CN100371416C - Inorganic-organic compound solution type electrochromism material and appliance and preparation process thereof - Google Patents
Inorganic-organic compound solution type electrochromism material and appliance and preparation process thereof Download PDFInfo
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- CN100371416C CN100371416C CNB2005101124093A CN200510112409A CN100371416C CN 100371416 C CN100371416 C CN 100371416C CN B2005101124093 A CNB2005101124093 A CN B2005101124093A CN 200510112409 A CN200510112409 A CN 200510112409A CN 100371416 C CN100371416 C CN 100371416C
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Abstract
The present invention relates to an inorganic-organic compound solution type electrochromism material, an appliance and a preparation method thereof, and belongs to the field of electrochromism material and appliances. The inorganic-organic compound solution type electrochromism material contains inorganic material and organic discoloring material, wherein the inorganic material is obtained through the process that one kind or several kinds of inorganic titanium sources which can generate titanium ions are dissolved in water or organic solvent, and the organic discoloring material is purple rose essence. The inorganic-organic compound solution type electrochromism appliance comprises substrates (a and f), conductive electrodes (b and e), organic-inorganic compound discoloring solution (g), an insulation thin film (d) and encapsulation material (c). When the appliance is prepared, by a sol-gel magnetron sputtering technology and a CVD and PVD method, a layer of the substrates is formed with a surface conductive electrode layer; then, the conductive surface of the substrate provided with surface conductive electrodes is positioned inwards, three edges uses the insulation thin film as space, the distance between the two conductive surfaces is controlled, and the outer part of the insulation thin film is glued with the encapsulation material and solidified; and finally, the inorganic-organic compound electrochromism material is injected into the appliance, an injecting mouth is solidified with the encapsulation material, and the electrodes are connected.
Description
Technical field
The present invention relates to a kind of inorganic-organic compound solution type electrochromic material and device and preparation method, belong to electrochromic material and devices field.
Technical background
Along with the information age today develop rapidly, in the research of the flat-panel monitor of pursuing ultra-thin, reduce power consumption, electrochromic display device has low driving voltage, super contrast gradient clearly, broad visual angle and superior memory effect become the research focus of new display and e-book and electronic newspaper.Add that to the serious day by day energy and the attention of environmental problem, national governments have dropped into great amount of manpower and financial resources are carried out the research and development of electrochromic material and device.
Electrochromic material can be divided into two big classes, and a class is inorganic off-color material, and is modal as MoO
3, V
2O
5, NiO
2, WO
3Or the like.But, for this class electrochromic material, reach practical requirement in order to make its coloration efficiency, must make the ion of injection and electronics be deep into the sull body phase material, its variable color is longer switching time as a result.In addition, the preparation of this type oxide film is had relatively high expectations, should not be too high as Tc, and crystal formation needs strict control.So this class material can not be as MATERIALS FOR DISPLAY.
Another kind of is the organic electrochromic material, by the gain and loss generation oxidation-reduction reaction of electronics, thereby realize painted and fade reversible change.Compare with inorganic electrochromic material, the organic electrochromic material has following several main advantage: the first, and organic electrochromic material variable color speed is very fast, can reach femtosecond; The second, the organic electrochromic material is painted and the contrast gradient of fading is very high, and simultaneously, different gray scales can realize by the size of extra electric field.This just means that the organic electrochromic material has superiority aspect ultra thin device; The 3rd, organic electrochromic material driving voltage is very low, saves the energy; Simultaneously, even after the outage, also keep color changeable effect, has memory effect.
Therefore, people adopt inorganic thin film as photochromic layer usually, or use organic off-color material to prepare electrochromic device as photochromic layer.But up to now, inorganic-organic composite electrochromic material and device yet there are no report.
Summary of the invention
One of purpose of the present invention is to develop a kind of electrochromic material of organic and inorganic compound solution type, makes this class material have all fast (<1s) the advantage of painted time and fading time.
The electrochromic material of this organic and inorganic compound solution type, it has comprised inorganic materials and organic off-color material.
Wherein inorganic materials mainly comprises TiCl
3, TiCl
4Wait one or several can produce the inorganic ti sources of titanium ion.Water-soluble or the organic solvent of one or several inorganic ti sources wherein just can obtain Ti
+ 3Perhaps Ti
+ 4Solution.This inorganic titanium ion solution is transparent faint yellow.
Organic off-color material mainly is all kinds of straight chain purpurines, as methyl viologen, and ethyl purpurine etc.; And all kinds of purpurine polymkeric substance, as gathering ethyl purpurine etc.They are dissolved in the inorganic titanium ion solution in accordance with the appropriate ratio, just can obtain the compound variable color solution of organic and inorganic.This solution is clear, colorless.
In order to improve coloration efficiency and time of response, the ratio by titanium ion and straight chain purpurine or purpurine polymer molecule realizes.The mole ratio range of general titanium ion and straight chain purpurine or purpurine polymkeric substance is 1: 50-10: between 1.
Organic and inorganic compound solution type electrochromic material of the present invention, its painted and reaction mechanism that fade be organic and the contention of inorganics for electronics on, with methyl viologen and Ti
+ 4System be example, when impressed current, following reaction takes place:
MV
2+(colourless)+e → MV
+(blueness) (1)
When external voltage removed, following reaction took place:
Ti
+ 4+ MV
+(blueness) → Ti
+ 3+ MV
2+(colourless) (2)
Another object of the present invention provides a kind of novel solutions type electrochromic device and preparation method, and as shown in Figure 1 in the Figure of description, this novel solutions type electrochromic device comprises:
Substrate (a, f), conductive electrode (b, e), inorganic-organic compound solution type electrochromic material (g), insulation film (d), packaged material (c).
Wherein: substrate adopts opticglass or flexible transparent plastic, and conductive electrode is made by the conductive film of metal oxide, can pass through sol-gel, magnetron sputtering technique, CVD, the preparation of technology such as PVD, packaged material can adopt UV to solidify glue or silicon rubber or double faced adhesive tape.
Device adopts sandwich structure, totally three layers.Conductive electrode is attached on the substrate, the conductive electrode face in opposite directions inwardly, insulation film is controlled the distance between two conducting surfaces as pad, between two-layer conductive electrode, encapsulation one deck inorganic-organic compound solution type electrochromic material.The outside of insulation film is bonding and curing with packaged material.Between two-layer conductive electrode, add the dc low-voltage driving voltage, just can realize the reversible change of color.
This preparation of devices method is at first to prepare the surface conduction electrode layer on substrate layer.Then, with the conducting surface of this substrate with surface conduction electrode inwardly, three limits as the space, controls the distance between two conducting surfaces with insulation film, and the outside of insulation film is bonding and curing with packaged material.At last, with organic and inorganic compound electrochromic material wherein with injection, geat place encapsulation material solidifies, the connection of electrode can be chosen in before the encapsulation or after the encapsulation, this electrochromic device is as long as variable color under the driving of external volts DS.Remove voltage, just can fade.Adding driving voltage can conveniently select between 3-5V DC.
This novel electrochromic device has following characteristics:
(1) device of the present invention is that the photochromic layer and the ion conductive layer of common electrochromic device is alternative with organic and inorganic compound electrochromic material, has simple sandwich structure.
(2) such novel electrochromic device quality is light, cost is low, and preparation technology is simple, when realizing fast colorizing, can realize fading fast (<1s).
Because These characteristics, the present invention can satisfy the requirement of smart window and antidazzle mirror, aspect plate electrochromic display device, has shown bigger potentiality in addition.
Description of drawings
Fig. 1 is a structural representation of the present invention.Comprise: substrate (a, f), conductive electrode (b, e), inorganic-organic compound solution type electrochromic material (g), insulation film (d), packaged material (c).
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further detailed, but is not only to be confined to embodiment.
The ito thin film of magnetron sputtering on opticglass (thickness 100-300nm) can abbreviate ito glass as.Its transmittance>80%, resistivity is less than 200 Ω cm.Its resistivity is the smaller the better.
Ito glass is cut into 2.5 * 3cm
2Size is attached to insulation film on three limits of ito glass conducting surface, leaves certain space outside the edge.The conducting surface of an other ito glass is placed on the packing ring of insulation film composition inwardly, clamps,, solidify the glue package curing with UV with the outside of the packing ring between two ito glasses with clip; Adopt TiCl
4With methyl viologen be raw material, the mole ratio range of pressing titanium ion and purple sieve essence feeds nitrogen 30min earlier at 1: 20 preparation organic and inorganic compound variable color solution, then, with syringe the compound variable color solution of organic and inorganic is injected, injection port solidifies glue with UV to be sealed.At two substrate conductive electrode extraction electrode external direct current power supplies, can obtain electrochromic device as shown in Figure 1, realize electrochromism.
Claims (6)
1. the electrochromic material of an organic and inorganic compound solution type, it is characterized in that comprising inorganic materials and organic off-color material, wherein inorganic materials is one or several water-soluble or organic solvents of inorganic ti sources that can produce titanium ion, and organic off-color material is straight chain purpurine or purpurine polymkeric substance.
2. by the electrochromic material of the described a kind of organic and inorganic compound solution type of claim 1, the mole proportioning that it is characterized in that described titanium ion and straight chain purpurine or purpurine polymkeric substance is 1: 50-10: 1.
3. by the electrochromic material of claim 1 or 2 described a kind of organic and inorganic compound solution types, it is characterized in that described inorganic ti sources is TiCl
3Or TiCl
4
4. inorganic-organic compound solution type electrochromic device that uses claim 1 or the preparation of 2 or 3 described inorganic-organic compound solution type electrochromic materials is characterized in that device comprises:
Substrate (a, f), conductive electrode (b, e), the compound variable color solution of organic and inorganic (g), insulation film (d), packaged material (c);
Device adopts sandwich structure, conductive electrode is attached on the substrate, the conductive electrode face in opposite directions inwardly, insulation film is as pad, control the distance between two conducting surfaces, between two-layer conductive electrode, encapsulation one deck inorganic-organic compound solution type electrochromic material, the outside of insulation film is bonding and curing with packaged material.
5. by the described inorganic-organic compound solution type electrochromic device of claim 4, it is characterized in that substrate adopts opticglass or flexible transparent plastic, conductive electrode adopts conductive film to make, and packaged material adopts UV to solidify glue or silicon rubber or double faced adhesive tape.
6. by the preparation method of claim 4 or 5 described inorganic-organic compound solution type electrochromic devices, it is characterized in that:
At first pass through sol-gel, magnetron sputtering technique, CVD, the method for PVD prepares the surface conduction electrode layer on substrate layer,
Then, with the conducting surface of this substrate with surface conduction electrode inwardly, three limits as the space, controls the distance between two conducting surfaces with insulation film, and the outside of insulation film is bonding and curing with packaged material,
At last, with injecting wherein, geat place encapsulation material solidifies is before the connection of electrode can be chosen in and encapsulate or after the encapsulation with organic and inorganic compound electrochromic material.
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CNB2005101124093A CN100371416C (en) | 2005-12-30 | 2005-12-30 | Inorganic-organic compound solution type electrochromism material and appliance and preparation process thereof |
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CNB2005101124093A CN100371416C (en) | 2005-12-30 | 2005-12-30 | Inorganic-organic compound solution type electrochromism material and appliance and preparation process thereof |
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CN100371416C true CN100371416C (en) | 2008-02-27 |
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CN102540607A (en) * | 2010-12-07 | 2012-07-04 | 介面光电股份有限公司 | Electrochromism module made of organic and inorganic materials and display device combined with module |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1024394A1 (en) * | 1999-01-26 | 2000-08-02 | Bayer Aktiengesellschaft | Photochromic and electrochromic device, solutions for uses therein and use thereof |
WO2004067672A1 (en) * | 2003-01-31 | 2004-08-12 | Ntera Limited | Electrochromic particles |
US20050179012A1 (en) * | 2003-12-22 | 2005-08-18 | Kwon Won J. | Electrochromic material with improved lifetime |
-
2005
- 2005-12-30 CN CNB2005101124093A patent/CN100371416C/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1024394A1 (en) * | 1999-01-26 | 2000-08-02 | Bayer Aktiengesellschaft | Photochromic and electrochromic device, solutions for uses therein and use thereof |
WO2004067672A1 (en) * | 2003-01-31 | 2004-08-12 | Ntera Limited | Electrochromic particles |
US20050179012A1 (en) * | 2003-12-22 | 2005-08-18 | Kwon Won J. | Electrochromic material with improved lifetime |
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