CN109455947A - Self-cleaning, antifog, heat-insulated coated glass of one kind and preparation method thereof - Google Patents

Self-cleaning, antifog, heat-insulated coated glass of one kind and preparation method thereof Download PDF

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Publication number
CN109455947A
CN109455947A CN201910019890.3A CN201910019890A CN109455947A CN 109455947 A CN109455947 A CN 109455947A CN 201910019890 A CN201910019890 A CN 201910019890A CN 109455947 A CN109455947 A CN 109455947A
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CN
China
Prior art keywords
substrate
layer
cleaning
antifog
self
Prior art date
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CN201910019890.3A
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Chinese (zh)
Inventor
简明德
王乾廷
董俊豪
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Fujian University of Technology
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Fujian University of Technology
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Priority to CN201910019890.3A priority Critical patent/CN109455947A/en
Publication of CN109455947A publication Critical patent/CN109455947A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • C03C17/3447—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a halide
    • C03C17/3452—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a halide comprising a fluoride
    • 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)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention discloses a kind of self-cleaning, antifog, heat-insulated coated glasses and preparation method thereof, glass includes substrate, the surface of substrate is equipped with composite film, composite film is by sequentially including internal layer, middle layer and outer layer except interior, internal layer is silicon dioxide layer, middle layer is silica+diamond-like rock layers, and outer layer is fluorinated dlc layer.Glass of the invention has good self-cleaning, antifog and heat insulating function, while the bond strength between film layer is high.

Description

Self-cleaning, antifog, heat-insulated coated glass of one kind and preparation method thereof
Technical field
The present invention relates to coated glass fields, more particularly to a kind of self-cleaning, antifog, heat-insulated coated glass and its preparation side Method.
Background technique
Glass is amorphous inorganic non-metallic material, and usually with a variety of inorganic minerals, (such as quartz sand, borax, boric acid, weight are brilliant Stone, barium carbonate, lime stone, feldspar, soda ash etc.) be primary raw material, additionally incorporate made of a small amount of auxiliary material, it is main at It is divided into silica and other oxides.The chemical composition of simple glass is Na2SiO3、CaSiO3、SiO2Or Na2OCaO6SiO2 Deng, it is a kind of non-crystalline solids of random structure that main component, which is silicate double salt, be widely used in building, be used to every Wind light transmission.With silica (SiO2) it as the inorganic thin film material of glass surface is a good selection, because of titanium dioxide Silicon is a kind of inorganic material, and physics, chemical property are stablized, and heat-resisting, wearability and mechanical property are good.Its ingredient inherently glass One important component of basis material can generate good combination with glass surface, and film is not easy to peel off.In addition, two Silicon oxide surface is easy to produce OH group, and its film is porous, therefore has good hydrophily.But single use two When silicon oxide film, surface be easy to be killed in a disaster volatilization grease type or other organic pollutants accompanying by, block its micropore, make glass Glass surface loses hydrophily and forms hydrophobic surface, and moisture can not come in glass surface drawout, and glass just loses anti-fog effect. There is no self-cleaning effects for silica itself, not can effectively prevent and remove the difficult volatile organic compounds of glass surface.If SiO2Layer is used as outermost layer, since film surface is rich in hydrophilic radical (Si-OH), easily absorbs the steam of ambient enviroment, leads to tunic Light transmittance decline.Furthermore the dust in air is also easily adsorbed in film surface layer, if film do not have self-cleaning performance will Film transmission rate is impacted.Therefore, Yao Shixian glass surface is permanently effective antifog, and single silica dioxide coating is not Capable.
Summary of the invention
The purpose of the present invention is to provide a kind of high self-cleaning, antifog, the heat-insulated coated glass of film layer conjugation and its preparations Method.
To achieve the above object, the invention adopts the following technical scheme:
The surface of a kind of self-cleaning, antifog, heat-insulated coated glass, including substrate, substrate is equipped with composite film, composite film By sequentially including internal layer, middle layer and outer layer except interior, the internal layer is silicon dioxide layer, and middle layer is silica+eka-gold Hard rock layer, outer layer are fluorinated dlc layer.
The silicon dioxide layer with a thickness of 20-50nm.
The silica+diamond-like rock layers are with a thickness of 10-30nm.
The fluorinated dlc layer with a thickness of 50-80nm.
The substrate with a thickness of 3-7mm.
Method for glass preparation of the present invention the following steps are included:
1) substrate is cleaned with cleaning machine；
2) internal layer: sending substrate into coating chamber, rf magnetron sputtering silicon dioxide layer, and the temperature of substrate is 25-60 DEG C, is born Bias 100-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, silica target current 2-4A, argon flow 15- 25mL/min, sputtering time 45-135min, radio-frequency power 100-300W, titanium dioxide silicon target and base distance between plates are 40- 60mm；
3) middle layer: continuing rf magnetron sputtering silica+diamond-like rock layers, and the temperature of substrate is 25-60 DEG C, negative bias Press 100-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, silica target current 2-4A, carbon target electric current 2-4A, argon Throughput is 15-25mL/min, sputtering time 10-50min, radio-frequency power 100-300W, titanium dioxide silicon target, carbon target and base Distance between plates is 40-60mm；
4) outer layer: continuing rf magnetron sputtering fluorinated dlc layer, and the temperature of substrate is 25-60 DEG C, back bias voltage 100- 150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, carbon target electric current 2-4A, CHF3Throughput is 5-10mL/min, argon gas Flow is 15-25mL/min, sputtering time 10-50min, radio-frequency power 100-300W, and carbon target and base distance between plates are 40- 60mm。
The invention adopts the above technical scheme, has the advantages that
1、SiO2Layer has refractive index low, and there is chemical property to stablize, and film adhesion is strong, can generate with substrate surface good The features such as good combination, wearability is good, while being ideal reflection-reducing material；There is high rejection rate in infrared light district, visible The transmitance of light Qu Yougao has high absorptivity in ultra-violet (UV) band, so that glass surface has good insulative properties.
2, all there are diamond-like rock layers in middle layer and outer layer, diamond-like rock layers have hardness height, wearability good and good The transparency；F-DLC layer surface can be low simultaneously, has waterproof and anti-adhesive properties, and self-cleaning performance is excellent；Furthermore diamond-like Layer also has hydrophobic surface, has good anti-fog function；Therefore, diamond-like rock layers can make glass surface have it is splendid from Clean, anti-fog function.
3, there is identical ingredient to carry out transition between two neighboring film layer, can effectively improve the knot between adjacent film layers in this way Close intensity.
Detailed description of the invention
The present invention is described in further details below in conjunction with the drawings and specific embodiments:
Fig. 1 is schematic diagram of the invention.
Specific embodiment
As shown in Figure 1, a kind of self-cleaning, antifog, heat-insulated coated glass of the present invention, including substrate 1, set on the surface of substrate 1 There is a composite film, for composite film by sequentially including internal layer 2, middle layer 3 and outer layer 4 except interior, the internal layer is silicon dioxide layer (SiO2Layer), middle layer is silica+diamond-like rock layers (SiO2+ DLC layer), outer layer is fluorinated dlc layer (F-DLC Layer).
Wherein, substrate with a thickness of 3-7mm, silicon dioxide layer with a thickness of 20-50nm, silica+diamond-like rock layers With a thickness of 10-30nm, fluorinated dlc layer with a thickness of 50-80nm.
Embodiment 1, method for glass preparation of the present invention the following steps are included:
1) substrate is cleaned with cleaning machine；
2) substrate internal layer: is sent into coating chamber, rf magnetron sputtering SiO2Layer, the temperature of substrate are 25 DEG C, back bias voltage 100V, operating air pressure 0.2Pa, substrate revolving speed 2rpm, silica target current 2A, argon flow 15mL/min, sputtering time For 10min, radio-frequency power 100W, titanium dioxide silicon target and base distance between plates are 40mm；
3) middle layer: continue rf magnetron sputtering SiO2+ DLC layer, the temperature of substrate are 25 DEG C, back bias voltage 100V, work Air pressure 0.2Pa, substrate revolving speed 2rpm, silica target current 2A, carbon target electric current 2A, argon flow 15mL/min, when sputtering Between be 10min, radio-frequency power 100W, titanium dioxide silicon target, carbon target and base distance between plates are 40mm；
4) outer layer: continue rf magnetron sputtering F-DLC layers, the temperature of substrate is 25 DEG C, back bias voltage 50V, operating air pressure 0.2Pa, substrate revolving speed 2rpm, carbon target electric current 2A, CHF3Throughput is 5mL/min, argon flow 15mL/min, sputtering time For 10min, radio-frequency power 100W, carbon target and base distance between plates are 40mm.
Embodiment 2, method for glass preparation of the present invention the following steps are included:
1) substrate is cleaned with cleaning machine；
2) substrate internal layer: is sent into coating chamber, rf magnetron sputtering SiO2Layer, the temperature of substrate are 40 DEG C, back bias voltage 120V, operating air pressure 0.8Pa, substrate revolving speed 5rpm, silica target current 4A, argon flow 20mL/min, sputtering time For 30min, radio-frequency power 300W, titanium dioxide silicon target and base distance between plates are 50mm；
3) middle layer: continue rf magnetron sputtering SiO2+ DLC layer, the temperature of substrate are 40 DEG C, back bias voltage 120V, work Air pressure 0.8Pa, substrate revolving speed 5rpm, silica target current 4A, carbon target electric current 4A, argon flow 20mL/min, when sputtering Between be 30min, radio-frequency power 300W, titanium dioxide silicon target, carbon target and base distance between plates are 50mm；
4) outer layer: continue rf magnetron sputtering F-DLC layers, the temperature of substrate is 40 DEG C, back bias voltage 120V, operating air pressure 0.8Pa, substrate revolving speed 5rpm, carbon target electric current 4A, CHF3 throughput are 7mL/min, argon flow 20mL/min, sputtering time For 30min, radio-frequency power 300W, carbon target and base distance between plates are 50mm.
Embodiment 3, method for glass preparation of the present invention the following steps are included:
1) substrate is cleaned with cleaning machine；
2) substrate internal layer: is sent into coating chamber, rf magnetron sputtering SiO2Layer, the temperature of substrate are 60 DEG C, back bias voltage 150V, operating air pressure 1Pa, substrate revolving speed 8rpm, silica target current 4A, argon flow 25mL/min, sputtering time are 50min, radio-frequency power 300W, titanium dioxide silicon target and base distance between plates are 60mm；
3) middle layer: continue rf magnetron sputtering SiO2+ DLC layer, the temperature of substrate are 60 DEG C, back bias voltage 150V, work Air pressure 1Pa, substrate revolving speed 8rpm, silica target current 4A, carbon target electric current 4A, argon flow 25mL/min, sputtering time For 50min, radio-frequency power 300W, titanium dioxide silicon target, carbon target and base distance between plates are 60mm；
4) outer layer: continue rf magnetron sputtering F-DLC layers, the temperature of substrate is 60 DEG C, back bias voltage 150V, operating air pressure 1Pa, substrate revolving speed 8rpm, carbon target electric current 4A, CHF3Throughput is 10mL/min, argon flow 25mL/min, sputtering time For 50min, radio-frequency power 300W, carbon target and base distance between plates are 60mm.
In order to verify self-cleaning, antifog, the heat-insulated film plating layer of one kind made from preparation method of the present invention, in the various embodiments described above Composite film is tested for the property, it is known that, fluorinated diamond-like carbon films layer preparation of the present invention is with existing traditional DLC film Comparison, carries out technique, light transmittance, Contact-angle measurement, micro-structure, the detection of heat-insulated film plating layer, adhesion test result is as follows table:

Claims (6)

1. a kind of self-cleaning, antifog, heat-insulated coated glass, including substrate, the surface of substrate is equipped with composite film, composite film by It sequentially include internal layer, middle layer and outer layer except interior, it is characterised in that: the internal layer is silicon dioxide layer, and middle layer is dioxy SiClx+diamond-like rock layers, outer layer are fluorinated dlc layer.
2. self-cleaning, antifog, the heat-insulated coated glass of one kind according to claim 1, it is characterised in that: the silicon dioxide layer With a thickness of 20-50nm.
3. self-cleaning, antifog, the heat-insulated coated glass of one kind according to claim 1, it is characterised in that: the silica+ Diamond-like rock layers with a thickness of 10-30nm.
4. self-cleaning, antifog, the heat-insulated coated glass of one kind according to claim 1, it is characterised in that: the fluorination diamond-like Rock layers with a thickness of 50-80nm.
5. self-cleaning, antifog, the heat-insulated coated glass of one kind according to claim 1, it is characterised in that: the thickness of the substrate For 3-7mm.
6. the preparation method of glass according to claim 1, it is characterised in that: the preparation method comprises the following steps:
1) substrate is cleaned with cleaning machine；
2) internal layer: substrate is sent into coating chamber, rf magnetron sputtering silicon dioxide layer, the temperature of substrate is 25-60 DEG C, back bias voltage 100-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, silica target current 2-4A, argon flow 15-25mL/ Min, sputtering time 45-135min, radio-frequency power 100-300W, titanium dioxide silicon target and base distance between plates are 40-60 mm；
3) middle layer: continuing rf magnetron sputtering silica+diamond-like rock layers, and the temperature of substrate is 25-60 DEG C, back bias voltage 100-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, silica target current 2-4A, carbon target electric current 2-4A, argon gas Flow is 15-25mL/min, sputtering time 10-50min, radio-frequency power 100-300W, titanium dioxide silicon target, carbon target and substrate Between distance be 40-60 mm；
4) outer layer: continuing rf magnetron sputtering fluorinated dlc layer, and the temperature of substrate is 25-60 DEG C, back bias voltage 100-150V, Operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, carbon target electric current 2-4A, CHF3Throughput is 5-10mL/min, and argon flow is 15-25mL/min, sputtering time 10-50min, radio-frequency power 100-300W, carbon target and base distance between plates are 40-60 mm.
CN201910019890.3A 2019-01-09 2019-01-09 Self-cleaning, antifog, heat-insulated coated glass of one kind and preparation method thereof Pending CN109455947A (en)

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CN201910019890.3A CN109455947A (en) 2019-01-09 2019-01-09 Self-cleaning, antifog, heat-insulated coated glass of one kind and preparation method thereof

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107475667A (en) * 2017-08-16 2017-12-15 信利光电股份有限公司 A kind of high hydrophobic DLC film and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107475667A (en) * 2017-08-16 2017-12-15 信利光电股份有限公司 A kind of high hydrophobic DLC film and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
汤顺清等: "《无机生物材料学》", 31 October 2008, 华南理工大学出版社 *

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Application publication date: 20190312