CN105607374B - Solid-state full-inorganic electrochomeric glass and preparation method thereof - Google Patents
Solid-state full-inorganic electrochomeric glass and preparation method thereof Download PDFInfo
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- CN105607374B CN105607374B CN201610144186.7A CN201610144186A CN105607374B CN 105607374 B CN105607374 B CN 105607374B CN 201610144186 A CN201610144186 A CN 201610144186A CN 105607374 B CN105607374 B CN 105607374B
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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 present invention relates to a kind of solid-state full-inorganic electrochomeric glass and preparation method thereof, it is characterized by: the structure of the electrochomeric glass includes glass substrate and is sequentially depositing transparency conducting layer, electrochromic layer, electrolyte layer, ion storage, transparency conducting layer on a glass substrate, the electrolyte layer is the lithia film of amorphous structure.The electrolyte layer of electrochomeric glass of the invention is amorphous lithia, be conducive to the insertion and extraction of Li+, it not will cause the change of electrolyte structure and composition, to improve the ionic conductivity of its electrolyte layer, extend the cycle life of electrochomeric glass.
Description
Technical field
The present invention relates to a kind of electrochomeric glass, more particularly to a kind of solid-state full-inorganic electrochomeric glass and its system
Preparation Method.
Background technique
Electrochromism phenomenon refers to material under DC Electric Field, along with the injection of H+, Li+, Na+ plasma or de-
Electrochemical reaction process occurs when out, thus optical property generates reversible change, to realize to light reflection, transmission, absorb
Regulation.Electrochromic device is known as by the device that electrochromic material is made into, electrochromic device has efficient, low consumption, nothing
The advantages that pollution, intelligence, before all having wide application on the windowpane of building, visor, aircraft, steamer etc. after automobile
Scape.Electrochomeric glass is common electrochromism device, and wherein the electrolyte layer of electrochomeric glass is electrochromic effect institute
Need the transmission channel of ion.There is presently no the building light modulation solid-state full-inorganic electrochromism glass for haveing excellent performance, changing colour stable
Glass high-volume puts goods on the market, and main cause is that the electrolyte layer of electrochomeric glass used at present has the following problems: first is that
Ionic conductivity is lower, causes discoloration rate slower, second is that electrolyte layer is after recycling a period of time, Li+ causes electrolyte group
It changes at, structure, leads to the reduction of Li+ mobility, change colour amplitude reduction.
Summary of the invention
It is a primary object of the present invention to, a kind of New Solid full-inorganic electrochomeric glass and preparation method thereof is provided,
The technical problem to be solved is that keeping the conductivity of its electrolyte layer high, thus more suitable for practical.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.It proposes according to the present invention
A kind of solid-state full-inorganic electrochomeric glass, the structure of the electrochomeric glass includes glass substrate and is sequentially depositing
Transparency conducting layer, electrochromic layer, electrolyte layer, ion storage, transparency conducting layer on a glass substrate, the electrolysis
Matter layer is the lithia film of amorphous structure.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, solid-state full-inorganic electrochomeric glass above-mentioned, wherein the transparency conducting layer is tin dope oxidation
Indium or fluorine-doped tin oxide, the electrochromic layer are tungsten oxide film, and the ion storage is the oxide of nickel tungsten.
Preferably, solid-state full-inorganic electrochomeric glass above-mentioned, wherein the electrolyte layer of the electrochomeric glass
With a thickness of 5-200nm, transmitance in visible-range is greater than 80%.
Also the following technical solution is employed for the object of the invention to solve the technical problems to realize.It proposes according to the present invention
A kind of solid-state full-inorganic electrochomeric glass preparation method, the electrolyte layer of the electrochomeric glass is by institute
The electrochromic layer or ion storage stated are made using magnetron sputtering lithia target or reaction magnetocontrol sputtering lithium target.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the preparation method of solid-state full-inorganic electrochomeric glass above-mentioned, wherein described utilizes magnetron sputtering
It includes: to be passed through argon gas to vacuum chamber that lithia target, which prepares electrolyte layer, and the flow for controlling argon gas is 10-50sccm, keeps work
Air pressure 0.2-2Pa starts to carry out sputter coating to electrochromic layer or ion storage layer surface.
Preferably, the preparation method of solid-state full-inorganic electrochomeric glass above-mentioned, wherein the lithia target is by oxygen
Change lithium powder to be prepared.
Preferably, the preparation method of solid-state full-inorganic electrochomeric glass above-mentioned, wherein described utilizes reaction magnetic control
It includes: to be passed through argon gas and air to vacuum chamber that sputtering lithium target, which prepares electrolyte layer, and keeping the ratio of oxygen and argon gas is 1:1-1:
20, operating air pressure 0.2-2Pa is kept, starts to carry out sputter coating to electrochromic layer or ion storage layer surface.
Preferably, the preparation method of solid-state full-inorganic electrochomeric glass above-mentioned, wherein the electrochomeric glass
Electrolyte layer with a thickness of 5-200nm, transmitance in visible-range is greater than 80%.
By above-mentioned technical proposal, solid-state full-inorganic electrochomeric glass of the present invention and preparation method thereof at least has following
Advantage:
1, lithia target of the invention is prepared by the higher oxidation lithium powder of purity, avoids secondary pollution；
2, the electrolyte layer of electrochomeric glass of the invention is amorphous lithia, is conducive to the insertion and pumping of Li+
Out, it not will cause the change of electrolyte structure and composition, to improve the ionic conductivity of its electrolyte layer, extend electroluminescent
The cycle life of photo chromic glass；
3, preparation method of the invention is simple, easily operated.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the solid-state full-inorganic electrochomeric glass of the embodiment of the present invention 1.
Fig. 2 is the relationship of solid-state the full-inorganic electrochomeric glass cycle-index and transmitance of the embodiment of the present invention 1.
Fig. 3 is the relationship of solid-state the full-inorganic electrochomeric glass cycle-index and transmitance of the embodiment of the present invention 2.
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to the electrolyte proposed according to the present invention for solid-state full-inorganic electrochromic device and its preparation
Method its specific embodiment, feature and its effect, detailed description is as follows.In the following description, different " embodiment " or
What " embodiment " referred to is not necessarily the same embodiment.In addition, the special characteristic or feature in one or more embodiments can be by any
Suitable form combination.
The embodiment of the present invention proposes a kind of solid-state full-inorganic electrochomeric glass, structure include glass substrate and according to
Transparency conducting layer, electrochromic layer, electrolyte layer, ion storage, the transparency conducting layer of secondary deposition on a glass substrate, it is described
Electrolyte layer be amorphous structure lithia film.The transparency conducting layer is that tin-doped indium oxide or Fluorin doped aoxidize
Tin, the electrochromic layer are tungsten oxide film, and the ion storage is the oxide of nickel tungsten.The electrochomeric glass
Electrolyte layer with a thickness of 5-200nm, transmitance in visible-range is greater than 80%.
The embodiment of the present invention also proposes a kind of preparation method of solid-state full-inorganic electrochomeric glass, the electroluminescent change
The electrolyte layer of color glass is by utilizing magnetron sputtering lithia target or magnetic in the electrochromic layer or ion storage
Control sputtering lithium target is made；It includes: to be passed through argon gas to vacuum chamber that the utilization magnetron sputtering lithia target, which prepares electrolyte layer, control
The flow of argon gas processed is 10-50sccm, keeps operating air pressure 0.2-2Pa, starts to electrochromic layer or ion storage layer surface
Carry out sputter coating；The lithia target is prepared by oxidation lithium powder；Described prepares electricity using magnetron sputtering lithium target
Solution matter layer includes: to be passed through argon gas and air to vacuum chamber, and keeping the ratio of oxygen and argon gas is 1:1-1:3, keeps operating air pressure
0.2-2Pa starts to carry out sputter coating to electrochromic layer or ion storage layer surface.
Embodiment 1
After completing the coating process of electrochromic layer tungsten oxide of solid-state full-inorganic electrochomeric glass, splashed using magnetic control
It penetrates lithia target and prepares lithia thin-film electrolyte in tungsten oxide layer, be passed through argon gas to vacuum chamber, the flow for controlling argon gas is
20sccm keeps operating air pressure 0.4Pa, starts to carry out sputter coating to tungsten oxide surface, makes oxygen by controlling sputtering time
Change lithium film thickness is 20nm.
The cycle-index of solid-state full-inorganic electrochomeric glass and the relationship of transmitance in the present embodiment as shown in Fig. 2,
1 is colour fading state in Fig. 2, and 2 be coloured state, recycles 4000 after stain states and colour fading state transmitance is stablized.
Embodiment 2
After completing the coating process of ion storage nickel protoxide of solid-state full-inorganic electrochomeric glass, magnetic control is utilized
It sputters lithia target and prepares lithia thin-film electrolyte in nickel protoxide layer, be passed through argon gas to vacuum chamber, control the flow of argon gas
For 30sccm, operating air pressure 0.8Pa is kept, starts to carry out sputter coating to nickel protoxide surface, is made by controlling sputtering time
Obtaining lithia film thickness is 35nm.
Solid-state full-inorganic electrochomeric glass in the present embodiment recycles 4000 after stain states and colour fading state transmitance is steady
It is fixed.
Embodiment 3
After completing the coating process of electrochromic layer tungsten oxide of solid-state full-inorganic electrochomeric glass, splashed using magnetic control
It penetrates lithium target and prepares lithia thin-film electrolyte in tungsten oxide layer, be passed through argon gas and oxygen to vacuum chamber, keep argon gas and oxygen
Ratio is 2:1, keeps operating air pressure 1.0Pa, starts to carry out sputter coating to tungsten oxide surface, is made by controlling sputtering time
Lithia film thickness is 100nm.
The cycle-index of solid-state full-inorganic electrochomeric glass and the relationship of transmitance in the present embodiment as shown in figure 3,
3 be colour fading state in Fig. 3, and 4 be coloured state, recycles 4000 after stain states and colour fading state transmitance is stablized.
Embodiment 4
After completing the coating process of ion storage layer nickel protoxide of solid-state full-inorganic electrochomeric glass, magnetic control is utilized
It sputters lithium target and prepares lithia thin-film electrolyte in nickel protoxide layer, be passed through argon gas and oxygen to vacuum chamber, keep argon gas and oxygen
The ratio of gas is 1.5:1, keeps operating air pressure 1.5Pa, starts to carry out sputter coating to nickel protoxide surface, be sputtered by control
Time makes lithia film thickness be 90nm.
Solid-state full-inorganic electrochomeric glass in the present embodiment recycles 4000 after stain states and colour fading state transmitance is steady
It is fixed.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, this hair is still fallen within
In the range of bright technical solution.
Claims (6)
1. a kind of solid-state full-inorganic electrochomeric glass, it is characterised in that: the structure of the electrochomeric glass includes glass
Substrate and it is sequentially depositing transparency conducting layer on a glass substrate, electrochromic layer, electrolyte layer, ion storage, transparent
Conductive layer, the electrolyte layer are the lithia film of amorphous structure；The electrolyte layer with a thickness of 5-200nm,
Transmitance in visible-range is greater than 80%.
2. solid-state full-inorganic electrochomeric glass according to claim 1, which is characterized in that the transparency conducting layer is
Tin-doped indium oxide or fluorine-doped tin oxide, the electrochromic layer are tungsten oxide film, and the ion storage is nickel tungsten
Oxide.
3. a kind of preparation method of solid-state full-inorganic electrochomeric glass of any of claims 1 or 2, which is characterized in that described
Electrochomeric glass electrolyte layer be by the electrochromic layer or ion storage utilize magnetron sputtering oxidation
Lithium target or reaction magnetocontrol sputtering lithium target are made；The electrolyte layer of the electrochomeric glass with a thickness of 5-200nm, visible
Transmitance in optical range is greater than 80%.
4. the preparation method of solid-state full-inorganic electrochomeric glass according to claim 3, which is characterized in that the benefit
Preparing electrolyte layer with magnetron sputtering lithia target includes: to be passed through argon gas to vacuum chamber, and the flow for controlling argon gas is 10-
50sccm keeps operating air pressure 0.2-2Pa, starts to carry out sputter coating to electrochromic layer or ion storage layer surface.
5. the preparation method of solid-state full-inorganic electrochomeric glass according to claim 4, which is characterized in that the oxygen
Change lithium target to be prepared by oxidation lithium powder.
6. the preparation method of solid-state full-inorganic electrochomeric glass according to claim 3, which is characterized in that the benefit
Preparing electrolyte layer with reaction magnetocontrol sputtering lithium target includes: to be passed through argon gas and air to vacuum chamber, keeps the ratio of oxygen and argon gas
Example is 1:1-1:3, keeps operating air pressure 0.2-2Pa, starts to carry out sputter coating to electrochromic layer or ion storage layer surface.
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| CN201610144186.7A CN105607374B (en) | 2016-03-14 | 2016-03-14 | Solid-state full-inorganic electrochomeric glass and preparation method thereof |
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Families Citing this family (8)
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| 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 |
| 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 |
| 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 |
| 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 |
| CN111176046B (en) * | 2018-11-12 | 2021-04-16 | 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 |
| CN113204146B (en) * | 2021-05-07 | 2023-04-25 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device with water vapor as electrolyte and preparation method thereof |
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| US4390460A (en) * | 1980-09-29 | 1983-06-28 | Hitachi, Ltd. | Lithium oxide based amorphous material and process for preparation thereof |
| CN103771724A (en) * | 2012-10-19 | 2014-05-07 | 中国南玻集团股份有限公司 | All-solid-state film electrochromic glass and preparation method thereof |
| CN104834145A (en) * | 2015-03-30 | 2015-08-12 | 上方能源技术(杭州)有限公司 | Laminated electrochromism glass and application thereof |
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| CN204667022U (en) * | 2015-03-30 | 2015-09-23 | 上方能源技术(杭州)有限公司 | A kind of lamination electrochomeric glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8031389B2 (en) * | 2008-10-01 | 2011-10-04 | Soladigm, Inc. | Reflection-controllable electrochromic device using a base metal as a transparent conductor |
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2016
- 2016-03-14 CN CN201610144186.7A patent/CN105607374B/en active Active
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| US4390460A (en) * | 1980-09-29 | 1983-06-28 | Hitachi, Ltd. | Lithium oxide based amorphous material and process for preparation thereof |
| CN103771724A (en) * | 2012-10-19 | 2014-05-07 | 中国南玻集团股份有限公司 | All-solid-state film electrochromic glass and preparation method thereof |
| CN204595399U (en) * | 2015-02-16 | 2015-08-26 | 浙江上方电子装备有限公司 | A kind of electrochomeric glass |
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