CN107015412A - A kind of structure and preparation method of the full film electrochromic device of solid-state - Google Patents
A kind of structure and preparation method of the full film electrochromic device of solid-state Download PDFInfo
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- CN107015412A CN107015412A CN201710240528.XA CN201710240528A CN107015412A CN 107015412 A CN107015412 A CN 107015412A CN 201710240528 A CN201710240528 A CN 201710240528A CN 107015412 A CN107015412 A CN 107015412A
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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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- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention belongs to electrochromism manufacture field, and in particular to a kind of structure and preparation method of the full film electrochromic device of solid-state.The electrochromic device send top to bottm to be made up of successively metallic reflector or transparency conducting layer, electrochromic layer, dielectric layer, lithium alloy layer, ion storage layer, transparency conducting layer.The full-solid electrochromic device that the present invention is provided, is made up of MULTILAYER COMPOSITE film layer, has the advantages that concise in technology, plated film speed are fast, Composition Control is good, device good weatherability.The design of device film layer is breached, is far above the characteristics of property of lithiumation thing, and lithium metal alloy sputter rate are far above oxidate for lithium using the unit volume effectively amount containing lithium of lithium metal or lithium alloy；Improve device production efficiency, the purpose for reducing equipment cost, improving cycle life, the device discoloration speed of response improved, with the good market competitiveness.
Description
Technical field
The invention belongs to electrochromism manufacture field, and in particular to a kind of structure of full film electrochromic device of solid-state and
Preparation method.
Background technology
Electrochromism refers to the optical properties (reflectivity, transmitance, absorptivity etc.) of material in the presence of extra electric field
Occur the phenomenon of stable, reversible color change, the reversible change of color and transparency is shown as in appearance.Electrochromism intelligence
Can glass there is the controllability that light absorbs are passed through under electric field action, optionally absorb or reflect extraneous heat radiation and
Internal hot diffusion, plays improvement natural lighting degree, the purpose of peep-proof.Therefore, electrochromic device is in building field, car
There is very wide value with anti-dazzle, sun light-sensitive sunglasses aspect.
Electrochromic device working region is general by a discoloration material layer, electrode layer, an ion storage
Layer composition.Existing electrochromic device, its discoloration material layer, electrode layer, ion storage layer are generally required by difference
Kinds of processes be made, then need just be made by complicated packaging technology.Using all solid state of inorganic ions storage layer
Device is amenable to the solar radiation of longer time than the full solid-state device of organic ion storage layer.And lithium in inorganic full-solid device
Source derives from oxidate for lithium ion conducting layer or oxidate for lithium ion storage layer.Existing technology is using directly sputtering oxidate for lithium
Ion conducting layer or oxidate for lithium ion storage layer, have that the effective lithium content of unit volume in oxidate for lithium is low, oxidate for lithium film
The defect that the control of composition of layer uniformity is difficult, relatively low caused this section of equipment investment of sputter rate is costly.
The content of the invention
Therefore, to be to overcome electrochromic device composition in the prior art consistent for the technical problems to be solved by the invention
Property control is difficult, Li source compound deposits slow bottleneck so that propose a kind of full film electrochromic device of solid-state structure and
Preparation method.
In order to solve the above technical problems, the invention discloses a kind of full-solid electrochromic device (as shown in Figure 1), it is described
Electrochromic device send top to bottm successively by metallic reflector or transparency conducting layer, electrochromic layer, dielectric layer, lithium alloy layer,
Ion storage layer, transparency conducting layer composition.
It is preferred that, the metallic reflector is one kind in silver, aluminium.
It is preferred that, the transparency conducting layer is tin indium oxide, aluminium-doped zinc oxide, one kind of fluorine-doped tin oxide.
It is preferred that, the electrochromic layer can be transition metal oxide.
It is preferred that, the transition metal oxide is tungsten oxide, vanadic anhydride, niobium oxide, titanium oxide, yittrium oxide, oxygen
Change one kind in cobalt, molybdenum oxide.
It is preferred that, the dielectric layer is Si oxide, one kind of silicon-oxygen nitride.
It is preferred that, the lithium alloy layer is lithium-aluminium alloy, one kind of lithium magnesium alloy.
It is preferred that, the thickness of dielectric layers is 10~500nm；The lithium alloy layer is 5~100nm；The ion storage
Thickness degree is 300~1000nm；The electrochromic layer thickness is 300~1000nm；The metallic reflector thickness be 20~
500nm。
The invention also discloses a kind of method for preparing any one electrochromic device, methods described step is as follows：
A. it is substrate to take glass or flexible polymer, and is placed in burner hearth after being cleaned；
B. magnetron sputtering is used in the surface metal reflective layer or transparency conducting layer of the substrate；
C. mask plate is taken to be placed in above the metallic reflector, to reserve Wiring area；Then set by physical vapour deposition (PVD)
It is standby to deposit electrochromic layer；
D. then by magnetron sputtering or thermal evaporation or electron beam evaporation or chemical vapor depsotition equipment in the electroluminescent change
One layer of dielectric layer is deposited on chromatograph；
E. on the dielectric layer physical vapour deposition (PVD) layer of metal lithium or lithium alloy layer.
F. ion storage layer is deposited by magnetron sputtering mode on lithium alloy layer；
G. in the ion storage layer, mask plate is covered with, to reserve Wiring area, second layer nesa coating is plated out.
The above-mentioned technical proposal of the present invention has advantages below compared with prior art：The all solid state electroluminescent change that the present invention is provided
Color device, is made up of MULTILAYER COMPOSITE film layer, with concise in technology, plated film speed are fast, Composition Control is good, device good weatherability,
The high advantage of cyclical stability.Target in the technique can use dc source, compared to traditional work using radio-frequency power supply
Skill, is traditional 8-11 times in plated film speed, production capacity greatly improved, also have on the discoloration rate of integral device and significantly change
Enter.The present invention breaches the slow limitation excessively of existing full-solid electrochromic device structure lithium source layer plated film speed, and innovative carries
Go out and magnetron sputtering is solved the problem of sputtering lithiumation thing ceramic target efficiency is low by Pvd equipment, it is easier to realized
Large-scale production.Before application in terms of scape, according to the selection of primer, the industry available for two general orientation.Such as：Bottom is used
Metallic reflector can be used for Electrochromic automobile rearview mirror, and bottom then can be used for building curtain wall to save glass using transparency conducting layer
Glass.
Brief description of the drawings
In order that present disclosure is more likely to be clearly understood, specific embodiment and combination below according to the present invention
Accompanying drawing, the present invention is further detailed explanation, wherein
Fig. 1 is the vertical section structural representation for automobile rearview mirror electrochromic device described in embodiment；
Fig. 2 is the front schematic view for automobile rearview mirror electrochromic device described in embodiment；
Fig. 3 is the comparison diagram of the faded color reflectivity for automobile rearview mirror electrochromic device described in embodiment；
Fig. 4 is that the reflectivity for automobile rearview mirror electrochromic device described in embodiment is bent with the change of corresponding time
Line；
Fig. 5 is the vertical section structural representation of the electrochromic device for building curtain wall energy-saving glass described in embodiment
Figure；
Fig. 6 be the electrochromic device for building curtain wall energy-saving glass described in embodiment colour fading and color change state it is saturating
Cross rate effect contrast figure；
Fig. 7 is that the electrochromic device for building curtain wall energy-saving glass described in embodiment is passed through at a wavelength of 850 nm
The design sketch that rate changes with the response time；
Reference is：1- full-solid electrochromic device films.
Embodiment
Embodiment 1
Embodiment 1 is present embodiment discloses a kind of full-solid electrochromic device for automobile rearview mirror (such as Fig. 1,2 institutes
Show), it will be placed in after car mirror size glass bevelling angle lap in magnetron sputtering cavity, in glass surface successively plated film formation device, institute
Stating electrochromic device send top to bottm to include successively：
Argentum reflecting layer, tungsten oxide layer, silicon oxide layer, lithium magnesium alloy layer, titanium doped ferric phosphate lithium layer, indium tin oxide layer.
The test of rearview mirror performance characterization is then carried out to it, as shown in Figure 3,4, its reflectivity amplitude of accommodation is big and with quick response
Ability.
The argentum reflecting layer thickness is 60nm；Tungsten oxide layer thickness is 350nm；Silicon oxide layer thickness is 30nm；Lithium magnesium
Alloy-layer thickness degree is 20nm；Titanium doped LiFePO4 thickness degree is 600nm；Indium tin oxide layer is 200nm；
Embodiment 2 send top to bottm present embodiment discloses a kind of full-solid electrochromic device, the electrochromic device
Include aluminium reflecting layer, tungsten oxide layer, silicon oxynitride layer, lithium-aluminium alloy layer, nickel oxide, transparency conducting layer successively.
The aluminium reflector thickness is 100nm；Tungsten oxide layer thickness is 400nm；Silicon oxynitride layer thickness is 50nm；Lithium
Thickness is 25nm to magnesium alloy layer by layer；Nickel oxide layer thickness is 650nm；Indium tin oxide layer is 200nm；
(its overall vertical section structural representation is such as present embodiment discloses a kind of full-solid electrochromic device for embodiment 3
Shown in Fig. 5), the electrochromic device send top to bottm successively include aluminium alloy reflecting layer, tungsten oxide layer, silicon oxynitride layer,
Lithium-aluminium alloy layer, Copper-cladding Aluminum Bar ferric phosphate lithium layer.
The tungsten oxide thickness is 500nm；The lithium-aluminium alloy layer is 30nm；Silicon oxynitride layer is 100nm；Nickel oxide
Layer is 500nm；
Present embodiment discloses a kind of system of the full-solid electrochromic device for building curtain wall energy-saving glass for embodiment 4
Standby technique, step is as follows：
1.8mm glass is placed in magnetic-controlled sputtering coating equipment after plasma clean.
Using magnetically controlled DC sputtering transparency conducting layer ito film：Background vacuum is 1.8X10-3Pa, is passed through pure argon to chamber
Body air pressure 0.3Pa, power setting is 6W/cm2, it is conductive for 100nm transparent that glass heats 200 degree of lower sputtered layer thickness
Layer.
Then mask plate is placed in above silver layer, electrochromism tungsten oxide layer is plated using metal tungsten target DC reactive sputtering：
Background vacuum is 1.8X10-3Pa, is passed through pure argon to argon partial pressure 1.3Pa, is passed through oxygen to partial pressure of oxygen 2.2Pa, power setting
For 12W/cm2, sputtered layer thickness is 600nm tungsten oxide electrochromic layer.
Ion conducting layer is then used as using intermediate frequency power supply Magnetron Sputtering Thin Film on the basis of technique 3：Target uses sial
Target, base vacuum 1.8X10 is evacuated to by instrument-3Pa, cavity is passed through oxygen to pressure and reaches 1.3Pa, and radio-frequency power is 2.2W/
cm2, sputtered layer thickness is 50nm sieve and silica-sesquioxide ion conducting layer.
Ion storage layer is used as using dc source magnetron sputtering Li and Ti doped nickel oxide film on the basis of technique 4：
Target uses 7% lithium, 5% titanium doped nickel oxide ceramic target, and instrument is evacuated into base vacuum 1.8X10-3Pa, is passed through straight argon
Gas is to 1.3Pa, and dc power is 5W/cm2, sputtered layer thickness is 700nm Li and Ti doped nickel oxide film.
On carbon doping LiFePO4 film, using magnetically controlled DC sputtering transparency conducting layer ito film：Background vacuum is
1.8X10-3Pa, is passed through pure argon to cavity air pressure 0.3Pa, power setting is 6W/cm2, sputtered layer thickness is 100nm ITO
Transparency conducting layer.
Experimental example
Experimental example 1
Transmitance change curve before and after device discoloration is tested, as shown in Figure 6.Transmitance regulation width before and after device discoloration
Degree is big, and maximum can be especially suitable for electrochromism building curtain wall and use by 85% regulation to 5%.
Experimental example 2
Test device at a wavelength of 850 nm, the performance that transmitance changes with the response time.As shown in fig. 7, the device has
There is capability of fast response, high transmittance can be completed under the several seconds to the change of high-absorbility.
Electrochromic device described in 3 pairs of experimental example carries out faded color percent of pass and the change experiment test with the corresponding time
As a result as shown in Figure 3, Figure 4, it can be seen that the response speed of electrochromic device quickly, can be obtained by embodiment
The state that height arrives high light absorbs thoroughly is completed in several seconds.
Fig. 3 regression colour contrast figures：Transmitance comparison diagram of the integral device in the case where discoloration is faded.Integral device discoloration amplitude is very
Greatly, with very high light modulation effect.
Fig. 4 discoloration response time figures：Integral device response speed quickly, height can be completed within the several seconds and arrives high light absorbs thoroughly
State.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (9)
1. a kind of full-solid electrochromic device, it is characterised in that the electrochromic device is anti-by metal successively from top to bottom
Layer or transparency conducting layer, electrochromic layer, dielectric layer, lithium alloy layer, ion storage layer, transparency conducting layer composition are penetrated,
Wherein, dielectric layer is one in nano amorphous silicon, transparent nano nonmetal oxide layer, transparent nano metal oxide layer
Kind；
Lithium alloy layer is aluminium or magnesium or silicon, 0 ＜ x ＜ 0.8,0 ＜ y ＜ 0.8 for LiMxNy, M and N.
2. full-solid electrochromic device as claimed in claim 1, it is characterised in that dielectric layer includes nano amorphous silicon, received
Rice Si oxide, nano-silicon nitrogen oxides, nanometer aluminum oxide, nanometer magnesium oxide, nano-iron oxide, Nano-Zinc oxidation
Thing, nanometer titanium oxide, the nanometer mixed compound of nanometer tantalum pentoxide or these materials, nitridation lithium phosphate.
3. the full-solid electrochromic device as described in claim 1 and 2, it is characterised in that the dielectric layer, lithium alloy layer exist
After prepared by device, then the lithiumation that is powered forms corresponding loose lithiumation thing ion conducting layer.
4. full-solid electrochromic device as claimed in claim 3, it is characterised in that the electrochromic layer can be transition gold
Belong to oxide.
5. full-solid electrochromic device as claimed in claim 4, it is characterised in that the transition metal oxide is oxidation
One kind in tungsten, vanadic anhydride, niobium oxide, titanium oxide, cobalt oxide, molybdenum oxide.
6. full-solid electrochromic device as claimed in claim 5, it is characterised in that the ion storage layer be nickel oxide,
Nickel tungsten oxide, Prussian blue, yttrium oxide, nickel titanium oxide, nickel aluminum oxide, LiFePO4, titanium or zinc or Copper-cladding Aluminum Bar phosphoric acid
Iron lithium.
7. full-solid electrochromic device as claimed in claim 6, it is characterised in that the transparency conducting layer is indium oxide
Tin, aluminium-doped zinc oxide, fluorine-doped tin oxide.
8. full-solid electrochromic device as claimed in claim 7, it is characterised in that the ion conducting layer thickness is 10~
500nm；The lithium alloy thickness degree is 10-100nm；The ion storage layer thickness is 200~1000nm；The electrochromism
Thickness degree is 200~1000nm, the metallic reflector thickness 10-1000nm, institute transparency conducting layer 50-300nm.
9. a kind of method for preparing the electrochromic device as described in claim any one of 1-8, it is characterised in that methods described is walked
It is rapid as follows：
A. it is substrate to take glass or flexible polymer, and is placed in burner hearth after being cleaned；
B. dc source magnetron sputtering is used in the surface metal reflective layer or transparency conducting layer of the substrate；
C. mask plate is taken to be placed in above the metallic reflector or transparency conducting layer, to reserve Wiring area；Then pass through physics gas
Phase deposition method goes out electrochromic layer；
D. leafing son biography is then deposited on the electrochromic layer by physical vapour deposition (PVD) or chemical vapor depsotition equipment
Conducting shell；
E. lithium alloy layer is plated out by physical vapour deposition (PVD) mode on the ion conducting layer；
F. ion storage layer is plated out by magnetron sputtering mode on the ion conducting layer；
G. in the ion storage layer, second layer transparency conducting layer is plated out using dc source magnetron sputtering.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710240528.XA CN107015412A (en) | 2017-04-13 | 2017-04-13 | A kind of structure and preparation method of the full film electrochromic device of solid-state |
| PCT/CN2017/084792 WO2018188154A1 (en) | 2017-04-13 | 2017-05-18 | Structure of full-solid-state thin-film electrochromic device and preparation method therefor |
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| CN201710240528.XA CN107015412A (en) | 2017-04-13 | 2017-04-13 | A kind of structure and preparation method of the full film electrochromic device of solid-state |
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