CN104570534B - All solid state inorganic electrochromic device and preparation method thereof - Google Patents
All solid state inorganic electrochromic device and preparation method thereof Download PDFInfo
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- CN104570534B CN104570534B CN201310467114.2A CN201310467114A CN104570534B CN 104570534 B CN104570534 B CN 104570534B CN 201310467114 A CN201310467114 A CN 201310467114A CN 104570534 B CN104570534 B CN 104570534B
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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
- 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
Abstract
The invention provides a kind of all solid state inorganic electrochromic device and preparation method thereof, the all solid state inorganic electrochromic device includes transparency conducting layer, electrochromic layer and dielectric substrate, and the dielectric substrate is the transparent nanoparticles film of the silica of silica or phosphorus doping.The all solid state inorganic electrochromic device that the present invention is provided, it is made up of multilayer Solid inorganic composite membrane, with electrochromic device most typically, simplest structure, the stable target of extensive industrialization, all solid state, device performance can be realized, the field of intelligent window and Display Technique etc. is used directly for, is had a good application prospect.Utilize the electrochromic device being made up of all solid state inorganic substances compound membrane that the method for the present invention can obtain inexpensive, extensive industrialization, device performance is stablized, the manufacturing line of existing industrialization electrochromic device is used directly for, with important application value.
Description
Technical field
The present invention relates to electrochromism technical field, more particularly to a kind of all solid state inorganic electrochromic device and its system
Preparation Method.
Background technology
Electrochromic material refers to after making alive, its optical properties（Emissivity, percent of pass, absorptivity etc.）Can occur stabilization
The material of reversible change.The scope that electrochromic material includes is wider, is broadly divided into electrodeless electrochromic material and organic
Two kinds of electrochromic material.The device made with electrochromic material referred to as electrochromic device, electrochromic device has height
Effect, low consumption, it is pollution-free, intelligent the advantages of, be respectively provided with automobile rearview mirror, the windowpane of building, aircraft, steamer etc. wide
Application prospect.
Electrochromic device generally comprises transparency conducting layer, electrochromic layer and dielectric substrate, and by a transparent substrates
Support, or be placed between two transparent substrates.Dielectric substrate is the transmission channel of ion needed for electrochromic effect, is divided into solid-state
Electrolyte and liquid electrolyte.Liquid electrolyte mass-energy provides good electrochromism response and high ionic conductivity, but its is resistance to
Corrosivity and poor chemical stability and encapsulation difficulty.Solid electrolyte is generally organic polymer, and its heat endurance is poor, in reality
It is extremely restricted in, and is unfavorable for the large-scale production of electrochromic device.
The content of the invention
Based on above mentioned problem, the invention provides a kind of all solid state inorganic electrochromic device and preparation method thereof, solve
Liquid electrolyte corrosion-resistant, poor chemical stability, encapsulation is difficult and polymer dielectric heat endurance is poor, be unfavorable for advising
The problem of modelling is produced.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of all solid state inorganic electrochromic device, including transparency conducting layer, electrochromic layer and dielectric substrate, it is described
Dielectric substrate is the transparent nanoparticles film of the silica of silica or phosphorus doping.
In one of the embodiments, transmitance >=80% of the transparency conducting layer in visible-range, thickness is
50nm~5 μm.
In one of the embodiments, transmitance >=80% of the electrochromic layer in visible-range, thickness is
50nm~2 μm.
In one of the embodiments, the grain of the transparent nanoparticles film of the silica of the silica or phosphorus doping
Spend for 1nm~20nm.
In one of the embodiments, the transparent nanoparticles film of the silica of the silica or phosphorus doping is can
Transmitance >=80% seen in optical range, thickness is 100nm~10 μm.
A kind of preparation method of described all solid state inorganic electrochromic device, comprises the following steps：
1. chooses the transparent substrates of certain area and cleaned up；
2. deposits the first transparency conducting layer using coating process on the transparent substrates surface；
3. is by one jiao of covering of first transparency conducting layer, as electrode contact area, and using coating process described
The surface of the non-cover part of first transparency conducting layer deposits the first electrochromic layer；
4. plasma enhanced chemical vapor deposition methods the first electrochromism layer surface deposit silica or
The transparent nanoparticles film of the silica of phosphorus doping, is used as dielectric substrate；
5. deposits the second transparency conducting layer using coating process on the transparent nanoparticles film surface, obtains individual layer electricity
Mutagens color device；The second electrochromic layer is first either deposited on the transparent nanoparticles film surface using coating process, so
Afterwards in redeposited second transparency conducting layer of the second electrochromism layer surface, double-deck electrochromic device is obtained.
In one of the embodiments, step 4. in, in addition to the transparent nanoparticles film carry out H+Or Li+It is molten
The step of immersion is steeped.
In one of the embodiments, first transparency conducting layer, the second transparency conducting layer, the first electrochromic layer and
Second electrochromic layer uses magnetron sputtering membrane process.
The all solid state inorganic electrochromic device that the present invention is provided, is made up of multilayer Solid inorganic composite membrane, with electroluminescent
Electrochromic device most typically, simplest structure, can realize the stable target of extensive industrialization, all solid state, device performance, can
To be directly used in the field of intelligent window and Display Technique etc., have a good application prospect.
In addition, inorganic oxide prepared by using plasma enhancing chemical vapor deposition (PECVD) technology of the present invention is received
Rice grain film is with low cost as solid electrolyte, and preparation method is simple and easy to apply.Therefore, the present invention breaches existing electroluminescent
The Organic inorganic film structure limitation of Electrochromic device, is innovatively proposed with all solid state inorganic electrochromic device
Part, its with low cost, making is simple, easily accomplish scale production, and has broad application prospects.
Brief description of the drawings
Fig. 1 is the three-dimensional cutaway view of the electrochromic device of the embodiment of the present invention 1；
Fig. 2 is the three-dimensional cutaway view of the electrochromic device of the embodiment of the present invention 2；
Fig. 3 is the transmission electron microscope figure of the transparent nanoparticles film of the embodiment of the present invention 1.
Embodiment
The invention provides a kind of all solid state inorganic electrochromic device and preparation method thereof, the electrochromic device is many
Layer structure of composite membrane, including transparency conducting layer, electrochromic layer and dielectric substrate.In an embodiment of the present invention, electrically conducting transparent
Layer includes the first transparency conducting layer and the second transparency conducting layer, respectively as cathode/anode electrode and anode/cathode electrodes；Electricity
Mutagens chromatograph is divided into negative electrode photochromic layer and anode photochromic layer, in electrochromic device, can be only comprising one layer of negative electrode photochromic layer
Or one layer of anode photochromic layer, negative electrode photochromic layer and anode photochromic layer can also be included simultaneously；Dielectric substrate is ion transport layers,
In the present invention, dielectric substrate is the transparent nanoparticles film of the silica of silica or phosphorus doping.Preferably, each film
Transmitance of the layer in visible-range is up to more than 80%.The present invention is described in further detail below, it should be pointed out that
Embodiment described below is intended to be easy to the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1：
As shown in figure 1, the present embodiment provides a kind of all solid state inorganic electrochromic device of individual layer, transparent substrates 1 are common
Sheet glass；First transparency conducting layer 2 is indium zinc oxygen (IZO) film, is connected with extraneous power supply, is used as cathode electrode；First electroluminescent change
Chromatograph 3 is tungsten oxide (WOx) film, it is used as negative electrode photochromic layer；Dielectric substrate 4 is silica（SiO2）Transparent nanoparticles film, makees
For dielectric substrate；Second transparency conducting layer 5 is indium zinc oxygen film, is connected with extraneous power supply, is used as anode electrode.
The preparation method of above-mentioned all solid state inorganic electrochromic device comprises the following steps：
Step 1：It is 2.5 × 2.5cm to be cleaned by ultrasonic clean area through acetone and ethanol solution2Simple glass make
For transparent substrates 1, transmitance of the simple glass in visible-range is up to more than 80%, and surface is smooth and has planar junction
Structure；
Step 2：Magnetron sputtering method is used to deposit indium zinc oxygen film of a layer thickness for 50nm~5 μm in transparent substrates 1；
Step 3：By one jiao of covering of indium zinc oxygen film, as electrode contact area, using magnetron sputtering method on indium zinc oxygen film
Area's deposition tungsten oxide layer film, preferred 50nm~2 μm of its thickness are not covered；
Step 4：Using plasma enhanced chemical vapor deposition (PECVD) technology one layer of dioxy is deposited on oxidation tungsten film
SiClx (SiO2) nano-particular film；
Step 5：Using magnetron sputtering method in silica (SiO2) one layer of indium zinc oxygen (IZO) film is deposited on film, thickness is
50nm~5 μm, obtain individual layer electrochromic device.
Add 5V and -10V side's pressure, the list between the cathode electrode and anode electrode of obtained individual layer electrochromic device
Layer electrochromism device is in the transparent reversible change between blueness.This device is using PECVD deposition silica (SiO2) film conduct
The dielectric substrate of inorganic electrochromic device, with low cost, preparation method is simple and easy to apply, and all solid state preparation technology is more favourable
In the large-scale production of product.It is preferred that silica (SiO2) thickness of nano-particular film is 100nm~10 μm, thick herein
Under degree, silica (SiO2) film have higher transparency and good ionic adsorption-desorption performance.Preferably, titanium dioxide
Silicon (SiO2) nano-particular film granularity be 1nm~20nm, Fig. 3 be the present embodiment in transparent nanoparticles film transmitted electron show
Micro mirror figure, as can be seen from Figure, the membrane-coating granules are evenly distributed and dense porous, its adsorption-desorption for being conducive to ion and transfer,
The sensitivity of electrochromic device can be lifted.
Embodiment 2：
As shown in Fig. 2 the present embodiment provides a kind of double-deck all solid state inorganic electrochromic device, transparent substrates 1 are common
Sheet glass；First transparency conducting layer 2 is indium tin oxygen (ITO) film, is used as cathode electrode；First electrochromic layer 3 is tungsten oxide
(WOx) film, it is used as negative electrode photochromic layer；Dielectric substrate 4 is the silica (SiO of phosphorus doping2:P) film, is used as dielectric substrate；Second
Transparency conducting layer 5 is indium tin oxygen (ITO) film, is used as anode electrode；Second electrochromic layer 6 is nickel oxide (NiO) film, is used as sun
Pole photochromic layer.
The preparation method of above-mentioned inorganic electrochromic device comprises the following steps：
Step 1：It is 2.5 × 2.5cm to be cleaned by ultrasonic clean area through acetone and ethanol solution2Simple glass make
For transparent substrates 1；
Step 2：Deposit one layer of indium tin oxygen (ITO) film in transparent substrates 1 using magnetron sputtering method, thickness is the μ of 50nm~5
m；
Step 3：By one jiao of covering of indium tin oxygen (ITO) film, as electrode contact area, using magnetron sputtering method in indium tin oxygen
(ITO) area is not covered on film and deposits the tungsten oxide (WO that a layer thickness is 50nm~2 μmx) film；
Step 4：Using plasma enhanced chemical vapor deposition technology in tungsten oxide (WOx) one layer of phosphorus doping is deposited on film
Silica (SiO2:P) film, as the dielectric substrate of inorganic electrochromic device, its thickness is 100nm~10 μm；
Step 5：Using magnetron sputtering method in phosphorus doped silicon dioxide (SiO2:P it is 50nm~2 that a layer thickness) is deposited on film
μm nickel oxide (NiO) film；
Step 6：The indium tin oxygen that a layer thickness is 50nm~5 μm is deposited on nickel oxide (NiO) film using magnetron sputtering method
(ITO) film, obtains double-deck electrochromic device.
Add 5V and -10V side's pressure, the double-layer electric between the cathode electrode and anode electrode of obtained double-deck Electrochromic device
Cause color-changing device reversible change between clear, colorless and blueness and the secondary colour of brown.The device of double-deck electrochromism membrane structure,
The ion of dielectric substrate can be enable to colour or fade to two membranes simultaneously；And a more neutral visual appearance can be formed, fit
For being normally applied in building.The present embodiment uses phosphorus doped silicon dioxide (SiO2:P) film is used as inorganic electrochromic device
Dielectric substrate, sedimentary origin be silane (SiH4) and phosphine (PH3) mixture, it is preferable that PH3Shared mol ratio be 5%~
10%, within this range, the incorporation of phosphorus improves the proton conductivity of dielectric substrate, so that the response of electrochromic device
Time shortens.
Embodiment 3：
The present embodiment provides a kind of all solid state inorganic electrochromic device of individual layer, and transparent substrates are common glass sheet；First
Transparency conducting layer is indium zinc oxygen (IZO) film, is connected with extraneous power supply, is used as cathode electrode；First electrochromic layer is tungsten oxide
(WOx) film, it is used as negative electrode photochromic layer；Dielectric substrate is perchloric acid (HClO4) solution immersion after silica (SiO2) film, make
For dielectric substrate；Second transparency conducting layer is indium zinc oxygen film, is connected with extraneous power supply, is used as anode electrode.
The preparation method of above-mentioned inorganic electrochromic device comprises the following steps：
Step 1：It is 2.5 × 2.5cm to be cleaned by ultrasonic clean area through acetone and ethanol solution2Simple glass make
For transparent substrates；
Step 2：One layer of indium zinc oxygen (IZO) film is deposited on substrate using magnetron sputtering method, all solid state inorganic electroluminescence is used as
The cathode electrode of Electrochromic device, it is preferable that transmitance >=80% of the cathode electrode in visible-range, and thickness is 50nm~5
μm；
Step 3：By one jiao of covering of indium zinc oxygen film, as electrode contact area, using magnetron sputtering method on indium zinc oxygen film
Area is not covered deposits the tungsten oxide (WO that a layer thickness is 50nm~2 μmx) film；
Step 4：Using plasma enhanced chemical vapor deposition technology in tungsten oxide (WOx) deposition a layer thickness is on film
Silica (the SiO of 100nm~10 μm2) film, and by silica (SiO2) film carry out concentration be 10% perchloric acid (HClO4) molten
The dielectric substrate of inorganic electrochromic device is used as after liquid immersion treatment；
Step 5：Using magnetron sputtering method in silica (SiO2) deposition a layer thickness is 50nm~5 μm on dielectric substrate
Indium zinc oxygen (IZO) film, obtain individual layer electrochromic device.
Add 5V and -10V side's pressure, the list between the cathode electrode and anode electrode of obtained individual layer electrochromic device
Layer electrochromism device is in the transparent reversible change between blueness.In perchloric acid (HClO4) dielectric substrate that soaked in solution, inhale
It is attached-to be desorbed more H+Ion, makes Electrochromic device to colour or fade faster when in use, reduces the response time.In addition,
Dielectric substrate can also contain H other+Or Li+Solution such as phosphoric acid（H3PO4）And lithium perchlorate（LiClO4）Soaked in solution
Bubble, and can obtain and perchloric acid solution identical beneficial effect.
Embodiments of the invention use magnetron sputtering deposition transparency conducting layer and electrochromic layer, the original of magnetically controlled sputter method
Son with being sputtered after energetic ion positive energy exchange, and its energy is higher, and often the atom than evaporation is higher by 1~2 order of magnitude,
The film thus formed with sputtering method has more preferable adhesiveness with substrate.
It should be noted that the transparency conducting layer of the present invention and the coating process of electrochromic layer are not limited to above-described embodiment
In magnetron sputtering technique, in addition to vacuum thermal evaporation technology, chemical vapour deposition technique, PECVD be heavy
Product technology (PECVD), sol-gel technique or spraying technology.The transparency conducting layer of the present invention is not limited in above-described embodiment
Tin indium oxide (ITO) film and indium zinc oxygen (IZO) film, in addition to indium gallium zinc oxygen (IGZO) film, aluminium zinc oxygen (AZO) film etc. is to visible
The higher oxidation film of light transmission rate；Anode electrochromic film also includes yttrium oxide, rhodium oxide, manganese oxide, cobalt oxide, oxidation
Iron, chromium oxide, vanadium oxide, negative electrode color-changing membrane also includes molybdenum oxide, niobium oxide, tantalum oxide, titanium oxide, vanadium oxide.
Inorganic oxide nanoparticles prepared by using plasma enhancing chemical vapor deposition (PECVD) technology of the present invention
Film is with low cost as solid electrolyte, and preparation method is simple and easy to apply.Therefore, the present invention breaches existing electrochromism device
Part Organic inorganic film structure limitation, innovatively propose with all solid state inorganic electrochromic device, its into
Cheap, making is simple for this, easily accomplish scale production, and has broad application prospects.In addition, the present invention provide it is all solid state
Inorganic electrochromic device, is made up of multilayer Solid inorganic composite membrane, with electrochromic device most typically, simplest knot
Structure, can realize the stable target of extensive industrialization, all solid state, device performance, be used directly for intelligent window and display
The field of technology etc., has a good application prospect.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. a kind of all solid state inorganic electrochromic device, including transparency conducting layer, electrochromic layer and dielectric substrate, its feature
Be, the dielectric substrate is the transparent nanoparticles film of the silica of silica or phosphorus doping, the silica or
The particle diameter of the transparent nanoparticles film of the silica of phosphorus doping is 1nm~20nm, the dioxy of the silica or phosphorus doping
Transmitance >=80% of the transparent nanoparticles film of SiClx in visible-range, thickness is 100nm~10 μm.
2. all solid state inorganic electrochromic device according to claim 1, it is characterised in that the transparency conducting layer is can
Transmitance >=80% seen in optical range, thickness is 50nm~5 μm.
3. all solid state inorganic electrochromic device according to claim 1, it is characterised in that the electrochromic layer is can
Transmitance >=80% seen in optical range, thickness is 50nm~2 μm.
4. a kind of preparation method of all solid state inorganic electrochromic device described in any one of claim 1-3, it is characterised in that
Comprise the following steps：
1. chooses the transparent substrates of certain area and cleaned up；
2. deposits the first transparency conducting layer using coating process on the transparent substrates surface；
3. is by one jiao of covering of first transparency conducting layer, as electrode contact area, and using coating process described first
The surface of the non-cover part of transparency conducting layer deposits the first electrochromic layer；
4. plasma enhanced chemical vapor deposition methods deposit silica in the first electrochromism layer surface or phosphorus is mixed
The transparent nanoparticles film of miscellaneous silica, is used as dielectric substrate；
5. deposits the second transparency conducting layer using coating process on the transparent nanoparticles film surface, obtains the electroluminescent change of individual layer
Color device；The second electrochromic layer, Ran Hou are first either deposited on the transparent nanoparticles film surface using coating process
Redeposited second transparency conducting layer of the second electrochromism layer surface, obtains double-deck electrochromic device.
5. preparation method according to claim 4, it is characterised in that step 4. in, in addition to the transparent nano
Membrana granulosa carries out H+Or Li+The step of solution soaks.
6. preparation method according to claim 4, it is characterised in that first transparency conducting layer, the second electrically conducting transparent
Layer, the first electrochromic layer and the second electrochromic layer use magnetron sputtering membrane process.
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| CN105633282B (en) * | 2016-03-08 | 2018-04-17 | 中国计量学院 | A kind of photosensitive organic field-effect transistor with electrochomeric films |
| CN105911790A (en) * | 2016-06-03 | 2016-08-31 | 深圳市华星光电技术有限公司 | Display device and appearance structural element thereof |
| WO2018064353A1 (en) * | 2016-09-30 | 2018-04-05 | Gentex Corporation | Color excursion mitigation in electrochromic devices |
| CN108254989B (en) * | 2016-12-29 | 2020-09-29 | 宁波祢若电子科技有限公司 | All-solid-state electrochromic window, solid-state electrochromic mirror and preparation method of all-solid-state electrochromic window and solid-state electrochromic mirror |
| CN114994997B (en) * | 2021-03-01 | 2023-10-13 | 中国科学院上海硅酸盐研究所 | Electrochromic device with mesoporous structure and preparation method thereof |
| CN114563896A (en) * | 2022-01-27 | 2022-05-31 | 南方科技大学 | Multicolor inorganic all-solid-state electrochromic device and preparation method thereof |
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| CN1426543A (en) * | 2000-12-27 | 2003-06-25 | 索尼公司 | Electrochromic display device and electrodeposition display device |
| CN101765808A (en) * | 2007-06-07 | 2010-06-30 | 索拉迪格姆公司 | Electrochromic devices and fabrication method |
| US7646526B1 (en) * | 2008-09-30 | 2010-01-12 | Soladigm, Inc. | Durable reflection-controllable electrochromic thin film material |
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