CN110451817B - Intelligent window film based on vanadium dioxide and metamaterial structure and preparation method thereof - Google Patents
Intelligent window film based on vanadium dioxide and metamaterial structure and preparation method thereof Download PDFInfo
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- CN110451817B CN110451817B CN201910699510.5A CN201910699510A CN110451817B CN 110451817 B CN110451817 B CN 110451817B CN 201910699510 A CN201910699510 A CN 201910699510A CN 110451817 B CN110451817 B CN 110451817B
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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
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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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
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
-
- 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
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/155—Deposition methods from the vapour phase by sputtering by reactive sputtering
Abstract
The invention discloses an intelligent window film based on vanadium dioxide and a metamaterial structure and a preparation method thereof, wherein the intelligent window film sequentially comprises a bottom vanadium dioxide thin film layer, a medium thin film layer and a top vanadium dioxide thin film layer with a porous metamaterial structure from bottom to top, and the high-T window film is realized by fully utilizing the phase change characteristic of a vanadium dioxide material and the resonance absorption characteristic of the metamaterial structurelum(50.4%), high Δ Tsol(22.8%) of the intelligent window film layer is beneficial to the application in the field of intelligent windows.
Description
Technical Field
The invention belongs to the field of functional thin film materials, and particularly relates to an intelligent window film based on vanadium dioxide and a metamaterial structure and a preparation method thereof.
Background
Vanadium dioxide (VO)2) Is a typical thermal insulator-metal phase change material and is used for VO2Thin film studies have shown that vanadium dioxide undergoes a reversible structural transition from the monoclinic phase (M phase, infrared radiation transmission) to the rutile phase (R phase, infrared radiation reflection) under thermal excitation. The phase transition temperature is about 68 ℃, and the change of the electrical and optical properties is brought along with the 3-5 orders of magnitude change of the resistance. Due to VO2The great change of physical properties before and after phase change makes VO2Becomes an excellent material for the thermochromic intelligent coating.
The metamaterial is an artificial composite structure and is formed by periodically arranging natural materials in a sub-wavelength unit structure. The electromagnetic parameters of the metamaterial mainly depend on the equivalent dielectric constant epsilon and the equivalent permeability mu of the basic unit. By adjusting the structural parameters of the metamaterial, any epsilon and mu can be obtained theoretically, and special physical phenomena can occur when the metamaterial resonates with electromagnetic waves, so that the specific function is realized.
The intelligent window applies special color-changing materials to a lighting system of buildings or automobiles and the like so as to realize dynamic adjustment of the solar energy transmittance. The transparent to opaque state of near infrared radiation can be realized by utilizing the thermochromic intelligent coating so as to respond to the change of the ambient temperature from low to high, and the process does not need additional excitation, so that the energy consumption can be saved.
In the research of the intelligent window film based on vanadium dioxide, a plurality of improving methods such as adding a buffer layer, an antireflection layer and a multilayer structure are available at present. For example, Powell MJ et al obtained a.DELTA.T of 15.29% by adding an anti-reflective layersolBut T islumOnly 18% [ chem.mater.,2016,28(5), pp 1369-](ii) a Mlyuka NR et al prepared VO-based2And TiO2The multilayer structure obtained a.DELTA.T of 12.1%solAnd 45% of Tlum[Solar Energy Mater Solar Cells 93(9):1685-1687]However, there is still a gap between the actual application requirements. In addition, Zhou, Min et al achieved a high T of 70.2% by preparing a porous filmlumBut its Δ TsolOnly 7.9% [ chem.Commun.2013,49,6021-](ii) a Shuniang Dou et al prepared VO2A high T of 75.5% is obtained for a particular microstructure oflumBut Δ TsolOnly 7.7% [ Solar Energy Materials&Solar Cells 160(2017):164-173]. The patent number is CN109207929A, the name is a porous periodic vanadium dioxide structure and a preparation method thereof, and nano-particle VO is prepared2Structure, 60.1% of T is obtainedlumAnd Δ T thereofsolOnly 9.2%; the patent number is CN104250068A, the name is a vanadium dioxide-based film system for an intelligent energy-saving window and a preparation method thereof, a vanadium dioxide-based multilayer film system structure is prepared, and 46.3 percent of T is obtainedlumHowever, the difference in transmittance (Δ T) between high and low temperatures is around 2.5um2.5μm) It is only 40.2%.
Disclosure of Invention
The invention aims to: solves the problem of difficulty in simultaneously ensuring the existence of vanadium dioxide-based intelligent window filmHigh TlumAnd higher Δ TsolThe invention provides an intelligent window film based on vanadium dioxide and a metamaterial structure.
The invention also aims to provide a preparation method of the intelligent window film based on the vanadium dioxide and metamaterial structure.
The technical scheme adopted by the invention is as follows:
the utility model provides an intelligence window membrane based on vanadium dioxide and metamaterial structure which characterized in that, intelligence window membrane from the bottom up includes bottom vanadium dioxide thin layer, medium thin layer and top layer have the vanadium dioxide thin layer of poroid metamaterial structure in proper order.
Preferably, circular holes with the diameter 2R of 0.8-1.2 μm are distributed on the vanadium dioxide thin film layer of the metamaterial structure, and the value range of the distance d between adjacent circular holes on the vanadium dioxide thin film layer of the metamaterial structure is 1000-1600 nm.
Preferably, the thickness of the vanadium dioxide thin film layer of the metamaterial structure is 90-280 nm.
Preferably, the thickness of the bottom vanadium dioxide thin film layer is 30-80nm, and the thickness of the medium thin film layer is 50-150 nm.
Preferably, the material of the dielectric thin film layer is TiO2、Al2O3、SiNxAnd SiO2One or more of them.
A preparation method of an intelligent window film based on vanadium dioxide and metamaterial structures is characterized by comprising the following steps:
(1) cleaning a substrate;
(2) preparing a bottom vanadium dioxide thin film layer;
(3) preparing a dielectric thin film layer on the bottom vanadium dioxide thin film layer;
(4) uniformly spraying polystyrene microspheres with the diameter of 0.8-1.2 mu m onto the dielectric film layer prepared in the step (3) by adopting an air spraying method;
(5) preparing a vanadium dioxide thin film layer with a metamaterial structure on the medium thin film layer sprayed with the polystyrene microspheres;
(6) and removing the polystyrene microspheres by using an acetone solution and ultrasonic treatment, and preparing the vanadium dioxide film with the round-hole-shaped metamaterial structure on the top layer.
Preferably, in the step (2), the adopted preparation method is one or more of sputtering, vacuum evaporation, sol-gel and vapor deposition; in the step (3), the adopted preparation method is one or more of sputtering, vacuum evaporation, sol-gel and vapor deposition; in the step (5), the adopted preparation method is one or more of sputtering, vacuum evaporation, sol-gel and vapor deposition processes.
Preferably, in the step (4), the dispersion or the diluent of the polystyrene microspheres with the diameter of 0.8-1.2 μm is compressed by high-pressure gas through a gas spraying method to form an aerosol carrying the microspheres, and the aerosol is uniformly sprayed on the dielectric layer.
Preferably, the thickness of the bottom layer vanadium dioxide film layer is 30-80 nm; the thickness of the dielectric thin film layer is 50-150 nm; the thickness of the vanadium dioxide thin film layer of the metamaterial structure is 90-280 nm.
Preferably, the material of the substrate in the step (1) is common glass or quartz glass.
An intelligent window film based on a vanadium dioxide and metamaterial structure is based on the principle that an external temperature change is utilized to excite a vanadium dioxide film to generate reversible phase change from a semiconductor state to a metal state, and the infrared transmittance of the vanadium dioxide film is correspondingly greatly changed.
Firstly, in a semiconductor state, for a visible light section, the visible light section passes through a vanadium dioxide thin film layer with a hole-shaped metamaterial structure on the top layer with a specific thickness, so that the optical path is an integral multiple of half-wavelength, and is in a high transmittance state, and the refractive index of a medium thin film layer is smaller than that of a material of a bottom vanadium dioxide thin film layer, and an anti-reflection effect is realized; for the near infrared band, the vanadium dioxide film is in a high transmittance state, so that high visible light transmittance and high near infrared transmittance can be obtained.
Secondly, in a metal state, for a visible light section, the state that the vanadium dioxide thin film layer with the porous metamaterial structure on the top layer penetrates through and the medium thin film layer is anti-reflection is still shown; for near infrared wave bands, the bottom vanadium dioxide thin film layer is in a low transmittance state, and due to the resonance effect of the vanadium dioxide thin film layer with the metamaterial structure, the near infrared transmittance is greatly reduced, so that high visible light transmittance and extremely low near infrared transmittance can be obtained.
Based on the above principle, the dielectric thin film material can be selected to be TiO with similar properties2、Al2O3、SiNxAnd SiO2And the substrate can be selected from common glass or quartz glass with similar properties, and the effects can still be ensured.
In summary, compared with the prior art, the invention has the beneficial effects that:
1. the final expression result of the structure designed by the invention is that the visible light band has higher transmittance, and the near infrared band is VO2And a huge transmittance difference value exists before and after the phase change, so that strong solar spectrum modulation capability is brought. Compared with the research results, the invention has the advantages of ensuring higher TlumAnd greatly increases Δ TsolAnd the method has wide application prospect in the aspect of intelligent windows.
2. The invention has the beneficial effects that the phase change characteristic of the vanadium dioxide material and the resonance absorption characteristic of the metamaterial structure are fully utilized, and the high T is realizedlum(50.4%), high Δ Tsol(22.8%) of a smart window film layer.
Drawings
FIG. 1 is a schematic process flow diagram of the process of the present invention;
FIG. 2 is a front view of a portion of a cell structure of a smart window film designed in accordance with the present invention;
FIG. 3 is a top plan view of a portion of a cell structure of a smart window film designed in accordance with the present invention;
FIG. 4 is a graph of simulation results for a structure without a top layer of metamaterial (example 3); the dotted line is the semiconductor state M and the solid line is the metal state R;
FIG. 5 is a graph of simulation results under the optimized parameters in embodiment 1; the dotted line is the semiconductor state M and the solid line is the metal state R;
FIG. 6 is a graph showing simulation results of different values of the distance d between adjacent circular holes; the dotted line is the semiconductor state M and the solid line is the metal state R;
labeled as: 1-a bottom vanadium dioxide thin film layer, 2-a dielectric thin film layer, 3-a vanadium dioxide thin film layer with a metamaterial structure and 4-a substrate.
Detailed Description
All features disclosed in this specification may be combined in any combination, except features and/or steps that are mutually exclusive.
Visible light transmittance (T)lum) And higher solar spectral modulation capability (Δ T)sol) Are key performance indicators for smart window films, which are defined by the following calculation formula (I):
Tlum,sol＝∫Φlum,sol(λ)T(λ)dλ/∫Φlum,sol(λ)dλ
ΔTsol＝Tsol,lt-Tsol,ht
wherein, Tlum,solRespectively representing the transmission in the visible range and the whole solar spectrum, philum,sol(lambda) represents the standard efficiency function of photopic vision and the solar irradiance spectrum with an air mass of 1.5 for the corresponding wavelength, respectively, T (lambda) represents the transmittance of the sample at the corresponding wavelength, Tsol,ltDenotes the transmittance, T, over the entire solar spectral range at low temperaturessol,htIndicating the transmittance over the entire solar spectral range at high temperature.
The present invention will be described in detail with reference to FIGS. 1 to 6.
Example 1
The purpose of the invention is realized by the following technical scheme: the utility model provides an intelligence window membrane based on vanadium dioxide and metamaterial structure, intelligence window membrane from the bottom up includes bottom vanadium dioxide thin layer 1, medium thin layer 2 and top layer have the vanadium dioxide thin layer 3 of poroid metamaterial structure in proper order.
The method specifically comprises the following steps:
(1) using a common glass substrate 4: scrubbing a common glass substrate 4, putting the cleaned common glass substrate into acetone, performing ultrasonic treatment for 30min to remove surface impurities, then respectively putting the cleaned common glass substrate into absolute ethyl alcohol and deionized water, performing ultrasonic treatment for 30min to remove residues, finally putting the cleaned common glass substrate into the absolute ethyl alcohol for storage, and using the cleaned common glass substrate before useHigh purity N2Drying;
(2) sputtering a bottom vanadium dioxide thin film layer 1, wherein the specific process conditions are as follows:
target material: a metal vanadium target; background vacuum degree: less than 2 x 10-3Pa; the working gas is argon and oxygen; sputtering temperature: 60 ℃; ar flow rate in sputtering process: 98 sccm; o in sputtering process2Flow rate: 2sccm, sputtering current: 0.34A; sputtering to a thickness of 30nm, and annealing at 400 ℃ for 15 minutes;
(3) sputtering dielectric film layer 2TiO2The specific process conditions of the film are as follows:
target material: a metallic titanium target; background vacuum degree: less than 2 x 10-3Pa; the working gas is argon and oxygen; sputtering temperature: 150 ℃; ar flow rate in sputtering process: 98 sccm; o in sputtering process2Flow rate: 4sccm, sputtering current: 0.34A; sputtering to a thickness of 50nm, and annealing at 400 ℃ for 15 minutes;
(4) by using high-pressure high-purity N and gas-jet method2Atomizing polystyrene microsphere dispersion liquid with the diameter of 1 mu m in an air-jet pen to form aerial fog, and uniformly spraying the aerial fog on the medium film layer 2;
(5) and (3) sputtering the vanadium dioxide thin film layer 3 with the porous metamaterial structure on the top layer, wherein the specific process conditions are as in the step (2), sputtering the vanadium dioxide thin film layer with the thickness of 92nm, and annealing for 30 minutes at 400 ℃.
(6) Removing the polystyrene microspheres by using an acetone solution and ultrasonic treatment, and leaving a round hole structure with the diameter of 1 mu m on the top layer to obtain the three-layer structure intelligent window film layer with the round hole-shaped metamaterial structure.
The intelligent window film is prepared according to the method, and the vanadium dioxide film is subjected to reversible phase change from a semiconductor state to a metal state by using an external heating source and is tested. The visible light transmittance T is measured at low temperature (20 ℃) and high temperature (90 ℃) respectivelylumAnd near infrared transmittance, and calculating to obtain delta Tsol(according to formula I). Calculated according to fig. 5 and formula i, the visible light transmittance at 20 ℃ is T when the parameter d is 1100nmlum,lt50.4 percent and the visible light transmittance at the high temperature of 90 ℃ is Tlum,ht41.8%, and a difference Δ T between high and low temperature transmittances in the vicinity of 2.5um2.5μm63.8 percent and the solar spectrum modulation capability is delta Tsol22.8%. Compared with FIG. 4, the Δ T of the metamaterial structure with the top layer designed by the invention2.5μm、ΔTsolThereby greatly improving the operation.
Example 2
This example 2 is the same as example 1 except that the parameter d is different from example 1.
Table 1 is a simulation result statistical table in FIG. 6
Table 1 shows the simulation results in FIG. 6, which are measured in the parameters d and Tlum,lt、Tlum,htAnd Δ TsolRespectively counting in a table; it can be seen that a significant weakening begins to appear as d increases to 1600 nm; it can be seen that the beneficial effects of the present invention are ensured when d is between 1000nm and 1600 nm.
Example 3
Control experiment
In comparison to example 1, the control experiment did not contain a top layer metamaterial structure, and the rest was the same as example 1.
According to the calculation of the formula I and the figure 4, the visible light transmittance at the low temperature of 20 ℃ is Tlum,lt59.4 percent and the visible light transmittance at the high temperature of 90 ℃ is Tlum,ht51.1%, and a difference Δ T between high and low temperature transmittances in the vicinity of 2.5um2.5μm31.7 percent, and the solar spectrum modulation capability is delta Tsol＝9.7％。
Claims (4)
1. The intelligent window film based on the vanadium dioxide and metamaterial structure is characterized by comprising a bottom vanadium dioxide thin film layer, a medium thin film layer and a top vanadium dioxide thin film layer with a porous metamaterial structure from bottom to top in sequence;
round holes with the diameter 2R of 0.8-1.2 mu m are distributed on the vanadium dioxide thin film layer of the metamaterial structure, and the value range of the distance d between the adjacent round holes on the vanadium dioxide thin film layer of the metamaterial structure is 1000-1600 nm;
the thickness of the vanadium dioxide thin film layer of the metamaterial structure is 90-280 nm; the thickness of the bottom vanadium dioxide thin film layer is 30-80nm, and the thickness of the medium thin film layer is 50-150 nm;
the medium film layer is made of TiO2 、Al2O3、SiNxAnd SiO2One or more of them.
2. The method for preparing the intelligent window film based on the vanadium dioxide and metamaterial structure as claimed in claim 1, comprising the following steps:
(1) cleaning a substrate;
(2) preparing a bottom vanadium dioxide thin film layer;
(3) preparing a dielectric thin film layer on the bottom vanadium dioxide thin film layer;
(4) uniformly spraying polystyrene microspheres with the diameter of 0.8-1.2 mu m onto the dielectric film layer prepared in the step (3) by adopting an air spraying method;
(5) preparing a vanadium dioxide thin film layer with a metamaterial structure on the medium thin film layer sprayed with the polystyrene microspheres;
(6) and removing the polystyrene microspheres by using an acetone solution and ultrasonic treatment, and preparing the vanadium dioxide film with the round-hole-shaped metamaterial structure on the top layer.
3. The preparation method of the intelligent window film based on the vanadium dioxide and metamaterial structure as claimed in claim 2, wherein in the step (2), the adopted preparation method is one or more of sputtering, vacuum evaporation and sol-gel; in the step (3), the adopted preparation method is one or more of sputtering, vacuum evaporation and sol-gel; in the step (5), the adopted preparation method is one or more of sputtering, vacuum evaporation and sol-gel.
4. The method for preparing the intelligent window film based on the vanadium dioxide and metamaterial structure as claimed in claim 2, wherein the substrate in the step (1) is made of common glass or quartz glass.
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| CN112993583B (en) * | 2021-01-31 | 2023-03-10 | 郑州大学 | Vanadium dioxide metamaterial structure capable of realizing tunable ultra-wideband and application thereof |
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| KR101202335B1 (en) * | 2010-07-27 | 2012-11-16 | 삼성에스디아이 주식회사 | Thermochromic Smart Window and Method of Manufacturing the Same |
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