CN1492274A - Full solid plastic electrochromism device and its preparing method - Google Patents
Full solid plastic electrochromism device and its preparing method Download PDFInfo
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- CN1492274A CN1492274A CNA031402755A CN03140275A CN1492274A CN 1492274 A CN1492274 A CN 1492274A CN A031402755 A CNA031402755 A CN A031402755A CN 03140275 A CN03140275 A CN 03140275A CN 1492274 A CN1492274 A CN 1492274A
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Landscapes
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The device includes conducting electrode layer, electrochromism layer, ionic conducting layer, ionic storage layer, etc., and substrate of optical plastic; and the ionic conducting layer is of polymer solid electrolyte material. The device is made through setting the ionic conducting layer between the electrochromism layer on one substrate and the ionic storage layer on one other substrate, pressing and packing protecting plastic layer. The device made on optical plastic substrate has clear structure, simple making process and wide use, and is flexible and suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of electrochromic device.
Background technology
Electrochromism is meant material under the effect of external electric field or electric current, and reversible color change takes place.Electrochromic effect is observed on alkali bittern crystal the earliest, Deb (DebS K, Appl Optics, 1969, P193) reported first amorphous WO in 1969
3Electrochromic effect in the film causes extensive attention, and electrochromic device has purposes widely in fields such as energy conversion, light adjusting, information record, plane demonstrations, has succeeded in developing practical devices such as dexterous electrochromic and vehicle glare proof mirror at present.Nissan released the ECD window that is used for automobile first in 1986, made electrochromism light modulation window become the most real commodity target of electrochromic material.
But the research and development in electrochromism field at present mainly is based on glass substrate, and with respect to plastic, glass substrate has many limitation at thickness, weight, aspect such as shock-resistant.Plastics have characteristics such as thickness is little, light weight, shock-resistant, anti-extruding, cost is low, the design use is flexible, in many applications, replace glass to become a kind of trend with plastics, for example show the field on the plane, the display device based on plastic successively appears in liquid crystal display, electroluminescence demonstration etc.But when selecting plastics,, specific (special) requirements is all arranged, therefore just limited the application of electrochromic device at aspects such as material preparation and device package because plastics have characteristics such as non-refractory as backing material.
Summary of the invention
For addressing the above problem, the purpose of this invention is to provide a kind of light weight, shock-resistant, anti-extruding, cost all solid state plastics electrochromic device low, easy to prepare.
Another object of the present invention provides a kind of preparation method of all solid state plastics electrochromic device.
The object of the present invention is achieved like this: a kind of all solid state plastics electrochromic device, comprise substrate, conductive electrode layer, electrochromic layer and ion conductive layer, its substrate adopts the optical plastic material, and ion conductive layer adopts the high molecular polymer solid electrolyte material.Device adopts the layering preparation, and the pressing encapsulation forms.
Above-mentioned device is made up of eight layers of structure, is followed successively by conductive electrode layer, plastic lining bottom, packaging protection plastic layer at ion conductive layer and electrochromic layer both sides.The external dc low-voltage driving realizes reversible color change between two conductive electrode layers.
Also be provided with ion storage between above-mentioned surface conduction electrode layer and the ion conductive layer.
Device of the present invention is that the ion storage pressing that ion conductive layer is placed on electrochromic layer on the conductive substrates and another layer conductive substrates is formed, and then through two outside layers transparent plastic packaging protection.The preparation method is: prepare surface conduction electrode layer, ion storage successively at first respectively on surperficial plastic lining bottom; prepare back side conductive electrode layer, electrochromic layer successively on the plastic lining bottom overleaf; then the conductive polymer polymkeric substance for preparing is made the solid electrolyte film and be placed on middle pressing; perhaps the conductive polymer polymkeric substance for preparing is coated with therein on a slice substrate; cover an other substrate; exerting pressure then, it is bonding to flatten, and then carries out packaging protection through the transparent packaging protection plastic layer of two outside layers.Electrode connects and can be chosen in before or after the encapsulation.The external dc low-voltage driving can be carried out variable color between surface conduction electrode layer and back side conductive electrode layer, adds driving power and is advisable with practical and convenient.
The present invention is the full-solid electrochromic device of a kind of preparation on the optical plastic substrate, device architecture is clear, and the preparation method is simple, and device can crookedly be reeled, of many uses, be easy to select for use commercial units such as takeup type coating machine, screen process press, injection machine to carry out large-scale production.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Embodiment
Usually, electrochromic device must contain the two-layer conductive electrode that is deposited on the substrate, middle electrochromic layer and ion conductive layer.But ion storage can be cancelled, and has its function concurrently by conductive electrode layer, and wherein two-layer conductive electrode one of comprises in the substrate at least it being transparent.If one deck conductive electrode and substrate thereof also are transparent in addition, then device is a transmission-type, if other one deck conductive electrode and substrate thereof are opaque, then device is a reflection type.Usually the electrochromic device of transmission-type is applicable to display device and dexterous smart window etc.The device of reflection type is applicable to display device and EC mirror etc.
Substrate of the present invention adopts the optical plastic material, optical plastic is meant the transparent material with certain optical property, be a kind of plastics that can compare favourably with optical glass, the preferred polymethylmethacrylate of the present invention (PMMA), polystyrene (PS), polycarbonate (PC), polyester slice (PET), Poly-s 179, polyethylene terephthalate, epoxy optical plastics etc.
The transparency conductive electrode layer can be made by the metallic film of gold, silver, aluminium, copper or by the conductive film of metal oxide, can also adopt laminated film or polyelectrolyte film.Its preparation method depends on the type that forms electrode material, can form by physical vacuum deposition, chemical vapor deposition, sol-gel method.
It is that full impregnated is bright at visible region that transparent substrates and conductive electrode generally require whole, and its specific examples is the ITO (In that adopts magnetron sputtering technique to prepare on the polyester plastics substrate
2O
3-SnO
2), zinc oxide transparent conducting film.Now widely used is ito thin film, optimizes between high permeability and low resistance.Ito thin film is a kind of Oxide Semiconductor Transparent Conductive Films, and the raising of its conductance is owing to nonstoichiometry realizes to increase carrier concentration with mixing than the oxygen room that forms.The thickness of the ITCO film of preparation on plastic is usually at 10-1000nm at present, and transmittance is at 60%-100%, and resistivity is generally about 1-1000 Ω .cm.Under the prerequisite that guarantees high transmission rate, the resistivity of conductive electrode is the smaller the better.
The reflective conductive electrode layer represents to have high reflectance and the conductive film of stable performance on galvanochemistry, normally metallic film or alloy firm.Can be the alloy etc. of gold, silver, copper, aluminium, chromium, tungsten, titanium or its composition, its preparation method depends on the type that forms electrode material, generally forms by the physical vacuum sedimentation.Its specific examples is Al, Ag, the Ni-Cr film that adopts magnetron sputtering technique to prepare on the polyester plastics substrate.Reflectivity is at 50%-100%.The thickness of film is usually at 10nm-10um, and surface resistance is at 0.1-100 Ω/sq.Transparency to plastic when using the reflective conductive electrode layer is not strict with.
The present invention includes electrochromic layer and ion storage, is the core texture of entire device.Electrochromic layer is the negative electrode coloured material, promptly is painted when connecing negative voltage, is to fade when connecing positive voltage.Ion storage is the anode coloured material, promptly is painted when connecing positive voltage, is to fade when connecing negative voltage.The ion storage fundamental purpose is and the electrochromic layer complementary colors, and the balancing charge transmission is with the electrochromic layer oxidation-reduction electrode that partners jointly.Ion storage can cancel or achromatization corresponding; Because electrochromic device is a symmetrical structure, ion storage and electrochromic layer can carry out location swap.
Electrochromic layer can adopt inorganic off-color material or the preparation of organic off-color material, and inorganic off-color material is generally transition metal oxide, can be WO
3, MoO
3, TiO
2, Nb
2O5, V
2O
3Deng in one or more doping form, owing to adopt plastic, have can not pyroprocessing etc. requirement, specific (special) requirements is arranged on the preparation method, for example on the vacuum coating basis, increase ion plating etc., can adopt method preparations such as magnetron sputtering, ion assisted deposition, ionic reaction deposition, laser deposition.Organic off-color material has Prussia orchid (prussianblue), purple sieve essence (viologens), metal phthalein cyanine (metalphthalocyanines), polymer/metallic complex compound (metallopolymers) and organic conductive polymkeric substance etc., can adopt print process, impact system, gluing method etc. according to the material of selecting for use during preparation.
Ion storage can be TiO
2, NiO, CeO
2, IrO, RhO, V
2O
3Deng in one or more doping form, consider the reason of plastic equally, can adopt the preparation of methods such as magnetron sputtering, ion assisted deposition, ionic reaction deposition, laser deposition.
For further improving the electrochromic property of film, can adopt methods such as doping, finishing, this does not change the structure of device.
Ion conductive layer of the present invention adopts the high molecular polymer solid electrolyte material, makes ion (H
+, Li
+Deng) between electrochromic layer and ion storage, transmit.Because adopt plastic, liquid electrolyte can't satisfy requirements such as encapsulation, the use of solid electrolyte becomes inevitable.Being applicable to that solid electrolyte requirement of the present invention has good ionic conductivity, viscoelasticity and light transmission, can be PEU-LiClO
4, PEO-LiClO
4, PPG-PMMA-LiClO
4, conduction high polymer such as Nafion, PESA, PAMPS.If the conduction high polymer that ion conductive layer adopts has the electrochromism feature simultaneously, then electrochromic layer and ion conductive layer can be merged into one deck, make structure more simple.
Purposes difference according to device; can carry out certain structure increases; in device, increase protective seam, insulation course or picture and text layer; for example in the middle of transparency conducting layer and electrochromic layer, increase insulation course and can increase variable color memory time, increase the picture and text layer on the plastic surface and can be used for display pattern.
Below in conjunction with specific embodiment and accompanying drawing the present invention is further detailed.
Embodiment 1:
Plastic lining bottom b, h adopt polyester slice PET film (thickness is 125 μ m), adopt magnetron sputtering technique to prepare ITO transparency conductive electrode layer c, g (thickness is 30nm) on plastic lining bottom b, h.The ITO electrically conducting transparent plastics that make are cut out, and wherein one is adopted the low-voltage ion reactive plating technology to prepare WO on ITO surface
3Electrochromic layer f, thickness are 400nm, adopt the low-voltage ion reactive plating technology to prepare NiO ion storage d on another substrate ITO surface, and thickness is 250nm.Get the PEU-LiClO that fritter prepares in advance
4Solid electrolyte material is placed on above-mentioned two-layer centre as ion conductive layer e; the flattening of under 90 ℃ of temperature, exerting pressure; make three layers tight compound; the protection of plastic packaging dress is crossed through two-layer packaging protection plastic layer a, i again in the outside then; the external two 1.5V button cells of extraction electrode on two-layer substrate conductive electrode layer c, g; promptly make all solid state plastics electrochromic device as shown in Figure 1, realize electrochromism.
Embodiment 2:
Plastic lining bottom b, h adopt polyester slice PET film (thickness is 125 μ m).A plastic lining bottom h goes up and adopts magnetron sputtering technique to prepare ITO transparency conductive electrode layer g (thickness is 30nm) therein, and then adopts low pressure reaction ion assisted deposition electron beam evaporation deposition technology to prepare WO on its surface
3Electrochromic layer f, thickness are 400nm.The WO that applies of Nafion solution with dilution
3The surface, air drying 2 hours makes the Nafion film forming form ion conductive layer e.Adopt magnetron sputtering technique to prepare Al metallic conduction electrode layer c on another piece plastic lining bottom b, thickness is 300nm, and then adopts low-voltage ion assistant depositing electron beam evaporation deposition technology to prepare NiO ion storage d on its surface, and thickness is 300nm.Then above-mentioned two parts that make are carried out pressing; the protection of plastic packaging dress is crossed through two-layer transparent packaging protection plastic layer a, i again in last outside; the external two 1.5V button cells of extraction electrode are promptly made the reflecting type electrochromic device of structure as shown in Figure 1 on two-layer substrate conductive electrode layer c, g.
Claims (9)
1. all solid state plastics electrochromic device, comprise substrate layer (b, h), conductive electrode layer (c, g), electrochromic layer (f) and ion conductive layer (e), it is characterized in that: described substrate layer (b, h) adopts the optical plastic material, and ion conductive layer (e) adopts the high molecular polymer solid electrolyte material.
2. all solid state plastics electrochromic device according to claim 1; it is characterized in that: described device comprises eight layers of structure, is followed successively by conductive electrode layer (c, g), plastic lining bottom (b, h) and packaging protection plastic layer (a, i) at ion conductive layer (e) and electrochromic layer (f) both sides.
3. all solid state plastics electrochromic device according to claim 2 is characterized in that: described ion conductive layer (e) and electrochromic layer (f) are merged into one deck.
4. all solid state plastics electrochromic device according to claim 2 is characterized in that: be provided with ion storage (d) between described conductive electrode layer (c) and the ion conductive layer (e).
5. according to claim 1,2,3 or 4 described all solid state plastics electrochromic devices, it is characterized in that: also can increase protective seam, insulation course or picture and text layer in the described device architecture.
6. the preparation method of an all solid state plastics electrochromic device, it is characterized in that: this method comprises the processing step of following order:
(1) on plastic lining bottom (b), prepares conductive electrode layer (c), ion storage (d) successively;
(2) on plastic lining bottom (h), prepare conductive electrode layer (g), electrochromic layer (f) successively;
(3) ion conductive layer (e) is placed in the middle of two substrates that step (1) and step (2) make pressing;
(4) at last by packaging protection plastic layer (a, i) packaging protection.
7. the preparation method of a kind of all solid state plastics electrochromic device according to claim 6, it is characterized in that: the step of this method (3) is: the solid electrolyte film that will be made by the conductive polymer polymkeric substance is placed on pressing in the middle of two substrates that step (1) and step (2) make as ion conductive layer (e), perhaps the conductive polymer polymkeric substance is coated with therein and forms ion conductive layer (e) on a slice substrate, cover an other substrate, exerting pressure then, it is bonding to flatten.
8. the preparation method of a kind of all solid state plastics electrochromic device according to claim 6, it is characterized in that: preparation conductive electrode layer (c, g) can adopt physical vacuum deposition, chemical vapor deposition or sol-gel method in the step of this method (1) and (2), preferred magnetron sputtering technique.
9. the preparation method of a kind of all solid state plastics electrochromic device according to claim 6, it is characterized in that: preparation ion storage (d) and electrochromic layer (f) can adopt methods such as magnetron sputtering, ion assisted deposition, ionic reaction deposition or laser deposition in the step of this method (1) and (2), and preparation electrochromic layer (f) also can adopt methods such as print process, impact system, gluing method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031402755A CN1492274A (en) | 2003-08-26 | 2003-08-26 | Full solid plastic electrochromism device and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031402755A CN1492274A (en) | 2003-08-26 | 2003-08-26 | Full solid plastic electrochromism device and its preparing method |
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| CN1492274A true CN1492274A (en) | 2004-04-28 |
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| CN101852960A (en) * | 2010-05-14 | 2010-10-06 | 马鞍山市盛宁高分子材料科技有限公司 | Full-solid state macromolecule controllable electrochromism flexible film device and manufacturing method thereof |
| CN102057323A (en) * | 2008-06-06 | 2011-05-11 | 应用材料股份有限公司 | Method for manufacturing electrochromic devices |
| CN102830565A (en) * | 2012-09-03 | 2012-12-19 | 京东方科技集团股份有限公司 | An electrochromic thin film, an electrochromic device and a manufacturing method thereof |
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| CN104391413A (en) * | 2012-09-03 | 2015-03-04 | 京东方科技集团股份有限公司 | Electrochromic device |
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