CN116284850A - Preparation method of ionic hydrogel electrolyte, intelligent window device and preparation method of intelligent window device - Google Patents
Preparation method of ionic hydrogel electrolyte, intelligent window device and preparation method of intelligent window device Download PDFInfo
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- CN116284850A CN116284850A CN202211447577.8A CN202211447577A CN116284850A CN 116284850 A CN116284850 A CN 116284850A CN 202211447577 A CN202211447577 A CN 202211447577A CN 116284850 A CN116284850 A CN 116284850A
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- conductive substrate
- window device
- temperature
- electrolyte
- intelligent window
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
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- 239000002904 solvent Substances 0.000 claims abstract description 21
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 20
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 10
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 8
- 229920002379 silicone rubber Polymers 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical group CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 claims description 3
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- 229910000480 nickel oxide Inorganic materials 0.000 claims description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 3
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- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 3
- 230000006798 recombination Effects 0.000 claims description 2
- 238000005215 recombination Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 238000002834 transmittance Methods 0.000 abstract description 14
- 239000011245 gel electrolyte Substances 0.000 abstract description 11
- 230000009977 dual effect Effects 0.000 abstract description 10
- 230000005684 electric field Effects 0.000 abstract description 10
- 230000010354 integration Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 229920003213 poly(N-isopropyl acrylamide) Polymers 0.000 description 20
- 230000003287 optical effect Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
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- 229910052757 nitrogen Inorganic materials 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
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Abstract
The invention provides a preparation method of an ionic hydrogel electrolyte, a dual-response intelligent window device and a preparation method thereof. The ion hydrogel electrolyte prepared by the invention is ion hydrogel electrolyte with temperature response characteristic, PNIPAM temperature-sensitive gel has temperature sensitive characteristic and ion conductivity characteristic, and the PNIPAM temperature-sensitive gel is used as an electrolyte unit of an electrochromic intelligent window device, so that the characteristics of electric field and temperature driving of the intelligent window device can be simultaneously endowed, and the problems of low light transmittance, low conversion efficiency and the like caused by integration of a plurality of independent devices can be effectively avoided; the ionic conductivity of the PNIPAM thermosensitive gel electrolyte is endowed by adding a deep eutectic solvent; the ion hydrogel electrolyte can be used as a temperature response unit, can provide ion electrolyte for electrochromic materials, is applied to intelligent window devices, and can endow the intelligent window devices with a regulation mode of electric field-temperature dual response.
Description
Technical Field
The invention relates to the technical field of building energy conservation and intelligent regulation, in particular to a preparation method of an ion hydrogel electrolyte, an intelligent window device and a preparation method thereof.
Background
The building glass curtain wall (intelligent window) prepared based on the responsive materials (electricity, heat, magnetism and the like) can change the color and the light transmittance of the intelligent window through external stimulus, and then the radiation quantity of incident sunlight is regulated and controlled, so that the indoor vision and the thermal comfort are improved, and the building energy consumption is effectively reduced. Among them, the electrochromic intelligent window most typical in research has advantages of simple operation, rich colors, low driving voltage, etc., and is the first choice of the next generation intelligent window. However, the electrochromic intelligent window can only be actively regulated and controlled according to the requirement, and cannot respond spontaneously according to the change of the external environment temperature. In order to endow the intelligent window with an electric field and temperature dual-drive regulation mode and realize a new solar photo-thermal regulation technology, an intelligent window device with electric field-temperature dual-response needs to be constructed.
The electrochromic material realizes reversible conversion of color and optical performance under an external electric field, has the advantages of simple operation, rich colors, low driving voltage and the like, but the intelligent window device based on the material has single response mode, and is usually required to be compositely used with the material with temperature response in order to endow the material with the characteristics of electric field-temperature dual response. The main research ideas at present are as follows: (1) The electrochromic material and the vanadium dioxide thermochromic material are respectively used as electrodes to construct the intelligent window device. However, vanadium dioxide has high response temperature and intrinsic yellow color, and affects visual characteristics; (2) The (poly) ionic liquid electrolyte gel with temperature and electric field dual response characteristics is prepared, and an all-in-one device is constructed, so that the structure is simple, but the stability of organic matters is poor; (3) Poly (N-isopropyl acrylamide) temperature-sensitive polymer solution is added into the electrolyte, but the liquid electrolyte is easy to leak, and practical application is limited.
There is a need for improvements in smart window devices based on the current electric field-temperature dual response.
Disclosure of Invention
In view of the above, the invention provides a preparation method of an ionic hydrogel electrolyte, an intelligent window device and a preparation method thereof, so as to solve the technical defects in the prior art.
In a first aspect, the present invention provides a method for preparing an ionic hydrogel electrolyte, comprising the steps of:
mixing lithium chloride and acrylamide, and heating at 90-110 ℃ to obtain a deep eutectic solvent;
adding N-isopropyl acrylamide, sodium dodecyl sulfate, potassium persulfate or ammonium persulfate and di-tert-butyl peroxyisopropyl benzene into water, adding a deep eutectic solvent, stirring, adding tetramethyl ethylenediamine, and continuing stirring to obtain a gel precursor;
after the gel precursor is solidified, the ionic hydrogel electrolyte with temperature response characteristic is obtained.
Preferably, in the preparation method of the ionic hydrogel electrolyte, in the step of mixing lithium chloride and acrylamide, the mass ratio of the lithium chloride to the acrylamide is (1-3): 1-3;
in the step of preparing the hydrogel precursor, the mass ratio of the N-isopropyl acrylamide, the sodium dodecyl sulfate, the potassium persulfate or the ammonium persulfate, the di-tert-butyl peroxy isopropyl benzene, the water, the deep eutectic solvent and the tetramethyl ethylenediamine is (0.2-2.0): 0.005-0.05): 0.01-0.1): 0.02-0.2): 5-50): 0.05-0.5): 0.03-0.3;
in the step of curing the gel precursor, the curing temperature is 23-27 ℃ and the curing time is 0.5-1 h.
In a second aspect, the present invention also provides an intelligent window apparatus, including:
a first conductive substrate;
a second conductive substrate disposed opposite to the first conductive substrate;
the accommodating cavity is positioned between the first conductive substrate and the second conductive substrate, an accommodating cavity is formed by enclosing the first conductive substrate, the accommodating cavity and the second conductive substrate, and the accommodating cavity is filled with the ionic hydrogel electrolyte prepared by the preparation method;
and an electrochromic functional layer is arranged on one side surface of at least one of the first conductive substrate and the second conductive substrate, which is positioned in the accommodating cavity.
Preferably, in the smart window device, the temperature response range of the ionic hydrogel electrolyte with temperature response characteristics is 25-40 ℃.
Preferably, in the smart window device, the first conductive substrate and the second conductive substrate are any one of ITO conductive glass, FTO conductive glass or conductive PET.
Preferably, in the smart window device, the electrochromic functional layer is made of at least one of tungsten oxide, prussian blue, vanadium oxide and nickel oxide, and doped or compounded with the above materials;
and/or the accommodating cavity is made of silicon rubber.
In a third aspect, the present invention further provides a method for manufacturing the intelligent window device, including the following steps:
providing a first conductive substrate, a second conductive substrate and a containing cavity;
preparing an electrochromic functional layer on at least one side of the first conductive substrate and the second conductive substrate;
and enclosing the first conductive substrate, the second conductive substrate and the accommodating cavity to form an accommodating cavity, and injecting the ion hydrogel electrolyte with temperature response characteristic into the accommodating cavity.
Preferably, in the method for manufacturing a smart window device, the electrochromic functional layer is made of tungsten oxide, and the step of manufacturing the electrochromic functional layer on at least one side of the first conductive substrate and the second conductive substrate specifically includes:
will H 2 WO 4 Adding to water, then adding H 2 O 2 Stirring to obtain a mixed solution;
adding HCl and acetonitrile into the mixed solution, and stirring to obtain a tungsten oxide precursor solution;
placing the first conductive substrate or the second conductive substrate in tungsten oxide precursor solution to react for 20-30 h at 170-190 ℃ to form WO 3 A film.
Preferably, in the step of preparing the mixed solution by the preparation method of the intelligent window device, H 2 WO 4 、H 2 O 2 The mass volume ratio of water is (1-2) g (20-40) mL (30-90) mL; the H is 2 O 2 The mass concentration of (2) is 25-30%;
in the step of preparing the tungsten oxide precursor solution, the volume ratio of the mixed solution to the HCl to the acetonitrile is (5-15): 1-3): 30-50, and the concentration of the HCl is 6-12M.
Preferably, in the method for manufacturing the intelligent window device, before the first conductive substrate or the second conductive substrate is placed in the tungsten oxide precursor solution, ultrasonic cleaning is performed on the first conductive substrate or the second conductive substrate sequentially in acetone, ethanol and deionized water.
The preparation method of the ionic hydrogel electrolyte, the intelligent window device and the preparation method thereof have the following beneficial effects compared with the prior art:
1. the ion hydrogel electrolyte prepared by the invention is ion hydrogel electrolyte with temperature response characteristic, PNIPAM temperature-sensitive gel has temperature sensitive characteristic and ion conductivity characteristic, and the PNIPAM temperature-sensitive gel is used as an electrolyte unit of an electrochromic intelligent window device, so that the characteristics of electric field and temperature driving of the intelligent window device can be simultaneously endowed, and the problems of low light transmittance, low conversion efficiency and the like caused by integration of a plurality of independent devices can be effectively avoided; the ionic conductivity of the PNIPAM thermosensitive gel electrolyte is endowed by adding a deep eutectic solvent; the ionic hydrogel electrolyte can be used as a temperature response unit, can provide ionic electrolyte for electrochromic materials, is applied to intelligent window devices, and can endow the intelligent window devices with a regulation and control mode of electric field-temperature dual response;
2. according to the intelligent window device, the poly (N-isopropyl acrylamide) (PNIPAM) temperature-sensitive gel is used as an electrolyte, so that the problems of low light transmittance and the like caused by integration of a plurality of independent devices can be effectively avoided, high optical modulation is realized, and the driving voltage is low; the response temperature of the ionic hydrogel based on PNIPAM is near room temperature, and the decolored state is a colorless transparent state, so that high optical modulation is realized near room temperature; the deep eutectic solvent is a green solvent with excellent conductivity, and the PNIPAM gel electrolyte prepared by using the deep eutectic solvent can endow the PNIPAM gel electrolyte with high conductive property, so that the response rate, the coloring efficiency and the like of the device are improved; the intelligent window device based on PNIPAM temperature-sensitive gel electrolyte prepared by the invention has the dual response characteristics of electric field driving and room temperature spontaneous regulation;
3. according to the preparation method of the intelligent window device, the used raw materials are all common materials which are mature in commercial production, and the intelligent window device is low in price, sufficient in raw materials and environment-friendly; the adopted preparation method has the characteristics of simplicity, high efficiency, safety and the like, has low technical difficulty and has industrial large-scale application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is evident that the drawings in the following description are only some embodiments of the present invention and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a schematic diagram of a smart window device of the present invention;
FIG. 2 is a scanning electron microscope image of the ionic hydrogel electrolyte prepared in example 1;
FIG. 3 is a graph showing the AC impedance spectrum of the ionic hydrogel electrolyte prepared in example 1 at high and low temperatures;
FIG. 4 is a graph showing the change in transmittance with temperature at a wavelength of 550nm of the ionic hydrogel electrolyte prepared in example 1;
FIG. 5 is a graph showing light transmittance in four states of the smart window device prepared in example 2;
fig. 6 is an optical photograph of the smart window device prepared in example 2 in four states.
Detailed Description
The following description of the embodiments of the present invention will be made in detail and with reference to the embodiments of the present invention, but it should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
The application provides a preparation method of an ionic hydrogel electrolyte, which comprises the following steps:
s1, mixing lithium chloride and acrylamide, and heating at 90-110 ℃ to obtain a deep eutectic solvent;
s2, adding N-isopropyl acrylamide, sodium dodecyl sulfate, potassium persulfate or ammonium persulfate and di-tert-butyl peroxyisopropyl benzene into water, adding a deep eutectic solvent, stirring, adding tetramethyl ethylenediamine, and continuing stirring to obtain a gel precursor;
s3, after the gel precursor is solidified, the ionic hydrogel electrolyte with temperature response characteristic is obtained. In some embodiments, in the step of mixing lithium chloride and acrylamide, the mass ratio of lithium chloride to acrylamide is (1-3): 1-3;
in the step of preparing the hydrogel precursor, the mass ratio of the N-isopropyl acrylamide, the sodium dodecyl sulfate, the potassium persulfate or the ammonium persulfate, the di-tert-butyl peroxy isopropyl benzene, the water, the deep eutectic solvent and the tetramethyl ethylenediamine is (0.2-2.0): 0.005-0.05): 0.01-0.1): 0.02-0.2): 5-50): 0.05-0.5): 0.03-0.3;
in the step of curing the gel precursor, the curing temperature is 23-27 ℃ and the curing time is 0.5-1 h.
The ionic hydrogel electrolyte prepared by the method is the ionic hydrogel electrolyte with temperature response characteristics, can be used as a temperature response unit, can provide the ionic electrolyte for electrochromic materials, is applied to intelligent window devices, and can be endowed with an electric field-temperature dual-response regulation and control mode.
Specifically, in the step S2, water is placed in a beaker, nitrogen (about 5-10 min) is introduced into the beaker to remove dissolved oxygen, then N-isopropyl acrylamide (NIPAM), sodium Dodecyl Sulfate (SDS), BIS-tert-butyl peroxyisopropyl Benzene (BIS), potassium persulfate or ammonium persulfate, and the prepared deep eutectic solvent are added into the beaker, and after stirring until the materials are dissolved, a proper amount of catalyst tetramethyl ethylenediamine (TEMED) is removed, and stirring is continued to obtain a gel precursor.
Based on the same inventive concept, the embodiment of the present application further provides an intelligent window device, as shown in fig. 1, including:
a first conductive substrate 1;
a second conductive substrate 2 disposed opposite to the first conductive substrate 1;
the accommodating cavity 3 is positioned between the first conductive substrate 1 and the second conductive substrate 2, an accommodating cavity 31 is formed by enclosing the first conductive substrate 1, the accommodating cavity 3 and the second conductive substrate 2, and the accommodating cavity 31 is filled with the ionic hydrogel electrolyte 4 prepared by the preparation method;
wherein, at least one of the first conductive substrate 1 and the second conductive substrate 2 is provided with an electrochromic functional layer 5 on one side surface in the accommodating cavity.
In some embodiments, the ionic hydrogel electrolyte having temperature response characteristics has a temperature response in the range of 25 to 40 ℃.
In some embodiments, the first conductive substrate 1, the second conductive substrate 2 employ any one of ITO conductive glass, FTO conductive glass, or conductive PET.
In some embodiments, the material used for the electrochromic functional layer 5 includes at least one of tungsten oxide, prussian blue, vanadium oxide, nickel oxide, and doping or recombination of the above.
In some embodiments, the material used for the receiving cavity 3 is silicone rubber. Specifically, a silicone rubber ring is adopted, the silicone rubber ring is in a hollow cylinder structure, the first conductive substrate 1 and the second conductive substrate 2 are separated from each other by the silicone rubber ring, and the silicone rubber ring is respectively abutted against the first conductive substrate 1 and the second conductive substrate 2 to form a containing chamber 31.
Based on the same inventive concept, the embodiment of the application also provides a preparation method of the intelligent window device, which comprises the following steps:
s1, providing a first conductive substrate, a second conductive substrate and a containing cavity;
s2, preparing an electrochromic functional layer on at least one side surface of the first conductive substrate and the second conductive substrate;
s3, enclosing the first conductive substrate, the second conductive substrate and the accommodating cavity to form an accommodating cavity, and injecting the ion hydrogel electrolyte with temperature response characteristic into the accommodating cavity.
In some embodiments, the electrochromic functional layer is made of tungsten oxide, and the preparation of the electrochromic functional layer on at least one side of the first conductive substrate and the second conductive substrate specifically includes:
s21, H 2 WO 4 Adding to water, then adding H 2 O 2 Stirring to obtainA mixed solution;
s22, adding HCl and acetonitrile into the mixed solution, and stirring to obtain a tungsten oxide precursor solution;
s23, placing the first conductive substrate or the second conductive substrate in a tungsten oxide precursor solution to react for 20-30 hours at 170-190 ℃ to form WO 3 A film.
In some embodiments, in the step of preparing the mixed solution, H 2 WO 4 、H 2 O 2 The mass volume ratio of water is (1-2) g (20-40) mL (30-90) mL; h 2 O 2 The mass concentration of (2) is 25-30%;
in the step of preparing the tungsten oxide precursor solution, the volume ratio of the mixed solution to the HCl to the acetonitrile is (5-15): 1-3): 30-50, and the concentration of the HCl is 6-12M.
In some embodiments, prior to placing the first conductive substrate or the second conductive substrate in the tungsten oxide precursor solution, further comprising, sequentially placing the first conductive substrate or the second conductive substrate in acetone, ethanol, and deionized water for ultrasonic cleaning.
In some embodiments, preparing the electrochromic functional layer on at least one side of the first conductive substrate, the second conductive substrate specifically includes:
s21, 1 to 2 portions 2g H 2 WO 4 Adding into 25-35 mL of water, then adding 20-40 mL of H with mass concentration of 25-30% 2 O 2 Heating and stirring for 20-40 min at 90-110 ℃ to obtain a clear solution, continuously adding 50-70 mL of water, and stirring to obtain a mixed solution;
s22, taking 5-20 mL of mixed solution, adding 1-3 mL of HCl solution with the mass concentration of 10-15M and 30-50 mL of acetonitrile into the mixed solution, and stirring to obtain tungsten oxide precursor solution;
s23, placing the first conductive substrate or the second conductive substrate in a tungsten oxide precursor solution to react for 20-30 hours at 170-190 ℃ to form WO 3 A film.
According to the preparation method of the intelligent window device, the used raw materials are common materials which are mature in commercial production, and the intelligent window device is low in price, sufficient in raw materials and environment-friendly; the adopted preparation method has the characteristics of simplicity, high efficiency, safety and the like, has low technical difficulty and has industrial large-scale application prospect; the intelligent window device prepared by the method has the following advantages and characteristics: poly (N-isopropyl acrylamide) (PNIPAM) temperature-sensitive gel is used as electrolyte, so that the problems of low light transmittance and the like caused by integration of a plurality of independent devices can be effectively avoided, high optical modulation is realized, and driving voltage is low; the response temperature of the ionic hydrogel based on PNIPAM is near room temperature, and the decolored state is a colorless transparent state, so that high optical modulation is realized near room temperature; the deep eutectic solvent is a green solvent with excellent conductivity, and the PNIPAM gel electrolyte prepared by using the deep eutectic solvent can endow the PNIPAM gel electrolyte with high conductive property, so that the response rate, the coloring efficiency and the like of the device are improved; the intelligent window device based on the PNIPAM temperature-sensitive gel electrolyte prepared by the method has the dual response characteristics of electric field driving and room temperature spontaneous regulation; the PNIPAM thermosensitive gel prepared by the method has thermosensitive property and ionic conductivity, is used as an electrolyte unit of an electrochromic intelligent window device, can simultaneously endow the intelligent window device with electric field and temperature driving property, and can effectively avoid the problems of low light transmittance, low conversion efficiency and the like caused by integration of a plurality of independent devices; the composition of a hydrogen bond donor and a hydrogen bond acceptor in the deep eutectic solvent is regulated to endow the PNIPAM temperature-sensitive gel electrolyte with ionic conductivity, and the mechanical strength is improved. The phase transition temperature of PNIPAM is regulated and controlled by optimizing the proportion of comonomer and SDS, and the adjustability of PNIPAM near room temperature is maintained.
The method of preparing the ionic hydrogel electrolyte, the smart window device and the method of preparing the same of the present application are further described in specific examples below. This section further illustrates the summary of the invention in connection with specific embodiments, but should not be construed as limiting the invention. The technical means employed in the examples are conventional means well known to those skilled in the art, unless specifically stated. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Example 1
The embodiment of the application provides a preparation method of an ionic hydrogel electrolyte, which comprises the following steps:
s1, mixing lithium chloride and acrylamide according to a mass ratio of 1:2, and heating at 100 ℃ to obtain a deep eutectic solvent;
s2, placing 30mL of deionized water in a beaker, introducing nitrogen into the beaker for 10min to remove dissolved oxygen, then adding 1.0g N-isopropyl acrylamide (NIPAM), 0.05g of Sodium Dodecyl Sulfate (SDS), 0.1g of di-tert-butyl peroxyisopropyl Benzene (BIS), 0.03g of potassium persulfate and 0.1g of deep eutectic solvent prepared in the step S1 into the beaker, stirring until the materials are dissolved, and then removing 0.3g of catalyst tetramethyl ethylenediamine (TEMED), and continuing stirring for 5min to obtain a gel precursor;
s3, curing the gel precursor for 1h at 25 ℃ to obtain the ionic hydrogel electrolyte with temperature response characteristics.
Example 2
The embodiment of the application provides a preparation method of an intelligent window device, which comprises the following steps:
s1, providing a first conductive substrate, a second conductive substrate and a containing cavity; the first conductive substrate and the second conductive substrate are FTO transparent conductive glass, and the accommodating cavity is a silicone rubber ring with a hollow cylinder structure;
s2, sequentially placing the first conductive substrate or the second conductive substrate in acetone, ethanol and deionized water for ultrasonic cleaning, wherein the ultrasonic cleaning time is 5min each time, and drying by using nitrogen after ultrasonic treatment for later use;
s3, will 1.25g H 2 WO 4 Added into 30mL of deionized water, and then added into 30mL of 30% H by mass concentration 2 O 2 Heating and stirring for 30min at 100deg.C to obtain clear solution, continuously adding 60mL deionized water, and stirring to obtain mixed solution;
s4, taking 10mL of mixed solution, adding 2mL of 12M HCl solution and 40mL of acetonitrile to the mixed solution, and stirring to obtain tungsten oxide precursor solution;
s5, respectively placing the first conductive substrate and the second conductive substrate in a tungsten oxide precursor solution to react for 24 hours at 180 ℃ so as to form WO on the surfaces of the first conductive substrate and the second conductive substrate 3 A film;
s6, enclosing the first conductive substrate, the second conductive substrate and the accommodating cavity to form an accommodating cavity, and injecting the ion hydrogel electrolyte with the temperature response characteristic, which is prepared in the embodiment 1, into the accommodating cavity.
Performance testing
Fig. 2 is a scanning electron microscope image of the ionic hydrogel electrolyte prepared in example 1, and it can be seen from fig. 2 that the ionic hydrogel electrolyte prepared in example 1 has a large porosity and satisfies the migration condition of ions.
The ionic hydrogel electrolyte prepared in example 1 was tested for ac impedance spectra at room temperature (25 ℃) and high temperature (60 ℃) respectively, and the results are shown in fig. 3. Specifically, the ionic hydrogel electrolyte prepared in example 1 was sandwiched between stainless steel plates for electrochemical impedance spectroscopy. The gel electrolyte was 40mm in size (length). Times.40 mm in width). Times.4 mm in thickness, and the frequency range of the test was 0.1 to 1MHz.
As can be seen from fig. 3, the ionic hydrogel electrolyte has good ionic conductivity at both high and low temperatures.
The change in transmittance at 550nm with temperature of the ionic hydrogel electrolyte prepared in test example 1 is shown in fig. 4. Specifically, the ionic hydrogel electrolyte prepared in example 1 was sandwiched between two pieces of transparent glass, and a temperature-driven light transmittance test was performed using a spectrophotometer and a heating stage. The gel electrolyte was 40mm (length) ×40mm (width) ×2mm (thickness), and the temperature range for the test was 25 to 45℃and the test wavelength was 550nm.
As can be seen from fig. 4, the ionic hydrogel electrolyte obtained in the present invention can undergo a significant change in light transmittance upon temperature driving, and the phase transition temperature is 33.6 ℃, thus enabling optical modulation around room temperature.
The transmittance curves of the smart window device prepared in example 2 under four conditions (specifically, the transmittance curves of the device under different temperatures and voltages were measured using a spectrophotometer) were tested, and the results are shown in fig. 5. In FIG. 5, the room temperature is 25 ℃, the high temperature is 60 ℃, the coloring voltage is 2.3V, and the decoloring voltage is-2.3V;
as can be seen from fig. 5, the intelligent window device obtained by the invention can respectively show different spectral transmittance characteristics under the driving of an electric field and temperature, so as to realize larger optical modulation.
The optical photographs of the smart window device prepared in example 2 in four states are shown in fig. 6, wherein a, b, c, d in fig. 6 is room temperature transparent/voltage decolored, room temperature transparent/voltage colored (blue), high temperature white/voltage decolored, high temperature white/voltage colored (blue), respectively.
As can be seen from fig. 6, the smart window device obtained in the invention can realize four optical states, namely a colorless transparent state (a in fig. 6), a blue transparent state (b in fig. 6), a white opaque state (c in fig. 6) and a blue opaque state (d in fig. 6) under the driving of temperature and an electric field, so that solar spectrum modulation under different driving can be realized.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. A method for preparing an ionic hydrogel electrolyte, comprising the steps of:
mixing lithium chloride and acrylamide, and heating at 90-110 ℃ to obtain a deep eutectic solvent;
adding N-isopropyl acrylamide, sodium dodecyl sulfate, potassium persulfate or ammonium persulfate and di-tert-butyl peroxyisopropyl benzene into water, adding a deep eutectic solvent, stirring, adding tetramethyl ethylenediamine, and continuing stirring to obtain a gel precursor;
after the gel precursor is solidified, the ionic hydrogel electrolyte with temperature response characteristic is obtained.
2. The method for producing an ionic hydrogel electrolyte according to claim 1, wherein in the step of mixing lithium chloride and acrylamide, the mass ratio of lithium chloride to acrylamide is (1-3): 1-3;
in the step of preparing the hydrogel precursor, the mass ratio of the N-isopropyl acrylamide, the sodium dodecyl sulfate, the potassium persulfate or the ammonium persulfate, the di-tert-butyl peroxy isopropyl benzene, the water, the deep eutectic solvent and the tetramethyl ethylenediamine is (0.2-2.0): 0.005-0.05): 0.01-0.1): 0.02-0.2): 5-50): 0.05-0.5): 0.03-0.3;
in the step of curing the gel precursor, the curing temperature is 23-27 ℃ and the curing time is 0.5-1 h.
3. An intelligent window device, comprising:
a first conductive substrate;
a second conductive substrate disposed opposite to the first conductive substrate;
the accommodating cavity is positioned between the first conductive substrate and the second conductive substrate, an accommodating cavity is formed by enclosing the first conductive substrate, the accommodating cavity and the second conductive substrate, and the accommodating cavity is filled with the ion hydrogel electrolyte prepared by the preparation method of claim 1;
and an electrochromic functional layer is arranged on one side surface of at least one of the first conductive substrate and the second conductive substrate, which is positioned in the accommodating cavity.
4. The smart window device of claim 3, wherein the ionic hydrogel electrolyte having a temperature response characteristic has a temperature response in the range of 25 to 40 ℃.
5. A smart window device as recited in claim 3, wherein the first and second conductive substrates are any one of ITO conductive glass, FTO conductive glass, or conductive PET.
6. The smart window device of claim 3, wherein the electrochromic functional layer comprises at least one of tungsten oxide, prussian blue, vanadium oxide, nickel oxide, and a doping or recombination thereof;
and/or the accommodating cavity is made of silicon rubber.
7. A method of manufacturing an intelligent window device according to any one of claims 2 to 6, comprising the steps of:
providing a first conductive substrate, a second conductive substrate and a containing cavity;
preparing an electrochromic functional layer on at least one side of the first conductive substrate and the second conductive substrate;
and enclosing the first conductive substrate, the second conductive substrate and the accommodating cavity to form an accommodating cavity, and injecting the ion hydrogel electrolyte with temperature response characteristic into the accommodating cavity.
8. The method for manufacturing a smart window device according to claim 7, wherein the electrochromic functional layer is made of tungsten oxide, and the step of manufacturing the electrochromic functional layer on at least one side of the first conductive substrate and the second conductive substrate specifically comprises:
will H 2 WO 4 Adding to water, then adding H 2 O 2 Stirring to obtain a mixed solution;
adding HCl and acetonitrile into the mixed solution, and stirring to obtain a tungsten oxide precursor solution;
placing the first conductive substrate or the second conductive substrate in tungsten oxide precursor solution to react for 20-30 h at 170-190 ℃ to form WO 3 A film.
9. The method of manufacturing a smart window device of claim 8, wherein in the step of preparing the mixed solution, H 2 WO 4 、H 2 O 2 The mass volume ratio of water is (1-2) g (20-40) mL (30-90) mL; the H is 2 O 2 The mass concentration of (2) is 25-30%;
in the step of preparing the tungsten oxide precursor solution, the volume ratio of the mixed solution to the HCl to the acetonitrile is (5-15): 1-3): 30-50, and the concentration of the HCl is 6-12M.
10. The method of manufacturing a smart window device of claim 8, wherein prior to placing the first conductive substrate or the second conductive substrate in the tungsten oxide precursor solution, further comprising sequentially placing the first conductive substrate or the second conductive substrate in acetone, ethanol, and deionized water for ultrasonic cleaning.
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