CN103896497A - Single silver thermochromism glass and preparation method thereof - Google Patents
Single silver thermochromism glass and preparation method thereof Download PDFInfo
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- CN103896497A CN103896497A CN201210590203.1A CN201210590203A CN103896497A CN 103896497 A CN103896497 A CN 103896497A CN 201210590203 A CN201210590203 A CN 201210590203A CN 103896497 A CN103896497 A CN 103896497A
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Abstract
The invention relates to a piece of single silver thermochromism glass and a preparation method thereof. The single silver thermochromism glass comprises a glass substrate as well as a first medium layer, a bottom protecting layer, an infrared reflection layer, an upper part protecting layer and a second medium layer formed on the glass substrate, wherein one of the first medium layer and the second medium layer comprises a vanadium dioxide film layer; the other one of the first medium layer and the second medium layer is a compound medium layer. The single silver thermochromism glass has the advantages that indoor temperature and light can be intelligently adjusted.
Description
Technical field
The present invention relates to a kind of energy-saving glass, especially a kind of single silver-colored thermochromism glass and preparation method thereof.
Background technology
The implementation dynamics that reduces discharging policy along with national energy-saving strengthens and the reinforcement of people to low-carbon environment-friendly consciousness, and the application of the energy-saving glass take low emissivity glass as representative in door and window, glass curtain wall is more and more extensive.In low emissivity glass family, single silver-layer low-radiation glass of excellent performance is widely applied.
But, existing single silver-layer low-radiation glass also has some limitations, cannot realize the intellectuality of room temp and light is regulated according to the variation of environment, once for example it installs, its optical characteristics is just fixed up, can not change with the variation of envrionment conditions, therefore on comfortableness and energy-saving effect, still be short of to some extent.
Summary of the invention
In view of above-mentioned condition, being necessary to provide a kind of can carry out silver-colored thermochromism glass of list of intelligence adjusting and preparation method thereof to room temp and light.
The invention provides a kind of single silver-colored thermochromism glass; it comprises glass substrate and is formed at successively first medium layer, bottom protective layer, infrared reflecting layer, upper protective layer and the second medium layer on this glass substrate; wherein one of them of this first medium layer and this second medium layer comprises hypovanadic oxide-based thin film layer, and another is compound medium layer.
This hypovanadic oxide-based thin film layer is to be formed by the vanadium dioxide of mixing tungsten, niobium or molybdenum, wherein the doping of tungsten, niobium or molybdenum be vanadium in vanadium dioxide quality 0.5% ~ 3%.
This hypovanadic oxide-based thin film layer is to be formed by the vanadium dioxide of mixing tungsten, and the thickness of this hypovanadic oxide-based thin film layer is 20 ~ 120nm.
This infrared reflecting layer is to be formed by silver or Kufil, and the thickness of this infrared reflecting layer is 5 ~ 25nm.
This bottom protective layer or this upper protective layer are to be formed by titanium, nichrome or Ni-Ti alloy, and the thickness of this bottom protective layer or this upper protective layer is 0.5 ~ 5nm.
This bottom protective layer or this upper protective layer are to be formed by Al-Doped ZnO, and the thickness of this bottom protective layer or this upper protective layer is 2 ~ 25nm.
The present invention also provides the preparation method of the silver-colored thermochromism glass of a kind of list, and it comprises the following steps: glass substrate is provided; And on this glass substrate, deposit successively first medium layer, bottom protective layer, infrared reflecting layer, upper protective layer and second medium layer by the mode of magnetron sputtering plating; wherein one of them of this first medium layer and this second medium layer comprises hypovanadic oxide-based thin film layer, and another is compound medium layer.
Temperature in the time of this hypovanadic oxide-based thin film layer of deposition is 350 ~ 480 ℃, and the temperature while depositing other layer is room temperature.
Temperature when magnetron sputtering plating deposits each layer is room temperature, is depositing after each layer, also comprises that the glass substrate to being formed with each layer carries out tempering processing, and wherein, the temperature of tempering processing is 650 ~ 700 ℃, and the time is 1-10 minute.
Temperature when magnetron sputtering plating deposits each layer is room temperature, is depositing after each layer, also comprises that the glass substrate to being formed with each layer carries out anneal, and wherein, the temperature of annealing is 400 ~ 650 ℃, and annealing time is 20 minutes to 2 hours.
The silver-colored thermochromism glass of above-mentioned list is on the basis of heat-proof quality that retains single silver-layer low-radiation glass excellence, the variation that solar irradiation energy is seen through that the reversible transition due to semi-conductor phase and metallographic phase that also can utilize hypovanadic oxide-based thin film layer to occur near room temperature shows, realize the light thermal property that changes single silver-colored thermochromism glass according to the change of envrionment temperature, this makes single silver-colored thermochromism glass in the time being applied to material of construction, can carry out intelligence adjusting to room temp and light, and then not only can increase the comfortableness of indoor environment but also capable of reducing energy consumption.
Accompanying drawing explanation
Fig. 1 is the silver-colored thermochromism glass of the list of first embodiment of the invention schematic diagram.
Fig. 2 is the silver-colored thermochromism glass of the list of second embodiment of the invention schematic diagram.
Embodiment
Below in conjunction with drawings and Examples, silver-colored thermochromism glass of list of the present invention and preparation method thereof is described in further detail.
Refer to Fig. 1, the silver-colored thermochromism glass 100 of list of first embodiment of the invention comprises glass substrate 10 and the first medium layer 11, bottom protective layer 12, infrared reflecting layer 13, the upper protective layer 14 and second medium layer 15 that are formed at successively on glass substrate 10.Wherein one of them comprised vanadium dioxide (VO of first medium layer 11 and second medium layer 15
2) base film layer, another is compound medium layer.
Specifically in the present embodiment, first medium layer 11 is hypovanadic oxide-based thin film layers; Second medium layer 15 is compound medium layers.Wherein, first medium layer 11 can be formed by the vanadium dioxide of mixing tungsten, niobium or molybdenum, wherein the doping of tungsten, niobium or molybdenum can be vanadium in vanadium dioxide quality 0.5% ~ 3%; Preferably, first medium layer 11 is to be formed by the vanadium dioxide of mixing tungsten.And now the thickness of first medium layer 11 can be 20 ~ 120 nanometers (nm).Second medium layer 15 can be formed by metal or nonmetallic oxide compound or nitride, for example titanium oxide (TiO
2), zinc tin oxide (ZnSnO
x), stannic oxide (SnO
2), zinc oxide (ZnO), silicon oxide (SiO
2), tantalum oxide (Ta
2o
5), bismuth oxide (BiO
2), aluminum oxide (Al
2o
3), niobium oxides (Nb
2o
5), silicon nitride (Si
3n
4) or Zinc-aluminium (AZO) form.And the thickness of second medium layer 15 can be 15 ~ 80nm.
Infrared reflecting layer 13 can be formed by silver (Ag) or copper silver (AgCu) alloy.The thickness of infrared reflecting layer 13 can be 5 ~ 25nm.
Bottom protective layer 12 can be formed by metal or metal alloy respectively with upper protective layer 14, for example titanium (Ti), nickel chromium triangle (NiCr) alloy or NiTi (NiTi) alloy; And bottom protective layer 12 can be respectively 0.5 ~ 5nm with the thickness of upper protective layer 14.In another embodiment, bottom protective layer 12 also can be formed by Al-Doped ZnO (AZO) respectively with upper protective layer 14, and now bottom protective layer 12 can be respectively 2 ~ 25nm with the thickness of upper protective layer 14.
First medium layer 11 in the silver-colored thermochromism glass 100 of above-mentioned list is hypovanadic oxide-based thin film layers.Because vanadium dioxide is a kind of functional materials with phase-change characteristic, when temperature is during lower than transformation temperature, be monoclinic structure, show as characteristic of semiconductor; When temperature is during higher than transformation temperature, change cubic rutile structure into, show as metallic character.The transition process from cryogenic semiconductor to hot metal phase, the transmitance of visible region changes little, but the transmitance of infrared light region is changed significantly, the region of ultra-red transmitance of hot metal phase is compared cryogenic semiconductor and is decreased significantly mutually, and the mid and far infrared region that is particularly greater than 2500nm for wavelength almost can not see through.And the transformation between this cryogenic semiconductor phase of vanadium dioxide and hot metal phase is reversible.The temperature spot of the reversible transition between vanadium dioxide generation semi-conductor phase and metallographic phase is 68 ℃, and it is carried out to suitable doping, introduces predetermined metal ion (being tungsten, niobium or molybdenum in the present embodiment) and can reduce phase transformation temperature points near room temperature in lattice.So, the silver-colored thermochromism glass 100 of above-mentioned list, in having kept the superior heat-proof quality of single silver-layer low-radiation glass, can change sunlight infrared energy according to the variation of envrionment temperature again sees through, in the time that envrionment temperature is lower, thereby can allow sunlight see through improves room temp as far as possible, reduce the required energy consumption of heating; In the time that envrionment temperature is higher, can shield again all or part of sunlight, further play the effect of thermal resistance, reduce the required energy consumption of refrigeration, thereby realize intellectuality control and the adjusting to room temp and light.Therefore, the silver-colored thermochromism glass 100 of above-mentioned list is on the basis of heat-proof quality that retains single silver-layer low-radiation glass excellence, the variation that solar irradiation energy is seen through that the reversible transition due to semi-conductor phase and metallographic phase that also can utilize hypovanadic oxide-based thin film layer to occur near room temperature shows, realize the light thermal property that changes single silver-colored thermochromism glass 100 according to the change of envrionment temperature, this makes single silver-colored thermochromism glass 100 in the time being applied to material of construction, can carry out intelligence adjusting to room temp and light, and then not only can increase the comfortableness of indoor environment but also capable of reducing energy consumption.
Refer to Fig. 2, be depicted as the silver-colored thermochromism glass 300 of list of second embodiment of the invention.Single silver-colored thermochromism glass 300 is similar to single silver-colored thermochromism glass 100, and its difference is: second medium layer 35 is hypovanadic oxide-based thin film layers, and first medium layer 31 is compound medium layers; The thickness of second medium layer 35 can be 20 ~ 120 nanometers, and the thickness of first medium layer 31 can be 15 ~ 80nm.
The present invention also provides a kind of preparation method of two silver-colored thermochromism glass, and first it be to provide glass substrate.Wherein, glass substrate generally need to clean up, dry, and is then placed in vacuum chamber coating film area.
Then; mode by magnetron sputtering plating deposits first medium layer, bottom protective layer, infrared reflecting layer, upper protective layer and second medium layer successively on this glass substrate; wherein one of them of first medium layer and second medium layer comprises hypovanadic oxide-based thin film layer, and another is compound medium layer.
In the present embodiment, describe as hypovanadic oxide-based thin film layer as example take first medium layer.In the time of magnetron sputtering plating, the depositing temperature of first medium layer is 350 ~ 480 ℃, and the depositing temperature of bottom protective layer, infrared reflecting layer, upper protective layer and second medium layer is room temperature.The present invention is not as limit, in another embodiment, the depositing temperature of first medium layer also can be room temperature, being each layer is all at room temperature to carry out magnetron sputtering plating formation of deposits, but need the glass substrate to being formed with each layer to carry out aftertreatment having deposited after each layer, so that vanadium dioxide base film possesses thermochromic properties.The mode of aftertreatment can comprise that the glass substrate to being formed with each layer carries out tempering processing, and wherein the temperature of tempering processing is 650 ~ 700 ℃, about 1-10 minute of time; Or comprise that the glass substrate to being formed with each layer carries out anneal, wherein, the temperature of annealing is 400 ~ 650 ℃, and annealing time is 20 minutes to 2 hours.
Specific embodiment
Embodiment 1
A kind of single silver-colored thermochromism glass, its film layer structure by glass substrate outwards successively: Si
3n
4(20nm)/AZO (15nm)/AgCu (12nm)/AZO (15nm)/VO
2: W (50nm).
Prepare the method for the silver-colored thermochromism glass of this list successively:
(1) glass substrate cleans up and dries up, and is placed in vacuum sputtering district;
(2) on glass substrate, adopt the mode of magnetron sputtering to deposit Si
3n
4layer, target used is SiAl rotary target, and power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of argon gas and nitrogen, at room temperature deposition;
(3) at Si
3n
4layer adopts the mode of magnetron sputtering to deposit AZO layer above, and target used is ceramic AZO rotary target, and power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of pure argon or argon gas and oxygen, at room temperature deposition;
(4) on AZO layer, adopt the mode of magnetron sputtering to deposit AgCu layer, target used is AgCu planar target, and power supply is that direct current adds the pulse power, and power is 1 ~ 10KW, and process gas is pure argon, at room temperature deposition;
(5) on AgCu layer, adopt the mode of magnetron sputtering to deposit AZO layer, target used is ceramic AZO rotary target, and power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of pure argon or argon gas and oxygen, at room temperature deposition;
(6) on AZO layer, adopt the mode of magnetron sputtering to deposit VO
2: W layer, target used is the VO of doping W
2(W doping ratio is 1wt%) ceramic rotary target, power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of argon gas and oxygen, and when deposition, the temperature of glass substrate is 400 ℃.
Embodiment 2
A kind of single silver-colored thermochromism glass, its film layer structure by glass substrate outwards successively: VO
2: W (30nm)/NiCr (1.5nm)/Ag (11nm)/NiCr (1.5nm)/AZO (14nm)/Si
3n
4(26nm).
Prepare the method for the silver-colored thermochromism glass of this list successively:
(1) glass substrate cleans up and dries up, and is placed in vacuum sputtering district;
(2) on glass substrate, adopt the mode of magnetron sputtering to deposit VO
2: W layer, target used is the V of doping W
2o
5(W doping ratio is 1.5wt%) ceramic rotary target, power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of argon gas and oxygen, at room temperature deposition;
(3) at VO
2: above W layer, adopt the mode of magnetron sputtering to deposit NiCr layer, target used is metal NiCr planar target, and power supply is that direct current adds the pulse power, and power is 1 ~ 10KW, and process gas is pure argon, at room temperature deposition;
(4) on NiCr layer, adopt the mode of magnetron sputtering to deposit Ag layer, target used is Ag planar target, and power supply is that direct current adds the pulse power, and power is 1 ~ 10KW, and process gas is pure argon, at room temperature deposition;
(5) on Ag layer, adopt the mode of magnetron sputtering to deposit NiCr layer, target used is metal NiCr planar target, and power supply is that direct current adds the pulse power, and power is 1 ~ 10KW, and process gas is pure argon, at room temperature deposition;
(6) on NiCr layer, adopt the mode of magnetron sputtering to deposit AZO layer, target used is ceramic AZO rotary target, and power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of argon gas or argon gas and oxygen, at room temperature deposition;
(7) on AZO layer, adopt the mode of magnetron sputtering to deposit Si
3n
4layer, target used is SiAl rotary target, and power supply is intermediate frequency power supply, and power is 10 ~ 100KW, and process gas is the mixed gas of argon gas and nitrogen, at room temperature deposition;
(8) glass of making is carried out to tempering processing.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, although the present invention discloses as above with preferred embodiment, but not in order to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when can utilizing the technology contents of above-mentioned announcement to make a little change or being modified to the equivalent embodiment of equivalent variations, in every case be not depart from technical solution of the present invention content, any simple modification of above embodiment being done according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (10)
1. the silver-colored thermochromism glass of list; it comprises glass substrate; it is characterized in that; the silver-colored thermochromism glass of this list also comprises the first medium layer, bottom protective layer, infrared reflecting layer, upper protective layer and the second medium layer that are formed at successively on this glass substrate; wherein one of them of this first medium layer and this second medium layer comprises hypovanadic oxide-based thin film layer, and another is compound medium layer.
2. the silver-colored thermochromism glass of list as claimed in claim 1, is characterized in that: this hypovanadic oxide-based thin film layer is to be formed by the vanadium dioxide of mixing tungsten, niobium or molybdenum, wherein the doping of tungsten, niobium or molybdenum be vanadium in vanadium dioxide quality 0.5% ~ 3%.
3. the silver-colored thermochromism glass of list as claimed in claim 2, it is characterized in that: this hypovanadic oxide-based thin film layer is to be formed by the vanadium dioxide of mixing tungsten, and the thickness of this hypovanadic oxide-based thin film layer is 20 ~ 120nm.
4. the silver-colored thermochromism glass of list as claimed in claim 1, it is characterized in that: this infrared reflecting layer is to be formed by silver or Kufil, and the thickness of this infrared reflecting layer is 5 ~ 25nm.
5. the silver-colored thermochromism glass of list as claimed in claim 1, it is characterized in that: this bottom protective layer or this upper protective layer are to be formed by titanium, nichrome or Ni-Ti alloy, and the thickness of this bottom protective layer or this upper protective layer is 0.5 ~ 5nm.
6. the silver-colored thermochromism glass of list as claimed in claim 1, it is characterized in that: this bottom protective layer or this upper protective layer are to be formed by Al-Doped ZnO, and the thickness of this bottom protective layer or this upper protective layer is 2 ~ 25nm.
7. a preparation method for the silver-colored thermochromism glass of list, it comprises the following steps:
Glass substrate is provided; And
Mode by magnetron sputtering plating deposits first medium layer, bottom protective layer, infrared reflecting layer, upper protective layer and second medium layer successively on this glass substrate; wherein one of them of this first medium layer and this second medium layer comprises hypovanadic oxide-based thin film layer, and another is compound medium layer.
8. the preparation method of the silver-colored thermochromism glass of list as claimed in claim 7, is characterized in that: the temperature in the time of this hypovanadic oxide-based thin film layer of deposition is 350 ~ 480 ℃, and the temperature while depositing other layer is room temperature.
9. the preparation method of the silver-colored thermochromism glass of list as claimed in claim 7, it is characterized in that: temperature when magnetron sputtering plating deposits each layer is room temperature, depositing after each layer, also comprise that the glass substrate to being formed with each layer carries out tempering processing, wherein, the temperature of tempering processing is 650 ~ 700 ℃, and the time is 1-10 minute.
10. the preparation method of the silver-colored thermochromism glass of list as claimed in claim 7, it is characterized in that: temperature when magnetron sputtering plating deposits each layer is room temperature, depositing after each layer, also comprise that the glass substrate to being formed with each layer carries out anneal, wherein, the temperature of annealing is 400 ~ 650 ℃, and annealing time is 20 minutes to 2 hours.
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|---|---|---|---|
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| CN105800951A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院广州能源研究所 | Method for preparing thermochromic intelligent glass |
| CN105800955A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院广州能源研究所 | Thermochromic intelligent film and preparation method therefor |
| CN115536287A (en) * | 2022-10-21 | 2022-12-30 | 长虹美菱股份有限公司 | Heat-preservation color-changing coated glass and preparation method thereof |
| CN116655255A (en) * | 2023-08-01 | 2023-08-29 | 中国耀华玻璃集团有限公司 | Easy-to-clean temperature-induced energy-saving solar control film glass and online production method |
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| CN105800955A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院广州能源研究所 | Thermochromic intelligent film and preparation method therefor |
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| CN115536287A (en) * | 2022-10-21 | 2022-12-30 | 长虹美菱股份有限公司 | Heat-preservation color-changing coated glass and preparation method thereof |
| CN116655255A (en) * | 2023-08-01 | 2023-08-29 | 中国耀华玻璃集团有限公司 | Easy-to-clean temperature-induced energy-saving solar control film glass and online production method |
| CN116655255B (en) * | 2023-08-01 | 2023-10-13 | 中国耀华玻璃集团有限公司 | Easy-to-clean temperature-induced energy-saving solar control film glass and online production method |
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Application publication date: 20140702 |
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