CN106399940B - A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane and preparation method thereof - Google Patents

A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane and preparation method thereof Download PDF

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CN106399940B
CN106399940B CN201610634821.XA CN201610634821A CN106399940B CN 106399940 B CN106399940 B CN 106399940B CN 201610634821 A CN201610634821 A CN 201610634821A CN 106399940 B CN106399940 B CN 106399940B
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transition zone
glass substrate
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CN106399940A (en
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李宏
贺慧婷
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Wuhan University of Technology WUT
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • 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
    • C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
    • 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
    • C03C17/3642—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 containing a metal layer
    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering

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Abstract

The present invention relates to solar energy thermal-power-generating reflecting mirror material manufacturing technology fields.A kind of solar energy thermal-power-generating reflecting mirror SiO2‑Ag‑SiO2Composite membrane, which is characterized in that it includes glass substrate and the film layer being formed on glass substrate；Film layer is made of transition zone, reflecting layer and protective layer, and transition zone, reflecting layer and protective layer are successively arranged from the surface of glass substrate outward, and transition zone, reflecting layer, protective layer are made by radio-frequency magnetron sputter method；The material of the transition zone is SiO2, with a thickness of 20nm-50nm；The material in the reflecting layer is Ag, with a thickness of 100nm-200nm；The material of the protective layer is SiO2, with a thickness of 50nm-150nm.The composite membrane that this method obtains has the characteristics that high reflectance, adhesion be good and outdoor long service life.

Description

A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane and its preparation Method
Technical field
The present invention relates to solar energy thermal-power-generating reflecting mirror material manufacturing technology fields, and in particular to a kind of solar energy Hot power generation reflector SiO2-Ag-SiO2Composite membrane and preparation method thereof.
Background technique
With the shortage of the energy in world wide and the aggravation of environmental problem, renewable energy based on solar energy is ground Study carefully, develop, using increasingly being paid attention to.Solar power generation is broadly divided into photovoltaic power generation and photo-thermal power generation.Photovoltaic power generation was in the past Decades in be rapidly developed.In recent years, photo-thermal power generation was profitable with its, cleanliness without any pollution, it is stable, convenient for simultaneously Many advantages, such as entering power grid attracts attention.According to scholarly forecast, in the near future photo-thermal power generation capacity will considerably beyond photovoltaic, and It is possible that replacing conventional energy resource and widely being utilized by the mankind.Solar heat power generation system is received using large-sized solar reflecting mirror Collection solar energy be used to generate electricity, these systems economically whether it is feasible depend primarily on can develop durability it is good, reflection The mirror system that rate is high and production cost is low.Photo-thermal power station is mostly built in the area that illumination is sufficient, solar radiation is strong, such as China On the gobi and desert of the western length and breadth of land, but these area surroundings are more severe, therefore reflecting mirror in solar heat power generation system Service life will determine the cost in power station.So reflectivity is high, adhesion is good, reflecting mirror with long service life is studied at present Emphasis.
Since silver has higher reflectivity in infrared region, so it has very big potentiality to can be used as high-performance reflecting mirror Film material, however, silverskin has a very big problem to need to consider when being used as reflecting material, i.e., durability cannot be protected Card, because silverskin mechanical strength and chemical stability are all bad, it is easy to be oxidized or vulcanize, tarnish, this will lead The reduction of reflectivity is caused, therefore it is essential that layer protecting film is plated on silverskin.Further, since the attachment of Ag and substrate of glass Power is poor, and is easily corroded and falls off in some special atmosphere, so that its service performance is affected, therefore, in reality In the application of border, it is also necessary to plate one layer of dielectric layer, therebetween to improve the adhesive force in reflecting layer and substrate.But if protection Film thickness cannot be effectively controlled, and also will affect the raising of reflectivity.
High reflectance, adhesion be good in order to obtain, reflecting mirror reflecting material with long service life, and researchers carry out A series of research.Zhao Yong is praised et al. the problem of having studied the adhesive force size in the preparation process of solar concentrator film, One layer thin of chromium film is first deposited on the surface of the substrate before aluminium film is deposited, since chromium can capture oxygen and shape from oxide substrate At oxide, there is stronger chemical bond force, so greatly improving the adhesion of condenser film layer.Tetsuya Goto is used Sputtering method prepares silverskin on cyclic olefin polymer and silica respectively, using Si3N4Film makees protective layer, has obtained reflectivity High and good durability reflectance coating.Kennedy etc. makees protective layer using aluminium oxide, and silver is outermost reflector, makes its sunlight Reflectivity reach 95%.Xu Yongjun etc. uses nano silver for outermost reflector, and the reflectivity of sunlight has reached 96.74 %. Chinese patent (patent publication No.: CN102260854A) discloses a kind of self-cleaning solar energy high reflectance nano thin-film and manufacturer Method, when reflectance coating is silverskin, the reflectivity to sunlight is 94%~97%, and when reflectance coating is aluminium film, reflectivity is 90%~92%.Chinese patent (patent publication No.: CN104681662A) discloses a kind of system of high reflectance solar energy film Preparation Method, when silverskin with a thickness of 130nm and silica with a thickness of 320nm when, film reflectivity highest, sunlight and visible Light reflectivity is respectively 96.66% and 98.84%, and the wearability of membrane material and ageing resistance are good.
Summary of the invention
The technical problems to be solved by the present invention are: in order to avoid defect and shortcoming existing in the prior art, this Invention provides a kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane and preparation method thereof, what this method obtained answers Closing film has the characteristics that high reflectance, adhesion be good and outdoor long service life.
Present invention provide the technical scheme that a kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane, it is special Sign is that it includes glass substrate 1 and the film layer being formed on glass substrate；Film layer is by transition zone (or dielectric layer), anti- It penetrates layer and protective layer to constitute, transition zone, reflecting layer and protective layer are successively arranged from the surface of glass substrate 1 outward, transition zone, anti- Penetrating layer, protective layer is made by radio-frequency magnetron sputter method；The material of the transition zone 2 is SiO2, with a thickness of 20nm- 50nm；The material in the reflecting layer 3 is Ag, with a thickness of 100nm-200nm；The material of the protective layer 4 is SiO2, thickness For 50nm-150nm.
A kind of above-mentioned solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, it is characterised in that packet Include following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, washes off the impurity on surface (foul) is then washed away completely with tap water, is placed into ultrasonic cleaning 10-30min in deionized water, is finally putting into anhydrous second Ultrasonic cleaning 10-30min in alcohol [99.99% (quality) is analyzed pure], obtains glass substrate；By cleaned glass substrate It is stored in spare in dehydrated alcohol [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 0.5-1.5Pa, target-substrate distance are fixed on 60-100mm, argon flow are 40sccm, sputtering power 100-200W, sputtering time 10-30min；On the glass substrate To a transition zone；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 0.5-1.5Pa, target-substrate distance are fixed on 60-100mm, and argon flow is 40sccm, sputtering power 100-200W, sputtering time 10-30min；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 0.5-1.5Pa, target-substrate distance are fixed on 60-100mm, and argon flow is 40sccm, sputtering power 100-200W, sputtering time 20-40min；Obtain solar energy thermal-power-generating reflecting mirror SiO2- Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
The film structure prepared using this method, infrared reflectivity can achieve 99.73%, and due to SiO2The increasing of film Saturating effect, infrared reflectivity can be more than 100%.
It is tested using peeling off, with reference to adhesive force testing standard GBT9286-1998, adhesive force can achieve 0 grade (altogether 6 grades, wherein 0 grade of expression adhesion is best, 5 grades of expression adhesions are worst).
Compared with prior art, the present invention have the advantage that the film structure that (1) present invention obtains, infrared reflectivity Up to 99.73% or more.(2) especially there is good adhesion, with reference to adhesive force between film layer between film layer and glass substrate Testing standard GBT9286-1998, adhesive force can achieve 0 grade (6 grades altogether, wherein 0 grade of expression adhesion is best, 5 grades of tables Show that adhesion is worst), there is in the adverse circumstances locating for photo-thermal power station long service life.(3) process route is simple, It is suitble to industrialization large-scale production, has both saved cost, also saved maintenance cost, reduced environmental pollution.
Detailed description of the invention
Fig. 1 is a kind of solar energy thermal-power-generating reflecting mirror SiO of the present invention2-Ag-SiO2The schematic diagram of composite membrane.
Fig. 2 is the SiO in the embodiment of the present invention 12-Ag-SiO2Composite membrane reflectance map.
Fig. 3 is a kind of solar energy thermal-power-generating reflecting mirror SiO of the embodiment of the present invention 12-Ag-SiO2The attachment of composite membrane film Power test chart: where a is figure before test, and b is to scheme after testing.
Fig. 4 is the SiO in the embodiment of the present invention 22-Ag-SiO2Composite membrane reflectance map.
Fig. 5 is the SiO in the embodiment of the present invention 32-Ag-SiO2Composite membrane reflectance map.
Fig. 6 is the SiO in the embodiment of the present invention 42-Ag-SiO2Composite membrane reflectance map.
Fig. 7 is the SiO in the embodiment of the present invention 52-Ag-SiO2Composite membrane reflectance map.
Fig. 8 is the SiO in the embodiment of the present invention 62-Ag-SiO2Composite membrane reflectance map.
In Fig. 1: 1 is glass substrate, and 2 be transition zone, and 3 be reflecting layer, and 4 be protective layer.
Specific embodiment
For a better understanding of the present invention, below with reference to the example content that the present invention is furture elucidated, but the present invention is not only It is limited only to the following examples.
Embodiment 1:
A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, comprising the following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, washes off the impurity on surface (foul) is then washed away completely with tap water, is placed into ultrasonic cleaning 20min in deionized water, is finally putting into dehydrated alcohol Ultrasonic cleaning 20min in [99.99% (quality) is analyzed pure], obtains glass substrate 1；Cleaned glass substrate is saved It is spare in dehydrated alcohol [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 0.5Pa, target-substrate distance are fixed on 60mm, argon Flow is 40sccm, sputtering power 100W, sputtering time 10min；A transition zone (SiO is obtained on glass substrate 12 Film) 2, SiO2Film thickness is 30nm；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, sputtering Power is 108W, sputtering time 20min, and reflecting layer 3 (silverskin), silver film thickness 110nm are obtained on transition zone 2；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 0.5Pa, target-substrate distance are fixed on 60mm, and argon flow is 40sccm, Sputtering power is 100W, sputtering time 20min, SiO2Film thickness is 55nm；Obtain solar energy thermal-power-generating reflecting mirror SiO2- Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
1 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Composite membrane is as shown in Figure 1, the film is pressed Sequentially include:
Glass substrate 1；Transition zone (SiO2Film) 2, material SiO2, with a thickness of 30nm；Reflecting layer 3, material Ag, thickness For 110nm, protective layer 4, material SiO2, with a thickness of 55nm.
1 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Compound film system infrared reflectivity is higher than 99.76%, and due to SiO2The antireflective effect of film, infrared reflectivity are even more than 100%, and adhesive force is up to 0 grade, outdoor use Service life is long.
Embodiment 2:
A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, comprising the following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, washes off the impurity on surface (foul) is then washed away completely with tap water, is placed into ultrasonic cleaning 20min in deionized water, is finally putting into dehydrated alcohol Ultrasonic cleaning 20min in [99.99% (quality) is analyzed pure], obtains glass substrate；Cleaned glass substrate is stored in It is spare in dehydrated alcohol [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, argon Flow is 40sccm, sputtering power 150W, sputtering time 20min；A transition zone (SiO is obtained on glass substrate 12 Film) 2, SiO2Film thickness is 40nm；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, sputtering Power is 108W, sputtering time 20min, and reflecting layer 3 (silverskin), silver film thickness 110nm are obtained on transition zone 2；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, Sputtering power is 150W, sputtering time 30min, obtain protective layer (SiO2Film), SiO2Film thickness is 102nm；It finally obtains Solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
2 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Compound film system infrared reflectivity is higher than 99.81%, and due to SiO2The antireflective effect of film, infrared reflectivity are even more than 100%, and adhesive force is up to 0 grade, outdoor use Service life is long.
Embodiment 3:
A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, comprising the following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, washes off the impurity on surface (foul) is then washed away completely with tap water, is placed into ultrasonic cleaning 20min in deionized water, is finally putting into dehydrated alcohol Ultrasonic cleaning 20min in [99.99% (quality) is analyzed pure], obtains glass substrate；Cleaned glass substrate is stored in It is spare in dehydrated alcohol [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.5Pa, target-substrate distance are fixed on 100mm, Argon flow is 40sccm, sputtering power 200W, sputtering time 30min；A transition zone (SiO is obtained on the glass substrate2 Film), SiO2Film thickness is 50nm；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, sputtering Power is 108W, sputtering time 20min, and reflecting layer 3 (silverskin), silver film thickness 110nm are obtained on transition zone 2；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.5Pa, target-substrate distance are fixed on 100mm, and argon flow is 40sccm, Sputtering power is 200W, sputtering time 40min, SiO2Film thickness is 139nm；Obtain solar energy thermal-power-generating reflecting mirror SiO2- Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
3 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Compound film system infrared reflectivity is higher than 99.90%, and due to SiO2The antireflective effect of film, infrared reflectivity are even more than 100%, and adhesive force is up to 0 grade, outdoor use Service life is long.
Embodiment 4:
A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, comprising the following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, washes off the impurity on surface (foul) is then washed away completely with tap water, is placed into ultrasonic cleaning 20min in deionized water, is finally putting into dehydrated alcohol Ultrasonic cleaning 20min in [99.99% (quality) is analyzed pure], obtains glass substrate；Cleaned glass substrate is stored in It is spare in dehydrated alcohol [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, argon Flow is 40sccm, sputtering power 150W, sputtering time 20min；A transition zone (SiO is obtained on the glass substrate2Film), SiO2Film thickness is 40nm；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, sputtering Power is 160W, sputtering time 20min, and reflecting layer 3 (silverskin), silver film thickness 150nm are obtained on transition zone 2；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, Sputtering power is 150W, sputtering time 30min, SiO2Film thickness is 102nm；Obtain solar energy thermal-power-generating reflecting mirror SiO2- Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
4 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Compound film system infrared reflectivity is higher than 99.87%, and due to SiO2The antireflective effect of film, infrared reflectivity are even more than 100%, and adhesive force is up to 0 grade, outdoor use Service life is long.
Embodiment 5:
A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, comprising the following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, the impurity for washing off surface is right It is washed away completely with tap water afterwards, places into ultrasonic cleaning 10min in deionized water, be finally putting into dehydrated alcohol [99.99% (quality), analyze it is pure] in ultrasonic cleaning 10min, obtain glass substrate；Cleaned glass substrate is stored in dehydrated alcohol It is spare in [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, argon Flow is 40sccm, sputtering power 150W, sputtering time 20min；A transition zone (SiO is obtained on the glass substrate2Film), SiO2Film thickness is 40nm；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 1.5Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, sputtering Power is 160W, sputtering time 30min, and reflecting layer 3 (silverskin), silver film thickness 200nm are obtained on transition zone 2；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, and argon flow is 40sccm, Sputtering power is 150W, sputtering time 230min, SiO2Film thickness is 102nm；Obtain solar energy thermal-power-generating reflecting mirror use SiO2-Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
5 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Compound film system infrared reflectivity is higher than 99.82%, and due to SiO2The antireflective effect of film, infrared reflectivity are even more than 100%, and adhesive force is up to 0 grade, outdoor use Service life is long.
Embodiment 6:
A kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2The preparation method of composite membrane, comprising the following steps:
1) common glass slide (as substrate) is chosen, (such as 2-5 times) is cleaned multiple times with dish washing liquid, the impurity for washing off surface is right It is washed away completely with tap water afterwards, places into ultrasonic cleaning 30min in deionized water, be finally putting into dehydrated alcohol [99.99% (quality), analyze it is pure] in ultrasonic cleaning 30min, obtain glass substrate；Cleaned glass substrate is stored in dehydrated alcohol It is spare in [99.99% (quality) is analyzed pure]；
2) prepare in glass substrate (or substrate of glass) transition zone (or dielectric layer): method is splashed with radio frequency magnetron Penetrate depositional mode, SiO2Target size isPurity is 99.999wt%, and sputter gas is that volume fraction is 99.999% high-purity argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 1.0Pa, target-substrate distance are fixed on 80mm, argon Flow is 40sccm, sputtering power 150W, sputtering time 10-30min；A transition zone (SiO is obtained on the glass substrate2 Film), SiO2Film thickness is 40nm；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, Silver target size bePurity is 99.99wt%, and sputter gas is the high-purity argon that volume fraction is 99.999%, Sputtering chamber vacuum degree is 4.0 × 10-4Pa, operating air pressure 0.5Pa, target-substrate distance are fixed on 60mm, and argon flow is 40sccm, sputtering Power is 100W, sputtering time 30min, and reflecting layer 3 (silverskin), silver film thickness 200nm are obtained on transition zone 2；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target size isPurity is 99.999wt%, sputter gas be volume fraction be 99.999% it is high-purity Argon, sputtering chamber vacuum degree are 4.0 × 10-4Pa, operating air pressure 0.5Pa, target-substrate distance are fixed on 60mm, and argon flow is 40sccm, Sputtering power is 100W, sputtering time 20min, SiO2Film thickness is 137nm；Obtain solar energy thermal-power-generating reflecting mirror SiO2- Ag-SiO2Composite membrane.
In step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering, to remove target material surface residual Oxide and pollutant.
6 gained solar energy thermal-power-generating reflecting mirror SiO of embodiment2-Ag-SiO2Compound film system infrared reflectivity is higher than 99.89%, and due to SiO2The antireflective effect of film, infrared reflectivity are even more than 100%, and adhesive force is up to 0 grade, outdoor use Service life is long.
And bound, the section value of each technological parameter of the present invention (such as air pressure, target-substrate distance, sputtering power, time) It can realize the present invention, embodiment numerous to list herein.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist Under the premise of not departing from present inventive concept, several deduction or replace can be also made, all should be considered as protection scope of the present invention.

Claims (3)

1. a kind of solar energy thermal-power-generating reflecting mirror SiO2-Ag-SiO2Composite membrane, which is characterized in that it include glass substrate and The film layer being formed on glass substrate；Film layer is made of transition zone, reflecting layer and protective layer, transition zone, reflecting layer and protective layer It is successively arranged outward from the surface of glass substrate, transition zone, reflecting layer, protective layer are made by radio-frequency magnetron sputter method； The material of the transition zone is SiO2, with a thickness of 20nm-50nm；The material in the reflecting layer is Ag, with a thickness of 100nm- 200nm；The material of the protective layer is SiO2, with a thickness of 50nm-150nm.
2. a kind of solar energy thermal-power-generating reflecting mirror SiO as described in claim 12-Ag-SiO2The preparation method of composite membrane, Be characterized in that the following steps are included:
1) common glass slide is chosen, is cleaned multiple times with dish washing liquid, the impurity on surface is washed off and then is washed away completely with tap water, then is put Enter ultrasonic cleaning 10-30min in deionized water, is finally putting into ultrasonic cleaning 10-30min in dehydrated alcohol, obtains glass Substrate；Cleaned glass substrate is stored in spare in dehydrated alcohol；
2) prepare transition zone on the glass substrate: method is with r. f. magnetron sputtering mode, SiO2Target size is Φ 76.2 × 5mm, purity 99.999wt%, sputter gas are the high-purity argon that volume fraction is 99.999%, and sputtering chamber vacuum degree is 4.0 ×10-4Pa, operating air pressure 0.5-1.5Pa, target-substrate distance are fixed on 60-100mm, and argon flow is 40sccm, and sputtering power is 100-200W, sputtering time 10-30min；A transition zone is obtained on the glass substrate；
3) reflecting layer is prepared on transition zone: method is to use r. f. magnetron sputtering mode, and the material in reflecting layer is silver, silver-colored Target size is 45 × 4mm of Φ, and purity 99.99wt%, sputter gas is the high-purity argon that volume fraction is 99.999%, sputtering Room vacuum degree is 4.0 × 10-4Pa, operating air pressure 0.5-1.5Pa, target-substrate distance are fixed on 60-100mm, and argon flow is 40sccm, Sputtering power is 100-200W, sputtering time 10-30min；
4) protective layer is prepared on reflecting layer: method is to use r. f. magnetron sputtering mode, and the material of protective layer is SiO2, target Material is the high-purity argon that volume fraction is 99.999% having a size of 76.2 × 5mm of Φ, purity 99.999wt%, sputter gas, is splashed Penetrating room vacuum degree is 4.0 × 10-4Pa, operating air pressure 0.5-1.5Pa, target-substrate distance are fixed on 60-100mm, and argon flow is 40sccm, sputtering power 100-200W, sputtering time 20-40min；Obtain solar energy thermal-power-generating reflecting mirror SiO2-Ag- SiO2Composite membrane.
3. a kind of solar energy thermal-power-generating reflecting mirror SiO according to claim 22-Ag-SiO2The preparation method of composite membrane, It is characterized by: in step 2), 3), 4) in, be both needed to carry out 5 minutes pre-sputterings to target before sputtering.
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