CN100410791C - Method for preparing full solid electrochromic device with sol-gel - Google Patents
Method for preparing full solid electrochromic device with sol-gel Download PDFInfo
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Abstract
The related manufacture method for full-solid photochromic device comprises: with sol-gel method, preparing the transparent conductive layer, the photochromic layer, the ion conductive layer and the ion storage layer in turns; then assembling together. Compared with prior art, this invention is low cost and easy controlled, and fit to large-scale industrial production.
Description
Technical field
The invention belongs to function element and electrochemical material technical field, be specifically related to a kind of preparation full-solid electrochromic device method.
Background technology
So-called electrochromism (Electrochromic is called for short EC) is meant material under the extra electric field effect, and the phenomenon that stable reversible color changes takes place, and then shows as the reversible variation of color and transparency on appearance property.Along with energy-saving and environmental protection, aesthetics are deep day by day, (Lampert C.M., Solar Energy Mater.﹠amp such as Lampert; Solar Cells, 1994,32:307-321) propose electrochromic device (ECD) is applied to the energy-saving lighting system of buildings, vehicle etc., the exploitation electrochromic is smart window (Smart Window).Adopt this smart window when obtaining best daylighting condition, control enters the solar radiation energy of buildings effectively, thereby reduces the energy that consumes because of indoor temperature control, has efficient, low consumption, green, pollution-free, intelligentized characteristics.Simultaneously, electrochromic device (ECD) automobile Antiglaring rear mirror, controlled smart window, Optical Electro-Chemistry can conversion and fields such as storage, low energy consumption display screen have a wide range of applications.The tradition electrochromic device is formed (as shown in Figure 1) by the five-layer structure of transparency conducting layer/electrochromism (EC) layer/ion conductive layer/ion storage (IS) layer/transparency conducting layer.Transparency conducting layer plays the effect of conduction electron as electrode, prepares transparent conductive film at present and mainly adopts direct current magnetron sputtering process, but the price height of large-scale magnetron sputtering apparatus, causes preparing the cost height of this film.Electrochromic layer plays a decisive role to the performance of whole electrochromism smart window, is accompanied by H
+, L
1 +Deng the injection or the extraction of small ion, the optical absorption characteristics generation modulation of film, that research is comprehensive, the most deep at present is WO
3, preparation WO
3Layer also mainly adopts sputtering technology, its technology controlling and process complexity, manufacturing cost height.The function of ion storage layer is to stop the deposition of ion on electrode, and when the EC layer was injected into ion, the IS layer was supplied with ion to dielectric substrate, and the EC layer is when being drawn out of ion, and the IS layer gets up ion collection, with the electric neutrality of maintenance dielectric substrate.Nickel oxide is proved to be a kind of good ion storage layer material, and the preparation method of nickel oxide film mainly contains physical methods such as electron beam evaporation and sputter, also has the high problem of cost.Ion conductive layer provides the transmission channel of electrochromic effect desired ion.Electrolyte traditional among the ECD is generally liquid electrolyte, and there are the problems such as accumulation of the freezing of device package, liquid, side reaction product in this class electrolyte, so people have studied the high solid material of ionic conductivity and replace liquid electrolyte.The technology controlling and process complexity of traditional each layer of preparation electrochromic device, the manufacturing cost height, thus limited the development of electrochromic device to large tracts of landization, industrialization direction.
Summary of the invention
It is convenient to the objective of the invention is to propose a kind of technology controlling and process, and manufacturing cost is lower, is easy to realize the industrialized method for preparing full-solid electrochromic device.
The full-solid electrochromic device structure that the present invention relates to as shown in Figure 1, five-layer structure by transparency conducting layer/electrochromic layer/ion conductive layer/ion storage/transparency conducting layer is formed, wherein, each layers such as transparency conducting layer, electrochromic layer, ion storage, ion conductive layer all adopt the sol-gel process preparation.
The composition weight share meter of described transparency conducting layer is as follows:
100 parts of the homodisperse slurries of nanosize metal oxide powder,
Film forming agent 0.1-80 part,
PH regulator agent 0-50 part,
Cosolvent 0-50 part,
The homodisperse slurry of nanosize metal oxide powder here is a kind of of tin indium oxide, tin-antiomony oxide, Al-Doped ZnO or titania, and slurry is dispersed in the ethanol by above-mentioned metal-oxide powder and forms, and its weight concentration is 20-30%.
Described film forming agent refers to nanometer grade powder to be sticked together and is attached on material on the substrate material surface, and its composition proportion is as follows:
25 parts of silane coupling agents (as KH560) (weight),
Silicasol (as FSI) 50-70 part (weight),
Ethanol (analyzing pure AR) 20-60 part (weight),
Ethyl orthosilicate 20-80 part (weight),
Epoxy resin (as E-51) 0.5-1 part (weight),
Maleic acid (analyzing pure AR) 2-4 part (weight).
Described pH regulator agent is meant and is used for the pH value of regulation system and the acidity or the basic component that add in system, example hydrochloric acid, acetic acid, ammoniacal liquor etc., but be not limited only to this.
Described cosolvent is meant the solvent that adds for the evaporation rate of controlling solvent, as normal butyl alcohol.
Described electrochromic layer is meant and is accompanied by H
+The river go into or extract out, the high molecular coating of the metal oxide or the tool conjugated structure of modulation can take place in the optical absorption characteristics of film, as tungsten oxide, molybdena, yttrium oxide, polyaniline, polypyrrole, polypyridine or polythiophene etc., but is not limited only to this.
Described ion storage, be meant when the working electrode electrochromic layer is broken when injecting ion, supply with ion, and working electrode is when being drawn out of ion to dielectric substrate, ion collection is got up to keep dielectric substrate to be electroneutral inorganic or organic coating, as nickel oxide (N
1O
x), vanadium oxide (V
2O
3) or cobalt oxide (CoO) etc., but be not limited only to this.
Described ion conductive layer is the full solid state polymer electrolyte layer with higher proton conductive ability, and it consists of:
100 parts in polymkeric substance (repetitive molal quantity)
Lewis-acidic components 01-80 part (molal quantity)
The polymkeric substance here refers to be polymkeric substance lewis base property, have certain transparency under filminess, as polyvinyl alcohol (PVA), polyoxyethylene, polyvinylpyrrolidone, polyvinyl butyral alcohol or polyvinyl alcohol tetrazole etc., but is not limited only to this.
Described Lewis-acidic components is meant can provide proton (H
+), nonvolatile inorganic, organic acid or acidic salt, as phosphoric acid, sulfuric acid, phosphotungstic acid or ammonium dihydrogen phosphate (ADP) etc., but be not limited only to this.
The present invention relates to prepare the concrete steps of electrochromic device with sol-gel as follows:
(1) processing of glass baseplate, glass baseplate is 2, removes the dust and the dirt on glass baseplate surface.As cleaning with acetone earlier, in 10% NaOH solution, soaked 2 hours then, take out the back and clean dry for standby with clear water;
(2) the preparation transparency conducting layer adds film forming agent, pH regulator agent and cosolvent in finely dispersed nanosize metal oxide slurry, and the pH value of slurry is 3-3.5, and it is coated on treated two glass baseplate surfaces, makes transparent conductive film;
(3) adopt sol-gel process on the transparency conducting layer of two glass baseplates, to prepare electrochromic layer and ion storage layer respectively;
(4) the full solid state polymer electrolyte layer that adopts the sol-gel process preparation to have higher proton conductive ability, specifically can be the electrochromic layer of base material with glass or be direct pouring full solid state polymer electrolyte layer on the ion storage layer of base material with glass, drying and forming-film then, compound with another part again, another part is meant the part of the full solid state polymer electrolyte layers of not casting, also can be earlier at template top casting polyelectrolyte floor, film forming then, reusable heat platen press and other parts layer are compound, and be promptly compound with electrochromic layer and ion storage layer two parts of with glass being base material.
(5) adopt the epoxy sealing device, note making the electrically conducting transparent layer segment to expose during sealing or introduce in advance picking out lead.
The employing sol-gel process that the present invention proposes prepares the method for each layer of full-solid electrochromic device, compare with other traditional preparation method, it is simple to have process equipment, do not need other expensive equipment of special vacuum coating conditioned disjunction, cost is lower, is convenient to application, the technological process temperature is low, make uniform multivariant oxide film easily, be easy to quantitative doping, can control advantages such as the composition of film and micromechanism effectively.So there is very big advantage in the technology of this preparation full solid-state device at aspects such as cost, preparation technologies, all assemble with each layer of sol-gel process fabricate devices and based on this preparation technology's device, similar report is not arranged in the document as yet.
Description of drawings
Fig. 1 Structures of Electrochromic Devices and/synoptic diagram of color fading reaction.
Fig. 2 full-solid electrochromic device respectively+3V and-the visible light spectrogram of the painted and colour killing attitude of 3V voltage.
Embodiment
Following examples are only for further specifying the present invention, are not violating under the purport of the present invention, and the present invention should be not limited to the content that following experimental example is specifically expressed.
The preparation of each layer of electrochromic device:
(1) preparation of transparency conducting layer:
Raw materials used as follows:
Nano-indium stannum oxide alcohol slurry (20-30nm) east, Ningxia non-ferrous metal group
Normal butyl alcohol (analyzing pure AR) Shanghai Ling Feng chemical reagent company limited
Hydrochloric acid (analyzing pure AR) Chemical Reagent Co., Ltd., Sinopharm Group
Silane coupling agent (KH560) Nanjing and good fortune chemical plant
Silicasol (FSI) Zhejiang Province Yuda Chemical Co., Ltd
Ethanol (analyzing pure AR) Chemical Reagent Co., Ltd., Sinopharm Group
Chemical reagent purchase and supply 5-linked chemical plant, ethyl orthosilicate Shanghai
Epoxy resin (E-51) Zhejiang goodization Industry Co.,Ltd
Maleic acid (analyzing pure AR) Chemical Reagent Co., Ltd., Sinopharm Group
Homemade film forming agent raw material proportioning is as follows:
25 parts of silane coupling agents (KH560) (weight)
50 parts of silicasol (FSI) (weight)
Ethanol (analyzing pure AR) 20 parts (weight)
20 parts of ethyl orthosilicates (weight)
0.5 part of epoxy resin (E-51) (weight)
Maleic acid (analyzing pure AR) 3 parts (weight)
The raw material proportioning of prepared transparency conducting layer is as follows:
100 parts of homodisperse slurries of ito powder (weight)
15 parts of film forming agents (weight)
10 parts of hydrochloric acid (weight)
2 parts of normal butyl alcohols (weight)
Preparation technology: according to proportioning the nano-indium stannum oxide alcohol slurry is slowly added film forming agent and cosolvent normal butyl alcohol under magnetic agitation, with the pH value of watery hydrochloric acid regulation system to 3-3.5.Continue to stir 1h, slurry is mixed.The employing spin-coating method (sol evenning machine, the KW-4A type, Chemat Technology, Inc, USA) coating with above-mentioned preparation is coated on the glass basis surface of handling, and at room temperature will put into baking oven after the solvent evaporates, at 120 ℃ of following film-formings.
(2) the preparation reference literature method of electrochromic layer (ozkan E., Tepehan F.Z., Solar EnergyMaterials ﹠amp; Solar Cells, 2001,68265-277)
Raw materials used as follows:
Wolframic acid (H
2WO
4) (analyzing pure AR) Shanghai chemical reagents corporation provides.
Shanghai chemical reagents corporation of citric acid (analyzing pure AR) Chinese Medicine group
Hydrochloric acid (analyzing pure AR) Chemical Reagent Co., Ltd., Sinopharm Group
Hydrogen peroxide (analyzing pure AR) Yixing City second chemical reagent work
Preparation technology: in the high purity water of 100ml, ultrasonic dispersion made its dissolving in 10 minutes, added the citric acid solution of low-grade fever therein with the tungsten oxide powder dissolution, and regulating the pH value is 1, and this liquid is gel very easily, according to 10ml (colloid): 0.6ml (15%H
2O
2) ratio add hydrogen peroxide with stable sol.Continue ultrasonic dispersion, obtain the water white WO that contains the nano-scale of citric acid
3.2H
2O colloidal sol adopts spin-coating method to form WO at the ITO substrate surface
3Film.In baking oven, film is dried processing (100 ℃, constant temperature 1h), the film of oven dry is put into baking oven, carry out the 2h annealing in process, promptly obtain amorphous WO at 150 ℃
3Film.(strict control programming rate in the time of annealing in process, about 2 ℃/minute, otherwise crackle and hole can appear in film, and also can badly influence the discoloration of film.)
(3) the preparation reference literature method of ion storage (Wang Lianchao, Meng Fanli, Sun Yufeng, Huang Hangjiu, Liu Jinhuai, Journal of Inorganic Materials, 2004,19 (6): 1391-1396):
Raw materials used as follows:
Prompt chemical reagent company limited is moistened in nickel acetate (analyzing pure AR) Shanghai.
NaOH Jiangsu Jin Cheng chemical reagent work (Kunshan)
Shanghai chemical reagents corporation of ethanol (analyzing pure AR) Chinese Medicine group
Ammoniacal liquor (analyzing pure AR) Shanghai development chemical industry two factories
Preparation technology: adopt nickel acetate to be dissolved in the alkoxide of making nickel in distilled water and the ethanol, solution is carried out the basic hydrolysis catalytic reaction, add an amount of stabilizing agent again, prepare no flocculent deposit, the translucent precursor glue of homogeneous phase through fully stirring with NaOH.Adopt spin-coating method to form N at the ITO substrate surface
1O
xFilm, dry 30min in 80 ℃ of drying boxes puts into 500 ℃ of muffle furnace insulations 1 hour more then, finally obtains having the nickel oxide film of electrochromic property.
(4) preparation reference literature ten thousand methods of ion conductive layer (Petty-Weeks, Zupancic J.J., Swedo J.R., Solid State Ionics, 1988,31:117-125).
Raw materials used as follows:
Polyvinyl alcohol (PVA), number-average molecular weight Mn are 17200, Aldrich company product.
The phosphoric acid of 85wt%, Shanghai amalgamation factory products.
Preparation technology: take by weighing a certain amount of polyvinyl alcohol (PVA) (PVA), phosphoric acid according to certain proportioning, earlier PVA is dissolved in deionized water, being stirred to PVA with magnetic stirring apparatus at 90-105 ℃ of following constant temperature dissolves fully, get the thick liquid of transparent homogeneous, add phosphoric acid then, continue constant temperature and stir 2h, mix, method film forming on polyfluortetraethylene plate with this solution adopts casting to film after the vacuum drying, promptly gets all solid state polymer non-aqueous proton conducting film.
(5) assembling of full-solid electrochromic device: the ionic conduction layer material that makes above both can adopt the method for blade coating directly in electrochromic layer (or ion storage layer) top casting, drying and forming-film then, which floor is compound with other again by mode shown in Figure 1, also can adopt and make earlier all solid state film on other template, which floor is compound for reusable heat platen press and other.Adopt the epoxy sealing device, note making the ITO layer segment to expose during sealing or introduce in advance picking out lead.
The test of electrochromic device (ECD) performance: the transmittance of employing 760CTR twin-beam ultra-violet and visible spectrophotometer (Shanghai Precision Scientific Apparatus Co., Ltd) mensuration ECD as shown in Figure 2.
The preparation of transparency conducting layer:
Raw materials used as follows:
Al-Doped ZnO (AZO) is east, Ningxia non-ferrous metal group (20-30nm).
The raw material proportioning of prepared transparency conducting layer is as follows:
100 parts of homodisperse slurries of AZO (weight)
15 parts of film forming agents (weight)
10 parts of hydrochloric acid (weight)
2 parts of normal butyl alcohols (weight)
The preparation of film forming agent, similar shown in the preparation flow of the preparation flow of transparency conducting layer and other layer of full-solid electrochromic device and device assembling and the embodiment 1, obtain the electrochromic property of device and shown in Figure 2 similar.
The preparation of transparency conducting layer:
Raw materials used as follows:
Al-Doped ZnO (AZO) is east, Ningxia non-ferrous metal group (20-30nm).
The raw material proportioning of prepared transparency conducting layer is as follows:
100 parts of homodisperse slurries of AZO (weight)
15 parts of film forming agents (weight)
10 parts of hydrochloric acid (weight)
2 parts of normal butyl alcohols (weight)
The preparation of film forming agent, similar shown in the preparation flow of the preparation flow of transparency conducting layer and other layer of full-solid electrochromic device and device assembling and the embodiment 1, obtain the electrochromic property of device and shown in Figure 2 similar.
In the foregoing description, the parameter of each component raw material and consumption and preparation process, it only is the representative of choosing in order to describe the present invention, in fact a large amount of experiments show, all can obtain each layer of electrochromism and corresponding full-solid electrochromic device with above-mentioned similar performance in experiment content part institute restricted portion.
Claims (6)
1. the preparation method of a full-solid electrochromic device, this device is formed by transparency conducting layer, electrochromic layer, ion conductive layer, ion storage and transparency conducting layer are compound successively, it is characterized in that adopting sol-gel process to prepare transparency conducting layer, electrochromic layer, ion conductive layer and ion storage successively, concrete steps are as follows:
(1) processing of glass baseplate, glass baseplate is 2, removes the dust and the dirt on glass baseplate surface;
(2) the preparation transparency conducting layer adds film forming agent, pH regulator agent and cosolvent in the finely dispersed slurry of nanosize metal oxide powder, and it is coated on treated two glass baseplate surfaces, makes transparent conductive film;
(3) adopt sol-gel process on the transparency conducting layer of two glass baseplates, to prepare electrochromic layer and ion storage layer respectively;
(4) the full solid state polymer electrolyte layer that adopts the sol-gel process preparation to have higher proton conductive ability, direct pouring full solid state polymer electrolyte layer on the ion storage layer of the electrochromic layer of glass baseplate or glass baseplate, drying and forming-film is compound with another part more then; Perhaps earlier at template top casting polyelectrolyte floor, film forming then, reusable heat platen press and other parts layer are compound; Here said another part is meant the part of the full solid state polymer electrolyte of not casting;
(5) adopt the epoxy sealing device, note making the electrically conducting transparent layer segment to expose during sealing or introduce in advance picking out lead;
Wherein, it is as follows that described transparency conducting layer is formed the weight share meter:
100 parts of the homodisperse slurries of nanosize metal oxide powder,
Film forming agent 0.1-80 part,
PH regulator agent 0-50 part,
Cosolvent 0-50 part,
Here, described nanosize metal oxide powder is one or more of tin indium oxide, tin-antiomony oxide, Al-Doped ZnO, titania, and slurry is that above-mentioned metal-oxide powder is scattered in the ethanol and forms, and weight concentration is 20-30%;
Described film forming agent, its composition weight share meter is as follows:
25 parts of silane coupling agents,
Silicasol 50-70 part,
Ethanol 20-60 part,
Ethyl orthosilicate 20-80 part,
Epoxy resin 0.5-1 part,
Maleic acid 2-4 part,
Described pH regulator agent is to be used for the pH value of regulation system and the acidity or the basic component that add in system;
Described cosolvent is the solvent that adds for the rate of volatilization of controlling solvent.
2. preparation method according to claim 1, its feature is being that described electrochromism layer material is tungsten oxide, molybdena, yttrium oxide, polyaniline, polypyrrole, polypyridine or polythiophene.
3. preparation method according to claim 1 is characterized in that described ion storage layer material is nickel oxide, vanadium oxide or cobalt oxide.
4. preparation method according to claim 1 is characterized in that described ion conductive layer consists of:
100 parts in polymkeric substance, by the repetitive molal quantity,
Lewis acid 0.1-80 part, by molal quantity,
The polymkeric substance here is to be polymkeric substance lewis base property, have the transparency under filminess;
Described lewis acid is that proton (H can be provided
+), nonvolatile inorganic, organic acid or acidic salt.
5. preparation method according to claim 4 is characterized in that described polymkeric substance is polyvinyl alcohol (PVA), polyoxyethylene, polyvinylpyrrolidone, polyvinyl butyral alcohol or polyvinyl alcohol tetrazole.
6. preparation method according to claim 4 is characterized in that described lewis acid is phosphoric acid, sulfuric acid, phosphotungstic acid or phosphoric acid dihydro amine.
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