CN104570534A - All-solid-state inorganic electrochromic device and fabrication method thereof - Google Patents
All-solid-state inorganic electrochromic device and fabrication method thereof Download PDFInfo
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- CN104570534A CN104570534A CN201310467114.2A CN201310467114A CN104570534A CN 104570534 A CN104570534 A CN 104570534A CN 201310467114 A CN201310467114 A CN 201310467114A CN 104570534 A CN104570534 A CN 104570534A
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- electrochromic device
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- silicon dioxide
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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 an all-solid-state inorganic electrochromic device and a fabrication method thereof. The all-solid-state inorganic electrochromic device comprises a transparent conductive layer, an electrochromic layer and an electrolyte layer, wherein the electrolyte layer is a silicon dioxide or phosphor-doped silicon dioxide transparent nano-particulate film. The all-solid-state inorganic electrochromic device provided by the invention comprises multiple layers of solid inorganic composite membranes, has the most typical and simplest structure of an electrochromic device, can achieve the targets of large-scale industrialization, full solid state and stable device performance, and can be directly applied to the fields of smart windows, display technologies and the like, thereby having a good application prospect. The electrochromic device with low cost, large-scale industrialization and stable performance can be obtained by utilizing the method provided by the invention, and comprises the all-solid-state inorganic solid inorganic composite membranes; the method can be directly applied to the manufacturing line of an existing industrialized electrochromic device, and has an important application value.
Description
Technical field
The present invention relates to electrochromism technical field, particularly relate to a kind of all solid state inorganic electrochromic device and preparation method thereof.
Background technology
After electrochromic material refers to making alive, its optical properties (emissivity, percent of pass, absorptivity etc.) can stablize the material of reversible change.The scope that electrochromic material comprises is comparatively wide, is broadly divided into electrodeless electrochromic material and organic electrochromic material two kinds.Be called electrochromic device with the device that electrochromic material is made, electrochromic device have efficiently, low consumption, the advantage such as pollution-free, intelligent, at automobile rearview mirror, the windowpane of building, aircraft, steamer etc. all has broad application prospects.
Electrochromic device generally comprises transparency conducting layer, electrochromic layer and dielectric substrate, and is supported by a transparent substrates, or is placed between two transparent substrates.Dielectric substrate is the transmission channel of electrochromic effect desired ion, is divided into solid electrolyte and liquid electrolyte.Liquid electrolyte mass-energy provides good electrochromism response and high ionic conductivity, but its corrosion resistance and poor chemical stability and encapsulation is difficult.Solid electrolyte is generally organic polymer, and its poor heat stability, is extremely restricted in actual applications, and is unfavorable for the large-scale production of electrochromic device.
Summary of the invention
Based on the problems referred to above; 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 difficulty and polymer dielectric poor heat stability, be unfavorable for the problem of large-scale production.
For achieving the above object, the present invention adopts following technical scheme:
A kind of all solid state inorganic electrochromic device, comprise transparency conducting layer, electrochromic layer and dielectric substrate, described dielectric substrate is the transparent nanoparticles film of the silicon dioxide of silicon dioxide or phosphorus doping.
Wherein in an embodiment, transmitance >=80% of described transparency conducting layer in visible-range, thickness is 50nm ~ 5 μm.
Wherein in an embodiment, transmitance >=80% of described electrochromic layer in visible-range, thickness is 50nm ~ 2 μm.
Wherein in an embodiment, the granularity of the transparent nanoparticles film of the silicon dioxide of described silicon dioxide or phosphorus doping is 1nm ~ 20nm.
Wherein in an embodiment, transmitance >=80% of transparent nanoparticles film in visible-range of the silicon dioxide of described silicon dioxide or phosphorus doping, thickness is 100nm ~ 10 μm.
A preparation method for described all solid state inorganic electrochromic device, comprises the following steps:
1.. choose the transparent substrates of certain area and clean up;
2.. adopt coating process at described transparent substrates surface deposition first transparency conducting layer;
3.. by one jiao of described first transparency conducting layer covering, as electrode contact district, and adopt coating process at surface deposition first electrochromic layer of the non-cover part of described first transparency conducting layer;
4.. with the plasma enhanced chemical vapor deposition method transparent nanoparticles film at the silicon dioxide of described first electrochromic layer surface deposition silicon dioxide or phosphorus doping, as dielectric substrate;
5.. adopt coating process at described transparent nanoparticles film surface deposition second transparency conducting layer, obtain individual layer electrochromic device; Or adopt coating process first to deposit the second electrochromic layer on described transparent nanoparticles film surface, then deposit described second transparency conducting layer again on described second electrochromic layer surface, obtain double-deck electrochromic device.
Wherein in an embodiment, step 4. in, also comprise and H carried out to described transparent nanoparticles film
+or Li
+the step that solution soaks.
Wherein in an embodiment, described first transparency conducting layer, the second transparency conducting layer, the first electrochromic layer and the second electrochromic layer all adopt magnetron sputtering membrane process.
All solid state inorganic electrochromic device provided by the invention, be made up of multilayer Solid inorganic composite membrane, there is the most typical, the simplest structure of electrochromic device, extensive industrialization, the target that all solid state, device performance is stable can be realized, the field of intelligent window and display technique etc. can be directly used in, have a good application prospect.
In addition, inorganic oxide nanoparticles film prepared by using plasma enhancing chemical vapor deposition (PECVD) technology of the present invention is as solid electrolyte, and with low cost, method for making is simple.Therefore; the present invention breaches the Organic inorganic film structural limitations of existing electrochromic device; propose innovatively and there is all solid state inorganic electrochromic device, it is with low cost, making simply, is easily accomplished scale production, have broad application prospects.
Accompanying drawing explanation
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, this electrochromic device is MULTILAYER COMPOSITE membrane structure, comprises transparency conducting layer, electrochromic layer and dielectric substrate.In an embodiment of the present invention, transparency conducting layer comprises the first transparency conducting layer and the second transparency conducting layer, respectively as cathode/anode electrode and anode/cathode electrodes; Electrochromic layer is divided into negative electrode photochromic layer and anode photochromic layer, in electrochromic device, only can comprise one deck negative electrode photochromic layer or one deck anode photochromic layer, also can comprise negative electrode photochromic layer and anode photochromic layer simultaneously; Dielectric substrate is ion transport layers, and in the present invention, dielectric substrate is the transparent nanoparticles film of the silicon dioxide of silicon dioxide or phosphorus doping.As preferably, the transmitance of each rete in visible-range reaches more than 80%.Below the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.
Embodiment 1:
As shown in Figure 1, the present embodiment provides a kind of individual layer all solid state inorganic electrochromic device, and transparent substrates 1 is common glass sheet; First transparency conducting layer 2 is indium zinc oxygen (IZO) film, is communicated with, as cathode electrode with extraneous power supply; First electrochromic layer 3 is tungsten oxide (WO
x) film, as negative electrode photochromic layer; Dielectric substrate 4 is silicon dioxide (SiO
2) transparent nanoparticles film, as dielectric substrate; Second transparency conducting layer 5 is indium zinc oxygen film, is communicated with, as anode electrode with extraneous power supply.
The method for making of above-mentioned all solid state inorganic electrochromic device comprises the steps:
Step 1: the area through acetone and ethanol solution ultrasonic cleaning cleaning is 2.5 × 2.5cm
2simple glass as transparent substrates 1, the transmitance of this simple glass in visible-range reaches more than 80%, and smooth surface have planar structure;
Step 2: adopt magnetron sputtering method to deposit in transparent substrates 1 indium zinc oxygen film that a layer thickness is 50nm ~ 5 μm;
Step 3: by one jiao of covering of indium zinc oxygen film, as electrode contact district, utilizes magnetron sputtering method on indium zinc oxygen film, not hide district's deposition tungsten oxide layer film, preferred 50nm ~ 2 μm of its thickness;
Step 4: utilize plasma enhanced chemical vapor deposition (PECVD) technology to deposit layer of silicon dioxide (SiO on oxidation tungsten film
2) nano-particular film;
Step 5: utilize magnetron sputtering method at silicon dioxide (SiO
2) film deposits one deck indium zinc oxygen (IZO) film, thickness is 50nm ~ 5 μm, obtains individual layer electrochromic device.
Between the cathode electrode and anode electrode of the individual layer electrochromic device obtained, add 5V press with the side of-10V, the reversible change between transparent and blueness of this individual layer electrochromism device.This device adopts PECVD deposition of silica (SiO
2) film is as the dielectric substrate of inorganic electrochromic device, with low cost, method for making is simple, and all solid state preparation technology is more conducive to the large-scale production of product.Preferably, silicon dioxide (SiO
2) thickness of nano-particular film is 100nm ~ 10 μm, under this thickness, silicon dioxide (SiO
2) film has higher transparency and good ionic adsorption-desorption performance.Preferably, silicon dioxide (SiO
2) granularity of nano-particular film is 1nm ~ 20nm, Fig. 3 is the transmission electron microscope figure of transparent nanoparticles film in the present embodiment, and as can be seen from Figure, this membrane-coating granules is evenly distributed and dense porous, it is conducive to adsorption-desorption and the transfer of ion, can promote the sensitivity of electrochromic device.
Embodiment 2:
As shown in Figure 2, the present embodiment provides a kind of double-deck all solid state inorganic electrochromic device, and transparent substrates 1 is common glass sheet; First transparency conducting layer 2 is indium tin oxygen (ITO) film, as cathode electrode; First electrochromic layer 3 is tungsten oxide (WO
x) film, as negative electrode photochromic layer; Dielectric substrate 4 is the silicon dioxide (SiO of phosphorus doping
2: P) film, as dielectric substrate; Second transparency conducting layer 5 is indium tin oxygen (ITO) film, as anode electrode; Second electrochromic layer 6 is nickel oxide (NiO) films, as anode photochromic layer.
The method for making of above-mentioned inorganic electrochromic device comprises the steps:
Step 1: the area through acetone and ethanol solution ultrasonic cleaning cleaning is 2.5 × 2.5cm
2simple glass as transparent substrates 1;
Step 2: adopt magnetron sputtering method to deposit one deck indium tin oxygen (ITO) film in transparent substrates 1, thickness is 50nm ~ 5 μm;
Step 3: by one jiao of indium tin oxygen (ITO) film covering, as electrode contact district, utilizes magnetron sputtering method on indium tin oxygen (ITO) film, do not hide district and deposits the tungsten oxide (WO that a layer thickness is 50nm ~ 2 μm
x) film;
Step 4: utilize plasma enhanced chemical vapor deposition technology at tungsten oxide (WO
x) film deposits one deck phosphorus doped silicon dioxide (SiO
2: P) film, as the dielectric substrate of inorganic electrochromic device, its thickness is 100nm ~ 10 μm;
Step 5: utilize magnetron sputtering method at phosphorus doped silicon dioxide (SiO
2: P) film deposits nickel oxide (NiO) film that a layer thickness is 50nm ~ 2 μm;
Step 6: utilize magnetron sputtering method to deposit on nickel oxide (NiO) film indium tin oxygen (ITO) film that a layer thickness is 50nm ~ 5 μm, obtains double-deck electrochromic device.
Between the cathode electrode and anode electrode of the double-deck Electrochromic device obtained, add 5V press with the side of-10V, this double-deck electroluminescent color-changing device is in clear, colorless and reversible change between blueness and brown color mixture.The device of double-deck electrochromic film structure, can make the ion of dielectric substrate can be simultaneously painted to two membranes or fade; And a comparatively neutral visual appearance can be formed, be applicable to the general application in building.The present embodiment adopts phosphorus doped silicon dioxide (SiO
2: P) film is as the dielectric substrate of inorganic electrochromic device, and sedimentary origin is silane (SiH
4) and phosphine (PH
3) potpourri, preferably, PH
3shared mol ratio is 5% ~ 10%, within the scope of this, phosphorus mix the proton conductivity that improve dielectric substrate, thus shortened the response time of electrochromic device.
Embodiment 3:
The present embodiment provides a kind of individual layer all solid state inorganic electrochromic device, and transparent substrates is common glass sheet; First transparency conducting layer is indium zinc oxygen (IZO) film, is communicated with, as cathode electrode with extraneous power supply; First electrochromic layer is tungsten oxide (WO
x) film, as negative electrode photochromic layer; Dielectric substrate is perchloric acid (HClO
4) solution soak after silicon dioxide (SiO
2) film, as dielectric substrate; Second transparency conducting layer is indium zinc oxygen film, is communicated with, as anode electrode with extraneous power supply.
The method for making of above-mentioned inorganic electrochromic device comprises the steps:
Step 1: the area through acetone and ethanol solution ultrasonic cleaning cleaning is 2.5 × 2.5cm
2simple glass as transparent substrates;
Step 2: adopt magnetron sputtering method at deposited on substrates one deck indium zinc oxygen (IZO) film, as the cathode electrode of all solid state inorganic electrochromic device, preferably, transmitance >=80% of 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 district, utilizes magnetron sputtering method on indium zinc oxygen film, do not hide district and deposits the tungsten oxide (WO that a layer thickness is 50nm ~ 2 μm
x) film;
Step 4: utilize plasma enhanced chemical vapor deposition technology at tungsten oxide (WO
x) film deposits the silicon dioxide (SiO that a layer thickness is 100nm ~ 10 μm
2) film, and by silicon dioxide (SiO
2) to carry out concentration be 10% perchloric acid (HClO to film
4) after solution immersion treatment as the dielectric substrate of inorganic electrochromic device;
Step 5: utilize magnetron sputtering method at silicon dioxide (SiO
2) dielectric substrate deposits indium zinc oxygen (IZO) film that a layer thickness is 50nm ~ 5 μm, obtain individual layer electrochromic device.
Between the cathode electrode and anode electrode of the individual layer electrochromic device obtained, add 5V press with the side of-10V, the reversible change between transparent and blueness of this individual layer electrochromism device.At perchloric acid (HClO
4) dielectric substrate that soaked in solution, the more H of adsorption-desorption
+ion, makes Electrochromic device in use can be painted or fade faster, reduces the response time.In addition, dielectric substrate can also contain H at other
+or Li
+solution as phosphoric acid (H
3pO
4) and lithium perchlorate (LiClO
4) soak in solution, and the beneficial effect identical with perchloric acid solution can be obtained.
Embodiments of the invention adopt magnetron sputtering deposition transparency conducting layer and electrochromic layer, the atom of magnetically controlled sputter method be with energetic ion positive energy exchange after sputter and go out, its energy is higher, often than evaporation atom exceed 1 ~ 2 order of magnitude, thus with sputtering method formed film and substrate there is better adhesiveness.
It should be noted that, the coating process of transparency conducting layer of the present invention and electrochromic layer is not limited to the magnetron sputtering technique in above-described embodiment, also comprises vacuum thermal evaporation technology, chemical vapour deposition technique, plasma enhanced chemical vapor deposition technology (PECVD), sol-gel technique or spraying technology.Transparency conducting layer of the present invention is not limited to tin indium oxide (ITO) film in above-described embodiment and indium zinc oxygen (IZO) film, also comprise indium gallium zinc oxygen (IGZO) film, the oxidation film that aluminium zinc oxygen (AZO) film etc. are higher to visible light transmissivity; Anode electrochromic film also comprises yttrium oxide, rhodium oxide, manganese oxide, cobalt oxide, iron oxide, chromium oxide, vanadium oxide, and negative electrode color-changing membrane also comprises molybdena, niobium oxide, tantalum oxide, titanium dioxide, vanadium oxide.
Inorganic oxide nanoparticles film prepared by using plasma enhancing chemical vapor deposition (PECVD) technology of the present invention is as solid electrolyte, and with low cost, method for making is simple.Therefore; the present invention breaches the Organic inorganic film structural limitations of existing electrochromic device; propose innovatively and there is all solid state inorganic electrochromic device, it is with low cost, making simply, is easily accomplished scale production, have broad application prospects.In addition, all solid state inorganic electrochromic device provided by the invention, be made up of multilayer Solid inorganic composite membrane, there is the most typical, the simplest structure of electrochromic device, extensive industrialization, the target that all solid state, device performance is stable can be realized, the field of intelligent window and display technique etc. can be directly used in, have a good application prospect.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. an all solid state inorganic electrochromic device, comprises transparency conducting layer, electrochromic layer and dielectric substrate, it is characterized in that, described dielectric substrate is the transparent nanoparticles film of the silicon dioxide of silicon dioxide or phosphorus doping.
2. all solid state inorganic electrochromic device according to claim 1, is characterized in that, transmitance >=80% of described transparency conducting layer in visible-range, and thickness is 50nm ~ 5 μm.
3. all solid state inorganic electrochromic device according to claim 1, is characterized in that, transmitance >=80% of described electrochromic layer in visible-range, and thickness is 50nm ~ 2 μm.
4. all solid state inorganic electrochromic device according to claim 1, is characterized in that, the particle diameter of the transparent nanoparticles film of the silicon dioxide of described silicon dioxide or phosphorus doping is 1nm ~ 20nm.
5. all solid state inorganic electrochromic device according to claim 1, is characterized in that, transmitance >=80% of transparent nanoparticles film in visible-range of the silicon dioxide of described silicon dioxide or phosphorus doping, thickness is 100nm ~ 10 μm.
6. a preparation method for all solid state inorganic electrochromic device described in any one of claim 1-5, is characterized in that, comprise the following steps:
1.. choose the transparent substrates of certain area and clean up;
2.. adopt coating process at described transparent substrates surface deposition first transparency conducting layer;
3.. by one jiao of described first transparency conducting layer covering, as electrode contact district, and adopt coating process at surface deposition first electrochromic layer of the non-cover part of described first transparency conducting layer;
4.. with the plasma enhanced chemical vapor deposition method transparent nanoparticles film at the silicon dioxide of described first electrochromic layer surface deposition silicon dioxide or phosphorus doping, as dielectric substrate;
5.. adopt coating process at described transparent nanoparticles film surface deposition second transparency conducting layer, obtain individual layer electrochromic device; Or adopt coating process first to deposit the second electrochromic layer on described transparent nanoparticles film surface, then deposit described second transparency conducting layer again on described second electrochromic layer surface, obtain double-deck electrochromic device.
7. preparation method according to claim 6, is characterized in that, step 4. in, also comprise and H carried out to described transparent nanoparticles film
+or Li
+the step that solution soaks.
8. preparation method according to claim 6, is characterized in that, described first transparency conducting layer, the second transparency conducting layer, the first electrochromic layer and the second electrochromic layer all adopt magnetron sputtering membrane process.
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|---|---|---|---|---|
| CN105633282A (en) * | 2016-03-08 | 2016-06-01 | 中国计量学院 | Photosensitive organic field-effect transistor with electrochromic film |
| 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 |
| CN108254989A (en) * | 2016-12-29 | 2018-07-06 | 宁波祢若电子科技有限公司 | Full-solid electrochromic window and solid-state electrochromic mirror and preparation method thereof |
| CN109690395A (en) * | 2016-09-30 | 2019-04-26 | 金泰克斯公司 | Color offset in electrochromic device is alleviated |
| 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 |
| CN114994997A (en) * | 2021-03-01 | 2022-09-02 | 中国科学院上海硅酸盐研究所 | Electrochromic device with mesoporous structure and preparation method thereof |
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| CN108254989A (en) * | 2016-12-29 | 2018-07-06 | 宁波祢若电子科技有限公司 | Full-solid electrochromic window and solid-state electrochromic mirror and preparation method thereof |
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| CN114994997A (en) * | 2021-03-01 | 2022-09-02 | 中国科学院上海硅酸盐研究所 | Electrochromic device with mesoporous structure and preparation method thereof |
| 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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