CN105204263A - High-sun-blocking automobile window based on electrochromism device and manufacturing method thereof - Google Patents

High-sun-blocking automobile window based on electrochromism device and manufacturing method thereof Download PDF

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Publication number
CN105204263A
CN105204263A CN201510628135.7A CN201510628135A CN105204263A CN 105204263 A CN105204263 A CN 105204263A CN 201510628135 A CN201510628135 A CN 201510628135A CN 105204263 A CN105204263 A CN 105204263A
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fto
film
electrode
glass
electrochromic device
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杨林
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
    • B60J1/00—Windows; Windscreens; Accessories therefor
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect
    • G02F1/153—Constructional details
    • G02F1/155—Electrodes

Abstract

The invention discloses a novel-electrochromism-device-based automobile window with the high sun blocking performance and a manufacturing method thereof. According to the automobile window and the manufacturing method, the structure and the manufacturing technology of the electrochromism device are both improved, the electrochromism device has the self energy supplying characteristic accordingly, and therefore the novel service-life-prolonged automobile window which is high in sun blocking performance, free of a film pasting procedure and good in freezing resistance is manufactured; in addition, the method is simple and easy to operate, and industrial production is facilitated.

Description

Sun-proof automotive window of height based on electrochromic device and preparation method thereof
Technical field
The invention belongs to automotive field, more specifically relate to the sun-proof automotive window of height and preparation method thereof based on electrochromic device.
Background technology
In routine techniques, automotive window generally pastes sunscreen film, general sunscreen film adopts PET (tygon) base material, higher sunscreen film uses multiple layer metal sputtering technology and vacuum technique and ion technology and thin film physics, fine chemical technology, makes it have high heat-insulating efficiency, high-tension, high elongation, by force anti acid alkali performance energy.
But sunscreen film is sticked to automotive window, exist cost higher, need to increase pad pasting program, difficulty be installed, the easy shortcoming such as aging.
Summary of the invention
The present invention is directed to background technology Problems existing, propose a kind ofly based on electrochromic device, there is automotive window of high sun-proof performance and preparation method thereof, it all improves the structure of electrochromic device and manufacture craft, make it have self-energizing feature, thus obtained there is high sun-proof performance, without the need to pad pasting program, life, the new automobile vehicle window 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:
A method for making for the sun-proof automotive window of height based on electrochromic device, this vehicle window increases one deck electrochromic device on traditional vehicle window basis, and electrochromic device is made up of electrochromism substrate and controller:
One, the making step of controller is as follows:
(1) rearrangeable switch is made, for connecting;
(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 substrate manufacture step of automotive window 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 ultrapure 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 ethylene glycol monomethyl ether (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 0.02-0.03 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 4aqueous 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) electrolytic solution 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 workplace 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 beaded glass 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.
A method for making for the sun-proof automotive window of height based on electrochromic device, this vehicle window increases one deck electrochromic device on traditional vehicle window basis, and electrochromic device is made up of electrochromism substrate and controller:
One, the making step of controller is as follows:
(1) rearrangeable switch is made, for connecting;
(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 substrate manufacture step of automotive window 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 ultrapure 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 ethylene glycol monomethyl ether as 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 4aqueous 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) electrolytic solution 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 workplace 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 beaded glass 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 automotive window that above-mentioned method for making prepares.
Select inorganic WO 3the benefit of nano-stick array thin film:
1) there is unstable chemcial property, bond the shortcomings such as undertighten, anti-ultraviolet radiation be indifferent with substrate in organic electrochromic material;
2) inorganic electrochromic material (tungstic acid, vanadium pentoxide, 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 surface 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: the automotive window that the present invention makes has higher sun-proof performance, reduces cost, without the need to pad pasting program, installation is simple and the life-span is longer.
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 instructions and to form the part of this instructions, shows embodiment according to the invention, and is used from instructions one and explains principle of the present invention.
Fig. 1 is the structural representation of the automotive window of the application.
Embodiment
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 Deb.S.K. Late Cambrian WO in 1969 3since the electrochromism phenomenon of film, 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 electrolytic solution.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 electrolytic solution, has the electrolyte of support performance electrode work.Whole device is similar to sandwich structure, working electrode and asking in being clipped in by electrolytic solution 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 vehicle window parts 10, electrochromic device 20 and controller 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 ultrapure 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 ethylene glycol monomethyl ether (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 4aqueous 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 electrolytic solution 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 workplace 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 beaded glass 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 vehicle window parts 10, electrochromic device 20 and controller 30.
Make electrochromic device 20:
(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 ultrapure 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 ethylene glycol monomethyl ether (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 4aqueous 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 electrolytic solution 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 workplace 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 beaded glass 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 vehicle window parts 10, electrochromic device 20 and controller 30.
Make electrochromic device 20:
(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 ultrapure 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 ethylene glycol monomethyl ether (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 4aqueous 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 electrolytic solution 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 workplace 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 beaded glass 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 vehicle window parts 10, electrochromic device 20 and controller 30.
Make electrochromic device 20:
(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 ultrapure 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 ethylene glycol monomethyl ether (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 4aqueous 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 electrolytic solution 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 workplace 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 beaded glass 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 vehicle window parts 10, electrochromic device 20 and controller 30.
Make electrochromic device 20:
(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 ultrapure 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 ethylene glycol monomethyl ether (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 4aqueous 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 electrolytic solution 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 workplace 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 beaded glass 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 automotive window with high sun-proof performance based on electrochromic device that the present invention obtains can realize self energizing variable color, photovoltaic energy conversion ultrahigh in efficiency, 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.
In addition, the automotive window that the present invention makes has higher sun-proof performance, reduces cost, without the need to pad pasting program, installation is simple and the life-span is longer.
The above; be only the present invention's preferably embodiment; 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., based on a method for making for the sun-proof automotive window of height of electrochromic device, this vehicle window increases one deck electrochromic device on traditional vehicle window basis, and electrochromic device is made up of electrochromism substrate and controller:
One, the making step of controller is as follows:
(1) rearrangeable switch is made, for connecting;
(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 substrate manufacture step of automotive window 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 ultrapure 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 ethylene glycol monomethyl ether as solvent, be configured to the colloidal sol of 50mM equimolar ratio, and then the aqueous trehalose solution of the 10g/L of slow instillation 0.02-0.03 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 4aqueous 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) electrolytic solution 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 workplace 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 beaded glass 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 automotive window for preparing of method for making according to claim 1.
CN201510628135.7A 2015-09-28 2015-09-28 High-sun-blocking automobile window based on electrochromism device and manufacturing method thereof Withdrawn CN105204263A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107561812A (en) * 2017-10-20 2018-01-09 上海博历机械科技有限公司 Outdoor billboard based on electrochromic device and preparation method thereof
CN108983523A (en) * 2018-07-25 2018-12-11 京东方科技集团股份有限公司 The protective device and guard method of a kind of cover sheet, head-up display
CN113212122A (en) * 2021-06-23 2021-08-06 东风云南汽车有限公司 Automobile front windshield dodging system
CN113791510A (en) * 2021-08-06 2021-12-14 河北光兴半导体技术有限公司 Preparation system for electrochromic glass

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107561812A (en) * 2017-10-20 2018-01-09 上海博历机械科技有限公司 Outdoor billboard based on electrochromic device and preparation method thereof
CN108983523A (en) * 2018-07-25 2018-12-11 京东方科技集团股份有限公司 The protective device and guard method of a kind of cover sheet, head-up display
CN113212122A (en) * 2021-06-23 2021-08-06 东风云南汽车有限公司 Automobile front windshield dodging system
CN113791510A (en) * 2021-08-06 2021-12-14 河北光兴半导体技术有限公司 Preparation system for electrochromic glass

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