CN105607374A - Solid-state full-inorganic electrochromic glass and preparation method thereof - Google Patents
Solid-state full-inorganic electrochromic glass and preparation method thereof Download PDFInfo
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- CN105607374A CN105607374A CN201610144186.7A CN201610144186A CN105607374A CN 105607374 A CN105607374 A CN 105607374A CN 201610144186 A CN201610144186 A CN 201610144186A CN 105607374 A CN105607374 A CN 105607374A
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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
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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
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- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention relates to solid-state full-inorganic electrochromic glass and a preparation method thereof. The solid-state full-inorganic electrochromic glass is characterized in that the structure of the electrochromic glass comprises a glass substrate and a transparent conducting layer, an electrochromic layer, an electrolyte layer, an ion storage layer and a transparent conducting layer which are sequentially deposited on the glass substrate, and a lithium oxide thin film of a non-crystalline structure serves as the electrolyte layer. According to the electrochromic glass, the electrolyte layer adopts non-crystalline lithium oxide, embedding and extracting of Li<+> are facilitated, changing of the structure and composition of an electrolyte cannot be caused, and therefore the ion conductivity of the electrolyte layer is improved, and the cycle life of the electrochromic glass is prolonged.
Description
Technical field
The present invention relates to a kind of electrochomeric glass, particularly relate to a kind of solid-state full-inorganic electrochromismGlass and preparation method thereof.
Background technology
Electrochromism phenomenon refers to that material is under DC Electric Field, be accompanied by H+, Li+, Na+ etc. fromThe injection of son or electrochemical reaction process occurs while deviating from, its optical property produces reversible variation thus,Thereby realize the regulation and control to light reflection, transmission, absorption. The device of being made by electrochromic material is calledElectrochromic device, electrochromic device has efficiently, low consumption, the advantage such as pollution-free, intelligent,After automobile, on the windowpane of building, visor, aircraft, steamer etc., all have broad application prospects.Electrochomeric glass is conventional electrochromism device, and wherein the dielectric substrate of electrochomeric glass is that electricity causesThe transmission channel of discoloration effect desired ion. Also do not have at present excellent performance, the stable building of variable color to adjustLight puts goods on the market in enormous quantities with solid-state full-inorganic electrochomeric glass, and main cause is the electricity using at presentThere is following problem in the dielectric substrate that causes photo chromic glass: the one, and ionic conductance is lower, causes variable color speedRate is slower, and the 2nd, dielectric substrate is after circulation a period of time, and Li+ causes that electrolyte ingredient, structure occurChange, cause Li+ mobility to reduce, variable color amplitude reduces.
Summary of the invention
Main purpose of the present invention is, provide a kind of New Solid full-inorganic electrochomeric glass andPreparation method, technical problem to be solved is to make the conductivity of its dielectric substrate high, thereby suitableeerIn practicality.
The object of the invention to solve the technical problems realizes by the following technical solutions. FoundationThe solid-state full-inorganic electrochomeric glass of one that the present invention proposes, the structure of described electrochomeric glassComprise glass substrate and be deposited on successively transparency conducting layer, electrochromic layer, the electricity on glass substrateSeparate matter layer, ion storage, transparency conducting layer, the oxidation that described dielectric substrate is amorphous structureLithium film.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Preferably, aforesaid solid-state full-inorganic electrochomeric glass, wherein said transparency conducting layer isTin-doped indium oxide or fluorine-doped tin oxide, described electrochromic layer is tungsten oxide film, described ionAccumulation layer is the oxide of nickel tungsten.
Preferably, aforesaid solid-state full-inorganic electrochomeric glass, wherein said electrochomeric glassThe thickness of dielectric substrate be 5-200nm, the transmitance in visible-range is greater than 80%.
The object of the invention to solve the technical problems also adopts following technical scheme to realize. FoundationThe preparation method of a kind of solid-state full-inorganic electrochomeric glass that the present invention proposes, described electrochromismThe dielectric substrate of glass is to utilize magnetron sputtering oxygen by the electrochromic layer described or ion storageChanging lithium target or reaction magnetocontrol sputtering lithium target makes.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Preferably, the preparation method of aforesaid solid-state full-inorganic electrochomeric glass, wherein said profitPreparing dielectric substrate with magnetron sputtering lithia target comprises: pass into argon gas to vacuum chamber, control argon gasFlow is 10-50sccm, keeps operating air pressure 0.2-2Pa, starts to electrochromic layer or ion storageSputter coating is carried out on layer surface.
Preferably, the preparation method of aforesaid solid-state full-inorganic electrochomeric glass, wherein said oxygenChanging lithium target is obtained by lithia powder preparation.
Preferably, the preparation method of aforesaid solid-state full-inorganic electrochomeric glass, wherein said profitPreparing dielectric substrate with reaction magnetocontrol sputtering lithium target comprises: pass into argon gas and air to vacuum chamber, keepThe ratio of oxygen and argon gas is 1:1-1:20, keeps operating air pressure 0.2-2Pa, starts to cause change to electricitySputter coating is carried out on chromatograph or ion storage surface.
Preferably, the preparation method of aforesaid solid-state full-inorganic electrochomeric glass, wherein said electricityThe thickness that causes the dielectric substrate of photo chromic glass is 5-200nm, and the transmitance in visible-range is greater than80％。
By technique scheme, solid-state full-inorganic electrochomeric glass of the present invention and preparation method thereof extremelyThere is less following advantages:
1, lithia target of the present invention obtains by the higher lithia powder preparation of purity, has avoidedSecondary pollution;
2, the dielectric substrate of electrochomeric glass of the present invention is amorphous lithia, is conducive to Li+Embedding and extraction, can not cause the change of electrolyte structure and composition, thereby improve its electrolyteThe ionic conductance of layer, the cycle life that has extended electrochomeric glass;
3, preparation method of the present invention is simple, easy operating.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, of the present invention in order to better understandTechnological means, and can being implemented according to the content of description, below with preferred embodiment of the present inventionAnd coordinate accompanying drawing to be described in detail as follows.
Brief description of the drawings
Fig. 1 is the structural representation of the solid-state full-inorganic electrochomeric glass of the embodiment of the present invention 1.
Fig. 2 is solid-state full-inorganic electrochomeric glass cycle-index and the transmitance of the embodiment of the present invention 1Relation.
Fig. 3 is solid-state full-inorganic electrochomeric glass cycle-index and the transmitance of the embodiment of the present invention 2Relation.
Detailed description of the invention
Technological means and the merit taked for reaching predetermined goal of the invention for further setting forth the present inventionEffect, below in conjunction with accompanying drawing and preferred embodiment, to causing completely without electromechanics for solid-state of proposing according to the present inventionIts detailed description of the invention of electrolyte of variable color device and preparation method thereof, feature and effect thereof, say in detailBright as after. In following explanation, different " embodiment " or " embodiment " refer to not necessarilySame embodiment. In addition, the special characteristic in one or more embodiment or feature can be by any suitable shapesFormula combination.
Embodiments of the invention propose a kind of solid-state full-inorganic electrochomeric glass, and its structure comprises glassSubstrate and be deposited on successively transparency conducting layer on glass substrate, electrochromic layer, dielectric substrate,Ion storage, transparency conducting layer, the lithia film that described dielectric substrate is amorphous structure.Described transparency conducting layer is tin-doped indium oxide or fluorine-doped tin oxide, and described electrochromic layer is oxygenChange W film, described ion storage is the oxide of nickel tungsten. The electrolysis of described electrochomeric glassThe thickness of matter layer is 5-200nm, and the transmitance in visible-range is greater than 80%.
Embodiments of the invention also propose a kind of preparation method of solid-state full-inorganic electrochomeric glass, instituteThe dielectric substrate of the electrochomeric glass of stating is by the electrochromic layer described or ion storage profitMake with magnetron sputtering lithia target or magnetron sputtering lithium target; The described magnetron sputtering lithia target that utilizesPreparing dielectric substrate comprises: pass into argon gas to vacuum chamber, the flow of controlling argon gas is 10-50sccm, protectsHold operating air pressure 0.2-2Pa, start to carry out sputter coating to electrochromic layer or ion storage surface;Described lithia target is obtained by lithia powder preparation; Described utilizes the preparation of magnetron sputtering lithium target electricSeparating matter layer comprises: pass into argon gas and air to vacuum chamber, keeping the ratio of oxygen and argon gas is 1:1-1:3, keep operating air pressure 0.2-2Pa, start to carry out sputter to electrochromic layer or ion storage surfacePlated film.
Embodiment 1
Complete after the coating process of electrochromic layer tungsten oxide of solid-state full-inorganic electrochomeric glass,Utilize magnetron sputtering lithia target to prepare lithia thin-film electrolyte in tungsten oxide layer, pass into vacuum chamberArgon gas, the flow of controlling argon gas is 20sccm, keeps operating air pressure 0.4Pa, starts to tungsten oxide tableFace carries out sputter coating, and making lithia film thickness by control sputtering time is 20nm.
The cycle-index of solid-state full-inorganic electrochomeric glass in the present embodiment and the relation of transmitance asShown in Fig. 2, in Fig. 2,1 is the state of fading, and 2 is coloured state, 4000 the after stain states of circulating with fadeState transmitance is stable.
Embodiment 2
Complete the coating process of ion storage nickel protoxide of solid-state full-inorganic electrochomeric glassAfter, utilize magnetron sputtering lithia target to prepare lithia thin-film electrolyte at nickel protoxide layer, to vacuumChamber passes into argon gas, and the flow of controlling argon gas is 30sccm, keeps operating air pressure 0.8Pa, starts to oxygenChange sub-nickel surface and carry out sputter coating, making lithia film thickness by control sputtering time is 35nm.
4000 after stain states of solid-state full-inorganic electrochomeric glass circulation in the present embodiment and the state of fadingTransmitance is stable.
Embodiment 3
Complete after the coating process of electrochromic layer tungsten oxide of solid-state full-inorganic electrochomeric glass,Utilize magnetron sputtering lithium target to prepare lithia thin-film electrolyte in tungsten oxide layer, pass into argon gas to vacuum chamberAnd oxygen, keeping the ratio of argon gas and oxygen is 2:1, keeps operating air pressure 1.0Pa, starts to oxygenChange tungsten surface and carry out sputter coating, making lithia film thickness by control sputtering time is 100nm.
The cycle-index of solid-state full-inorganic electrochomeric glass in the present embodiment and the relation of transmitance asShown in Fig. 3, in Fig. 3,3 is the state of fading, and 4 is coloured state, 4000 the after stain states of circulating with fadeState transmitance is stable.
Embodiment 4
Complete the coating process of ion storage layer nickel protoxide of solid-state full-inorganic electrochomeric glassAfter, utilize magnetron sputtering lithium target to prepare lithia thin-film electrolyte at nickel protoxide layer, logical to vacuum chamberEnter argon gas and oxygen, keeping the ratio of argon gas and oxygen is 1.5:1, keeps operating air pressure 1.5Pa,Start to carry out sputter coating to nickel protoxide surface, make lithia film thick by controlling sputtering timeDegree is 90nm.
4000 after stain states of solid-state full-inorganic electrochomeric glass circulation in the present embodiment and the state of fadingTransmitance is stable.
The above, be only preferred embodiment of the present invention, not the present invention made to any formOn restriction, any simple modification of above embodiment being done according to technical spirit of the present invention, etc.With changing and modifying, all still belong in the scope of technical solution of the present invention.
Claims (8)
1. a solid-state full-inorganic electrochomeric glass, is characterized in that: described electrochomeric glassStructure comprise glass substrate and be deposited on successively transparency conducting layer, the electrochromism on glass substrateLayer, dielectric substrate, ion storage, transparency conducting layer, described dielectric substrate is amorphous structureLithia film.
2. solid-state full-inorganic electrochomeric glass according to claim 1, is characterized in that instituteThe transparency conducting layer of stating is tin-doped indium oxide or fluorine-doped tin oxide, and described electrochromic layer is oxidationW film, described ion storage is the oxide of nickel tungsten.
3. according to the solid-state full-inorganic electrochomeric glass described in claim 1-2 any one, its featureBe, the thickness of the dielectric substrate of described electrochomeric glass is 5-200nm, in visible-rangeTransmitance be greater than 80%.
4. a preparation method for solid-state full-inorganic electrochomeric glass, is characterized in that, described electricityThe dielectric substrate that causes photo chromic glass is to utilize magnetic control by the electrochromic layer described or ion storageSputter lithia target or reaction magnetocontrol sputtering lithium target make.
5. the preparation method of solid-state full-inorganic electrochomeric glass according to claim 4, its spyLevy and be, described utilize magnetron sputtering lithia target to prepare dielectric substrate to comprise: pass into vacuum chamberArgon gas, the flow of controlling argon gas is 10-50sccm, keeps operating air pressure 0.2-2Pa, starts to cause to electricitySputter coating is carried out on photochromic layer or ion storage surface.
6. the preparation method of solid-state full-inorganic electrochomeric glass according to claim 5, its spyLevy and be, described lithia target is obtained by lithia powder preparation.
7. the preparation method of solid-state full-inorganic electrochomeric glass according to claim 4, its spyLevy and be, described utilize reaction magnetocontrol sputtering lithium target to prepare dielectric substrate to comprise: pass into vacuum chamberArgon gas and air, keeping the ratio of oxygen and argon gas is 1:1-1:20, keeps operating air pressure 0.2-2Pa,Start to carry out sputter coating to electrochromic layer or ion storage surface.
8. according to the preparation side of the solid-state full-inorganic electrochomeric glass described in claim 4-7 any oneMethod, is characterized in that, the thickness of the dielectric substrate of described electrochomeric glass is 5-200nm, canSee that the transmitance in optical range is greater than 80%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950740A (en) * | 2017-05-02 | 2017-07-14 | 东旭（昆山）显示材料有限公司 | Display panel, display and the method for manufacturing display panel |
| CN107315298A (en) * | 2017-07-07 | 2017-11-03 | 中国航发北京航空材料研究院 | A kind of brown electrochromism charge storage electrode and preparation method |
| CN107604334A (en) * | 2017-09-21 | 2018-01-19 | 中国建筑材料科学研究总院 | Nickel-tungsten oxide film and preparation method 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 |
| CN109143714A (en) * | 2018-08-23 | 2019-01-04 | 中国建筑材料科学研究总院有限公司 | A kind of electrochromic device and preparation method thereof |
| CN111176046A (en) * | 2018-11-12 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | Lithium cobaltate film and preparation method and application thereof |
| CN112028483A (en) * | 2020-08-21 | 2020-12-04 | 江苏黄金屋光学眼镜有限公司 | Processing technology of dustproof color-changeable lens |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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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| CN106950740A (en) * | 2017-05-02 | 2017-07-14 | 东旭（昆山）显示材料有限公司 | Display panel, display and the method for manufacturing display panel |
| CN107315298A (en) * | 2017-07-07 | 2017-11-03 | 中国航发北京航空材料研究院 | A kind of brown electrochromism charge storage electrode and preparation method |
| CN107315298B (en) * | 2017-07-07 | 2020-04-28 | 中国航发北京航空材料研究院 | Brown electrochromic charge storage electrode and preparation method thereof |
| CN107604334A (en) * | 2017-09-21 | 2018-01-19 | 中国建筑材料科学研究总院 | Nickel-tungsten oxide film and preparation method thereof |
| CN109143714A (en) * | 2018-08-23 | 2019-01-04 | 中国建筑材料科学研究总院有限公司 | A kind of electrochromic device and preparation method thereof |
| CN109143714B (en) * | 2018-08-23 | 2021-09-28 | 中国建筑材料科学研究总院有限公司 | Electrochromic device and preparation method thereof |
| CN111176046A (en) * | 2018-11-12 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | Lithium cobaltate film and preparation method and application thereof |
| CN112028483A (en) * | 2020-08-21 | 2020-12-04 | 江苏黄金屋光学眼镜有限公司 | Processing technology of dustproof color-changeable lens |
| 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 |
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| CN105607374B (en) | 2019-09-20 |
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