CN101289283A - TiN<x> coated glass with combined function of heat insulation and heat preservation and method for preparing same - Google Patents
TiN<x> coated glass with combined function of heat insulation and heat preservation and method for preparing same Download PDFInfo
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- CN101289283A CN101289283A CNA2008100621891A CN200810062189A CN101289283A CN 101289283 A CN101289283 A CN 101289283A CN A2008100621891 A CNA2008100621891 A CN A2008100621891A CN 200810062189 A CN200810062189 A CN 200810062189A CN 101289283 A CN101289283 A CN 101289283A
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Abstract
The invention discloses a TiNx coated glass with the functions of thermal insulation and heat preservation, and a preparation method thereof. A TiNx film on a glass substrate contains 44 percent to 59 percent of Ti and 41 percent to 56 percent of N by the atomic mol percentage and is deposited on the clean surface of the glass substrate by adopting the method of chemical vaporous deposition. The TiNx coated glass of the invention has the advantages of simple preparation technology, low production cost and high production efficiency. The TiNx film obtained by the method of the invention is uniform and compact texture, has good bonding with the glass substrate and high reflectivity both in a near-infrared region and far-infrared region, showing excellent performance of energy saving and having the function of solar light control and the performance of low radiation. Meanwhile, the rate of visible light transmission of the TiNx film can be ensured. Therefore, the TiNx film can be widely applied to various facilities requiring thermal insulation and heat preservation, such as buildings, vehicles, and the like, and can also be used in areas at high latitudes, where the weather is cold in winter, as well as in areas at low latitudes, where the weather is hot in summer.
Description
Technical field
The present invention relates to coated glass and preparation method thereof, especially have concurrently heat insulation and TiN heat insulation function
xCoated glass and preparation method thereof.
Background technology
Along with global science and technology and economic fast development, the consumption of the energy is day by day significantly increased, make problem of energy crisis become increasingly conspicuous, energy-conservationly caused the extensive concern of countries in the world as a national strategy problem.Especially in buildings, along with the ratio that the development of Building technology makes glass use is increasing, even some Highrise buildings has adopted full glass outer wall structure.At present, developed multiple energy-saving glass, the low emissivity glass that wherein has the sunlight feed glass of high-reflectivity in the near-infrared region and have high-reflectivity in the mid and far infrared district has obtained development preferably.The former has heat insulating function, is fit to the hot area and uses.The latter has heat insulation function, is fit to cold district and uses.In recent years, people focus on attention on the heat insulation coated glass of light modulation (Sun-E) that exploitation has sunlight control function and low radiation functions simultaneously.At present, generally adopt solar control film and low-radiation film MULTILAYER COMPOSITE to realize the compound of these two kinds of functions, and adopt off-line technology preparation such as magnetron sputtering, therefore this energy-efficient film cost is very high.
The TiN film has high transmittance at visible region, and in near-infrared region and mid and far infrared district higher reflectivity is arranged simultaneously, can prepare single-layer membrane structure and realize energy-efficient coated glass.But there is a reflection peak in the TiN film and causes light pollution at visible region, and simultaneously the plasma resonance point is in the near-infrared region and effect of heat insulation is not fully up to expectations.Therefore, by preparation nonstoichiometry TiN
xFilm, the optic response scope of change film makes film disappear at the reflection peak of visible region, plasma resonance point near visible region, further improves the luminous reflectance of near-infrared region, thereby improves the energy-efficient performance of film as far as possible.Surface deposition individual layer nonstoichiometry TiN
xThe glass of film makes it have sunlight control function and low radiance concurrently, realizes high-efficient energy-saving function.Can be widely used in the various facilities that need heat-insulation and heat-preservation such as various buildingss, vehicle; Both can be applied in the high latitude area of cold in winter, can be applied in the low latitudes of sweltering heat in summer again, and also can be used for the big zone of the four seasons temperature difference cold in winter and hot in summer simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of heat insulation and TiN heat insulation function of having concurrently
xCoated glass and preparation method thereof.
Of the present inventionly have heat insulation and TiN heat insulation function concurrently
xCoated glass, the TiN on its glass substrate
xFilm contains the atomic molar percentage composition: titanium elements 44%～59%, nitrogen element 41%～56%.
Usually make TiN
xThe thickness of film is 50 nanometers～350 nanometers.
Have concurrently heat insulation and TiN heat insulation function
xThe preparation method of coated glass, employing be chemical Vapor deposition process, step is as follows:
1) cleans glass substrate;
2) glass substrate is put into phase depositing reaction chamber, reaction chamber vacuumizes, and feeds rare gas element;
3) keeping under the state that vacuumizes reaction chamber being heated to 450～700 ℃;
4) with nitrogenous source with to be preheating to 41-70 ℃ titanium source be that carrier gas feeds reaction chamber with the rare gas element, the control rare gas element: nitrogenous source: the throughput ratio in titanium source is 20～100: 2～10: 1, and keep pressure in the reaction chamber in-0.02 MPa, depositing TiN on glass substrate
xThin film layer, reaction times 2～150s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature.
Among the present invention, said titanium source can be TiCl
4, TiCl
3, Ti[N (CH
3)
2]
4And Ti[N (C
2H
5)
2]
4In a kind of or its mixture.
Said nitrogenous source can be NH
3Perhaps N
2With H
2Mixed gas, or NH
3, N
2With H
2Mixed gas.
Said rare gas element can be a kind of or its mixture in nitrogen, helium, neon, argon gas and the xenon.
Among the present invention, TiN
xThe content of the titanium elements of film and nitrogen element can recently be controlled by the flow of regulating titanium source and nitrogenous source.The thickness of film can be realized by the control depositing time.
Beneficial effect of the present invention is:
The TiN of the present invention's preparation
xFilm is fine and close evenly, combine well with glass substrate.TiN
xCoated glass all has high-reflectivity in near-infrared region and mid and far infrared district, with power saving function heat insulation and insulation, can be widely used in the facility that various buildingss, vehicle etc. need heat-insulation and heat-preservation; Both can be applied in the high latitude area of cold in winter, can be applied in the low latitudes of sweltering heat in summer again, and also can be used for simultaneously the big zone of the four seasons temperature difference cold in winter and hot in summer, for people's life provides comfortable and convenient.Adopt chemical Vapor deposition process preparation technology simple, production cost is low, the production efficiency height.
Description of drawings
Fig. 1 is TiN
xThe surface topography of film;
Fig. 2 has concurrently heat insulation and TiN heat insulation function
xCoated glass is at Visible-to-Near InfaRed district reflectivity spectrogram.
Embodiment
Embodiment 1
1) cleans glass substrate;
2) glass substrate is put into phase depositing reaction chamber, reaction chamber vacuumizes, and feeds N
2
3) keeping under the state that vacuumizes reaction chamber being heated to 450 ℃;
4) with NH
3With the TiCl that is preheating to 41.2 ℃
4With N
2For carrier gas feeds reaction chamber, control NH
3And TiCl
4Flow be respectively 60 and 11.25sccm, and N
2Flow is fixed on 930sccm, keeps pressure in the reaction chamber in-0.02 MPa, depositing TiN on glass substrate
xThin film layer, reaction times 60s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature.
The TiN that this example prepares
xThe fine and close evenly (see figure 1) of film, thin film composition adopts (EDX) analytic statistics of X ray energy dispersion spectrum, wherein characterizes the content x=0.83 of N element, and promptly the atomic molar percentage composition is: titanium elements 55%, nitrogen element 45%.The Visible-to-Near InfaRed reflectance test shows, TiN
xThere is a reflection peak in coated glass at visible region, and (1050nm) locates (see figure 2) to plasma resonance point in the near-infrared region.Film is 32.6% at the average reflectance of visible region, and can reach 32.6% at the reflectivity of near-infrared region, and the square resistance of film is 234 Ω/, can guarantee that film has low radiance preferably.
Embodiment 2
1) cleans glass substrate;
2) glass substrate is put into phase depositing reaction chamber, reaction chamber vacuumizes, and feeds Ar;
3) keeping under the state that vacuumizes reaction chamber being heated to 600 ℃;
4) with NH
3With the Ti[N (CH that is preheating to 70 ℃
3)
2]
4With Ar is that carrier gas feeds reaction chamber, control NH
3And Ti[N (CH
3)
2]
4Flow be respectively 78 and 13.5sccm, and the Ar flow is fixed on 900sccm, keeps pressure in the reaction chamber in-0.02 MPa, depositing TiN on glass substrate
xThin film layer, reaction times 75s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature.
The TiN that this example prepares
xFilm is evenly fine and close, and thin film composition adopts (EDX) analytic statistics of X ray energy dispersion spectrum, wherein characterizes the content x=1.13 of N element, and promptly the atomic molar percentage composition is: titanium elements 47%, nitrogen element 53%.The Visible-to-Near InfaRed reflectance test shows, TiN
xThe film reflectance spectrum is compared with example 1 obviously " blue shift " is taken place, and the reflection peak of visible region disappears, and plasma resonance point " blue shift " is to 740nm place (see figure 2).Film is 5.48% at the average reflectance of visible region, and can reach 31.1% at the reflectivity of near-infrared region, and the square resistance of film is 11 Ω/, can guarantee that film has excellent low radiance.
Embodiment 3
1) cleans glass substrate;
2) glass substrate is put into phase depositing reaction chamber, reaction chamber vacuumizes, and feeds N
2With the Ar mixed gas;
3) keeping under the state that vacuumizes reaction chamber being heated to 700 ℃;
4) with N
2With H
2Mixed gas and be preheating to 70 ℃ Ti[N (CH
3)
2]
4With N
2With the Ar mixed gas be that carrier gas feeds reaction chamber, control N
2With H
2The flow of mixed gas be 102sccm, Ti[N (CH
3)
2]
4Flow be 13.5sccm, and N
2Be fixed on 880sccm with the Ar mixed gas flow, keep pressure in the reaction chamber in-0.02 MPa, depositing TiN on glass substrate
xThin film layer, reaction times 100s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature.
The TiN that this example prepares
xFilm is evenly fine and close, and thin film composition adopts (EDX) analytic statistics of X ray energy dispersion spectrum, wherein characterizes the content x=1.25 of N element, and promptly the atomic molar percentage composition is: titanium elements 44%, nitrogen element 56%.The Visible-to-Near InfaRed reflectance test shows, TiN
xThe film reflectance spectrum is compared with example 2 further " blue shift " is taken place, and the plasma resonance point moves to visible region (493nm) and locates (see figure 2).Film is 13.3% at the average reflectance of visible region, and can reach 55.2% at the reflectivity of near-infrared region, and the square resistance of film is 5 Ω/, can guarantee that film has excellent low radiance.
Claims (6)
1. have concurrently heat insulation and TiN heat insulation function
xCoated glass is characterized in that the TiN on the glass substrate
xFilm contains the atomic molar percentage composition: titanium elements 44%～59%, nitrogen element 41%～56%.
2. according to claim 1ly have heat insulation and TiN heat insulation function concurrently
xCoated glass is characterized in that TiN
xThe thickness of film is 50 nanometers～350 nanometers.
3. according to claim 1ly have heat insulation and TiN heat insulation function concurrently
xThe preparation method of coated glass is characterized in that step is as follows:
1) cleans glass substrate;
2) glass substrate is put into phase depositing reaction chamber, reaction chamber vacuumizes, and feeds rare gas element;
3) keeping under the state that vacuumizes reaction chamber being heated to 450～700 ℃;
4) with nitrogenous source with to be preheating to 41-70 ℃ titanium source be that carrier gas feeds reaction chamber with the rare gas element, the control rare gas element: nitrogenous source: the throughput ratio in titanium source is 20～100: 2～10: 1, and keep pressure in the reaction chamber in one 0.02 MPas, depositing TiN on glass substrate
xThin film layer, reaction times 2～150s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature.
4. according to claim 3ly have heat insulation and TiN heat insulation function concurrently
xThe preparation method of coated glass is characterized in that said titanium source is TiCl
4, TiCl
3, Ti[N (CH
3)
2]
4And Ti[N (C
2H
5)
2]
4In a kind of or its mixture.
5. according to claim 3ly have heat insulation and TiN heat insulation function concurrently
xThe preparation method of coated glass is characterized in that said nitrogenous source is NH
3Perhaps N
2With H
2Mixed gas, or NH
3, N
2With H
2Mixed gas.
6. nonstoichiometry TiN according to claim 3
xThe preparation method of film is characterized in that said rare gas element is a kind of or its mixture in nitrogen, helium, neon, argon gas and the xenon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100621891A CN101289283A (en) | 2008-06-13 | 2008-06-13 | TiN<x> coated glass with combined function of heat insulation and heat preservation and method for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100621891A CN101289283A (en) | 2008-06-13 | 2008-06-13 | TiN<x> coated glass with combined function of heat insulation and heat preservation and method for preparing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101289283A true CN101289283A (en) | 2008-10-22 |
Family
ID=40033763
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100621891A Pending CN101289283A (en) | 2008-06-13 | 2008-06-13 | TiN<x> coated glass with combined function of heat insulation and heat preservation and method for preparing same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101289283A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891400A (en) * | 2010-07-02 | 2010-11-24 | 浙江大学 | Preparation method of coated glass with self-cleaning and energy-saving functions |
| CN105800950A (en) * | 2016-03-18 | 2016-07-27 | 海南中航特玻科技有限公司 | Coated glass capable of blocking ultraviolet light efficiently and preparation method |
| CN109734332A (en) * | 2019-01-26 | 2019-05-10 | 殷红平 | A kind of low radiation coated glass and its processing technology |
| CN110518152A (en) * | 2019-09-26 | 2019-11-29 | 江苏集萃有机光电技术研究所有限公司 | Organic light emitting display panel and display device |
-
2008
- 2008-06-13 CN CNA2008100621891A patent/CN101289283A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891400A (en) * | 2010-07-02 | 2010-11-24 | 浙江大学 | Preparation method of coated glass with self-cleaning and energy-saving functions |
| CN105800950A (en) * | 2016-03-18 | 2016-07-27 | 海南中航特玻科技有限公司 | Coated glass capable of blocking ultraviolet light efficiently and preparation method |
| CN109734332A (en) * | 2019-01-26 | 2019-05-10 | 殷红平 | A kind of low radiation coated glass and its processing technology |
| CN110518152A (en) * | 2019-09-26 | 2019-11-29 | 江苏集萃有机光电技术研究所有限公司 | Organic light emitting display panel and display device |
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| PB01 | Publication | ||
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Open date: 20081022 |