CN102030485A - Intelligent control composite film glass and preparation method thereof - Google Patents
Intelligent control composite film glass and preparation method thereof Download PDFInfo
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- CN102030485A CN102030485A CN 201010545724 CN201010545724A CN102030485A CN 102030485 A CN102030485 A CN 102030485A CN 201010545724 CN201010545724 CN 201010545724 CN 201010545724 A CN201010545724 A CN 201010545724A CN 102030485 A CN102030485 A CN 102030485A
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Abstract
The invention discloses intelligent control composite film glass and a preparation method thereof. The composite film glass is structurally characterized in that a composite film is deposited on a glass substrate and comprises a first isolating layer, a vanadium oxide layer and a second isolating layer, wherein the first isolating layer is silicon nitride with the thickness of 50-150nm; the vanadium oxide layer has the thickness of 30-100nm and adopts a thermal phase change vanadium oxide film material with the transverse grain size of 5-30nm and thermal phase change temperature of 30-40 DEG C; and the second isolating layer is silicon nitride with the thickness of 50-150nm. The composite film glass can intelligently regulate the near-infrared spectrum band reflectivity according to the ambient temperature, block the sun heat radiation under high-temperature environment, transmit sun heat radiation under low-temperature environment, can be used in an intelligent energy-saving glass window, reduces the summer energy consumption, and increases the utilization of the winter sun radiation energy.
Description
Technical field
The present invention relates to building material technical field, particularly employing is fundamental construction sun heat radiation intelligent power saving composite membrane and preparation method thereof with the thermochromism vanadium oxide film.
Background technology
Two infrared sources of main existence on the earth: one is the solar radiation source, main component is the visible light (0.38～0.75 μ m) that accounts for total energy 45% and to account for total energy be 50% near infrared light (0.76～2.9 μ m), and other 5% are far red light (3～50 μ m) and UV-light etc.; Second source of radiation is earth surface, and (mainly being visible light and near infrared light) changes heat into after the optical radiation of its absorption sun, and the earth surface temperature is raise, and earth surface is again with the outside thermal radiation of far mode.Summer earth surface temperature height, far-infrared radiation intensity is big, outdoor to indoor thermal radiation much larger than indoor to outdoor thermal radiation, cause indoor temperature rise in the solar energy inlet chamber, produce air conditioning energy consumption; Winter, room temp was higher than external temperature, indoor to outdoor far-infrared radiation in the highest flight, indoor thermal energy is escaped from glass door and window.Modern architecture adopts glass door and window and glass curtain wall in a large number, the door and window power consumption it is reported and accounts for 50% of whole building energy consumption, the ideal energy-saving glass should reduce heat in the inlet chamber in summer, can reduce the heat that door and window is overflowed winter, just can reduce building energy consumption greatly.
At present utilize the energy-saving glass of sun power mainly to adopt low radiation coated glass both at home and abroad, also claim Low-E (low emittance) glass.For example the product and the patent of the MB Group Plc of the U.S., Dao Sen company, Weir company and Suo Si company have occupied principal market, the world.It is that being coated with extremely thin low radiation metal material (for example silver etc.) or conductive metallic compound such as TiN conductivity ceramics or ITO conducting metal oxide at glass surface is the film system of base, it mainly acts on is to guarantee under certain visible light transmissivity prerequisite, raising is near infrared and the reflection of mid and far infrared radiating, as patent documentation CN1296304C and CN101070226A etc.With regard to application, with covering positive coefficient S
c(be defined as the ratio that solar radiation energy under the same terms sees through amount with the amount that sees through 3 millimeters transparent glasses of certain glass assembly, shading coefficient is more little, and block sunlight direct heat radiating performance is good more) described glass and covered thermal-radiating ability.Select different S for use according to territory of use's difference
cGlass.To the area of the north, need select S for use based on heating
cThe glass of＞0.5 high-sunshade coefficient; To southern area sweltering heat in summer, then select S for use
c＜0.5 low shading coefficient glass.From the structure of traditional low radiation coated glass, the energy of near infrared part does not make full use of, for S
c＞0.5 low-emission coated, utilized near infrared light winter, but introduced summer in the more near infrared light inlet chamber, room temp is raise; In like manner, to S
c＜0.5 low radiation coated glass, it is indoor to have stoped summer near infrared light to incide, and has alleviated the burden of air-conditioning, but that also stoped near infrared light to incide winter is indoor, does not alleviate the burden of heating installation.Therefore, traditional low emissivity glass can not accomplish that winter and summer are simultaneously energy-efficient, and its key is can not be according to the amount in environment or the room temp control near-infrared radiation composition inlet chamber.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of glass composite film, this glass composite film Heat stability is good, and visible transmission can just be adjusted according to envrionment temperature than high simultaneously; The present invention also provides the preparation method of this glass composite film, and this method has the function of regulating near infrared spectral coverage reflectivity according to envrionment temperature intelligence, can obtain low radiation functions under hot environment simultaneously, and obtains high solar energy under low temperature environment.
A kind of glass composite film provided by the invention is characterized in that, deposits composite membrane on glass substrate, and this composite membrane comprises first sealing coat, vanadium oxide layer and second sealing coat, and described first sealing coat is a silicon nitride, and thickness is 50～150nm; Described vanadium oxide layer thickness is 30～100nm, and adopting horizontal particle diameter is 5～30nm, and the thermal induced phase transition temperature is 30～40 ℃ a thermal induced phase transition vanadium oxide thin film material; Described second sealing coat is a silicon nitride, and thickness is 50～150nm.The effect of first sealing coat is that metal ion is to the diffusion of vanadium oxide material in the insulating glass, and the effect of second sealing coat is that the oxygen molecule that obstructs in outer membrane or the atmosphere spreads to vanadium oxide membrane.
As improvement of the technical scheme, between the glass substrate and first sealing coat, also be provided with the bottom dielectric layer, this bottom dielectric layer is a silicon oxide, thickness is at 50～100nm.
As further improvement in the technical proposal, on second sealing coat, also be provided with the top layer dielectric layer, this top layer dielectric layer is a titanium dioxide, thickness is 40～100nm.
Increase top layer and bottom dielectric medium, can regulate the color and the luminous reflectance factor of glassy membrane system, the top layer dielectric medium adopts TiO simultaneously
2Also has self-cleaning function.
The preparation method of above-mentioned intelligent control glass composite film comprises the steps:
The 1st step obtained silicon nitride adopting silicon target reactive sputter-deposition under argon and nitrogen mixture atmosphere on the glass substrate, and as sealing coat, sputtering sedimentation air pressure is 0.05～0.1Pa;
The 2nd step obtained the thermal induced phase transition vanadium oxide thin film material, as the vanadium oxide layer adopting vanadium metal target reactive ion beam sputter-deposition under the mixed atmosphere of argon and oxygen on the sealing coat; The sputtering sedimentation air pressure of described vanadium oxide layer is 0.05～0.08Pa;
The 3rd step obtained silicon nitride, as protective layer adopting silicon target reactive sputter-deposition under argon and nitrogen mixture atmosphere on the vanadium oxide layer; Sputtering sedimentation air pressure is 0.05～0.1Pa;
The 4th step deposited final vacuum annealing, and annealing temperature is controlled at 350～450 ℃.
Adopt conductive films such as silver, titanium nitride or ITO different with the low radiation energy-saving glass of routine, the present invention adopts nanometer thermochromic material vanadium oxide intelligent control near-infrared band reflectivity.Particularly, the invention has the advantages that:
(1) with respect to the low emissivity glass of routine owing to adopt the nano particle size vanadium oxide film, not only have the function that outside temperature intelligence is regulated sun heat radiation, and attemperation than traditional micron granularity vanadium oxide film more near room temperature, Application Areas is wider.
(2) adopt composite membrane of the present invention, the color of coated glass and luminous reflectance factor performance-adjustable improve greatly.Regulate the thickness of each layer in the multilayer film, the color that can regulate coated glass by regulating processing parameter.
Adopt coated glass of the present invention, the visible transmission ratio can＞70%.In the hot environment in summer, shading coefficient S
cCan be less than 0.3, under the low temperature environment in winter, shading coefficient S
cCan all can use in the north and south greater than 0.6.
Description of drawings
Fig. 1 is the transmission scanning electron microscope photo of polycrystalline Nano structure vanadium oxide structure.
Fig. 2 is the contrast that varies with temperature reflectance curve that has nano particle size and micron granularity vanadium oxide film at near-infrared band.
Fig. 3 is the structural representation of three layers of intelligent control glass composite film.
Fig. 4 is the structural representation of five layers of intelligent control glass composite film.
Fig. 5 is the transmissivity spectrum contrasts of five layers of glass composite film under low temperature and high temperature.
Embodiment
The vanadium oxide nanoparticle thin-film material that the present invention adopts, laterally granularity is 5～30nm (the present invention claims that the direction parallel with the depositional plane of glass substrate is for horizontal), it has reversible thermal induced phase transition characteristic, transformation temperature is about about 30～40 ℃, than the transformation temperature (～68 ℃) of the vanadium oxide film of traditional micron granularity (about 1 μ m) more near room temperature.Fig. 1 is the transmission electron microscope photo of the vanadium oxide film 2 of making on silicon nitride sealing coat 1, shows that in conjunction with XRD analysis the horizontal size of vanadium oxide is at 8～10nm.Because quantum size effect, the vanadium oxide of nano particle size is compared the vanadium oxide film of traditional micron granularity, and the thermal induced phase transition temperature moves on near the room temperature.Fig. 2 locates temperature variant reflection spectrum curve for mono-layer oxidized vanadium film on the glass substrate is 2.5 microns at wavelength, curve 1 corresponding micron granularity vanadium oxide wherein, curve 2 corresponding nano particle size vanadium oxides.Be lower than the transformation temperature vanadium oxide film and be the semi-conductor phase, transparent near infrared light, reflectivity is low; Being higher than transformation temperature is metallographic phase, to infrared light (containing near, far infrared) reflectivity height.
Below by by embodiment the present invention being described in further detail, but following examples only are illustrative, and protection scope of the present invention is not subjected to the restriction of these embodiment.
As shown in Figure 3, this embodiment is a kind of structure of composite membrane of being made up of three-layer thin-film, it is first sealing coat, the vanadium oxide layer with nano particle size be made up of silicon nitride of sputtering sedimentation and the composite membrane of being made up of silicon nitride second sealing coat successively on the glass substrate of 3 millimeters thickness, and promptly the composite film structure is glass substrate/silicon nitride/vanadium oxide/silicon nitride.Wherein the thickness of the first sealing coat silicon nitride is 60nm, and the thickness of vanadium oxide nanoparticle layer is 30nm, and transformation temperature is 30 ℃, and the thickness of the second sealing coat silicon nitride is 80nm.Calculating the visible transmission ratio according to the method for GBT 2680-94 is 0.61, and the sheltering coefficient of sun heat radiation is 0.29 when the residing envrionment temperature of glass is 38 ℃, and the sheltering coefficient of sun heat radiation is 0.72 when the residing envrionment temperature of glass is 23 ℃.
Glass composite film performance under other parameter conditions is as shown in table 1.
As shown in Figure 2, this embodiment is a kind of composite membrane of being made up of five layer films, it be by on the glass substrate of 3 millimeters thickness successively sputtering sedimentation by SiO
2The bottom dielectric layer of forming, first sealing coat of forming by silicon nitride, vanadium oxide layer, second sealing coat of forming by silicon nitride and by TiO with nano particle size
2The composite membrane that the top layer dielectric layer of forming is formed, promptly the composite film structure is glass substrate/silicon dioxide/silicon nitride/vanadium oxide/silicon nitride/titanium dioxide.The thickness of bottom dielectric medium silicon-dioxide is 120nm, and the thickness of the first sealing coat silicon nitride is 50nm, and the thickness of vanadium oxide nanoparticle layer is 50nm, its grain size is about 10nm, transformation temperature is about 28 ℃, and the thickness of the second sealing coat silicon nitride is 30nm, top layer dielectric medium TiO
2Thickness be 40nm.Calculating the visible transmission ratio according to the method for GBT 2680-94 is 0.68, and the sheltering coefficient of sun heat radiation is 0.26 when the residing envrionment temperature of glass is 38 ℃, and the sheltering coefficient of sun heat radiation is 0.75 when the residing envrionment temperature of glass is 23 ℃.
Glass composite film performance under other preparation parameter conditions is as shown in table 2.
When producing above-mentioned structure of composite membrane, composite membrane on glass can prepare by the vacuum sputtering deposition techniques: earlier substrate is passed through each sputter coating chamber successively, use vacuum sputtering deposition techniques bottom dielectric layer, first sealing coat, vanadium oxide layer, second sealing coat and top layer dielectric layer respectively in each sputtering chamber.The thickness of each coating be can control by control sputtering power and glass by the speed of each sputtering chamber, wherein when being coated with vanadium oxide film, target voltage feedback control system or spectrographic detection feedback control system needed to adopt, to reduce the fluctuation of argon oxygen partial pressure ratio.
Illustrate that to produce example procedure shown in Figure 3 the present invention prepares the production technique of intelligent control composite membrane below.
The 1st goes on foot not, and the film plating substrate glass substrate enters silicon target sputter coating chamber, in the silicon target sputtering chamber, silicon target adopts reaction magnetocontrol sputtering deposited silicon nitride first sealing coat in the mixed gas of argon and nitrogen, sputtering pressure is 0.05～0.1Pa, and the speed that enters the sputter coating chamber by control sputtering target power and glass is controlled first sealing coat to needed thickness;
The 2nd step will have been plated the glass substrate of first sealing coat and sent into vanadium target ion beam sputtering coating chamber, in vanadium target ion beam sputtering coating chamber, the vanadium target relies on the reactive ion beam sputter-deposition in the mixed atmosphere of argon gas and oxygen, sputtering pressure is 0.05～0.08Pa, comes the needed thickness of controlled oxidation vanadium floor by control sputtering target power and glass substrate by the speed of sputter coating chamber;
The 3rd step will have been plated the glass substrate of vanadium oxide floor and sent into silicon target sputter coating chamber, in the silicon target sputtering chamber, silicon target adopts reaction magnetocontrol sputtering deposited silicon nitride second sealing coat in the mixed gas of argon and nitrogen, sputtering pressure is 0.05～0.1Pa, and the speed that enters the sputter coating chamber by control sputtering target power and glass is controlled second sealing coat to needed thickness;
The 4th step will deposit the glass of composite membrane and send into the high temperature annealing chamber, and about 30 minutes, annealing temperature is controlled at 350～450 ℃ at high temperature annealing under vacuum or the inert gas atmosphere, take out after cooling and promptly obtain the intelligent control glass composite film.
If process the glass composite film of other embodiment, the step that only need increase or reduce response on the basis of above-mentioned technology gets final product.
The present invention not only is confined to above-mentioned embodiment; persons skilled in the art are according to content disclosed by the invention; can adopt other multiple embodiment to implement the present invention; therefore; every employing project organization of the present invention and thinking; do some simple designs that change or change, all fall into the scope of protection of the invention.
Claims (4)
1. a glass composite film is characterized in that, deposits composite membrane on glass substrate, and this composite membrane comprises first sealing coat, vanadium oxide layer and second sealing coat, and described first sealing coat is a silicon nitride, and thickness is 50～150nm; Described vanadium oxide layer thickness is 30～100nm, and adopting horizontal particle diameter is 5～30nm, and the thermal induced phase transition temperature is 30～40 ℃ a thermal induced phase transition vanadium oxide thin film material; Described second sealing coat is a silicon nitride, and thickness is 50～150nm.
2. glass composite film according to claim 1 is characterized in that: also be provided with the bottom dielectric layer between the glass substrate and first sealing coat, this bottom dielectric layer is a silicon oxide, and thickness is at 50～100nm.
3. glass composite film according to claim 1 and 2 is characterized in that: also be provided with the top layer dielectric layer on second sealing coat, this top layer dielectric layer is a titanium dioxide, and thickness is 40～100nm.
4. the preparation method of the described glass composite film of claim 1 is characterized in that, this preparation method comprises the steps:
The 1st step obtained silicon nitride adopting silicon target reactive sputter-deposition under argon and nitrogen mixture atmosphere on the glass substrate, and as sealing coat, sputtering sedimentation air pressure is 0.05～0.1Pa;
The 2nd step obtained the thermal induced phase transition vanadium oxide thin film material, as the vanadium oxide layer adopting vanadium metal target reactive ion beam sputter-deposition under the mixed atmosphere of argon and oxygen on the sealing coat; The sputtering sedimentation air pressure of described vanadium oxide layer is 0.05～0.08Pa;
The 3rd step obtained silicon nitride, as protective layer adopting silicon target reactive sputter-deposition under argon and nitrogen mixture atmosphere on the vanadium oxide layer; Sputtering sedimentation air pressure is 0.05～0.1Pa;
The 4th step deposited final vacuum annealing, and annealing temperature is controlled at 350～450 ℃.
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| CN102910837A (en) * | 2012-10-16 | 2013-02-06 | 中国科学院上海技术物理研究所 | Intelligent low-emissivity coated glass capable of offline tempering and preparation method thereof |
| CN102953482A (en) * | 2011-08-31 | 2013-03-06 | 深圳光启高等理工研究院 | Glass curtain wall |
| CN103158290A (en) * | 2011-12-12 | 2013-06-19 | 三星康宁精密素材株式会社 | Method of manufacturing thermochromic substrate |
| CN103507389A (en) * | 2012-06-27 | 2014-01-15 | 三星康宁精密素材株式会社 | Method of manufacturing thermochromic window |
| CN103692730A (en) * | 2013-12-17 | 2014-04-02 | 河北省沙河玻璃技术研究院 | Thermochromic smart window and preparation method thereof |
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| CN104310799A (en) * | 2014-10-18 | 2015-01-28 | 中山市创科科研技术服务有限公司 | Vanadium dioxide membranous layer glass and preparation method thereof |
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| CN106143520A (en) * | 2015-03-27 | 2016-11-23 | 中国科学院广州能源研究所 | A kind of energy-saving glass that can be used for bullet train side window and preparation method thereof |
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| JP2019162747A (en) * | 2018-03-19 | 2019-09-26 | トヨタ自動車株式会社 | Method for producing heat-radiation structure |
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| CN103692730A (en) * | 2013-12-17 | 2014-04-02 | 河北省沙河玻璃技术研究院 | Thermochromic smart window and preparation method thereof |
| CN104310798A (en) * | 2014-10-10 | 2015-01-28 | 武汉理工大学 | Preparation method of thermotropic reflective infrared coated glass |
| CN104310799A (en) * | 2014-10-18 | 2015-01-28 | 中山市创科科研技术服务有限公司 | Vanadium dioxide membranous layer glass and preparation method thereof |
| CN106150290A (en) * | 2015-03-27 | 2016-11-23 | 中国科学院广州能源研究所 | A kind of thermocolour intelligent dimming energy-saving glass and preparation method thereof |
| CN106143520A (en) * | 2015-03-27 | 2016-11-23 | 中国科学院广州能源研究所 | A kind of energy-saving glass that can be used for bullet train side window and preparation method thereof |
| CN106150290B (en) * | 2015-03-27 | 2018-04-10 | 中国科学院广州能源研究所 | A kind of thermocolour intelligent dimming energy-saving glass and preparation method thereof |
| CN104775101A (en) * | 2015-04-22 | 2015-07-15 | 武汉理工大学 | Preparation method and application of porous vanadium dioxide thin film |
| CN104775101B (en) * | 2015-04-22 | 2017-06-13 | 武汉理工大学 | A kind of preparation method and application of loose structure vanadium dioxide film |
| JP2018025745A (en) * | 2016-07-27 | 2018-02-15 | 株式会社リコー | Multilayer film, multilayer film composite, optical component, and window |
| JP2019162747A (en) * | 2018-03-19 | 2019-09-26 | トヨタ自動車株式会社 | Method for producing heat-radiation structure |
| JP7084172B2 (en) | 2018-03-19 | 2022-06-14 | トヨタ自動車株式会社 | Manufacturing method of heat radiation structure |
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Application publication date: 20110427 |