CN106938892A - It is a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control - Google Patents
It is a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control Download PDFInfo
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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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Abstract
It is a kind of to belong to field of material technology to the preparation method of the Novel compound film of visible near-infrared double regulation and control.Methods described step is as follows：Prepare tungsten oxide nanometer material solution, polyoxometallic acid salting liquid and polyelectrolyte solution；It is standby to conductive transparent material substrate pretreatment；Substrate is alternately immersed into tungsten oxide nanometer material solution and polyelectrolyte solution；Substrate is alternately immersed into polyoxometallic acid salting liquid and polyelectrolyte solution again, that is, obtains the multi-layer compound film material using conductive transparent material as substrate.It is an advantage of the invention that：The laminated film of acquisition can be realized distinguishes reversible regulation and control to visible ray and near-infrared region, and have the advantages that preparation process is simple, low cost, switch efficiency height, good stability, good reversibility, and the species and the number of plies of tungsten oxide nanometer material and many metallized metal oxygen hydrochlorates can be adjusted according to different performance requirement.
Description
Technical field
The invention belongs to field of material technology, and in particular to it is a kind of can be to the Novel compound films of visible near-infrared double regulation and control
Preparation method.
Background technology
Now, 40% and carbon dioxide for maintaining the energy that building is used to account for annual energy resource consumption total amount are always arranged
High-volume 30%, for example, maintaining the energy used in indoor temperature and brightness of building etc..Disappear to further reduce the energy
Consumption and environmental pollution is reduced, new energy-saving material need to be developed to help people to regulate and control the temperature of building according to the need for environment
And light and shade environment, to reach the purpose for saving the energy.Sunshine is as most important lamp, and it reaches the light of earth surface
Can be divided into 53% or so near infrared light (regulating and controlling temperature change), 42% or so visible ray (regulation and control lightness change) and
5% or so ultraviolet light, so new energy-saving material can reach the purpose for saving the energy by regulating and controlling the transmitance of sunshine.
Electrochromic material can produce color and transmission as a kind of advanced composite material (ACM) in the presence of extra electric field
The change of rate, it can be used for the transmitance of regulation and control sunshine, realizes building lightness or the regulation of temperature, built so as to reduce
Build the energy resource consumption of thing.
Although existing part electrochromic material reduces the energy loss of building by regulating and controlling solar radiation now, such as
The conductive film and nanocrystal and the complex thin film of glass of doped metal oxide nanocrystal, but still exist
Some problems, such as most materials are only capable of regulation and control visible ray or near infrared light, it is impossible to regulate and control while realizing Liang Zhongguang areas；Build multiple
The process for closing thin-film material is complex；Material cost is too high；The problems such as regulating and controlling inefficient.
The content of the invention
The invention aims to solve problems of the prior art, there is provided one kind regulation and control efficiency high, stability
It is good and can to it is visible near-infrared it is double regulate and control Novel compound film preparation method.At ambient temperature, LBL self-assembly is passed through
Tungsten oxide nanometer material and polyoxometallate are assembled on the electro-conductive glass pre-processed by method through electrostatic adsorption, are led to
Cross suitable method for packing and prepare electrochromism composite film material.In addition, can be by regulating and controlling tungsten oxide nanometer material and many
The species and the number of plies of oxometallate obtain the electrochromic device of different performance.
Polyoxometallate (Polyoxometalates, abridge POMs, abbreviation polyacid) is used as a kind of excellent electroluminescent change
Color material, can form mixed valence by electroreduction, so as to cause the color change of polyacid, be shown in visible region strong
Absorb, and tungsten oxide nanometer material, under extraneous electric field action, strong infrared absorption can be produced, when both complicated utilizations are suitable
When method is prepared into electrochromism composite film material, can obtain on-off ratio, regulation and control efficiency high, can be achieved near infrared light with it is visible
The new energy-saving material regulated and controled while light.
To achieve the above object, the technical scheme taken is as follows by the present invention：
It is a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, methods described specific steps are such as
Under：
Step one：The tungsten oxide nanometer material solution with negative electrical charge, the polyoxometallic acid with negative electrical charge are prepared respectively
Salting liquid and the polyelectrolyte solution with positive charge；
Step 2：Using conductive transparent material as substrate, conductive transparent material is sized and is cut into fritter, successively in
Each ultrasonic 15min in acetone, isopropanol and water, each ultrasound is finished, and ultra-pure water is washed away except residual organic solvent, is preparedSolution, conductive transparent material is vertically placed in the solution, 80 DEG C of water-bath 1h, is taken out cold
But to room temperature, cleaned with ultra-pure water, N2Drying, conduction is placed in culture dish up, toluene 20mL steams again after is added, in gloves
300 μ LAPTES are taken out in case, are added in the culture dish, sealing lucifuge reaction 24h takes out conductive transparent material, toluene is abandoned
In waste liquid barrel, conductive transparent material acetone is cleaned by ultrasonic 3 times, and each 1min, ultra-pure water is cleaned, and is placed in 4 DEG C of preservations in ultra-pure water
It is standby；
Step 3：Conductive substrates are alternately immersed to the polyelectrolyte solution of positive charge and the tungsten oxide nanometer material of negative electrical charge
In solution, nitrogen drying obtains polyelectrolyte and tungsten oxide nanometer material multilayer film；
Step 4：The plural layers are alternately immersed to the polyelectrolyte solution of positive charge and the polyoxometallic acid of negative electrical charge
In salting liquid, nitrogen drying, prepare polyelectrolyte and polyoxometallate plural layers, finally give using conductive transparent material as
The multi-layer compound film material of substrate, electrochromism test is carried out to it.
The present invention is relative to the beneficial effect of prior art：
(1) it is of the invention to be particularly advantageous in that its preparation process is extremely simple, easily accomplish scale production, and obtain device
Structure is homogeneous controllable.
(2) laminated film that the present invention is obtained can be realized distinguishes reversible regulation and control, and tool to visible ray and near-infrared region
There are low cost, switch efficiency height, good stability, good reversibility, and can require that regulation tungsten oxide is received according to different performance
The species and the number of plies of rice material and polyoxometallate.
Brief description of the drawings
Fig. 1 is W18O49The transmission electron microscope picture of nano wire；
Fig. 2 be different voltages under, electrochromism composite film material (PEI/W18O49)20(PEI/P8W48)20Under different voltages
Transmitance variation diagram；
Fig. 3 is composite film material (PEI/W18O49)20(PEI/P8W48)20500 cyclical stabilities at 1060nm are surveyed
Attempt；
Fig. 4 is composite film material (PEI/W18O49)20(PEI/P8W48)20500 cyclical stabilities at 500nm are surveyed
Attempt；
Fig. 5 changes test chart for the transmitance of composite film material device near infrared light under different voltages；
Fig. 6 be different voltages under, electrochromism composite film material (PAH/W18O49)20(PAH/P8W48)20Under different voltages
Transmitance variation diagram；
Fig. 7 be different voltages under, electrochromism composite film material (PEI/W18O49)20(PEI/P5W30)5Under different voltages
Transmitance variation diagram.
Embodiment
Technical scheme is further described with reference to embodiment, but is not limited thereto, it is every right
Technical solution of the present invention is modified or equivalent, without departing from the spirit and scope of technical solution of the present invention, all should be contained
Cover in protection scope of the present invention.
Embodiment：What present embodiment was recorded be it is a kind of can be to the Novel compound films of visible near-infrared double regulation and control
Preparation method, methods described comprises the following steps that：
Step one：The tungsten oxide nanometer material solution with negative electrical charge, the polyoxometallic acid with negative electrical charge are prepared respectively
Salting liquid and the polyelectrolyte solution with positive charge；
Step 2：Using conductive transparent material as substrate, conductive transparent material is sized and is cut into fritter, successively in
Each ultrasonic 15min in acetone, isopropanol and water, each ultrasound is finished, and ultra-pure water is washed away except residual organic solvent, is preparedSolution, conductive transparent material is vertically placed in the solution, 80 DEG C of water-bath 1h, is taken out cold
But to room temperature, cleaned with ultra-pure water, N2Drying, conduction is placed in culture dish up, toluene 20mL steams again after is added, in gloves
300 μ LAPTES are taken out in case, are added in the culture dish, sealing lucifuge reaction 24h takes out conductive transparent material, toluene is abandoned
In waste liquid barrel, conductive transparent material acetone is cleaned by ultrasonic 3 times, and each 1min, ultra-pure water is cleaned, and is placed in 4 DEG C of preservations in ultra-pure water
It is standby；
Step 3：Conductive substrates are alternately immersed to the polyelectrolyte solution of positive charge and the tungsten oxide nanometer material of negative electrical charge
In solution, nitrogen drying obtains polyelectrolyte and tungsten oxide nanometer material multilayer film；
Step 4：The plural layers are alternately immersed to the polyelectrolyte solution of positive charge and the polyoxometallic acid of negative electrical charge
In salting liquid, nitrogen drying, prepare polyelectrolyte and polyoxometallate plural layers, finally give using conductive transparent material as
The multi-layer compound film material of substrate, electrochromism test is carried out to it；
Step 5：Using FDAC is ultraviolet, visible and near infrared spectrometer (U-4100) and CHI860D electrochemical operations
Stand (Beijing China Tech Pu Tian Co., Ltds), analyze under different voltages, electrochromism composite film material it is visible-near red
The change of the absorbent properties of outside line；High stable light source and the U.S. using CrownTech companies of the U.S. (CTTH-150W)
THORLABS PM-100D digital light powers and energy meter (PM100D), solar simulating radiation test device to visible and infrared
The changed power that area's wavelength is passed through；Using the color change of the real-time registering device of Canon (660D) camera.
Embodiment two：It is a kind of described in embodiment one can be thin to the NEW TYPE OF COMPOSITEs of visible near-infrared double regulation and control
The preparation method of film, the preparation side of described polyelectrolyte solution, tungsten oxide nanometer material solution and polyoxometallic acid salting liquid
Method is：Dissolve polyelectrolyte, tungsten oxide nanometer material and polyoxometallate, above-mentioned three kinds of solution concentrations respectively with deionized water
It is 0.1~10mg/mL.
Embodiment three：It is a kind of described in embodiment one or two can be to the new multiple of visible near-infrared double regulation and control
The preparation method of film is closed, described polyelectrolyte is polyethyleneimine, PAH or polydiene dimethylamine
One kind in base ammonium salt hydrochlorate.
Embodiment four：Described in embodiment one or two it is a kind of to visible and near-infrared region through controllable
The preparation method of Novel compound film, described tungsten oxide nanometer material is W18O49Nano wire, W18O49Nanosphere or W18O49Receive
One kind in rice pin.
Embodiment five：It is a kind of described in embodiment one or two can be to the new multiple of visible near-infrared double regulation and control
The preparation method of film is closed, described polyoxometallate is [PW12O40]3-、[P2W18O62]6-、[NaP5W30O110]14-Or
[H7P8W48O184]33-In one kind.
Embodiment six：It is a kind of described in embodiment one can be thin to the NEW TYPE OF COMPOSITEs of visible near-infrared double regulation and control
In the preparation method of film, step 2, the substrate is for the tin indium oxide using glass as substrate or using flexible material as the oxygen of substrate
Change indium tin.
Embodiment seven：It is a kind of described in embodiment one can be thin to the NEW TYPE OF COMPOSITEs of visible near-infrared double regulation and control
In the preparation method of film, step 3, the conductive substrates alternately immerse the oxidation of the polyelectrolyte solution and negative electrical charge of positive charge
The tungsten nanomaterial solution time is 5~20min；In step 4, the polyelectrolyte that the plural layers alternately immerse positive charge is molten
The polyoxometallate solution min of liquid and negative electrical charge is 5~20min.
Embodiment eight：It is a kind of described in embodiment one can be thin to the NEW TYPE OF COMPOSITEs of visible near-infrared double regulation and control
In the preparation method of film, step 3, the number of plies for obtaining the polyelectrolyte and tungsten oxide nanometer material multilayer film is 5~50
It is double-deck.
Embodiment nine：It is a kind of described in embodiment one can be thin to the NEW TYPE OF COMPOSITEs of visible near-infrared double regulation and control
In the preparation method of film, step 4, the number of plies of the polyelectrolyte and polyoxometallate plural layers is obtained double for 5~50
Layer.
Embodiment 1：
(1) using [PW that deionized water configuration concentration is 0.1~10mg/mL12O40]3-(PW12) solution, concentration be 0.1~
10mg/mL W18O49Nanowire solution, concentration is 0.1~10mg/mL polyethyleneimine (PEI) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PEI solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in PW125~20min of solution, nitrogen
Cleaning is dried up, then is immersed in 5~20min in PEI solution, and nitrogen cleaning drying is repeated after 20 layers of assembling, and holding outermost layer is
PW12, structure is finally prepared for (PEI/W18O49)20(PEI/PW12)20Electrochromism composite film material；
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode)；
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Embodiment 2：
(1) using [P that deionized water configuration concentration is 0.1~10mg/mL2W18O62]6-(P2W18) solution, concentration is 0.1
~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polyethyleneimine
(PEI) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PEI solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in P2W185~20min of solution, nitrogen
Cleaning is dried up, then is immersed in 5~20min in PEI solution, and nitrogen cleaning drying is repeated after 20 layers of assembling, and holding outermost layer is
P2W18, structure is finally prepared for (PEI/W18O49)20(PEI/P2W18)20Electrochromism composite film material；
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode)；
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Embodiment 3：
(1) using [NaP that deionized water configuration concentration is 0.1~10mg/mL5W30O110]14-(P5W30) solution, concentration is
0.1~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polyethyleneimine
(PEI) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PEI solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in P5W305~20min of solution, nitrogen
Cleaning is dried up, then is immersed in 5~20min in PEI solution, and nitrogen cleaning drying is repeated after 20 layers of assembling, and holding outermost layer is
P5W30, structure is finally prepared for (PEI/W18O49)20(PEI/P5W30)20Electrochromism composite film material；
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode)；
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Embodiment 4：
(1) using [H that deionized water configuration concentration is 0.1~10mg/mL7P8W48O184]33-(P8W48) solution, concentration is
0.1~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polyethyleneimine
(PEI) solution；
(2) pretreated ito glass is submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then immerse
5~20min into PEI solution, nitrogen cleaning drying, repeats after 20 layers of assembling, is immersed in P8W485~20min of solution, nitrogen is clear
Drying is washed, then is immersed in 5~20min in PEI solution, nitrogen cleaning drying is repeated after 20 layers of assembling, and holding outermost layer is
P8W48, structure is finally prepared for (PEI/W18O49)20(PEI/P8W48)20Electrochromism composite film material；
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode) test result such as Fig. 2, cyclical stability test such as Fig. 3 and 4；
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light, test result such as Fig. 5.
Embodiment 5：
(1) using [H that deionized water configuration concentration is 0.1~10mg/mL7P8W48O184]33-(P8W48) solution, concentration is
0.1~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polyallyl ammonium
Hydrochloride (PAH) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PAH solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in P8W485~20min of solution, nitrogen
Cleaning is dried up, then is immersed in 5~20min in PAH solution, and nitrogen cleaning drying is repeated after 20 layers of assembling, and holding outermost layer is
P8W48, structure is finally prepared for (PAH/W18O49)20(PAH/P8W48)20Electrochromism composite film material.
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode).
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Embodiment 6：
(1) using [H that deionized water configuration concentration is 0.1~10mg/mL7P8W48O184]33-(P8W48) solution, concentration is
0.1~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polyallyl ammonium
Hydrochloride (PAH) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PAH solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in P8W485~20min of solution, nitrogen
Cleaning is dried up, then is immersed in 5~20min in PAH solution, and nitrogen cleaning drying is repeated after 30 layers of assembling, and holding outermost layer is
P8W48, structure is finally prepared for (PAH/W18O49)20(PAH/P8W48)30Electrochromism composite film material.
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode).
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Embodiment 7：
(1) using [H that deionized water configuration concentration is 0.1~10mg/mL7P8W48O184]33-(P8W48) solution, concentration is
0.1~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polydiene propyl group
Dimethyl Ammonium hydrochloride (PDDA) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PDDA solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in P8W485~20min of solution, nitrogen
Gas cleaning drying, then 5~20min in PDDA solution is immersed in, nitrogen cleaning drying repeats after 20 layers of assembling, keeps outermost layer
For P8W48, structure is finally prepared for (PDDA/W18O49)20(PDDA/P8W48)20Electrochromism composite film material.
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode).
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Embodiment 8：
(1) using [NaP that deionized water configuration concentration is 0.1~10mg/mL5W30O110]14-(P5W30) solution, concentration is
0.1~10mg/mL W18O49Nanowire solution (transmission electron microscope picture such as Fig. 1), concentration is 0.1~10mg/mL polyethyleneimine
(PEI) solution；
(2) pretreated conductive substrates are submerged initially in W18O495~20min in solution, nitrogen cleaning drying, then soak
Enter 5~20min into PEI solution, nitrogen cleaning drying repeats after 20 layers of assembling, is immersed in P5W305~20min of solution, nitrogen
Cleaning is dried up, then is immersed in 5~20min in PEI solution, and nitrogen cleaning drying is repeated after 5 layers of assembling, and holding outermost layer is
P5W30, structure is finally prepared for (PEI/W18O49)20(PEI/P5W30)5Electrochromism composite film material；
(3) with the electrochromic property of three-electrode system test compound thin-film material and its under different voltages to visible
(saturation Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, conduction for the transmitance change of light area and near-infrared region
Substrate is working electrode), such as Fig. 6 and Fig. 7；
(4) it is to electrode, the light source analogy sun by the conductive substrates to electrode, assembling composite construction of blank conductive substrates
Light, using optical filter it will be seen that light and near infrared light are distinguished respectively, test compound thin-film material is distinguished under the effect of different voltages
To the transmitance situation of change of visible ray and near infrared light.
Claims (9)
1. a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, it is characterised in that：Methods described has
Body step is as follows：
Step one：It is molten that the tungsten oxide nanometer material solution with negative electrical charge, the polyoxometallate with negative electrical charge are prepared respectively
Liquid and the polyelectrolyte solution with positive charge；
Step 2：Using conductive transparent material as substrate, conductive transparent material is sized and is cut into fritter, successively in third
Each ultrasonic 15min in ketone, isopropanol and water, each ultrasound is finished, and ultra-pure water is washed away except residual organic solvent, is preparedSolution, conductive transparent material is vertically placed in the solution, 80 DEG C of water-bath 1h, is taken out cold
But to room temperature, cleaned with ultra-pure water, N2Drying, conduction is placed in culture dish up, toluene 20mL steams again after is added, in gloves
300 μ LAPTES are taken out in case, are added in the culture dish, sealing lucifuge reaction 24h takes out conductive transparent material, toluene is abandoned
In waste liquid barrel, conductive transparent material acetone is cleaned by ultrasonic 3 times, and each 1min, ultra-pure water is cleaned, and is placed in 4 DEG C of preservations in ultra-pure water
It is standby；
Step 3：Conductive substrates are alternately immersed to the polyelectrolyte solution of positive charge and the tungsten oxide nanometer material solution of negative electrical charge
In, nitrogen drying obtains polyelectrolyte and tungsten oxide nanometer material multilayer film；
Step 4：By the plural layers, alternately the polyelectrolyte solution of immersion positive charge and the polyoxometallate of negative electrical charge are molten
In liquid, nitrogen drying prepares polyelectrolyte and polyoxometallate plural layers, finally given using conductive transparent material as substrate
Multi-layer compound film material, electrochromism test is carried out to it.
2. a kind of according to claim 1 can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, it is special
Levy and be：The compound method of described polyelectrolyte solution, tungsten oxide nanometer material solution and polyoxometallic acid salting liquid is：With
Deionized water dissolves polyelectrolyte, tungsten oxide nanometer material and polyoxometallate respectively, and above-mentioned three kinds of solution concentrations are 0.1
~10mg/mL.
3. it is according to claim 1 or claim 2 it is a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, its
It is characterised by：Described polyelectrolyte is polyethyleneimine, PAH or diallyl dimethyl ammonium salt acid
One kind in salt.
4. it is according to claim 1 or claim 2 it is a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, its
It is characterised by：Described tungsten oxide nanometer material is W18O49Nano wire, W18O49Nanosphere or W18O49One kind in nanoneedle.
5. it is according to claim 1 or claim 2 it is a kind of can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, its
It is characterised by：Described polyoxometallate is [PW12O40]3-、[P2W18O62]6-、[NaP5W30O110]14-Or [H7P8W48O184]33-
In one kind.
6. a kind of according to claim 1 can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, it is special
Levy and be：In step 2, the substrate is for the tin indium oxide using glass as substrate or using flexible material as the tin indium oxide of substrate.
7. a kind of according to claim 1 can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, it is special
Levy and be：In step 3, the conductive substrates alternately immerse the polyelectrolyte solution of positive charge and the tungsten oxide nanometer of negative electrical charge
The material solution time is 5~20min；In step 4, the plural layers alternately immerse the polyelectrolyte solution of positive charge with bearing
The polyoxometallate solution min of electric charge is 5~20min.
8. a kind of according to claim 1 can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, it is special
Levy and be：In step 3, it is 5~50 bilayers to obtain the number of plies of the polyelectrolyte and tungsten oxide nanometer material multilayer film.
9. a kind of according to claim 1 can be to the preparation method of the Novel compound film of visible near-infrared double regulation and control, it is special
Levy and be：In step 4, it is 5~50 bilayers to obtain the number of plies of the polyelectrolyte and polyoxometallate plural layers.
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| CN109233798A (en) * | 2018-07-17 | 2019-01-18 | 吉林化工学院 | A kind of composite material and preparation method and application |
| CN111025811A (en) * | 2019-09-25 | 2020-04-17 | 吉林化工学院 | Electrochromic film and preparation method and application thereof |
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| US20030031858A1 (en) * | 2001-08-01 | 2003-02-13 | Bernd Bronstert | Primer layers for EC windows |
| CN103575781A (en) * | 2012-07-18 | 2014-02-12 | 国家纳米科学中心 | Electrochemical sensor and its preparation method |
| CN106398208A (en) * | 2016-08-31 | 2017-02-15 | 西安电子科技大学 | Photosensitive composite thin film material and preparation method and application thereof |
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| US20030031858A1 (en) * | 2001-08-01 | 2003-02-13 | Bernd Bronstert | Primer layers for EC windows |
| CN103575781A (en) * | 2012-07-18 | 2014-02-12 | 国家纳米科学中心 | Electrochemical sensor and its preparation method |
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| CN109233798A (en) * | 2018-07-17 | 2019-01-18 | 吉林化工学院 | A kind of composite material and preparation method and application |
| CN109233798B (en) * | 2018-07-17 | 2021-09-24 | 吉林化工学院 | Composite material and preparation method and application thereof |
| CN111025811A (en) * | 2019-09-25 | 2020-04-17 | 吉林化工学院 | Electrochromic film and preparation method and application thereof |
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