CN114890689A - Oxidation-resistant silver-based LOW-E membrane surface laminated glass and preparation method thereof - Google Patents

Oxidation-resistant silver-based LOW-E membrane surface laminated glass and preparation method thereof Download PDF

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Publication number
CN114890689A
CN114890689A CN202210486163.XA CN202210486163A CN114890689A CN 114890689 A CN114890689 A CN 114890689A CN 202210486163 A CN202210486163 A CN 202210486163A CN 114890689 A CN114890689 A CN 114890689A
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China
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silver
layer
laminated glass
based low
film
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Inventor
陈忠根
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Zhejiang Jufeng Glass Co ltd
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Zhejiang Jufeng Glass Co ltd
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Priority to CN202210486163.XA priority Critical patent/CN114890689A/en
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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
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/06—Joining glass to glass by processes other than fusing
    • C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10165—Functional features of the laminated safety glass or glazing
    • B32B17/10174—Coatings of a metallic or dielectric material on a constituent layer of glass or polymer
    • B32B17/1022—Metallic coatings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/306—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1284—Application of adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0004—Cutting, tearing or severing, e.g. bursting; Cutter details
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0012—Mechanical treatment, e.g. roughening, deforming, stretching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/162—Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • C03C17/3626—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 one layer at least containing 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
    • 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
    • C03C17/3644—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 metal being silver
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Surface Treatment Of Glass (AREA)
  • Laminated Bodies (AREA)

Abstract

The application relates to the technical field of laminated glass, and particularly discloses anti-oxidation silver-based LOW-E membrane laminated glass and a preparation method thereof. The visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass obtained by the method are respectively 92.3%, 90.9% and 59h to the maximum, the radiance is 0.050% to the minimum, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved.

Description

Oxidation-resistant silver-based LOW-E membrane surface laminated glass and preparation method thereof
Technical Field
The application relates to the field of laminated glass, in particular to oxidation-resistant silver-based LOW-E membrane surface laminated glass and a preparation method thereof.
Background
Laminated glass, also known as laminated glass, is a composite glass product formed by sandwiching one or more organic polymer intermediate films between two or more pieces of glass, and permanently bonding the glass and the intermediate films into a whole after special high-temperature prepressing and high-temperature high-pressure processing. The laminated glass can prevent the falling time caused by the puncture or penetration of the fragments, and the safety of the glass is improved. In addition, laminated glass has excellent anti-seismic invasion capacity and is widely applied to the fields of buildings and automobiles.
The LOW-E film surface laminated glass, also called LOW-radiation glass, is a film system product formed by plating a plurality of layers of metal or other compounds on the surface of the glass, and the film plating layer has the characteristics of high transmission of visible light and high reflection of far infrared rays with the wavelength of 4.5-25 mu m, so that the LOW-E film surface laminated glass has excellent heat insulation effect and good light transmission compared with common glass and traditional film plating glass for buildings. However, the metal film layer in the low-emissivity glass is easy to be oxidized, and the appearance color of the low-emissivity glass is changed, so that the lighting, heat insulation, attractiveness and other factors of the building are all adversely affected.
Disclosure of Invention
In order to improve the oxidation resistance of the LOW-E film surface laminated glass, the application provides oxidation-resistant silver-based LOW-E film surface laminated glass and a preparation method thereof.
In a first aspect, the application provides an oxidation-resistant silver-based LOW-E membrane surface laminated glass, which adopts the following technical scheme: the utility model provides an anti-oxidation silver base LOW-E membrane face laminated glass, an anti-oxidation silver base LOW-E membrane face laminated glass which characterized in that: the silver-based LOW-E film surface laminated glass comprises two LOW-E glass single sheets and films embedded in the two LOW-E glass single sheets, wherein the two LOW-E glass single sheets respectively comprise a glass substrate and a coating layer plated on one surface of the glass substrate, and the coating layer comprises a zirconium oxide layer, a first silicon nitride layer, a first nickel-chromium layer, a first tantalum layer, a silver base layer, a second tantalum layer, a second nickel-chromium layer and a second silicon nitride layer from top to bottom; the raw material of the zirconia layer comprises 90-100 parts of zirconia; the raw materials of the first silicon nitride layer and the second silicon nitride layer respectively comprise 95-98 parts by weight of silicon nitride; the first nickel-chromium layer and the second nickel-chromium layer respectively comprise 90-100 parts by weight of nickel and chromium; the first tantalum layer and the second tantalum layer respectively comprise 90-100 parts by weight of tantalum; the silver-based layer includes 90-100 parts by weight of silver.
By adopting the technical scheme, the coating layer comprises a zirconium oxide layer, a first silicon nitride layer, a first nickel-chromium layer, a first tantalum layer, a silver base layer, a second tantalum layer, a second nickel-chromium layer and a second silicon nitride layer from top to bottom.
The zirconia layer is a hard film with high refraction and LOW absorption extinction coefficient, and is used as an outer protective layer, so that the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved, the silver-based LOW-E film surface laminated glass can be better combined with an adjacent film layer, and the wear resistance and the weather resistance of the silver-based LOW-E film surface laminated glass are improved. In addition, the zirconium oxide layer plays a role in antireflection in visible light and near-infrared solar spectrums, so that the solar energy transmittance is improved, and the silver base layer is protected.
The silver base layer is stronger in oxidation resistance than copper and aluminum, but the silver base layer is soft in texture and easy to scratch, the bonding force with the glass substrate is poor, and the silver base layer is easy to corrode by water vapor in the air, so that the first silicon nitride layer and the second silicon nitride layer of the dielectric layer are added on two sides of the silver base layer for protection, the bonding force between the silver base layer and the glass plate is improved, and the optical performance and the color effect of the whole coating layer are adjusted.
The first silicon nitride layer and the second silicon nitride layer are used as dielectric layers, the silicon nitride is used as a raw material, and the silicon nitride has high hardness, is wear-resistant and high-temperature oxidation-resistant, and can improve the oxidation resistance of the silver-based LOW-E film surface laminated glass.
The nickel-chromium layer serves as a shielding layer and can prevent the silver-based layer from being oxidized. The tantalum layer is used as a stable layer, so that the silver base layer can be prevented from being easily damaged at high temperature, the surface appearance of the coating layer is changed, the surface roughness is reduced, and the heat resistance of the coating layer is improved.
This application sets up the coating film layer to top-down including zirconia layer, first silicon nitride layer, first nickel-chromium layer, first tantalum layer, silver-based layer, second tantalum layer, second nickel-chromium layer and second silicon nitride layer, and the cooperation of multilayer coating film has improved silver-based LOW-E membrane face laminated glass's oxidation resistance.
Preferably, the method comprises the following steps: the first and second silicon nitride layers further include 2-5 parts by weight of aluminum and 1-3 parts by weight of trifluoroacetic acid.
By adopting the technical scheme, the aluminum has good electrical conductivity, thermal conductivity and radiation resistance and good optical performance, and the bonding force between the first silicon nitride layer and the adjacent layer and the bonding force between the second silicon nitride layer and the adjacent layer can be improved by adding the aluminum. The addition of trifluoroacetic acid can improve the visible light transmittance of the film coating layer reduced by the addition of aluminum and the LOW radiation performance of the silver-based LOW-E film surface laminated glass.
Preferably, the method comprises the following steps: the silver-based layer raw material also comprises 1-3 parts by weight of lead and 1-3 parts by weight of molybdenum.
By adopting the technical scheme, the phenomenon that the silver-based layer is aggregated into islands at high temperature can be improved by lead, the oxidation resistance is improved, but the conductivity is reduced after the lead is added, so that the conductivity of the silver-based layer is improved by adding molybdenum.
Preferably, the method comprises the following steps: the silver-based layer raw material also comprises 10-20 parts by weight of 2, 5-di-tert-butylhydroquinone.
By adopting the scheme, the tert-butyl hydroquinone has the characteristics of high efficiency and good thermal stability, and has higher oxidation resistance.
Preferably, the method comprises the following steps: the silver-based layer raw material also comprises 5-8 parts by weight of phosphoric acid.
By adopting the technical scheme, the phosphoric acid is added into the silver-based layer raw material, so that the oxidation activity of the tert-butyl hydroquinone can be enhanced, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved.
Preferably, the method comprises the following steps: the zirconia layer also includes 2 to 5 parts by weight iridium.
By adopting the technical scheme, the iridium has hard texture, higher gas resistance, salt resistance, water corrosion resistance and oxidation resistance, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved.
Preferably, the method comprises the following steps: one of a PVB film, an SGP film, an EVA film and a TPU film is selected from the films.
In a second aspect, the present application provides a method for preparing any one of the above oxidation-resistant silver-based LOW-E film surface laminated glasses, which is specifically realized by the following technical scheme:
a preparation method of oxidation-resistant silver-based LOW-E membrane surface laminated glass comprises the following operation steps:
carrying out ultrasonic cleaning on a glass substrate, drying, carrying out magnetron sputtering on one surface of the glass substrate in sequence to form a zirconium oxide layer, a first silicon nitride layer, a first nickel-chromium layer, a first tantalum layer, a silver base layer, a second tantalum layer, a second nickel-chromium layer and a second silicon nitride layer, and cooling to obtain a LOW-E glass single sheet;
cutting and edging the LOW-E glass single sheets, cleaning and drying, laminating the two LOW-E glass single sheets and the film, prepressing and exhausting, discharging air between the LOW-E glass single sheets and the film, and forming under high pressure to obtain the silver-based LOW-E film surface laminated glass.
Preferably, the method comprises the following steps: the thickness of the zirconium oxide coating is 10-15 nm.
Preferably, the method comprises the following steps: the film coating thickness of the first nickel-chromium layer is 8-12nm, the film coating thickness of the first tantalum layer is 1-3nm, the film coating thickness of the silver base layer is 8-10nm, the film coating thickness of the second tantalum layer is 1-3nm, and the film coating thickness of the second nickel-chromium layer is 8-12 nm.
In summary, the present application includes at least one of the following beneficial technical effects:
(1) according to the application, by controlling the structure of the coating layer, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass are respectively 80.5%, 78.3% and 48h, which are higher than those of the embodiment 1, the lowest radiance is 0.076%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved under the condition of ensuring the basic performance of the silver-based LOW-E film surface laminated glass.
(2) According to the application, the aluminum and the trifluoroacetic acid are added into the raw materials of the first silicon nitride layer and the second silicon nitride layer, so that the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass are respectively 80.9%, 78.5% and 50h, the lowest radiation rate is 0.070%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is further improved.
(3) According to the application, the lead and the molybdenum are added into the silver-based layer raw material, so that the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass are respectively 90.5%, 87.9% and 51h, the lowest radiance is 0.067%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved.
(4) According to the application, on the basis of adding lead and molybdenum into a silver-based layer raw material, 2, 5-di-tert-butyl hydroquinone is added, so that the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass are respectively 91.4%, 89.8% and 53h, the lowest radiance is 0.063%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is further improved.
(5) According to the application, on the basis of adding lead, molybdenum and 2, 5-di-tert-butyl hydroquinone into a silver-based layer raw material, phosphoric acid is added, so that the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass are respectively 91.9%, 90.3% and 57h, the lowest radiance is 0.053%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved.
(6) According to the application, the iridium is added into the zirconia layer raw material, so that the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass are respectively 92.3%, 90.9% and 59h, the lowest radiance is 0.050%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved.
Detailed Description
The present application will be described in further detail with reference to specific examples.
The following raw materials are all commercially available products, and are all sufficient for disclosure of the raw materials in the present application, and should not be construed as limiting the source of the raw materials. The method specifically comprises the following steps: the content of effective substances in the zirconium dioxide target material is 99 percent; the content of effective substances in the silicon nitride target material is 99.9 percent; the nickel-chromium alloy target material has the effective content ratio of nickel to chromium of 80: 20; the content of effective substances in the tantalum target material is 99.9 percent; the content of effective substances in the silver target material is 99.999 percent.
The film can be any one of a PVB film, an SGP film, an EVA film and a TPU film, and all performance indexes of the silver-based LOW-E film surface laminated glass can be expected.
Example 1
The silver-based LOW-E film surface laminated glass of the example 1 is prepared by the following operation steps:
carrying out ultrasonic cleaning on a glass substrate, drying, and carrying out magnetron sputtering on one surface of the glass substrate to form a zirconium oxide layer, a first silicon nitride layer, a first nickel-chromium layer, a first tantalum layer, a silver base layer, a second tantalum layer, a second nickel-chromium layer and a second silicon nitride layer in sequence;
the zirconia layer is made of zirconia target material; the raw materials of the first silicon nitride layer and the second silicon nitride layer are silicon nitride targets respectively; the first nickel-chromium layer and the second nickel-chromium layer are respectively nickel-chromium alloy target materials; the first tantalum layer and the second tantalum layer are respectively tantalum target materials; the silver base layer is a silver target material;
the coating thickness of the zirconium oxide layer is 15nm, the coating thickness of the first silicon nitride layer is 20nm, the coating thickness of the first nickel-chromium layer is 12nm, the coating thickness of the first tantalum layer is 3nm, the coating thickness of the silver base layer is 10nm, the coating thickness of the second tantalum layer is 3nm, the coating thickness of the second nickel-chromium layer is 12nm, the coating thickness of the second silicon nitride layer is 20nm, and cooling is carried out to obtain a LOW-E glass single sheet;
cutting and edging the LOW-E glass single sheet, cleaning and drying, laminating the two LOW-E glass single sheets and the film, prepressing and exhausting, discharging air between the LOW-E glass single sheet and the PVB film, and forming under high pressure to obtain the silver-based LOW-E film surface laminated glass.
Example 2
The silver-based LOW-E membrane surface laminated glass of the embodiment 2 has the same preparation method as the silver-based LOW-E membrane surface laminated glass of the embodiment 1, and is characterized in that the raw materials of the first silicon nitride layer and the second silicon nitride layer also comprise aluminum and trifluoroacetic acid, and the mass ratio of the aluminum to the silicon nitride target is 1: 25; the weight ratio of the trifluoroacetic acid to the silicon nitride target material is 1:15, and the types and the doping amount of the other raw materials are the same as those in the embodiment 1.
Example 3
The silver-based LOW-E film surface laminated glass of the embodiment 3 has the same preparation method as the embodiment 2, and is characterized in that the silver-based layer raw material also comprises lead and molybdenum, and the mass ratio of the aluminum to the silicon nitride target is 1: 45; the weight ratio of the trifluoroacetic acid to the silicon nitride target material is 1:35, and the types and the doping amount of the other raw materials are the same as those in the embodiment 2.
Example 4
The silver-based LOW-E film surface laminated glass of the embodiment 4 has the same preparation method as the embodiment 2, and is different in that the silver-based layer raw material also comprises 2, 5-di-tert-butyl hydroquinone, the weight ratio of the 2, 5-di-tert-butyl hydroquinone to the silver target material is 1:8, and the types and the doping amount of the other raw materials are the same as the embodiment 2.
Example 5
The silver-based LOW-E film surface laminated glass of the embodiment 5 has the same preparation method as the embodiment 2, and is different in that the silver-based layer raw material also comprises phosphoric acid, the weight ratio of the phosphoric acid to the silver target material is 1:15, and the types and the doping amount of the other raw materials are the same as the embodiment 2.
Example 6
The silver-based LOW-E film surface laminated glass of the embodiment 6 has the same preparation method as the embodiment 3, and is different in that the silver-based layer raw material also comprises 2, 5-di-tert-butyl hydroquinone, the weight ratio of the 2, 5-di-tert-butyl hydroquinone to the silver target material is 1:8, and the types and the doping amount of the other raw materials are the same as the embodiment 3.
Example 7
The silver-based LOW-E film surface laminated glass of the embodiment 7 has the same preparation method as the embodiment 4, and is different in that the silver-based layer raw material also comprises phosphoric acid, the weight ratio of the phosphoric acid to the silver target material is 1:15, and the types and the doping amount of the other raw materials are the same as the embodiment 4.
Example 8
The silver-based LOW-E film surface laminated glass of the embodiment 8 has the same preparation method as the embodiment 6, and is characterized in that the silver-based layer raw material also comprises phosphoric acid, the weight ratio of the phosphoric acid to the silver target material is 1:15, and the types and the doping amount of the other raw materials are the same as the embodiment 6.
Example 9
The silver-based LOW-E film surface laminated glass of the embodiment 9 has the same preparation method as the embodiment 8, and is characterized in that the raw materials of the zirconia layer also comprise iridium, the mass ratio of the iridium to the zirconia target material is 1:35, and the types and the doping amount of the other raw materials are the same as the embodiment 8.
Comparative example 1
The silver-based LOW-E film surface laminated glass of the comparative example 1 is completely the same as the preparation method of the example 1, and the difference is that: the first nickel-chromium layer and the second nickel-chromium layer were not sputtered, and the remaining raw materials and the amounts thereof were the same as in example 1.
Comparative example 2
The silver-based LOW-E film surface laminated glass of the comparative example 2 is completely the same as the preparation method of the example 1, and the difference is that: the first tantalum layer and the second tantalum layer were not sputtered, and the remaining raw materials and the doping amount were the same as those in example 1.
Comparative example 3
The silver-based LOW-E film surface laminated glass of the comparative example 3 is completely the same as the preparation method of the example 1, and the difference is that: the first zirconia layer was replaced with a nickel target material, and the remaining raw materials and the amounts of the added materials were the same as in example 1.
Comparative example 4
The silver-based LOW-E film surface laminated glass of the comparative example 4 is completely the same as the preparation method of the example 1, and the difference is that: the first tantalum layer and the second tantalum layer were replaced with iron targets, and the remaining raw materials and the doping amount were the same as in example 1.
Performance detection
The following detection standards or methods are adopted to respectively carry out performance detection on the silver-based LOW-E membrane surface laminated glass obtained in different examples 1-9 and comparative examples 1-4, and the detection results are shown in Table 1.
Visible light transmittance: and testing the visible light transmittance of the silver-based LOW-E film surface laminated glass before and after wear resistance by using a visible light transmittance tester.
Emissivity: and (3) detecting the radiance of the silver-based LOW-E film surface laminated glass according to GB/T2680-94 'determination of visible light transmittance, sunlight direct transmittance, solar total transmittance, ultraviolet transmittance and related window glass parameters' of architectural glass.
And (3) oxidation resistance time: and (5) staining sweat on the surface of the silver-based LOW-E membrane surface laminated glass, and recording the time for the silver-based LOW-E membrane surface laminated glass to be oxidized.
TABLE 1 Performance test results of different silver-based LOW-E film surface laminated glasses
Figure BDA0003630043840000061
Figure BDA0003630043840000071
The detection results in the table 1 show that the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass obtained by the method are respectively 92.3%, 90.9% and 59h at most; the lowest radiance of the silver-based LOW-E film surface laminated glass obtained by the method is 0.050%, and the oxidation resistance of the silver-based LOW-E film surface laminated glass is improved under the condition that the basic performance of the silver-based LOW-E film surface laminated glass is ensured.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 1 and the example 2, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 2 are respectively 80.9 percent, 78.5 percent and 50h, which are higher than those of the silver-based LOW-E film surface laminated glass of the example 1, and the radiation rate is at least 0.070 percent and lower than that of the silver-based LOW-E film surface laminated glass of the example 1, which shows that the addition of aluminum and trifluoroacetic acid in the raw materials of the first silicon nitride layer and the second silicon nitride layer can improve the wear resistance, the visible light transmittance and the oxidation resistance of the silver-based LOW-E film surface laminated glass, reduce the radiation rate, possibly have good electrical conductivity, thermal conductivity and radiation resistance with aluminum, and have good optical performance, and the addition of aluminum can improve the bonding force of the first silicon nitride layer and the second silicon nitride layer with the adjacent layer. The addition of trifluoroacetic acid can improve the visible light transmittance of the film coating layer reduced by adding aluminum and the LOW radiation performance of the silver-based LOW-E film surface laminated glass.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 2 and the example 3, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 3 are respectively 90.5 percent, 87.9 percent and 51h, which are all higher than those of the silver-based LOW-E film surface laminated glass of the example 2, and the radiance is 0.067 percent at the lowest and is lower than that of the example 2, which shows that the addition of lead and molybdenum in the silver-based layer raw material can improve the wear resistance, the visible light transmittance and the oxidation resistance of the silver-based LOW-E film surface laminated glass, reduce the radiance, possibly relate to the phenomenon that lead can improve the aggregation of the silver-based layer into islands at high temperature and simultaneously improve the oxidation resistance, but the conductivity can be reduced after the addition of lead, so the addition of molybdenum can improve the conductivity of the silver-based layer.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 4 and the example 2, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 4 are respectively 90.9 percent, 88.1 percent and 52 hours, which are all higher than those of the silver-based LOW-E film surface laminated glass of the example 2, the radiance is 0.061 percent at the lowest and is lower than that of the example 2, which shows that the wear resistance and the visible light transmittance of the silver-based LOW-E film surface laminated glass can be improved and the radiance is reduced by adding 2, 5-di-tert-butyl hydroquinone into the silver-based layer raw material, and the silver-based LOW-E film surface laminated glass is probably related to the characteristics of high efficiency and good thermal stability of the 2, 5-tert-butyl hydroquinone and has higher oxidation resistance.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 2 and the example 5, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 5 are respectively 91.0 percent, 89.3 percent and 52 hours which are higher than those of the example 2, and the results show that the addition of the phosphoric acid into the silver-based layer raw material can improve the wear resistance and the visible light transmittance of the silver-based LOW-E film surface laminated glass, but the addition of the phosphoric acid only has little influence on the oxidation resistance of the silver-based LOW-E film surface laminated glass.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 3 and the silver-based LOW-E film surface laminated glass of the example 6, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 6 are respectively 91.4 percent, 89.8 percent and 53h, which are all higher than those of the silver-based LOW-E film surface laminated glass of the example 3, and the radiation rate is 0.063 percent at the lowest and is lower than that of the example 3, which shows that the wear resistance, the visible light transmittance and the oxidation resistance of the silver-based LOW-E film surface laminated glass can be further improved and the radiation rate can be reduced by adding 2, 5-di-tert-butyl hydroquinone on the basis of adding lead and molybdenum into the silver-based layer raw materials.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 7 and the example 4, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 7 are respectively 91.5 percent, 90.0 percent and 53h, which are all higher than those of the example 4, and the radiation rate is at least 0.058 percent and lower than that of the example 4, which shows that the adding of the 2, 5-di-tert-butyl hydroquinone and the adding of the phosphoric acid into the silver-based layer raw material improves the wear resistance, the visible light transmittance and the oxidation resistance of the silver-based LOW-E film surface laminated glass and reduces the radiation rate. It may be associated with phosphoric acid that enhances the oxidation activity of tertiary butyl hydroquinone, thereby improving the oxidation resistance of silver-based LOW-E membrane face-laminated glass.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 8 and the example 6, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 8 are respectively 91.9 percent, 90.3 percent and 57h, which are all higher than those of the silver-based LOW-E film surface laminated glass of the example 6, and the radiation rate is 0.053 percent at the lowest and is lower than that of the silver-based glass of the example 6, which shows that the addition of phosphoric acid on the basis of the addition of lead, molybdenum and 2, 5-di-tert-butyl hydroquinone in the silver-based layer raw material can further improve the wear resistance, the visible light transmittance and the oxidation resistance of the silver-based LOW-E film surface laminated glass and reduce the radiation rate.
Combining the performance test data of the silver-based LOW-E film surface laminated glass of the example 9 and the example 8, the visible light transmittance before wear resistance, the visible light transmittance after wear resistance and the oxidation resistance time of the silver-based LOW-E film surface laminated glass of the example 9 are respectively 92.3 percent, 90.9 percent and 59h, which are respectively higher than those of the silver-based LOW-E film surface laminated glass of the example 8, and the radiation rate is at least 0.050 percent and lower than that of the silver-based LOW-E film surface laminated glass of the example 8, and the addition of iridium into the zirconia layer raw material can further improve the wear resistance, the visible light transmittance and the oxidation resistance of the silver-based LOW-E film surface laminated glass and reduce the radiation rate. Possibly related to the hard texture of iridium, higher gas resistance, salt resistance, water corrosion resistance and oxidation resistance, and the improvement of the oxidation resistance of the silver-based LOW-E film surface laminated glass.
In addition, by combining various index data of the terylene fabrics in comparative examples 1-4 and example 1, the oxidation resistance of the silver-based LOW-E film surface laminated glass can be improved to different degrees by the first nickel-chromium layer, the second nickel-chromium layer, the first tantalum layer, the second tantalum layer and the first zirconium oxide layer which are arranged on the film coating layer.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (10)

1. An oxidation-resistant silver-based LOW-E membrane surface laminated glass is characterized in that: the silver-based LOW-E film surface laminated glass comprises two LOW-E glass single sheets and films embedded in the two LOW-E glass single sheets, wherein the two LOW-E glass single sheets respectively comprise a glass substrate and a coating layer plated on one surface of the glass substrate, and the coating layer comprises a zirconium oxide layer, a first silicon nitride layer, a first nickel-chromium layer, a first tantalum layer, a silver base layer, a second tantalum layer, a second nickel-chromium layer and a second silicon nitride layer from top to bottom; the raw material of the zirconia layer comprises a zirconia target material; the raw materials of the first silicon nitride layer and the second silicon nitride layer respectively comprise a silicon nitride target material; the first nickel-chromium layer and the second nickel-chromium layer respectively comprise a nickel-chromium alloy target material; the first tantalum layer and the second tantalum layer respectively comprise a tantalum target material; the silver base layer includes a silver target material.
2. The oxidation-resistant silver-based LOW-E film face laminated glass according to claim 1, wherein: the first silicon nitride layer and the second silicon nitride layer further comprise aluminum and trifluoroacetic acid, and the mass ratio of the aluminum to the silicon nitride target is 1: (20-30); the material weight ratio of the trifluoroacetic acid to the silicon nitride target is 1: (10-20).
3. The oxidation-resistant silver-based LOW-E film face laminated glass according to claim 1, wherein: the silver-based layer raw material also comprises lead and molybdenum, and the weight ratio of the lead to the silver target material is 1: (40-50); the material weight ratio of the molybdenum to the silver target is 1: (30-40).
4. The oxidation-resistant silver-based LOW-E membrane face laminated glass according to claim 1, characterized in that: the silver base layer raw material also comprises 2, 5-di-tert-butyl hydroquinone, and the mass ratio of the 2, 5-di-tert-butyl hydroquinone to the silver target is 1: (5-10).
5. The oxidation-resistant silver-based LOW-E film face laminated glass according to claim 1, wherein: the silver base layer raw material also comprises phosphoric acid, and the mass ratio of the phosphoric acid to the silver target is 1: (12-18).
6. The oxidation-resistant silver-based LOW-E film face laminated glass according to claim 1, wherein: the zirconia layer further comprises iridium, and the mass ratio of the iridium to the zirconia target material is 1: (20-50).
7. The oxidation-resistant silver-based LOW-E film side laminated glass according to claim 1, wherein the film is one selected from PVB film, SGP film, EVA film and TPU film.
8. The method for preparing the oxidation-resistant silver-based LOW-E film surface laminated glass according to any one of claims 1 to 7, which is characterized by comprising the following operation steps:
carrying out ultrasonic cleaning on a glass substrate, drying, carrying out magnetron sputtering on a zirconium oxide layer, a first silicon nitride layer, a first nickel-chromium layer, a first tantalum layer, a silver base layer, a second tantalum layer, a second nickel-chromium layer and a second silicon nitride layer on one surface of the glass substrate in sequence, and cooling to obtain a LOW-E glass single sheet;
cutting and edging the LOW-E glass single sheets, cleaning and drying, laminating the two LOW-E glass single sheets and the film, prepressing and exhausting, discharging air between the LOW-E glass single sheets and the film, and forming under high pressure to obtain the silver-based LOW-E film surface laminated glass.
9. The oxidation-resistant silver-based LOW-E film face laminated glass according to claim 8, wherein: the thickness of the zirconium oxide coating is 10-15 nm.
10. The oxidation-resistant silver-based LOW-E film face laminated glass according to claim 8, wherein: the coating thickness of the first nickel-chromium layer is 8-12nm, the coating thickness of the first tantalum layer is 1-3nm, the coating thickness of the silver base layer is 8-10nm, the coating thickness of the second tantalum layer is 1-3nm, and the coating thickness of the second nickel-chromium layer is 8-12 nm.
CN202210486163.XA 2022-05-06 2022-05-06 Oxidation-resistant silver-based LOW-E membrane surface laminated glass and preparation method thereof Pending CN114890689A (en)

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