CN106681078A - Large-area, uniform and fast-responding WO3 electrochromic device and preparation method thereof - Google Patents
Large-area, uniform and fast-responding WO3 electrochromic device and preparation method thereof Download PDFInfo
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- CN106681078A CN106681078A CN201611193888.0A CN201611193888A CN106681078A CN 106681078 A CN106681078 A CN 106681078A CN 201611193888 A CN201611193888 A CN 201611193888A CN 106681078 A CN106681078 A CN 106681078A
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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
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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
- G02F1/1506—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
-
- 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
- G02F1/1506—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
- G02F1/1508—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode using a solid electrolyte
-
- 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
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention provides a large-area, uniform and fast-responding WO3 electrochromic device and a preparation method thereof and belongs to the field of technological application of function materials. Tungsten powder reacts with hydrogen peroxide, then absolute ethyl alcohol is added, pH is regulated to 2-3 by using acetic acid, and a precursor solution is obtained; a plate graphite electrode is selected as a counter electrode, ITO plate conductive glass is selected as a working electrode, Ag/KC1 is selected as a reference electrode, the working electrode and the counter electrode are parallelly and oppositely placed, electro-deposition is performed by adopting a constant current deposition mode, and a WO3 electrochromic film is obtained on the surface of the ITO plate conductive glass; a certain amount of LiClO4 is added in a propylene carbonate solvent, and stirring is performed for dissolution; then, polymethyl methacrylate powder is added, and the state of electrolyte is adjusted to be close to a solid state; the WO3 electrochromic film and blank ITO glass are bonded through solid electrolyte, and then forming processing is performed; the edge is sealed to obtain the device. The method is simple.
Description
Technical field
The present invention relates to large area WO3Electrochromic device and preparation method thereof, belongs to functional material technical applications.
Background technology
With developing rapidly for industry, energy shortage and environmental pollution have become the key that human society is badly in need of solving and have asked
Topic.Mass energy is applied to the temperature adjustment of building for developed country, and wherein air conditioning energy consumption accounts for first place.Therefore, take various
Measure reducing energy consumption is increasingly becoming the common recognition of people, for example, the smart window of solar spectrum is adjusted with energy-conservation and comfort requirement,
Have broad application prospects in future architecture thing, receive the extensive concern of people.Many materials are being heated, illumination, outer power-up
During the external influences such as field, its color can change, that is, produce coloring phenomenon.Off-color material is caused to refer in extraneous conditioning
Under, can continuous reversible regulation solar electromagnetic radiation material, mutagens color can be divided into photochromic, thermochromism, electrochromism,
Gas-discoloration and Photoelectrochromic etc., wherein electrochromic material are one of focuses of Recent study.
Electrochromism refers to that material color under electric field action is produced and stablizes reversible change phenomenon.When material is in electrochemistry
When the injection of the lower generation electronics of effect and ion is with extracting out, its valence state and chemical constituent will change, so that material is anti-
Penetrate and transmission performance changes, the reversible change of color and transparency is shown as on appearance property.Electric charge in electrochromic material
Injection can be conveniently realized by the change of external voltage or electric current with extracting out, inject or extract electric charge number it is direct
The coloring degree of material is determined, adjusting external voltage or electric current can control the electrochromism degree of electrochromic material；It is logical
Crossing the polarity of change voltage can conveniently realize coloring or colour killing；There is no oxidation also in cut-out electric current in colored material
In the case of original reaction, color state is can hold, i.e., with memory function.The excellent properties of electrochomeric films and section
Application prospect in terms of energy is subject to the common concern of people, meets the development trend of following intellectual material.、
WO3Electrochromic material is currently mainly studied majority and is concentrated on as the research direction of presently most focus to it
The improvement of the aspect of performances such as the optical modulation amplitude of single thin film, response time and electrochromism efficiency.For electrochromism device
The large-area preparation and development of part is than relatively limited.It is current to prepare WO3The most ripe method of electrochromic device is that magnetic control splashes
Technology is penetrated, but the method preparation technology is more complicated, and it is relatively costly.Due to prepare thin film compactness it is larger, so that should
The coloring of thin film and colour fading response speed are longer, and required applied voltage is larger (being more than 2V), is unfavorable for cyclical stability.Secondly,
WO3Electrochromic device principal organ is five-layer structure, i.e. glass ITO/NiO/LiClO4+PC+PMMA/WO3/ ito glass.Its
In, electrolyte be in electrochromism WO3Between layer and ion storage NiO, for example same sandwich of whole device architecture.The knot
Structure determines that good electrochromic device needs electrochromism WO3The electrochromism that layer and ion storage NiO have had simultaneously
Performance.The influence factor of the structure is more, preparation technology is more complicated, corresponding preparation cost is higher.And the color of the device is
WO3The blueness of layer and the brown of ion storage NiO are overlapped so that color does not have single WO3Electrochromism is attractive in appearance, surely
The qualitative double influence for being also subject to two kinds of thin film.
The content of the invention
The main electrochemical deposition technique relatively low, simple to operate by cost of the invention, prepares large area, uniformity
It is good ,/fading rate is fast, optical modulation amplitude is big and simple structure, the electrochromism WO of beautiful appearance3Device.
To realize low cost, this purpose simple to operate, the present invention adopts following steps：
(1) by tungsten powder and hydrogen peroxide according to 3g：The ratio of 10ml is reacted, and is subsequently adding and the isopyknic nothing of hydrogen peroxide
Water-ethanol, then carry out pH value with acetic acid and adjust to 2-3, obtain electro-deposition WO3Precursor solution；
(2) from plate graphite electrode as to electrode, ITO flat boards electro-conductive glass is working electrode, selects Ag/KCl to make
For reference electrode, by working electrode with electrode is carried out parallel staggered relatively, the precursor solution using step (1) is used as electrolyte
Electro-deposition is carried out, electro-deposition is carried out using galvanostatic deposition pattern, in ITO conductive glass surfaces WO is obtained3Electrochomeric films；
It is preferred that being 0.5mA/cm in given electric current density2Electro-deposition 400s obtains WO under galvanostatic deposition pattern3Electrochromism
Thin film；
Bondability holding one further preferably in order to ensure each compactness for plating thin film, thickness and with thin film
Cause, it is of the invention with special electrochemical deposition technique：And working electrode and parallel with electrolyte upper surface to electrode, and graphite
To electrode above, pH value monitor in real time of the pH meter used in electrochemical deposition process to solution, while molten with the KOH for preparing
Liquid is adjusted with position titration, it is ensured that the electrolyte ph moment is all identical with initial state.Its structure is as shown in Figure 1.
(3) LiClO is prepared4Solid electrolyte：A certain amount of LiClO is added toward Allyl carbonate (PC) solvent4, stirring
Dissolving；Polymethyl methacrylate (PMMA) powder is subsequently adding, the close solid-state of state of the electrolyte is adjusted to.
It is preferred that：A certain amount of LiClO is added toward Allyl carbonate (PC) solvent4, stirring and dissolving is finally configured to 1-
2mol/L；Polymethyl methacrylate (PMMA) powder is subsequently adding, the close solid-state of state of the electrolyte is adjusted to；It is preferred that institute
The solid-state for obtaining has mobility at 50 DEG C,
(4) by the WO obtained by step (2)3The solid-state that electrochomeric films pass through step (3) configuration with the ito glass of blank
Electrolyte is bonded, formed sandwich sandwich, be then placed in vacuum environment heat (preferably 50 DEG C) keep one section when
Between carry out device formation process；
(5) edge of the finished article to preparing carries out encapsulation process, that is, obtain required area size as needed
The WO of regulation3Electrochromic device.
Present configuration is simple, the WO of stable performance3Electrochromic device, the present invention selects four-layer structure as device
Overall structure, does not use NiO as ion storage, is directly to carry out device assembling to electrode with ITO electrode.Structure such as Fig. 2
It is shown.
Description of the drawings
Fig. 1 prepares large area, uniform WO3Electrochomeric films installation drawing；
Fig. 2 is four layers of WO prepared by the present invention3Electrochromic device structural representation.
30 × 30cm in Fig. 3 embodiments 12WO3Electrochromic device response time table under the control voltage effect of ± 2V
Levy.
30 × 30cm in Fig. 4 embodiments 12WO3Visible ray modulated amplitude under the control voltage effect of electrochromic device ± 2V
Degree is characterized.
Specific embodiment
With reference to the accompanying drawings and detailed description, the substantive distinguishing features and remarkable advantage of the present invention are further elucidated, this
Invention is limited only to by no means stated embodiment, and the patent is made for there is other similar preparation technologies identical to instruct
With.
Embodiment 1
Prepare 30 × 30cm2WO3Electrochromic device
1) WO needed for electro-deposition is prepared3Precursor solution：At ambient temperature, 120g tungsten powders and 400mL hydrogen peroxide are weighed
Reacted, question response obtains yellow in 12 hours afterwards by white precipitate centrifugal filtration under 8000 revs/min of rotating speed
WO3Precursor solution.The solution for preparing is diluted with the dehydrated alcohol of 440mL and the acetic acid of 12mL and pH=2.5 values are adjusted
Section.
2). by potentiostat given electric current density be 0.5mA/cm2Electrodeposition time is under galvanostatic deposition pattern
400s, in ITO conductive glass surfaces electrochemical deposition WO is carried out3Electrochomeric films；Select 30 × 30cm2Graphite electrode make
It is to electrode.With 30 × 30cm2ITO electro-conductive glass be working electrode, working electrode is carried out into Parallel Symmetric row with to electrode
Row, spacing is 3cm.Ag/KCl is selected simultaneously as reference electrode.
3). the thin film of deposition is dried 5 hours in 80 DEG C of environment, is taken out preserve stand-by afterwards.
4). prepare solid electrolyte.The LiClO of 160g is added toward 1000ml Allyl carbonate PC solution4Dissolving, adds afterwards
Enter the PMMA powder of 600g so that the close solid-state of state of electrolyte, and there is certain fluid ability at a temperature of 50 DEG C.
5). deposition there is into WO3The ito glass of thin film is glued with the ito glass of blank by the solid electrolyte for configuring
Close, formed sandwich sandwich, after be placed in 50 DEG C of vacuum environment keep 12h carry out device formation process.
5). the edge of the finished device to preparing carries out encapsulation process, that is, obtain 30 × 30cm2Large area WO3Electricity
Mutagens color device.
Claims (6)
1. large area, uniformity, fast-response WO3The preparation method of electrochromic device, it is characterised in that comprise the following steps：
(1) by tungsten powder and hydrogen peroxide according to 3g：The ratio of 10ml is reacted, and is subsequently adding anhydrous second isopyknic with hydrogen peroxide
Alcohol, then carry out pH value with acetic acid and adjust to 2-3, obtain electro-deposition WO3Precursor solution；
(2) from plate graphite electrode as to electrode, ITO flat boards electro-conductive glass is working electrode, selects Ag/KCl as ginseng
Than electrode, by working electrode with electrode is carried out parallel staggered relatively, carried out as electrolyte using the precursor solution of step (1)
Electro-deposition, using galvanostatic deposition pattern electro-deposition is carried out, and in ITO conductive glass surfaces WO is obtained3Electrochomeric films；
(3) LiClO is prepared4Solid electrolyte：A certain amount of LiClO is added toward Allyl carbonate (PC) solvent4, stirring and dissolving；
Polymethyl methacrylate (PMMA) powder is subsequently adding, the close solid-state of state of the electrolyte is adjusted to.
(4) by the WO obtained by step (2)3The solid state electrolysis that electrochomeric films pass through step (3) configuration with the ito glass of blank
Matter is bonded, and forms sandwich sandwich, is then placed on heating in vacuum environment and is kept for a period of time carry out device formation
Process；
(5) edge of the finished article to preparing carries out encapsulation process, that is, obtain required area size and adjust as needed
WO3Electrochromic device.
2. according to the large area described in claim 1, uniformity, fast-response WO3The preparation method of electrochromic device, its feature
It is that step (2) is 0.5mA/cm in given electric current density2Electro-deposition 400s obtains WO under galvanostatic deposition pattern3Electrochromism
Thin film.
3. according to the large area described in claim 1, uniformity, fast-response WO3The preparation method of electrochromic device, its feature
Be, step (2) working electrode and parallel with electrolyte upper surface to electrode, and graphite to electrode above, in electrochemistry
PH value monitor in real time of the pH meter to solution used in deposition process, while being adjusted with position titration with the KOH solution for preparing, it is ensured that electricity
The solution liquid pH value moment is all identical with initial state.
4. according to the large area described in claim 1, uniformity, fast-response WO3The preparation method of electrochromic device, its feature
It is that step (3) adds a certain amount of LiClO toward Allyl carbonate (PC) solvent4, stirring and dissolving is finally configured to 1-
2mol/L；Polymethyl methacrylate (PMMA) powder is subsequently adding, the close solid-state of state of the electrolyte is adjusted to；Gained
Solid-state has mobility at 50 DEG C.
5. according to the large area described in claim 1, uniformity, fast-response WO3The preparation method of electrochromic device, its feature
It is that step (4) heating-up temperature is 50 DEG C.
6. the WO for preparing according to claim 1-5 any one method3Electrochromic device.
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| CN201611193888.0A CN106681078A (en) | 2016-12-21 | 2016-12-21 | Large-area, uniform and fast-responding WO3 electrochromic device and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311468A (en) * | 2017-07-13 | 2017-11-03 | 北京工业大学 | A kind of electrokinetic potential electrochemical deposition prepares WO3The method of electrochomeric films |
| CN107991819A (en) * | 2017-11-23 | 2018-05-04 | 北京工业大学 | One kind improves Prussian blue electrochomeric films in LiClO4The method of cyclical stability in/PC electrolyte |
| CN109809489A (en) * | 2019-03-22 | 2019-05-28 | 华南理工大学 | A kind of method of rapid synthesis high quality tungstic acid solution |
| CN109856882A (en) * | 2019-03-25 | 2019-06-07 | 华南理工大学 | A kind of electrochomeric glass and its packaging method |
| CN110426143A (en) * | 2019-07-11 | 2019-11-08 | 南京理工大学 | A kind of vibration visible sensor based on pressure photochromic effect |
| CN113264690A (en) * | 2021-05-27 | 2021-08-17 | 同济大学 | Porous tungsten oxide electrochromic film and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311468A (en) * | 2017-07-13 | 2017-11-03 | 北京工业大学 | A kind of electrokinetic potential electrochemical deposition prepares WO3The method of electrochomeric films |
| CN107991819A (en) * | 2017-11-23 | 2018-05-04 | 北京工业大学 | One kind improves Prussian blue electrochomeric films in LiClO4The method of cyclical stability in/PC electrolyte |
| CN109809489A (en) * | 2019-03-22 | 2019-05-28 | 华南理工大学 | A kind of method of rapid synthesis high quality tungstic acid solution |
| CN109856882A (en) * | 2019-03-25 | 2019-06-07 | 华南理工大学 | A kind of electrochomeric glass and its packaging method |
| CN110426143A (en) * | 2019-07-11 | 2019-11-08 | 南京理工大学 | A kind of vibration visible sensor based on pressure photochromic effect |
| CN113264690A (en) * | 2021-05-27 | 2021-08-17 | 同济大学 | Porous tungsten oxide electrochromic film and preparation method thereof |
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Application publication date: 20170517 |
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