CN104250068A - Vanadium dioxide film system for intelligent energy saving window and preparation method thereof - Google Patents
Vanadium dioxide film system for intelligent energy saving window and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a vanadium dioxide film system for an intelligent energy saving window and a preparation method thereof. The film system includes a functional layer and an antireflection protective layer, wherein the functional layer is a doped vanadium dioxide film, the antireflection protective layer is an optical media, such as silica, titanium dioxide, silicon nitride, alumina, aluminum nitride, tantalum pentoxide and the like, and the antireflection protective layer can be one layer or multilayer. The doped vanadium dioxide film is prepared as follows: a doped metal vanadium film is deposited on a substrate by sputtering method, and the doped metal vanadium film is annealed by oxygen introduction under vacuum to obtain the doped vanadium dioxide film with the phase transition temperature near room temperature. An optical media layer is deposited on the surface of the prepared doped vanadium dioxide film to improve the visible light transmittance and weatherability of the film. The film system can intelligently adjust solar infrared radiation incidence quantity according to the temperature, and achieve the effect of being warm in winter and cool in summer.
Description
Technical field
The present invention relates to field of functional materials, relate to a kind of doped vanadium dioxide method for manufacturing thin film, particularly relate to design and the preparation method of the doping vanadium oxide membrane system of a kind of smart window application.
Technical background
From eighties of last century the eighties, just proposing vanadium dioxide can be applied to smart window field, and from then on vanadium dioxide is widely studied, and be that preparation technology or performance are all improved and promote, but vanadium dioxide smart window does not emerge.Vanadium dioxide film has three key factors as the application of intelligent temperature control window: transformation temperature, infrared regulation rate and visible transmitance.But, these three indexs are not separate, a large amount of research work is all optimized improvement mainly for wherein certain or Partial key performance, sacrifices the performance of other key parameters, but the rare work simultaneously considered as smart window application three large key element researchs is reported.As document (Jin P, Nakao S, Tanemura S.Tungsten doping into vanadium dioxide thermochromic films by high-energy ion implantation and thermal annealing [J] .Thin Solid Films, 1998,324:151 – 158) report has been adjusted to transformation temperature near 30 DEG C by mixing tungsten, but its infrared regulation rate in 2000nm place only has 18%; And separately have document (Balu R, Ashrit P V.Near-zero IR transmission in the metal-insulator transition of VO
2thin films [J] .Applied Physics Letters, 2008,92:021904) report brings up to about 70% by changing vanadium dioxide thickness film infrared regulation rate, but because its film thickness is 300nm, visible waveband almost without through, and transformation temperature is near 68 DEG C, far above room temperature.Therefore, only often cause other degradations for partial properties optimization, the actual demand of smart window application can not be met, need consider and take into account each salient features of film system.
The typical phase transition temperature of vanadium dioxide is 68 DEG C, and higher than glass surface temperature in summer, film does not undergo phase transition, and does not have infrared transmittivity Intelligent adjustment function, therefore can not realize effect cool in summer and warm in winter.By thin film phase change temperature being adjusted to nearly room temperature to film doping, doped element comprises W, Mo, AI, Ti, Nb and Ta etc., and adulterating also has certain influence to infrared regulation rate, and along with doping increases, infrared regulation rate also can reduce.
Improve infrared regulation rate, just need the thickness increasing vanadium dioxide film, but the increase of vanadium dioxide film thickness, visible light transmissivity can be made to decline; And visible light transmissivity is too low, then daylighting weak effect, is difficult to apply as smart window.Therefore need to select suitable doping and vanadium dioxide film thickness, take into account transformation temperature and infrared regulation rate.On this basis, then pass through to introduce one deck antireflective film, improve visible light transmissivity.
The invention discloses a kind of preparation method being suitable for the high-performance doped vanadium dioxide film system of industrialization.Wherein by vanadium target and doping vanadium target co-sputtering, the doping of prepared vanadium dioxide can be controlled, and then regulate the transformation temperature of vanadium dioxide film, obtain suitable transformation temperature and infrared regulation rate; And by Film Design, obtain high performance intelligent fenestrated membrane system; Preparation method is simple and easy to do in film system, compatible with extensive coating process, can be generalized in smart window and applies.
Summary of the invention
The invention provides a kind of Intelligent energy-saving window vanadium dioxide basement membrane system and preparation method thereof.Film system comprises two major portions: functional layer and supplementary layer.
As shown in Figure 1; film structure is: have functional layer 2 and anti-reflection protective layer 1 on the substrate 3 successively; wherein functional layer 2 is doped vanadium dioxide layers of suitable dopant ratio, and anti-reflection protective layer 1 is one or more layers silicon-dioxide, silicon nitride, titanium dioxide, aluminum oxide, aluminium nitride or tantalum pentoxide light layer of dielectric material.
When vanadium dioxide is lower than transformation temperature, present semi-conductor phase, infrared transmittivity is high, and during lower than transformation temperature, infrared transmission is too low, in phase transition process, vanadium dioxide film visible light transmission rate is almost unchanged, as long as therefore transformation temperature is suitable, room temperature just can be followed automatically to regulate the amount of incident of sunlight ir radiation, realize effect cool in summer and warm in winter.Phase transition temperature of vanadium dioxide can be adjusted near room temperature by doping, doped element comprises W, Mo, AI, Ti, Nb and Ta etc., selects suitable dopant ratio just can obtain the suitable vanadium dioxide film of transformation temperature.Wherein dopant ratio scope is 0.5 ~ 4.0%, and film thickness is at 20 ~ 100nm.
On the basis of the vanadium dioxide film of functional layer doping, prepare one or more layers anti-reflection protective layer to improve film system overall performance.
Anti-reflection protective layer has two effects:
A () improves the visible transmitance of film system
If the optical thickness of rete is 1/4th of a certain wavelength, the path difference of adjacent two-beam is π just, and namely direction of vibration is contrary, and the result of superposition makes optical surface reduce the reflected light of this wavelength.Suitable selection thin-film refractive index, at this moment the reflected light of optical surface can be eliminated completely.In order to reduce the reflected light on surface, normally plate the film of one deck low-refraction at glass surface thin.Reflectivity can calculate with eigen matrix, to individual layer antireflective film:
For centre wavelength, have
the position of centre wavelength is decided by the thickness and specific refractory power regulating coatings.
The equivalent refractive index of substrate and coatings is:
obtaining specular reflectance included is
Visible, when
time, when namely coatings specific refractory power is the square root of substrate and air refraction product, reflectivity is 0, anti-reflection best results.
B () prevents doped vanadium dioxide layer to be oxidized
In vanadium dioxide, v element valence state is tetravalence, and in the various valence states of vanadium, pentavalent vanadium is the most stable.Therefore in order to prevent vanadium dioxide in atmosphere slow oxidation become Vanadium Pentoxide in FLAKES, need to be coated with layer protective layer at film surface, improve film system weathering resistance.
The preparation method of smart window doped vanadium dioxide film system disclosed by the invention, mainly comprises the steps:
1, by the vanadium metal film of the method preparation doping of sputtering, in order to make subsequent processes caudacoria cording have certain visible light transmissivity and infrared control characteristic, vanadium metal tungsten film thickness controls at 15 ~ 80nm;
2, adopt the method that vacuum leads to oxygen annealing that doping metals vanadium film anneal oxidation is become doped vanadium dioxide film, film thickness is 20 ~ 100nm;
3, test transmission spectrum and the reflectance spectrum of doped vanadium dioxide film, extracted the optical constant of doped vanadium dioxide film by software;
4, apply the optical constant of doped vanadium dioxide film and optical medium, design smart window vanadium dioxide film system, simulates the impact of each layer thickness on film system overall performance in software;
5, by the vanadium metal film of the method preparation doping of sputtering, thicknesses of layers is selected according to the section of excellent performance in simulation;
6, adopt the method that vacuum leads to oxygen annealing that vanadium metal tungsten film anneal oxidation is become doped vanadium dioxide film;
7, deposit one deck anti-reflection layer by the method for sputtering at film surface, anti-reflection layer thickness is selected according to the section of excellent performance in simulation.
After have employed technique scheme, the present invention has following beneficial effect:
1, over-all properties: the doped vanadium dioxide film system prepared by this method design, is had the transformation temperature close to room temperature, but also have high infrared regulation rate and higher visible light transmissivity.Therefore, film system not only has good lighting performance, and can regulate the amount of incident of infrared light adaptively along with seasonal variation, is a kind of intelligent fenestrated membrane system of excellent performance.
2, film system transformation temperature is close to room temperature: when direct sunlight in summer, glass surface temperature is higher than this film system transformation temperature, and doped vanadium dioxide layer change becomes metallographic phase, and infrared transmittivity diminishes, significantly can reduce sunlight ir radiation amount of incident, reduce refrigeration power consumption.And when winter, glass surface temperature is lower than this transformation temperature, doped vanadium dioxide layer change becomes semi-conductor phase, allows most of sunlight ir radiation to enter indoor, reduces heating energy consumption.
3, film cording has very high infrared regulation rate: the infrared regulation rate of film system refers to the difference of its room temperature infrared transmittivity and high-temperature infrared transmitance, infrared transmittivity is high means that film has very low infrared transmittivity when high temperature, and has very high ir transmissivity when low temperature.Therefore significantly can regulate sunlight ir radiation along with temperature Change.
4, film cording has higher visible light transmissivity: owing to have employed anti-reflection design, film ties up to visible waveband and has higher visible light transmissivity.Therefore a part of visible ray can be allowed to enter indoor, namely there is certain daylighting effect, reduce interior lighting power consumption.
Accompanying drawing explanation
Accompanying drawing 1 is for high-performance smart window is with mixing tungsten vanadium dioxide film structure schematic diagram.
Accompanying drawing 2 is the infrared regulation rate (a) of smart window vanadium dioxide basement membrane system in embodiment 1, peaks visible transmitance (b) and high-temperature infrared transmitance (c) with the variation relation of vanadium dioxide film thickness and silicon dioxide thickness.
Accompanying drawing 3 is smart window vanadium dioxide basement membrane system's room temperature and high temperature transmitted spectrum in embodiment 1.
Accompanying drawing 4 is smart window vanadium dioxide basement membrane system 2000nm wavelength place Hysteresis cycle in embodiment 1.
Accompanying drawing 5 is the infrared regulation rate (a) of smart window vanadium dioxide basement membrane system in embodiment 2, peaks visible transmitance (b) and high-temperature infrared transmitance (c) with the variation relation of vanadium dioxide film thickness and silicon dioxide thickness.
Accompanying drawing 6 is smart window vanadium dioxide basement membrane system's room temperature and high temperature transmitted spectrum in embodiment 2.
Accompanying drawing 7 is smart window vanadium dioxide basement membrane system 2000nm wavelength place Hysteresis cycle in embodiment 2.
Accompanying drawing 8 is the infrared regulation rate (a) of smart window vanadium dioxide basement membrane system in embodiment 3, peaks visible transmitance (b) and high-temperature infrared transmitance (c) with the variation relation of vanadium dioxide film thickness and silicon dioxide thickness.
Accompanying drawing 9 is smart window vanadium dioxide basement membrane system's room temperature and high temperature transmitted spectrum in embodiment 3.
embodiment
For making content of the present invention, technical scheme and advantage clearly understand, set forth the present invention further below in conjunction with specific embodiment, these embodiments are only for illustration of the present invention, and the present invention is not limited only to following examples.Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated:
Embodiment 1:
This example take float glass as substrate, is coated with mixes tungsten vanadium dioxide film on its surface, then plates silicon-dioxide anti-reflection protective layer, formation glass/mix tungsten vanadium dioxide/silicon dioxide film system, then testing film performance.Concrete implementation step is as follows:
1, substrate cleaning.Glass substrate is put into alcohol ultrasonic 10 minutes, remove substrate surface greasy dirt, after ultrasonic cleaning terminates, taken out rapidly, dry up with nitrogen, put into plated film chamber.
2,80nm vanadium metal W film is coated with.The vanadium target that coating system uses and vanadium tungsten target are all 320 × 140mm planar targets, and wherein vanadium target purity is 99.99%; Vanadium tungsten target vanadium tungsten atom is than being 96:4.Sputtering technology gas is argon gas, purity 99.999%.System-based vacuum is 1 × 10
-3pa.During sputter coating, argon flow amount is adjusted to 50sccm, now system air pressure is 0.22Pa; Setting vanadium target sputtering power is 500W, and now its sputtering voltage is 350V, and setting vanadium tungsten target sputtering power is 100W, and now its sputtering voltage is 290V, and dopant ratio is 0.5%; After being coated with vanadium metal W film 80nm, film is taken out.
3 control oxygen flow annealing.Vanadium metal film is placed in tubular annealing stove, with mechanical pump, annealing furnace cavity is found time, remove the impact of remnant oxygen; When temperature arrives after 530 DEG C, pass into 20sccm oxygen, now stove internal gas pressure is 18Pa, in this temperature and oxygen partial pressure environment, keep 30min; Then allow annealing furnace naturally cool to less than 100 DEG C, be filled with air, take out sample.
4, properties of sample test.Transmission spectrum when visible ray optical fiber spectrograph and infrared optical fiber spectrophotometer film system room temperature (20 DEG C) and high temperature (100 DEG C).
5, the matching of CODE Film Design software matching transmission spectrum is used to mix room temperature optical constant and the High Temperature Optical constant of tungsten vanadium dioxide film, and simulate combined films system glass/mix in tungsten vanadium dioxide/silicon-dioxide, each layer thickness is on the impact of infrared regulation rate (2400nm wavelength place), peaks visible transmitance and high-temperature infrared transmitance (1500nm wavelength place), as shown in Figure 2, optimum thickness section is determined.
6, according to the doped vanadium dioxide optimum thickness section that step 5 is determined, repeating step 1-3, by vanadium dioxide film gauge control at 100nm.
7, the sample of taking-up is put into coating system, the silicon-dioxide optimum thickness section determined according to step 5, be coated with 50nm silica membrane, film system has been coated with.
8, properties of sample test.Transmission spectrum when visible ray optical fiber spectrograph and infrared optical fiber spectrophotometer film system room temperature (20 DEG C) and high temperature (100 DEG C), as shown in Figure 3.In addition, infrared optical fiber spectrograph also measured weres the optics Hysteresis cycle of sample at 2000nm wavelength place, as shown in Figure 4.
This film cording has good smart window over-all properties: at room temperature, and 2400nm wavelength place transmissivity is 51.0%, and is at high temperature 10.6%, and transmission rate variance is 40.2%, has good infrared regulating power; At visible waveband, its peak transmission is 46.3%, has good lighting performance; Film system transformation temperature is 38.6 DEG C, close to room temperature, can meet most area smart window application demand.Therefore this film system is a kind of intelligent fenestrated membrane system well.
Embodiment 2:
This example take float glass as substrate, is coated with mixes tungsten vanadium dioxide film on its surface, then plates silicon nitride anti-reflection protective layer, formation glass/mix tungsten vanadium dioxide/silicon nitride film system, then testing film performance.Concrete implementation step is as follows:
1, substrate cleaning.Glass substrate is put into alcohol ultrasonic 10 minutes, remove substrate surface greasy dirt, after ultrasonic cleaning terminates, taken out rapidly, dry up with nitrogen, put into plated film chamber.
2,50nm vanadium metal W film is coated with.The vanadium target that coating system uses and vanadium tungsten target are all 320 × 140mm planar targets, and wherein vanadium target purity is 99.99%; Vanadium tungsten target vanadium tungsten atom is than being 96:4.Sputtering technology gas is argon gas, purity 99.999%.System-based vacuum is 1 × 10
-3pa.During sputter coating, argon flow amount is adjusted to 50sccm, now system air pressure is 0.22Pa; Setting vanadium target sputtering power is 500W, and now its sputtering voltage is 350V, and setting vanadium tungsten target sputtering power is 300W, and now its sputtering voltage is 310V, and dopant ratio is 2%; After being coated with vanadium metal W film 50nm, film is taken out.
3, oxygen flow annealing is controlled.Vanadium metal film is placed in tubular annealing stove, with mechanical pump, annealing furnace cavity is found time, remove the impact of remnant oxygen; When temperature arrives after 530 DEG C, pass into 20sccm oxygen, now stove internal gas pressure is 18Pa, in this temperature and oxygen partial pressure environment, keep 30min; Then allow annealing furnace naturally cool to less than 100 DEG C, be filled with air, take out sample.
4, properties of sample test.Transmission spectrum when visible ray optical fiber spectrograph and infrared optical fiber spectrophotometer film system room temperature (20 DEG C) and high temperature (100 DEG C).
5, the matching of CODE Film Design software matching transmission spectrum is used to mix room temperature optical constant and the High Temperature Optical constant of tungsten vanadium dioxide film, and simulate combined films system glass/mix in tungsten vanadium dioxide/silicon nitride, each layer thickness is on the impact of infrared regulation rate (2400nm wavelength place), peaks visible transmitance and high-temperature infrared transmitance (1500nm wavelength place), as shown in Figure 5, optimum thickness section is determined.
6, according to the doped vanadium dioxide optimum thickness section that step 6 is determined, repeating step 1-3, by vanadium dioxide film gauge control at 70nm.
7, the sample of taking-up is put into coating system, the silicon nitride optimum thickness section determined according to step 6, be coated with 50nm silicon nitride film, film system has been coated with.
8, properties of sample test.Transmission spectrum when visible ray optical fiber spectrograph and infrared optical fiber spectrophotometer film system room temperature (20 DEG C) and high temperature (100 DEG C), as shown in Figure 6.In addition, infrared optical fiber spectrograph also measured weres the optics Hysteresis cycle of sample at 2000nm wavelength place, as shown in Figure 7.
Embodiment 3:
This example take float glass as substrate, is coated with mixes tungsten vanadium dioxide film on its surface, then plates silicon nitride anti-reflection protective layer, formation glass/mix tungsten vanadium dioxide/aluminium nitride film system, then testing film performance.Concrete implementation step is as follows:
1, substrate cleaning.Glass substrate is put into alcohol ultrasonic 10 minutes, remove substrate surface greasy dirt, after ultrasonic cleaning terminates, taken out rapidly, dry up with nitrogen, put into plated film chamber.
2,15nm vanadium metal W film is coated with.The vanadium target that coating system uses and vanadium tungsten target are all 320 × 140mm planar targets, and wherein vanadium target purity is 99.99%; Vanadium tungsten target vanadium tungsten atom is than being 96:4.Sputtering technology gas is argon gas, purity 99.999%.System-based vacuum is 1 × 10
-3pa.During sputter coating, argon flow amount is adjusted to 50sccm, now system air pressure is 0.22Pa; Setting vanadium tungsten target sputtering power is 500W, and now its sputtering voltage is 360V, and dopant ratio is 4%; After being coated with vanadium metal W film 15nm, film is taken out.
3, oxygen flow annealing is controlled.Vanadium metal film is placed in tubular annealing stove, with mechanical pump, annealing furnace cavity is found time, remove the impact of remnant oxygen; When temperature arrives after 530 DEG C, pass into 20sccm oxygen, now stove internal gas pressure is 18Pa, in this temperature and oxygen partial pressure environment, keep 30min; Then allow annealing furnace naturally cool to less than 100 DEG C, be filled with air, take out sample.
4, properties of sample test.Transmission spectrum when visible ray optical fiber spectrograph and infrared optical fiber spectrophotometer film system room temperature (20 DEG C) and high temperature (100 DEG C).
5, the matching of CODE Film Design software matching transmission spectrum is used to mix room temperature optical constant and the High Temperature Optical constant of tungsten vanadium dioxide film, and simulate combined films system glass/mix in tungsten vanadium dioxide/silicon nitride, each layer thickness is on the impact of infrared regulation rate (2400nm wavelength place), peaks visible transmitance and high-temperature infrared transmitance (1500nm wavelength place), as shown in Figure 8, optimum thickness section is determined.
6, according to the doped vanadium dioxide optimum thickness section that step 6 is determined, repeating step 1-3, by vanadium dioxide film gauge control at 20nm.
7, the sample of taking-up is put into coating system, the silicon nitride optimum thickness section determined according to step 6, be coated with 40nm silicon nitride film, film system has been coated with.
8, properties of sample test.Transmission spectrum when visible ray optical fiber spectrograph and infrared optical fiber spectrophotometer film system room temperature (20 DEG C) and high temperature (100 DEG C), as shown in Figure 9.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. an Intelligent energy-saving window vanadium dioxide basement membrane system, its structure, for have functional layer (2) and anti-reflection protective layer (1) on substrate (3) successively, is characterized in that:
Described functional layer (2) is dopant ratio is 0.5 ~ 4.0% doped vanadium dioxide film, and doped element is W, Mo, AI, Ti, Nb or Ta, and film thickness is 20 ~ 100nm;
Described anti-reflection protective layer (1) is one or more layers silicon-dioxide, silicon nitride, titanium dioxide, aluminum oxide, aluminium nitride or tantalum pentoxide light layer of dielectric material.
2. prepare a method for Intelligent energy-saving window vanadium dioxide basement membrane system as claimed in claim 1, it is characterized in that comprising the following steps:
1) by the vanadium metal film of the method preparation doping of sputtering, in order to make subsequent processes caudacoria cording have certain visible light transmissivity and infrared control characteristic, vanadium metal tungsten film thickness controls at 20 ~ 80nm;
2) adopt the method that vacuum leads to oxygen annealing that doping metals vanadium film anneal oxidation is become doped vanadium dioxide film, film thickness is 20 ~ 100nm;
3) test transmission spectrum and the reflectance spectrum of doped vanadium dioxide film, extracted the optical constant of doped vanadium dioxide film by software;
4) apply the optical constant of doped vanadium dioxide film and optical medium, design smart window vanadium dioxide film system, simulates the impact of each layer thickness on film system overall performance in software;
5) by the vanadium metal film of the method preparation doping of sputtering, thicknesses of layers is selected according to the section of excellent performance in simulation;
6) adopt the method that vacuum leads to oxygen annealing that vanadium metal tungsten film anneal oxidation is become doped vanadium dioxide film;
7) deposit one deck anti-reflection layer by the method for sputtering at film surface, anti-reflection layer thickness is selected according to the section of excellent performance in simulation.
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| CN107686971A (en) * | 2017-08-24 | 2018-02-13 | 苏州鑫河镜业有限公司 | A kind of durable coating process of high thang-kng of eyeglass multilayer |
| CN109095499A (en) * | 2018-06-27 | 2018-12-28 | 深圳大学 | A kind of vanadium dioxide Multilayer system and its preparation method and application |
| CN109280894A (en) * | 2018-10-12 | 2019-01-29 | 天津大学 | A kind of VO based on antireflective substrate2The preparation method of laminated film |
| CN109653652A (en) * | 2018-12-19 | 2019-04-19 | 吉林省建安实业股份有限公司 | Energy-saving door and window |
| CN110158034A (en) * | 2019-05-10 | 2019-08-23 | 中国科学院上海技术物理研究所 | The method of a kind of More target sputtering together preparation heterogeneity and doping than film |
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| CN107686971A (en) * | 2017-08-24 | 2018-02-13 | 苏州鑫河镜业有限公司 | A kind of durable coating process of high thang-kng of eyeglass multilayer |
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| CN109280894A (en) * | 2018-10-12 | 2019-01-29 | 天津大学 | A kind of VO based on antireflective substrate2The preparation method of laminated film |
| TWI675929B (en) * | 2018-10-16 | 2019-11-01 | 崑山科技大學 | Method for preparing electrochromic ion storage membrane |
| CN109653652A (en) * | 2018-12-19 | 2019-04-19 | 吉林省建安实业股份有限公司 | Energy-saving door and window |
| CN110158034A (en) * | 2019-05-10 | 2019-08-23 | 中国科学院上海技术物理研究所 | The method of a kind of More target sputtering together preparation heterogeneity and doping than film |
| CN113764145A (en) * | 2020-06-05 | 2021-12-07 | 高尔科技股份有限公司 | Thermistor and microbolometer based on thermistor |
| CN116577850A (en) * | 2023-03-31 | 2023-08-11 | 云南驰宏国际锗业有限公司 | Infrared germanium window sheet of HD film with wave band of 8-12um |
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Application publication date: 20141231 |