CN104407483A - Electrochromic device and preparation method and application thereof - Google Patents
Electrochromic device and preparation method and application thereof Download PDFInfo
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- CN104407483A CN104407483A CN201410826306.2A CN201410826306A CN104407483A CN 104407483 A CN104407483 A CN 104407483A CN 201410826306 A CN201410826306 A CN 201410826306A CN 104407483 A CN104407483 A CN 104407483A
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- G—PHYSICS
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- 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
- G02F1/1506—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
- G02F1/1508—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 using a solid electrolyte
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Abstract
The invention discloses an electrochromic device and a preparation method and application thereof. The preparation method comprises the following steps: depositing a first conductive layer on the surface of a first substrate by adopting a coating process; depositing a first electrochromic layer on a mask on the surface of the first conductive layer; sequentially depositing an electrolyte layer and a second conductive layer on the surface of the first electrochromic layer by adopting a coating process; or preparing an electrolyte layer between the second conductive layer and the first electrochromic layer after the second conductive layer is deposited on the surface of a second substrate; obtaining a single-layer electrochromic device; or, sequentially depositing an electrolyte layer, a second electrochromic layer and a second conductive layer on the surface of the first electrochromic layer by adopting a coating process; or sequentially depositing the second conductive layer and the second electrochromic layer on the surface of the second substrate, and preparing the electrolyte layer between the second electrochromic layer and the first electrochromic layer; thereby obtaining a double-layer electrochromic device, wherein the electrolyte layer is a transparent solid-state organic lithium ion conductor film. According to the all-solid-state preparation process, the problem that large-area scale production is difficult to realize is effectively solved.
Description
Technical field
The present invention relates to field of electronic devices, particularly relate to a kind of electrochromic device and its preparation method and application.
Background technology
Electrochromism refers to that the phenomenon of stable, reversible color change occurs the optical properties (reflectivity, transmitance, absorptivity etc.) of material under the effect of extra electric field, shows as the reversible change of color and transparency in appearance.The material with electrochromic property is called electrochromic material.Therefore, electrochromic material has bistable performance, does not only need backlight with the electrochromic display device that electrochromic material is made, and after display still image, as long as the picture material of display is constant, would not power consumption.Therefore, there is good energy-saving effect.And, because electrochromic display device is compared with other display devices, have without the blind angle of vision, contrast is high, operating temperature range is wide, driving voltage is low and the advantage such as rich color, have great application prospect in fields such as instrument display, outdoor advertising and static state display.
In electrochromic transition metal oxide, vanadium pentoxide shows anode variable color and negative electrode variable color, and the vanadium pentoxide films based on molybdenum doping has many electrochromism (orange-yellow-green-blue) behavior, the optical modulation of the 30%-90% in 550nm-900nm spectral region.Therefore, adopt the vanadium pentoxide of molybdenum doping as the electrochromic layer in electrochromic device, effectively can improve the performance of electrochromic device.But, when carrying out electrochromic device and preparing, because its raw materials cost and cost of manufacture are all higher, be difficult to realize large area large-scale production, and the electrochromic device performance of preparation is also stable not.
Summary of the invention
Based on this, be necessary for existing electrochromic device cost of manufacture higher, be difficult to the problem realizing large area large-scale production, a kind of electrochromic device and its preparation method and application is provided.
For realizing a kind of electrochromic device preparation method that the object of the invention provides, comprise the steps:
Adopt coating process at the first substrate surface depositing first conductive layer;
At described first conductive layer surface mask deposition first electrochromic layer;
Adopt described coating process on described first electrochromic layer surface successively deposit electrolyte layer and the second conductive layer; Or after described second conductive layer of the second substrate surface deposition, between described second conductive layer and described first electrochromic layer, prepare described dielectric substrate; Obtain individual layer electrochromic device;
Or, adopt described coating process to deposit described dielectric substrate, the second electrochromic layer and described second conductive layer successively on described first electrochromic layer surface; Or after described second substrate surface deposits described second conductive layer and described second electrochromic layer successively, between described second electrochromic layer and described first electrochromic layer, prepare described dielectric substrate; Obtain double-deck electrochromic device;
Described dielectric substrate is transparent solid-state organolithium ion conductor film.
Wherein in an embodiment, prepare described dielectric substrate and comprise:
Between described second conductive layer and described first electrochromic layer, or inject between described second electrochromic layer and described first electrochromic layer or after injection electrolyte colloidal sol, under default baking temperature, be baked to described electrolyte colloidal sol be polymerized and solidify to form described transparent solid-state organolithium ion conductor film;
Wherein, described electrolyte colloidal sol is organolithium ion colloidal sol.
Wherein in an embodiment, described default baking temperature is 50 DEG C-200 DEG C.
Wherein in an embodiment, the depositing operation of described first electrochromic layer and described second electrochromic layer is electrochemical deposition process or magnetron sputtering deposition technique.
Accordingly, present invention also offers a kind of electrochromic device, adopt any one preparation method above-mentioned to prepare, comprise conductive layer, electrochromic layer and dielectric substrate;
Wherein, described dielectric substrate is transparent solid-state organolithium ion conductor film.
Wherein in an embodiment, the transmitance of described transparent solid-state organolithium ion conductor film in visible-range is more than or equal to 80%; And,
The thickness of described transparent solid-state organolithium ion conductor film is 50nm ~ 5mm.
Wherein in an embodiment, the ionic conductivity of described transparent solid-state organolithium ion conductor film is more than or equal to 1 × 10
-5s/cm.
Wherein in an embodiment, described electrochromic layer is molybdenum doping vanadium pentoxide films; And,
Described molybdenum doping vanadium pentoxide films is the layer structure of [001] orientation.
Wherein in an embodiment, in described molybdenum doping vanadium pentoxide films, the doping content of molybdenum is 5% ~ 10%mol; And,
The thickness of described molybdenum doping vanadium pentoxide films is 50nm ~ 5 μm.
Accordingly, present invention also offers a kind of any one electrochromic device application on mobile terminals as above.
The beneficial effect of above-mentioned electrochromic device preparation method:
By preparing transparent solid-state organolithium ion conductor film as dielectric substrate in individual layer electrochromic device or double-deck electrochromic device, achieve the preparation of full-solid electrochromic device.Its preparation technology is simple, with low cost, is easy to realize, and all solid state preparation technology (namely conductive layer, electrochromic layer and dielectric substrate are solid-state) is conducive to large-scale production.Thus it is higher to efficiently solve existing electrochromic device cost of manufacture, be difficult to the problem realizing large area large-scale production.
Further, the electrical equipment Electrochromic device adopting said method to prepare is full-solid electrochromic device, and all solid state electrochromic device is compared to the electrochromic device of solid-liquid, and its stability is higher.Thus effectively improve the stability of electrochromic device.
Accompanying drawing explanation
Fig. 1 is the structure cut-open view of electrochromic device one specific embodiment of the present invention;
Fig. 2 is the structure cut-open view of another specific embodiment of electrochromic device of the present invention;
Fig. 3 is the XRD collection of illustrative plates of the molybdenum doping vanadium pentoxide electrochomeric films adopting electrochromic device preparation method embodiment 1 of the present invention preparation;
Fig. 4 is the transmitance data plot of the electrochromic device adopting electrochromic device preparation method embodiment 1 of the present invention preparation.
Embodiment
For making technical solution of the present invention clearly, below in conjunction with drawings and the specific embodiments, the present invention is described in further details.
As a specific embodiment of electrochromic device preparation method provided by the invention, comprise the steps:
Step S100, adopts coating process at the first substrate surface depositing first conductive layer.
Step S200, at the first conductive layer surface mask deposition first electrochromic layer.
Step S300, adopts coating process at the first electrochromic layer surface successively deposit electrolyte layer and the second conductive layer.Namely after the first electrochromic layer surface deposition dielectric substrate, then at electrolyte layer surface deposit second conductive layer.The preparation of individual layer electrochromic device can be completed.Or, after the second substrate surface deposit second conductive layer, by the second conductive layer and the encapsulation of the first electrochromic layer, between the second conductive layer and the first electrochromic layer, directly prepare dielectric substrate to realize the preparation of individual layer electrochromic device.
Or step S300 ', adopts coating process at the first electrochromic layer surface successively deposit electrolyte layer, the second electrochromic layer and the second conductive layer, realizes the preparation of double-deck electrochromic device.Or after the second substrate surface successively deposit second conductive layer and the second electrochromic layer, between the second electrochromic layer and the first electrochromic layer, prepare dielectric substrate, reach the object preparing double-deck electrochromic device.
Wherein, the dielectric substrate in the individual layer electrochromic device of above-mentioned preparation or double-deck electrochromic device is transparent solid-state organolithium (Li) ion conductor film.
The electrochromic device prepared by above-mentioned preparation method is made up of multilayer complex films, has the most typical, the simplest structure of electrochromic device.And by preparing transparent solid-state organic Li ion conductor film as solid-state electrolyte layer, achieve full-solid electrochromic device, device performance is more stable.Further, preparation technology is simple, is easy to realize large area large-scale production.
As a specific embodiment, when preparing dielectric substrate, by adopting injection or priming by vacuum method, electrolyte colloidal sol is injected or is injected between the first electrochromic layer and the first conductive layer, or first between electrochromic layer and the second electrochromic layer, and under default baking temperature, be baked to electrolyte colloidal sol be polymerized and solidify to form transparent solid-state organolithium ion conductor film.Wherein, electrolyte colloidal sol is organolithium ion colloidal sol.
It is by forming solid-state electrolyte layer by organolithium ion colloidal sol, and manufacture craft is simple, with low cost.Wherein, preset temperature is preferably 50 DEG C-200 DEG C.
See Fig. 1, illustrate with the individual layer electrochromic device prepared.
First, coating process depositing first conductive layer 120 is passed through on the first substrate 110 surface.First conductive layer 120 is as the cathode electrode of electrochromic device, and therefore, the first conductive layer 120 also can be referred to as cathode conductive layer.First substrate 110 can select clear glass, draws materials easy, with low cost.Meanwhile, the first conductive layer 120 is preferably transparency conducting layer.Concrete realizes by depositing metal oxide film.Wherein, metal-oxide film can be: tin indium oxide (ITO) film, indium zinc oxygen (IZO) film, indium gallium zinc (IGZO) film or aluminium zinc oxygen (AZO) film.
Then, at surperficial mask deposition first electrochromic layer 130 of the first conductive layer 120.Mask mentioned here refers to, adopts mask plate or has any one jiao covering of overlay by the first conductive layer 120 of covering function, as electrode contact district.And then surface deposition first electrochromic layer 130 of non-cover part at the first conductive layer 120.The depositing operation of the first electrochromic layer 130 realizes by electrochemical deposition process or magnetron sputtering deposition technique.Certainly, also other physical gas-phase depositions or chemical vapor deposition method can be selected.Be preferably electrochemical deposition process or magnetron sputtering deposition technique, it can at room temperature deposit, and operates more simple; and process costs is more cheap; easy large scale growth, compatible better with existing electronic device process, be more conducive to realizing large area large-scale production.
It is pointed out that the structure of the first electrochromic layer 130 is layer structure.By adjusting the deposition process parameters of the first electrochromic layer 130, making the structure of the first electrochromic layer 130 be layer structure, being more conducive to passing through of the lithium ion in dielectric substrate 140.First electrochromic layer 130 of layer structure makes the lithium ion in dielectric substrate 140 have higher degree of freedom and better ion transmission performance, thus improve adsorption-desorption and the transfer of lithium ion, make the reversible change of color of the first electrochromic layer 130 more stable.Finally improve performance and the stability of electrochromic device.
When after the first conductive layer 120 surface deposition first electrochromic layer 130, the preparation of dielectric substrate 140 can be carried out.As previously mentioned, the preparation of dielectric substrate 140 realizes by two kinds of modes.One, adopts coating process directly at the first electrochromic layer 130 surface deposition dielectric substrate 140; Its two, adopt injection or priming by vacuum method to be prepared.
Be specifically described to adopt injection to prepare dielectric substrate 140 below.
When adopting injection to prepare, need to inject electrolyte colloidal sol between the first electrochromic layer 130 and the second conductive layer 150 (i.e. anode conductive layer).Therefore, the preparation carrying out the second conductive layer 150 is first needed.The preparation technology of the second conductive layer 150 can directly adopt coating process to carry out depositing on the second substrate 160 surface.Wherein, the second substrate 160 can select clear glass equally; Second conductive layer 150 is preferably transparency conducting layer equally, specifically realizes by depositing metal oxide film.
When after complete second conductive layer 150 of the second substrate 160 surface deposition, encapsulating material (can be epoxy resin) is adopted the second conductive layer 150 and the first electrochromic layer 130 to be encapsulated.Then, then between the second conductive layer 150 and the first electrochromic layer 130 adopt syringe directly to inject electrolyte colloidal sol.Because the dielectric substrate in electrochromic device of the present invention is transparent solid-state organolithium ion conductor film, therefore, the electrolyte colloidal sol injected is preferably organolithium ion colloidal sol.
Organolithium ion colloidal sol is injected to after between the second conductive layer 150 and the first electrochromic layer 130, by toasting under default baking temperature the organolithium ion colloidal sol be injected between the second conductive layer 150 and electrochromic layer 130.Until organolithium ion colloidal sol is polymerized and solidify to form transparent solid-state organolithium ion conductor film.
It should be noted that, when vacuum tightness is the baking carrying out organolithium ion colloidal sol under 1Pa-1000Pa atmosphere, its baking temperature and baking time are inversely proportional to.Baking temperature is higher, and baking time is shorter.Otherwise baking temperature is lower, baking temperature is then longer.In addition, when organolithium ion colloidal sol is toasted, directly carry out in air atmosphere.Simple to operate, be easy to realize.Be conducive to large-scale production.
In addition, adopt transparent solid-state organolithium ion conductor film as dielectric substrate 140, its transmitance in visible-range is more than or equal to 80%.Further, the thickness of transparent solid-state organolithium ion conductor film is preferably 50nm (nanometer) ~ 5mm (millimeter).
Further, the first electrochromic layer 130 is preferably molybdenum doping vanadium pentoxide films.Adopt molybdenum doping vanadium pentoxide films as the first electrochromic layer 130 of electrochromic device, when adding side's pressure of+3.0V ,+1.0V ,-1.0V and-3.0V at the cathode electrode of electrochromic device and anode electrode, can make electrochromic device can reversible change between orange-Huang-green-basket.
Meanwhile, preferably, at the molybdenum doping vanadium pentoxide films of the first conductive layer 120 surface deposition be the layer structure of [001] orientation.That is, at [001] crystal orientation, molybdenum doping vanadium pentoxide films edge preferential growth that the first conductive layer 120 deposits.
It should be noted that, in molybdenum doping vanadium pentoxide films, the doping content of molybdenum is 5% ~ 10%mol.
Further, the color due to electrochromic device is relevant with the thickness of its first electrochromic layer 130.Under equal steps voltage, the thickness of electrochromic layer 130 is larger, and color is darker.When molybdenum doping vanadium pentoxide films reaches certain thickness, electrochromic device is under the side of+3.0V ,+1.0V ,-1.0V and-3.0V pressure drives, its color can reversible change between orange-yellow-(yellow-green)-(green-blue), and is not only reversible change between orange-Huang-green-basket.This also just increases the color change of electrochromic device.Thus, the thickness of molybdenum doping vanadium pentoxide films can be 50nm (nanometer) ~ 5 μm (micron).
By power management and circuit integrated, this electrochromic device is integrated in electric terminal equipment, as on the rear shell on the back of mobile phone, panel computer etc., the personalized color demand of consumer can be met.
Further, coating process can be physical gas-phase deposition or chemical vapor deposition method.When carrying out the preparation of electrochromic device of the present invention, coating process can be selected according to actual conditions, adds dirigibility and the compatibility of technique.Further, magnetron sputtering deposition technique is preferably.In magnetron sputtering deposition technique, sputter and go out after atom and energetic ion positive energy exchange, its energy wants high 1-2 orders of magnitude compared to the atom of evaporation.Thus, the conductive layer (i.e. the first conductive layer 120 and the second conductive layer 150) in the electrochromic device adopting magnetron sputtering deposition technique to prepare is better with the adhesiveness of substrate (i.e. the first substrate 110 and the second substrate 160).
Should be understood to, the preparation of the first electrochromic layer 130 and conductive layer is not limited in foregoing electrochemical deposition process and magnetron sputtering deposition technique.It also comprises vacuum thermal evaporation depositing operation, strengthens chemical vapor deposition method (PECVD), sol-gel depositing operation or spray deposition techniques etc.
See Fig. 2, as a specific embodiment of double-deck electrochromic device, it adds one deck second electrochromic layer 180 at dielectric substrate 140 and the second conductive layer 150.Wherein, the preparation of the second electrochromic layer 180 and the first electrochromic layer 130 is same or similar, therefore no longer repeats.Equally, the second electrochromic layer 180 is preferably layered structure.
Further, the second electrochromic layer 180 can be identical with the material of the first electrochromic layer 130, also can be different.Different preparations can be carried out as the case may be.
In sum, the electrochromic device of the present invention adopting above-mentioned steps to prepare is individual layer electrochromic device or double-deck electrochromic device, is made up of all solid state composite membrane of multilayer.Wherein, dielectric substrate 140 is transparent solid-state organolithium ion conductor film.Structure is simple, and performance is more stable.Further, except electrochromic layer 130, the transmitance of other each retes in visible-range all reaches more than 80%, effectively improves the performance of electrochromic device.
More specifically, with specific embodiment, further description is done to the present invention below.
Embodiment 1
See Fig. 1, the individual layer multicolour electrochromic device that embodiment 1 provides, the first substrate 110 is conventional clear glass sheet.First conductive layer 120 is indium tin oxygen (ITO) film, for being communicated with extraneous power supply, as cathode electrode.First electrochromic layer 130 is molybdenum doping vanadium pentoxide films.Dielectric substrate 140 is polymkeric substance lithium salts solid electrolyte membrane.Second substrate 160 is conventional clear glass sheet.Second conductive layer 150 is ito film, for being communicated with extraneous power supply, as anode electrode.Use epoxy resin 170 by superimposed for the transparent glass sheet of two pieces of plated films edge sealing.
The preparation method of above-mentioned individual layer electrochromic device comprises the steps:
First, the area through acetone and ethanol solution ultrasonic cleaning cleaning is 2.5 × 2.5cm
2conventional clear glass as the first substrate 110, the transmitance of this simple glass in visible-range reaches more than 80%, and smooth surface have planar structure.
Then, adopt magnetron sputtering method to deposit on the first substrate 110 ito thin film that a layer thickness is 50nm ~ 5 μm, as the first conductive layer 120.
Secondly, adopt mask plate by one of ito thin film jiao of covering, as electrode contact district, and utilize electrodeposition process in ito film, deposit the molybdenum doping vanadium pentoxide films that a layer thickness is 800nm, as the first electrochromic layer 130.
Then, utilize magnetron sputtering method at the ito thin film that to deposit a layer thickness on the second substrate 160 be 50nm ~ 5 μm, as the second conductive layer 150.And adopt mask plate or other overlays with identical covering function by one jiao of covering of ito thin film (referring to the second conductive layer 150 herein), as electrode contact district.
Then, serigraphy is adopted epoxide-resin glue at V
2o
5: on Mo/ITO and ito film sheet edge, figure dissolves the broken colour full-solid electrochromic device cellular of a reserved aperture.By V
2o
5: the edge of Mo/ITO diaphragm and ito film sheet sticks together at 130 DEG C of-140 DEG C of curing epoxy resin adhesives, is assembled into a diaphragm cavity, is used for follow-up filling Li
+ionic liquid electrolyte.The height of diaphragm cavity is generally 30 μm ~ 200 μm (being controlled by the ball-type glass ball height limiting device in epoxide-resin glue).This diaphragm cavity is called in " cellular space " in liquid crystal industry.Again then, adopt priming by vacuum method and " drip-exert pressure " method to inject Li
+ionic liquid electrolyte material enters diaphragm cavity, i.e. V
2o
5: between Mo/ITO diaphragm and ito film sheet.
Particularly, before priming by vacuum, to diaphragm cavity and Li
+ionic liquid electrolyte vacuumizes in advance, to eliminate the residual gas being under low pressure easy to volatilize.First, be clamped in by diaphragm cavity on base, its reserved aperture is placed on the top of liquid electrolyte container and its position can arbitrarily regulate.Subsequently, close filling room and vacuumize with mechanical pump.When gaseous tension drops to about 10Pa, rotating base and reduce broken colour full-solid electrochromic device so that liquid electrolyte immerses reserved aperture.Due to liquid capillarity principle, Li
+the air intake opening inflow diaphragm cavity of ionic liquid electrolyte owing to opening.Close vacuum pump and maintain certain hour low pressure (about 5min).When air in is opened lentamente, inner air pressure can rise slowly.The vacuum in the atmospheric pressure of liquid surface and diaphragm cavity can be made like this to produce pressure reduction, and this pressure reduction can promote Li
+ionic liquid electrolyte flows in diaphragm cavity.As the Li in diaphragm cavity
+when ionic liquid electrolyte fills about 80%, the air in of chamber is opened completely so that air pressure goes back up to atmospheric pressure fast, and the liquid of 100% is filled.After having poured into, rotating base air intake opening is removed from liquid electrolyte again.The open portion UV fat of reserved aperture clings and rapid curing.Finally, toast 2 hours at 85 DEG C, the organic Li in diaphragm cavity
+ionic liquid electrolyte crosslinking curing completes, and forms organic lithium ion conductor film, as the dielectric substrate 140 of electrochromic device, thus obtains individual layer broken colour full-solid electrochromic device.
See Fig. 3, for the molybdenum doping vanadium pentoxide films prepared embodiment 1 carries out the XRD collection of illustrative plates of XRD (X-raydiffraction, X-ray diffraction) scanning acquisition.Can obviously be found out by XRD collection of illustrative plates, except the diffraction peak of ito thin film, only have the diffraction peak of stronger vanadium pentoxide films [001] orientation, show that molybdenum doping vanadium pentoxide films (i.e. electrochromic layer 130) is along [001] preferential growth.It is under the molybdenum doping vanadium pentoxide films structure of edge [001] preferential growth, and lithium ion has higher degree of freedom and good ion transmission performance, is conducive to adsorption-desorption and the transfer of ion, can promotes the sensitivity of electrochromic device.
See Fig. 4, it is the transmitance data plot of electrochromic device prepared by above-described embodiment 1.From its transmitance data plot, can the optical transmittance of Effective Regulation electrochromic device by the voltage applied between cathode electrode and anode electrode.
In addition, by adding+3.0V between the cathode electrode of all solid state individual layer multicolour electrochromic device for preparing in embodiment 1 and anode electrode, side's pressure of+1.0V ,-1.0V and-3.0V, learns the reversible change between orange-Huang-green-basket of this individual layer electrochromic device.
Embodiment 2
See Fig. 2, be a specific embodiment of double-deck electrochromic device, the first substrate 110 is conventional clear glass sheet.First conductive layer 120 is indium tin oxygen (ITO) film, for being communicated with extraneous power supply, as cathode electrode.First electrochromic layer 130 is molybdenum doping vanadium pentoxide films.Dielectric substrate 140 is polymkeric substance lithium salts solid electrolyte membrane.Second substrate 160 is conventional clear glass sheet.Second conductive layer 150 is indium tin oxygen (ITO) film, for being communicated with extraneous power supply, as anode electrode.Second electrochromic layer 180 is tungsten oxide (WO
3) or nickel oxide (NiO) film.Use epoxy resin 170 by superimposed for the transparent glass sheet of two pieces of plated films edge sealing.
The method for making of above-mentioned double-deck electrochromic device comprises the steps:
First, the area through acetone and ethanol solution ultrasonic cleaning cleaning is 2.5 × 2.5cm
2simple glass as the first transparent substrate 110.The transmitance of this simple glass in visible-range reaches more than 80%, and smooth surface there is planar structure.
Secondly, adopting magnetron sputtering method on the first substrate 110, deposit a layer thickness is that the ito thin film of 50nm ~ 5 μm is as the first conductive layer 120, i.e. cathode conductive layer.
Then, adopt mask plate or other overlays by one of ito thin film jiao of covering, as electrode contact district, utilize magnetron sputtering method on ito thin film, deposit the molybdenum doping vanadium pentoxide films that a layer thickness is 800nm, as the first electrochromic layer 130.
Then, magnetron sputtering method is utilized on the second substrate 160, to deposit the ito thin film that a layer thickness is 50nm ~ 5 μm, as the second conductive layer 150, i.e. anode conductive layer equally.
Then, same employing mask plate or other overlays with identical covering function are by one jiao of covering of ito thin film (referring to the second conductive layer 150 herein), as electrode contact district, utilize magnetron sputtering method at ito thin film (referring to the second conductive layer 150) upper deposition one deck WO
3or NiO film, as the second electrochromic layer 180.
And then, utilize epoxy resin 170 will V
2o
5: Mo/ITO diaphragm and WO
3(NiO)/ito film sheet separates with certain thickness organic glass frame and seals, and stays aperture to be used as electrolysis colloidal sol injection inlet.
Finally, the diaphragm that two prepare is placed in vacuum chamber and toasts at 300 DEG C at 100 DEG C, to dispel aqueous vapor.Then, water white organolithium ion colloidal sol priming by vacuum method is injected between two diaphragms, toast under default baking temperature, organolithium ion colloidal sol is made to be polymerized and to solidify to form organolithium ion conductor film completely, as the dielectric substrate 140 of electrochromic device, finally obtain all solid state multicolour electrochromic device of multilayer.
By adding+3.0V between the cathode electrode of all solid state multicolour electrochromic device for preparing in embodiment 2 and anode electrode, + 1.0V,-1.0V presses with the driving side of-3.0V, this multilayer electrochromic device can be that (orange-blue)-(yellow-blue)-green-blue multicolour changes, instead of only changes between orange-Huang-green-basket.Thereby increase the multicolour of full-solid electrochromic device.
Embodiment 3
See Fig. 1, the electrochromic device that the present embodiment provides is individual layer multicolour electrochromic device.Wherein, the first substrate 110 is conventional clear glass sheet.First conductive layer 120 is indium tin oxygen (ITO) film, for being communicated with extraneous power supply, as cathode electrode.First electrochromic layer 130 is molybdenum doping vanadium pentoxide films.Dielectric substrate 140 is polymkeric substance lithium salts solid electrolyte membrane.Second substrate 160 is similarly conventional clear glass sheet.Second conductive layer 150 is ito film, for being communicated with extraneous power supply, as anode electrode.It uses epoxy resin 170 by superimposed for the transparent glass sheet of two pieces of plated films edge sealing.
The method for making of above-mentioned individual layer electrochromic device comprises the steps:
First, the area through acetone and ethanol solution ultrasonic cleaning cleaning is 2.5 × 2.5cm
2simple glass as the first transparent substrate 110.The transmitance of this simple glass in visible-range reaches more than 80%, and smooth surface there is planar structure.
Secondly, adopting magnetron sputtering method on the first substrate 110, deposit a layer thickness is that the ito thin film of 50nm ~ 5 μm is as the first conductive layer 120, i.e. cathode conductive layer.
Then, adopt mask plate or other overlays by one of ito thin film jiao of covering, as electrode contact district, utilize magnetron sputtering method on ito thin film, deposit the molybdenum doping vanadium pentoxide films that a layer thickness is 800nm, as the first electrochromic layer 130.
Then, magnetron sputtering method is utilized on the second substrate 160, to deposit the ito thin film that a layer thickness is 50nm ~ 5 μm, as the second conductive layer 150, i.e. anode conductive layer equally.
Then, adopt mask plate or other overlays with identical covering function by one jiao of covering of ito thin film (referring to the second conductive layer 150 herein) equally, as electrode contact district.Utilize epoxy resin 170 by the second conductive layer diaphragm and deposit molybdenum doping vanadium pentoxide films diaphragm and to separate with certain thickness organic glass frame and to use epoxy sealing.Meanwhile, aperture is stayed to be used as electrolyte colloidal sol injection inlet.
Finally, citric acid is dissolved in absolute ethyl alcohol, then adds ethyl orthosilicate, then add lithium carbonate and fully dissolve, finally add ethylene glycol, at 80 DEG C, kept by gained colourless transparent solution 24h (hour) to obtain electrolyte colloidal sol (i.e. organolithium ion colloidal sol).Then, water white organolithium ion colloidal sol syringe is injected between two diaphragms, under default baking temperature, make colloidal sol be polymerized and solidify completely, form organic lithium ion conductor film, as the dielectric substrate 140 of electrochromic device, thus obtain all solid state individual layer multicolour electrochromic device.
By adding+3.0V ,+1.0V between the cathode electrode of all solid state individual layer multicolour electrochromic device for preparing in embodiment 1 and anode electrode ,-1.0V presses with the side of-3.0V, learns the reversible change between orange-Huang-green-basket of this individual layer electrochromic device.
Accordingly, present invention also offers any one electrochromic device above-mentioned application on mobile terminals.By power management and circuit integrated, any one individual layer electrochromic device above-mentioned or double-deck electrochromic device are applied on the shell on the back of mobile terminal, as: mobile phone shell on the back or panel computer shell on the back etc., improve personalization and the stability of mobile terminal, meet the personalized color demand of consumer.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. an electrochromic device preparation method, is characterized in that, comprises the steps:
Adopt coating process at the first substrate surface depositing first conductive layer;
At described first conductive layer surface mask deposition first electrochromic layer;
Adopt described coating process on described first electrochromic layer surface successively deposit electrolyte layer and the second conductive layer; Or after described second conductive layer of the second substrate surface deposition, between described second conductive layer and described first electrochromic layer, prepare described dielectric substrate; Obtain individual layer electrochromic device;
Or, adopt described coating process to deposit described dielectric substrate, the second electrochromic layer and described second conductive layer successively on described first electrochromic layer surface; Or after described second substrate surface deposits described second conductive layer and described second electrochromic layer successively, between described second electrochromic layer and described first electrochromic layer, prepare described dielectric substrate; Obtain double-deck electrochromic device;
Described dielectric substrate is transparent solid-state organolithium ion conductor film.
2. electrochromic device preparation method according to claim 1, is characterized in that, prepares described dielectric substrate and comprises:
Between described second conductive layer and described first electrochromic layer, or inject between described second electrochromic layer and described first electrochromic layer or after injection electrolyte colloidal sol, under default baking temperature, be baked to described electrolyte colloidal sol be polymerized and solidify to form described transparent solid-state organolithium ion conductor film;
Wherein, described electrolyte colloidal sol is organolithium ion colloidal sol.
3. electrochromic device preparation method according to claim 2, is characterized in that, described default baking temperature is 50 DEG C-200 DEG C.
4. electrochromic device preparation method according to claim 1, is characterized in that, the depositing operation of described first electrochromic layer and described second electrochromic layer is electrochemical deposition process or magnetron sputtering deposition technique.
5. an electrochromic device, is characterized in that, adopts the electrochromic device preparation method preparation described in any one of Claims 1-4, comprises conductive layer, electrochromic layer and dielectric substrate;
Wherein, described dielectric substrate is transparent solid-state organolithium ion conductor film.
6. electrochromic device according to claim 5, is characterized in that, the transmitance of described transparent solid-state organolithium ion conductor film in visible-range is more than or equal to 80%; And,
The thickness of described transparent solid-state organolithium ion conductor film is 50nm ~ 5mm.
7. electrochromic device according to claim 6, is characterized in that, the ionic conductivity of described transparent solid-state organolithium ion conductor film is more than or equal to 1 × 10
-5s/cm.
8. electrochromic device according to claim 5, is characterized in that, described electrochromic layer is molybdenum doping vanadium pentoxide films; And,
Described molybdenum doping vanadium pentoxide films is the layer structure of [001] orientation.
9. electrochromic device according to claim 8, is characterized in that, in described molybdenum doping vanadium pentoxide films, the doping content of molybdenum is 5% ~ 10%mol; And,
The thickness of described molybdenum doping vanadium pentoxide films is 50nm ~ 5 μm.
10. the application on mobile terminals of the electrochromic device as described in any one of claim 5 to 9.
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