CN110376816A - Self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel and preparation method thereof - Google Patents
Self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel and preparation method thereof Download PDFInfo
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- G—PHYSICS
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- 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
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- 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
- G02F1/1514—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 characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—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 characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
- G02F1/1524—Transition metal compounds
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- 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
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- 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
- G02F1/163—Operation of electrochromic cells, e.g. electrodeposition cells; Circuit arrangements therefor
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Abstract
Self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel and preparation method thereof, includes the following steps；1) it cleans FTO electro-conductive glass and dries；2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；4) polyacrylamide hydrogel is prepared；5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；6) aluminium chlorohydrol is packaged by sticking the transparent Indium tungsten base electrochomeric films that the simple glass of aluminium electrode is obtained with step 3), obtains electrochromic intelligent window device；7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtains no-voltage and erasable ion is driven to write screen.Preparation method of the present invention is simple, it is easy to accomplish.
Description
Technical field
The present invention relates to intelligent window setting technique and plasma screen field of display technology, in particular to based on aluminium ion hydrogel from
Power supply tungsten oxide base electrochromic device and preparation method thereof.
Background technique
Electrochromism refers under the driving of electric field, by electrochemical reaction, realize substance optical properties (absorptivity,
Transmitance or reflectivity) lasting, reversible transition, and then show the reversible change of color and transparency.Electrochromic device
Because it can be had greatly as the characteristics of the reversible regulation of the transmitance of the wish of people realization visible light and infrared light in photoelectric field
Application prospect.Electrochromic device can play as building energy-saving the effects of with display, thus can be used as electrochromic intelligent
The concrete application of the devices such as window, Antiglaring rear mirror, electrochromic display device (ECD).
Electrochromic device structure is complex at present, increases interface transmission and industry manufacturing cost.Electrochromic device
Color and two processes of decoloration require the driving of applied voltage in realization.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide the confession electroxidation based on aluminium ion hydrogel
Tungsten base electrochromic device and preparation method thereof simplifies the structure of electrochromic device, benefit by introducing aluminium ion hydrogel
In the transmission of ion, the electrochromic intelligent window and erasable ion write screen and have self-powered, and no-voltage drives erasable
Function, and preparation method is simple, it is easy to accomplish.
To achieve the goals above, the technical solution adopted by the present invention is that:
Self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel, respectively electrochromic intelligent window, nothing
Voltage drives erasable ion to write screen.
The preparation method of self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel, includes the following steps；
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of the step 1) are as follows: successively surpass electro-conductive glass using deionized water, acetone and ethyl alcohol
Sound cleaning, dries in dustfree environment.
The concrete operations of the step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 2-8ml hydrogen peroxide, negate 50 DEG C -70 DEG C of the supernatant after answering it is dry
To tungsten complex, then ultrasound 1-3h dispersion in ethanol, stand 2h-5h filter tungsten oxide precursor sol；By 40g oxygen
Change molybdenum powder to mix with 80-100ml ethyl alcohol, 3h is stood after ball milling 2-3h and takes supernatant, obtains oxidation molybdenum solution；The oxygen that will be obtained
Change tungsten precursor sol to mix with oxidation molybdenum solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide；
The volume ratio of the tungsten oxide precursor sol and oxidation molybdenum solution is 1:1.
Collosol and gel spin coating method is used in the step 3), on FTO electro-conductive glass spin coating precursor sol and at
Film when specific operation, carries out spin coating by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows: using molten
Glue gel spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide, spin coating (revolving speed on FTO electro-conductive glass
1000-2000r/min, spin-coating time 6-20s), in 100 DEG C of -200 DEG C of heating 5min-20min of heating plate after spin coating.
The condition of annealing is to be warming up to 300-400 DEG C with the heating rate of 5-20 DEG C/min, and keep the temperature 30min-
Then 60min cools to room temperature with the furnace.
The concrete operations of the step 4) are as follows:
Take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine is molten
In Xie Yushui, mixed solution is obtained, then mixed solution is stirred 10-30min at room temperature, be then injected into mold, then will
Mold is put into 50 DEG C of -60 DEG C of heat preservation 3-5h in incubator, obtains polyacrylamide hydrogel；
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 the step 5) are as follows:
By the 0.2M-2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide aqueous amine
Gel reaches diffusion balance, obtains the aluminium chlorohydrol of corresponding 0.1M-1M.
Aluminium chlorohydrol obtained by sticking the simple glass of aluminium electrode with step 3) in the step 6) saturating
The concrete operations that bright tungsten oxide base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in the step 7), is had
Gymnastics conduct:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
Beneficial effects of the present invention:
Self-powered oxide-base electrochromic device and preparation method thereof of the present invention based on aluminium ion hydrogel
When specific operation, tungsten oxide is become by the compound precursor sol of the spin coating tungsten oxide on FTO electro-conductive glass and molybdenum oxide
Base film, wherein molybdenum oxide also has electrochromic effect, so that tungsten oxide base electrochomeric films have bigger light
Modification scope.
In addition, the present invention is based on aluminium ion hydrogels, and electrochromic device is prepared, as electrochromic intelligent window
In application, colouring process does not need applied voltage effect, driven by internal potential；Decolorization only by low-voltage (1V) realize,
With energy-saving and environment-friendly advantage.The electrochromic device of full aluminium system with hydrogel pen and the hydrogen peroxide of extremely low concentration are molten
Liquid phase effect not only realizes that write screen writing and erase process drives without external voltage, and is the application of electrochromic device
Provide new direction.The preparation method of the two devices is relatively simple, it is easy to accomplish, in aircraft windows, smart home or intelligence
Electronics etc. is with a wide range of applications.
Detailed description of the invention
Fig. 1 is electrochromic device structural schematic diagram.
Fig. 2 is for electrochromic intelligent window in paint state and state of decolourizing through spectrum.
Fig. 3 is that electrochromic intelligent window confesses electric process respectively in feux rouges (660nm), blue light (435nm), green light
Original position at (520nm) penetrates spectrum.
Fig. 4 is that no-voltage drives erasable ion to write the multiple writing-erasing light transmission rate figure shielded.
Fig. 5 is that no-voltage drives erasable ion to write the writing-erasing optical photograph shielded.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
With reference to Fig. 1, its knot of the self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel
Structure is sandwich structure, wherein tungsten oxide base electrochomeric films, aluminium ion hydrogel, the simple glass point for sticking aluminium electrode
Not Gou Cheng structure every layer of substance.
The preparation method of self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel includes
Following steps:
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of step 1) are as follows: electro-conductive glass is successively cleaned by ultrasonic using deionized water, acetone and ethyl alcohol,
It is dried in dustfree environment again.
The concrete operations of step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 5ml hydrogen peroxide, 50 DEG C -70 DEG C of the supernatant after answering is negated and is dried to obtain
Tungsten complex, then ultrasound 1-3h dispersion in ethanol, stand 2h-5h filter tungsten oxide precursor sol；40g is aoxidized
Molybdenum powder is mixed with 80-100ml ethyl alcohol, and 3h is stood after ball milling 1-3h and takes supernatant, obtains oxidation molybdenum solution；The oxidation that will be obtained
Tungsten precursor sol is mixed with oxidation molybdenum solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide；
The volume ratio of the tungsten oxide precursor sol and oxidation molybdenum solution is 1:1.
Collosol and gel spin coating method is used in the step 3), on FTO electro-conductive glass spin coating precursor sol and at
Film when specific operation, carries out spin coating by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows: using molten
Glue gel spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide, spin coating (revolving speed on FTO electro-conductive glass
1000-2000r/min, spin-coating time 6-20s), in 100 DEG C of -200 DEG C of heating 5min-20min of heating plate after spin coating.
The condition of annealing is to be warming up to 300-400 DEG C with the heating rate of 5-20 DEG C/min, and keep the temperature 30min-
Then 60min cools to room temperature with the furnace.
The concrete operations of the step 4) are as follows:
Take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine is molten
In Xie Yushui, mixed solution is obtained, then mixed solution is stirred 10-30min at room temperature, be then injected into mold, then will
Mold is put into 50 DEG C of -60 DEG C of heat preservation 3-5h in incubator, obtains polyacrylamide hydrogel；
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:
By the 0.2M-2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide aqueous amine
Gel reaches diffusion balance, obtains the aluminium chlorohydrol of corresponding 0.1M-1M.
The transparent Indium for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode in step 6)
The concrete operations that tungsten base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in step 7), concrete operations
Are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
Embodiment one
The preparation method of self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel includes
Following steps:
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of step 1) are as follows: electro-conductive glass is successively cleaned by ultrasonic using deionized water, acetone and ethyl alcohol,
It is dried in dustfree environment.
The concrete operations of step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 2ml hydrogen peroxide, 70 DEG C of the supernatant after answering is negated and is dried to obtain tungsten network
Close object, then ultrasound 1h dispersion in ethanol, standing 3h filter tungsten oxide precursor sol；By 40g molybdenum oxide powder with
80ml ethyl alcohol mixes, and 3h is stood after ball milling 1h and takes supernatant, obtains oxidation molybdenum solution；By obtained tungsten oxide precursor sol with
Molybdenum solution mixing is aoxidized, tungsten oxide and the compound precursor sol of molybdenum oxide are obtained.
The volume ratio of tungsten oxide precursor sol and oxidation molybdenum solution is 1:1.
Collosol and gel spin coating method, the spin coating precursor sol on FTO electro-conductive glass, and the tool to form a film are used in step 3)
When gymnastics is made, 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 collosol and gel
Spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass, wherein the speed of spin coating is
1000r/min, spin-coating time 8s use heating plate to 200 DEG C of heating 10min after spin coating.
Annealing condition is that the heating rate of 10 DEG C/min is warming up to 400 DEG C, and keeps the temperature 30min, then furnace cooling
To room temperature.
The concrete operations of step 4) are as follows: take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ',
N '-tetramethylethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 10min at room temperature, then infuses
Enter in mold, then mold is put into 50 DEG C of incubators and keeps the temperature 4h, obtains polyacrylamide hydrogel.Wherein acryloyl in mixed solution
Amine, N, 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:
By the 2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide hydrogel reaches
It is balanced to diffusion, obtains the aluminium chlorohydrol of corresponding 1M.
The transparent Indium for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode in step 6)
The concrete operations that tungsten base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in step 7), concrete operations
Are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
Embodiment two
The preparation method of self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel includes
Following steps:
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of step 1) are as follows: electro-conductive glass is successively cleaned by ultrasonic using deionized water, acetone and ethyl alcohol,
It is dried in dustfree environment.
The concrete operations of step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 4ml hydrogen peroxide, 60 DEG C of the supernatant after answering is negated and is dried to obtain tungsten network
Close object, then ultrasound 2h dispersion in ethanol, standing 2h filter tungsten oxide precursor sol；By 40g molybdenum trioxide powder
It is mixed with 90ml ethyl alcohol, 3h is stood after ball milling 1h and takes supernatant, obtains molybdenum trioxide solution；Obtained tungsten oxide presoma is molten
Glue is mixed with molybdenum trioxide solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide.
The volume ratio of tungsten oxide precursor sol and molybdenum trioxide solution is 1:1.
Collosol and gel spin coating method, the spin coating precursor sol on FTO electro-conductive glass, and the tool to form a film are used in step 3)
When gymnastics is made, 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 collosol and gel
Spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass, wherein the speed of spin coating is
1500r/min, spin-coating time 8s use heating plate to 200 DEG C of heating 10min 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 15 DEG C/min
350 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 ',
N '-tetramethylethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 0.5h at room temperature, then infuses
Enter in mold, then mold is put into 55 DEG C of incubators and keeps the temperature 5h, obtains polyacrylamide hydrogel.Wherein acryloyl in mixed solution
Amine, N, 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:
By the 2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide hydrogel reaches
It is balanced to diffusion, obtains the aluminium chlorohydrol of corresponding 1M.
The transparent Indium for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode in step 6)
The concrete operations that tungsten base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in step 7), concrete operations
Are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electricity grade and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
Embodiment three
The preparation method of self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel includes
Following steps:
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of step 1) are as follows: electro-conductive glass is successively cleaned by ultrasonic using deionized water, acetone and ethyl alcohol,
It is dried in dustfree environment.
The concrete operations of step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 6ml hydrogen peroxide, 65 DEG C of the supernatant after answering is negated and is dried to obtain tungsten network
Close object, then ultrasound 1h dispersion in ethanol, standing 3h filter tungsten oxide precursor sol；By 40g molybdenum trioxide powder
It is mixed with 100ml ethyl alcohol, 3h is stood after ball milling 1h and takes supernatant, obtains molybdenum trioxide solution；The tungsten oxide presoma that will be obtained
Colloidal sol is mixed with molybdenum trioxide solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide.
The volume ratio of tungsten oxide precursor sol and molybdenum trioxide solution is 1:1.
Collosol and gel spin coating method, the spin coating precursor sol on FTO electro-conductive glass, and the tool to form a film are used in step 3)
When gymnastics is made, 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 collosol and gel
Spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass, wherein the speed of spin coating is
1000r/min, spin-coating time 10s use heating plate to 150 DEG C of heating 10min 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
300 DEG C are warming up to, and keeps the temperature 30min, 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 ',
N '-tetramethylethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 10min at room temperature, then infuses
Enter in mold, then mold is put into 50 DEG C of incubators and keeps the temperature 4h, obtains polyacrylamide hydrogel.Wherein acryloyl in mixed solution
Amine, N, 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:
By the 1M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide hydrogel reaches
It is balanced to diffusion, obtains the aluminium chlorohydrol of corresponding 0.5M.
The transparent Indium for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode in step 6)
The concrete operations that tungsten base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in step 7), concrete operations
Are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
Example IV
The preparation method of self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel includes
Following steps:
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of step 1) are as follows: electro-conductive glass is successively cleaned by ultrasonic using deionized water, acetone and ethyl alcohol,
It is dried in dustfree environment.
The concrete operations of step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 8ml hydrogen peroxide, 70 DEG C of the supernatant after answering is negated and is dried to obtain tungsten network
Close object, then ultrasound 3h dispersion in ethanol, standing 5h filter tungsten oxide precursor sol；By 40g molybdenum trioxide powder
It is mixed with 100ml ethyl alcohol, 3h is stood after ball milling 3h and takes supernatant, obtains molybdenum trioxide solution；The tungsten oxide presoma that will be obtained
Colloidal sol is mixed with molybdenum trioxide solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide.
The volume ratio of tungsten oxide precursor sol and molybdenum trioxide solution is 1:1.
Collosol and gel spin coating method, the spin coating precursor sol on FTO electro-conductive glass, and the tool to form a film are used in step 3)
When gymnastics is made, 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 collosol and gel
Spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass, wherein the speed of spin coating is
2000r/min, spin-coating time 20s use heating plate to 200 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 20 DEG C/min
400 DEG C are warming up to, and keeps the temperature 60min, 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 ',
N '-tetramethylethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 30min at room temperature, then infuses
Enter in mold, then mold is put into 60 DEG C of incubators and keeps the temperature 5h, obtains polyacrylamide hydrogel.Wherein acryloyl in mixed solution
Amine, N, 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:
By the 2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide hydrogel reaches
It is balanced to diffusion, obtains the aluminium chlorohydrol of corresponding 2M.
The transparent Indium for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode in step 6)
The concrete operations that tungsten base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in step 7), concrete operations
Are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
Embodiment five
The preparation method of self-powered tungsten oxide base electrochromic device of the present invention based on aluminium ion hydrogel includes
Following steps:
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound presoma of molybdenum oxide on FTO electro-conductive glass
Colloidal sol, and form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the transparent Indium tungsten base electricity for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
It causes optically variable films to be packaged, obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, obtaining no-voltage driving can
Erasable ion writes screen.
The concrete operations of step 1) are as follows: electro-conductive glass is successively cleaned by ultrasonic using deionized water, acetone and ethyl alcohol,
It is dried in dustfree environment.
The concrete operations of step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 2ml hydrogen peroxide, 50 DEG C of the supernatant after answering is negated and is dried to obtain tungsten network
Close object, then ultrasound 1h dispersion in ethanol, standing 2h filter tungsten oxide precursor sol；By 40g molybdenum trioxide powder
It is mixed with 80ml ethyl alcohol, 3h is stood after ball milling 2h and takes supernatant, obtains molybdenum trioxide solution；Obtained tungsten oxide presoma is molten
Glue is mixed with molybdenum trioxide solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide.
The volume ratio of tungsten oxide precursor sol and molybdenum trioxide solution is 1:1.
Collosol and gel spin coating method, the spin coating precursor sol on FTO electro-conductive glass, and the tool to form a film are used in step 3)
When gymnastics is made, 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 collosol and gel
Spin coating method spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass, wherein the speed of spin coating is
1000r/min, spin-coating time 6s use heating plate to 100 DEG C of heating 5min 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 5 DEG C/min
300 DEG C are warming up to, and keeps the temperature 30min, 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 ',
N '-tetramethylethylenediamine is dissolved in the water, and obtains mixed solution, then mixed solution is stirred 10min at room temperature, then infuses
Enter in mold, then mold is put into 50 DEG C of incubators and keeps the temperature 3h, obtains polyacrylamide hydrogel.Wherein acryloyl in mixed solution
Amine, N, 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:
By the 0.2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide hydrogel
Reach diffusion balance, obtains the aluminium chlorohydrol of corresponding 0.1M.
The transparent Indium for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode in step 6)
The concrete operations that tungsten base electrochomeric films are packaged are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then aluminium electrode will be sticked
Simple glass sticks together, and is packaged into electrochromic intelligent window device.
Hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains in step 7), concrete operations
Are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base
Electrochomeric films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator of extremely low concentration
It is acted on electrochomeric films.
By the manufacturing process of embodiment 1, as shown in Figure 2, electrochromic device colouring state and decoloration state regulate and control in visible light
Range is up to 51%, and with reference to Fig. 3, electrochromic intelligent window device confesses electric process, respectively in three coloured light (feux rouges 660nm, green light
520nm, blue light 435nm) at original position penetrate spectrum, light modulation range is respectively up to 49%, 45%, 40% during colouring；
Fig. 4 is that no-voltage drives erasable ion to write multiple writing-erasing light transmission rate figure of screen, writes the light modulation range of erasing
It is 45% or so, ensure that display function；By Fig. 5, it may be appreciated that the writing-that no-voltage drives erasable ion to write screen was wiped
Journey.
Claims (9)
1. the self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel, which is characterized in that be respectively electrochromism
Smart window, no-voltage drive erasable ion to write screen.
2. the preparation method of the self-powered tungsten oxide base electrochromic device based on aluminium ion hydrogel, which is characterized in that including
Following steps；
1) it cleans FTO electro-conductive glass and dries；
2) tungsten oxide and the compound precursor sol of molybdenum oxide are prepared；
3) collosol and gel spin coating method is used, spin coating tungsten oxide and the compound precursor sol of molybdenum oxide on FTO electro-conductive glass,
And form a film, it is then made annealing treatment, obtains transparent Indium tungsten base electrochomeric films；
4) polyacrylamide hydrogel is prepared；
5) polyacrylamide hydrogel is infiltrated into liquor alumini chloridi, obtains aluminium chlorohydrol；
6) the electroluminescent change of transparent Indium tungsten base for obtaining aluminium chlorohydrol by the simple glass and step 3) that stick aluminium electrode
Color film is packaged, and obtains electrochromic intelligent window device；
7) hydrogel pen is connect with the transparent Indium tungsten base electrochomeric films that step 3) obtains, it is erasable obtains no-voltage driving
Ion writes screen.
3. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that the concrete operations of the step 1) are as follows: electro-conductive glass is successively used to deionized water, acetone and ethyl alcohol
It is cleaned by ultrasonic, is dried in dustfree environment.
4. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that the concrete operations of the step 2) are as follows:
1g tungsten powder is reacted in ice-water bath with 2-8ml hydrogen peroxide, 50 DEG C -70 DEG C of the supernatant after answering is negated and is dried to obtain tungsten
Complex compound, then ultrasound 1-3h dispersion in ethanol, stand 2h-5h filter tungsten oxide precursor sol；By 40g molybdenum oxide
Powder is mixed with 80-100ml ethyl alcohol, and 3h is stood after ball milling 2-3h and takes supernatant, obtains oxidation molybdenum solution；The tungsten oxide that will be obtained
Precursor sol is mixed with oxidation molybdenum solution, obtains tungsten oxide and the compound precursor sol of molybdenum oxide；
The volume ratio of the tungsten oxide precursor sol and oxidation molybdenum solution is 1:1.
5. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that collosol and gel spin coating method is used in the step 3), spin coating presoma is molten on FTO electro-conductive glass
Glue simultaneously forms a film when specific operation, carries out spin coating by the way of multiple gluing, wherein the concrete operations of each secondary gluing are equal are as follows:
Using collosol and gel spin coating method, spin coating tungsten oxide and the compound precursor sol of molybdenum oxide, spin coating (turn on FTO electro-conductive glass
Fast 1000-2000r/min, spin-coating time 6-20s), in 100 DEG C of -200 DEG C of heating 5min- of heating plate after spin coating
20min。
The condition of annealing is to be warming up to 300-400 DEG C with the heating rate of 5-20 DEG C/min, and keep the temperature 30min-60min,
Then room temperature is cooled to the furnace.
6. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that the concrete operations of the step 4) are as follows:
Take acrylamide, N, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine is dissolved in
In water, mixed solution is obtained, then mixed solution is stirred 10-30min at room temperature, be then injected into mold, then by mold
50 DEG C of -60 DEG C of heat preservation 3-5h in incubator are put into, polyacrylamide hydrogel is obtained；
Acrylamide, N in mixed solution, N '-methylene-bisacrylamide, ammonium persulfate and N, N, N ', N '-tetramethylethylenediamine
Molar concentration be respectively 2.2M, 1.32mM, 3.74mM and 0.1mM.
7. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that the concrete operations of the step 5) are as follows:
By the 0.2M-2M aluminum chloride aqueous solution of polyacrylamide hydrogel infiltration same volume, until polyacrylamide hydrogel
Reach diffusion balance, obtains the aluminium chlorohydrol of corresponding 0.1M-1M.
8. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that obtain aluminium chlorohydrol by the simple glass and step 3) for sticking aluminium electrode in the step 6)
To the concrete operations that are packaged of transparent Indium tungsten base electrochomeric films are as follows:
Aluminium chlorohydrol is encapsulated using silicon rubber on tungsten oxide base electrochomeric films, then the common of aluminium electrode will be sticked
Glass sticks together, and is packaged into electrochromic intelligent window device.
9. the preparation side of the self-powered tungsten oxide base electrochromic device according to claim 2 based on aluminium ion hydrogel
Method, which is characterized in that the transparent Indium tungsten base electrochomeric films for obtaining hydrogel pen and step 3) in the step 7)
Connection, concrete operations are as follows:
Aluminium chlorohydrol and aluminium electrode are packaged into hydrogel pen, when writing, aluminium electrode and transparent Indium tungsten base are electroluminescent
Optically variable films connection, hydrogel pen are contacted with electrochomeric films；When erasing, the hydrogenperoxide steam generator and electricity of extremely low concentration
Mutagens color membrane action.
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