CN110262151A - A kind of multi-functional ultraviolet-responsive and shielding smart window and preparation method thereof - Google Patents
A kind of multi-functional ultraviolet-responsive and shielding smart window and preparation method thereof Download PDFInfo
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- CN110262151A CN110262151A CN201910556474.7A CN201910556474A CN110262151A CN 110262151 A CN110262151 A CN 110262151A CN 201910556474 A CN201910556474 A CN 201910556474A CN 110262151 A CN110262151 A CN 110262151A
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- purpurine
- spin coating
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- electrochromic device
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
- C03C17/256—Coating containing TiO2
-
- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B5/00—Doors, windows, or like closures for special purposes; Border constructions therefor
- E06B5/10—Doors, windows, or like closures for special purposes; Border constructions therefor for protection against air-raid or other war-like action; for other protective purposes
- E06B5/18—Doors, windows, or like closures for special purposes; Border constructions therefor for protection against air-raid or other war-like action; for other protective purposes against harmful radiation
-
- 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
- G02F1/1503—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 caused by oxidation-reduction reactions in organic liquid solutions, e.g. viologen solutions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/74—UV-absorbing coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
Abstract
The invention discloses a kind of multi-functional ultraviolet-responsives and shielding smart window and preparation method thereof, including electrochromic device, transparent ultraviolet detector and in-phase amplification circuit, wherein, substratum transparent is mutually be bonded between transparent ultraviolet detector and electrochromic device, transparent ultraviolet detector is electrically connected with electrochromic device by in-phase amplification circuit, the window has the function of detecting uitraviolet intensity and adjusts ultraviolet ray transmissivity, and preparation method is simple, it is easy to accomplish.
Description
Technical field
The invention belongs to smart window technical field, it is related to a kind of multi-functional ultraviolet-responsive and shielding smart window and its preparation
Method.
Background technique
Ultraviolet light is a kind of common electromagnetic radiation, and about 9% solar radiation is distributed in ultraviolet band.Suitable purple
The synthesis of body vitamin D can be sterilized and be promoted to outside line, but excessive ultraviolet radioactive then will lead to many skin diseases.According to
The standard of international lighting tissue, ultraviolet light are divided into three parts: UV-A (320-400nm), UV-B (280-320nm) and
UV-C(100-280nm).Wherein, UV-A is the main source of skin disease.Therefore, detect and regulate and control the ultraviolet spoke of UV-A wave band
Penetrate be the development of following smart electronics an important directions.
It is purple to reach detection that ultraviolet radioactive signal can be changed into electric signal by photoelectric effect by UV photodetector
The purpose of outside line.But the ultraviolet detector studied at present, which is only capable of passively detecting uitraviolet intensity, cannot actively adjust ultraviolet spoke
It penetrates, therefore can not synchronize and realize ultraviolet detection and shielding.And electrochromic device is a kind of excellent spectrum adjusting means, it can be with
The variation of color is realized by reversible redox reaction and achievees the purpose that adjust transmitance.Currently, electrochromic device
The effects of being mainly used for adjusting the electromagnetic wave of infrared band and visible waveband, playing as building energy-saving with display, but seldom
For adjusting ultraviolet ray transmissivity.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of multi-functional ultraviolet-responsive and screen are provided
Smart window and preparation method thereof is covered, which has the function of detecting uitraviolet intensity and adjust ultraviolet ray transmissivity, and preparation side
Method is simple, it is easy to accomplish.
In order to achieve the above objectives, multi-functional ultraviolet-responsive of the present invention and shielding smart window include electrochromism device
Part, transparent ultraviolet detector and in-phase amplification circuit, wherein by transparent between transparent ultraviolet detector and electrochromic device
Glue-line is mutually bonded, and transparent ultraviolet detector is electrically connected with electrochromic device by in-phase amplification circuit.
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows:
By ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and are then stood after magnetic agitation, are obtained titanium dioxide
Precursor sol.
The volume ratio of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride is 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Using the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, uses and add after spin coating
Hot plate is in 200-400 DEG C of heating 10-40min.
The concrete operations of step 4) are as follows:
Take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine, so
After will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine is dissolved in water
In, mixed solution is obtained, then mixed solution is stirred at room temperature, is then injected into mold, then mold is put into incubator
Heat preservation, obtains hydrogel, is then freeze-dried hydrogel, obtain polyacrylamide hydrogel dry glue.
Acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethyl second
The molar concentration of diamines is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows:
Purpurine is dissolved in deionized water, purpurine aqueous solution is obtained, wherein the concentration of purpurine is 1- in purpurine aqueous solution
10mg/ml, then polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, it is up to polyacrylamide hydrogel dry glue is transparent
Only, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows:
Electrochromic device is sealed using silicon rubber, then passes through dimethyl silicone polymer for ultraviolet detector and electricity
Mutagens color device sticks together, and is connected by in-phase amplification circuit.
The invention has the following advantages:
Multi-functional ultraviolet-responsive of the present invention and shielding smart window and preparation method thereof pass through when specific operation
The precursor sol of spin coating titanium dioxide becomes titanium deoxid film on striped electro-conductive glass, wherein titanium deoxid film tool
The characteristics of having forbidden bandwidth big and only absorbing ultraviolet light, has high transparency in visible light wave range, so that visiting outside transparent violet
Surveying device has high optical transparency, high optical responsivity and excellent on-off ratio.In addition, the present invention is based on purpurine hydrogels to be prepared into
To electrochromic device, so that under the voltage of 2V, apparent discoloration can be realized, in visible-range in the electrochromic device
Interior transmitance modulation is maximum up to 60%, 94% ultraviolet light can be obstructed within the scope of UV-A, by transparent ultraviolet detector
After being integrated with electrochromic device, it can be realized dynamic and visual detection uitraviolet intensity and adjust the dual work of ultraviolet radioactive
With and preparation method is relatively simple, it is easy to accomplish, ultraviolet protection, smart home or in terms of have it is extensive
Application prospect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of transparent ultraviolet detector；
Fig. 2 is the light transmission rate curve graph of transparent ultraviolet detector；
Fig. 3 is the photoelectric respone curve graph of transparent ultraviolet detector；
Fig. 4 is the sandwich structure schematic diagram of electrochromic device；
Fig. 5 is transmitance schematic diagram of the electrochromic device under colouring state and decolored state.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawing:
With reference to Fig. 1 and Fig. 4, multi-functional ultraviolet-responsive of the present invention and shielding smart window include electrochromism device
Part, transparent ultraviolet detector and in-phase amplification circuit, wherein use transparent adhesive tape between transparent ultraviolet detector and electrochromic device
Layer is mutually bonded, and the material of substratum transparent is dimethyl silicone polymer, and transparent ultraviolet detector passes through same phase with electrochromic device
Amplifying circuit electrical connection.
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows: by ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and then magnetic force stirs
12h is stood after mixing 2-4h, obtains the precursor sol of titanium dioxide, wherein the body of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride
Product is than being 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Use the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, wherein the speed of spin coating
For 2000-4000r/min, spin-coating time 10-30s, use heating plate in 200-400 DEG C of heating 10- after spin coating
40min；
The concrete operations made annealing treatment in step 3) are as follows: the sample for obtaining spin coating is with the heating speed of 5-20 DEG C/min
Rate is warming up to 450-500 DEG C, and keeps the temperature 1-3h, then cools to room temperature with the furnace.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
Then N '-tetramethylethylenediamine will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-four
Methyl ethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 0.5-1h at room temperature, is then injected into mould
In tool, then mold is put into 45-55 DEG C of incubator and keeps the temperature 1-3h, obtained hydrogel, be then freeze-dried hydrogel, obtain
Polyacrylamide hydrogel dry glue, wherein acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and
N, N, N ', the molar concentration of N '-tetramethylethylenediamine is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows: purpurine is dissolved in deionized water, obtains purpurine aqueous solution, wherein purpurine is water-soluble
The concentration of purpurine is 1-10mg/ml in liquid, then polyacrylamide hydrogel dry glue is infiltrated purpurine aqueous solution, until polyacrylamide
Until aqueous amine gel dry glue is transparent, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows: electrochromic device is sealed using silicon rubber, then by dimethyl silicone polymer by ultraviolet spy
It surveys device to stick together with electrochromic device, and is connected by in-phase amplification circuit.
Embodiment one
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows: by ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and then magnetic force stirs
12h is stood after mixing 2h, obtains the precursor sol of titanium dioxide, wherein the volume of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride
Than for 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Use the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, wherein the speed of spin coating
For 4000r/min, spin-coating time 20s, use heating plate in 350 DEG C of heating 30min after spin coating；
The concrete operations made annealing treatment in step 3) are as follows: the sample for obtaining spin coating is with the heating rate of 10 DEG C/min
500 DEG C are warming up to, and keeps the temperature 1h, then cools to room temperature with the furnace.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
Then N '-tetramethylethylenediamine will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-four
Methyl ethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 0.5h at room temperature, is then injected into mold
In, then mold is put into 50 DEG C of incubator and keeps the temperature 1h, hydrogel is obtained, is then freeze-dried hydrogel, obtains polypropylene
Amide hydrogel dry glue, wherein acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N,
The molar concentration of N ', N '-tetramethylethylenediamine is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows: purpurine is dissolved in deionized water, obtains purpurine aqueous solution, wherein purpurine is water-soluble
The concentration of purpurine is 5mg/ml in liquid, then polyacrylamide hydrogel dry glue is infiltrated purpurine aqueous solution, until polyacrylamide
Until hydrogel dry glue is transparent, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows: electrochromic device is sealed using silicon rubber, then by dimethyl silicone polymer by ultraviolet spy
It surveys device to stick together with electrochromic device, and is connected by in-phase amplification circuit.
Embodiment two
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows: by ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and then magnetic force stirs
12h is stood after mixing 4h, obtains the precursor sol of titanium dioxide, wherein the volume of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride
Than for 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Use the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, wherein the speed of spin coating
For 4000r/min, spin-coating time 30s, use heating plate in 400 DEG C of heating 40min after spin coating；
The concrete operations made annealing treatment in step 3) are as follows: the sample for obtaining spin coating is with the heating rate of 20 DEG C/min
550 DEG C are warming up to, and keeps the temperature 3h, then cools to room temperature with the furnace.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
Then N '-tetramethylethylenediamine will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-four
Methyl ethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 1h at room temperature, is then injected into mold
In, then mold is put into 55 DEG C of incubator and keeps the temperature 3h, hydrogel is obtained, is then freeze-dried hydrogel, obtains polypropylene
Amide hydrogel dry glue, wherein acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N,
The molar concentration of N ', N '-tetramethylethylenediamine is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows: purpurine is dissolved in deionized water, obtains purpurine aqueous solution, wherein purpurine is water-soluble
The concentration of purpurine is 10mg/ml in liquid, then polyacrylamide hydrogel dry glue is infiltrated purpurine aqueous solution, until polyacrylamide
Until hydrogel dry glue is transparent, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows: electrochromic device is sealed using silicon rubber, then by dimethyl silicone polymer by ultraviolet spy
It surveys device to stick together with electrochromic device, and is connected by in-phase amplification circuit.
Embodiment three
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows: by ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and then magnetic force stirs
12h is stood after mixing 3h, obtains the precursor sol of titanium dioxide, wherein the volume of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride
Than for 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Use the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, wherein the speed of spin coating
For 3000r/min, spin-coating time 20s, use heating plate in 300 DEG C of heating 25min after spin coating；
The concrete operations made annealing treatment in step 3) are as follows: the sample for obtaining spin coating is with the heating rate of 12 DEG C/min
480 DEG C are warming up to, and keeps the temperature 2h, then cools to room temperature with the furnace.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
Then N '-tetramethylethylenediamine will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-four
Methyl ethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 0.7h at room temperature, is then injected into mold
In, then mold is put into 48 DEG C of incubator and keeps the temperature 2h, hydrogel is obtained, is then freeze-dried hydrogel, obtains polypropylene
Amide hydrogel dry glue, wherein acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N,
The molar concentration of N ', N '-tetramethylethylenediamine is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows: purpurine is dissolved in deionized water, obtains purpurine aqueous solution, wherein purpurine is water-soluble
The concentration of purpurine is 5mg/ml in liquid, then polyacrylamide hydrogel dry glue is infiltrated purpurine aqueous solution, until polyacrylamide
Until hydrogel dry glue is transparent, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows: electrochromic device is sealed using silicon rubber, then by dimethyl silicone polymer by ultraviolet spy
It surveys device to stick together with electrochromic device, and is connected by in-phase amplification circuit.
Example IV
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows: by ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and then magnetic force stirs
12h is stood after mixing 2.5h, obtains the precursor sol of titanium dioxide, wherein the body of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride
Product is than being 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Use the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, wherein the speed of spin coating
For 2500r/min, spin-coating time 15s, use heating plate in 250 DEG C of heating 20min after spin coating；
The concrete operations made annealing treatment in step 3) are as follows: the sample for obtaining spin coating is with the heating rate of 8 DEG C/min
460 DEG C are warming up to, and keeps the temperature 1.2h, then cools to room temperature with the furnace.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
Then N '-tetramethylethylenediamine will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-four
Methyl ethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 0.6h at room temperature, is then injected into mold
In, then mold is put into 48 DEG C of incubator and keeps the temperature 1.5h, hydrogel is obtained, is then freeze-dried hydrogel, obtains poly- third
Acrylamide hydrogel dry glue, wherein acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N,
The molar concentration of N ', N '-tetramethylethylenediamine is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows: purpurine is dissolved in deionized water, obtains purpurine aqueous solution, wherein purpurine is water-soluble
The concentration of purpurine is 3mg/ml in liquid, then polyacrylamide hydrogel dry glue is infiltrated purpurine aqueous solution, until polyacrylamide
Until hydrogel dry glue is transparent, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows: electrochromic device is sealed using silicon rubber, then by dimethyl silicone polymer by ultraviolet spy
It surveys device to stick together with electrochromic device, and is connected by in-phase amplification circuit.
Embodiment five
Multi-functional ultraviolet-responsive of the present invention and shielding smart window preparation method the following steps are included:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and at
Then film is made annealing treatment, transparent ultraviolet detector is obtained；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, much
Function ultraviolet-responsive and shielding smart window.
The concrete operations of step 1) are as follows: successively use deionized water, acetone and ethyl alcohol to carry out ultrasound striped electro-conductive glass
Cleaning, then dried in dustfree environment.
The concrete operations of step 2) are as follows: by ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and then magnetic force stirs
12h is stood after mixing 3.5h, obtains the precursor sol of titanium dioxide, wherein the body of ethylene glycol monomethyl ether, butyl titanate and acetic anhydride
Product is than being 9:3:2.
Collosol and gel spin coating method is used in step 3), the presoma of spin coating titanium dioxide is molten on striped electro-conductive glass
Glue, and form a film when specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Use the precursor sol of collosol and gel spin coating method spin coating titanium dioxide on striped electro-conductive glass, wherein the speed of spin coating
For 3500r/min, spin-coating time 28s, use heating plate in 350 DEG C of heating 55min after spin coating；
The concrete operations made annealing treatment in step 3) are as follows: the sample for obtaining spin coating is with the heating rate of 18 DEG C/min
520 DEG C are warming up to, and keeps the temperature 2.5h, then cools to room temperature with the furnace.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
Then N '-tetramethylethylenediamine will take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-four
Methyl ethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 0.9h at room temperature, is then injected into mold
In, then mold is put into 52 DEG C of incubator and keeps the temperature 2.5h, hydrogel is obtained, is then freeze-dried hydrogel, obtains poly- third
Acrylamide hydrogel dry glue, wherein acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N,
The molar concentration of N ', N '-tetramethylethylenediamine is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
The concrete operations of step 5) are as follows: purpurine is dissolved in deionized water, obtains purpurine aqueous solution, wherein purpurine is water-soluble
The concentration of purpurine is 8mg/ml in liquid, then polyacrylamide hydrogel dry glue is infiltrated purpurine aqueous solution, until polyacrylamide
Until hydrogel dry glue is transparent, purpurine hydrogel is obtained.
The electrochromic device that the transparent ultraviolet detector for obtaining step 3) in step 7) is obtained with step 6) collects
At concrete operations are as follows: electrochromic device is sealed using silicon rubber, then by dimethyl silicone polymer by ultraviolet spy
It surveys device to stick together with electrochromic device, and is connected by in-phase amplification circuit.
By the manufacturing process of embodiment 1, as shown in Figure 2, transparent ultraviolet detector transmitance in visible-range is reachable
90%, with reference to Fig. 3, under the bias of 1V, under the ultraviolet lighting of light intensity 18.7mW, the photoelectric current of transparent ultraviolet detector reaches
489.95 μ A, brightness electric current ratio is up to 1.48 × 104.As shown in Figure 4, electrochromic device maximum transmission in visible-range
Modulation can obstruct 94% ultraviolet light in UV-A range up to 60%.
Claims (10)
1. a kind of multi-functional ultraviolet-responsive and shielding smart window, which is characterized in that including being visited outside electrochromic device, transparent violet
Survey device and in-phase amplification circuit, wherein it is mutually be bonded by substratum transparent between transparent ultraviolet detector and electrochromic device, thoroughly
Bright ultraviolet detector is electrically connected with electrochromic device by in-phase amplification circuit.
2. the preparation method of multi-functional ultraviolet-responsive described in a kind of claim 1 and shielding smart window, which is characterized in that including
Following steps:
1) it cleans striped electro-conductive glass and dries；
2) precursor sol of titanium dioxide is configured；
3) collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass are used, and is formed a film, so
After made annealing treatment, obtain transparent ultraviolet detector；
4) polyacrylamide hydrogel dry glue is prepared；
5) polyacrylamide hydrogel dry glue is infiltrated into purpurine aqueous solution, obtains purpurine hydrogel；
6) purpurine hydrogel is packaged by electro-conductive glass, obtains electrochromic device；
7) electrochromic device that the transparent ultraviolet detector for obtaining step 3) is obtained with step 6) integrates, and obtains multi-functional
Ultraviolet-responsive and shielding smart window.
3. the preparation method of multi-functional ultraviolet-responsive according to claim 2 and shielding smart window, which is characterized in that step
Rapid concrete operations 1) are as follows: be successively cleaned by ultrasonic striped electro-conductive glass using deionized water, acetone and ethyl alcohol, then in nothing
It is dried in dirt environment.
4. the preparation method of multi-functional ultraviolet-responsive according to claim 2 and shielding smart window, which is characterized in that step
Rapid concrete operations 2) are as follows:
By ethylene glycol monomethyl ether, butyl titanate and acetic anhydride are mixed, and are then stood after magnetic agitation, before obtaining titanium dioxide
Drive body colloidal sol.
5. the preparation method of multi-functional ultraviolet-responsive according to claim 4 and shielding smart window, which is characterized in that second
The volume ratio of glycol methyl ether, butyl titanate and acetic anhydride is 9:3:2.
6. the preparation method of multi-functional ultraviolet-responsive according to claim 2 and shielding smart window, which is characterized in that step
It is rapid 3) middle using collosol and gel spin coating method, the precursor sol of spin coating titanium dioxide on striped electro-conductive glass, and form a film
When specific operation, spin coating is carried out by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows: solidifying using colloidal sol
The precursor sol of glue spin coating method spin coating titanium dioxide on striped electro-conductive glass, using heating plate in 200- after spin coating
400 DEG C of heating 10-40min.
7. the preparation method of multi-functional ultraviolet-responsive according to claim 2 and shielding smart window, which is characterized in that step
Rapid concrete operations 4) are as follows:
Take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', then N '-tetramethylethylenediamine will
Take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine is dissolved in the water,
Mixed solution is obtained, then mixed solution is stirred at room temperature, is then injected into mold, then mold is put into incubator and is protected
Temperature obtains hydrogel, is then freeze-dried hydrogel, obtains polyacrylamide hydrogel dry glue.
8. the preparation method of multi-functional ultraviolet-responsive according to claim 7 and shielding smart window, which is characterized in that mixed
Close acrylamide, N in solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', mole of N '-tetramethylethylenediamine
Concentration is respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
9. the preparation method of multi-functional ultraviolet-responsive according to claim 2 and shielding smart window, which is characterized in that step
Rapid concrete operations 5) are as follows:
Purpurine is dissolved in deionized water, purpurine aqueous solution is obtained, wherein the concentration of purpurine is 1-10mg/ in purpurine aqueous solution
Ml, then polyacrylamide hydrogel dry glue infiltration purpurine aqueous solution is obtained until polyacrylamide hydrogel dry glue is transparent
Purpurine hydrogel.
10. the preparation method of multi-functional ultraviolet-responsive according to claim 2 and shielding smart window, which is characterized in that
The electrochromic device for obtaining transparent ultraviolet detector that step 3) obtains and step 6) in step 7) carries out integrated specific
Operation are as follows:
Electrochromic device is sealed using silicon rubber, then passes through dimethyl silicone polymer for ultraviolet detector and electroluminescent change
Color device sticks together, and is connected by in-phase amplification circuit.
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