CN109298579A - A kind of full-solid electrochromic device and preparation method thereof - Google Patents
A kind of full-solid electrochromic device and preparation method thereof Download PDFInfo
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- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1506—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
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- G—PHYSICS
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- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/155—Electrodes
Abstract
A kind of full-solid electrochromic device and preparation method thereof, it is related to a kind of electrochromic device and preparation method thereof.The invention aims to solve the problems, such as that the full-solid electrochromic material color change of existing method preparation is slow, production difficulty is big and high production cost.A kind of full-solid electrochromic device is made of substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer and top conductive layer；The substrate is glass；The bottom conductive layer and top conductive layer is two electrodes of full-solid electrochromic device；The material of first photochromic layer and the second photochromic layer is electrochromic material, and the material of at least one photochromic layer is containing lithium salts in the first photochromic layer and the second photochromic layer.Method: bottom conductive layer, the first photochromic layer, the second photochromic layer and top conductive layer are prepared using empty coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation respectively in substrate.The present invention is suitable for preparing full-solid electrochromic device.
Description
Technical field
The present invention relates to a kind of electrochromic devices and preparation method thereof.
Background technique
Electrochromism refers to that material makes the valence state and chemical group of material under DC Electric Field, inside ion intercalation materials
There is a phenomenon where reversible transitions so as to cause the optical properties of material for the raw reversible change of distribution.There are many kinds of electrochromic materials,
It mainly include transition metal oxide, conducting polymer, small molecule dyes and complex compound etc..The electricity assembled by electrochromic material
Mutagens color device has a wide range of applications, such as smart window, Anti-glare rearview mirror, space flight thermal control and aircraft windows.Therefore novel
Safe and reliable, inexpensive electrochromic device technology of preparing research significance it is very great.
Full-solid electrochromic technology mostly uses independent layer containing lithium electrolyte or lithium metal as discoloration ion at present, but
There are still some problems, and when such as using independent containing the lithium electrolyte layer, electrolyte layer ionic resistance with higher itself can shadow
Transmission of the ion in entire device is rung, thus slow down device color change, generally more than ten seconds to more than ten minutes.And it uses
Although the method for splash-proofing sputtering metal lithium can solve the high problem of electrolyte layer ionic resistance, but lithium metal property is active, target sheet
Preparation, transport and the storage of body are more difficult, and sputtering difficulty is big.
Summary of the invention
The invention aims to solve, the full-solid electrochromic material color change of existing method preparation is slow, production is difficult
The problem of degree is big and high production cost, and a kind of full-solid electrochromic device is provided and preparation method thereof.
A kind of full-solid electrochromic device is by substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer and top conductive layer
Composition；The substrate is glass；The bottom conductive layer and top conductive layer is two electrodes of full-solid electrochromic device；
The material of first photochromic layer and the second photochromic layer is electrochromic material, and in the first photochromic layer and the second photochromic layer extremely
The material of a few photochromic layer is containing lithium salts.
A kind of preparation method of full-solid electrochromic device, is completed by the following steps:
One, bottom is prepared in substrate using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Conductive layer；
Two, it is made on the conductive layer of bottom using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Standby first photochromic layer；
Three, using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation on the first photochromic layer
Prepare the second photochromic layer；
Four, using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation on the second photochromic layer
Preparation top conductive layer, obtains full-solid electrochromic device.
The principle of the present invention and advantage:
One, a kind of full-solid electrochromic device of the present invention is by substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer
With top conductive layer composition, two electrodes of indsole conductive layer and top conductive layer as full-solid electrochromic device, first becomes
Chromatograph and the second photochromic layer are as two electrochromic layers, unlike other methods, the first photochromic layer and the second photochromic layer
In at least one photochromic layer be containing lithium salts；The full-solid electrochromic device of this structure had both possessed good electrochromic property,
The difficulty and cost in production process are reduced again, are had great importance；
Two, a kind of full-solid electrochromic device of the preparation present invention does not need the active lithium metal of property, it is possible to reduce raw
It produces, the cost of storage；A kind of full-solid electrochromic device of the present invention does not contain individual electrolyte layer, so entire device
Performance is better than the electrochromic device with electrolyte layer structure；
Three, colour change function can be realized after the completion of full-solid electrochromic device prepared by the present invention preparation, it can also be into
Row heat treatment optimization colour change function, heat treatment carry out in vacuum, air atmosphere or inert gas atmosphere.
Four, a kind of full-solid electrochromic device of the present invention has good electrochromic property, transmitance change modulates
Amplitude is 1%~75%, and Coloring Time is within 30 seconds.
The present invention is suitable for preparing full-solid electrochromic device.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of full-solid electrochromic device described in specific embodiment one, and 1 is base in figure
Bottom, 2 be bottom conductive layer, and 3 be the first photochromic layer, and 4 be the second photochromic layer, and 5 be top conductive layer.
Specific embodiment
Specific embodiment 1: embodiment is described with reference to Fig. 1, a kind of full-solid electrochromic device of present embodiment
It is made of substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer and top conductive layer；The substrate is glass；The bottom
Two electrodes of conductive layer and top conductive layer as full-solid electrochromic device；First photochromic layer and the second photochromic layer
Material be electrochromic material, and in the first photochromic layer and the second photochromic layer at least one photochromic layer material be containing lithium salts.
Fig. 1 is a kind of structural schematic diagram of full-solid electrochromic device described in specific embodiment one, and 1 is base in figure
Bottom, 2 be bottom conductive layer, and 3 be the first photochromic layer, and 4 be the second photochromic layer, and 5 be top conductive layer.
Specific embodiment 2: the differences between this implementation mode and the specific implementation mode are that: the thickness of the bottom conductive layer
Degree is 3nm~500nm；The described top conductive layer with a thickness of 3nm~500nm.Other steps are same as the specific embodiment one.
Specific embodiment 3: one of present embodiment and specific embodiment one or two difference are: described first
Photochromic layer with a thickness of 30nm~800nm；Second photochromic layer with a thickness of 30nm~800nm.Other steps and specific
Embodiment one or two is identical.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: leading at the bottom
Electric layer be tin indium oxide, Al-Doped ZnO, fluorine-doped tin oxide, containing one of Ag films and graphene or in which several mixing
Object.Other steps are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: leading on the top
Electric layer be tin indium oxide, Al-Doped ZnO, fluorine-doped tin oxide, containing one of Ag films and graphene or in which several mixing
Object.Other steps are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: described is electroluminescent
Off-color material is oxide and the mixture containing one or both of lithium salts.Other steps and one to five phase of specific embodiment
Together.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: the oxidation
Object is one of tungsten oxide, nickel oxide, vanadium oxide, tantalum oxide, titanium oxide and cobalt oxide or in which several compounds.It is other
Step is identical as specific embodiment one to six.
Specific embodiment 8: one of present embodiment and specific embodiment one to seven difference are: described contains lithium
Salt is one of tungstate lithium, lithium nickelate, lithium vanadate, lithium tantalate, lithium titanate and cobalt acid lithium or in which several compounds.It is other
Step is identical as specific embodiment one to seven.
Specific embodiment 9: present embodiment is a kind of preparation method of full-solid electrochromic device, it is by following
What step was completed:
One, bottom is prepared in substrate using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Conductive layer；
Two, it is made on the conductive layer of bottom using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Standby first photochromic layer；
Three, using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation on the first photochromic layer
Prepare the second photochromic layer；
Four, using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation on the second photochromic layer
Preparation top conductive layer, obtains full-solid electrochromic device.Other steps are identical as specific embodiment one to eight.
The principle and advantage of present embodiment:
One, a kind of full-solid electrochromic device of present embodiment is become by substrate, bottom conductive layer, the first photochromic layer, second
Chromatograph and top conductive layer composition, two electrodes of indsole conductive layer and top conductive layer as full-solid electrochromic device, the
One photochromic layer and the second photochromic layer are as two electrochromic layers, and unlike other methods, the first photochromic layer and second becomes
At least one photochromic layer is containing lithium salts in chromatograph；The full-solid electrochromic device of this structure had both possessed good electrochromism
Can, and the difficulty and cost in production process are reduced, have great importance；
Two, a kind of preparation full-solid electrochromic device of present embodiment does not need the active lithium metal of property, can subtract
Few cost for producing, storing；A kind of full-solid electrochromic device of present embodiment does not contain individual electrolyte layer, so whole
The performance of a device is better than the electrochromic device with electrolyte layer structure；
Three, colour change function can be realized after the completion of the full-solid electrochromic device preparation of present embodiment preparation, it can also
To carry out heat treatment optimization colour change function, heat treatment carries out in vacuum, air atmosphere or inert gas atmosphere；
Four, a kind of full-solid electrochromic device of present embodiment has good electrochromic property, transmitance variation
Modulation amplitude is 1%~75%, and Coloring Time is within 30 seconds.
Present embodiment is suitable for preparing full-solid electrochromic device.
Specific embodiment 10: the difference of present embodiment and specific embodiment nine is: being obtained to step 4 complete
Solid-state electrochromic device is heat-treated, and heat treatment carries out in vacuum, air atmosphere or inert gas atmosphere, heat treatment temperature
Degree is 10 DEG C~500 DEG C, and heat treatment time is 10min~500min；The inert gas is argon gas or nitrogen.Other steps
It is identical as specific embodiment nine.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one: a kind of full-solid electrochromic device is by substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer
With top conductive layer composition；The substrate is glass；The bottom conductive layer and top conductive layer is as full-solid electrochromic device
Two electrodes of part；A kind of preparation method of full-solid electrochromic device is completed by the following steps:
One, the bottom conductive layer with a thickness of 200nm is prepared in substrate using magnetron sputtering method；
Bottom conductive layer described in step 1 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 0.5Pa, sputtering power 50W, deposition atmosphere is argon gas, sputtering
Time is 20min；
Two, the first photochromic layer with a thickness of 420nm is prepared on the conductive layer of bottom using magnetron sputtering method；
First photochromic layer described in step 2 is tungsten oxide；The parameter of the magnetron sputtering method are as follows: target is tungsten target
Material, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is the mixing of argon gas and oxygen
Gas, wherein the volume ratio of argon gas and oxygen is 1:1, sputtering time 60min；
Three, the second photochromic layer with a thickness of 400nm is prepared on the first photochromic layer using magnetron sputtering method；
Second photochromic layer described in step 3 is lithium nickelate；The parameter of the magnetron sputtering method are as follows: target is nickel acid
Lithium target, sputtering type are radio-frequency sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is argon gas and oxygen
Mixed gas, wherein the volume ratio of argon gas and oxygen is 1:0.1, sputtering time 150min；
Four, the top conductive layer with a thickness of 200nm is prepared on the second photochromic layer using magnetron sputtering method, obtains all solid state electricity
Mutagens color device；
Bottom conductive layer described in step 4 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 0.5Pa, sputtering power 50W, deposition atmosphere is argon gas, sputtering
Time is 20min；
Five, it is heat-treated: full-solid electrochromic device being heat-treated in air atmosphere, heat treatment temperature 350
DEG C, heat treatment time 100min.
The Coloring Time of full-solid electrochromic device prepared by embodiment one is 15 seconds, and transmitance change modulates amplitude is
20%~70%.
Embodiment two: a kind of full-solid electrochromic device is by substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer
With top conductive layer composition；The substrate is glass；The bottom conductive layer and top conductive layer is as full-solid electrochromic device
Two electrodes of part；A kind of preparation method of full-solid electrochromic device is completed by the following steps:
One, the bottom conductive layer with a thickness of 180nm is prepared in substrate using magnetron sputtering method；
Bottom conductive layer described in step 1 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 50W, deposition atmosphere is argon gas, when sputtering
Between be 20min；
Two, the first photochromic layer with a thickness of 400nm is prepared on the conductive layer of bottom using magnetron sputtering method；
First photochromic layer described in step 2 is tungsten oxide；The parameter of the magnetron sputtering method are as follows: target is tungsten target
Material, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is the mixing of argon gas and oxygen
Gas, wherein the volume ratio of argon gas and oxygen is 1:1, sputtering time 60min；
Three, the second photochromic layer with a thickness of 400nm is prepared on the first photochromic layer using magnetron sputtering method；
Second photochromic layer described in step 3 is the compound of tungstate lithium and lithium nickelate, wherein tungstate lithium and lithium nickelate
Molar ratio is 1:1；The parameter of the magnetron sputtering method are as follows: target is the mixture target of tungstate lithium and lithium nickelate, sputters class
Type is radio-frequency sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is the mixed gas of argon gas and oxygen, wherein
The volume ratio of argon gas and oxygen is 1:0.1, sputtering time 150min；
Four, the top conductive layer with a thickness of 180nm is prepared on the second photochromic layer using magnetron sputtering method, obtains all solid state electricity
Mutagens color device；
Bottom conductive layer described in step 4 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 50W, deposition atmosphere is argon gas, when sputtering
Between be 20min；
Five, it is heat-treated: full-solid electrochromic device being heat-treated in air atmosphere, heat treatment temperature 350
DEG C, heat treatment time 100min.
The Coloring Time of full-solid electrochromic device prepared by embodiment two is 7 seconds, and transmitance change modulates amplitude is
15%~70%.
Embodiment three: a kind of full-solid electrochromic device is by substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer
With top conductive layer composition；The substrate is glass；The bottom conductive layer and top conductive layer is as full-solid electrochromic device
Two electrodes of part；A kind of preparation method of full-solid electrochromic device is completed by the following steps:
One, the bottom conductive layer with a thickness of 180nm is prepared in substrate using magnetron sputtering method；
Bottom conductive layer described in step 1 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 50W, deposition atmosphere is argon gas, when sputtering
Between be 20min；
Two, the first photochromic layer with a thickness of 400nm is prepared on the conductive layer of bottom using magnetron sputtering method；
First photochromic layer described in step 2 is tungstate lithium；The parameter of the magnetron sputtering method are as follows: target is wolframic acid
Lithium target, sputtering type are radio-frequency sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is argon gas and oxygen
Mixed gas, wherein the volume ratio of argon gas and oxygen is 1:0.1, sputtering time 150min；
Three, the second photochromic layer with a thickness of 400nm is prepared on the first photochromic layer using magnetron sputtering method；
Second photochromic layer described in step 3 is lithium nickelate；The parameter of the magnetron sputtering method are as follows: target is nickel acid
Lithium target, sputtering type are radio-frequency sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is argon gas and oxygen
Mixed gas, wherein the volume ratio of argon gas and oxygen is 1:0.1, sputtering time 150min；
Four, the top conductive layer with a thickness of 180nm is prepared on the second photochromic layer using magnetron sputtering method, obtains all solid state electricity
Mutagens color device；
Bottom conductive layer described in step 4 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 50W, deposition atmosphere is argon gas, when sputtering
Between be 20min；
Five, it is heat-treated: full-solid electrochromic device being heat-treated in air atmosphere, heat treatment temperature 350
DEG C, heat treatment time 100min.
The Coloring Time of full-solid electrochromic device prepared by embodiment three is 10 seconds, and transmitance change modulates amplitude is
10%~70%.
Example IV: a kind of full-solid electrochromic device is by substrate, bottom conductive layer, the first photochromic layer, the second photochromic layer
With top conductive layer composition；The substrate is glass；The bottom conductive layer and top conductive layer is as full-solid electrochromic device
Two electrodes of part；A kind of preparation method of full-solid electrochromic device is completed by the following steps:
One, the bottom conductive layer with a thickness of 180nm is prepared in substrate using magnetron sputtering method；
Bottom conductive layer described in step 1 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: target is oxidation
Indium tin target, sputtering type are d.c. sputtering, and deposition pressure 1Pa, sputtering power 50W, deposition atmosphere is argon gas, when sputtering
Between be 20min；
Two, the first photochromic layer with a thickness of 400nm is prepared on the conductive layer of bottom using magnetron sputtering method；
First photochromic layer described in step 2 is the mixture of tungsten oxide and tungstate lithium, wherein tungsten oxide and tungstate lithium
Molar ratio is 1:1；The parameter of the magnetron sputtering method are as follows: target is tungsten target material and tungstate lithium target, and sputtering type is direct current
Sputtering and radio-frequency sputtering cosputtering, deposition pressure 1Pa, sputtering power 80W, rf sputtering power 120W, deposition
Atmosphere is the mixed gas of argon gas and oxygen, and wherein the volume ratio of argon gas and oxygen is 1:0.1, sputtering time 80min；
Three, the second photochromic layer with a thickness of 400nm is prepared on the first photochromic layer using magnetron sputtering method；
Second photochromic layer described in step 3 is lithium nickelate；The parameter of the magnetron sputtering method are as follows: target is nickel acid
Lithium target, sputtering type are radio-frequency sputtering, and deposition pressure 1Pa, sputtering power 100W, deposition atmosphere is argon gas and oxygen
Mixed gas, wherein the volume ratio of argon gas and oxygen is 1:0.1, sputtering time 150min；
Four, the top conductive layer with a thickness of 180nm is prepared on the second photochromic layer using magnetron sputtering method, obtains all solid state electricity
Mutagens color device；
Bottom conductive layer described in step 4 is tin indium oxide；The parameter of the magnetron sputtering method are as follows: deposition pressure is
1Pa, sputtering power 50W, deposition atmosphere are argon gas, sputtering time 20min；
Five, it is heat-treated: full-solid electrochromic device being heat-treated in air atmosphere, heat treatment temperature 350
DEG C, heat treatment time 100min.
The Coloring Time of the full-solid electrochromic device of example IV preparation is 6 seconds, and transmitance change modulates amplitude is
2%~65%.
Claims (10)
1. a kind of full-solid electrochromic device, it is characterised in that a kind of full-solid electrochromic device by substrate, bottom conductive layer,
First photochromic layer, the second photochromic layer and top conductive layer composition；The substrate is glass；The bottom conductive layer and top conductive layer
Two electrodes as full-solid electrochromic device；The material of first photochromic layer and the second photochromic layer is electrochromism
Material, and the material of at least one photochromic layer is containing lithium salts in the first photochromic layer and the second photochromic layer.
2. a kind of full-solid electrochromic device according to claim 1, it is characterised in that the thickness of the bottom conductive layer
Degree is 3nm~500nm；The described top conductive layer with a thickness of 3nm~500nm.
3. a kind of full-solid electrochromic device according to claim 1, it is characterised in that first photochromic layer
With a thickness of 30nm~800nm；Second photochromic layer with a thickness of 30nm~800nm.
4. a kind of full-solid electrochromic device according to claim 1, it is characterised in that the bottom conductive layer is oxygen
Change indium tin, Al-Doped ZnO, fluorine-doped tin oxide, containing one of Ag films and graphene or in which several mixtures.
5. a kind of full-solid electrochromic device according to claim 1, it is characterised in that the top conductive layer is oxygen
Change indium tin, Al-Doped ZnO, fluorine-doped tin oxide, containing one of Ag films and graphene or in which several mixtures.
6. a kind of full-solid electrochromic device according to claim 1, it is characterised in that the electrochromic material
For oxide and containing the mixture of one or both of lithium salts.
7. a kind of full-solid electrochromic device according to claim 6, it is characterised in that the oxide is oxidation
One of tungsten, nickel oxide, vanadium oxide, tantalum oxide, titanium oxide and cobalt oxide or in which several compounds.
8. a kind of full-solid electrochromic device according to claim 1 or 6, it is characterised in that described is tungsten containing lithium salts
One of sour lithium, lithium nickelate, lithium vanadate, lithium tantalate, lithium titanate and cobalt acid lithium or in which several compounds.
9. a kind of preparation method of full-solid electrochromic device as described in claim 1, it is characterised in that a kind of all solid state
The preparation method of electrochromic device is completed by the following steps:
One, bottom conduction is prepared in substrate using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Layer；
Two, is prepared on the conductive layer of bottom using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
One photochromic layer；
Three, it is prepared on the first photochromic layer using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Second photochromic layer；
Four, it is prepared on the second photochromic layer using Vacuum Coating method, magnetron sputtering method, vacuum thermal evaporation or e-beam evaporation
Conductive layer is pushed up, full-solid electrochromic device is obtained.
10. a kind of preparation method of full-solid electrochromic device according to claim 9, it is characterised in that step 4
Obtained full-solid electrochromic device is heat-treated, and heat treatment carries out in vacuum, air atmosphere or inert gas atmosphere,
Heat treatment temperature is 10 DEG C~500 DEG C, and heat treatment time is 10min~500min；The inert gas is argon gas or nitrogen.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109709737A (en) * | 2019-02-27 | 2019-05-03 | 暨南大学 | A kind of production method of novel electrochromic film |
| CN110737143A (en) * | 2019-10-30 | 2020-01-31 | 哈尔滨工业大学 | all-solid-state electrochromic devices with quick response and preparation method thereof |
| CN111290186A (en) * | 2020-03-24 | 2020-06-16 | 江苏繁华玻璃股份有限公司 | Method for forming film microstructure of electrochromic device and electrochromic device |
| CN112285981A (en) * | 2020-10-27 | 2021-01-29 | 哈尔滨工业大学 | Preparation method of electrochromic device with high charge storage capacity |
| CN112285982A (en) * | 2020-11-06 | 2021-01-29 | 哈尔滨工业大学 | All-solid-state electrochromic device with lithium aluminum silicate as electrolyte layer and preparation method thereof |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101188886A (en) * | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | An inorganic full-solid electric driven color-changing part and its making method |
| CN102096262A (en) * | 2009-12-09 | 2011-06-15 | 中国科学院物理研究所 | Photoelectric device including lithium titanate membrane electrode and application thereof |
| CN103365017A (en) * | 2013-07-15 | 2013-10-23 | 天津南玻节能玻璃有限公司 | Inorganic all-solid electrochromic device and preparation method thereof |
| CN103771724A (en) * | 2012-10-19 | 2014-05-07 | 中国南玻集团股份有限公司 | All-solid-state film electrochromic glass and preparation method thereof |
| CN104122730A (en) * | 2013-04-27 | 2014-10-29 | 珠海兴业绿色建筑科技有限公司 | Reflection type electrochromism device |
| CN204595399U (en) * | 2015-02-16 | 2015-08-26 | 浙江上方电子装备有限公司 | A kind of electrochomeric glass |
| CN105278198A (en) * | 2015-11-17 | 2016-01-27 | 崔玉柱 | Complementary inorganic full-solid electrochromic device and preparation method thereof |
| CN107045241A (en) * | 2017-05-19 | 2017-08-15 | 浙江大学 | One kind is based on Al3+Full-solid electrochromic device of ion and preparation method thereof |
| CN107300819A (en) * | 2011-07-21 | 2017-10-27 | Sage电致变色显示有限公司 | Simultaneously doped with lithium and the electrochromic nickel oxide of metalic contamination |
| KR20180031145A (en) * | 2016-09-19 | 2018-03-28 | 주식회사 엘지화학 | A Electrochromic Device, method for preparing the same, and Method for Controlling Optical Properties of the same |
-
2018
- 2018-12-07 CN CN201811496768.7A patent/CN109298579A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101188886A (en) * | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | An inorganic full-solid electric driven color-changing part and its making method |
| CN102096262A (en) * | 2009-12-09 | 2011-06-15 | 中国科学院物理研究所 | Photoelectric device including lithium titanate membrane electrode and application thereof |
| CN107300819A (en) * | 2011-07-21 | 2017-10-27 | Sage电致变色显示有限公司 | Simultaneously doped with lithium and the electrochromic nickel oxide of metalic contamination |
| CN103771724A (en) * | 2012-10-19 | 2014-05-07 | 中国南玻集团股份有限公司 | All-solid-state film electrochromic glass and preparation method thereof |
| CN104122730A (en) * | 2013-04-27 | 2014-10-29 | 珠海兴业绿色建筑科技有限公司 | Reflection type electrochromism device |
| CN103365017A (en) * | 2013-07-15 | 2013-10-23 | 天津南玻节能玻璃有限公司 | Inorganic all-solid electrochromic device and preparation method thereof |
| CN204595399U (en) * | 2015-02-16 | 2015-08-26 | 浙江上方电子装备有限公司 | A kind of electrochomeric glass |
| CN105278198A (en) * | 2015-11-17 | 2016-01-27 | 崔玉柱 | Complementary inorganic full-solid electrochromic device and preparation method thereof |
| KR20180031145A (en) * | 2016-09-19 | 2018-03-28 | 주식회사 엘지화학 | A Electrochromic Device, method for preparing the same, and Method for Controlling Optical Properties of the same |
| CN107045241A (en) * | 2017-05-19 | 2017-08-15 | 浙江大学 | One kind is based on Al3+Full-solid electrochromic device of ion and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| FUMIAKI MITSUGI等: "Preparation of inorganic solid state thin film for electrochromic application", 《THIN SOLID FILMS》 * |
| XINGWANG SONG等: "Properties of NiOx and its influence upon all-thin-film ITO/NiOx/LiTaO3/WO3/ITO electrochromic devices prepared by magnetron sputtering", 《VACUUM》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109709737A (en) * | 2019-02-27 | 2019-05-03 | 暨南大学 | A kind of production method of novel electrochromic film |
| CN110737143A (en) * | 2019-10-30 | 2020-01-31 | 哈尔滨工业大学 | all-solid-state electrochromic devices with quick response and preparation method thereof |
| CN111290186A (en) * | 2020-03-24 | 2020-06-16 | 江苏繁华玻璃股份有限公司 | Method for forming film microstructure of electrochromic device and electrochromic device |
| CN111290186B (en) * | 2020-03-24 | 2022-10-18 | 江苏繁华应材科技股份有限公司 | Method for forming film microstructure of electrochromic device and electrochromic device |
| CN112285981A (en) * | 2020-10-27 | 2021-01-29 | 哈尔滨工业大学 | Preparation method of electrochromic device with high charge storage capacity |
| CN112285981B (en) * | 2020-10-27 | 2022-11-01 | 哈尔滨工业大学 | Preparation method of electrochromic device with high charge storage capacity |
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| CN112764286A (en) * | 2021-01-29 | 2021-05-07 | 哈尔滨工业大学 | Thermal control device for intelligently regulating infrared emissivity and preparation method thereof |
| CN112764286B (en) * | 2021-01-29 | 2023-07-07 | 哈尔滨工业大学 | Thermal control device capable of intelligently regulating and controlling infrared emissivity and preparation method thereof |
| CN113204146A (en) * | 2021-05-07 | 2021-08-03 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device taking water vapor as electrolyte and preparation method thereof |
| CN113204146B (en) * | 2021-05-07 | 2023-04-25 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device with water vapor as electrolyte and preparation method thereof |
| CN115872632A (en) * | 2022-12-04 | 2023-03-31 | 航天材料及工艺研究所 | Intelligent thermal control device and preparation method thereof |
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