CN104076568A - Preparation method for multi-state electrochromic device - Google Patents
Preparation method for multi-state electrochromic device Download PDFInfo
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Abstract
The invention relates to a preparation method for a multi-state electrochromic device, which belongs to the technical field of functional materials and devices. The preparation method comprises the following specific steps: 1) preparing electrolyte solution; 2) cutting two transparent conductive substances and a polytetrafluoroethylene plate with the width which is equal to the width of the transparent conductive substances, the length which is 3-7mm less than the length of the transparent conductive substances, and the thickness of 0.3-0.7mm, forming a square through hole in the middle of the polytetrafluoroethylene plate, the distance from the edge of the through hole to the edge of the corresponding polytetrafluoroethylene plate being 3-7 mm, washing and drying for the future use; 3) spin-coating a base metal oxide nano-particle dispersion liquid on one substrate conductive layer, and then sintering; 4) bonding the polytetrafluoroethylene plate on the substrate conductive layers which are not spin-coated, pouring the electrolyte solution in the through hole, then bonding the spin-coated substrate conductive layers towards the through hole, two substrates being staggered at a distance of 3-7mm in a long side direction and completely covering the polytetrafluoroethylene plate, and finally encapsulating by epoxy resin. The electrochromic device prepared by the preparation method disclosed by the invention is capable of realizing transparent, mirror-surface and black three-colour-state reversible conversion.
Description
Technical field
The present invention relates to a kind of preparation of polymorphic electrochromic device, belong to functional material and device technology field.
Background technology
The electrochromism phenomenon of material refers to that some material under the effect of applying electrical potential, redox reaction occurs and causes it that optical transmission rate or reflectivity are occurred to for phenomenon of reversible variation.Since Deb utilized WO in 1969
3film preparation has gone out to beat the world since an electrochromic device (ECD), electrochromic device based on various material systems and different structure is constantly devised, with regard to its system, be mainly divided into following three classes: the first kind is (to be mainly Li by executing that alive mode injects or extract ion out in electrochromic material
+, H
+) realize variable color, as transition metal oxide WO
3, NiO, V
2o
5, MoO
3deng (Crystalline WO
3nanoparticles for Highly Improved Electrochromic Applications-Adv.Mater.2006,18,763); Equations of The Second Kind is brought out and is caused the potpourri of rare earth element, rare earth element and potpourri that magnesium forms with transition metal to occur to change mutually by hydrogen, thereby realize the regulation and control of reflection coefficient (Surface Coating of Electrochromic Switchable Mirror Glass Based on Mg – Ni Thin Film for High Durability in the Environment-Appl.Phys.Express2010,3,042201); The 3rd class is the method deposition and resolution metal on electrically conducting transparent substrate by reversible electro-deposition, to realize the adjusting of substrate optical states (Bismuth Electrochromic Device with High Paper-Like Quality and High Performances-ACS Appl.Mater.Interfaces2010,2,1471).
Traditional electro-deposition method can only give electrochromic device transparent or light and minute surface two states conventionally, be difficult to realize the black state that light is had to extremely strong absorptive character, although at present existing bibliographical information (Electrochemical Optical-Modulation Device with Reversible Transformation Between Transparent, Mirror, and Black-Adv.Matter.2012, 24, OP122) can realize black state, but the nano-indium stannum oxide of its use (ITO) particle dispersion cost is very high, be unfavorable for practical application on a large scale and at industrial circle utilization and extention.
Summary of the invention
The present invention is directed to the problem proposing in above-mentioned background technology, the method based on reversible electro-deposition, has proposed a kind of preparation method of polymorphic electrochromic device.The present invention utilizes the nano particle of base metal oxide to realize black state, makes the conversion that the device for preparing can be between transparent, minute surface and three kinds of states of black, and three kinds of state successfuls, only need ± 2.5V of changing voltage.
Its preparation method comprises the steps:
Step 1: the AgNO that takes 0.1～2.5mmol
3, the Quaternary ammonium bromide of 0.5～12.5mmol, 0.1～0.5mmol mantoquita, be dissolved in the polar organic solvent of 10～50mL, and carried out magnetic agitation until solute all dissolves;
Step 2: 2 of the electrically conducting transparent substrates of selection 2.0cm * 1.5cm～25.5 * 25cm, utilize successively 2 electrically conducting transparent substrates described in deionized water and alcohol immersion, and in supersonic cleaning machine, clean 3～7 times, after washes clean, under the condition of 60～100 ℃, dry, standby;
Step 3: cutting width is consistent with the width of electrically conducting transparent substrate, short 3～the 7mm of length of Length Ratio electrically conducting transparent substrate, thickness is the polyfluortetraethylene plate of 0.3～0.7mm, in the middle of the polyfluortetraethylene plate cutting down, dig a square through hole, between through hole and corresponding teflon panel edges, width is 3～7mm, utilize respectively deionized water and absolute ethyl alcohol to rinse this polyfluortetraethylene plate 3～5 times, after cleaning, at 50～70 ℃, dry;
Step 4: compound concentration is the base metal oxide nanoparticulate dispersion that 0.01～0.1g/mL, grain size are 5～500nm, by it in 200～2000 revs/min of rotating speeds, time 3～20s is spun on any electrically conducting transparent substrate conductive layer in step 2, before spin coating, by needing to cover one deck width on the minor face of the transparent substrates conductive layer of spin coating, be wherein the seamless adhesive tape that 3～5mm, length are identical with minor face, the seamless adhesive tape that needs to tear after spin coating finishes, then at 200～700 ℃ of sintering 20～60 minutes in tubular annealing stove;
Step 5: polyfluortetraethylene plate prepared by step 3 binds on the conductive layer of the electrically conducting transparent substrate that the not spin coating of preparing in described step 2 has base metal oxide nanoparticulate dispersion, in its through hole, pour described step 1 product into, the conductor planes of being prepared by described step 4 to transparent substrates is again binded to through hole, two substrate long side directions, the 3～7mm that staggers wherein, polyfluortetraethylene plate is covered completely by electrically conducting transparent substrate, finally with epoxy resin, encapsulates again.
Quaternary ammonium bromide described in above-mentioned steps one is any one in cetab, tetrabutyl ammonium bromide, tetramethylammonium bromide, teabrom, ammonium bromide, DTAB.
Mantoquita in above-mentioned steps one is any one in copper nitrate, cupric chloride, copper sulphate.
Polar organic solvent in above-mentioned steps one is any one in formamide, dimethyl sulfoxide (DMSO) (DMSO), dimethyl formamide (DMF), dimethyl acetamide (DMAC), hexamethyl phosphoramide.
Electrically conducting transparent substrate in above-mentioned steps two is for scribbling In
2o
3: Sn (ITO), In
2o
3: Zn (IZO), In
2o
3: Nb, ZnO:Al (AZO), ZnO:Ga (GZO), ZnO:In (IZO), ZnO:Si (SZO), ZnO:B (BZO), ZnO:F (FZO), ZnO:Nb, ZnO:Sc, SnO
2: F (FTO), SnO
2: Sb (ATO), SnO
2: Ta or SnO
2: glass or the flexible substrate of W codope oxide, for example ITO/PET (polyethylene terephthalate), AZO/PET, AZO/PC (polycarbonate), AZO/PES (polyethersulfone), AZO/PVDF (polyvinylidene fluoride), AZO/TPT (polyvinyl fluoride composite membrane), GZO/PET, GZO/PC, GZO/PEN (Polyethylene Naphthalate), IZO/PET, IZO/PC, FTO/PET, ATO/PES.
In above-mentioned steps four, preparing the spreading agent that base metal nanoparticulate dispersion used is hydrophilic solvent: water, ethanol, ethylene glycol, or lipophilicity solvent: dimethylbenzene, diethylene glycol dibenzoate.
In above-mentioned steps four, described base metal oxide is any one in the oxide of titanium, zinc, aluminium, tin, tungsten, molybdenum, tantalum, magnesium, zirconium, germanium.
In above-mentioned steps four, the spin coating mode of base metal oxide nanoparticulate dispersion is: under 200～600 revs/min of the first slow-speed of revolution, rotate 3～8s, then rotate 10～20s under 1000～2000 revs/min of high rotating speeds.
In sum, the invention has the advantages that a kind of electro-deposition electrochromic device is provided, can be transparent, minute surface and black tri-state change, with low cost, and successful, adopts base metal oxide nano particle cheap and easy to get to substitute expensive nano-indium stannum oxide (ITO) particle dispersion electrode is modified.
Accompanying drawing explanation
Fig. 1. (a), for the side view of the device that assembles, (b) be device vertical view, is (c) polyfluortetraethylene plate (center section is through hole) with through hole.
Fig. 2. three kinds of states and the corresponding fundamental diagram thereof of this electrochromic device, (a) be mirror status; (b) be pellucidity; (c) be black state.
Embodiment
The experimental technique adopting in following embodiment, if no special instructions, is conventional method; Agents useful for same, material etc., if no special instructions, all can obtain from commercial channels.Below the specific embodiment of the present invention is specifically described, with TiO
2, ZnO is that example represents base metal oxide:
Embodiment 1
Step 1: the AgNO that takes 85mg (0.5mmol)
3, the tetrabutyl ammonium bromide (TBABr) of 806mg (2.5mmol) is, the CuCl of 13mg (0.1mmol)
2, be dissolved in the DMSO of 10mL, and carried out magnetic agitation until solute all dissolves;
Step 2: choose two block sizes and be the FTO glass of 3cm * 2.5cm as electrode, utilize successively deionized water and ethanol to soak it, and utilize supersonic cleaning machine to clean 5 times, after cleaning, at 80 ℃, dry, standby;
Step 3: getting a block size is 2.5cm * 2.5cm, the polyfluortetraethylene plate that thickness is 5mm digs the through hole of one 2cm * 2cm therebetween, then utilizes respectively deionized water, absolute ethyl alcohol to rinse polyfluortetraethylene plate 4 times, then at 60 ℃, dries, standby;
Step 4: the TiO that takes 0.5g
2nano particle, grain size is 20nm, is dissolved in the absolute ethyl alcohol (purity>=99.7%) of 10mL, sonic oscillation 30min, until TiO
2be dispersed in solution.Get any FTO glass in step 2, cover the seamless adhesive tape of one deck on the minor face of its conductive layer, width is 5mm, by the TiO configuring
2nanoparticulate dispersion is in 500 revs/min of low speed, 5s, and 1500 revs/min at a high speed, 15s, is spun on the conductive layer of this FTO glass, and the seamless adhesive tape of tearing after spin coating finishes utilizes tubular annealing stove sintering 30 minutes at 500 ℃ by the good FTO glass of spin coating;
Step 5: polyfluortetraethylene plate is binded to the not spin coating of preparing in step 2 TiO
2on the conductive layer of the FTO glass of nanoparticulate dispersion, and to the product of one preparation of implantation step in its through hole, then FTO glass spin coating prepared by step 4 has TiO
2the one side of nano particle is binded towards through hole, and wherein polyfluortetraethylene plate is covered completely by FTO glass, the long side direction 5mm that staggers between two blocks of FTO glass, and broadside overlaps, and encapsulates with epoxy resin.
The device that the present embodiment prepares, has fine electrochromic effect, can realize three kinds of obvious states---transparent, minute surface, black (seeing Fig. 2).Wherein only need 1～2s painted switching time, the long 1～2min that needs of fading time, whole process is all reversible, between three states, can arbitrarily change.
Embodiment 2
Step 1: the AgNO that takes 127.5mg (1mmol)
3, the tetrabutyl ammonium bromide (TBABr) of 1612mg (5mmol) is, the CuCl of 26mg (0.2mmol)
2, be dissolved in the DMSO of 20mL, and carried out magnetic agitation until solution all dissolves;
Step 2: choose two block sizes and be the FTO glass of 5.5cm * 5cm as electrode, utilize successively deionized water and ethanol to soak it, and utilize supersonic cleaning machine to clean 5 times.After cleaning, at 80 ℃, dry, standby;
Step 3: getting a block size is 5cm * 5cm, the polyfluortetraethylene plate that thickness is 5mm digs the through hole of one 4.5cm * 4.5cm therebetween, then utilizes respectively deionized water, absolute ethyl alcohol to rinse polyfluortetraethylene plate 4 times, then at 60 ℃, dries, standby;
Step 4: the TiO that takes 1g
2nano particle, grain size is 150nm, is dissolved in the absolute ethyl alcohol (purity>=99.7%) of 20mL, sonic oscillation 30min, until TiO
2be dispersed in solution, get any FTO glass in step 2, cover the seamless adhesive tape of one deck on the minor face of its conductive layer, width is 5mm, by the TiO configuring
2nanoparticulate dispersion is in 400 revs/min of low speed, 5s, and 1200 revs/min at a high speed, 10s, is spun on this FTO glass conductive layer, and the seamless adhesive tape of tearing after spin coating finishes utilizes tubular annealing stove sintering 30 minutes at 500 ℃ by the good FTO glass of spin coating;
Step 5: polyfluortetraethylene plate is binded to the not spin coating of preparing in step 2 TiO
2on the conductive layer of the FTO glass of nanoparticulate dispersion, and to the product of one preparation of implantation step in its through hole, then FTO glass spin coating prepared by step 4 has TiO
2the one side of nano particle is binded towards through hole, and wherein polyfluortetraethylene plate is covered completely by electrically conducting transparent substrate, and between two blocks of FTO glass, the long side direction 5mm broadside that staggers overlaps, and encapsulates with epoxy resin.
The device that the present embodiment prepares, has obvious electrochromic effect, can be at three kinds of states---between transparent, minute surface, black, change.Wherein only need 3s painted switching time, the long 3min left and right that needs of fading time, whole process is all reversible, between three states, can arbitrarily change.
Embodiment 3
Step 1: the AgNO that takes 255mg (2mmol)
3, the tetrabutyl ammonium bromide (TBABr) of 3224mg (10mmol) is, the CuCl of 52mg (0.4mmol)
2, be dissolved in the DMSO of 40mL, and carried out magnetic agitation until solute all dissolves.
Step 2: choose two block sizes and be the FTO glass of 10.5cm * 10cm as electrode, utilize successively deionized water and ethanol to soak it, and utilize supersonic cleaning machine to clean 5 times, after cleaning, at 80 ℃, dry, standby;
Step 3: getting a block size is 10cm * 10cm, the polyfluortetraethylene plate that thickness is 5mm digs the through hole of one 9.5cm * 9.5cm therebetween, then utilizes respectively deionized water, absolute ethyl alcohol to rinse 4 then oven dry at 60 ℃ of polyfluortetraethylene plate, standby;
Step 4: the TiO that takes 1g
2nano particle, grain size is 50nm, is dissolved in the absolute ethyl alcohol (purity>=99.7%) of 20mL, sonic oscillation 30min, until TiO
2be dispersed in solution, get any FTO glass in step 2, cover the seamless adhesive tape of one deck on the minor face of its conductive layer, width is 5mm, by the TiO configuring
2nanoparticulate dispersion is in 200 revs/min of low speed, 5s, and 1000 revs/min at a high speed, 10s, is spun on the conductive layer of this FTO glass, and the seamless adhesive tape of tearing after spin coating finishes utilizes tubular annealing stove sintering 30 minutes at 500 ℃ by the good FTO glass of spin coating;
Step 5: polyfluortetraethylene plate is binded to the not spin coating of preparing in step 2 TiO
2on the FTO glass conductive layer of nanoparticulate dispersion, and inject described step 1 product in through hole, then FTO glass spin coating prepared by step 4 there is TiO
2the one side of nanoparticulate dispersion is binded towards through hole, and wherein polyfluortetraethylene plate is covered completely by electrically conducting transparent substrate, and between two blocks of FTO glass, the long side direction 5mm broadside that staggers overlaps, and encapsulates with epoxy resin.
The device that the present embodiment prepares, has significant electrochromic effect, can be at three kinds of states---between transparent, minute surface, black, change.Wherein only need 5～6s painted switching time, fading time is longer, needs 4min left and right, and whole process is all reversible, between three states, can arbitrarily change.
Embodiment 4
Step 1: the AgNO that takes 85mg (0.5mmol)
3, the tetrabutyl ammonium bromide (TBABr) of 806mg (2.5mmol) is, the CuCl of 13mg (0.1mmol)
2, be dissolved in the DMSO of 10mL, and carried out magnetic agitation until solute all dissolves;
Step 2: choose two block sizes and be the FTO glass of 3cm * 2.5cm as electrode, utilize successively deionized water and ethanol to soak it, and utilize supersonic cleaning machine to clean 5 times, after cleaning, 80, dry under washing, standby;
Step 3: getting a block size is 2.5cm * 2.5cm, the polyfluortetraethylene plate that thickness is 5mm digs the through hole of one 2cm * 2cm therebetween, then utilizes respectively deionized water, absolute ethyl alcohol to rinse polyfluortetraethylene plate 4 times, then at 60 ℃, dries, standby;
Step 4: take the ZnO nano particle of 0.5g, grain size is 50nm, is dissolved in the absolute ethyl alcohol (purity >=99.7%) of 10mL, and sonic oscillation 40min, until ZnO nano uniform particles is dispersed in solution.Get any FTO glass in step 2, on the minor face of its conductive layer, cover the seamless adhesive tape of one deck, width is 5mm, by the ZnO nano particle dispersion configuring in 500 revs/min of low speed, 5s, 1500 revs/min at a high speed, 15s, be spun on the conductive layer of this FTO glass, the seamless adhesive tape of tearing after spin coating finishes, utilizes tubular annealing stove sintering 60 minutes at 450 ℃ by the good FTO glass of spin coating;
Step 5: polyfluortetraethylene plate is binded to the not spin coating of preparing in step 2 to be had on the FTO glass conductive layer of ZnO nano particle dispersion, and to the product of one preparation of implantation step in its through hole, the FTO glass spin coating of again being prepared by step 4 has the one side of ZnO nano particle to bind towards through hole, wherein polyfluortetraethylene plate is covered completely by FTO glass, the long side direction 5mm that staggers between two blocks of FTO glass, broadside overlaps, and encapsulates with epoxy resin.
The device that the present embodiment prepares, has fine electrochromic effect, can realize three kinds of obvious states---transparent, minute surface, black.Wherein only need 1～2s painted switching time, the long 1～2min that needs of fading time, whole process is all reversible, between three states, can arbitrarily change.
Embodiment 5
Step 1: the AgNO that takes 85mg (0.5mmol)
3, the tetrabutyl ammonium bromide (TBABr) of 806mg (2.5mmol) is, the CuCl of 13mg (0.1mmol)
2, be dissolved in the DMSO of 10mL, and carried out magnetic agitation until solute all dissolves;
Step 2: choose two block sizes and be the AZO glass of 3cm * 2.5cm as electrode, utilize successively deionized water and ethanol to soak it, and utilize supersonic cleaning machine to clean 5 times, after cleaning, 80, dry under washing, standby;
Step 3: getting a block size is 2.5cm * 2.5cm, the polyfluortetraethylene plate that thickness is 5mm digs the through hole of one 2cm * 2cm therebetween, then utilizes respectively deionized water, absolute ethyl alcohol to rinse polyfluortetraethylene plate 4 times, then at 60 ℃, dries, standby;
Step 4: the TiO that takes 0.5g
2nano particle, grain size is 20nm, is dissolved in the absolute ethyl alcohol (purity>=99.7%) of 10mL, sonic oscillation 30min, until TiO
2be dispersed in solution.Get any AZO glass in step 2, cover the seamless adhesive tape of one deck on the minor face of its conductive layer, width is 5mm, by the TiO configuring
2nanoparticulate dispersion is in 500 revs/min of low speed, 5s, and 1500 revs/min at a high speed, 15s, is spun on the conductive layer of this AZO glass, and the seamless adhesive tape of tearing after spin coating finishes utilizes tubular annealing stove sintering 30 minutes at 400 ℃ by the good AZO glass of spin coating;
Step 5: polyfluortetraethylene plate is binded to the not spin coating of preparing in step 2 TiO
2on the conductive layer of the AZO glass of nanoparticulate dispersion, and to the product of one preparation of implantation step in its through hole, then AZO glass spin coating prepared by step 4 has TiO
2the one side of nano particle is binded towards through hole, and wherein polyfluortetraethylene plate is covered completely by AZO glass, the long side direction 5mm that staggers between two blocks of AZO glass, and broadside overlaps, and encapsulates with epoxy resin.
The device that the present embodiment prepares, has fine electrochromic effect, can realize three kinds of obvious states---transparent, minute surface, black (seeing Fig. 2).Wherein only need 2～3s painted switching time, the long 1～2min that needs of fading time, whole process is all reversible, between three states, can arbitrarily change.
Claims (9)
1. a preparation method for polymorphic electrochromic device, is characterized in that, comprises the steps:
Step 1: the AgNO that takes 0.1～2.5mmol
3, the Quaternary ammonium bromide of 0.5～12.5mmol, 0.1～0.5mmol mantoquita, be dissolved in the polar organic solvent of 10～50mL, and carried out magnetic agitation until solute all dissolves;
Step 2: 2 of the electrically conducting transparent substrates of selection 2.0cm * 1.5cm～25.5 * 25cm, utilize successively 2 electrically conducting transparent substrates described in deionized water and alcohol immersion, and in supersonic cleaning machine, clean 3～7 times, after washes clean, under the condition of 60～100 ℃, dry, standby;
Step 3: cutting width is consistent with the width of electrically conducting transparent substrate, short 3～the 7mm of length of Length Ratio electrically conducting transparent substrate, thickness is the polyfluortetraethylene plate of 0.3～0.7mm, in the middle of the polyfluortetraethylene plate cutting down, dig a square through hole, between through hole and corresponding teflon panel edges, width is 3～7mm, utilize respectively deionized water and absolute ethyl alcohol to rinse this polyfluortetraethylene plate 3～5 times, after cleaning, at 50～70 ℃, dry;
Step 4: compound concentration is the base metal oxide nanoparticulate dispersion that 0.01～0.1g/mL, grain size are 5～500nm, by it in 200～2000 revs/min of rotating speeds, time 3～20s is spun on any electrically conducting transparent substrate conductive layer in step 2, before spin coating, by needing to cover one deck width on the minor face of the transparent substrates conductive layer of spin coating, be wherein the seamless adhesive tape that 3～5mm, length are identical with minor face, the seamless adhesive tape that needs to tear after spin coating finishes, then at 200～700 ℃ of sintering 20～60 minutes in tubular annealing stove;
Step 5: polyfluortetraethylene plate prepared by step 3 binds on the conductive layer of the electrically conducting transparent substrate that the not spin coating of preparing in described step 2 has base metal oxide nanoparticulate dispersion, in its through hole, pour described step 1 product into, the conductor planes of being prepared by described step 4 to transparent substrates is again binded to through hole, wherein two substrate long side directions, 3～7mm polyfluortetraethylene plate that staggers is covered completely by electrically conducting transparent substrate, finally with epoxy resin, encapsulates again.
2. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, is characterized in that: the Quaternary ammonium bromide in described step 1 is any one in cetab, tetrabutyl ammonium bromide, tetramethylammonium bromide, teabrom, ammonium bromide, DTAB.
3. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, is characterized in that: the mantoquita in described step 1 is any one in copper nitrate, cupric chloride, copper sulphate.
4. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, is characterized in that: the polar organic solvent in described step 1 is any one in formamide, dimethyl sulfoxide (DMSO) (DMSO), dimethyl formamide (DMF), dimethyl acetamide (DMAC), hexamethyl phosphoramide.
5. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, is characterized in that: the electrically conducting transparent substrate in described step 2 is for scribbling In
2o
3: Sn (ITO), In
2o
3: Zn (IZO), In
2o
3: Nb, ZnO:Al (AZO), ZnO:Ga (GZO), ZnO:In (IZO), ZnO:Si (SZO), ZnO:B (BZO), ZnO:F (FZO), ZnO:Nb, ZnO:Sc, SnO
2: F (FTO), SnO
2: Sb (ATO), SnO
2: Ta or SnO
2: glass or the flexible substrate of W codope oxide.
6. a kind of preparation method of polymorphic electrochromic device as claimed in claim 5, is characterized in that: described in scribble codope oxide flexible substrate be polyethylene terephthalate (PET), polycarbonate (PC), polyethersulfone (PES), polyvinylidene fluoride (PVDF), polyvinyl fluoride composite membrane (TPT), Polyethylene Naphthalate (PEN).
7. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, it is characterized in that: in described step 4, preparing the spreading agent that base metal nanoparticulate dispersion used is hydrophilic solvent or lipophilicity solvent, wherein hydrophilic solvent is water, ethanol, ethylene glycol, and lipophilicity solvent is dimethylbenzene, diethylene glycol dibenzoate.
8. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, is characterized in that: in described step 4, base metal oxide is any one in titanium, zinc, aluminium, tin, tungsten, molybdenum, tantalum, magnesium, zirconium, germanium oxide.
9. a kind of preparation method of polymorphic electrochromic device as claimed in claim 1, it is characterized in that: in described step 4, the spin coating mode of base metal oxide nanoparticulate dispersion is: under 200～600 revs/min of the first slow-speed of revolution, rotate 3～8s, then rotate 10～20s under 1000～2000 revs/min of high rotating speeds.
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| SHINGO ARAKI: "Electrochemical Optical-Modulation Device with Reversible Transformation Between Transparent, Mirror, and Black", 《ADVANCED MATERIALS》 * |
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