CN108803183A - A kind of bilayer full-inorganic electrochromic device and preparation method thereof - Google Patents
A kind of bilayer full-inorganic electrochromic device and preparation method thereof Download PDFInfo
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- CN108803183A CN108803183A CN201810346457.6A CN201810346457A CN108803183A CN 108803183 A CN108803183 A CN 108803183A CN 201810346457 A CN201810346457 A CN 201810346457A CN 108803183 A CN108803183 A CN 108803183A
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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
- G02F1/1525—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 characterised by a particular ion transporting layer, e.g. 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
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Abstract
The present invention relates to a kind of double-deck full-inorganic electrochromic device and preparation method thereof, the bilayer full-inorganic electrochromic device includes the lower separation layer set gradually from top to bottom, lower ion barrier, lower transparency conducting layer B, lower ion storage, lower sheath, lower electrochromic layer, lower transparency conducting layer A, substrate, upper transparency conducting layer A, upper electrochromic layer, upper sheath, upper ion storage, upper transparency conducting layer B, upper ion barrier and upper separation layer；The bilayer full-inorganic electrochromic device can form the double-deck full-inorganic electrochromic device by two-sided magnetron sputtering membrane process in substrate both sides.The advantage of the invention is that：Bilayer full-inorganic electrochromic device of the invention, can will be seen that light percent of pass is adjusted to 50%~0.01%, and then can greatly reduce the transmitance of coloured state, achieve the effect that opaque privacy；The present invention is lower compared to coating cost twice by two-sided magnetron sputtering membrane process.
Description
Technical field
The invention belongs to electrochromic device field, more particularly to a kind of double-deck full-inorganic electrochromic device and its preparation
Method.
Background technology
Electrochromism refers to optical properties（Reflectivity, transmitance, absorptivity etc.）Occur under the action of extra electric field steady
Calmly, the phenomenon that reversible color change.The development of electrochromism technology has more than 40 years, electrochromic device
（Electrochromic Device, ECD）Since it has, tool low to continuous adjustability, the energy loss of transmitted intensity
There is the features such as open circuit memory function, it is hidden without dizzy rearview mirror, weaponry in smart window, display, spacecraft temperature control modulation, automobile
The fields such as body have broad application prospects.
Electrochromic device is generally 5 layers of structure：Transparent conductive electrode layer, electrochromic material layer, electrolyte layer, ion
Accumulation layer and another conductive electrode layer, as 107085339 A of patent CN disclose a kind of preparation of full-solid electrochromic device
Method, wherein be mentioned to full-solid electrochromic device, the device is successively by ito glass substrate, electrochromic layer, electrolyte
Layer, ion storage and top layer ITO compositions, i.e., existing full-solid electrochromic device are generally single layer full-inorganic electronic color-changing
Device, transmitance are not to be not through light completely, do not have the effect of complete privacy under strong light 60% ~ 1%.
Therefore, research and development are a kind of can greatly reduce the transmitance of coloured state, and reach the bilayer of opaque privacy effect
Full-inorganic electrochromic device and preparation method thereof is necessary.
Invention content
The transmitance of coloured state can be greatly reduced the technical problem to be solved in the present invention is to provide a kind of, and is reached not
Double-deck full-inorganic electrochromic device of light transmission privacy effect and preparation method thereof.
In order to solve the above technical problems, the technical scheme is that：A kind of bilayer full-inorganic electrochromic device, wound
New point is：The bilayer full-inorganic electrochromic device includes the lower separation layer set gradually from top to bottom, lower ion barrier
It is layer, lower transparency conducting layer B, lower ion storage, lower sheath, lower electrochromic layer, lower transparency conducting layer A, substrate, upper transparent
Conductive layer A, upper electrochromic layer, upper sheath, upper ion storage, upper transparency conducting layer B, upper ion barrier and upper isolation
Layer.
A kind of preparation method of the above-mentioned double-deck full-inorganic electrochromic device, innovative point are：The preparation method
Include the following steps：
（1）Transparency conducting layer A and lower transparency conducting layer A in preparation：Using clean high transparency material as substrate, and pass through Vacuum Deposition
Film, evaporation coating or sol gel process are respectively formed the high temperature that a layer thickness is 20nm~100nm on the upper and lower surface of substrate
Transparent conductive film, and then it is respectively formed upper transparency conducting layer A and lower transparency conducting layer A on the upper and lower surface of substrate；
（2）Electrochromic layer and lower electrochromic layer in preparation：Using tungsten as target, oxygen is working gas, oxygen doping
Ratio is 2%~50% or with the ceramics of oxide for target, using two-sided magnetron sputtering membrane process upper transparency conducting layer A's
Upper surface and the lower surface of lower transparency conducting layer A prepare the upper electrochromic layer and lower electrochromism that film thickness is 200nm~600nm
Layer；
（3）Sheath and lower sheath in preparation：By plated film mode in the upper surface of upper electrochromic layer and lower electrochromism
The lower surface of layer plates the metal-lithium ion layer that a tunic thickness is 10nm~300nm respectively, so formed upper sheath and under from
Sublayer；
（4）Ion storage and lower ion storage in preparation：Using tungsten as target, oxygen is working gas, oxygen doping
Ratio is 0.5%~20% or with the ceramics of oxide for target, using two-sided magnetron sputtering membrane process in the upper of upper sheath
Surface and the lower surface of lower sheath prepare the upper ion storage and lower ion storage that film thickness is 150nm~650nm；
（5）Transparency conducting layer B and lower transparency conducting layer B in preparation：Existed by vacuum coating, evaporation coating or sol gel process
The upper surface of upper ion storage and the lower surface of lower ion storage are respectively formed the height that a layer thickness is 200nm~400nm
Warm transparent conductive film, and then form upper transparency conducting layer B and lower transparency conducting layer B；
（6）Ion barrier and lower ion barrier in preparation：Using Si/SiAl as target, using two-sided magnetron sputtering plating work
It is 20nm~80nm that skill deposits a layer thickness respectively in the lower surface of the upper surface of upper transparency conducting layer B and lower transparency conducting layer B
Upper ion barrier and lower ion barrier；
（7）Separation layer and lower separation layer in preparation：It is target with one or more of Si, Ti, Al or B, using two-sided magnetic control
Sputter coating process deposits a layer thickness respectively in the lower surface of the upper surface of upper ion barrier and lower ion barrier
The upper separation layer of 100nm~1000nm and lower separation layer.
Further, the step（1）In transparent conductive film select square resistance be 5~15ohm, it is seen that light is average
The transparent conductive film of transmitance > 83%, and the transparent conductive film of the transparency conducting layer selects one kind in ITO or AZO
Or it is several.
Further, the step（2）In the electrochomeric films of upper electrochromic layer and lower electrochromic layer select
WO3、MO3、Nb2O5Or TiO2One or more of.
Further, the step（3）In metal-lithium ion layer in doped with one kind in tantalum, niobium or cobalt material or several
Kind.
Further, the step（4）In the ion storage film of upper ion storage and lower ion storage select
NiOx or IrO2One or more of.
Further, the step（5）In transparent conductive film select square resistance be 5~15ohm, it is seen that light is average
The transparent conductive film of transmitance > 80%, and the transparent conductive film of the transparency conducting layer selects one kind in ITO or AZO
Or it is several.
Further, the step（6）In the ion barrier film of upper ion barrier and lower ion barrier select
SiOx、Nb2O5、Ta2O5Or one or more of SiAlOx.
The advantage of the invention is that：
（1）Bilayer full-inorganic electrochromic device of the invention, transparency conducting layer A, electroluminescent change are symmetrically arranged in the both sides of substrate
Chromatograph, sheath, ion storage layer, transparency conducting layer B, ion barrier and separation layer form the double-deck full-inorganic electrochromism
Device can will be seen that light percent of pass is adjusted to 50%~0.01%, and then can greatly reduce the transmitance of coloured state, reach
The effect of opaque privacy；
（2）The preparation method of bilayer full-inorganic electrochromic device of the invention, passes through two-sided magnetron sputtering membrane process, Ke Yi
Substrate both sides form the double-deck full-inorganic electrochromic device, lower compared to coating cost twice；In addition, the process route of the present invention
The products such as compatible plane, curved surface, flexibility are can be very good, realize the diversification of product；
（3）The preparation method of bilayer full-inorganic electrochromic device of the invention, wherein electrochromic layer using tungsten as target,
Oxygen is working gas, and oxygen doping ratio is 2%~50% progress plated film；Using tungsten as target, oxygen is ion storage
Working gas, oxygen doping ratio are 0.5%~20% to carry out plated film, can be modulated by changing the ratio of oxygen doping it is double-deck completely without
The optical transmittance and electrochromic property of machine electrochromic device；
（4）The preparation method of bilayer full-inorganic electrochromic device of the invention, wherein doped with tantalum, niobium in metal-lithium ion layer
Or one or more of cobalt material, the characteristic of sheath can be effectively improved.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the structural schematic diagram of the double-deck full-inorganic electrochromic device of the present invention.
Specific implementation mode
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment
The present embodiment bilayer full-inorganic electrochromic device, as shown in Figure 1, the double-deck full-inorganic electrochromic device includes certainly
Lower separation layer 1, lower ion barrier 2, lower transparency conducting layer B 3, lower ion storage 4, the lower ion set gradually under above
Layer 5, lower electrochromic layer 6, lower transparency conducting layer A 7, substrate 8, upper transparency conducting layer A 9, upper electrochromic layer 10, upper ion
Layer 11, upper ion storage 12, upper transparency conducting layer B 13, upper ion barrier 14 and upper separation layer 15.
The preparation method of the present embodiment bilayer full-inorganic electrochromic device, the preparation method include the following steps：
（1）Transparency conducting layer A 9 and lower transparency conducting layer A 7 in preparation：Using clean organic glass as substrate 8, and by true
It is 20nm~100nm that empty plated film, evaporation coating or sol gel process are respectively formed a layer thickness on the upper and lower surface of substrate 8
Square resistance be 5~15ohm, it is seen that the transparent conductive film of light mean transmissivity > 83%, so substrate 8 it is upper,
Lower surface is respectively formed transparency conducting layer A 9 and lower transparency conducting layer A 7；
（2）Electrochromic layer 10 and lower electrochromic layer 6 in preparation：Using tungsten as target, oxygen is working gas, and oxygen is mixed
Miscellaneous ratio is 2%~50%, using two-sided magnetron sputtering membrane process in the upper surface of upper transparency conducting layer A 9 and lower electrically conducting transparent
The lower surface of layer A 7 prepares the upper electrochromic layer 10 and lower electrochromic layer 6 that film thickness is 200nm~600nm, and powers on mutagens
The electrochomeric films of chromatograph 10 and lower electrochromic layer 6 select WO3；
（3）Sheath 11 and lower sheath 5 in preparation：It is electroluminescent under in the upper surface of upper electrochromic layer 10 by plated film mode
The lower surface of photochromic layer 6 plates the metal-lithium ion layer that a tunic thickness is 10nm~300nm respectively, and then forms upper sheath 11
With lower sheath 5；In order to effectively improve the characteristic of sheath, doped with tantalum, niobium or cobalt material in metal-lithium ion layer
One or more of；
（4）Ion storage 12 and lower ion storage 4 in preparation：Using tungsten as target, oxygen is working gas, and oxygen is mixed
Miscellaneous ratio is 0.5%~20%, using two-sided magnetron sputtering membrane process under the upper surface of upper sheath 11 and lower sheath 5
Surface prepares the upper ion storage 12 and lower ion storage 4 that film thickness is 150nm~650nm, and 12 He of upper ion storage
The ion storage film of lower ion storage 4 selects NiOx；
（5）Transparency conducting layer 13 and lower transparency conducting layer 3 in preparation：Pass through vacuum coating, evaporation coating or sol gel process
It is 200nm~400nm to be respectively formed a layer thickness in the lower surface of the upper surface of upper ion storage 12 and lower ion storage 4
Square resistance be 5~15ohm, it is seen that the transparent conductive film of light mean transmissivity > 80%, and then form upper transparent lead
Electric layer B 13 and lower transparency conducting layer B 3；
（6）Ion barrier 14 and lower ion barrier 2 in preparation：Using Si/SiAl as target, using two-sided magnetron sputtering plating
It is 20nm that technique deposits a layer thickness respectively in the lower surface of the upper surface of upper transparency conducting layer B 13 and lower transparency conducting layer B 3
The upper ion barrier 14 of~80nm and lower ion barrier 2, and the ion of upper ion barrier 14 and lower ion barrier 2 hinders
It keeps off film and selects SiOx；
（7）Separation layer 15 and lower separation layer 1 in preparation：It is target with one or more of Si, Ti, Al or B, using double-side magnetic
Control sputter coating process deposits a layer thickness in the lower surface of the upper surface of upper ion barrier and lower ion barrier and is respectively
The upper separation layer 15 of 100nm~1000nm and lower separation layer 1.
For substrate 8 in the present embodiment in addition to selecting organic glass, it is substrate 8 that any one high transparency material, which also can be selected,；It is real
Apply the mixing that AZO or ITO and AZO also can be selected in the transparent conductive film in example；Upper electrochromic layer 10 in embodiment is under
MO also can be selected in the electrochomeric films of electrochromic layer 63、Nb2O5、TiO2In one kind or WO3、MO3、Nb2O5、TiO2In
It is several；IrO also can be selected in the ion storage film of upper ion storage 12 and lower ion storage 4 in embodiment2Or NiOx with
IrO2Mixing；Nb also can be selected in the ion barrier film of upper ion barrier 14 and lower ion barrier 2 in embodiment2O5、
Ta2O5, one kind or SiOx, Nb in SiAlOx2O5、Ta2O5, with it is several in SiAlOx.
The double-deck full-inorganic electrochromic device prepared through this embodiment, it is seen that light percent of pass is 50%~0.01%,
And then the transmitance of coloured state can be greatly reduced, achieve the effect that opaque privacy.
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (8)
1. a kind of bilayer full-inorganic electrochromic device, it is characterised in that：The bilayer full-inorganic electrochromic device includes certainly
It is upper and under set gradually lower separation layer, lower ion barrier, lower transparency conducting layer B, lower ion storage, lower sheath, under
Electrochromic layer, lower transparency conducting layer A, substrate, upper transparency conducting layer A, upper electrochromic layer, upper sheath, upper ion storage
Layer, upper transparency conducting layer B, upper ion barrier and upper separation layer.
2. a kind of preparation method of the double-deck full-inorganic electrochromic device described in claim 1, it is characterised in that：The preparation
Method includes the following steps：
（1）Transparency conducting layer A and lower transparency conducting layer A in preparation：Using clean high transparency material as substrate, and pass through Vacuum Deposition
Film, evaporation coating or sol gel process are respectively formed the high temperature that a layer thickness is 20nm~100nm on the upper and lower surface of substrate
Transparent conductive film, and then it is respectively formed upper transparency conducting layer A and lower transparency conducting layer A on the upper and lower surface of substrate；
（2）Electrochromic layer and lower electrochromic layer in preparation：Using tungsten as target, oxygen is working gas, oxygen doping
Ratio is 2%~50% or with the ceramics of oxide for target, using two-sided magnetron sputtering membrane process upper transparency conducting layer A's
Upper surface and the lower surface of lower transparency conducting layer A prepare the upper electrochromic layer and lower electrochromism that film thickness is 200nm~600nm
Layer；
（3）Sheath and lower sheath in preparation：By plated film mode in the upper surface of upper electrochromic layer and lower electrochromism
The lower surface of layer plates the metal-lithium ion layer that a tunic thickness is 10nm~300nm respectively, so formed upper sheath and under from
Sublayer；
（4）Ion storage and lower ion storage in preparation：Using tungsten as target, oxygen is working gas, oxygen doping
Ratio is 0.5%~20% or with the ceramics of oxide for target, using two-sided magnetron sputtering membrane process in the upper of upper sheath
Surface and the lower surface of lower sheath prepare the upper ion storage and lower ion storage that film thickness is 150nm~650nm；
（5）Transparency conducting layer B and lower transparency conducting layer B in preparation：Existed by vacuum coating, evaporation coating or sol gel process
The upper surface of upper ion storage and the lower surface of lower ion storage are respectively formed the height that a layer thickness is 200nm~400nm
Warm transparent conductive film, and then form upper transparency conducting layer B and lower transparency conducting layer B；
（6）Ion barrier and lower ion barrier in preparation：Using Si/SiAl as target, using two-sided magnetron sputtering plating work
It is 20nm~80nm that skill deposits a layer thickness respectively in the lower surface of the upper surface of upper transparency conducting layer B and lower transparency conducting layer B
Upper ion barrier and lower ion barrier；
（7）Separation layer and lower separation layer in preparation：It is target with one or more of Si, Ti, Al or B, using two-sided magnetic control
Sputter coating process deposits a layer thickness respectively in the lower surface of the upper surface of upper ion barrier and lower ion barrier
The upper separation layer of 100nm~1000nm and lower separation layer.
3. the preparation method of bilayer full-inorganic electrochromic device according to claim 2, it is characterised in that：The step
（1）In transparent conductive film select square resistance be 5~15ohm, it is seen that the electrically conducting transparent of light mean transmissivity > 83% is thin
Film, and the transparent conductive film of the transparency conducting layer selects one or more of ITO or AZO.
4. the preparation method of bilayer full-inorganic electrochromic device according to claim 2, it is characterised in that：The step
（2）In the electrochomeric films of upper electrochromic layer and lower electrochromic layer select WO3、MO3、Nb2O5Or TiO2In one kind or
It is several.
5. the preparation method of bilayer full-inorganic electrochromic device according to claim 2, it is characterised in that：The step
（3）In metal-lithium ion layer in doped with one or more of tantalum, niobium or cobalt material.
6. the preparation method of bilayer full-inorganic electrochromic device according to claim 2, it is characterised in that：The step
（4）In the ion storage film of upper ion storage and lower ion storage select NiOx or IrO2One or more of.
7. the preparation method of bilayer full-inorganic electrochromic device according to claim 2, it is characterised in that：The step
（5）In transparent conductive film select square resistance be 5~15ohm, it is seen that the electrically conducting transparent of light mean transmissivity > 80% is thin
Film, and the transparent conductive film of the transparency conducting layer selects one or more of ITO or AZO.
8. the preparation method of bilayer full-inorganic electrochromic device according to claim 2, it is characterised in that：The step
（6）In the ion barrier film of upper ion barrier and lower ion barrier select SiOx, Nb2O5、Ta2O5Or in SiAlOx
It is one or more of.
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| CN111286710A (en) * | 2020-03-30 | 2020-06-16 | 天津耀皮工程玻璃有限公司 | V for electrochromic-based glass2O5Preparation method of multi-layer ion storage layer |
| CN112987439A (en) * | 2019-12-14 | 2021-06-18 | 传奇视界有限公司 | Electrochromic glass and preparation method thereof |
| KR20220058589A (en) * | 2019-09-06 | 2022-05-09 | 난통 판후아 뉴 머티리얼즈 테크놀로지 컴퍼니 리미티드 | Electrochromic glass and its manufacturing method |
| 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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| CN112987439A (en) * | 2019-12-14 | 2021-06-18 | 传奇视界有限公司 | Electrochromic glass and preparation method thereof |
| CN111286710A (en) * | 2020-03-30 | 2020-06-16 | 天津耀皮工程玻璃有限公司 | V for electrochromic-based glass2O5Preparation method of multi-layer ion storage layer |
| CN111286710B (en) * | 2020-03-30 | 2022-08-05 | 天津耀皮工程玻璃有限公司 | V for electrochromic-based glass 2 O 5 Preparation method of multi-layer ion storage layer |
| 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 |
| CN116819842A (en) * | 2023-05-23 | 2023-09-29 | 浙江大学 | Ultraviolet erasable screen, preparation method, ultraviolet erasable system and method |
| CN116819842B (en) * | 2023-05-23 | 2024-05-28 | 浙江大学 | Ultraviolet erasable screen, preparation method, ultraviolet erasable system and method |
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Application publication date: 20181113 Assignee: Jiangsu prosperous Yingcai Technology Co.,Ltd. Assignor: NANTONG FANHUA NEW MATERIAL TECHNOLOGY Co.,Ltd. Contract record no.: X2022980008694 Denomination of invention: A double-layer all inorganic electrochromic device and its preparation method Granted publication date: 20220225 License type: Exclusive License Record date: 20220630 |