CN108279541A - A kind of inorganic full-solid electric driven color-changing thin-film device and preparation method thereof that reliability is high - Google Patents
A kind of inorganic full-solid electric driven color-changing thin-film device and preparation method thereof that reliability is high Download PDFInfo
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/1533—Constructional details structural features not otherwise provided for
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/213—SiO2
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/219—CrOx, MoOx, WOx
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/23—Mixtures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/23—Mixtures
- C03C2217/231—In2O3/SnO2
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/155—Deposition methods from the vapour phase by sputtering by reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/1533—Constructional details structural features not otherwise provided for
- G02F2001/1536—Constructional details structural features not otherwise provided for additional, e.g. protective, layer inside the cell
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Abstract
This application provides a kind of inorganic full-solid electric driven color-changing thin-film device and preparation method thereof, which includes：Substrate；The first protective layer, the first transparent conductor layer, the second protective layer, inorganic photochromic layer, inorganic ions conducting shell, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protective layer being arranged in substrate successively.The above-mentioned film combinations of the present invention are inorganic full-solid structure, and all film layers are inorganic solid-state, and film material activity will not be changed over time to decompose and be reduced with activity, and storeroom will not have mutual etching problem.Multiple protective layers are arranged in the present invention, mainly avoid transparent conductor layer internal short-circuit, and discoloration is avoided to fail.Therefore, the present invention enhances each film performance, can be accurately controlled to light percent of pass, improves the response time, improves film forming yields, extends the Electrochromic device service life, reduces cost.
Description
Technical field
The present invention relates to the fields of the electrochemical appliance with reciprocal optical and/or transfer of energy properties that can be automatically controlled, especially
It is related to a kind of inorganic full-solid electric driven color-changing thin-film device and preparation method thereof, and yields, reliability are high.
Background technology
With the rapid growth of the world economy, huge resource and ring have also been paid while obtaining every great achievement
The contradiction of border cost, economic development and resource environment is increasingly sharp.Energy demand is nervous, and greenhouse gas emission causes global climate
It warms and also becomes clear day by day, therefore Development of Novel energy-saving material, reinforcing energy-saving and emission-reduction work is particularly important.For traditional glass
For glass, it is only capable of the fixed transmitance for changing light, therefore electrochomeric glass comes into being, and belongs to the model of energy-saving and emission-reduction
Farmland.Using electrochromism technology obtain electrochomeric glass under electric field action, not only can actively regulate light absorptivity,
Transmitance improves natural lighting intensity, it is also an option that property absorb or reflect the expansion of extraneous heat radiation and internal heat
It dissipates, consumed huge energy is kept the temperature to reduce the places such as office block, residential houses, the vehicles.
So-called electrochromism refers to that off-color material passes through H under the action of alternate high existing fringing field+、Li+、Na+Equal alkali gold
Belong to the insertion of ion or other transportable ions and take off and owe, reversible electrochemical reaction occurs for off-color material, makes its optical property
Reversible linear change occurs with the variation of extra electric field.Thus, it is possible to easily according to environment temperature, illumination condition, artificial
Wish etc. is relaxed by realizing the accuracy controlling to light reflection, transmission, absorption to the control of extra electric field with meeting energy saving, vision
The different personal needs such as appropriateness, secret protection.Therefore, electrochromic device can be widely applied to building, vehicles etc.
Field has broad application prospects in today that the energy is increasingly in short supply.
Existing electrochromism technology is in the majority with liquid crystal molecule technology and organic material, and liquid crystal molecule technology is i.e. by two
The filling liquid crystal molecule of electrode layer applies voltage to electrode layer and changes Liquid Crystal Molecules Alignment so that there is device light to pass through switch
Effect, but this technology cannot linearly change light percent of pass.The electrochromic device of organic material is affected by temperature cycles,
Service life is seriously limited.
And prior art discloses some inorganic solid-state electrochomeric films and preparation method thereof, for example, Authorization Notice No.
A kind of full solid thin film electrochomeric glass is reported for the Chinese patent literature of 202953940 U of CN.Full solid thin film electricity
Mutagens color glass includes substrate, also thoroughly comprising the ion barrier sequentially formed by vapour deposition process based on the substrate, first
Bright conductive layer and protective layer, inorganic photochromic layer, inorganic ions conductor layer, inorganic ions storage layer, the second transparency conducting layer and guarantor
Sheath.The full solid thin film electrochomeric glass is made of solid material, increases the stability that product uses, but film forming
Yields is low, and production cost is higher.
Invention content
In view of this, a kind of inorganic full-solid electric driven color-changing thin-film device of the application offer and preparation method thereof, this is inorganic
Full-solid electrochromic thin-film device can accurately control light percent of pass, while film forming yields is high, reduce production cost.
The present invention provides a kind of inorganic full-solid electric driven color-changing thin-film device, including：
Substrate；
The first protective layer for being arranged in substrate successively, the first transparent conductor layer, the second protective layer, inorganic photochromic layer, nothing
Machine ion conducting layer, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protective layer.
Preferably, the material of first protective layer, the second protective layer, third protective layer and the 4th protective layer independently selects
From SiO2、TiO2And Si3N4In it is one or more.
Preferably, the light penetration ＞ 90% of the substrate；The thickness of first protective layer and the 4th protective layer is only
It is on the spot 10nm~50nm.
Preferably, the thickness of second protective layer and third protective layer, which is independently less than, is equal to 100nm.
Preferably, the thickness of first transparency conducting layer and the second transparency conducting layer independently is 20nm~500nm, institute
The thickness for stating inorganic photochromic layer is 50nm~500nm, and the thickness of the inorganic ion-storage layer is 50nm~500nm.
Preferably, the thickness of the inorganic ions conducting shell is 5nm~100nm, within membrane uniformity control ± 1%.
Preferably, the material of the inorganic ions conducting shell is selected from the compound of doping, and the compound is preferably silicic acid
It is one or more in salt, phosphate, borate, tantalates, tungsten oxide, silica and tantalum oxide；The dopant is preferred
For H+, it is lithium, one or more in sodium and potassium.
Preferably, the material of first transparent conductor layer and the second transparent conductor layer is independently selected from metal or doping
Metal oxide；The metal oxide of the doping is preferably tin indium oxide, adulterates the SnO of fluorine2Or the zinc oxide of adulterated al；Institute
It is preferably platinum, gold, silver, copper or aluminium to state metal.
Preferably, the material of the inorganic photochromic layer and inorganic ion-storage layer correspondingly be selected from cathode off-color material,
It is one or more in anode off-color material and bipolar off-color material.
The present invention provides a kind of preparation method of inorganic full-solid electric driven color-changing thin-film device, includes the following steps：In base
On bottom, by way of vapor deposition, the first protective layer, the first transparent conductor layer, the second protective layer, inorganic discoloration are sequentially formed
Layer, inorganic ions conducting shell, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protective layer, obtain nothing
Machine full-solid electrochromic thin-film device.
Inorganic full-solid electric driven color-changing thin-film device provided by the invention includes：Substrate, the first protective layer, first transparent are led
It is body layer, the second protective layer, inorganic photochromic layer, inorganic ions conducting shell, inorganic ion-storage layer, third protective layer, second transparent
Conductor layer and the 4th protective layer.The above-mentioned film combinations of the present invention are inorganic full-solid structure, and all film layers are inorganic solid-state, film
Layer material activity will not be changed over time to decompose and be reduced with activity, and storeroom will not have mutual etching problem.This hair
The bright multiple protective layers of setting, mainly avoid transparent conductor layer internal short-circuit, discoloration are avoided to fail.Therefore, the present invention enhances each film
Layer performance, can accurately control light percent of pass, improve the response time, improve film forming yields, extend the Electrochromic device longevity
Life, reduces cost.
Description of the drawings
Fig. 1 is the schematic cross-section of inorganic all-solid electrochromic device provided in an embodiment of the present invention；
Fig. 2 is the electrochromic device schematic cross-section according to the embodiment of the present invention in colored state；
Fig. 3 is the electrochromic device schematic cross-section according to the embodiment of the present invention in bleached state.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of inorganic full-solid electric driven color-changing thin-film devices, including：
Substrate；
The first protective layer for being arranged in substrate successively, the first transparent conductor layer, the second protective layer, inorganic photochromic layer, nothing
Machine ion conducting layer, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protective layer.
Reversible electrochemical reaction can occur inside inorganic full-solid electric driven color-changing thin-film device provided by the invention, it pair can
Light-exposed, infrared light, ultraviolet light light transmission rate accurately controlled, can absorb certain spectral region in light, reduce light
Reflectivity.Meanwhile the present invention has higher film forming yields, production cost relatively low.
Fig. 1 is the schematic cross-section of inorganic all-solid electrochromic device provided in an embodiment of the present invention, and in Fig. 1,1 is glass
Glass substrate, 2 be the first protective layer, 3 be the first transparent conductor layer, 4 be the second protective layer, 5 be inorganic photochromic layer, 6 for it is inorganic from
Sub- conducting shell, 7 be inorganic ion-storage layer, and 8 be third protective layer, and 9 be the second transparent conductor layer, and 10 be the 4th protective layer.
Fig. 1 is referred to, inorganic full-solid electric driven color-changing thin-film device provided in an embodiment of the present invention includes substrate 1；Substrate 1
With certain optics, calorifics, electrical and mechanical performance, general light penetration>90%, surface roughness is 5nm~50nm.
The surface roughness and uniformity concept is not much different to a certain extent；Surface roughness：The distance of peaks and troughs,
Certain point is raised at a distance from recess with respect to subsequent point.Uniformity：It can be used for describing the relative distance in face and face.Test
Method：It is obtained using step instrument measurement.The present invention is usually using glass, mirror or plastic products etc. as substrate；The present invention
Embodiment is using glass substrate as substrate, it is preferred to use ultrawhite glass (glass) substrate, thickness can be 1.7mm~2mm.
The inorganic full-solid electric driven color-changing thin-film device includes：The first protective layer 2 being arranged on the base 1.First protects
The material of sheath 2 is preferably SiO2、TiO2And Si3N4One or more, more preferably silica (SiO2)；Its specific thickness
It can be determined according to the transmitance of substrate demand, usually 10nm~50nm, preferably 10nm~30nm, more preferably 20nm, film
Layer uniformity controlling is in ± 2% range.When some embodiments of the invention use substrate of glass, the main work(of the first protective layer 2
Photochromic layer performance can be avoided to be affected to prevent the sodium ion of glass substrate from migrating；Other embodiments of the invention are using modeling
It is to protect other functional layers not since substrate has certain flexibility, the major function of the first protective layer 2 when material products are as substrate
It is destroyed.
The inorganic full-solid electric driven color-changing thin-film device includes the first transparent conductor layer 3, is bottom transparent electrode layer,
On the first protective layer 2.The transparent conductor layer can provide electric field, and the material of the first transparent conductor layer 3 can be one kind
The metal oxide of doping or the Multimetal oxide of doping, including but not limited to tin indium oxide (ITO), the SnO for adulterating fluorine2
(FTO) or the transparent conductive materials such as the zinc oxide of adulterated al (AZO)；May be metal coating layer material, the metal include platinum,
Gold, silver, copper or aluminium etc., the embodiment of the present invention preferably use tin indium oxide (ITO) for transparent conductor layer.
In the present invention, the thickness of first transparent conductor layer is usually 20nm~500nm, and preferably 100nm~
350nm, more preferably 150nm~300nm.The sheet resistance of first transparent conductor layer 3 can be 5 Ω -30 Ω, preferably 10 Ω -15 Ω；
Membrane uniformity controls in ± 2%.Wherein, Hitachi cold field emission scanning electron microscope S-4800 detections, side can be used in thicknesses of layers
Resistance detection is using double electrical measurement four-point probes.
On the first transparent conductor layer 3, inorganic full-solid electric driven color-changing thin-film device described in the embodiment of the present invention is provided with
Second protective layer 4 mainly avoids 3 internal short-circuit of the first transparent conductor layer, and causes device portions discoloration failure.Second protective layer
4 material is preferably SiO2、TiO2And Si3N4One or more, more preferably SiO2, with 2 material identical of the first protective layer.Institute
The thickness for stating the second protective layer is preferably smaller than equal to 100nm, more preferably 1nm~50nm, further preferably 10nm~20nm；
Membrane uniformity controls within ± 2%.
The inorganic full-solid electric driven color-changing thin-film device includes inorganic photochromic layer 5, is located on the second protective layer 4；It is main
It is act as the insertion by ion or de- deficient, material generation electrochemical reaction, and the reaction is reversible, to change device
Such as transmitance, absorptivity, reflectivity optical property.The material of the inorganic photochromic layer can be divided into cathode off-color material, anode
Off-color material, bipolar off-color material, cathode off-color material include：Tungsten oxide, doping oxide, molybdenum oxide, niobium oxide, titanium oxide
Deng；Anode off-color material such as nickel oxide, indium oxide are Prussian blue etc.；Bipolar off-color material such as vanadium oxide, cobalt oxide, rhodium oxide
Deng.In the specific device of the embodiment of the present invention, electrochromic layer can include one or more kinds of off-color materials, specific photochromic layer
Material preferably adulterates a certain amount of other materials or ion, including doping H+, lithium, sodium, potassium, molybdenum, metals or the gold such as vanadium or titanium
Belong to compound, such as inorganic photochromic layer is tungsten oxide layer or tungsten oxide lithium layer.
In an embodiment of the present invention, the inorganic photochromic layer is cathode discoloration material layer, preferably tungsten oxide elements doped lithium
Alloy film layer.The thickness of the inorganic photochromic layer can be 50nm~500nm, preferably 150nm~500nm, more preferably 200nm
~450nm；Membrane uniformity ± 2%, material shape are amorphous structure.
The inorganic full-solid electric driven color-changing thin-film device includes inorganic ions conducting shell 6, is located at inorganic photochromic layer 5
On；Main function is to provide high ionic mobility and block electronics movement, promotes off-color material that electrochemical reaction occurs.It is described
The main material of inorganic ions conducting shell includes the substance of one or more suitable ionic conductions, is mainly selected from the chemical combination of doping
Object, the compound are preferably one or more in silicate, phosphate, borate, tungsten oxide, silica and tantalum oxide；
The dopant is preferably H+, it is lithium, one or more in sodium and potassium.In an embodiment of the present invention, the inorganic ions
The common specific material of conducting shell includes but not limited to lithium metasilicate, lithium aluminosilicate, lithium tantalate, lithium borate, lithium phosphate etc..
In an embodiment of the present invention, the thickness of the inorganic ions conducting shell be 5nm~100nm, preferably 10nm~
30nm, more preferably 20nm；Membrane uniformity controls within ± 1%.The thickness and uniformity of this layer are related to entire device
Performance, if thickness is too thick, then Ion transfer speed slowly to influence device change colour the response time, the too thin then technology difficulty of thickness
Greatly, and device production yields is difficult to control.
The inorganic full-solid electric driven color-changing thin-film device includes inorganic ion-storage layer 7, is located at inorganic ions and conducts
On layer 6；It is mainly used for providing ion storage space, structure is generally amorphous.The material and nothing of inorganic ion-storage layer 7
The material of machine photochromic layer 5 is corresponding, and even inorganic photochromic layer 5 selects anode off-color material, then inorganic ion-storage layer 7 selects the moon
Pole off-color material, if inorganic photochromic layer 5 selects cathode off-color material, inorganic ion-storage layer 7 to select anode off-color material.
In present example, inorganic ion-storage layer 7 is anode off-color material, preferably mixes the tungsten oxide nickel of lithium.The inorganic ions
The thickness of accumulation layer is usually 50nm~500nm, preferably 150nm~350nm, more preferably 150nm；Membrane uniformity controls
Within ± 2%.
On inorganic ion-storage layer 7, the inorganic full-solid electric driven color-changing thin-film device includes third protective layer successively
8, the second transparent conductor layer 9.Wherein, third protective layer 8 mainly avoids 9 internal short-circuit of the second transparent conductor layer, and causes device
Part discoloration failure.The material of third protective layer 8 is preferably SiO2、TiO2And Si3N4One or more, more preferably SiO2,
With 2 material identical of the first protective layer.The thickness of the third protective layer, which is preferably smaller than, is equal to 100nm, and more preferably 1nm~
50nm, further preferably 10nm~20nm；Membrane uniformity controls within ± 2%.Wherein, protection film layer thickness can be used
Hitachi cold field emission scanning electron microscope S-4800 is detected.
Second protective layer 4 and third protective layer 8 are arranged the present invention simultaneously in same device, the actual (real) thickness of the two with
Device overall light transmitance matches, and is conducive to improve product yield, reduces production cost.
In an embodiment of the present invention, the second transparent conductor layer 9 is top transparent electrode layer, is located on third protective layer 8.
The material of second transparent conductor layer 9 can be a kind of doping metal oxide or doping Multimetal oxide, including but
The SnO for being not limited to tin indium oxide (ITO), adulterating fluorine2(FTO) or the transparent conductive materials such as the zinc oxide of adulterated al (AZO)；Also may be used
Think that metal coating layer material, the metal include platinum, gold, silver, copper or aluminium etc..First transparent conductor layer 3 and the second transparent conductor
The material of layer 9 can be identical or different；The embodiment of the present invention preferably uses ITO for transparent conductor layer.
In the present invention, the thickness of second transparent conductor layer is usually 20nm~500nm, and preferably 100nm~
350nm, more preferably 150nm~300nm.The sheet resistance of first transparent conductor layer 3 and the second transparent conductor layer 9 is essentially identical；Film
Layer uniformity controlling is in ± 2%.Wherein, Hitachi cold field emission scanning electron microscope S-4800 detections, sheet resistance can be used in thicknesses of layers
Detection is using double electrical measurement four-point probes.
Finally, the inorganic full-solid electric driven color-changing thin-film device described in the embodiment of the present invention includes the 4th protective layer 10,
Air can be completely cut off and moisture is avoided to invade, to achieve the purpose that protection film layer.The material of 4th protective layer 10 is preferably SiO2、
TiO2And Si3N4One or more, more preferably silica, it is identical as the first protective layer material.4th protective layer
Thickness is usually 10nm~50nm, preferably 10nm~30nm, more preferably 20nm, and membrane uniformity is controlled in ± 2% range
It is interior.
In some specific embodiments of the present invention, the combination of device film layer is followed successively by：Protective layer SiO2, thickness 10nm~
50nm；Bottom transparent electrodes layer ITO, thickness 20nm~500nm；Protective layer SiO2, thickness≤100nm；Photochromic layer tungsten oxide layer,
Thickness range 50nm~500nm；Ionic conduction tungsten oxide lithium layer, thickness range 5nm~100nm；Ion storage mixes the oxygen of lithium
Change tungsten nickel layer, thickness range 50nm~500nm.Protective layer SiO2, thickness≤100nm；Top transparent electrode layer ITO, thickness
20nm~500nm；Protective layer SiO2, thickness 10nm~50nm.
In other specific embodiments of the present invention, the combination of device film layer is followed successively by：Protective layer SiO2, thickness 10nm~
30nm；Bottom transparent electrodes layer ITO, thickness 100nm~350nm；Protective layer SiO2, thickness≤50nm；Photochromic layer tungsten oxide layer,
Thickness range 150nm~500nm；Ion conducting layer tungsten oxide lithium layer, thickness range 10nm~30nm；Ion storage mixes lithium
Tungsten oxide nickel layer, thickness range 150nm~350nm.Protective layer SiO2, thickness≤50nm；Top transparent electrode layer ITO, thickness
100nm~350nm；Protective layer SiO2, thickness 10nm~30nm.
Fig. 2 is the electrochromic device schematic cross-section according to the embodiment of the present invention in colored state, according to fig. 2, this
Case select tungsten oxide be used as off-color material, free lithium ion as migration ion, amorphous tungsten oxide nickel layer as from
Sub- accumulation layer.Transparent electrode layer connects DC power supply at two, and photochromic layer side conductor layer connects cathode, accumulation layer side conductor layer
Anode is connect, electric field is formed between two conductor layers so that the lithium ion in ion storage is passed under the action of field strength by ion
Conducting shell moves in photochromic layer, is embedded into photochromic layer hole, and discoloration layer material structures change, to change the light of device
Performance is learned, showing as the transmitance of light reduces, and device color subduing.
Fig. 3 is electrochromic device schematic cross-section according to the embodiment of the present invention in bleached state, in Fig. 2 and Fig. 3,
1 is glass substrate, and 2 be the first protective layer, and 3 be the first transparent conductor layer, and 4 be the second protective layer, and 5 be inorganic photochromic layer, and 6 be nothing
Machine ion conducting layer, 7 be inorganic ion-storage layer, and 8 be third protective layer, and 9 be the second transparent conductor layer, and 10 be the 4th protection
Layer.
According to fig. 3, in conjunction with above-mentioned principle, when reverse power connection, the lithium ion in photochromic layer is under the action of field strength from change
It is taken off in chromatograph and owes out, ion storage to be returned to by ion conducting layer.The optical property of device is restored, and the transmission of light is shown as
Rate increases, and device fades.Device coloration efficiency CE can be given by the following formula：
Wherein：CE(λ)：Coloration efficiency；
Δ OD=In (T bleaches state (λ)/T coloured states (λ))；
Q：Per unit area injects the electronic charge size of electrochromic material；
T bleaches state (λ)：Under (colour fading) state of bleaching, wavelength is the light penetration of λ；
T coloured states (λ)：Under colored state, wavelength is the light penetration of λ.
Therefore, by control unit area on inject unit charge Q by realize electrochomeric films optical density (or comparison
Degree) variation, indicated with coloration efficiency, unit is with cm2/ coulomb indicates；There is the material of higher coloration efficiency to have faster
Response time and better durability.
An embodiment of the present invention provides a kind of preparation methods of inorganic full-solid electric driven color-changing thin-film device, including following step
Suddenly：In substrate, by way of vapor deposition, sequentially form the first protective layer, the first transparent conductor layer, the second protective layer,
Inorganic photochromic layer, inorganic ions conducting shell, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protection
Layer, obtains inorganic full-solid electric driven color-changing thin-film device.
Substrate can be cleaned, be dried by the embodiment of the present invention, into coating system, sequentially form above-mentioned film layer.The substrate
Content with each layer is as previously mentioned, details are not described herein.
Physical vapour deposition (PVD) (Physical Vapor Deposition, PVD) technology indicates under vacuum, to use
Physical method, by material source -- solid or liquid surface are gasificated into gaseous atom, molecule or partial ionization at ion, and by low
It calms the anger body (or plasma) process, in the technology of film of the matrix surface deposition with certain specific function.Physical vapor is heavy
Long-pending main method has：Vacuum evaporation, sputter coating, arc-plasma plating, ion film plating and molecular beam epitaxy etc..
Wherein, under vacuum, using the particle bombardment target surfaces for obtaining function, target material surface atom is made to obtain
Enough energy and the process escaped is known as sputtering；The target material deposition being sputtered is referred to as sputter coating to substrate surface.Sputtering
Incident ion in plated film generally uses glow discharge to obtain, in l0-2Pa~10Pa ranges, so the particle sputtered out is flying
To during matrix, easily collides with the gas molecule in vacuum chamber, keep the direction of motion random, the film of deposition is easy to uniform.
Scale magnetron sputtering plating has gradually developed, and deposition rate is higher, good process repeatability, convenient for automation.
The embodiment of the present invention mainly uses the sputter coating mode in physical vapour deposition (PVD), such as medium frequency reactive sputtering, magnetic control
Sputtering, RF-reactively sputtered titanium, DC pulse sputtering etc., according to common process condition, are sequentially prepared to obtain each of respective thickness
Film layer.
Therefore, electrochromic device made from the embodiment of the present invention is mainly made of following film layer：Substrate, the first protection
Layer, bottom transparent electrode layer, the second protective layer, photochromic layer, ion conducting layer, ion storage, third protective layer, upper layer are transparent
Electrode layer, the 4th protective layer.By applying voltage in bottom transparent electrodes layer and top transparent electrode layer, make between two electrode layers
Electric field is formed, under the action of field strength, the ion in ion storage is embedded into photochromic layer by conducting shell or photochromic layer
In ion de- owe by conducting shell return ion storage.Due to ion insertion or it is de- owe, cause photochromic layer that electricity occurs
Chemical reaction, forms new structure, which has certain blocking, absorption to light, cashes and occurs for photochromic layer color
Variation, to make the transmitance of light change.The present invention can accurately control the transmitance of light；The present invention can be to film layer
Area, migration ionic weight precise quantification, by controlling electrochromic device conduction time and electron injection amount so that electrochromism
Device coloration efficiency can be accurately controlled.In practice, due to the diversity of electrochromic device size, to make device
Color changeable effect it is unified, be unlikely to patch phenomenon occur, need it is unified limit light penetration, to various sizes of electrochromism
The different control power supply of device matching.
Also, multiple protective layers are arranged in the present invention, mainly avoid transparent conductor layer internal short-circuit, avoid discoloration from failing, carry
High film forming yields extends the Electrochromic device service life, reduces cost.In the present invention, the electrochemistry that device inside occurs is anti-
It should be reversible；Light penetration is controllable precise, linear change；Light, reduction in absorbable certain spectral region
Light reflectance.The concrete application field of the present invention includes：The fields such as building curtain wall, space partition, door and window；Camera optical filtering etc.
Need the field of change light spectral；Automobile later stage visor, the military fields such as stealthy, anti-fake.
It is thin to inorganic full-solid electric driven color-changing provided by the present application with reference to embodiment for a further understanding of the application
Membrane module and preparation method thereof is specifically described.
Embodiment 1
The device architecture of the present embodiment film layer combination is as follows：Using 1.8mm thickness ultrawhite glass as substrate, sequentially form：Bottom
Portion's protective layer：Silica；Bottom transparent conductor layer：Tin indium oxide；Protective layer：Silica；Photochromic layer：Tungsten oxide layer；From
Sub- conductor layer：Tungsten oxide lithium layer；Ion storage：Mix the tungsten oxide nickel layer of lithium；Protective layer, silica；Top transparent electrode layer：
Tin indium oxide；Top protection layer, silica.
It is as follows that technique specifically is made：
(1) substrate of glass cleans drying, into coating system.
(2) medium frequency reactive sputtering rotates silicon target, prepares silica；Set power AC 30KW, atmosphere：Argon gas and oxygen
Mixing, air pressure 3 × 10-4Mbar, thicknesses of layers 20nm.
(3) magnetron sputtering rotates tin indium oxide target, prepares indium tin oxide conductor layer；Direct current pulse power source, power DC
60KW, argon sputter, air pressure 5 × 10-4Mbar, thicknesses of layers 150nm.
(4) medium frequency reactive sputtering rotates silicon target, prepares silica；Set power AC 30KW, atmosphere：Argon gas and oxygen
Mixing, air pressure 3 × 10-4Mbar, thicknesses of layers 20nm.
(5) reactive magnetron sputtering rotates tungsten target, prepares tungsten oxide layer；Reaction gas oxygen, direct current pulse power source, power DC
60KW, argon sputter, content：0~70%, air pressure 5 × 10-4Mbar, thicknesses of layers 150nm；
(6) lithium is embedded in tungsten oxide layer by pulsed sputter lithium target, and tungsten oxide lithium layer is made.Frequency 13.65MHz, atmosphere argon
Gas, air pressure 8 × 10-4Mbar, then using direct current pulse power source sputtering rotation lithium target in argon atmosphere, frequency 200KHz is embedded
Depth 15nm.
(7) pulsed sputter prepares the tungsten oxide nickel layer for mixing lithium；First use tungsten nickel target, oxygen and argon gas mixed atmosphere
Middle pulse reactive sputtering, is made tungsten oxide nickel layer.Frequency 13.65MHz, atmosphere argon gas and oxygen mix, mixed volume ratio
Ar2：O2=2:8, air pressure 8 × 10-4Mbar forms thickness 150nm tungsten oxide nickel layers；Then DC pulse is used in argon atmosphere
Power supply sputtering rotation lithium target, frequency 200KHz, insert depth 15nm.
(8) medium frequency reactive sputtering rotates silicon target, prepares silica；Set power AC 30KW, atmosphere：Argon gas and oxygen
Mixing, air pressure 3 × 10-4Mbar, thicknesses of layers 20nm.
(9) magnetron sputtering rotates tin indium oxide target, prepares indium tin oxide conductor layer；Direct current pulse power source, power DC
60KW, argon sputter, air pressure 5 × 10-4Mbar, thicknesses of layers 150nm.
(10) medium frequency reactive sputtering rotates silicon target, prepares silica；Set power AC 30KW, atmosphere：Argon gas and oxygen
Mixing, air pressure 3 × 10-4Mbar, thicknesses of layers 50nm.
The present embodiment provides the method that EC device film layers make, yields 78.6%.EC glass after stain efficiency is made
70cm2C-1-120cm2C-1.The range is related to electrode wiring density, and the corresponding coloration efficiency of different density is different.
Embodiment 2
The device architecture of the present embodiment film layer combination is the same as embodiment 1；
It is specific technique is made the difference is that：Using rotation tungsten oxide lithium target, it is directly prepared into tungsten oxide lithium layer；Radio frequency
13.56MHz, atmosphere argon gas and oxygen mix, mixed volume ratio Ar2：O2=2:3, air pressure 8 × 10-4Mbar forms thickness
200nm tungsten oxide lithium layer.
Embodiment 3
The device architecture of the present embodiment film layer combination is the same as embodiment 1；
It is specific technique is made the difference is that：Using the tungsten nickel target for mixing lithium, it is directly prepared into the tungsten oxide nickel for mixing lithium
Layer, radio frequency 13.56MHz, atmosphere argon gas and oxygen mix, mixed volume ratio Ar2：O2=2:3, air pressure 8 × 10-4Mbar, shape
At thickness 150nm thickness tungsten oxide lithium layer.
Embodiment 4
The device architecture of the present embodiment film layer combination is the same as embodiment 1；
It is specific technique is made the difference is that：
Using rotation tungsten oxide lithium target, it is directly prepared into tungsten oxide lithium layer, radio frequency 13.56MHz, atmosphere argon gas and oxygen are mixed
It closes, mixed volume ratio Ar2：O2=2:3, air pressure 8 × 10-4Mbar forms thickness 200nm tungsten oxide lithium layer.
Using the tungsten nickel target for mixing lithium, be directly prepared into the tungsten oxide nickel layer for mixing lithium, radio frequency 13.56MHz, atmosphere argon gas and
Oxygen mix, mixed volume ratio Ar2：O2=2:3, air pressure 8 × 10-4Mbar forms thickness 150nm thickness tungsten oxide lithium layer.
Comparative example 1
The device architecture of this comparative example film layer combination is as follows：Using 1.8mm thickness ultrawhite glass as substrate, sequentially form：Bottom
Portion's protective layer：Silica；Transparent conductor layer：Tin indium oxide；Photochromic layer：Tungsten oxide lithium layer；Conducting shell：Lithium aluminosilicate；Storage
Layer：Mix the tungsten oxide nickel layer of lithium；Transparent electrode layer：Tin indium oxide；Top protection layer：Silica.
It is as follows that technique specifically is made：
(1) substrate of glass cleans drying, into coating system.
(2) medium frequency reactive sputtering rotates silicon target, prepares silica；Set power AC 30KW, atmosphere：Argon gas and oxygen
Mixing, air pressure 3 × 10-4Mbar, thicknesses of layers 20nm.
(3) magnetron sputtering rotates tin indium oxide target, prepares indium tin oxide conductor layer；Direct current pulse power source, power DC
60KW, argon sputter, air pressure 5 × 10-4Mbar, thicknesses of layers 150nm.
(4) lithium is embedded in tungsten oxide layer by pulsed sputter lithium target, and tungsten oxide lithium layer is made.Frequency 13.65MHz, atmosphere argon
Gas, air pressure 8 × 10-4Mbar, then using direct current pulse power source sputtering rotation lithium target in argon atmosphere, frequency 200KHz is embedded
Depth 15nm.
(5) DC pulse sputters lithium aluminosilicate target, and alumina silicate lithium layer (α-LiAlSi are made2O6), frequency 40kHz, atmosphere argon
Compression ring border sputters, air pressure 1 × 10-4Mbar, thickness 20nm.
(6) pulsed sputter prepares the tungsten oxide nickel layer for mixing lithium；First use tungsten nickel target, oxygen and argon gas mixed atmosphere
Middle pulse reactive sputtering, is made tungsten oxide nickel layer.Frequency 13.65MHz, atmosphere argon gas and oxygen mix, mixed proportion Ar2：O2=
2:8, air pressure 8 × 10-4Mbar forms thickness 150nm tungsten oxide nickel layers；Then it is sputtered using direct current pulse power source in argon atmosphere
Rotate lithium target, frequency 200KHz, insert depth 15nm.
(7) magnetron sputtering rotates tin indium oxide target, prepares indium tin oxide conductor layer；Direct current pulse power source, power DC
60KW, argon sputter, air pressure 5 × 10-4Mbar, thicknesses of layers 150nm.
(8) medium frequency reactive sputtering rotates silicon target, prepares silica；Set power AC 30KW, atmosphere：Argon gas and oxygen
Mixing, 3 × 10-4mbar of air pressure, thicknesses of layers 50nm.
This comparative example device yield is between 33.8%-50%；Relative to comparative example, the yields of the embodiment of the present invention
Higher.Inorganic full-solid electric driven color-changing thin-film device provided by the invention can accurately control light percent of pass, while film forming
Yields is high, reduces production cost, is conducive to application.
The above is only a preferred embodiment of the present invention, it is noted that for making the professional technique of the art
Personnel are that by various modifications to these embodiments without departing from the technical principles of the invention, and these
Modification also should be regarded as the range that the present invention should protect.
Claims (10)
1. a kind of inorganic full-solid electric driven color-changing thin-film device, including：
Substrate；
The first protective layer for being arranged in substrate successively, the first transparent conductor layer, the second protective layer, inorganic photochromic layer, it is inorganic from
Sub- conducting shell, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protective layer.
2. inorganic full-solid electric driven color-changing thin-film device according to claim 1, which is characterized in that first protection
The material of layer, the second protective layer, third protective layer and the 4th protective layer is independently selected from SiO2、TiO2And Si3N4In one kind or
It is a variety of.
3. inorganic full-solid electric driven color-changing thin-film device according to claim 1, which is characterized in that the light of the substrate
Transmitance ＞ 90%；The thickness of first protective layer and the 4th protective layer independently is 10nm~50nm.
4. according to claims 1 to 3 any one of them inorganic full-solid electric driven color-changing thin-film device, which is characterized in that described
The thickness of second protective layer and third protective layer, which is independently less than, is equal to 100nm.
5. inorganic full-solid electric driven color-changing thin-film device according to claim 4, which is characterized in that described first transparent leads
The thickness of electric layer and the second transparency conducting layer independently is 20nm~500nm, the thickness of the inorganic photochromic layer be 50nm~
The thickness of 500nm, the inorganic ion-storage layer are 50nm~500nm.
6. according to claims 1 to 3 any one of them inorganic full-solid electric driven color-changing thin-film device, which is characterized in that described
The thickness of inorganic ions conducting shell is 5nm~100nm, and membrane uniformity controls within ± 1%.
7. inorganic full-solid electric driven color-changing thin-film device according to claim 6, which is characterized in that the inorganic ions passes
The material of conducting shell is selected from the compound of doping, and the compound is preferably silicate, phosphate, borate, tantalates, oxidation
It is one or more in tungsten, silica and tantalum oxide；The dopant is preferably H+, it is lithium, one or more in sodium and potassium.
8. according to claims 1 to 3 any one of them inorganic full-solid electric driven color-changing thin-film device, which is characterized in that described
The material of first transparent conductor layer and the second transparent conductor layer is independently selected from metal or the metal oxide of doping；The doping
Metal oxide be preferably tin indium oxide, adulterate fluorine SnO2Or the zinc oxide of adulterated al；The metal be preferably platinum, gold,
Silver, copper or aluminium.
9. according to claims 1 to 3 any one of them inorganic full-solid electric driven color-changing thin-film device, which is characterized in that described
The material of inorganic photochromic layer and inorganic ion-storage layer is correspondingly selected from cathode off-color material, anode off-color material and bipolar change
It is one or more in color material.
10. a kind of preparation method of inorganic full-solid electric driven color-changing thin-film device, includes the following steps：
In substrate, by way of vapor deposition, sequentially form the first protective layer, the first transparent conductor layer, the second protective layer,
Inorganic photochromic layer, inorganic ions conducting shell, inorganic ion-storage layer, third protective layer, the second transparent conductor layer and the 4th protection
Layer, obtains inorganic full-solid electric driven color-changing thin-film device.
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