CN105239891B - Can the glass door that regulate transparency and preparation method thereof - Google Patents
Can the glass door that regulate transparency and preparation method thereof Download PDFInfo
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- CN105239891B CN105239891B CN201510628909.6A CN201510628909A CN105239891B CN 105239891 B CN105239891 B CN 105239891B CN 201510628909 A CN201510628909 A CN 201510628909A CN 105239891 B CN105239891 B CN 105239891B
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Abstract
The invention discloses a kind of can the glass door that regulate transparency and preparation method thereof, structure and the processing technology of electrochromic device are all improved by it, make it have self-energizing feature, furthermore with electrochromism principle so that it is transparency is adjustable, and it is short to have variable color response time, photovoltaic energy conversion ultrahigh in efficiency, life, the feature that freexing tolerance can be good, and the method for the present invention is simple to operation, it is easy to industrialization produces.
Description
Technical field
The invention belongs to mechanical field, being more particularly to can the glass door that regulate transparency and preparation method thereof.
Background technology
Glass door is the door leaf that a kind of comparison is special, and application is wide at present.The glass making glass door is general
Divide safety glass and common float glass.The characteristic of glass door is determined by glass itself, and such as tempering is saturating
Bright glass has penetrating feature, and ground glass has semipermeable feature.
But no matter be safety glass or ground glass etc., all there is the problem that can not arbitrarily regulate transparency.
Summary of the invention
The present invention is directed to the problem that background technology exists, it is provided that glass door and the making side thereof of transparency can be regulated
Method, structure and the processing technology of electrochromic device are all improved by it so that it is have self-energizing spy
Point, furthermore with electrochromism principle so that it is transparency is adjustable, and it is short to have variable color response time, light
Electric energy conversion ultrahigh in efficiency, life, the feature that freexing tolerance can be good, and also the method for the present invention is simple
Easily operation, it is easy to industrialization produces.
The purpose of the present invention is achieved through the following technical solutions:
The manufacture method of a kind of glass door that can regulate transparency, wherein electrochromic device panel utilizes machinery
Method is fixed on glass door body surfaces, specifically includes: assemble glass door main body, electrochromic device panel
With electricity mode transfer block:
One, the making step of electricity mode transfer block is as follows:
(1) make rearrangeable switch, be used for connecting electrochromic device and control circuit；
(2) control circuit is made, for applying the electric current of electrochromic device according to extraneous light intensity regulating, when
Ambient light tunes up electric current when becoming strong, turns electric current down when ambient light dies down；
Two, the electrochromic device making step of glass door is as follows:
(1)WO3Prepared by nano film material electrochromic electrode:
A. safety glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness is about
For 320-360nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 200-220nm；W film is used as WO3Nanometer
The growth source of line；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 400-420 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 400-420 DEG C, be incubated 4-4.5 hour, after be naturally cooling to room temperature, i.e. obtain cylinder
Shape WO3Nano-stick array thin film, i.e. obtains electrochromic electrode；
Wherein nanorod length is 0.5-0.6 μm, density of nanorods about 106/cm2。
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness is about
For 500-525nm, then it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, so
Clean 10 minutes, at N2 gas after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate afterwards
Atmosphere dries up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 1-2nm, after FTO glass is cleaned again according to the method for a step；
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and ethanolamine (Monoethanolamine) are used
With ethylene glycol monomethyl ether (2-methoxyethanol) as solvent, it is configured to the colloidal sol of 50mM equimolar ratio,
Then at the aqueous trehalose solution of the 10g/L being slowly dropped into 0.02-0.03 times of volume, and the formation that stirs
Uniformly admixture, is spun in the FTO substrate cleaned, and spin coating 3 times is thin to obtain continuous print nanoparticle
Film, promotes solvent volatilization, in an atmosphere by substrate by substrate infrared lamps finally between each spin coating
Anneal half an hour for 385 DEG C, form large area equally distributed ZnO nanoparticle Seed Layer, described Seed Layer
Thickness be 22-28nm；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ITO base
Plate is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water, dries in the air
Zinc oxide nanowire is i.e. obtained after Gan；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode improved；
(3) prepared by electrolyte:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
The manufacture method of a kind of glass door that can regulate transparency, wherein electrochromic device panel utilizes machinery
Method is fixed on glass door body surfaces, specifically includes: assemble glass door main body, electrochromic device panel
With electricity mode transfer block:
One, the making step of electricity mode transfer block is as follows:
(1) make rearrangeable switch, be used for connecting electrochromic device and control circuit；
(2) control circuit is made, for applying the electric current of electrochromic device according to extraneous light intensity regulating, when
Ambient light tunes up electric current when becoming strong, turns electric current down when ambient light dies down；
Two, the electrochromic device making step of glass door is as follows:
(1)WO3Prepared by nano film material electrochromic electrode:
A. safety glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness is about
For 360nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 200nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 420 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 400 DEG C, be incubated 4.5 hours, after be naturally cooling to room temperature, i.e. obtain cylinder WO3
Nano-stick array thin film, i.e. obtains electrochromic electrode；
Wherein nanorod length is 0.5 μm, density of nanorods about 106/cm2。
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness is about
For 525nm, then it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then use
EtOH Sonicate cleans 10 minutes, after taking-up in N2 atmosphere with UV ozone cleaning machine after cleaning 20 minutes again
Dry up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 1nm, after FTO glass is cleaned again according to the method for a step；
C. use Zinc diacetate dihydrate and ethanolamine with ethylene glycol monomethyl ether as solvent, be configured to 50mM equimolar
The colloidal sol of ratio, then at the aqueous trehalose solution of the 10g/L being slowly dropped into 0.03 times of volume, and stirs
Forming uniform admixture, be spun in the FTO substrate cleaned, spin coating 3 times is to obtain continuous print nanoparticle
Sub-thin film, promotes solvent volatilization, finally by substrate at air by substrate infrared lamps between each spin coating
In 385 DEG C annealing half an hour, formed large area equally distributed ZnO nanoparticle Seed Layer, described seed
The thickness of layer is 22nm；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ITO base
Plate is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water, dries in the air
Zinc oxide nanowire is i.e. obtained after Gan；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode improved；
(3) prepared by electrolyte:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
Use the glass door that above-mentioned manufacture method prepares.
Select inorganic WO3The benefit of nano-stick array thin film:
1) there is unstable chemcial property and substrate bonding defective tightness, anti-purple in organic electrochromic material
The shortcomings such as external radiation is indifferent；
2) inorganic electrochromic material (Tungstic anhydride., vanadic anhydride, nickel oxide etc.) research is relatively early,
Technology comparative maturity, has the most been shown in and has had been reported that.
Use Au to make catalyst, long at low temperatures have in the Seed Layer of ZnO nanoparticle carry out Hydrothermal Growth
ZnO nano-wire.ZnO nano process conditions are simple, efficiency is high for the growth of this kind of method, can large area deposition,
And the parameters such as the length of nano wire and diameter can be regulated and controled by catalyst.
The benefit of selection 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 improve further the current characteristics of battery；
ZnO can be prepared as multiple nanostructured, such as nano wire, nanotube, nanoparticle by simple process
Sub-thin film etc.；
ZnO nano-wire has higher specific surface area, it is possible to adsorb more dyestuff.
And the present invention is further by optimized production process, produce the WO that performance is more excellent3Nano thin-film and
ZnO nano-wire, and coordinate the optimization of other structures, prepare overall photovoltaic energy conversion ultrahigh in efficiency, life-span
The novel electrochromic device extended.
The invention have benefit that: the method for the present invention is simple to operation, it is easy to industrialization produces, this
The outer novel electrochromic device photoelectric energy conversion efficiency prepared is high, and life.
Accompanying drawing explanation
Accompanying drawing herein is merged in description and constitutes the part of this specification, it is shown that meet the present invention
Embodiment, and for explaining the principle of the present invention together with description.
Fig. 1 is the structural representation of the glass door of the application.
Detailed description of the invention
Understandable for enabling the above-mentioned purpose of the application, feature and advantage to become apparent from, below in conjunction with the accompanying drawings and
The application is described in further detail by detailed description of the invention.
Electrochromism (Electrochronism/EC) refers under the effect of electric current or electric field, the light of material
Learn attribute (absorbance, reflectance or absorbance) and stable reversible change phenomenon occurs, then in outward appearance
On will appear as the reversible change of color and transparency, then can regulate the number that sunlight passes through.Have
The material of electrochromic property is referred to as electrochromic material.Since Deb.S.K. in 1969 finds WO3 first
Since the electrochromism phenomenon of thin film, people have found that the material much with electrochromic property.Electroluminescent
Off-color material substantially can be divided into inorganic electrochromic material and organic electrochromic material by material type.Nothing
The stable performance of machine electrochromic material, its light Change of absorption is due to ion and the Dual Implantations of electronics and black soy sauce
Go out to cause.The light Change of absorption of organic electrochromic material from redox reaction, its rich color,
Easily carry out MOLECULE DESIGN, thus favored.
Electrochromic device is broadly divided into three parts: working electrode, to electrode, electrolyte.Working electrode
The electro-conductive glass being generally coated with electrochomeric films is constituted, and is then to be worked by cooperating electrode to electrode
Thin film (majority play store ion effect) cover electro-conductive glass composition, electrolyte has support work
Make the electrolyte of electrode work.Whole device is similar to sandwich structure, working electrode and will electrolysis to electrode
Liquid is asked in being clipped in, surrounding sealant sealing.Time between two electrodes plus different driving voltage, device
Transmitance can change, and is usually and changes between clear state and coloured state.That is: plus a certain particular job
During voltage, device can be in pellucidity；When plus another particular job voltage, device can become coloring
State.By changing two interelectrode voltages, it is achieved the change of device transmitance.
Why electrochromic material can show different colors under different driving voltages, be due to
Under different voltages, redox state residing for it is different, and then shows different band gaps, causes the change of color
Change.
Embodiment 1:
Assemble glass door main body 10, electrochromic device 20 and electricity mode transfer block 30.
Make electrochromic device 20 to include:
(1)WO3Prepared by nano thin-film 5 materials Electrochromic electrode:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 320nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 220nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 400 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 420 DEG C, be incubated 4 hours, after be naturally cooling to room temperature, i.e. obtain cylinder WO3Receive
Rice rod array film 5, i.e. obtains electrochromic electrode；
Wherein nanorod length is 0.6 μm, density of nanorods about 106/cm2。
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 500nm, then it is carried out the high temperature anneal, obtains the FTO electro-conductive glass that intensity is higher, so
Clean 10 minutes, at N after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate afterwards2Gas
Atmosphere dries up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 2nm, after FTO glass is cleaned again according to the method for a step；
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and ethanolamine (Monoethanolamine) are used
With ethylene glycol monomethyl ether (2-methoxyethanol) as solvent, it is configured to the colloidal sol of 50mM equimolar ratio,
It is slowly dropped into the aqueous trehalose solution of the 10g/L of 0.02 times of volume the most again, and the formation that stirs is the most mixed
Conjunction state, is spun in the FTO substrate cleaned, and spin coating 3 times is to obtain continuous print nanoparticulate thin films, often
Between secondary spin coating by substrate infrared lamps promote solvent volatilization, finally by substrate in an atmosphere 385 DEG C move back
Fiery half an hour, forming large area equally distributed ZnO nanoparticle Seed Layer, the thickness of described Seed Layer is
28nm；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ito substrate
Putting in solution, put into the baking oven of 95 DEG C after sealing, 2 as a child took out, and cleaned with deionized water, dried
After i.e. obtain zinc oxide nanowire；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode 3 improved；
(3) prepared by electrolyte 4:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid 4.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
At room temperature, 1000W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly are used
2400 source meter, irradiation intensity is 100W/cm2, battery is 0.25cm by illuminating area2Under the conditions of
Measuring photovoltaic energy conversion efficiency is 10.28%, measures photovoltaic energy conversion efficiency and be after circulating 5000 times
9.56%.After-20 DEG C are deposited 3 months, recover room temperature, measure photovoltaic energy conversion efficiency and have no significant change.
Embodiment 2:
Assemble glass door main body 10, electrochromic device 20 and electricity mode transfer block 30.
Make electrochromic device 20 to include:
(1)WO3Prepared by nano thin-film 5 materials Electrochromic electrode:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 360nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 200nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 420 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 400 DEG C, be incubated 4.5 hours, after be naturally cooling to room temperature, i.e. obtain cylinder WO3
Nano-stick array thin film 5, i.e. obtains electrochromic electrode；
Wherein nanorod length is 0.5 μm, density of nanorods about 106/cm2。
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness
It is about 525nm, then it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then
Clean 10 minutes, at N after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate2Atmosphere
In dry up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 1nm, after FTO glass is cleaned again according to the method for a step；
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and ethanolamine (Monoethanolamine) are used
With ethylene glycol monomethyl ether (2-methoxyethanol) as solvent, it is configured to the colloidal sol of 50mM equimolar ratio,
It is slowly dropped into the aqueous trehalose solution of the 10g/L of 0.03 times of volume the most again, and the formation that stirs is the most mixed
Conjunction state, is spun in the FTO substrate cleaned, and spin coating 3 times is to obtain continuous print nanoparticulate thin films, often
Between secondary spin coating by substrate infrared lamps promote solvent volatilization, finally by substrate in an atmosphere 385 DEG C move back
Fiery half an hour, forming large area equally distributed ZnO nanoparticle Seed Layer, the thickness of described Seed Layer is
22nm；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ITO base
Plate is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water, dries in the air
Zinc oxide nanowire is i.e. obtained after Gan；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode 3 improved；
(3) prepared by electrolyte 4:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid 4.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
At room temperature, 1000W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly are used
2400 source meter, irradiation intensity is 100W/cm2, battery is 0.25cm by illuminating area2Under the conditions of
Measuring photovoltaic energy conversion efficiency is 10.50%, measures photovoltaic energy conversion efficiency and be after circulating 5000 times
10.20%.After-20 DEG C are deposited 3 months, recover room temperature, measure photovoltaic energy conversion efficiency and have no significant change.
Embodiment 3:
Assemble glass door main body 10, electrochromic device 20 and electricity mode transfer block 30.
Make electrochromic device 20 to include:
(1)WO3Prepared by nano thin-film 5 materials Electrochromic electrode:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness
It is about 340nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 210nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 415 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 410 DEG C, be incubated 4.3 hours, after be naturally cooling to room temperature, i.e. obtain cylinder WO3
Nano-stick array thin film 5, i.e. obtains electrochromic electrode；
Wherein nanorod length is 0.6 μm, density of nanorods about 106/cm2。
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness
It is about 515nm, then it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then
Clean 10 minutes, in N2 atmosphere after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate
In dry up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 2nm, after FTO glass is cleaned again according to the method for a step；
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and ethanolamine (Monoethanolamine) are used
With ethylene glycol monomethyl ether (2-methoxyethanol) as solvent, it is configured to the colloidal sol of 50mM equimolar ratio,
It is slowly dropped into the aqueous trehalose solution of the 10g/L of 0.02 times of volume the most again, and the formation that stirs is the most mixed
Conjunction state, is spun in the FTO substrate cleaned, and spin coating 3 times is to obtain continuous print nanoparticulate thin films, often
Between secondary spin coating by substrate infrared lamps promote solvent volatilization, finally by substrate in an atmosphere 385 DEG C move back
Fiery half an hour, forming large area equally distributed ZnO nanoparticle Seed Layer, the thickness of described Seed Layer is
27nm；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ITO base
Plate is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water, dries in the air
Zinc oxide nanowire is i.e. obtained after Gan；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode 3 improved；
(3) prepared by electrolyte 4:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid 4.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
At room temperature, 1000W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly are used
2400 source meter, irradiation intensity is 100W/cm2, battery is 0.25cm by illuminating area2Under the conditions of
Measuring photovoltaic energy conversion efficiency is 9.50%, measures photovoltaic energy conversion efficiency and be after circulating 5000 times
9.34%.After-20 DEG C are deposited 3 months, recover room temperature, measure photovoltaic energy conversion efficiency and have no significant change.
Embodiment 4 comparative example:
Assemble glass door main body 10, electrochromic device 20 and electricity mode transfer block 30.
Make electrochromic device 20 to include:
(1)WO3Prepared by nano thin-film 5 materials Electrochromic electrode:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 500nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 500nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 500 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 500 DEG C, be incubated 4.1 hours, after be naturally cooling to room temperature, i.e. obtain cylinder WO3
Nano-stick array thin film 5, i.e. obtains electrochromic electrode；
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 520nm, then it is carried out the high temperature anneal, obtains the FTO electro-conductive glass that intensity is higher, so
Clean 10 minutes, at N2 gas after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate afterwards
Atmosphere dries up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 1nm, after FTO glass is cleaned again according to the method for a step；
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H20) and ethanolamine (Monoethanolamine) are used
With ethylene glycol monomethyl ether (2-methoxyethanol) as solvent, it is configured to the colloidal sol of 50mM equimolar ratio,
Be spun in the FTO substrate cleaned, spin coating 3 times to obtain continuous print nanoparticulate thin films, each spin coating it
Between by substrate with infrared lamps promote solvent volatilization, finally by substrate in an atmosphere 500 DEG C annealing half an hour,
Form large area equally distributed ZnO nanoparticle Seed Layer；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ITO base
Plate is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water, dries in the air
Zinc oxide nanowire is i.e. obtained after Gan；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode 3 improved；
(3) prepared by electrolyte 4:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid 4.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
At room temperature, 1000W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly are used
2400 source meter, irradiation intensity is 100W/cm2, battery is 0.25cm by illuminating area2Under the conditions of
Measuring photovoltaic energy conversion efficiency is 5.98%, measures photovoltaic energy conversion efficiency and be after circulating 5000 times
3.98%.After-20 DEG C are deposited 3 months, recover room temperature, measure photovoltaic energy conversion efficiency and reduce 9.7%.
Embodiment 5 comparative example:
Assemble glass door main body 10, electrochromic device 20 and electricity mode transfer block 30.
Make electrochromic device 20 to include:
(1)WO3Prepared by nano thin-film 5 materials Electrochromic electrode:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 600nm；
B. it is carried out the high temperature anneal, obtain the FTO electro-conductive glass that intensity is higher, then according to ultrapure
Water, acetone, ethanol order by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then,
Utilizing magnetron sputtering method to plate W film on FTO glass, its thickness is 400nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.3mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the ITO conductive glass surface of W film, at 500 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 600 DEG C, be incubated 5 hours, after be naturally cooling to room temperature, i.e. obtain cylinder WO3Receive
Rice rod array film 5, i.e. obtains electrochromic electrode；
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass 1 surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film 2 to specific dimensions is thick
Degree is about 600nm, then it is carried out the high temperature anneal, obtains the FTO electro-conductive glass that intensity is higher, so
Clean 10 minutes, at N2 gas after taking-up with UV ozone cleaning machine again after cleaning 20 minutes with EtOH Sonicate afterwards
Atmosphere dries up；
B. FTO glass is put in gold spraying instrument, at one layer of golden film of FTO surface spraying plating as catalyst, gold film
Thickness is about 5nm, after FTO glass is cleaned again according to the method for a step；
C. Zinc diacetate dihydrate (Zn (CH3C00) 2-2H is used20) and ethanolamine (Monoethanolamine)
With ethylene glycol monomethyl ether (2-methoxyethanol) as solvent, it is configured to the colloidal sol of 50mM equimolar ratio,
Be spun in the FTO substrate cleaned, spin coating 3 times to obtain continuous print nanoparticulate thin films, each spin coating it
Between by substrate with infrared lamps promote solvent volatilization, finally by substrate in an atmosphere 500 DEG C annealing half an hour,
Form large area equally distributed ZnO nanoparticle Seed Layer；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, by ITO base
Plate is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water, dries in the air
Zinc oxide nanowire is i.e. obtained after Gan；
E. pure organic doline dyes D102 is dissolved into the second eyeball and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode 3 improved；
(3) prepared by electrolyte 4:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid 4.
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve about 5mm width
Blank electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by the double-component aviation glue closed, and makes to leave between two electrodes the space of 100 μm, and in this space
Interior filling electrolyte, obtains self energizing electrochromic device after glue all solidifies.
At room temperature, 1000W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly are used
2400 source meter, irradiation intensity is 100W/cm2, battery is 0.25cm by illuminating area2Under the conditions of
Measuring photovoltaic energy conversion efficiency is 6.12%, measures photovoltaic energy conversion efficiency and be after circulating 5000 times
5.39%.After-20 DEG C are deposited 3 months, recover room 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 prepares is high, and
Life, freexing tolerance can be more preferable.Each parameter of comparative example is significantly lower than technical scheme, this
Illustrating that the 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, the only present invention preferably detailed description of the invention, but protection scope of the present invention not office
Being limited to this, any those familiar with the art is in the technical scope that the invention discloses, according to this
The technical scheme of invention and inventive concept thereof in addition equivalent or change, all should contain the protection in the present invention
Within the scope of.
Claims (2)
1. can regulate a manufacture method for the glass door of transparency, wherein electrochromic device panel utilizes machine
Tool method is fixed on glass door body surfaces, specifically includes: assemble glass door main body, electrochromic device face
Plate and electricity mode transfer block:
One, the making step of electricity mode transfer block is as follows:
(1) make rearrangeable switch, be used for connecting electrochromic device and control circuit；
(2) control circuit is made, for applying the electric current of electrochromic device according to extraneous light intensity regulating, when
Ambient light tunes up electric current when becoming strong, turns electric current down when ambient light dies down；
Two, the electrochromic device making step of glass door is as follows:
(1)WO3Prepared by nano film material electrochromic electrode:
A. safety glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness is
320-360nm；
B. it is carried out the high temperature anneal, obtains FTO electro-conductive glass, then according to ultra-pure water, acetone,
The order of ethanol is by FTO electro-conductive glass successively ultrasonic cleaning 15min, dry for standby；Then, magnetic control is utilized
Sputtering method plates W film on FTO electro-conductive glass, and its thickness is 200-220nm；W film is used as WO3Nano wire
Growth source；
C. prepare the sodium tungstate aqueous solution of 0.2mol/L, then drip the hydrochloric acid of 3mol/L to no longer producing
Till precipitation, obtain vitreosol, by vitreosol by being dissolved in hydrogen peroxide after the washing by centrifugation of gained precipitation
It is applied to be coated with the FTO conductive glass surface of W film, at 400-420 DEG C, calcines 40min obtain WO3Crystal seed layer；
D. by obtained above with WO3The FTO electro-conductive glass of crystal seed layer is put in box-type high-temperature furnace, is passed through Ar
Protection gas, be heated to 400-420 DEG C, be incubated 4-4.5 hour, after be naturally cooling to room temperature, i.e. obtain cylinder
Shape WO3Nano-stick array thin film, i.e. obtains electrochromic electrode；
Wherein nanorod length is 0.5-0.6 μm, density of nanorods 106/cm2；
(2) prepared by the ZnO nano-wire thin film photoactive electrode improved:
A. safety glass surface magnetic control sputtering fluorine-doped tin oxide (FTO) thin film to specific dimensions, thickness is
500-525nm, then carries out the high temperature anneal to it, obtains FTO electro-conductive glass, then uses EtOH Sonicate
Clean 10 minutes, at N after taking-up with UV ozone cleaning machine again after cleaning 20 minutes2Atmosphere dries up；
B. FTO electro-conductive glass is put in gold spraying instrument, in the golden film conduct of FTO conductive glass surface spraying plating one layer
Catalyst, gold film thickness be 1-2nm, after FTO electro-conductive glass is cleaned again according to the method for a step；
C. use Zinc diacetate dihydrate and ethanolamine with ethylene glycol monomethyl ether as solvent, be configured to 50mM equimolar
The colloidal sol of ratio, is slowly dropped into the aqueous trehalose solution of the 10g/L of 0.02-0.03 times of volume the most again, and stirs
Mixing and be formed uniformly uniform admixture, be spun on the FTO electro-conductive glass cleaned, spin coating 3 times is with the company of acquisition
Continuous nanoparticulate thin films, promotes solvent volatilization by FTO electro-conductive glass infrared lamps between each spin coating,
Finally by FTO electro-conductive glass in an atmosphere 385 DEG C annealing half an hour, formed the equally distributed ZnO of large area
Nanoparticle Seed Layer, the thickness of described Seed Layer is 22-28nm；
D. the ZnSO of 0.15M is prepared4Aqueous solution, with concentrated ammonia solution regulation pH value to 10, leads FTO
Electricity glass is put in solution, puts into the baking oven of 95 DEG C after sealing, and 2 as a child took out, and cleans with deionized water,
Zinc oxide nanowire is i.e. obtained after drying；
E. pure organic doline dyes D102 is dissolved into the acetonitrile and the solution of the tert-butyl alcohol that volume ratio is 1:1
In, concentration is 0.5mM, is immersed in D102 by ZnO nano-wire, keeps in Dark Place 5 hours, after taking-up,
Rinse the ZnO nano-wire after D102 sensitization with dehydrated alcohol, adsorbed by physical adsorption way fully to remove
To the D102 molecule on ZnO nano-wire surface, obtain the photoactive electrode improved；
(3) prepared by electrolyte:
It is made into 0.1M LiI and 0.001M I2PC solution, as self energizing electrochromic device support electricity
Solve liquid；
(4) device assembles:
Electrochromic electrode is relative with effective work surface of photoactive electrode, and two ends reserve the blank of 5mm width
Electro-conductive glass mixes as the electrode of reserved access external circuit, the surrounding bead of a diameter of 100 μm
Compacting smeared by double-component aviation glue, makes to leave between two electrodes the space of 100 μm, and fills out in this space
Fill electrolyte, after glue all solidifies, obtain self energizing electrochromic device.
2. the glass door that the manufacture method described in claim 1 prepares.
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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 |
| US10649298B2 (en) * | 2016-02-15 | 2020-05-12 | Sharp Kabushiki Kaisha | Electrochromic device and smart window provided 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 |
| US10247996B2 (en) * | 2016-06-22 | 2019-04-02 | Gentex Corporation | Thermal control of variable transmittance windows |
Citations (5)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130258436A1 (en) * | 2012-04-03 | 2013-10-03 | Sage Electrochromics, Inc. | Patterned obscuration lines for electrochromic devices |
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Patent Citations (5)
| 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 |
| 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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