CN105239891A - Transparency-adjustable glass door and manufacturing method thereof - Google Patents
Transparency-adjustable glass door and manufacturing method thereof Download PDFInfo
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- CN105239891A CN105239891A CN201510628909.6A CN201510628909A CN105239891A CN 105239891 A CN105239891 A CN 105239891A CN 201510628909 A CN201510628909 A CN 201510628909A CN 105239891 A CN105239891 A CN 105239891A
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- 239000011521 glass Substances 0.000 title claims abstract description 106
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 106
- 239000010408 film Substances 0.000 claims description 67
- 239000011787 zinc oxide Substances 0.000 claims description 49
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 239000002070 nanowire Substances 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 31
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 24
- 239000010409 thin film Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 239000003792 electrolyte Substances 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000005341 toughened glass Substances 0.000 claims description 18
- 239000010931 gold Substances 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 16
- 239000003292 glue Substances 0.000 claims description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 16
- 229910052737 gold Inorganic materials 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 238000004528 spin coating Methods 0.000 claims description 16
- 238000005507 spraying Methods 0.000 claims description 16
- 238000004544 sputter deposition Methods 0.000 claims description 16
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 16
- 229910001887 tin oxide Inorganic materials 0.000 claims description 16
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000002073 nanorod Substances 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 10
- 239000000975 dye Substances 0.000 claims description 9
- 239000002105 nanoparticle Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 8
- 206010070834 Sensitisation Diseases 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 239000011324 bead Substances 0.000 claims description 8
- 210000005252 bulbus oculi Anatomy 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 8
- 230000008313 sensitization Effects 0.000 claims description 8
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 8
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 239000003115 supporting electrolyte Substances 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 238000009827 uniform distribution Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- BEAZKUGSCHFXIQ-UHFFFAOYSA-L zinc;diacetate;dihydrate Chemical compound O.O.[Zn+2].CC([O-])=O.CC([O-])=O BEAZKUGSCHFXIQ-UHFFFAOYSA-L 0.000 claims description 8
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims description 6
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 claims description 6
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000002120 nanofilm Substances 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000004044 response Effects 0.000 abstract description 2
- 230000007914 freezing tolerance Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000005622 photoelectricity Effects 0.000 abstract 1
- BSIUFWMDOOFBSP-UHFFFAOYSA-N 2-azanylethanol Chemical compound NCCO.NCCO BSIUFWMDOOFBSP-UHFFFAOYSA-N 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005337 ground glass Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 239000003086 colorant Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000013555 soy sauce Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
Abstract
The invention discloses a transparency-adjustable glass door and a manufacturing method thereof. The transparency-adjustable glass door and the manufacturing method thereof have the advantages that a structure and a manufacturing technology of an electrochromic device are improved, so that the electrochromic device can be self-powered; according to an electrochromism principle, the transparency-adjustable glass door has the advantages of adjustability in transparency, short color change response time, quite high photoelectricity energy conversion efficiency, longer service life and good freezing tolerance; the manufacturing method is easy to operate and easy for industrial production.
Description
Technical field
The invention belongs to mechanical field, more specifically relating to can the glass door regulating transparency and preparation method thereof.
Background technology
Glass door is a kind of more special door leaf, and application is more extensive at present.The glass making glass door generally divides tempered glass and common float glass.The characteristic of glass door is determined by glass itself, and such as tempering clear glass has penetrating feature, and ground glass has semipermeable feature.
But no matter be tempered glass or ground glass etc., all there is the problem that arbitrarily can not regulate transparency.
Summary of the invention
The present invention is directed to background technology Problems existing, thering is provided can the glass door regulating transparency and preparation method thereof, and it all improves the structure of electrochromic device and manufacture craft, makes it have self-energizing feature, utilize electrochromism principle in addition, make its transparency adjustable, and it is short to have the variable color response time, photovoltaic energy conversion ultrahigh in efficiency, life, the feature that freexing tolerance energy is good, and method of the present invention is simple to operation, is easy to industrialization and produces.
Object of the present invention is achieved through the following technical solutions:
Can regulate a preparation method for the glass door of transparency, wherein electrochromic device panel utilizes mechanical means to be fixed on glass door body surfaces, specifically comprises: assembling glass door main body, electrochromic device panel and electric mode transfer block:
One, the making step of electric mode transfer block is as follows:
(1) rearrangeable switch is made, for connecting electrochromic device and control circuit;
(2) make control circuit, for applying the electric current of electrochromic device according to extraneous light intensity regulating, tune up electric current when ambient light grow, turn electric current down when ambient light dies down;
Two, the electrochromic device making step of glass door is as follows:
(1) WO
3prepared by nano film material electrochromic electrode:
A. to tempered glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 320-360nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 200-220nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 400-420 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, passes into Ar and protects gas, be heated to 400-420 DEG C, and insulation 4-4.5 hour, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film, namely obtains electrochromic electrode;
Wherein nanorod length is 0.5-0.6 μm, density of nanorods about 10
6/ cm
2.
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 500-525nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then clean 10 minutes with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate, dry up in N2 atmosphere after taking-up;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 1-2nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and monoethanolamine (Monoethanolamine) is adopted with EGME (2-methoxyethanol) for solvent, be configured to the colloidal sol of 50mM equimolar ratio, then at the aqueous trehalose solution of the 10g/L of slow instillation 0.02-0.03 times of volume, and the formation Homogeneous phase mixing state that stirs, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 385 DEG C annealing half an hour, form the ZnO nanoparticle Seed Layer of Large-Area-Uniform distribution, the thickness of described Seed Layer is 22-28nm,
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode be improved with absolute ethyl alcohol;
(3) electrolyte preparation:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
Can regulate a preparation method for the glass door of transparency, wherein electrochromic device panel utilizes mechanical means to be fixed on glass door body surfaces, specifically comprises: assembling glass door main body, electrochromic device panel and electric mode transfer block:
One, the making step of electric mode transfer block is as follows:
(1) rearrangeable switch is made, for connecting electrochromic device and control circuit;
(2) make control circuit, for applying the electric current of electrochromic device according to extraneous light intensity regulating, tune up electric current when ambient light grow, turn electric current down when ambient light dies down;
Two, the electrochromic device making step of glass door is as follows:
(1) WO
3prepared by nano film material electrochromic electrode:
A. to tempered glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 360nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 200nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 420 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, and pass into Ar and protect gas, be heated to 400 DEG C, be incubated 4.5 hours, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film, namely obtains electrochromic electrode;
Wherein nanorod length is 0.5 μm, density of nanorods about 10
6/ cm
2.
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 525nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then clean 10 minutes with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate, dry up in N2 atmosphere after taking-up;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 1nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate and monoethanolamine is adopted to take EGME as solvent, be configured to the colloidal sol of 50mM equimolar ratio, then at the aqueous trehalose solution of the 10g/L of slow instillation 0.03 times of volume, and the formation Homogeneous phase mixing state that stirs, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 385 DEG C annealing half an hour, form the ZnO nanoparticle Seed Layer of Large-Area-Uniform distribution, the thickness of described Seed Layer is 22nm;
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode be improved with absolute ethyl alcohol;
(3) electrolyte preparation:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
Adopt the glass door that above-mentioned preparation method prepares.
Select inorganic WO
3the benefit of nano-stick array thin film:
1) there is unstable chemcial property, bond the shortcomings such as defective tightness, anti-ultraviolet radiation be indifferent with substrate in organic electrochromic material;
2) inorganic electrochromic material (tungstic acid, vanadic anhydride, nickel oxide etc.) research comparatively early, and technology comparative maturity, has been shown in there is report for commercial applications.
Adopt Au to make catalyzer, length has in the Seed Layer of ZnO nanoparticle and carries out Hydrothermal Growth ZnO nano-wire at low temperatures.This kind of method growth ZnO nano process conditions are simple, efficiency is high, can large area deposition and catalyzer can regulate and control parameters such as the length of nano wire and diameters.
Select the benefit of ZnO nano-wire:
ZnO is broad stopband N-type semiconductor material, is widely used in dye-sensitized solar cells;
ZnO carrier mobility is higher, is expected to the current characteristics improving battery further;
ZnO can be prepared into multiple nanostructured by simple process, such as nano wire, nanotube, nanoparticulate thin films etc.;
ZnO nano-wire has higher specific area, can adsorb more dyestuff.
And the present invention is further by optimized production process, produce the WO that performance is more excellent
3nano thin-film and ZnO nano-wire, and the optimization coordinating other structures, prepare overall photovoltaic energy conversion ultrahigh in efficiency, the novel electrochromic device of life.
Usefulness of the present invention is: method of the present invention is simple to operation, and be easy to industrialization and produce, novel electrochromic device photoelectric energy conversion efficiency obtained is in addition high, and life.
Accompanying drawing explanation
Accompanying drawing to be herein merged in manual and to form the part of this manual, shows embodiment according to the invention, and is used from manual one and explains principle of the present invention.
Fig. 1 is the structural representation of the glass door of the application.
Detailed description of the invention
For enabling above-mentioned purpose, the feature and advantage of the application more become apparent, below in conjunction with the drawings and specific embodiments, the application is described in further detail.
Electrochromism (Electrochronism/EC) refers under the effect of electric current or electric field, there is the phenomenon of stable reversible change in the optical properties (transmissivity, reflectivity or absorptivity) of material, just show as the reversible change of color and transparency so in appearance, then can regulate sunshine through number.The material with electrochromic property is called electrochromic material.Since the electrochromism phenomenon of Deb.S.K. Late Cambrian WO3 film in 1969, people have just found the material much with electrochromic property.Electrochromic material roughly can be divided into inorganic electrochromic material and organic electrochromic material by material type.The stable performance of inorganic electrochromic material, its light absorption change is because the Dual Implantations of ion and electronics and black soy sauce go out to cause.The light absorption change of organic electrochromic material is from redox reaction, and its rich color, easily carries out MOLECULE DESIGN, thus favored.
Electrochromic device is mainly divided into three parts: working electrode, to electrode, and electrolyte.Working electrode is generally the electro-conductive glass being coated with electrochomeric films and forms, the electro-conductive glass that electrode is then covered by the film (majority plays the effect of storage of ions) of cooperating electrode work is formed, in electrolyte, has the electrolyte of support performance electrode work.Whole device is similar to sandwich structure, working electrode and asking in being clipped in by electrolyte electrode, surrounding sealant sealing.When adding different driving voltage between two electrodes, the transmitance of device can change, and is generally change between clear state and coloured state.That is:, when adding a certain particular job voltage, device can be in pellucidity; When adding another particular job voltage, device can become colored state.By changing two interelectrode voltages, realize the change of device transmitance.
Why electrochromic material can show different colors under different driving voltages, is because redox state residing for it is different under different voltage, and then shows different band gaps, cause the change of color.
Embodiment 1:
Assembling glass door main body 10, electrochromic device 20 and electric mode transfer block 30.
Make electrochromic device 20 to comprise:
(1) WO
3prepared by nano thin-film 5 materials Electrochromic electrode:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 320nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 220nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 400 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, and pass into Ar and protect gas, be heated to 420 DEG C, be incubated 4 hours, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film 5, namely obtains electrochromic electrode;
Wherein nanorod length is 0.6 μm, density of nanorods about 10
6/ cm
2.
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 500nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then 10 minutes are cleaned, at N after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate
2dry up in atmosphere;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 2nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and monoethanolamine (Monoethanolamine) is adopted with EGME (2-methoxyethanol) for solvent, be configured to the colloidal sol of 50mM equimolar ratio, and then the aqueous trehalose solution of the 10g/L of slow instillation 0.02 times of volume, and the formation Homogeneous phase mixing state that stirs, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 385 DEG C annealing half an hour, form the ZnO nanoparticle Seed Layer of Large-Area-Uniform distribution, the thickness of described Seed Layer is 28nm,
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed with absolute ethyl alcohol, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode 3 be improved;
(3) prepared by electrolyte 4:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte 4 of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
At room temperature, use 1000W simulated solar radiant xenon lamp (Oriel91192, USA), Keithly2400sourcemeter, irradiation intensity is 100W/cm
2, battery is 0.25cm by illuminating area
2measuring photovoltaic energy conversion efficiency under condition is 10.28%, and circulating, to measure photovoltaic energy conversion efficiency afterwards 5000 times be 9.56%.-20 DEG C deposit 3 months after, recover normal temperature, measure photovoltaic energy conversion efficiency and have no significant change.
Embodiment 2:
Assembling glass door main body 10, electrochromic device 20 and electric mode transfer block 30.
Make electrochromic device 20 to comprise:
(1) WO
3prepared by nano thin-film 5 materials Electrochromic electrode:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 360nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 200nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 420 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, and pass into Ar and protect gas, be heated to 400 DEG C, be incubated 4.5 hours, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film 5, namely obtains electrochromic electrode;
Wherein nanorod length is 0.5 μm, density of nanorods about 10
6/ cm
2.
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 525nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then 10 minutes are cleaned, at N after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate
2dry up in atmosphere;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 1nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and monoethanolamine (Monoethanolamine) is adopted with EGME (2-methoxyethanol) for solvent, be configured to the colloidal sol of 50mM equimolar ratio, and then the aqueous trehalose solution of the 10g/L of slow instillation 0.03 times of volume, and the formation Homogeneous phase mixing state that stirs, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 385 DEG C annealing half an hour, form the ZnO nanoparticle Seed Layer of Large-Area-Uniform distribution, the thickness of described Seed Layer is 22nm,
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed with absolute ethyl alcohol, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode 3 be improved;
(3) prepared by electrolyte 4:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte 4 of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
At room temperature, use 1000W simulated solar radiant xenon lamp (Oriel91192, USA), Keithly2400sourcemeter, irradiation intensity is 100W/cm
2, battery is 0.25cm by illuminating area
2measuring photovoltaic energy conversion efficiency under condition is 10.50%, and circulating, to measure photovoltaic energy conversion efficiency afterwards 5000 times be 10.20%.-20 DEG C deposit 3 months after, recover normal temperature, measure photovoltaic energy conversion efficiency and have no significant change.
Embodiment 3:
Assembling glass door main body 10, electrochromic device 20 and electric mode transfer block 30.
Make electrochromic device 20 to comprise:
(1) WO
3prepared by nano thin-film 5 materials Electrochromic electrode:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 340nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 210nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 415 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, and pass into Ar and protect gas, be heated to 410 DEG C, be incubated 4.3 hours, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film 5, namely obtains electrochromic electrode;
Wherein nanorod length is 0.6 μm, density of nanorods about 10
6/ cm
2.
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 515nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then clean 10 minutes with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate, dry up in N2 atmosphere after taking-up;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 2nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and monoethanolamine (Monoethanolamine) is adopted with EGME (2-methoxyethanol) for solvent, be configured to the colloidal sol of 50mM equimolar ratio, and then the aqueous trehalose solution of the 10g/L of slow instillation 0.02 times of volume, and the formation Homogeneous phase mixing state that stirs, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 385 DEG C annealing half an hour, form the ZnO nanoparticle Seed Layer of Large-Area-Uniform distribution, the thickness of described Seed Layer is 27nm,
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed with absolute ethyl alcohol, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode 3 be improved;
(3) prepared by electrolyte 4:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte 4 of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
At room temperature, use 1000W simulated solar radiant xenon lamp (Oriel91192, USA), Keithly2400sourcemeter, irradiation intensity is 100W/cm
2, battery is 0.25cm by illuminating area
2measuring photovoltaic energy conversion efficiency under condition is 9.50%, and circulating, to measure photovoltaic energy conversion efficiency afterwards 5000 times be 9.34%.-20 DEG C deposit 3 months after, recover normal temperature, measure photovoltaic energy conversion efficiency and have no significant change.
Embodiment 4 comparative example:
Assembling glass door main body 10, electrochromic device 20 and electric mode transfer block 30.
Make electrochromic device 20 to comprise:
(1) WO
3prepared by nano thin-film 5 materials Electrochromic electrode:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 500nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 500nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 500 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, and pass into Ar and protect gas, be heated to 500 DEG C, be incubated 4.1 hours, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film 5, namely obtains electrochromic electrode;
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 520nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then clean 10 minutes with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate, dry up in N2 atmosphere after taking-up;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 1nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and monoethanolamine (Monoethanolamine) is adopted with EGME (2-methoxyethanol) for solvent, be configured to the colloidal sol of 50mM equimolar ratio, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 500 DEG C annealing half an hour, formed Large-Area-Uniform distribution ZnO nanoparticle Seed Layer;
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed with absolute ethyl alcohol, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode 3 be improved;
(3) prepared by electrolyte 4:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte 4 of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
At room temperature, use 1000W simulated solar radiant xenon lamp (Oriel91192, USA), Keithly2400sourcemeter, irradiation intensity is 100W/cm
2, battery is 0.25cm by illuminating area
2measuring photovoltaic energy conversion efficiency under condition is 5.98%, and circulating, to measure photovoltaic energy conversion efficiency afterwards 5000 times be 3.98%.-20 DEG C deposit 3 months after, recover normal temperature, measure photovoltaic energy conversion efficiency and reduce 9.7%.
Embodiment 5 comparative example:
Assembling glass door main body 10, electrochromic device 20 and electric mode transfer block 30.
Make electrochromic device 20 to comprise:
(1) WO
3prepared by nano thin-film 5 materials Electrochromic electrode:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 600nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 400nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.3mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 500 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, and pass into Ar and protect gas, be heated to 600 DEG C, be incubated 5 hours, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film 5, namely obtains electrochromic electrode;
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) film 2 of specific dimensions, thickness is about 600nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then clean 10 minutes with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate, dry up in N2 atmosphere after taking-up;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 5nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H is adopted
20) and monoethanolamine (Monoethanolamine) with EGME (2-methoxyethanol) for solvent, be configured to the colloidal sol of 50mM equimolar ratio, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 500 DEG C annealing half an hour, formed Large-Area-Uniform distribution ZnO nanoparticle Seed Layer;
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed with absolute ethyl alcohol, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode 3 be improved;
(3) prepared by electrolyte 4:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte 4 of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
At room temperature, use 1000W simulated solar radiant xenon lamp (Oriel91192, USA), Keithly2400sourcemeter, irradiation intensity is 100W/cm
2, battery is 0.25cm by illuminating area
2measuring photovoltaic energy conversion efficiency under condition is 6.12%, and circulating, to measure photovoltaic energy conversion efficiency afterwards 5000 times be 5.39%.-20 DEG C deposit 3 months after, recover normal temperature, measure photovoltaic energy conversion efficiency and reduce 10.1%.
As can be seen here, the novel electrochromic device photoelectric energy conversion efficiency that the present invention obtains is high, and life, and freexing tolerance can be also better.Each parameter of comparative example is starkly lower than technical scheme of the present invention, this illustrates that integrated artistic of the present invention serves certain synergy, each component of integral formula and proportioning are all most important, change any one key element and photovoltaic energy conversion efficiency all can be caused to reduce, the lost of life.
The above; be only the present invention's preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (2)
1. can regulate a preparation method for the glass door of transparency, wherein electrochromic device panel utilizes mechanical means to be fixed on glass door body surfaces, specifically comprises: assembling glass door main body, electrochromic device panel and electric mode transfer block:
One, the making step of electric mode transfer block is as follows:
(1) rearrangeable switch is made, for connecting electrochromic device and control circuit;
(2) make control circuit, for applying the electric current of electrochromic device according to extraneous light intensity regulating, tune up electric current when ambient light grow, turn electric current down when ambient light dies down;
Two, the electrochromic device making step of glass door is as follows:
(1) WO
3prepared by nano film material electrochromic electrode:
A. to tempered glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 320-360nm;
B. the high temperature anneal is carried out to it, obtains the FTO electro-conductive glass that intensity is higher, then according to the order of ultra-pure water, acetone, ethanol by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby; Then, utilize magnetron sputtering method to plate W film on FTO glass, its thickness is 200-220nm; W film is used as WO
3the growth source of nano wire;
C. the sodium tungstate aqueous solution of 0.2mol/L is prepared, then the hydrochloric acid of 3mol/L is dripped to no longer producing precipitation, gained precipitation is dissolved in hydrogen peroxide after centrifuge washing and obtains vitreosol, vitreosol is applied to the ITO conductive glass surface being coated with W film, at 400-420 DEG C, calcines 40min obtain WO
3crystal seed layer;
D. by obtained above with WO
3box-type high-temperature furnace put into by the FTO electro-conductive glass of crystal seed layer, passes into Ar and protects gas, be heated to 400-420 DEG C, and insulation 4-4.5 hour, rear Temperature fall, to room temperature, namely obtains cylindrical WO
3nano-stick array thin film, namely obtains electrochromic electrode;
Wherein nanorod length is 0.5-0.6 μm, density of nanorods about 10
6/ cm
2.
(2) the ZnO nano-wire film photoactive electrode preparation improved:
A. to tempered glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) film of specific dimensions, thickness is about 500-525nm, then the high temperature anneal is carried out to it, obtain the FTO electro-conductive glass that intensity is higher, then clean 10 minutes with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate, dry up in N2 atmosphere after taking-up;
B. FTO glass is put into gold spraying instrument, at FTO surface spraying plating one deck gold film as catalyzer, golden film thickness is about 1-2nm, again cleans the method for FTO glass according to a step afterwards;
C. Zinc diacetate dihydrate and monoethanolamine is adopted to take EGME as solvent, be configured to the colloidal sol of 50mM equimolar ratio, then at the aqueous trehalose solution of the 10g/L of slow instillation 0.02-0.03 times of volume, and the formation Homogeneous phase mixing state that stirs, be spun in clean FTO substrate, spin coating 3 times is to obtain continuous print nanoparticulate thin films, between each spin coating, substrate infrared lamps is promoted solvent volatilization, finally by substrate in an atmosphere 385 DEG C annealing half an hour, form the ZnO nanoparticle Seed Layer of Large-Area-Uniform distribution, the thickness of described Seed Layer is 22-28nm,
D. the ZnSO of 0.15M is prepared
4the aqueous solution, by concentrated ammonia solution adjust ph to 10, ito substrate is put into solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and by washed with de-ionized water, namely obtained zinc oxide nanowire after drying;
E. pure organic doline dyes D102 being dissolved into volume ratio is in the second eyeball of 1:1 and the solution of the tert-butyl alcohol, concentration is 0.5mM, ZnO nano-wire is immersed in D102, keep in Dark Place 5 hours, after taking-up, the ZnO nano-wire after D102 sensitization is rinsed, fully to remove the D102 molecule being adsorbed onto ZnO nano-wire surface by physical adsorption way, the photoactive electrode be improved with absolute ethyl alcohol;
(3) electrolyte preparation:
Be made into 0.1MLiI and 0.001MI
2pC solution, as the supporting electrolyte of self energizing electrochromic device.
(4) device assembling:
Electrochromic electrode is relative with effective work plane of photoactive electrode, two ends reserve the electrode of blank electro-conductive glass as reserved access external circuit of about 5mm width, surrounding diameter is that compacting smeared by two component aviation glue of the bead mixing of 100 μm, make the space leaving 100 μm between two electrodes, and in this space filling electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
2. the glass door for preparing of preparation method according to claim 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105761379A (en) * | 2016-02-01 | 2016-07-13 | 蔡雄 | ATM input device capable of achieving free and quick brightness regulation |
| CN106057081A (en) * | 2016-02-18 | 2016-10-26 | 吴桂广 | Outdoor advertising board based on electrochromic device and manufacturing method of advertising board |
| CN108604034A (en) * | 2016-02-15 | 2018-09-28 | 夏普株式会社 | Electrochromic device and intelligent window with electrochromic device |
| CN109414979A (en) * | 2016-06-22 | 2019-03-01 | 金泰克斯公司 | The thermal control of variable transmittance windows |
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|---|---|---|---|---|
| WO1993021557A1 (en) * | 1992-04-10 | 1993-10-28 | Sun Active Glass Electrochromics, Inc. | Electrochromic structures and methods |
| WO2012018688A1 (en) * | 2010-08-05 | 2012-02-09 | Soladigm, Inc. | Multi-pane electrochromic windows |
| CA2822399A1 (en) * | 2011-01-06 | 2012-07-12 | Saint-Gobain Glass France | Substrate provided with a stack having thermal properties, in particular for manufacturing heated glass |
| US20130258436A1 (en) * | 2012-04-03 | 2013-10-03 | Sage Electrochromics, Inc. | Patterned obscuration lines for electrochromic devices |
| CN104768892A (en) * | 2012-11-08 | 2015-07-08 | 法国圣戈班玻璃厂 | Glazing having switchable optical properties |
| CN104898344A (en) * | 2015-05-08 | 2015-09-09 | 上方能源技术(杭州)有限公司 | All-solid state electrochromic device preparation method and prepared electrochromic glass |
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2015
- 2015-09-28 CN CN201510628909.6A patent/CN105239891B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1993021557A1 (en) * | 1992-04-10 | 1993-10-28 | Sun Active Glass Electrochromics, Inc. | Electrochromic structures and methods |
| WO2012018688A1 (en) * | 2010-08-05 | 2012-02-09 | Soladigm, Inc. | Multi-pane electrochromic windows |
| CA2822399A1 (en) * | 2011-01-06 | 2012-07-12 | Saint-Gobain Glass France | Substrate provided with a stack having thermal properties, in particular for manufacturing heated glass |
| US20130258436A1 (en) * | 2012-04-03 | 2013-10-03 | Sage Electrochromics, Inc. | Patterned obscuration lines for electrochromic devices |
| CN104768892A (en) * | 2012-11-08 | 2015-07-08 | 法国圣戈班玻璃厂 | Glazing having switchable optical properties |
| CN104898344A (en) * | 2015-05-08 | 2015-09-09 | 上方能源技术(杭州)有限公司 | All-solid state electrochromic device preparation method and prepared electrochromic glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105761379A (en) * | 2016-02-01 | 2016-07-13 | 蔡雄 | ATM input device capable of achieving free and quick brightness regulation |
| CN108604034A (en) * | 2016-02-15 | 2018-09-28 | 夏普株式会社 | Electrochromic device and intelligent window with electrochromic device |
| CN106057081A (en) * | 2016-02-18 | 2016-10-26 | 吴桂广 | Outdoor advertising board based on electrochromic device and manufacturing method of advertising board |
| CN109414979A (en) * | 2016-06-22 | 2019-03-01 | 金泰克斯公司 | The thermal control of variable transmittance windows |
| CN109414979B (en) * | 2016-06-22 | 2022-04-26 | 金泰克斯公司 | Thermal control of variable transmittance windows |
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| CN105239891B (en) | 2016-12-14 |
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