CN107390445A - A kind of total solids electrochromic device and preparation method thereof - Google Patents
A kind of total solids electrochromic device and preparation method thereof Download PDFInfo
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- CN107390445A CN107390445A CN201710483147.4A CN201710483147A CN107390445A CN 107390445 A CN107390445 A CN 107390445A CN 201710483147 A CN201710483147 A CN 201710483147A CN 107390445 A CN107390445 A CN 107390445A
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- 239000007787 solid Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010410 layer Substances 0.000 claims abstract description 400
- 239000011248 coating agent Substances 0.000 claims abstract description 120
- 238000000576 coating method Methods 0.000 claims abstract description 120
- 239000002346 layers by function Substances 0.000 claims abstract description 110
- 239000004020 conductor Substances 0.000 claims abstract description 68
- 150000002500 ions Chemical class 0.000 claims description 134
- 239000000203 mixture Substances 0.000 claims description 69
- 239000011521 glass Substances 0.000 claims description 57
- 239000000758 substrate Substances 0.000 claims description 46
- 239000011241 protective layer Substances 0.000 claims description 44
- 229910052751 metal Inorganic materials 0.000 claims description 39
- 239000002184 metal Substances 0.000 claims description 39
- 230000005540 biological transmission Effects 0.000 claims description 30
- 238000002310 reflectometry Methods 0.000 claims description 30
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical group O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 28
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 28
- DLJAAEQLNLSVPC-UHFFFAOYSA-N chromium(3+) oxonickel oxygen(2-) Chemical group [O-2].[Cr+3].[Ni]=O.[O-2].[O-2].[Cr+3] DLJAAEQLNLSVPC-UHFFFAOYSA-N 0.000 claims description 26
- 230000008859 change Effects 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 13
- 239000011701 zinc Substances 0.000 claims description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 12
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 claims description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 11
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 11
- 229910052744 lithium Inorganic materials 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 239000005357 flat glass Substances 0.000 claims description 3
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 3
- 229920002521 macromolecule Polymers 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 241000736199 Paeonia Species 0.000 claims 1
- 235000006484 Paeonia officinalis Nutrition 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 146
- 239000010408 film Substances 0.000 description 99
- 238000000034 method Methods 0.000 description 79
- 238000004544 sputter deposition Methods 0.000 description 76
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 66
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 41
- 239000001301 oxygen Substances 0.000 description 41
- 229910052760 oxygen Inorganic materials 0.000 description 41
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 39
- 229910001882 dioxygen Inorganic materials 0.000 description 39
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 38
- 229910052786 argon Inorganic materials 0.000 description 33
- 238000001579 optical reflectometry Methods 0.000 description 24
- 239000011651 chromium Substances 0.000 description 22
- 239000004411 aluminium Substances 0.000 description 19
- 229910052782 aluminium Inorganic materials 0.000 description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 19
- 229960001296 zinc oxide Drugs 0.000 description 19
- 239000011787 zinc oxide Substances 0.000 description 19
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 15
- 229910052804 chromium Inorganic materials 0.000 description 15
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 12
- 229910052721 tungsten Inorganic materials 0.000 description 12
- 239000010937 tungsten Substances 0.000 description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229910000423 chromium oxide Inorganic materials 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 10
- 230000002441 reversible effect Effects 0.000 description 10
- 230000009466 transformation Effects 0.000 description 10
- 206010061245 Internal injury Diseases 0.000 description 9
- 229910018487 Ni—Cr Inorganic materials 0.000 description 9
- BAPRMBRFVUJBEI-UHFFFAOYSA-N [O].[O].[Ni] Chemical group [O].[O].[Ni] BAPRMBRFVUJBEI-UHFFFAOYSA-N 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 9
- 239000002253 acid Substances 0.000 description 9
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 9
- 239000003599 detergent Substances 0.000 description 9
- 238000007602 hot air drying Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000000985 reflectance spectrum Methods 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000004313 glare Effects 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 238000004134 energy conservation Methods 0.000 description 5
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000004984 smart glass Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910001120 nichrome Inorganic materials 0.000 description 2
- 230000009919 sequestration Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000004446 light reflex Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention provides a kind of total solids electrochromic device and preparation method thereof.Described total solids electrochromic device, it is characterised in that including the transparency carrier set gradually from top to bottom, the first functional layer, media coating, the first photochromic layer, ion offer and conducting shell, the second photochromic layer, media coating and the second functional layer；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer and the second functional layer are all transparent conductor layer, or, one in the first functional layer and the second functional layer is transparent conductor layer, and another is high reflection state metallic diaphragm.Easy the beneficial effects of the present invention are preparation technology, the response device time is short.
Description
Technical field
The present invention relates to a kind of total solids electrochromic device, can be applied to automobile electrochromism anti-glare outside rear-view mirror,
On inside rear-view mirror, automobile front-rear windshield glass, side window glass and roof glass, can also be applied to interior dazzle mirror, building glass and
Fit up on glass.
Background technology
Electrochromic device can be divided into solution-type, gel-type, fully solid etc. according to the form of electrochromic material.Its
In ion containing solid-state form provide and conducting shell, and film forms the electrochromic devices of all solids and is referred to as total solids
Infiltration type electrochromic device.
The typical structure of existing total solids electrochromic device includes transparent conductive body, the first photochromic layer, ionic conduction
Layer, the second photochromic layer, transparent conductive body, wherein the first photochromic layer is nickel oxide, nickel material is magnetic in itself, and sputtering difficulty is big.
The typical structure of existing reflection-type total solids electrochromic device is two layers of transparency carrier, is prepared on the inside of two layers of transparency carrier,
Manufacturing cost is high, complex process.It is longer that the shortcomings that existing total solids electrochromic device, also resides in the response device time, is 4-
6 minutes, it is unable to reach user's request.
The content of the invention
Have it is an object of the invention to provide a kind of compared with the total solids electrochromic device of short response time and its preparation side
Method.
In order to achieve the above object, present invention employs following technical scheme：
A kind of total solids electrochromic device, it is characterised in that including the transparency carrier set gradually from top to bottom, first
Functional layer, media coating, the first photochromic layer, ion offer and conducting shell, the second photochromic layer, media coating and the second functional layer；
First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer and the second functional layer are all
Bright conductor layer, or, one in the first functional layer and the second functional layer is transparent conductor layer, and another is metal film
Layer.
Further, when applying voltage, ion transmits between the first photochromic layer and the second photochromic layer, the electroluminescent change of total solids
The transmitance or reflectivity of color device change.
Further, described transparency carrier is common glass substrates, quartz glass substrate or plastic base (such as PET
Deng).
Further, the first described photochromic layer is nickel oxide chromium oxide mixture layer.
Further, in described nickel oxide chromium oxide mixture layer, the content of chromium oxide is not between 0-50%, and not
For 0.
Further, the pattern of the first described photochromic layer is that nanometer is unformed or crystal type.
Further, the sheet resistivity of the first described photochromic layer is more than or equal to 50K Ω/, and thickness is in 100-400nm.
Further, the second described photochromic layer is tungsten oxide photochromic layer.
Further, the second described photochromic layer is made up of armorphous nano particle.
Further, the sheet resistivity of the second described photochromic layer is more than or equal to 50K Ω/, and thickness is in 100-900nm.
Further, the first described photochromic layer shows as transparent state when being ion implanted, it is seen that light transmission rate be more than etc.
In 75%；Coloured state is shown as when ion is moved out, it is seen that light transmission rate is less than or equal to 15%；The second described photochromic layer when from
Coloured state is shown as during son injection, it is seen that light transmission rate is less than or equal to 10%；Transparent state is shown as when ion is moved out, it is seen that light
Transmitance is more than or equal to 75%.
Further, the sheet resistivity of described transparent conductor layer is less than or equal to 100 Ω/, thickness 50-300nm.
Further, the material of described transparent conductor layer is ITO, FTO, at least one of ATO and AZO.
Further, described metallic diaphragm is high reflection state metallic diaphragm.
Further, the thickness of described metallic diaphragm is in 50nm-800nm.
Further, the visible reflectance 40%-80% of described metallic diaphragm.
Further, described metallic diaphragm contains metallic aluminium, argent, aerdentalloy, crome metal, cadmium metal, metal
At least one of copper, Titanium and metallic nickel.
Further, described electrode is connected directly between on metallic diaphragm.
Further, described media coating is containing at least one in silica, silicon nitride, zinc oxide, aluminum oxide and AZO
Kind.
Further, the thickness of described media coating is 5-200nm.
Further, described ion provides and conducting shell is undefined structure.
Further, described ion provides and the thickness of conducting shell is 200-800nm.
Further, described ion provides and conducting shell can supply lithium ion.
Further, described ion provides and conducting shell contains at least one of lithium tantalate and lanthanium titanate lithium.
Further, the maximum visible reflectance adjustable range of described total solids electrochromic device is 10-75%.
Control is applied to the time of voltage on electrode, and voltage swing, obtains different reflectivity.
Further, it is additionally provided with protective layer on the outside of the second described functional layer.
Further, the thickness of described protective layer is limited in 50nm-800nm.
Further, described protective layer is metal level, inorganic oxide layer or macromolecule membrane.
Further, described metal level contains in crome metal, cadmium metal, metallic copper, Titanium and metallic nickel extremely
Few one kind.
Further, described inorganic oxide layer contains in aluminum oxide, silica, zirconium oxide, titanium oxide and silicon nitride
At least one.
Further, described macromolecule membrane is PTFE.
Present invention also offers the preparation method of above-mentioned total solids electrochromic device, it is characterised in that including：
The first step：Clean transparency carrier；
Second step：The first functional layer is prepared on the transparent substrate, lays the circuit that can be connected with electrode；
3rd step：Media coating is prepared in the first functional layer；
4th step：The first photochromic layer is prepared on media coating；
5th step：Ion offer and conducting shell are provided on the first photochromic layer；
6th step：The second photochromic layer is prepared in ion offer and conducting shell；
7th step：Another media coating is prepared on the second photochromic layer；
8th step：The second functional layer is prepared on media coating, lays the circuit that can be connected with electrode；
9th step：Protective layer is prepared in the second functional layer.
Further, the first described photochromic layer is obtained by the reactive sputtering of nichrome, or oxide target material is entered
Row sputtering or electron beam evaporation obtain.
Further, described ion is provided and conducting shell can be obtained with magnetron sputtering method, or electron-beam vapor deposition method obtains.
Further, the second described photochromic layer is by the reactive magnetron sputtering method acquisition to tungsten, or tungsten oxide
The sputtering of target obtains, or is obtained by electron-beam vapor deposition method.
Present invention also offers above-mentioned total solids electrochromic device in automobile rearview mirror, mirror, external wall are dazzled in interior
On application.
Present invention also offers a kind of automobile rearview mirror, it is characterised in that contains above-mentioned total solids electrochromic device.
In the total solids electrochromic device of the present invention, the first functional layer and the second functional layer are all transparent conductor layer
When, it is possible to achieve transmission and reversible transformation between absorbing state, infiltration type electrochromic device is, can be applied to build, fits up glass
On glass, same energy-conservation is played, intelligence, sequestration, can also be applied on automobile front-rear windshield glass and side window glass, play
Energy-conservation, intelligence, sequestration.One in first functional layer and the second functional layer is transparent conductor layer, and another is metal
During film layer, device shows reflective electrochromic performance, is reflective electrochromic device, prevents available for automobile electrochromism
Dazzle the eyes mirror, it can also be used to which mirror is dazzled in external wall of high-rise building and interior.
In the total solids electrochromic device of the present invention, transparency carrier is used to carry subsequent thin film.Transparent conductor layer is made
Electrode is introduced for electric field, its surfacing is uniform, and with transparency carrier, the first photochromic layer is well combined.The surface of first photochromic layer
Even uniform is well combined with substrate layer, dielectric layer.Media coating is used to prevent photochromic layer and transparency conducting layer phase counterdiffusion, protects
The independence between each film layer is demonstrate,proved, prevents ion from entering transparent conductor layer.Media coating is transition zone, has smooth table
Face, beneficial to the metallic diaphragm of high reflection is obtained, the phenomenon for causing ion to be spread in transparent conductive body that is excessively powered can be prevented.Protect
Sheath is located at the surface of metallic diaphragm, protects oxidation of metallic diaphragm etc. to act on.The surfacing of the second described photochromic layer is equal
It is even to be well combined with metallic diaphragm, media coating.Metallic diaphragm effect is reflected light path.To the first photochromic layer and the second photochromic layer
When carrying out implanting ions or removing ion, it can substantially change its optical morphology, so as to control the transmission of light and reflection.
The total solids reflective electrochromic device of the present invention mutually ties photochromic layer and transparent conductor layer, metallic diaphragm
Close.Wherein, because metallic diaphragm is as reflecting layer, functioned simultaneously as the effect to electrode, and electric conductivity is good, prepare cost compared with
Transparent conductor layer is low.When ion is located at the first photochromic layer, the second photochromic layer is having the feelings of ion without ion, the first photochromic layer
Transparent state is shown as under condition, such light passes through the first photochromic layer, and the high reflection state metal film of bottom is irradiated to after the second photochromic layer
It is rear to pass through the second photochromic layer, the first photochromic layer outgoing, because first the second photochromic layer of photochromic layer is transparent, to bright shadow again on layer
Sound is less, therefore ensure that higher reflectivity.
When applying backward voltage, controlled by voltage, ion is moved into the second photochromic layer from the first photochromic layer, this
When, the first photochromic layer is without ion, and the second photochromic layer has ion, and the first photochromic layer shows as brown color, the performance of the second photochromic layer
For blueness, the translucency of light path is reduced, declines the overall reflectivity of device, and control circuit voltage and electricity can be passed through
Application time is pressed, reaches ionic portions and is migrated between the first photochromic layer and the second photochromic layer, the reflectivity of dynamic regulation device.
Total solids electrochromic device shows high reflection state, or high transmission state in colour killing state；Apply anti-
During to voltage, when ion is provided by ion and conducting shell enters the second photochromic layer, infiltration type electrochromic device shows to inhale
Receipts state, light transmittance reduce.Reflective electrochromic device shows reflectivity reduction.
It is well combined in the present invention between each layer, particularly, single first photochromic layer, or single ionic provides and conduction
Layer, or the single equal electron conduction of second photochromic layer are poor, and ionic conductivity is good.Between each layer only with contact adjacent layers,
Occur without the situation of cross-layer UNICOM.In circuit connection, external circuit mainly connects transparent conductor layer and high reflection state metal
Film layer, pass through the Ion transfer inside this two layers application voltage, control device.Due to using the whole face covering conduct of back-metal
Electrode, facilitate wiring, do not influence specular cross section, be not in that the visual field narrows.
The total solids reflective electrochromic device of the present invention is mainly used in the rearview mirror of automobile, and mirror is dazzled in interior, high-rise
External wall, the especially application in automobile rearview mirror field have important security implications.After being frequently encountered in driving conditions
The uncivil situation using high beam of car, dazzling, serious threat traffic safety is formed to front truck driver.And work as and use total solids
When reflective electrochromic device is as rearview mirror, coordinate light sensation circuit to use, can have by force by the control of electronic circuit
During light irradiation, the reflectivity of rearview mirror is greatly lowered, does not produce emergency light reflex, dazzling effect is not produced to driver.In height
It is both attractive in appearance when layer building uses total solids infiltration type electrochromic device as building glass, it can ensure not producing light dirt again
Dye.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, metallic diaphragm as reflecting layer, has functioned simultaneously as the effect to electrode, and electric conductivity is good, prepares in the present invention
The relatively transparent conductor layer of cost is low.
2nd, the present invention uses nickel oxide chromium oxide mixture as photochromic layer, and magnetic material is compensate for nichrome sputtering
Shortcoming, the solid electrochromic device of gained, the response time is shorter, is the 2-8 seconds.
3rd, total solids electrochromic device of the present invention prepares formation using protective layer on single-layer and transparent substrate, manufacture
Cost is low, and technique is simple.
Brief description of the drawings
Fig. 1 a are total solids infiltration type electrochromic device structural representation；
Fig. 1 b are total solids reflective electrochromic device structural representation (reflecting surface is substrate back)；
Fig. 1 c are total solids reflective electrochromic device structural representation (reflecting surface is substrate front side)；
Fig. 2 is total solids reflective electrochromic device cross-sectional scanning electron shooting figure；
Fig. 3 is electrochromic device encapsulation schematic diagram；
Fig. 4 is the transmitted light spectrogram of total solids electrochromic device；
Fig. 5 is the reflectance spectrum figure of total solids electrochromic device；
Fig. 6 is the transmitance of total solids electrochromic device with voltage responsive variation diagram.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Each degree in the present invention, it is molar percentage unless otherwise specified.
Embodiment 1
As shown in Figure 1a, the total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom,
First functional layer, media coating, the first photochromic layer, ion offer and conducting shell, the second photochromic layer, media coating, the second function
Layer and protective layer composition；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer and
Two functional layers are all transparent conductor layer.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer, Quan Gu
The transmitance or reflectivity of body electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixture layer, the wherein content of chromium oxide is 20%；Second photochromic layer is tungsten oxide photochromic layer, and media coating is zinc oxide
Layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is alumina layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：Transparent conductor layer is prepared on the transparent substrate：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, room temperature (25 DEG C) sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine table
Face sheet resistance, sheet resistivity are 50 Ω/, thickness 100nm.In the edge pin of transparent conductor layer, laying can be with electrode
The circuit of connection.
3rd step：Media coating is prepared in the first functional layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 20nm zinc-oxide film as media coating.
4th step：The first photochromic layer is prepared on media coating：The mixing of nickel oxide chromium oxide is prepared using magnetron sputtering method
Film, the 3rd step products obtained therefrom is put into magnetron sputtering cavity, target selects metal nickel chromium triangle target (Cr 20%), and purity is better than
99%, shielding power supply uses dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio
For 10%, pressure control 1Pa, sputtering time 10 minutes, nickel oxide chromium oxide mixed film is obtained, as the first photochromic layer；The
The pattern of one photochromic layer is unformed, and the sheet resistivity of the first photochromic layer is 50K Ω/, thickness 100nm.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, the thickness for obtaining unformed porosity and looseness are 500nm tungsten oxide films, as the second photochromic layer,
For unformed porosity and looseness film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by the 6th step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 20nm zinc-oxide film as media coating.
8th step：The second functional layer is prepared on media coating：Transparent conductor layer is prepared using magnetron sputtering method, by the
Seven step products obtained therefroms are put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/
cm2, atmosphere pure argon, pressure 0.3Pa, room temperature sputtering times ten minutes, the ITO conducting films of surfacing are obtained, determine surface
Sheet resistance, sheet resistivity are 50 Ω/, thickness 100nm.In the edge pin of transparent conductor layer, laying can connect with electrode
The circuit connect.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Obtain product and be put into magnetron sputtering cavity, target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 0.5Pa, sputtering time 60
Minute, acquisition thickness is 200nm aluminum oxide film as protective layer.Its section structure is as shown in Fig. 2 be encapsulated into such as figure
Structure shown in 3, in figure, the first functional layer 1 and the second functional layer 2 difference connection electrode.
The electrochromic device of such a structure can between transmission and absorption reversible transformation, its pellucidity and absorb shape
The spectrogram of state represents there is good infrared barrier function under Fig. 4, absorbing state.The electrochromic device of such a structure can
With with building energy conservation smart window.
The first described photochromic layer shows as transparent state when being ion implanted, it is seen that light transmission rate 75%；When ion moves
Coloured state is shown as when going out, it is seen that light transmission rate 10%；The second described photochromic layer shows as coloured state when ion implanting,
Visible light transmissivity is 10%；Transparent state is shown as when ion is moved out, it is seen that light transmission rate 75%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture layer, it is seen that light transmission rate 50%-80%.
As shown in fig. 6, the present invention controls the transmitance of total solids electrochromic device by voltage-regulation, such as in 1.5V electricity
Pressure 5s interior energies reach be changed to from 75% 45% transmitance, can reach from 75% in 5s under 2V voltages and be changed to 30%
Transmitance, can reach in 5s under 2.5V voltages be changed to from 75% 15% transmitance.
Embodiment 2
As shown in Figure 1 b, the total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom,
First functional layer, media coating, the first photochromic layer, ion offer and conducting shell, the second photochromic layer, media coating, the second function
Layer and protective layer composition；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer is
Bright conductor layer, the second functional layer are high reflection state metallic diaphragm.When applying voltage, ion changes colour in the first photochromic layer and second
Transmitted between layer, the transmitance or reflectivity of total solids electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixture layer, the wherein content of chromium oxide is 20%；Second photochromic layer is tungsten oxide photochromic layer, high reflection state metallic diaphragm
For aluminium lamination；Media coating is alumina layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is
Metallic chromium layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：Transparent conductor layer is prepared on the transparent substrate：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine sheet resistivity, surface
Sheet resistance is 50 Ω/, thickness 100nm.In the edge pin of transparent conductor layer, the circuit that can be connected with electrode is laid.
3rd step：Media coating is prepared in the first functional layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm aluminum oxide films as media coating.
4th step：The first photochromic layer is prepared on media coating：Using magnetron sputtering method, the 3rd step products obtained therefrom is put into
Magnetron sputtering cavity, target select metal nickel chromium triangle target (Cr 20%), and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/em2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 10%, pressure control 1Pa, sputtering time 10
Minute, acquisition thickness is 150nm nickel oxide chromium oxide mixture films, as the first photochromic layer；The pattern of first photochromic layer is
Unformed, the sheet resistivity of the first photochromic layer is 50K Ω/.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/em2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, acquisition thickness are 500nm tungsten oxide films, are unformed porosity and looseness as the second photochromic layer
Film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by the 6th step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm aluminum oxide films as media coating.
8th step：High reflection state metallic diaphragm is prepared on media coating：High reflection state gold is prepared using magnetron sputtering method
Belong to film layer, the 7th step products obtained therefrom is put into magnetron sputtering cavity, target selects metallic aluminium target, and shielding power supply uses direct current
Source, power density 1w/cm2, atmosphere pure argon, pressure 0.5Pa, sputtering time 5 minutes, the metallic aluminium for obtaining surfacing is thin
Film, as high reflection state metallic diaphragm, it is seen that light reflectivity 65%, thickness 500nm.On the side of high reflection state metallic diaphragm
Edge pin, lay the circuit that can be connected with electrode.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Obtain product and be put into magnetron sputtering cavity, target uses crome metal target, and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 6w/cm2, atmosphere uses argon gas, pressure control 0.5Pa, sputtering time 30 minutes, obtains the metal that thickness is 200nm
Chromium is as protective layer.
The device of this structure can between reflection and absorption reversible transformation, can be applied on vehicle glare proof mirror.Instead
The reflectance spectrum figure of emitting electrochromic device is represented in Fig. 5.Visible region reflectivity is 75%, the reflection of absorbing state
Rate is 15%.
The first described photochromic layer shows as reflecting state when being ion implanted, it is seen that light reflectivity 75%；When ion moves
Coloured state is shown as when going out, it is seen that light reflectivity 15%；The second described photochromic layer shows as coloured state when ion implanting,
Visible reflectance is 15%；Show as reflecting state when ion is moved out, it is seen that light reflectivity 75%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture layer, it is seen that light transmission rate is more than 75%.
The present invention controls the reflectivity of total solids electrochromic device by voltage-regulation, can be reached in 5s under 1.5V voltages
To the transmitance that 45% is changed to from 75%, can reach in 5s under 2V voltages be changed to from 75% 30% transmitance,
Under 2.5V voltages 5s interior energies reach be changed to from 75% 15% transmitance.
Under environment temperature, under 2.5V positive voltages, 6s internal reflections rate is from 75% near 15%, under 2.5V negative voltages in 2s
75% is risen to from 15%.
Embodiment 3
As illustrated in figure 1 c, the total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom,
First functional layer, media coating, the first photochromic layer, ion offer and conducting shell, the second photochromic layer, media coating, the second function
Layer and protective layer composition；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer is height
State metallic diaphragm is reflected, the second functional layer is transparent conductor layer.When applying voltage, ion changes colour in the first photochromic layer and second
Transmitted between layer, the transmitance or reflectivity of total solids electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixture layer, the wherein content of chromium oxide is 20%, and high reflection state metallic diaphragm is silver layer；Media coating is zinc oxide
Layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is silicon oxide layer.Second photochromic layer is oxygen
Change tungsten photochromic layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：High reflection state metallic diaphragm is prepared on the transparent substrate：High reflection state gold is prepared using magnetron sputtering method
Belong to film layer, the 7th step products obtained therefrom is put into magnetron sputtering cavity, target selects metallic silver target, and shielding power supply uses direct current
Source, power density 1w/cm2, atmosphere pure argon, pressure 0.5Pa, sputtering time 5 minutes, the argent for obtaining surfacing is thin
Film, as high reflection state metallic diaphragm, it is seen that light reflectivity 75%, thickness 200nm.On the side of high reflection state metallic diaphragm
Edge pin, lay the circuit that can be connected with electrode.
3rd step：Media coating is prepared on high reflection state metallic diaphragm：Media coating is prepared using magnetron sputtering method, will
Second step products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses direct current
Power supply, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering
2 minutes time, acquisition thickness are 10nm zinc-oxide films as media coating.
4th step：The first photochromic layer is prepared on media coating：Using magnetron sputtering method, the 3rd step products obtained therefrom is put into
Magnetron sputtering cavity, target select metal nickel chromium triangle target (Cr 20%), and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 10%, pressure control 1Pa, sputtering time 10
Minute, nickel oxide chromium oxide mixture film is obtained, as the first photochromic layer；The pattern of first photochromic layer is unformed, and first
The sheet resistivity of photochromic layer is 50K Ω/, thickness 100m.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, acquisition thickness are 500nm tungsten oxide films, are unformed porosity and looseness as the second photochromic layer
Film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10m zinc-oxide films as media coating.
8th step：Transparent conductor layer is prepared on media coating：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine sheet resistivity, surface
Sheet resistance 50K Ω/, thickness 100nm.In the edge pin of transparent conductor layer, the circuit that can be connected with electrode is laid.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Product is put into magnetron sputtering cavity, target use silicon target, and for purity better than 99%, shielding power supply uses dc source, and power is close
Spend 6w/cm2, atmosphere uses argon gas, pressure control 0.5Pa, sputtering time 60 minutes, obtains the silica that thickness is 500nm and make
For protective layer.
The device of this structure can between reflection and absorption reversible transformation, can be applied on vehicle glare proof mirror.Instead
The reflectance spectrum figure of emitting electrochromic device represents identical with Fig. 5.Metallic state reflectivity is 75%, the reflectivity of colored state
For 15%.
The first described photochromic layer shows as reflecting state when being ion implanted, it is seen that light reflectivity 75%；When ion moves
Coloured state is shown as when going out, it is seen that light reflectivity 15%；The second described photochromic layer shows as coloured state when ion implanting,
Visible reflectance is 15%；Show as reflecting state when ion is moved out, it is seen that light reflectivity 75%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture layer, it is seen that light transmission rate is more than 75%.
Under environment temperature, under 2.5V positive voltages, 6s internal reflections rate is from 75% near 15%, under 2.5V negative voltages in 2s
75% is risen to from 15%.
Embodiment 4
The total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom, the first functional layer,
Media coating, the first photochromic layer, ion provides and conducting shell, the second photochromic layer, media coating, the second functional layer and protective layer group
Into；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer and the second functional layer are all
Transparent conductor layer.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer, total solids electrochromism device
The transmitance or reflectivity of part change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixture photochromic layer, the content of chromium oxide is 50%；Second photochromic layer is tungsten oxide photochromic layer, and media coating is zinc oxide
Layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is alumina layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：Transparent conductor layer is prepared on the transparent substrate：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, room temperature (25 DEG C) sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine table
Face sheet resistance, sheet resistivity are 50 Ω/, thickness 100nm.In the edge pin of transparent conductor layer, laying can be with electrode
The circuit of connection.
3rd step：Media coating is prepared in the first functional layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 20nm zinc-oxide film as media coating.
4th step：The first photochromic layer is prepared on media coating：The mixing of nickel oxide chromium oxide is prepared using magnetron sputtering method
Film, the 3rd step products obtained therefrom is put into magnetron sputtering cavity, target selects metal nickel chromium triangle target (Cr 50%), and purity is better than
99%, shielding power supply uses dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio
For 10%, pressure control 1Pa, sputtering time 10 minutes, nickel oxide chromium oxide mixed film is obtained, as the first photochromic layer；The
The pattern of one photochromic layer is unformed, and the sheet resistivity of the first photochromic layer is 50K Ω/, thickness 100nm.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, the thickness for obtaining unformed porosity and looseness are 500nm tungsten oxide films, as the second photochromic layer,
For unformed porosity and looseness film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by the 6th step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 20nm zinc-oxide film as media coating.
8th step：The second functional layer is prepared on media coating：Transparent conductor layer is prepared using magnetron sputtering method, by the
Seven step products obtained therefroms are put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/
cm2, atmosphere pure argon, pressure 0.3Pa, room temperature sputtering times ten minutes, the ITO conducting films of surfacing are obtained, determine surface
Sheet resistance, sheet resistivity are 50 Ω/, thickness 100nm.In the edge pin of transparent conductor layer, laying can connect with electrode
The circuit connect.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Obtain product and be put into magnetron sputtering cavity, target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 0.5Pa, sputtering time 60
Minute, acquisition thickness is 200nm aluminum oxide film as protective layer.It is packaged into structure as shown in Figure 3, in figure, the first work(
The functional layer 2 of ergosphere 1 and second distinguishes connection electrode.
The electrochromic device of such a structure can between transmission and absorption reversible transformation, its pellucidity and absorb shape
The spectrogram of state represents identical with Fig. 4, has good infrared barrier function under absorbing state.The electrochromism device of such a structure
Part can be with building energy conservation smart window.
The first described photochromic layer shows as transparent state when being ion implanted, it is seen that light transmission rate 75%；When ion moves
Coloured state is shown as when going out, it is seen that light transmission rate 10%；The second described photochromic layer shows as coloured state when ion implanting,
Visible light transmissivity is 10%；Transparent state is shown as when ion is moved out, it is seen that light transmission rate 75%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture layer, it is seen that light transmission rate 50%-80%.
The present invention controls the transmitance of total solids electrochromic device, the energy in 5s such as under 1.5V voltages by voltage-regulation
Reach be changed to from 75% 45% transmitance, can reach in 5s under 2V voltages be changed to from 75% 30% transmitance,
Under 2.5V voltages 5s interior energies reach be changed to from 75% 15% transmitance.
Embodiment 5
The total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom, the first functional layer,
Media coating, the first photochromic layer, ion provides and conducting shell, the second photochromic layer, media coating, the second functional layer and protective layer group
Into；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer and the second functional layer are all
Transparent conductor layer.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer, total solids electrochromism device
The transmitance or reflectivity of part change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixing photochromic layer, the content of chromium oxide is 5%；Second photochromic layer is tungsten oxide photochromic layer, and media coating is zinc oxide film.
Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is alumina layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：Transparent conductor layer is prepared on the transparent substrate：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, room temperature (25 DEG C) sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine table
Face sheet resistance, sheet resistivity are 50 Ω/, thickness 100m.In the edge pin of transparent conductor layer, laying can connect with electrode
The circuit connect.
3rd step：Media coating is prepared in the first functional layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 20nm zinc-oxide film as media coating.
4th step：The first photochromic layer is prepared on media coating：The mixing of nickel oxide chromium oxide is prepared using magnetron sputtering method
Thing mixed film, the 3rd step products obtained therefrom is put into magnetron sputtering cavity, target selects metal nickel chromium triangle target (Cr 5%), and purity is excellent
In 99%, shielding power supply uses dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio
Example is 10%, pressure control 1Pa, sputtering time 10 minutes, nickel oxide chromium oxide mixed film is obtained, as the first photochromic layer；
The pattern of first photochromic layer is unformed, and the sheet resistivity of the first photochromic layer is 50K Ω/, thickness 100nm.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, the thickness for obtaining unformed porosity and looseness are 500nm tungsten oxide films, as the second photochromic layer,
For unformed porosity and looseness film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by the 6th step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 20nm zinc-oxide film as media coating.
8th step：The second functional layer is prepared on media coating：Transparent conductor layer is prepared using magnetron sputtering method, by the
Seven step products obtained therefroms are put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/
cm2, atmosphere pure argon, pressure 0.3Pa, room temperature sputtering times ten minutes, the ITO conducting films of surfacing are obtained, determine surface
Sheet resistance, sheet resistivity are 50 Ω/, thickness 100nmm.In the edge pin of transparent conductor layer, laying can connect with electrode
The circuit connect.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Obtain product and be put into magnetron sputtering cavity, target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 0.5Pa, sputtering time 60
Minute, acquisition thickness is 200nm aluminum oxide film as protective layer.It is packaged into structure as shown in Figure 3, in figure, the first work(
The functional layer 2 of ergosphere 1 and second distinguishes connection electrode.
The electrochromic device of such a structure can between transmission and absorption reversible transformation, its pellucidity and absorb shape
The spectrogram of state is identical with Fig. 4, has good infrared barrier function under absorbing state.The electrochromic device of such a structure can
With with building energy conservation smart window.
The first described photochromic layer shows as transparent state when being ion implanted, it is seen that light transmission rate 75%；When ion moves
Coloured state is shown as when going out, it is seen that light transmission rate 10%；The second described photochromic layer shows as coloured state when ion implanting,
Visible light transmissivity is 10%；Transparent state is shown as when ion is moved out, it is seen that light transmission rate 75%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture layer, it is seen that light transmission rate 50%-80%.
The present invention controls the transmitance of total solids electrochromic device, the energy in 5s such as under 1.5V voltages by voltage-regulation
Reach be changed to from 75% 45% transmitance, can reach in 5s under 2V voltages be changed to from 75% 30% transmitance,
Under 2.5V voltages 5s interior energies reach be changed to from 75% 15% transmitance.
Embodiment 6
The total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom, the first functional layer,
Media coating, the first photochromic layer, ion provides and conducting shell, the second photochromic layer, media coating, the second functional layer and protective layer group
Into；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer is transparent conductor layer,
Second functional layer is high reflection state metallic diaphragm.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer,
The transmitance or reflectivity of total solids electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixing photochromic layer, the wherein content of chromium oxide is 50%；Second photochromic layer is tungsten oxide photochromic layer, high reflection state metal film
Layer is aluminium lamination；Media coating is alumina layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer
For metallic chromium layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：Transparent conductor layer is prepared on the transparent substrate：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine sheet resistivity, surface
Sheet resistance is 50 Ω/, thickness 100nm.In the edge pin of transparent conductor layer, the circuit that can be connected with electrode is laid.
3rd step：Media coating is prepared in the first functional layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm aluminum oxide films as media coating.
4th step：The first photochromic layer is prepared on media coating：Using magnetron sputtering method, the 3rd step products obtained therefrom is put into
Magnetron sputtering cavity, target select metal nickel chromium triangle target (Cr50%), and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 10%, pressure control 1Pa, sputtering time 10
Minute, acquisition thickness is 150nm nickel oxide chromium oxide mixture films, as the first photochromic layer；The pattern of first photochromic layer is
Unformed, the sheet resistivity of the first photochromic layer is 50K Ω/.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, acquisition thickness are 500nm tungsten oxide films, are unformed porosity and looseness as the second photochromic layer
Film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by the 6th step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm aluminum oxide films as media coating.
8th step：High reflection state metallic diaphragm is prepared on media coating：High reflection state gold is prepared using magnetron sputtering method
Belong to film layer, the 7th step products obtained therefrom is put into magnetron sputtering cavity, target selects metallic aluminium target, and shielding power supply uses direct current
Source, power density 1w/cm2, atmosphere pure argon, pressure 0.5Pa, sputtering time 5 minutes, the metallic aluminium for obtaining surfacing is thin
Film, as high reflection state metallic diaphragm, it is seen that light reflectivity 65%, thickness 500nm.On the side of high reflection state metallic diaphragm
Edge pin, lay the circuit that can be connected with electrode.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Obtain product and be put into magnetron sputtering cavity, target uses crome metal target, and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 6w/cm2, atmosphere uses argon gas, pressure control 0.5Pa, sputtering time 30 minutes, obtains the metal that thickness is 200nm
Chromium is as protective layer.
The device of this structure can between reflection and absorption reversible transformation, can be applied on vehicle glare proof mirror.Instead
The reflectance spectrum figure of emitting electrochromic device is identical with Fig. 5.Visible region reflectivity is 65%, the reflectivity of absorbing state
For 15%.
The first described photochromic layer shows as reflecting state when being ion implanted, it is seen that light reflectivity 65%；When ion moves
Coloured state is shown as when going out, it is seen that light reflectivity 15%；The second described photochromic layer shows as coloured state when ion implanting,
Visible reflectance is 15%；Show as reflecting state when ion is moved out, it is seen that light reflectivity 65%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture mixed layer, it is seen that light transmission rate is more than 75%.
The present invention controls the reflectivity of total solids electrochromic device, the energy in 5s such as under 1.5V voltages by voltage-regulation
Reach be changed to from 75% 45% transmitance, can reach in 5s under 2V voltages be changed to from 75% 30% transmitance,
Under 2.5V voltages 5s interior energies reach be changed to from 75% 15% transmitance.
Under environment temperature, under 2.5V positive voltages, 6s internal reflections rate is from 75% near 15%, under 2.5V negative voltages in 2s
75% is risen to from 15%.
Embodiment 7
The total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom, the first functional layer,
Media coating, the first photochromic layer, ion provides and conducting shell, the second photochromic layer, media coating, the second functional layer and protective layer group
Into；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer is transparent conductor layer,
Second functional layer is high reflection state metallic diaphragm.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer,
The transmitance or reflectivity of total solids electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixing photochromic layer, the wherein content of chromium oxide is 5%；Second photochromic layer is tungsten oxide photochromic layer, high reflection state metal film
Layer is aluminium lamination；Media coating is alumina layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer
For metallic chromium layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：Transparent conductor layer is prepared on the transparent substrate：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine sheet resistivity, surface
Sheet resistance is 50 Ω/, thickness 100m.In the edge pin of transparent conductor layer, the circuit that can be connected with electrode is laid.
3rd step：Media coating is prepared in the first functional layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm aluminum oxide films as media coating.
4th step：The first photochromic layer is prepared on media coating：Using magnetron sputtering method, the 3rd step products obtained therefrom is put into
Magnetron sputtering cavity, target select metal nickel chromium triangle target (Cr5%), and purity is better than 99%, and shielding power supply uses dc source, power
Density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 10%, and pressure control 1Pa, sputtering time 10 divides
Clock, acquisition thickness is 150nm nickel oxide chromium oxide mixture films, as the first photochromic layer；The pattern of first photochromic layer is nothing
Sizing, the sheet resistivity of the first photochromic layer is 50K Ω/.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, acquisition thickness are 500nm tungsten oxide films, are unformed porosity and looseness as the second photochromic layer
Film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by the 6th step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic aluminium target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm aluminum oxide films as media coating.
8th step：High reflection state metallic diaphragm is prepared on media coating：High reflection state gold is prepared using magnetron sputtering method
Belong to film layer, the 7th step products obtained therefrom is put into magnetron sputtering cavity, target selects metallic aluminium target, and shielding power supply uses direct current
Source, power density 1w/cm2, atmosphere pure argon, pressure 0.5Pa, sputtering time 5 minutes, the metallic aluminium for obtaining surfacing is thin
Film, as high reflection state metallic diaphragm, it is seen that light reflectivity 65%, thickness 500nm.On the side of high reflection state metallic diaphragm
Edge pin, lay the circuit that can be connected with electrode.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Obtain product and be put into magnetron sputtering cavity, target uses crome metal target, and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 6w/cm2, atmosphere uses argon gas, pressure control 0.5Pa, sputtering time 30 minutes, obtains the metal that thickness is 200nm
Chromium is as protective layer.
The device of this structure can between reflection and absorption reversible transformation, can be applied on vehicle glare proof mirror.Instead
The reflectance spectrum figure of emitting electrochromic device represents identical with Fig. 5.Visible region reflectivity be 65%, absorbing state it is anti-
Rate is penetrated as 15%.
The first described photochromic layer shows as reflecting state when being ion implanted, it is seen that light reflectivity 65%；When ion moves
Coloured state is shown as when going out, it is seen that light reflectivity 15%；The second described photochromic layer shows as coloured state when ion implanting,
Visible reflectance is 15%；Show as reflecting state when ion is moved out, it is seen that light reflectivity 65%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture mixed layer, it is seen that light transmission rate is more than 75%.
The present invention controls the reflectivity of total solids electrochromic device, the energy in 5s such as under 1.5V voltages by voltage-regulation
Reach be changed to from 75% 45% transmitance, can reach in 5s under 2V voltages be changed to from 75% 30% transmitance,
Under 2.5V voltages 5s interior energies reach be changed to from 75% 15% transmitance.
Under environment temperature, under 2.5V positive voltages, 6s internal reflections rate is from 75% near 15%, under 2.5V negative voltages in 2s
75% is risen to from 15%.
Embodiment 8
The total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom, the first functional layer,
Media coating, the first photochromic layer, ion provides and conducting shell, the second photochromic layer, media coating, the second functional layer and protective layer group
Into；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer is high reflection state metal film
Layer, the second functional layer is transparent conductor layer.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer,
The transmitance or reflectivity of total solids electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixture layer, the wherein content of chromium oxide is 50%, and high reflection state metallic diaphragm is silver layer；Media coating is zinc oxide
Layer.Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is silicon oxide layer.Second photochromic layer is oxygen
Change tungsten photochromic layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：High reflection state metallic diaphragm is prepared on the transparent substrate：High reflection state gold is prepared using magnetron sputtering method
Belong to film layer, the 7th step products obtained therefrom is put into magnetron sputtering cavity, target selects metallic silver target, and shielding power supply uses direct current
Source, power density 1w/cm2, atmosphere pure argon, pressure 0.5Pa, sputtering time 5 minutes, the argent for obtaining surfacing is thin
Film, as high reflection state metallic diaphragm, it is seen that light reflectivity 65%, thickness 200m.On the side of high reflection state metallic diaphragm
Edge pin, lay the circuit that can be connected with electrode.
3rd step：Media coating is prepared on high reflection state metallic diaphragm：Media coating is prepared using magnetron sputtering method, will
Second step products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses direct current
Power supply, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering
2 minutes time, acquisition thickness are 10nm zinc-oxide films as media coating.
4th step：The first photochromic layer is prepared on media coating：Using magnetron sputtering method, the 3rd step products obtained therefrom is put into
Magnetron sputtering cavity, target select metal nickel chromium triangle target (Cr 50%), and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 10%, pressure control 1Pa, sputtering time 10
Minute, nickel oxide chromium oxide mixture mixture film is obtained, as the first photochromic layer；The pattern of first photochromic layer is without fixed
Type, the sheet resistivity of the first photochromic layer is 50K Ω/, thickness 100nm.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700m's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, acquisition thickness are 500nm tungsten oxide films, are unformed porosity and looseness as the second photochromic layer
Film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm zinc-oxide films as media coating.
8th step：Transparent conductor layer is prepared on media coating：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine sheet resistivity, surface
Sheet resistance 50K Ω/, thickness 100nm.In the edge pin of transparent conductor layer, the circuit that can be connected with electrode is laid.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Product is put into magnetron sputtering cavity, target use silicon target, and for purity better than 99%, shielding power supply uses dc source, and power is close
Spend 6w/cm2, atmosphere uses argon gas, pressure control 0.5Pa, sputtering time 60 minutes, obtains the silica that thickness is 500nm and make
For protective layer.
The device of this structure can between reflection and absorption reversible transformation, can be applied on vehicle glare proof mirror.Instead
The reflectance spectrum figure of emitting electrochromic device is identical with Fig. 5.Metallic state reflectivity is 75%, and the reflectivity of colored state is
15%.
The first described photochromic layer shows as reflecting state when being ion implanted, it is seen that light reflectivity 65%；When ion moves
Coloured state is shown as when going out, it is seen that light reflectivity 15%；The second described photochromic layer shows as coloured state when ion implanting,
Visible reflectance is 15%；Show as reflecting state when ion is moved out, it is seen that light reflectivity 65%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture mixed layer, it is seen that light transmission rate is more than 75%.
Under environment temperature, under 2.5V positive voltages, 6s internal reflections rate is from 75% near 15%, under 2.5V negative voltages in 2s
75% is risen to from 15%.
Embodiment 9
The total solids electrochromic device of the present embodiment, by the transparency carrier set gradually from top to bottom, the first functional layer,
Media coating, the first photochromic layer, ion provides and conducting shell, the second photochromic layer, media coating, the second functional layer and protective layer group
Into；First functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer is high reflection state metal film
Layer, the second functional layer is transparent conductor layer.When applying voltage, ion transmits between the first photochromic layer and the second photochromic layer,
The transmitance or reflectivity of total solids electrochromic device change.
Described transparency carrier is common glass substrates；Transparent conductor layer is ITO layer；First photochromic layer is nickel oxide oxygen
Change chromium mixture layer, the wherein content of chromium oxide is 5%, and high reflection state metallic diaphragm is silver layer；Media coating is zinc oxide film.
Ion provides and conducting shell is tantalic acid lithium layer, can supply lithium ion.Protective layer is silicon oxide layer.Second photochromic layer is tungsten oxide
Photochromic layer.
The preparation method of described total solids electrochromic device is：
The first step：Clean transparency carrier；By common glass substrates with detergent be cleaned by ultrasonic ten minutes, after rushed with clear water
Wash, be put into hot air drying box and dry, check whether glass surface has visible internal injury, out-of-flatness etc., it is ensured that glass surface is clean and tidy.
Second step：High reflection state metallic diaphragm is prepared on the transparent substrate：High reflection state gold is prepared using magnetron sputtering method
Belong to film layer, the 7th step products obtained therefrom is put into magnetron sputtering cavity, target selects metallic silver target, and shielding power supply uses direct current
Source, power density 1w/cm2, atmosphere pure argon, pressure 0.5Pa, sputtering time 5 minutes, the argent for obtaining surfacing is thin
Film, as high reflection state metallic diaphragm, it is seen that light reflectivity 65%, thickness 200nm.On the side of high reflection state metallic diaphragm
Edge pin, lay the circuit that can be connected with electrode.
3rd step：Media coating is prepared on high reflection state metallic diaphragm：Media coating is prepared using magnetron sputtering method, will
Second step products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses direct current
Power supply, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering
2 minutes time, acquisition thickness are 10nm zinc-oxide films as media coating.
4th step：The first photochromic layer is prepared on media coating：Using magnetron sputtering method, the 3rd step products obtained therefrom is put into
Magnetron sputtering cavity, target select metal nickel chromium triangle target (Cr 5%), and purity is better than 99%, and shielding power supply uses dc source, work(
Rate density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 10%, pressure control 1Pa, sputtering time 10
Minute, nickel oxide chromium oxide mixture film is obtained, as the first photochromic layer；The pattern of first photochromic layer is unformed, and first
The sheet resistivity of photochromic layer is 50K Ω/, thickness 100nm.
5th step：Ion offer and conducting shell are provided on the first photochromic layer：Prepared using magnetron sputtering method, by the 4th step
Products obtained therefrom is put into magnetron sputtering cavity, and target selects lithium tantalate target, and purity is better than 99%, and shielding power supply selects radio frequency electrical
Source, power density 3w/cm2, atmosphere uses pure argon, and pressure control 1Pa, sputtering time 20 minutes, it is 700nm's to obtain thickness
Ion provides and conducting shell, and ion provides and conducting shell is undefined structure.
6th step：The second photochromic layer is prepared in ion offer and conducting shell：It is thin that tungsten oxide is prepared using magnetron sputtering method
Film, the 5th step products obtained therefrom is put into magnetron sputtering cavity, target selects metal tungsten target, and purity is better than 99%, and shielding power supply is adopted
With dc source, power density 1w/cm2, atmosphere uses argon oxygen gas mixture, and wherein oxygen volume ratio is 6%, pressure control
2Pa, sputtering time 20 minutes, acquisition thickness are 500nm tungsten oxide films, are unformed porosity and looseness as the second photochromic layer
Film, it is made up of armorphous nano particle, sheet resistivity is 50K Ω/.
7th step：Media coating is prepared on the second photochromic layer：Media coating is prepared using magnetron sputtering method, by second step
Products obtained therefrom is put into magnetron sputtering cavity, and target uses metallic zinc target, and purity is better than 99%, and shielding power supply uses dc source,
Power density 1w/cm2, atmosphere uses argon oxygen gas mixture, wherein oxygen volume ratio 20%, pressure control 1Pa, sputtering time 2
Minute, acquisition thickness is 10nm zinc-oxide films as media coating.
8th step：Transparent conductor layer is prepared on media coating：Transparent conductor layer is prepared using magnetron sputtering method, will
Glass substrate is put into magnetron sputtering cavity, and target selects ITO target, and shielding power supply uses dc source, power density 1w/cm2,
Atmosphere pure argon, pressure 0.3Pa, sputtering time ten minutes, the ITO conducting films of surfacing are obtained, determine sheet resistivity, surface
Sheet resistance 50K Ω/, thickness 100m.In the edge pin of transparent conductor layer, the circuit that can be connected with electrode is laid.
9th step：Protective layer is prepared in the second functional layer：Protection film layer is prepared using magnetron sputtering method, by the 8th step institute
Product is put into magnetron sputtering cavity, target use silicon target, and for purity better than 99%, shielding power supply uses dc source, and power is close
Spend 6w/cm2, atmosphere uses argon gas, pressure control 0.5Pa, sputtering time 60 minutes, obtains the silica that thickness is 500nm and make
For protective layer.
The device of this structure can between reflection and absorption reversible transformation, can be applied on vehicle glare proof mirror.Instead
The reflectance spectrum figure of emitting electrochromic device is identical with Fig. 5.Metallic state reflectivity is 65%, and the reflectivity of colored state is
15%.
The first described photochromic layer shows as reflecting state when being ion implanted, it is seen that light reflectivity 65%；When ion moves
Coloured state is shown as when going out, it is seen that light reflectivity 15%；The second described photochromic layer shows as coloured state when ion implanting,
Visible reflectance is 15%；Show as reflecting state when ion is moved out, it is seen that light reflectivity 65%.Between -300 DEG C of room temperature
The first photochromic layer is heated, obtains transparent nickel oxide chromium oxide mixture, it is seen that light transmission rate is more than 75%.
Under environment temperature, under 2.5V positive voltages, 6s internal reflections rate is from 75% near 15%, under 2.5V negative voltages in 2s
75% is risen to from 15%.
Claims (12)
1. a kind of total solids electrochromic device, it is characterised in that including the transparency carrier set gradually from top to bottom, the first work(
Ergosphere, media coating, the first photochromic layer, ion offer and conducting shell, the second photochromic layer, media coating and the second functional layer；The
One functional layer and the second functional layer can be connected with electrode；Wherein, the first described functional layer and the second functional layer are all transparent
Conductor layer, or, one in the first functional layer and the second functional layer is transparent conductor layer, and another is metallic diaphragm.
2. total solids electrochromic device as claimed in claim 1, it is characterised in that when applying voltage, ion becomes first
Transmitted between chromatograph and the second photochromic layer, the transmitance or reflectivity of total solids electrochromic device change.
3. total solids electrochromic device as claimed in claim 1, it is characterised in that the first described photochromic layer is nickel oxide
Chromium oxide mixture layer.
4. total solids electrochromic device as claimed in claim 1, it is characterised in that described nickel oxide chromium oxide mixture
Chromic oxide content is 0-50% in layer, and is not 0.
5. total solids electrochromic device as claimed in claim 1, it is characterised in that the first described photochromic layer is planted in ion
It is fashionable to show as transparent state, it is seen that light transmission rate is more than or equal to 75%；Coloured state is shown as when ion is moved out, it is seen that light passes through
Rate is less than or equal to 15%；The second described photochromic layer shows as coloured state when ion implanting, it is seen that light transmission rate is less than or equal to
10%；Transparent state is shown as when ion is moved out, it is seen that light transmission rate is more than or equal to 75%.
6. total solids electrochromic device as claimed in claim 1, it is characterised in that the outside of the second described functional layer is also
Provided with protective layer.
7. total solids electrochromic device as claimed in claim 6, it is characterised in that described transparency carrier is simple glass
Substrate, quartz glass substrate or plastic base；The second described photochromic layer is tungsten oxide photochromic layer, described electrically conducting transparent
The material of body layer is ITO, FTO, at least one of ATO and AZO；Described media coating is containing silica, silicon nitride, oxidation
At least one of zinc, aluminum oxide and AZO；Described ion provides and conducting shell contains in lithium tantalate and lanthanium titanate lithium at least
It is a kind of；Described metallic diaphragm is high reflection state metallic diaphragm；Described protective layer be metal level, inorganic oxide layer or
Macromolecule membrane.
8. total solids electrochromic device as claimed in claim 1, it is characterised in that the surface side of the first described photochromic layer
Resistance is more than or equal to 50K Ω/, and thickness is in 100-400nm；The sheet resistivity of the second described photochromic layer be more than or equal to 50K Ω/
, thickness is in 100-900nm；The sheet resistivity of described transparent conductor layer is less than or equal to 100 Ω/, thickness 50-
300nm；The thickness of described metallic diaphragm is in 50nm-800nm；The thickness of described media coating is 5-200nm；It is described from
Son provides and the thickness of conducting shell is 200-800nm.
9. total solids electrochromic device as claimed in claim 1, it is characterised in that maximum visible reflectance adjustable range
For 10-75%.
10. the preparation method of the total solids electrochromic device any one of claim 1-9, it is characterised in that including：
The first step：Clean transparency carrier；
Second step：The first functional layer is prepared on the transparent substrate, lays the circuit that can be connected with electrode；
3rd step：Media coating is prepared in the first functional layer；
4th step：The first photochromic layer is prepared on media coating；
5th step：Ion offer and conducting shell are provided on the first photochromic layer；
6th step：The second photochromic layer is prepared in ion offer and conducting shell；
7th step：Another media coating is prepared on the second photochromic layer；
8th step：The second functional layer is prepared on media coating, lays the circuit that can be connected with electrode；
9th step：Protective layer is prepared in the second functional layer.
11. the total solids electrochromic device any one of claim 1-9 is in automobile outer rear-view mirror, inside rear-view mirror, vapour
Chinese herbaceous peony wind shield glass wind shield, side window glass and roof glass, interior dazzle the application in mirror, or external wall.
12. a kind of automobile rearview mirror, it is characterised in that contain the total solids electrochromism any one of claim 1-9
Device.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710483147.4A CN107390445A (en) | 2017-06-22 | 2017-06-22 | A kind of total solids electrochromic device and preparation method thereof |
| PCT/CN2017/095378 WO2018232839A1 (en) | 2017-06-22 | 2017-08-01 | Total-solid electrochromic device and preparation method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710483147.4A CN107390445A (en) | 2017-06-22 | 2017-06-22 | A kind of total solids electrochromic device and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107390445A true CN107390445A (en) | 2017-11-24 |
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|---|---|---|---|
| CN201710483147.4A Pending CN107390445A (en) | 2017-06-22 | 2017-06-22 | A kind of total solids electrochromic device and preparation method thereof |
Country Status (2)
| Country | Link |
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| CN (1) | CN107390445A (en) |
| WO (1) | WO2018232839A1 (en) |
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| CN108037628A (en) * | 2017-12-25 | 2018-05-15 | 兰州空间技术物理研究所 | Electrochomeric films that a kind of performance is stablized and preparation method thereof |
| TWI679483B (en) * | 2018-04-17 | 2019-12-11 | 台灣玻璃工業股份有限公司 | Improved electronically controlled all-solid-state intelligent dimming product and its glass window |
| CN111624829A (en) * | 2019-02-27 | 2020-09-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Colorful electrochromic structure, preparation method and application thereof |
| CN112180648A (en) * | 2019-07-03 | 2021-01-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Optical film structure, its preparation method and application |
| CN112835241A (en) * | 2019-11-25 | 2021-05-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electronic device and method for hiding functional components based on colorful electrochromic structure |
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| CN112826183A (en) * | 2019-11-25 | 2021-05-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | A color-controllable multi-color smart bracelet and method for controlling color changes |
| CN112987427A (en) * | 2019-12-14 | 2021-06-18 | 传奇视界有限公司 | Electro-dimming glass and preparation method thereof |
| CN114690500A (en) * | 2020-12-28 | 2022-07-01 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide-based wide-spectrum electrochromic device and preparation method and application thereof |
| CN114690500B (en) * | 2020-12-28 | 2023-10-13 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide-based broad spectrum electrochromic device and its preparation method and application |
| CN115202124A (en) * | 2021-04-02 | 2022-10-18 | 丰田自动车株式会社 | Electrically-controlled color film and vehicle outer plate |
| CN117389085A (en) * | 2023-12-13 | 2024-01-12 | 江苏繁华应材科技股份有限公司 | Electrochromic anti-dazzle mirror and manufacturing method thereof |
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| Publication number | Publication date |
|---|---|
| WO2018232839A1 (en) | 2018-12-27 |
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