more steady
It is fixed, and there are good fatigue-resistance characteristics.
Fig. 5 is the change of the electric current provided in an embodiment of the present invention obtained with driving voltage scanning electrochromic device at any time
Change curve graph.By in figure when voltage is -2.5V, preceding ten periods of the coloring process (Coloring) in measurement process and
Current value situation of change corresponding to ten periods afterwards, and when voltage is 2.5V, colour fading process (Bleaching) is measuring
The current value situation of change corresponding to preceding ten periods and rear ten periods in the process is it is found that electroluminescent change when recycling 100 times
Color device is consistent with the quantity of electric charge extracted in coloring and injection in the process of fading, and has good reversible denaturation, stability ratio
Preferably.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the element that the process, method, article or equipment including a series of elements is intrinsic.
In the case of more limiting, the element that is limited by sentence " including one ... ", it is not excluded that including the element
Process, method, article or equipment in there is also other identical elements.In addition, above-mentioned skill provided in an embodiment of the present invention
The part consistent with technical solution realization principle is corresponded in the prior art and unspecified in art scheme, in order to avoid excessively repeat.
The foregoing description of the disclosed embodiments enables those skilled in the art to realize or use the present invention.To this
A variety of modifications of a little embodiments will be apparent for a person skilled in the art, and the general principles defined herein can
Without departing from the spirit or scope of the present invention, to realize in other embodiments.Therefore, the present invention will not be limited
It is formed on the embodiments shown herein, and is to fit to consistent with the principles and novel features disclosed in this article widest
Range.
Claims (10)
1. a kind of electrochromic device preparation method, which is characterized in that including：
Tungsten oxide film precursor liquid is prepared using sol-gal process, the tungsten oxide film precursor liquid, which is deposited on first, transparent leads
Electric layer surface, and anneal, to obtain tungsten oxide electrochromic layer；
Electrolyte is prepared using sol-gal process, by the electrolyte deposition on the tungsten oxide electrochromic layer surface, to obtain
To electrolyte layer；
The electrolyte layer and the second transparency conducting layer are bonded, and is dried and is cured, to obtain electrochromism device
Part.
2. electrochromic device preparation method according to claim 1, which is characterized in that annealing temperature is 250 DEG C, annealing
Time is 2h.
3. electrochromic device preparation method according to claim 2, which is characterized in that by the tungsten oxide film forerunner
Liquid is deposited on the first layer at transparent layer, including：
The tungsten oxide film precursor liquid is spin-coated to first layer at transparent layer using spin-coating method.
4. electrochromic device preparation method according to claim 3, which is characterized in that using spin-coating method by the oxygen
Change W film precursor liquid when being spin-coated to first layer at transparent layer, drop glue rate is 1200r/min, drips the glue time and is
10s, spin coating rate are 3500r/min, spin coating time 25s.
5. electrochromic device preparation method according to claim 4, which is characterized in that using spin-coating method by the oxygen
When change W film precursor liquid is spin-coated to first layer at transparent layer, spin coating number is 5 times.
6. a kind of electrochromic device, which is characterized in that the electrochromic device is using such as any one of claim 1-5 institute
What the electrochromic device preparation method stated was prepared into, the electrochromic device includes successively：First transparency conducting layer, oxidation
Tungsten electrochromic layer, electrolyte layer, the second transparency conducting layer.
7. electrochromic device according to claim 6, which is characterized in that the tungsten oxide electrochromic layer is amorphous state
Tungsten oxide film.
8. electrochromic device according to claim 7, which is characterized in that the thickness of the amorphous state tungsten oxide film is
71nm。
9. electrochromic device according to claim 6, which is characterized in that first transparency conducting layer, described second
Transparency conducting layer is ITO electro-conductive glass.
10. electrochromic device according to claim 6, which is characterized in that first transparency conducting layer, described second
Transparency conducting layer is FTO electro-conductive glass.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109581776A (en) * | 2019-01-02 | 2019-04-05 | 华南理工大学 | A kind of low cost electrochromic device and preparation method thereof |
| CN110204217A (en) * | 2019-04-11 | 2019-09-06 | 广东工业大学 | A kind of electrochromic device and preparation method thereof |
| CN110357454A (en) * | 2019-06-25 | 2019-10-22 | 嘉兴快闪新材料有限公司 | Reduce the drying means to fade before electrochomeric films annealing |
| CN111240119A (en) * | 2020-03-03 | 2020-06-05 | 中国科学院长春光学精密机械与物理研究所 | Electrochromic non-metal salt electrolyte composite material, preparation method and application |
| CN112327555A (en) * | 2020-11-20 | 2021-02-05 | 浙江工业大学 | Electrochromic device, preparation method thereof and application of electrochromic device in intelligent window |
| CN113204146A (en) * | 2021-05-07 | 2021-08-03 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device taking water vapor as electrolyte and preparation method thereof |
| WO2022237066A1 (en) * | 2021-05-08 | 2022-11-17 | 华南理工大学 | Microcavity injection type electrochromic device, and manufacturing method therefor and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1710481A (en) * | 2005-06-17 | 2005-12-21 | 同济大学 | Fully-solid-state electrochromic device and making method therefor |
| CN1928685A (en) * | 2006-09-28 | 2007-03-14 | 同济大学 | Method for preparing full solid electrochromic device with sol-gel |
| CN101510038A (en) * | 2009-03-16 | 2009-08-19 | 浙江大学 | Method for producing full-solid electrochromic device |
| CN101576695A (en) * | 2009-04-28 | 2009-11-11 | 电子科技大学 | WO3 electrochromic thin film preparation method |
| CN106932992A (en) * | 2017-03-31 | 2017-07-07 | 中国航发北京航空材料研究院 | The flexible electro-chromic device and preparation method of a kind of regulation and control near infrared light |
-
2018
- 2018-04-26 CN CN201810384944.1A patent/CN108363256B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1710481A (en) * | 2005-06-17 | 2005-12-21 | 同济大学 | Fully-solid-state electrochromic device and making method therefor |
| CN1928685A (en) * | 2006-09-28 | 2007-03-14 | 同济大学 | Method for preparing full solid electrochromic device with sol-gel |
| CN101510038A (en) * | 2009-03-16 | 2009-08-19 | 浙江大学 | Method for producing full-solid electrochromic device |
| CN101576695A (en) * | 2009-04-28 | 2009-11-11 | 电子科技大学 | WO3 electrochromic thin film preparation method |
| CN106932992A (en) * | 2017-03-31 | 2017-07-07 | 中国航发北京航空材料研究院 | The flexible electro-chromic device and preparation method of a kind of regulation and control near infrared light |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109581776A (en) * | 2019-01-02 | 2019-04-05 | 华南理工大学 | A kind of low cost electrochromic device and preparation method thereof |
| CN109581776B (en) * | 2019-01-02 | 2020-06-19 | 华南理工大学 | Low-cost electrochromic device and preparation method thereof |
| WO2020140558A1 (en) * | 2019-01-02 | 2020-07-09 | 华南理工大学 | Low-cost electrochromic device and preparation method therefor |
| CN110204217A (en) * | 2019-04-11 | 2019-09-06 | 广东工业大学 | A kind of electrochromic device and preparation method thereof |
| CN110357454A (en) * | 2019-06-25 | 2019-10-22 | 嘉兴快闪新材料有限公司 | Reduce the drying means to fade before electrochomeric films annealing |
| CN110357454B (en) * | 2019-06-25 | 2022-01-21 | 嘉兴快闪新材料有限公司 | Drying method for reducing color fading of electrochromic film before annealing |
| CN111240119A (en) * | 2020-03-03 | 2020-06-05 | 中国科学院长春光学精密机械与物理研究所 | Electrochromic non-metal salt electrolyte composite material, preparation method and application |
| CN112327555A (en) * | 2020-11-20 | 2021-02-05 | 浙江工业大学 | Electrochromic device, preparation method thereof and application of electrochromic device in intelligent window |
| CN113204146A (en) * | 2021-05-07 | 2021-08-03 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device taking water vapor as electrolyte and preparation method thereof |
| WO2022237066A1 (en) * | 2021-05-08 | 2022-11-17 | 华南理工大学 | Microcavity injection type electrochromic device, and manufacturing method therefor and application thereof |
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