CN1555989A - Autombobile windshield glass possessing infrared reflection performance and its preparation method - Google Patents
Autombobile windshield glass possessing infrared reflection performance and its preparation method Download PDFInfo
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- CN1555989A CN1555989A CNA200410000007XA CN200410000007A CN1555989A CN 1555989 A CN1555989 A CN 1555989A CN A200410000007X A CNA200410000007X A CN A200410000007XA CN 200410000007 A CN200410000007 A CN 200410000007A CN 1555989 A CN1555989 A CN 1555989A
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Abstract
An anti-fogging insulating windshield with high infrared reflectivity (more than 70%) features that a semiconductor oxide film, which may be the indium oxide film doped by tin oxide or the zinc oxide film doped by at least one of aluminium oxide, silicon oxide, boron oxide, dysprosium oxide and gallium oxide, is arranged between PVB film and the internal or external surface of glass. Its preparing processis also disclosed.
Description
Technical field
A kind of automobile wind shield glass with properties of infrared reflection and preparation method thereof relates to automobile wind shield glass design and manufacturing technology field, particularly has the design and the manufacturing technology field of the high-grade automobile wind shield glass of energy-saving heat-insulating, anti-caking mist function.
Technical background
The energy and environmental protection all are the problems that the modern society people pay close attention to the most.Especially in car and boat, cold in winter and hot in summer is a ubiquitous problem.Because common windshield does not have tangible reflex to infrared, so the glass of automobile, boats and ships becomes the important window of degradation of energy.The automobile wind shield glass that exploitation has properties of infrared reflection has very practical meaning, and it can reflect infrared ray, thereby reduces the loss of automobile energy.In addition, this automobile wind shield glass with properties of infrared reflection has certain anti-caking mist ability, energy-conserving and environment-protective more.
Windshield on the market can only satisfy the requirement in intensity and the safety now.In the middle of the present technology, also do not have the ripe automobile wind shield glass with properties of infrared reflection, but a lot of companies have been arranged, comprise world-renowned big automobile brand company, for example BMW also begins to study in this respect.The general automobiles windshield, in Fig. 1, there is PVB film (3) layer glass (1) and (4), centre, and this kind glass has stronger impact resistance, but the ability of reflected infrared is very weak.In order to reduce the loss of energy, some automobile sticks organic film or colouring on the vehicle window of side, make monolithic glass present color, can reduce heat flowing by vehicle window.But the visible light transmissivity of the glass that these methods make is very low, and the visible light transmissivity of automobile wind shield glass that is lower than national requirements is greater than 70% requirement, so be not suitable for doing automobile wind shield glass.
Summary of the invention
Purpose of the present invention, utilize the high infrared reflectivity of oxide semiconductor film and good visible light transmissivity, a kind of windshield that contains oxide semiconductor film has been proposed, this glass has higher transmittance to visible light, infrared radiation to each wavelength has higher reflectivity, and certain anti-caking mist ability is arranged again simultaneously.
Automobile wind shield glass proposed by the invention contains glass outer, inner layer glass, and in described, PVB film between the glass outer, it is characterized in that, also containing the layer of semiconductor sull between described glass outer and the described PVB film or between described inner layer glass and described PVB film, described oxide semiconductor film is the indium oxide film that is mixed with oxide of tin, perhaps be mixed with aluminium oxide, monox, boron oxide, dysprosia, at least a above zinc-oxide film in the gallium oxide, the content percent by weight total value of above-mentioned doping is 0.1%～10%.
Preparation method with automobile wind shield glass of properties of infrared reflection, it is characterized in that, it adopts magnetically controlled sputter method, with above-mentioned conductor oxidate is raw MAT'L, inside face deposited semiconductor sull at described glass outer, wherein, the operating air pressure of sputter is 0.1Pa～5.0Pa, and base vacuum pressure is less than 6.0 * 10
-3Pa, voltage are 200V～600V, and the temperature of glass substrate is room temperature～400 ℃, and the frequency limit that the midfrequent AC that is adopted suppresses power supply is 15KHz～60KHz; After the inside face of described glass outer has deposited oxide semiconductor film, itself and described PVB film and inner layer glass are carried out heat-seal, constitute automobile wind shield glass.
Another kind of preparation method with automobile wind shield glass of properties of infrared reflection, it is characterized in that, it adopts magnetically controlled sputter method, with above-mentioned conductor oxidate is raw MAT'L, inside face deposited semiconductor sull at described inner layer glass, wherein, the operating air pressure of sputter is 0.1Pa～5.0Pa, and base vacuum pressure is less than 6.0 * 10
-3Pa, voltage are 200～600V, and the temperature of glass substrate is room temperature～400 ℃, and the frequency limit that the midfrequent AC that is adopted suppresses power supply is 15KHz～60KHz; After the inside face of described inner layer glass has deposited oxide semiconductor film, itself and described PVB film and glass outer are carried out heat-seal, constitute automobile wind shield glass.
Another preparation method with automobile wind shield glass of properties of infrared reflection, it is characterized in that, it adopts magnetically controlled sputter method, with above-mentioned conductor oxidate is raw MAT'L, a deposited semiconductor sull at described PVB film, wherein, the operating air pressure of sputter is 0.1Pa～5.0Pa, and base vacuum pressure is less than 6.0 * 10
-3Pa, voltage are 200～600V, and the frequency limit that the midfrequent AC that is adopted suppresses power supply is 15KHz～60KHz; After having deposited oxide semiconductor film on the described PVB film, itself and described glass outer and inner layer glass are carried out heat-seal, constitute automobile wind shield glass.
Beneficial effect: windshield proposed by the invention has following advantage in the use of car and boat:
1,, can satisfy country and will be higher than 70% requirement the automobile wind shield glass visible light transmissivity to the high transmitance of visible light;
2, infrared radiation is had high reflectivity (greater than 70%), make glass have heat-insulating performance.Can play energy-conservation effect;
3, certain anti-caking mist ability is arranged, can guarantee the visibility of windshield to a certain extent, energy-conserving and environment-protective, the convenient use.
Description of drawings
Fig. 1 is a general-utility car windshield constructional drawing, (1) glass outer wherein, (3) PVB film, (4) inner layer glass;
Fig. 2 is a kind of constructional drawing of the automobile wind shield glass that proposes of the present invention, (1) glass outer wherein, (2) oxide semiconductor film, (3) PVB film, (4) inner layer glass;
Fig. 3 is the another kind of constructional drawing of the automobile wind shield glass that proposes of the present invention, (1) glass outer wherein, (2) oxide semiconductor film, (3) PVB film, (4) inner layer glass;
Fig. 4 is the infrared reflectivity that contains the automobile wind shield glass of different oxide semiconductor films, wherein 1 represents the zinc-gallium oxide film, and 2 represent zinc oxide dysprosium film, 3 represent the zinc oxide boron membrane, 4 represent the zinc oxide aluminum film, and 5 represent the zinc oxide silicon thin film, and 6 represent indium tin oxide films.
Fig. 5 is an anti-caking mist contrast and experiment, and Fig. 5 (a) tests through 30 hours as embodiment 7 described automobile wind shield glass, and Fig. 5 (b) is that the general-utility car windshield was through experiment in 30 hours.
The specific embodiment:
As shown in Figure 2, automobile wind shield glass proposed by the invention has the layer of semiconductor sull between glass outer and PVB film, as shown in Figure 3, the automobile wind shield glass of the present invention's proposition also can be between inner layer glass and PVB film the layer of semiconductor sull to be arranged.The preparation method of automobile wind shield glass of the present invention utilizes the method for magnetron sputtering on the outside face of the inside face of glass outer or inner layer glass or a face at the PVB film, deposition last layer oxide semiconductor film is encapsulated into windshield then.
Embodiment is as follows:
With the tin indium oxide ceramic target that contains 10% oxide of tin is raw MAT'L, adopts magnetically controlled sputter method to deposit indium tin oxide films on the thick inside face as the hot bending glass of glass outer of 3mm, and its sputtering technology is operating air pressure 1.5Pa, base vacuum 3.0 * 10
-3Pa, voltage are 350V.The midfrequent AC arc suppresses the frequency 60KHz of power supply, and glass temperature is 350 ℃.Deposition obtains the thick indium tin oxide films of 350nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 2 with 0.8mm thick PVB film and the thick hot bending glass of 4mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 1 hour, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 47.5 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
With the zinc oxide aluminum ceramic target that contains 2.0% aluminium oxide, adopt sputtering method depositing zinc oxide aluminium film on the one side of the thick PVB film of 0.8mm, its sputtering technology is operating air pressure 2.0Pa, base vacuum 0.8 * 10
-3Pa, voltage are 350V.The midfrequent AC arc suppresses the frequency 25KHz of power supply, and the PVB film is a room temperature.Deposition obtains the thick zinc oxide aluminum film of 350nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 2 with 3mm thick hot bending glass (skin) and the thick hot bending glass (internal layer) of 4mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 48.3 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
With the zinc oxide silicon ceramic target that contains 1.5% monox, adopt sputtering method at the thick hot bending deposition on glass zinc oxide silicon thin film of 3mm, its sputtering technology is operating air pressure 2.5Pa, base vacuum 4.0 * 10
-3Pa, voltage are 370V.The midfrequent AC arc suppresses the frequency 30KHz of power supply, and glass temperature is 100 ℃.Deposition obtains the thick zinc oxide silicon thin film of 300nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 2 with 0.8mm thick PVB film and the thick hot bending glass of 4mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 50.5 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
With the zinc oxide boron ceramic target that contains 3.0% boron oxide, adopt sputtering method at the thick hot bending deposition on glass zinc oxide boron membrane of 3mm, its sputtering technology is operating air pressure 3.8Pa, base vacuum 6.0 * 10
-3Pa, voltage are 380V.The midfrequent AC arc suppresses the frequency 45KHz of power supply, and glass temperature is 250 ℃.Deposition obtains the thick zinc oxide boron membrane of 100nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 2 with 0.8mm thick PVB film and the thick hot bending glass of 4mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 48.9 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
Embodiment 5
With the zinc-gallium oxide ceramic target that contains 10% gallium oxide, adopt sputtering method at the thick hot bending deposition on glass zinc-gallium oxide film of 3mm, its sputtering technology is operating air pressure 0.1Pa, base vacuum 6.0 * 10
-3Pa, voltage are 600V.The midfrequent AC arc suppresses the frequency 15KHz of power supply, and glass temperature is 400 ℃.Deposition obtains the thick zinc-gallium oxide film of 250nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 2 with 0.8mm thick PVB film and the thick hot bending glass of 4mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 51.7 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
Embodiment 6
With the zinc oxide aluminum ceramic target that contains 2.0% aluminium oxide, adopt sputtering method depositing zinc oxide aluminium film on the thick PVB film of 0.8mm, its sputtering technology is operating air pressure 5.0Pa, base vacuum 6 * 10
-3Pa, voltage are 200V.The midfrequent AC arc suppresses the frequency 25KHz of power supply, and the PVB film temperature is a room temperature.Deposition obtains the thick zinc oxide aluminum film of 400nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 2 with 3mm thick hot bending glass (skin) and the thick hot bending glass (internal layer) of 4mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 59.7 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
Embodiment 7
With the zinc-gallium oxide dysprosium ceramic target that contains 5.7% gallium oxide and 0.1% dysprosia, adopt sputtering method at the thick hot bending deposition on glass zinc-gallium oxide dysprosium film of 4mm, its sputtering technology is operating air pressure 0.8Pa, base vacuum 2.6 * 10
-3Pa, voltage are 390V.The midfrequent AC arc suppresses the frequency 45KHz of power supply, and glass temperature is 200 ℃.Deposition obtains the thick zinc-gallium oxide dysprosium film of 250nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 3 with 0.8mm thick PVB film and the thick hot bending glass of 3mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 45.3 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
Embodiment 8
With the zinc oxide dysprosium ceramic target that contains 0.1% dysprosia, adopt sputtering method at the thick hot bending deposition on glass zinc oxide dysprosium film of 4mm, its sputtering technology is operating air pressure 1.2Pa, base vacuum 2.5 * 10
-3Pa, voltage are 300V.The midfrequent AC arc suppresses the frequency 45KHz of power supply, and glass temperature is a room temperature.Deposition obtains the thick zinc oxide dysprosium film of 150nm.Then it is packaged into the automobile wind shield glass of structure as shown in Figure 3 with 0.8mm thick PVB film and the thick hot bending glass of 3mm.This automobile wind shield glass is installed on the roadlice, outside car under 35 ℃ of conditions of temperature, vehicle stationary docks at the place of sun direct projection, after the PTO Power Take Off 2 hours, the vehicle interior temperature that general-utility car windshield automobile has been installed reaches 67 ℃, and the vehicle interior temperature that automobile wind shield glass of the present invention has been installed only has 53.4 ℃.Adopting model is the visible light transmissivity of the ultraviolet-visible photometer measurement present embodiment of UV2100, and measuring it is that the visible region transmitance of 400nm～850nm is all more than 70% at wavelength.
In the present invention, the oxide semiconductor film of doping has lower electrical resistivity, is about 1.0 * 10
-3～1.0 * 10
-4Cm. Ω, thereby higher infrared reflectivity is arranged.They have better visible light transmissivity again simultaneously.Adopt FT-IR5DX type infrared spectrometer and Spectrum GX type Fourier transformation infrared spectrometer to test the infrared reflectivity of the automobile wind shield glass among the present invention who mixes, as shown in Figure 4, provided the infrared reflectivity of the automobile wind shield glass of different oxide semiconductor films, wherein 1 represent the zinc-gallium oxide film, 2 represent zinc oxide dysprosium film, and 3 represent the zinc oxide boron membrane, and 4 represent the zinc oxide aluminum film, 5 represent the zinc oxide silicon thin film, and 6 represent indium tin oxide films.As seen from the figure, the automobile wind shield glass of various oxide semiconductor thin-films all is higher than 70% for wavelength greater than the reflectivity of the infrared light of 3500nm more than.This explanation the present invention has good properties of infrared reflection.
The present invention has also passed through anti-caking mist contrast experiment.The outer temperature of car is-10 ℃, and humidity is 50%, and vehicle interior temperature is 20 ℃, and humidity is 36%, after 30 hours.Adopt embodiment 7 described automobile wind shield glass to experimentize, outside window the scenery (being No. 60 word printing characters) of looking out for the car in the vehicle window, obvious knot mist phenomenon not is as Fig. 5 (a); Adopt the general-utility car windshield to experimentize, basic all knots mist is as Fig. 5 (b).Anti-caking mist contrast experiment explanation, the present invention has certain anti-caking mist ability.
The preparation of the oxide semiconductor film layer of patent of the present invention is a method of utilizing medium frequency magnetron sputtering, also can use methods such as ion beam depositing, evaporation in addition.
Claims (4)
1, a kind of automobile wind shield glass with properties of infrared reflection, contain glass outer, inner layer glass, and in described, PVB film between the glass outer, it is characterized in that, also containing the layer of semiconductor sull between described glass outer and the described PVB film or between described inner layer glass and described PVB film, described oxide semiconductor film is the indium oxide film that is mixed with oxide of tin, perhaps be mixed with aluminium oxide, monox, boron oxide, dysprosia, at least a above zinc-oxide film in the gallium oxide, the content percent by weight total value of above-mentioned doping is 0.1%～10%.
2, a kind of preparation method with automobile wind shield glass of properties of infrared reflection, it is characterized in that, it adopts magnetically controlled sputter method, with the conductor oxidate is raw MAT'L, described conductor oxidate is to be mixed with the indium oxide of oxide of tin or to be mixed with at least a above zinc oxide in aluminium oxide, monox, boron oxide, dysprosia, the gallium oxide, and the content percent by weight total value of above-mentioned doping is 0.1%～10%; Inside face at described glass outer deposits described oxide semiconductor film, and wherein, the operating air pressure of sputter is 0.1Pa～5.0Pa, and base vacuum pressure is less than 6.0 * 10
-3Pa, voltage are 200V～600V, and the temperature of glass substrate is room temperature～400 ℃, and the frequency limit that the midfrequent AC that is adopted suppresses power supply is 15KHz～60KHz; After the inside face of described glass outer has deposited oxide semiconductor film, itself and described PVB film and inner layer glass are carried out heat-seal, constitute automobile wind shield glass.
3, a kind of preparation method with automobile wind shield glass of properties of infrared reflection, it is characterized in that, it adopts magnetically controlled sputter method, with the conductor oxidate is raw MAT'L, described conductor oxidate is to be mixed with the indium oxide of oxide of tin or to be mixed with at least a above zinc oxide in aluminium oxide, monox, boron oxide, dysprosia, the gallium oxide, and the content percent by weight total value of above-mentioned doping is 0.1%～10%; Inside face at described inner layer glass deposits described oxide semiconductor film, and wherein, the operating air pressure of sputter is 0.1Pa～5.0Pa, and base vacuum pressure is less than 6.0 * 10
-3Pa, voltage are 200～600V, and the temperature of glass substrate is room temperature～400 ℃, and the frequency limit that the midfrequent AC that is adopted suppresses power supply is 15KHz～60KHz; After the inside face of described inner layer glass has deposited oxide semiconductor film, itself and described PVB film and glass outer are carried out heat-seal, constitute automobile wind shield glass.
4, a kind of preparation method with automobile wind shield glass of properties of infrared reflection, it is characterized in that, it adopts magnetically controlled sputter method, with the conductor oxidate is raw MAT'L, described conductor oxidate is to be mixed with the indium oxide of oxide of tin or to be mixed with at least a above zinc oxide in aluminium oxide, monox, boron oxide, dysprosia, the gallium oxide, and the content percent by weight total value of above-mentioned doping is 0.1%～10%; One side at described PVB film deposits described oxide semiconductor film, and wherein, the operating air pressure of sputter is 0.1Pa～5.0Pa, and base vacuum pressure is less than 6.0 * 10
-3Pa, voltage are 200～600V, and the frequency limit that the midfrequent AC that is adopted suppresses power supply is 15KHz～60KHz; After having deposited oxide semiconductor film on the described PVB film, itself and described glass outer and inner layer glass are carried out heat-seal, constitute automobile wind shield glass.
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| CNB200410000007XA CN100346992C (en) | 2004-01-02 | 2004-01-02 | Autombobile windshield glass possessing infrared reflection performance and its preparation method |
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| FR2634753B1 (en) * | 1988-07-27 | 1992-08-21 | Saint Gobain Vitrage | GLAZING WITH ELECTRICALLY CONDUCTIVE LAYER OBTAINED BY PYROLYSIS OF POWDERED COMPOUNDS, USEFUL AS A WINDSCREEN FOR A MOTOR VEHICLE |
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