CN113998900B - Manufacturing method of magnetron sputtering solar control film toughened glass - Google Patents
Manufacturing method of magnetron sputtering solar control film toughened glass Download PDFInfo
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- CN113998900B CN113998900B CN202111437409.6A CN202111437409A CN113998900B CN 113998900 B CN113998900 B CN 113998900B CN 202111437409 A CN202111437409 A CN 202111437409A CN 113998900 B CN113998900 B CN 113998900B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/012—Tempering or quenching glass products by heat treatment, e.g. for crystallisation; Heat treatment of glass products before tempering by cooling
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/04—Tempering or quenching glass products using gas
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
- C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Surface Treatment Of Glass (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to the technical field of solar control film glass, and particularly relates to a manufacturing method of magnetron sputtering solar control film toughened glass. The method comprises the steps of sequentially sputtering a silicon nitride layer, a zinc oxide layer, a chromium nitride layer and a silicon nitride layer on a glass substrate by magnetron sputtering to obtain solar control film glass, and then sending the solar control film glass into a tempering furnace for physical tempering to obtain the magnetron sputtering solar control film tempered glass; the tempering process comprises preheating treatment, heating treatment and cooling treatment; wherein the temperature of the preheating treatment is 550-580 ℃, the temperature of the heating treatment is 650-680 ℃, and the temperature of the cooling treatment is 30-40 ℃. Compared with the prior art, the manufacturing method of the magnetron sputtering solar control film toughened glass can efficiently prepare the light control film toughened glass with soft and transparent color tone, small chromatic aberration, small bending degree and uniform and firm film layer.
Description
Technical Field
The invention belongs to the technical field of solar control film glass, and particularly relates to a manufacturing method of magnetron sputtering solar control film toughened glass.
Background
Compared with common glass, the solar control film glass has lower transmittance and higher reflectivity and is widely applied to industries such as buildings and the like. In recent years, the market has made more demanding demands on the visual perception of solar control film glasses, requiring modern perception, soft silver gray tone, and good through perception.
In addition, in order to meet the requirements of safety regulations, the solar control film glass applied to public places such as buildings is usually required to be tempered to improve strength and optimize crushing state.
However, the solar control film glass has the characteristics that the solar control film glass is different from common glass in heat transfer in the tempering process, and the solar control film glass is heated unevenly on two sides due to the existence of a single-side coating layer, so that the glass is easy to bend. In addition, the tempering needs to be subjected to a physical change process of heating and cooling, and the problems of weak film binding force, large chromatic aberration, poor uniformity and the like are easily caused.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a manufacturing method of magnetron sputtering solar control film toughened glass.
The invention provides a manufacturing method of magnetron sputtering solar control film toughened glass, which comprises the steps of sequentially performing magnetron sputtering on a silicon nitride layer, a zinc oxide layer, a chromium nitride layer and a silicon nitride layer on a glass substrate to obtain solar control film glass, and then sending the solar control film glass into a toughening furnace for physical toughening to obtain the magnetron sputtering solar control film toughened glass; the tempering process comprises preheating treatment, heating treatment and cooling treatment; wherein the temperature of the preheating treatment is 550-580 ℃, the temperature of the heating treatment is 650-680 ℃, and the temperature of the cooling treatment is 30-40 ℃.
Further, according to the manufacturing method of the magnetron sputtering solar control film toughened glass, before the toughening process, cutting, edging and cleaning are carried out on the glass.
Further, in the manufacturing method of the magnetron sputtering solar control film toughened glass, during preheating treatment, the solar film glass is preheated in the preheating section of the convection toughening furnace, the heating time of the preheating furnace is 180-200 s, and the solar film glass is heated by convection generated by the convection fan.
Further, in the manufacturing method of the magnetron sputtering solar control film toughened glass, during heating treatment, the solar film glass is heated in the heating section of the convection tempering furnace, and the heating time of the heating furnace is 180-200 s.
Further, in the manufacturing method of the magnetron sputtering solar control film toughened glass, the cooling time is 120s during cooling treatment, the wind pressure of the upper air grid is 3800Pa, and the wind pressure of the lower air grid is 3300Pa.
Further, according to the manufacturing method of the magnetron sputtering solar control film toughened glass, the first layer of coating film of the solar control film glass is manufactured by sputtering silicon nitride on a dry and clean glass substrate by adopting a rotary cathode, wherein the gas component is argon and nitrogen in a volume ratio of = 15:100, and the magnetron sputtering SiNx layer is performed under the vacuum condition under the condition that the gas pressure is kept at 2.5bar, and SiAl is sputtered by adopting an alternating-current intermediate-frequency power supply and nitrogen as reactive gases.
Further, the manufacturing method of the magnetron sputtering solar control film toughened glass is that the second layer of coating film for manufacturing the solar control film glass adopts rotary cathode sputtering ZnO x The gas composition is argon to oxygen volume ratio=15:100, and under vacuum condition, the gas pressure is kept to be 2.5bar state for magnetron sputtering ZnO x Layer, sputtering ZnO by using AC intermediate frequency power supply and nitrogen as reactive gas x 。
Further, the method for manufacturing the magnetron sputtering solar control film toughened glass comprises the step of manufacturing a third layer of coating film of the solar control film glass by adopting planar cathode sputtering CrN x The gas composition is argon to nitrogen volume ratio=15:100, and the magnetron sputtering CrN is carried out under the vacuum condition under the condition that the gas pressure is kept to be 3.0bar x And sputtering Cr on the layer by using a direct current power supply.
Further, in the method for manufacturing the magnetron sputtering solar control film toughened glass, the fourth layer of coating film of the solar control film glass is manufactured by sputtering silicon nitride by adopting a rotary cathode, the gas component is argon to nitrogen volume ratio=15:100, and the magnetron sputtering SiN is kept under the vacuum condition, and the gas pressure is kept to be 2.5bar x And sputtering SiAl on the layer by using an alternating-current intermediate-frequency power supply and nitrogen as reactive gases.
The beneficial effects are that: compared with the prior art, the method for manufacturing the magnetron sputtering solar control film toughened glass ensures that the solar control film glass with obvious difference in heating at two sides can be toughened with high quality by optimizing the depth of the technology in the toughening stage, avoids the defects of bending, chromatic aberration and the like, and effectively shortens the toughening time. In addition, the method for manufacturing the magnetron sputtering solar control film toughened glass can manufacture the silicon nitride layer, the zinc oxide layer, the chromium nitride layer and the silicon nitride layer with firm and stable film layers on the glass substrate in batches through optimizing the depth of the magnetron sputtering process, so that the manufactured solar control film glass presents soft and transparent silver gray tone, and each coating can well resist adverse effects caused by temperature difference change in the subsequent toughening stage.
Drawings
Fig. 1 is a schematic structural diagram of a magnetron sputtering solar control film tempered glass.
In the figure, 1 is a silicon nitride layer, 2 is a zinc oxide layer, 3 is a chromium nitride layer, and 4 is a silicon nitride layer.
Detailed Description
The invention is further illustrated by the following specific examples, which are intended to illustrate the problem and to explain the invention, without limiting it.
A method for manufacturing magnetron sputtering solar control film toughened glass is disclosed in fig. 1, wherein a silicon nitride layer, a zinc oxide layer, a chromium nitride layer and a silicon nitride layer are sequentially subjected to magnetron sputtering on a glass substrate to obtain solar control film glass, and then the solar control film glass is sent into a toughening furnace for physical toughening to obtain the magnetron sputtering solar control film toughened glass.
The coating phase comprises the following steps:
1) Selecting a glass substrate, cutting the glass substrate into a specified size, placing the glass substrate on a conveyor belt, conveying the glass substrate along with the conveyor belt into a cleaning chamber, and cleaning the glass substrate by deionized water.
2) The cleaned glass substrate is conveyed along with a conveyer belt and enters a vacuum drying box for drying.
3) And sputtering a first layer of silicon nitride on the glass substrate by adopting a rotating cathode along with the conveying of the conveying belt in the No. 1 coating chamber.
4) Sputtering a second layer of ZnO on the glass substrate coated in the step 3) in a No. 1 coating chamber by adopting a rotating cathode x 。
5) Conveying the glass substrate coated in the step 4) to a No. 1 coating chamber, and sputtering a third layer of CrN by adopting a planar cathode x 。
6) And (3) conveying the glass substrate coated in the step (5) to a No. 2 coating chamber, and sputtering a fourth layer of silicon nitride by adopting a rotating cathode.
7) And (3) coating in the No. 3 coating chamber is completed, and conveying the glass substrate to a detection chamber for qualification detection of the low-emissivity coated glass.
8) And conveying the qualified glass substrates to the next process, carrying out waste picking treatment on the unqualified glass substrates, and placing the unqualified glass substrates on a waste picking special frame.
Specifically, in the step 3), siNx layers with the thickness of 10-120nm are subjected to magnetron sputtering in a 1# film plating chamber under the vacuum condition, wherein the gas component is argon and the nitrogen volume ratio is=15:100, and the SiAl is sputtered by using an alternating-current intermediate-frequency power supply and nitrogen as reactive gases under the condition that the gas pressure is kept at 2.5 bar.
Specifically, step 4) is to adopt gas components of argon and oxygen with the volume ratio of = 15:100 in a No. 1 coating chamber, and keep the magnetron sputtering thickness of ZnO with the thickness of 5-20nm under the state of 2.5bar under the vacuum condition x Layer, sputtering ZnO by using AC intermediate frequency power supply and nitrogen as reactive gas x 。
Specifically, in step 5), in a 2# film plating chamber, the gas component is argon, the volume ratio of nitrogen is=15:100, and the magnetron sputtering thickness is 2-30nm CrN under the vacuum condition and the gas pressure is kept at 3.0bar x And sputtering Cr on the layer by using a direct current power supply.
Specifically, in the step 6), siNx layers with the thickness of 20-60nm are subjected to magnetron sputtering in a 3# film plating chamber under the vacuum condition, wherein the gas component is argon and the nitrogen volume ratio is=15:100, and SiAl is sputtered by using an alternating-current intermediate-frequency power supply and nitrogen as reactive gases under the condition that the gas pressure is kept at 2.5 bar.
The travel speed of the glass in the No. 1 coating chamber, the No. 2 coating chamber and the No. 3 coating chamber is 90cm/min.
The tempering stage comprises the following steps:
1) And cutting, edging and cleaning the sunlight film glass.
2) And conveying the treated solar film glass into a convection tempering furnace through a roller way, wherein convection fans are respectively and correspondingly arranged above a preheating section and a heating section, preheating the solar film glass in the preheating section of the convection tempering furnace, the heating time of the preheating furnace is 180-200 s, the temperature of the preheating section is 550-580 ℃, and when the solar film glass is preheated, the solar film glass is heated by convection generated by the convection fans, and the convection frequency of the convection fans is 70Hz.
3) The preheated sunlight film glass enters a heating section of a convection tempering furnace, the heating time of the heating furnace is 180-200 s, the temperature of the heating section is 650-680 ℃, and the convection frequency of a primary convection fan is 70Hz and the time is 20s; the convection frequency of the middle section convection fan is 40-50 Hz, and the duration is 110s; the convection frequency of the convection fan of the tail convection section is 30Hz and the duration is 60s.
4) Taking out the solar film glass after the heating treatment from the convection tempering furnace, sending the solar film glass to an air grid to be cooled back and forth, cooling to 30-40 ℃, wherein the cooling time is 120s, the air grid blowing time is 120s, the upper air grid wind pressure is 3800Pa, the lower air grid wind pressure is 3300Pa, the air quantity balance is controlled to be 130 yards through an encoder, the air grid opening and closing is controlled to be 26/22 yards, and then cooling to normal temperature, so that the magnetron sputtering solar film tempered glass is obtained.
In the step 2), the upper furnace body temperature of the preheating furnace is 535 ℃, 550 ℃, 560 ℃, 550 ℃, 535 ℃, and the lower furnace body temperature of the preheating furnace is 545 ℃, 560 ℃, 570 ℃, 560 ℃ and 545 ℃ in sequence.
In the step 3), the upper furnace body temperature of the heating furnace is 635 ℃, 650 ℃, 660 ℃ and 635 ℃ in sequence, and the lower furnace body temperature is 645 ℃, 660 ℃, 670 ℃, 660 ℃ and 645 ℃.
In the step 4), the air quantity balance setting number is 130, namely 87% of the air outlet of the upper air grid static pressure box is opened, and 13% of the air outlet opening of the lower air grid static pressure box is opened; the opening and closing of the air grid are 26/22 yards, namely, the distance between the air outlet of the upper air grid and the upper surface of the sunlight film glass is 17mm, and the distance between the air outlet of the lower air grid and the lower surface of the sunlight film glass is 14mm.
The above embodiments are illustrative for the purpose of illustrating the technical concept and features of the present invention so that those skilled in the art can understand the content of the present invention and implement it accordingly, and thus do not limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (5)
1. A manufacturing method of magnetron sputtering solar control film toughened glass is characterized by comprising the following steps: sequentially magnetron sputtering SiNx layer with thickness of 10-120nm and ZnO with thickness of 5-20nm on glass substrate x Layer, crN with thickness of 2-30nm x The layer and the SiNx layer with the thickness of 20-60nm are used for obtaining solar control film glass, and then the solar control film glass is sent into a tempering furnace for physical tempering, so that the magnetron sputtering solar control film tempered glass is obtained; the tempering process comprises preheating treatment, heating treatment and cooling treatment; wherein the temperature of the preheating treatment is 550-580 ℃, the temperature of the heating treatment is 650-680 ℃, and the cooling treatment is carried outThe temperature of (2) is 30-40 ℃;
sputtering SiNx on a dry and clean glass substrate by adopting a rotary cathode, wherein the gas component is argon and nitrogen in a volume ratio of = 15:100, and sputtering SiNx layer by magnetron sputtering under a vacuum condition while keeping the gas pressure at 2.5bar, and sputtering SiAl by adopting an alternating-current medium-frequency power supply and nitrogen as reactive gases;
the second layer of film coating adopts rotary cathode sputtering ZnO x The gas composition is argon to oxygen volume ratio=15:100, and under vacuum condition, the gas pressure is kept to be 2.5bar state for magnetron sputtering ZnO x Layer, sputtering ZnO by using AC intermediate frequency power supply and nitrogen as reactive gas x ；
The third layer of film coating adopts planar cathode sputtering CrN x The gas composition is argon to nitrogen volume ratio=15:100, and the magnetron sputtering CrN is carried out under the vacuum condition under the condition that the gas pressure is kept to be 3.0bar x A layer, sputtering Cr by using a direct current power supply;
a fourth layer of film coating adopts rotary cathode sputtering SiN x The gas composition was argon to nitrogen volume ratio = 15:100, and under vacuum conditions, the gas pressure was kept at 2.5bar for magnetron sputtering of SiN x Sputtering SiAl by using an alternating-current intermediate-frequency power supply and nitrogen as reactive gases;
the prepared magnetron sputtering solar control film toughened glass is silver gray.
2. The method for manufacturing magnetron sputtering solar control film tempered glass according to claim 1, wherein: and (3) cutting, edging and cleaning the solar control film glass before the tempering process.
3. The method for manufacturing magnetron sputtering solar control film tempered glass according to claim 1, wherein: and during the preheating treatment, preheating the solar control film glass in a preheating section of the convection tempering furnace, wherein the heating time of the preheating furnace is 180-200 s, and the solar control film glass is heated by convection generated by a convection fan.
4. The method for manufacturing magnetron sputtering solar control film tempered glass according to claim 1, wherein: and during heating treatment, the solar control film glass is heated in a heating section of the convection tempering furnace, and the heating time of the heating furnace is 180-200 s.
5. The method for manufacturing magnetron sputtering solar control film tempered glass according to claim 1, wherein: during cooling treatment, the cooling time is 120s, the wind pressure of the upper air grid is 3800Pa, and the wind pressure of the lower air grid is 3300Pa.
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| CN202111437409.6A CN113998900B (en) | 2021-11-30 | 2021-11-30 | Manufacturing method of magnetron sputtering solar control film toughened glass |
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| CN113998900B true CN113998900B (en) | 2023-06-20 |
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| TW219953B (en) * | 1991-09-30 | 1994-02-01 | Ppg Industries Inc | |
| JP2518129B2 (en) * | 1991-10-30 | 1996-07-24 | 旭硝子株式会社 | Heat-treated coated glass and method for producing the same |
| DE10058700A1 (en) * | 2000-11-25 | 2002-06-06 | Saint Gobain | Glass pane with a metallic reflective layer system |
| CN100345787C (en) * | 2005-08-15 | 2007-10-31 | 上海耀华皮尔金顿玻璃股份有限公司 | Sunshine control film glass series of three-layer film structure |
| CN102786231B (en) * | 2012-08-24 | 2015-04-15 | 福耀玻璃工业集团股份有限公司 | Low-eradiation coated glass available for heat treatment and sandwich glass products thereof |
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