CN112521027B - High-transmittance low-radiation coated glass and preparation process thereof - Google Patents
High-transmittance low-radiation coated glass and preparation process thereof Download PDFInfo
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- CN112521027B CN112521027B CN202011437337.0A CN202011437337A CN112521027B CN 112521027 B CN112521027 B CN 112521027B CN 202011437337 A CN202011437337 A CN 202011437337A CN 112521027 B CN112521027 B CN 112521027B
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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
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
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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
- C03C17/001—General methods for coating; Devices therefor
- C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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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
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3649—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
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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
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3657—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
- C03C17/366—Low-emissivity or solar control coatings
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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
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
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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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
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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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
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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
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention discloses high-transmittance low-radiation coated glass and a preparation process thereof, wherein the low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top, the first dielectric film consists of a tin oxide layer and a titanium dioxide layer, the outer dielectric film consists of a zinc oxide layer and a silicon aluminum alloy layer, and the functional film comprises the following raw materials in parts by weight. The polyphenyl propylene film has high transparency, is convenient to process and low in cost, does not emit toxic gases such as hydrogen chloride when incinerated, can improve the high transparency and the water resistance of glass when used on the glass film, ensures the visible light transmittance, and can improve the wear resistance and the corrosion resistance of the film by doping with the polyphenol, thereby improving the visible light transmittance of the glass.
Description
Technical Field
The invention relates to the technical field of preparation of coated glass, in particular to high-transmittance low-radiation coated glass and a preparation process thereof.
Background
The low-emissivity coated glass is a film system product formed by coating a plurality of layers of metal or other compounds on the glass, the main performance of the functional film is to increase the permeability of visible light and the high reflection performance of middle far infrared rays, and the functional film has wide application in daily life of people.
The polystyrene film has high transparency, is convenient to process and low in cost, does not emit toxic gases such as hydrogen chloride when incinerated, can improve the high transparency and the water resistance of glass when used on the glass film, and ensures the visible light transmittance, but the wear resistance and the corrosion resistance of the polystyrene film are poorer than those of the traditional polyethylene and polypropylene, and the phenomenon that the polystyrene film is worn and corroded occurs in the preparation process, so the high-transparency low-radiation coated glass and the preparation process thereof are particularly important.
Disclosure of Invention
The invention aims to provide high-transmittance low-radiation coated glass and a preparation process thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the high-transmittance low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top.
Further, the first dielectric film is composed of a tin oxide layer and a titanium dioxide layer.
The first dielectric film is composed of a tin oxide layer and a titanium dioxide layer, and only the first dielectric film is made of a metal insulating material. Is used for improving the adhesive force between the functional film and the glass and improving the transparency and the color of the glass.
Further, the outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer.
The outer dielectric film is composed of the zinc oxide layer and the silicon aluminum alloy layer, so that the reflection capability of visible light and middle and far infrared light of the glass can be improved, the transmittance of the glass is increased, the glass has the effects of low radiation and heat insulation, the outer dielectric film also has the function of protecting the functional film, the service life of the glass is prolonged, and the maintenance cost is reduced.
Further, the thickness of the first dielectric film is 0.3-0.5 mu m, and the thickness of the outer dielectric film is 0.5-0.7 mu m.
Further, the functional film comprises, by weight, 40-50 parts of polystyrene, 10-15 parts of phenol, 5-7 parts of 4-chloronitrobenzene, 2-4 parts of ultraviolet-resistant anti-aging agent, 5-7 parts of binder, 2-4 parts of plasticizer and 0.5-1 part of dispersing agent.
Further, the ultraviolet-resistant anti-aging agent is a plurality of mixtures of paranitroaniline, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
Further, the binder is any one or a mixture of more than one of siloxane, polytetrafluoroethylene and ethylcellulose.
A preparation process of high-transmittance low-emissivity coated glass comprises the following steps,
(1) Surface treatment of glass: polishing one surface of the glass to obtain a glass substrate for standby;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, heating to 90-100 ℃, stirring, reacting for 4-5h, adding deionized water, cooling to 5-8 ℃, standing for 2-3 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2-3h, and filtering to obtain a modified polystyrene mixture;
(3) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding paranitrochlorobenzene, heating to 170-180 ℃, adding potassium carbonate and copper powder, stirring, reacting for 2-3h, adding an ultraviolet-resistant anti-aging agent, heating to 200-210 ℃, stirring, reacting for 2-3h, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
according to the method, polystyrene is firstly sulfonated by adding the polystyrene into the silver sulfate and concentrated sulfuric acid mixed solution dropwise, then phenol is added for doping, so that the added phenol is excessive for ensuring full reaction, and p-nitrochlorobenzene is added for reducing the content of the phenol, so that the p-nitrochlorobenzene can absorb excessive phenol under the conditions of potassium carbonate and copper powder, the content of phenol impurities is reduced, the problem that the boiling point of the phenol cannot be reached in the subsequent vacuum drying and baking process, the residue is caused, the visible light transmittance and the low radiation performance of glass are affected is avoided, the toxic gas pollution of the phenol is reduced, and the use efficiency of raw materials is improved.
The added copper powder can influence the surface resistance of the film, but copper is easily oxidized to form copper spots, and the visible light transmittance and the mid-far infrared light reflectance are influenced, so that the oxidation resistance needs to be improved, the p-nitrochlorobenzene and the aniline can generate 4-nitrodiphenylamine, the 4-nitrodiphenylamine can be used as an anti-aging agent, the oxidation resistance of the film is improved, the copper powder oxidation speed is reduced, and the visible light transmittance of glass is ensured.
The added paranitrochlorobenzene can also react with the uvioresistant antioxidant paranitroaniline under the condition of copper powder and potassium carbonate, so that the problems of increased product impurities and reduced qualification rate caused by excessive addition of the paranitrochlorobenzene are solved, 4' -trinitrotriphenylamine can be generated, and the triphenylamine compound can be used as an infrared light absorber to improve the heat insulation performance of glass and block infrared light.
(4) Coating:
(1) tin oxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to be 1200-1500 rmp, setting the pressure of a spray gun to be 0.2-0.25MPa, spraying for 15 seconds, spraying the functional film mixed solution on the surface of a titanium dioxide layer of a glass substrate B, vacuum drying for 10-15 minutes, and baking at 90-100 ℃ to obtain a glass substrate C coated with a functional film;
(4) zinc oxide is used as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
Further, in the step (1), one surface of the glass is polished, the polished surface is smooth, deionized water and isopropanol are used for flushing after polishing, and drying is carried out after flushing for 3 times.
Furthermore, in the step (2), when the polystyrene is added for modification, the polystyrene needs to be added for 10 times, and 1/10 of the total mass ratio is added for each time, so that the reaction is ensured to be complete.
Compared with the prior art, the invention has the following beneficial effects: the polystyrene film has high transparency, is convenient to process and low in cost, does not emit toxic gases such as hydrogen chloride when incinerated, can improve the high transparency and the water resistance of glass when used on the glass film, and ensures the visible light transmittance, but the wear resistance and the corrosion resistance of the polystyrene film are poorer than those of the traditional polyethylene and polypropylene, so the polystyrene film is modified, and the wear resistance and the corrosion resistance of the film can be improved by doping the polyphenol.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The high-transmittance low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top.
The first dielectric film is composed of a tin oxide layer and a titanium dioxide layer.
The outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer.
The thickness of the first dielectric film is 0.3 mu m, and the thickness of the outer dielectric film is 0.5 mu m.
The functional film comprises the following raw materials in parts by weight.
The ultraviolet-resistant anti-aging agent is a plurality of mixtures of p-nitroaniline, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
The binder is any one or a mixture of more of siloxane, polytetrafluoroethylene and ethylcellulose.
A preparation process of high-transmittance low-emissivity coated glass comprises the following steps,
(1) Surface treatment of glass: polishing one surface of the glass, flushing with deionized water and isopropanol for 3 times, and drying to obtain a glass substrate for later use;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, adding 10 times, heating at 90 ℃ each time by 1/10 of the total mass ratio, stirring for 4 hours, adding deionized water, cooling at 5 ℃ for 2 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2 hours, and filtering to obtain a modified polystyrene mixture;
(3) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding paranitrochlorobenzene, heating to 170 ℃, adding potassium carbonate and copper powder, stirring, reacting for 2 hours, adding an ultraviolet-resistant anti-aging agent, heating to 200 ℃, stirring, reacting for 2 hours, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
(4) Coating:
(1) tin oxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to be 1200rmp, the pressure of a spray gun to be 0.2MPa, the spraying time to be 15 seconds, spraying the functional film mixed solution on the surface of a titanium dioxide layer of a glass substrate B, and carrying out vacuum drying for 10 minutes, and baking at 90 ℃ to obtain a glass substrate C coated with a functional film;
(4) zinc oxide as target, intermediate frequencyPower supply, sputtering air pressure of 4×10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
Example 2
The high-transmittance low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top.
The first dielectric film is composed of a tin oxide layer and a titanium dioxide layer.
The outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer.
The thickness of the first dielectric film is 0.4 mu m, and the thickness of the outer dielectric film is 0.6 mu m.
The functional film comprises the following raw materials in parts by weight, 45 parts of polystyrene, 13 parts of phenol, 6 parts of 4-chloronitrobenzene, 3 parts of ultraviolet-resistant anti-aging agent, 6 parts of binder, 3 parts of plasticizer and 0.7 part of dispersing agent.
The ultraviolet-resistant anti-aging agent is a plurality of mixtures of p-nitroaniline, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
The binder is any one or a mixture of more of siloxane, polytetrafluoroethylene and ethylcellulose.
A preparation process of high-transmittance low-emissivity coated glass comprises the following steps,
(1) Surface treatment of glass: polishing one surface of the glass, flushing with deionized water and isopropanol for 3 times, and drying to obtain a glass substrate for later use;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, adding 10 times, heating at 95 ℃ each time by 1/10 of the total mass ratio, stirring for 4.5 hours, adding deionized water, cooling at 7 ℃, standing for 2 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2-3h, and filtering to obtain a modified polystyrene mixture;
(4) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding paranitrochlorobenzene, heating to 175 ℃, adding potassium carbonate and copper powder, stirring, reacting for 2.5 hours, adding an ultraviolet-resistant anti-aging agent, heating to 205 ℃, stirring, reacting for 2.5 hours, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
(4) Coating:
(1) tin oxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to 1400rmp, the spray gun pressure to 0.23MPa, the spraying time to 15 seconds, spraying the functional film mixed solution on the surface of the titanium dioxide layer of the glass substrate B, and carrying out vacuum drying for 13 minutes, and baking at the baking temperature of 95 ℃ to obtain a glass substrate C coated with a functional film;
(4) zinc oxide is used as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
Example 3
The high-transmittance low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top.
The first dielectric film is composed of a tin oxide layer and a titanium dioxide layer.
The outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer.
The thickness of the first dielectric film is 0.5 mu m, and the thickness of the outer dielectric film is 0.7 mu m.
The functional film comprises the following raw materials in parts by weight, 50 parts of polystyrene, 15 parts of phenol, 7 parts of 4-chloronitrobenzene, 4 parts of ultraviolet-resistant anti-aging agent, 7 parts of binder, 4 parts of plasticizer and 1 part of dispersing agent.
The ultraviolet-resistant anti-aging agent is a plurality of mixtures of p-nitroaniline, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
The binder is any one or a mixture of more of siloxane, polytetrafluoroethylene and ethylcellulose.
A preparation process of high-transmittance low-emissivity coated glass comprises the following steps,
(1) Surface treatment of glass: polishing one surface of the glass, flushing with deionized water and isopropanol for 3 times, and drying to obtain a glass substrate for later use;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, adding 10 times, heating at 100 ℃ each time, stirring for 5 hours, adding deionized water, cooling at 8 ℃, standing for 3 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2-3h, and filtering to obtain a modified polystyrene mixture;
(5) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding paranitrochlorobenzene, heating to 180 ℃, adding potassium carbonate and copper powder, stirring, reacting for 3 hours, adding an ultraviolet-resistant anti-aging agent, heating to 210 ℃, stirring, reacting for 3 hours, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
(4) Coating:
(1) tin oxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to be 1500rmp, the spray gun pressure to be 0.25MPa, the spraying time to be 15 seconds, spraying the functional film mixed solution on the surface of the titanium dioxide layer of the glass substrate B, and carrying out vacuum drying for 15 minutes, and baking at the baking temperature of 100 ℃ to obtain a glass substrate C coated with a functional film;
(4) zinc oxide is used as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
Comparative example 1
The high-transmittance low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top.
The first dielectric film is composed of a tin oxide layer and a titanium dioxide layer.
The outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer.
The thickness of the first dielectric film is 0.5 mu m, and the thickness of the outer dielectric film is 0.7 mu m.
The functional film comprises the following raw materials in parts by weight, namely 50 parts of polystyrene, 15 parts of phenol, 4 parts of ultraviolet-resistant anti-aging agent, 7 parts of binder, 4 parts of plasticizer and 1 part of dispersing agent.
The ultraviolet-resistant anti-aging agent is a plurality of mixtures of p-nitroaniline, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
The binder is any one or a mixture of more of siloxane, polytetrafluoroethylene and ethylcellulose.
A preparation process of high-transmittance low-emissivity coated glass comprises the following steps,
(1) Surface treatment of glass: polishing one surface of the glass, flushing with deionized water and isopropanol for 3 times, and drying to obtain a glass substrate for later use;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, adding 10 times, heating at 100 ℃ each time, stirring for 5 hours, adding deionized water, cooling at 8 ℃, standing for 3 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2-3h, and filtering to obtain a modified polystyrene mixture;
(6) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding potassium carbonate and copper powder, stirring, reacting for 3 hours, adding an ultraviolet-resistant anti-aging agent, heating at 210 ℃, stirring, reacting for 3 hours, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
(4) Coating:
(1) tin oxide is used as a target, an intermediate frequency power supply and sputtering gasThe pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to be 1500rmp, the spray gun pressure to be 0.25MPa, the spraying time to be 15 seconds, spraying the functional film mixed solution on the surface of the titanium dioxide layer of the glass substrate B, and carrying out vacuum drying for 15 minutes, and baking at the baking temperature of 100 ℃ to obtain a glass substrate C coated with a functional film;
(4) zinc oxide is used as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
Comparative example 2
The high-transmittance low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are laminated from bottom to top.
The first dielectric film is composed of a tin oxide layer and a titanium dioxide layer.
The outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer.
The thickness of the first dielectric film is 0.5 mu m, and the thickness of the outer dielectric film is 0.7 mu m.
The functional film comprises the following raw materials in parts by weight, 50 parts of polystyrene, 15 parts of phenol, 7 parts of 4-chloronitrobenzene, 4 parts of ultraviolet-resistant anti-aging agent, 7 parts of binder, 4 parts of plasticizer and 1 part of dispersing agent.
The ultraviolet-resistant anti-aging agent is a plurality of mixtures of p-phenylenediamine, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
The binder is any one or a mixture of more of siloxane, polytetrafluoroethylene and ethylcellulose.
A preparation process of high-transmittance low-emissivity coated glass comprises the following steps,
(1) Surface treatment of glass: polishing one surface of the glass, flushing with deionized water and isopropanol for 3 times, and drying to obtain a glass substrate for later use;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, adding 10 times, heating at 100 ℃ each time, stirring for 5 hours, adding deionized water, cooling at 8 ℃, standing for 3 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2-3h, and filtering to obtain a modified polystyrene mixture;
(7) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding paranitrochlorobenzene, heating to 180 ℃, adding potassium carbonate and copper powder, stirring, reacting for 3 hours, adding an ultraviolet-resistant anti-aging agent, heating to 210 ℃, stirring, reacting for 3 hours, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
(4) Coating:
(1) tin oxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to be 1500rmp, the spray gun pressure to be 0.25MPa, the spraying time to be 15 seconds, spraying the functional film mixed solution on the surface of the titanium dioxide layer of the glass substrate B, and carrying out vacuum drying for 15 minutes, and baking at the baking temperature of 100 ℃ to obtain a glass substrate C coated with a functional film;
(4) zinc oxide is used as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
Experiment
Comparative examples 1 and 2 were prepared by comparing the positions of example 3, wherein p-nitrochlorobenzene was not added in comparative example 1, and p-phenylenediamine was used in comparative example 2 instead of p-nitroaniline.
Control experiments were performed on examples 1, 2, 3, comparative example 1 and comparative example 2, and light transmittance and solar light transmittance were measured using the national standard GB/T2680-1994, and the results are as follows,
list one
The visible light transmittance, refractive index and solar light transmittance and refractive index of comparative example 1 are lower than those of examples 1, 2 and 3, because comparative example 1 does not add p-nitrochlorobenzene, so that excessive phenol impurities remain in the product, the light transmittance is reduced, the oxidation speed of copper powder is high, copper spots are formed, and the functional film loses working capacity, so that the solar light transmittance and refractive index are reduced.
The reason why the visible light transmittance, refractive index and solar light transmittance and refractive index of comparative example 2 are lower than those of examples 1, 2 and 3 is that p-phenylenediamine is used in comparative example 2 instead of p-nitroaniline, so that excessive p-nitrochlorobenzene remains, and the visible light transmittance, refractive index and solar light transmittance and refractive index are reduced.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A high-transmittance low-emissivity coated glass is characterized in that: the low-radiation coated glass comprises a glass substrate, a first dielectric film, a functional film and an outer dielectric film which are arranged in a laminated manner from bottom to top; the first dielectric film consists of a tin oxide layer and a titanium dioxide layer, and the glass substrate, the tin oxide layer and the titanium dioxide layer are laminated from bottom to top; the outer dielectric film consists of a zinc oxide layer and a silicon-aluminum alloy layer, and the functional film, the zinc oxide layer and the silicon-aluminum alloy layer are laminated from bottom to top; the functional film comprises, by weight, 40-50 parts of polystyrene, 10-15 parts of phenol, 5-7 parts of 4-chloronitrobenzene, 2-4 parts of ultraviolet-resistant anti-aging agent, 5-7 parts of binder, 2-4 parts of plasticizer and 0.5-1 part of dispersing agent.
2. The high-transmittance low-emissivity coated glass of claim 1, wherein: the thickness of the first dielectric film is 0.3-0.5 mu m, and the thickness of the outer dielectric film is 0.5-0.7 mu m.
3. The high-transmittance low-emissivity coated glass of claim 1, wherein: the ultraviolet-resistant anti-aging agent is a plurality of mixtures of p-nitroaniline, N-phenyl-alpha-naphthylamine and 4-methyl-6-tertiary butyl phenol.
4. The high-transmittance low-emissivity coated glass of claim 1, wherein: the binder is any one or a mixture of more of siloxane, polytetrafluoroethylene and ethylcellulose.
5. A preparation process of high-transmittance low-emissivity coated glass is characterized by comprising the following steps of: the steps are as follows,
(1) Surface treatment of glass: polishing one surface of the glass to obtain a glass substrate for standby;
(2) Modification of polystyrene:
(1) mixing silver sulfate and concentrated sulfuric acid, adding polystyrene, heating to 90-100 ℃, stirring, reacting for 4-5h, adding deionized water, cooling to 5-8 ℃, standing for 2-3 days, and filtering to obtain polystyrene sulfonic acid solution;
(2) adding phenol and deionized water into polystyrene sulfonic acid solution, stirring, adding ammonium persulfate, stirring, reacting for 2-3h, and filtering to obtain a modified polystyrene mixture;
(3) Preparation of functional film: adding N, N-dimethylformamide into the modified polystyrene mixture obtained in the step (2), stirring, adding 4-chloronitrobenzene, heating at 170-180 ℃, adding potassium carbonate and copper powder, stirring, reacting for 2-3h, adding an ultraviolet-resistant anti-aging agent, heating at 200-210 ℃, stirring, reacting for 2-3h, cooling to room temperature, adding a binder, a dispersing agent and a plasticizer, and stirring to obtain a functional film mixed solution;
(4) Coating:
(1) tin oxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the polished surface of the glass substrate under argon to form a tin oxide layer, so as to obtain a glass substrate A;
(2) titanium dioxide is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 The mbar is deposited on the surface of the tin oxide layer of the glass substrate under argon to form a titanium dioxide layer, so that a glass substrate B is obtained;
(3) placing the functional film mixed solution obtained in the step (3) into a spin coater, setting the rotating speed to be 1200-1500 rmp, the spray gun pressure to be 0.2-0.25MPa, the spraying time to be 15 seconds, spraying the functional film mixed solution on the surface of the titanium dioxide layer of the glass substrate B, and then carrying out vacuum drying and baking for 10-15 minutes at the baking temperature of 90-100 ℃ to obtain the glass substrate C coated with the functional film;
(4) zinc oxide is used as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 mbar, depositing on the surface of the glass substrate functional film under argon to form a zinc oxide layer, thereby obtaining a glass substrate D;
(5) the silicon-aluminum alloy layer is adopted as a target, an intermediate frequency power supply is adopted, and the sputtering air pressure is 4 multiplied by 10 -3 And (3) mbar, depositing the mbar on the surface of the zinc oxide layer of the glass substrate under argon to form a silicon-aluminum alloy layer, and obtaining the high-transmittance low-radiation coated glass.
6. The process for preparing high-transmittance low-emissivity coated glass of claim 5, wherein the process comprises the steps of: in the step (1), one surface of the glass is polished, the polished surface is smooth, deionized water and isopropanol are used for flushing after polishing, and drying is carried out after flushing for 3 times.
7. The process for preparing high-transmittance low-emissivity coated glass of claim 5, wherein the process comprises the steps of: in the step (2), when the polystyrene is added for modification, the polystyrene needs to be added for 10 times, and 1/10 of the total mass ratio is added each time, so that the reaction is ensured to be complete.
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