CN116589200A - Salt spray resistant composite film system with chalcogenide glass as substrate and preparation method thereof - Google Patents
Salt spray resistant composite film system with chalcogenide glass as substrate and preparation method thereof Download PDFInfo
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- CN116589200A CN116589200A CN202310369430.XA CN202310369430A CN116589200A CN 116589200 A CN116589200 A CN 116589200A CN 202310369430 A CN202310369430 A CN 202310369430A CN 116589200 A CN116589200 A CN 116589200A
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- film layer
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- zinc sulfide
- germanium
- chalcogenide glass
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- 239000000758 substrate Substances 0.000 title claims abstract description 60
- 239000005387 chalcogenide glass Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 150000003839 salts Chemical class 0.000 title claims abstract description 22
- 239000007921 spray Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 62
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 47
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 47
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000001704 evaporation Methods 0.000 claims abstract description 40
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 21
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 238000004334 fluoridation Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 35
- 238000007747 plating Methods 0.000 claims description 29
- 230000008020 evaporation Effects 0.000 claims description 26
- 238000005229 chemical vapour deposition Methods 0.000 claims description 16
- 150000002500 ions Chemical class 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 13
- XASAPYQVQBKMIN-UHFFFAOYSA-K ytterbium(iii) fluoride Chemical compound F[Yb](F)F XASAPYQVQBKMIN-UHFFFAOYSA-K 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- BHHYHSUAOQUXJK-UHFFFAOYSA-L Zinc fluoride Inorganic materials F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 224
- 230000003287 optical effect Effects 0.000 abstract description 10
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012788 optical film Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 138
- 238000012360 testing method Methods 0.000 description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 12
- 238000013461 design Methods 0.000 description 9
- 230000001681 protective effect Effects 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000002390 adhesive tape Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 238000000151 deposition Methods 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 238000010894 electron beam technology Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000002310 reflectometry Methods 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010549 co-Evaporation Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical group 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
- C03C17/3621—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 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
- 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
- C03C17/3628—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 sulfide
-
- 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
- C03C17/3639—Multilayers containing at least two functional metal layers
-
- 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
Landscapes
- 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)
Abstract
The invention belongs to the technical field of optical films, and relates to a salt spray resistant composite film system taking chalcogenide glass as a substrate and a preparation method thereof. The invention provides a salt spray resistant composite film system taking chalcogenide glass as a substrate, which sequentially comprises a first germanium film layer, a zinc sulfide film layer, a second germanium film layer, an M1 film layer, a third germanium film layer and a DLC film layer from the chalcogenide glass substrate, wherein the M1 film layer is a mixed film layer obtained by co-evaporating zinc sulfide and fluoridation through a physical vapor deposition technology. The composite film system solves the problems of poor adhesion of the film layer on the surface of the chalcogenide glass, improves the surface hardness, achieves the anti-reflection and protection effects, and improves the environmental resistance and the optical performance of the chalcogenide glass.
Description
Technical Field
The invention belongs to the technical field of optical films, and relates to a salt spray resistant composite film system taking chalcogenide glass as a substrate and a preparation method thereof.
Background
In recent years, infrared detection systems are widely used in the military and civil fields, and infrared window lenses are used as important protection components of the whole optical system, and the service life of the optical system is often determined by the performance of the infrared window lenses. The chalcogenide glass is an excellent athermal optical element, has a smaller refractive index temperature coefficient, can be prepared into an aspheric surface or a free curved surface by adopting a precise molding technology, improves the image quality of an optical instrument, reduces the number of lenses in a system, has high production efficiency by adopting the molding technology, and can reduce the manufacturing cost.
The chalcogenide glass has certain defects, low hardness, large thermal expansion coefficient and low softening point, so that the film stripping phenomenon is easy to occur when a film is deposited on the chalcogenide glass, and the film structure is not matched due to the limitation of the thickness of the DLC film layer. Therefore, a thin film plated on a chalcogenide glass is required to have high transmittance and to be suitable for severe environments.
At present, although a plurality of methods for preparing the anti-reflection and protective film on the surface of the chalcogenide glass are basically in the research and development stage of a laboratory, when the chalcogenide glass is used for mass production, the requirements on process conditions are harsh, the produced product often has defective products, the reasons for the defective products are not found, and the production is unstable.
Disclosure of Invention
In order to solve the problems, the invention provides a method for plating a dielectric film and a DLC composite film by taking chalcogenide glass as a substrate, and adopts a co-evaporation technology to develop a novel material M1 for matching a film structure, so that the problem of poor adhesion of a film layer on the surface of the chalcogenide glass is solved, the surface hardness is improved, the anti-reflection and protection effects are achieved, and the environmental resistance and the optical performance of the chalcogenide glass are improved.
Specifically, in one aspect, the invention provides a salt spray resistant composite film system taking chalcogenide glass as a substrate, which sequentially comprises a first germanium film layer, a zinc sulfide film layer, a second germanium film layer, an M1 film layer, a third germanium film layer and a DLC film layer from the chalcogenide glass substrate, wherein the M1 film layer is a mixed film layer obtained by co-evaporating zinc sulfide and fluoridation through a physical vapor deposition technology. FIG. 1 shows a schematic diagram of the design structure of the composite membrane system of the present invention.
More specifically, co-evaporating zinc sulfide and fluoride by physical vapor deposition techniques includes co-evaporating zinc sulfide by resistive evaporation and electron gun deposition of fluoride .
More specifically, the first germanium film layer, the zinc sulfide film layer, the second germanium film layer and the third germanium film layer are plated by physical vapor deposition technology. The particular physical vapor deposition technique for plating the germanium film and zinc film is not limited and may be routinely selected by one of skill in the art based on particular practices. Similarly, where evaporation is performed to plate each film layer using physical vapor deposition techniques, the evaporation rate may be routinely selected by one skilled in the art according to specific practices. For example, germanium may be evaporated using an electron beam at a rate of 0.1-0.5nm/s (e.g., including 0.1, 0.2, 0.3, 0.4, and 0.5 nm/s), and zinc sulfide may be evaporated using an evaporation-blocking method at a rate of 0.6-1.0nm/s (e.g., including 0.6, 0.7, 0.8, 0.9, and 1.0 nm/s).
More specifically, in the plating of the M1 film layer, the ytterbium fluoride has an evaporation rate of 0.5-0.6nm/s and the zinc sulfide has an evaporation rate of 0.5-0.6nm/s.
More specifically, the thicknesses of the first germanium film layer, the zinc sulfide film layer, the second germanium film layer, and the M1 film laminated third germanium film layer are not limited, and may be routinely selected by those skilled in the art according to specific practices, for example, the thicknesses of the respective film layers may be designed using film system design software. As an illustrative example, the thicknesses of the first germanium film, zinc sulfide film, second germanium film, M1 film, and third germanium film may be designed such that the composite film system of the present invention achieves antireflection in the 8-12 μm band. More specifically, as an illustrative example, the thicknesses of the first germanium film layer, the zinc sulfide film layer, the second germanium film layer, the M1 film layer, and the third germanium film layer may be 170-175nm (e.g., 172.76 nm), 280-285nm (e.g., 281.9 nm), 660-670nm (e.g., 665.15 nm), 155-160nm (e.g., 157.21 nm), and 145-155nm (e.g., 150 nm), respectively. More specifically, the composite film systems of the present invention can achieve an average reflectance of less than 6% (including, for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, and 5.5% average reflectance) for the 8-12 μm band. More specifically, the composite film system of the present invention can achieve an average reflectance of 5% for the 8-12 μm band. More specifically, the composite film system of the present invention can achieve an average reflectance of 1.5% for the 8-12 μm band.
More specifically, the temperature of the chalcogenide glass substrate is 70-100 ℃ during physical vapor deposition. More specifically, when germanium and zinc sulfide film layers are prepared on chalcogenide glass, the baking temperature of the substrate is 80 ℃.
More specifically, the DLC film layer is plated by a chemical vapor deposition technique. Methods of plating DLC film layers by chemical vapor deposition techniques are well known in the art and can be routinely selected by those skilled in the art according to specific practices.
More specifically, the chalcogenide glass substrate is not subjected to a heating treatment during chemical vapor deposition.
More specifically, the initial vacuum degree of the evaporation coating film layer is 1.0X10 -4 Pa～2.0×10 -3 Pa。
More specifically, the DLC film layer has a thickness of less than 1000nm. More specifically, the thickness of the DLC film layer may be 100-980nm. More specifically, the thickness of the DLC film layer may be 950nm.
In another aspect, the present invention provides a method of preparing a chalcogenide glass-based salt spray resistant composite film system, the method comprising the steps of:
1) The chalcogenide glass substrate is cleaned and the glass substrate is cleaned,
2) Plating a first germanium film layer, a zinc sulfide film layer and a second germanium film layer on the surface of the chalcogenide glass substrate in sequence by a physical vapor deposition technology,
3) The second germanium film layer is plated with an M1 film layer by co-evaporating zinc sulfide and fluoridation through a physical vapor deposition technology,
4) Plating a third germanium film layer on the M1 film layer by physical vapor deposition technology, and
5) And plating a DLC film layer on the third germanium film layer by a chemical vapor deposition technology.
More specifically, the cleaning in step 1) includes an ion-assisted cleaning process.
More specifically, co-evaporating zinc sulfide and fluoridation by physical vapor deposition techniques in step 3) includes co-evaporating zinc sulfide by resistive evaporation and electron gun deposition fluoridation .
The particular physical vapor deposition technique for plating the germanium film and zinc film is not limited and may be routinely selected by one of skill in the art based on particular practices. Similarly, where evaporation is performed to plate each film layer using physical vapor deposition techniques, the evaporation rate may be routinely selected by one skilled in the art according to specific practices. For example, germanium may be evaporated using an electron beam at a rate of 0.1-0.5nm/s (e.g., including 0.1, 0.2, 0.3, 0.4, and 0.5 nm/s), and zinc sulfide may be evaporated using an evaporation-blocking method at a rate of 0.6-1.0nm/s (e.g., including 0.6, 0.7, 0.8, 0.9, and 1.0 nm/s).
More specifically, ytterbium fluoride has a rate of 0.5 to 0.6nm/s and zinc sulfide has a rate of 0.5 to 0.6nm/s when evaporating the M1 material.
More specifically, the thicknesses of the first germanium film layer, the zinc sulfide film layer, the second germanium film layer, and the M1 film laminated third germanium film layer are not limited, and may be routinely selected by those skilled in the art according to specific practices, for example, the thicknesses of the respective film layers may be designed using film system design software. As an illustrative example, the thicknesses of the first germanium film, zinc sulfide film, second germanium film, M1 film, and third germanium film may be designed such that the composite film system of the present invention achieves antireflection in the 8-12 μm band. More specifically, as an illustrative example, the thicknesses of the first germanium film layer, the zinc sulfide film layer, the second germanium film layer, the M1 film layer, and the third germanium film layer may be 170-175nm (e.g., 172.76 nm), 280-285nm (e.g., 281.9 nm), 660-670nm (e.g., 665.15 nm), 155-160nm (e.g., 157.21 nm), and 145-155nm (e.g., 150 nm), respectively. More specifically, the composite film systems of the present invention can achieve an average reflectance of less than 6% (including, for example, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, and 5.5% average reflectance) for the 8-12 μm band. More specifically, the composite film system of the present invention can achieve an average reflectance of 5% for the 8-12 μm band. More specifically, the composite film system of the present invention can achieve an average reflectance of 1.5% for the 8-12 μm band.
More specifically, the temperature of the chalcogenide glass substrate is 70-100 ℃ during physical vapor deposition. More specifically, when germanium and zinc sulfide film layers are prepared on chalcogenide glass, the baking temperature of the substrate is 80 ℃.
More specifically, methods of plating DLC film layers by chemical vapor deposition techniques are well known in the art, and can be routinely selected by those skilled in the art according to specific practices.
More specifically, the chalcogenide glass substrate is not subjected to a heating treatment during chemical vapor deposition.
More specifically, the DLC film layer has a thickness of less than 1000nm. More specifically, the thickness of the DLC film layer may be 100-980nm. More specifically, the thickness of the DLC film layer may be 950nm.
More specifically, in the method, the initial vacuum degree is set to 1.0X10 -4 Pa～2.0×10 -3 Pa。
More specifically, in the method, when the initial vacuum degree reaches 1.0X10 -4 Pa～2.0×10 -3 And (3) during Pa, performing an ion-assisted cleaning process of the chalcogenide glass substrate, and then performing film plating.
The beneficial effects of the invention are that
The invention solves the problems of poor film firmness, easy film stripping, poor reliability and difficult large-scale use of the traditional chalcogenide glass when an infrared film is deposited. The invention adopts special film structure design, process optimization and research and development of novel mixed materials to deposit the film structure on the chalcogenide glass substrate, and has the following advantages:
(1) The DLC protective layer improves the surface hardness of the chalcogenide glass;
(2) The introduction of the M1 material adjusts the stress matching of the film and the optimization of the process, greatly improves the adhesive force of the film and solves the problem of film stripping on the surface of the chalcogenide glass;
(3) The film layer can pass through the reliability detection experiments of salt fog, high and low temperature, friction and the like.
The invention also successfully deposits the antireflection protective film with the wave band of 8-12 mu m on the chalcogenide glass substrate, and realizes that the average reflectivity of the antireflection protective film with the wave band of 8-12 mu m is 5 percent.
Drawings
FIG. 1 shows a schematic diagram of the design structure of the membrane system of the present invention.
FIG. 2 shows the design spectrum of the film system of the present invention.
FIG. 3 shows the actual test spectral curve of the inventive film system.
FIG. 4 shows a sample surface plot after environmental testing of a film-based sample of the present invention.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Example 1:
the embodiment provides a salt spray resistant composite film system with chalcogenide glass as a substrate, which is prepared as follows:
(1) In a typical chalcogenide glass IG2 (Ge 33 As 12 Se 55 Refractive index 2.49667@10μm), the antireflection film with the thickness of 8-12 μm is optimally designed by adopting film system design software, a theoretical design spectral curve is shown in fig. 2, the average reflectivity is 1.5%, and the specific film system design structure is as follows: the first layer is germanium, and the thickness of the film layer is 172.76nm; the second layer is zinc sulfide, and the thickness of the film layer is 281.9nm; the third layer is germanium, the thickness of the film layer is 665.15nm, the fourth layer is M1, the thickness of the film layer is 157.21nm, the fifth layer is germanium, and the thickness of the film layer is 150nm; the sixth layer is DLC, and the thickness of the film layer is 950nm.
(2) Plating a front 5-layer medium film by adopting a 1350-layer vacuum optical coating machine, wherein the equipment is provided with a 6-bit crystal control probe, a 6-steric hindrance steamer, a single e-type electron gun and a koufman ion source, and a vacuum system consists of a mechanical pump and a cold pump; DLC film is plated by LWT700-VI type radio frequency plasma chemical vapor deposition equipment which is provided with a radio frequency power supply, and a vacuum system consists of a mechanical pump and a molecular pump.
(3) Before plating the film, the chalcogenide glass substrate needs to be wiped, so that the phenomenon that the deposited film is not firm due to scratch, residual water vapor and dust is avoided, and the wiping cloth is used for dipping the reagent for treatment: alcohol-acetone-alcohol-polishing liquid-alcohol-acetone.
(4) Placing the wiped substrate on a male tray, vacuumizing the device, setting the temperature to 85deg.C, and when the initial vacuum degree reaches 2.0X10 -3 Pa, cleaning the substrate by adopting an ion source for 5 minutes, cleaning the surface of the substrate and improving the ion activity of the surface of the substrate.
(5) Germanium is evaporated by adopting an electron beam, the evaporation rate is 0.3nm/s, zinc sulfide is evaporated by adopting an evaporation blocking mode, the evaporation rate is 0.8nm/s, and when an M1 material is evaporated, the ytterbium fluoride rate is 0.5nm/s, and the zinc sulfide rate is 0.5nm/s.
(6) After the film system plating is completed, when the temperature is cooled to below 70 ℃, the chalcogenide glass substrate can be put into chemical vapor deposition equipment to start vacuumizing, and when the vacuum degree is 5 multiplied by 10 -3 Pa, the radio frequency power is 400W, a constant voltage mode is adopted to be 3Pa, 35SCCM argon is filled, and the substrate is cleaned for 300S. When the vacuum degree is pumped to 3 multiplied by 10 -3 pa, the radio frequency power is 600W, the reaction gas is methane, argon is used as carrier gas, and the ratio is CH 4:Ar=149: 10, vacuum pressure of 10Pa and deposition time of 2800S. After the preparation is completed, the substrate is cooled for 20 minutes, and the preparation of the protective film is completed.
(7) The reflectance curves for the spectra of 8-12 μm were measured using a PerkinElmer Spectrum infrared spectrometer and the average reflectance was 5% as shown in FIG. 3.
And (3) carrying out environmental test on the film:
the film layer using performance is tested by the film layer firmness, salt fog, high and low temperature and friction test in GBJ2485-1995 standard test, wherein
The firmness of the film layer is that a 3M adhesive tape with the width of 20mm and the adhesion of (10+/-1) N/25mm is adopted to be quickly pulled up vertically by 90 degrees, and no film layer is separated, so that the use requirement is met.
Salt mist: the HY-60 salt spray test box is adopted, the temperature is 35+/-2 ℃, the concentration is 4.9% -5.1%, the spray is continuously carried out for 24 hours in sodium chloride solution with the pH of 6.5-7.2, and the film layer has no defects of peeling, stripping, cracking, air bubbles and the like, thereby meeting the use requirements.
And (3) at high and low temperatures, namely placing the film coating sheet into a high and low temperature test box, respectively maintaining at the temperature of minus 60 ℃ and 70 ℃ for two hours, taking out, placing into room temperature, visually detecting, and carrying out firmness test by using an adhesive tape, wherein the film layer has no peeling, cracks and bubbles, and is not found to fall off after being adhered and pulled by the adhesive tape, so that the use requirement is met.
The friction is that the surface of the protective film is rubbed by super strong friction, an external rubber friction head is tied on a friction tester, the external rubber friction head is pressed on the surface of the film with a force of 0.196N, the surface of the film is rubbed for 1000 revolutions, no scratches and other damages appear on the surface of the film, and the use requirement is met.
The surface of the sample after the test is shown in fig. 4.
Example 2
The embodiment provides a salt spray resistant composite film system with chalcogenide glass as a substrate, which is prepared as follows:
(1) In a typical chalcogenide glass IG2 (Ge 33 As 12 Se 55 Refractive index 2.49667@10μm), the antireflection film with the thickness of 8-12 μm is optimally designed by adopting film system design software, the theoretical average reflectivity is 1.5%, and the specific film system design structure is as follows: the first layer is germanium, and the thickness of the film layer is 172.76nm; the second layer is zinc sulfide, and the thickness of the film layer is 281.9nm; the third layer is germanium, the thickness of the film layer is 665.15nm, the fourth layer is M1, the thickness of the film layer is 157.21nm, the fifth layer is germanium, and the thickness of the film layer is 150nm; the sixth layer is DLC, and the thickness of the film layer is 950nm.
(2) Plating a front 5-layer medium film by adopting a 1350-layer vacuum optical coating machine, wherein the equipment is provided with a 6-bit crystal control probe, a 6-steric hindrance steamer, a single e-type electron gun and a koufman ion source, and a vacuum system consists of a mechanical pump and a cold pump; DLC film is plated by LWT700-VI type radio frequency plasma chemical vapor deposition equipment which is provided with a radio frequency power supply, and a vacuum system consists of a mechanical pump and a molecular pump.
(3) Before plating the film, the chalcogenide glass substrate needs to be wiped, so that the phenomenon that the deposited film is not firm due to scratch, residual water vapor and dust is avoided, and the wiping cloth is used for dipping the reagent for treatment: alcohol-acetone-alcohol-polishing liquid-alcohol-acetone.
(4) Placing the wiped substrate on a male tray, vacuumizing the device, setting the temperature to 85deg.C, and when the initial vacuum degree reaches 1.0X10 -4 Pa, cleaning the substrate by adopting an ion source for 5 minutes, cleaning the surface of the substrate and improving the ion activity of the surface of the substrate.
(5) Germanium is evaporated by adopting an electron beam, the evaporation rate is 0.4nm/s, zinc sulfide is evaporated by adopting an evaporation blocking mode, the evaporation rate is 1.0nm/s, and when an M1 material is evaporated, the ytterbium fluoride rate is 0.6nm/s, and the zinc sulfide rate is 0.6nm/s.
(6) After the film system plating is completed, when the temperature is cooled to below 70 ℃, the chalcogenide glass substrate can be put into chemical vapor deposition equipment to start vacuumizing, and when the vacuum degree is 5 multiplied by 10 -3 Pa, the radio frequency power is 400W, a constant voltage mode is adopted to be 3Pa, 35SCCM argon is filled, and the substrate is cleaned for 300S. When the vacuum degree is pumped to 3 multiplied by 10 -3 pa, the radio frequency power is 600W, the reaction gas is methane, argon is used as carrier gas, and the ratio is CH 4:Ar=149: 10, vacuum pressure of 10Pa and deposition time of 2800S. After the preparation is completed, the substrate is cooled for 20 minutes, and the preparation of the protective film is completed.
(7) The reflectance curve of the spectrum with the average reflectance of 5% is tested by adopting a PerkinElmer Spectrum 3 infrared spectrometer with the spectrum reflectance of 8-12 mu m.
And (3) carrying out environmental test on the film:
the film layer using performance is tested by the film layer firmness, salt fog, high and low temperature and friction test in GBJ2485-1995 standard test, wherein
The firmness of the film layer is that a 3M adhesive tape with the width of 20mm and the adhesion of (10+/-1) N/25mm is adopted to be quickly pulled up vertically by 90 degrees, and no film layer is separated, so that the use requirement is met.
Salt mist: the HY-60 salt spray test box is adopted, the temperature is 35+/-2 ℃, the concentration is 4.9% -5.1%, the spray is continuously carried out for 24 hours in sodium chloride solution with the pH of 6.5-7.2, and the film layer has no defects of peeling, stripping, cracking, air bubbles and the like, thereby meeting the use requirements.
And (3) at high and low temperatures, namely placing the film coating sheet into a high and low temperature test box, respectively maintaining at the temperature of minus 60 ℃ and 70 ℃ for two hours, taking out, placing into room temperature, visually detecting, and carrying out firmness test by using an adhesive tape, wherein the film layer has no peeling, cracks and bubbles, and is not found to fall off after being adhered and pulled by the adhesive tape, so that the use requirement is met.
The friction is that the surface of the protective film is rubbed by super strong friction, an external rubber friction head is tied on a friction tester, the external rubber friction head is pressed on the surface of the film with a force of 0.196N, the surface of the film is rubbed for 1000 revolutions, no scratches and other damages appear on the surface of the film, and the use requirement is met.
Comparative example 1
The comparative example provides a salt spray resistant composite film system based on chalcogenide glass, which is prepared as follows:
(1) In a typical chalcogenide glass IG2 (Ge 33 As 12 Se 55 Refractive index 2.49667@10μm), the antireflection film with the thickness of 8-12 μm is optimally designed by adopting film system design software, the theoretical average reflectivity is 2.0%, and the specific film system design structure is as follows: the first layer is germanium, and the thickness of the film layer is 172.76nm; the second layer is zinc sulfide, and the thickness of the film layer is 281.9nm; the third layer is germanium, the thickness of the film layer is 665.15nm, the fourth layer is zinc sulfide, the thickness of the film layer is 157.21nm, the fifth layer is germanium, and the thickness of the film layer is 150nm; the sixth layer is DLC, and the thickness of the film layer is 950nm.
(2) Plating a front 5-layer medium film by adopting a 1350-layer vacuum optical coating machine, wherein the equipment is provided with a 6-bit crystal control probe, a 6-steric hindrance steamer, a single e-type electron gun and a koufman ion source, and a vacuum system consists of a mechanical pump and a cold pump; DLC film is plated by LWT700-VI type radio frequency plasma chemical vapor deposition equipment which is provided with a radio frequency power supply, and a vacuum system consists of a mechanical pump and a molecular pump.
(3) Before plating the film, the chalcogenide glass substrate needs to be wiped, so that the phenomenon that the deposited film is not firm due to scratch, residual water vapor and dust is avoided, and the wiping cloth is used for dipping the reagent for treatment: alcohol-acetone-alcohol-polishing liquid-alcohol-acetone.
(4) Placing the wiped substrate on a male tray, vacuumizing the device, setting the temperature to 85deg.C, and when the initial vacuum degree reaches 2.0X10 -3 Pa, cleaning the substrate by adopting an ion source for 5 minutes, cleaning the surface of the substrate and improving the ion activity of the surface of the substrate.
(5) Germanium is evaporated by adopting an electron beam, the evaporation rate is 0.3nm/s, zinc sulfide is evaporated by adopting an evaporation blocking mode, the evaporation rate is 0.8nm/s, and when an M1 material is evaporated, the ytterbium fluoride rate is 0.5nm/s, and the zinc sulfide rate is 0.5nm/s.
(6) After the film system plating is completed, when the temperature is cooled to below 70 ℃, the chalcogenide glass substrate can be put into chemical vapor deposition equipment to start vacuumizing, and when the vacuum degree is 5 multiplied by 10 -3 Pa, the radio frequency power is 400W, a constant voltage mode is adopted to be 3Pa, 35SCCM argon is filled, and the substrate is cleaned for 300S. When the vacuum degree is pumped to 3 multiplied by 10 -3 pa, the radio frequency power is 600W, the reaction gas is methane, argon is used as carrier gas, and the ratio is CH 4:Ar=149: 10, vacuum pressure of 10Pa and deposition time of 2800S. After the preparation is completed, the substrate is cooled for 20 minutes, and the preparation of the protective film is completed.
And (3) carrying out environmental test on the film:
film layer performance was tested by the film layer firmness test in the GBJ2485-1995 Standard test, wherein
Film firmness, namely, a 3M adhesive tape with the width of 20mm and the adhesion of (10+/-1) N/25mm is adopted to rapidly pull up at 90 degrees vertically, and the film has the phenomenon of film stripping and cannot meet the use requirement. The introduction of the material of the M1 film layer can improve the adhesive force of the film layer and solve the problem of film layer stripping on the surface of the chalcogenide glass.
Comparative example 2
The comparative example provides a salt spray resistant composite film system based on chalcogenide glass, which is prepared as follows:
(1) In a typical chalcogenide glass IG2 (Ge 33 As 12 Se 55 Refractive index 2.49667@10μm), the antireflection film with the thickness of 8-12 μm is optimally designed by adopting film system design software, the theoretical average reflectivity is 1.5%, and the specific film system design structure is as follows: the first layer is germaniumThe thickness of the film layer is 172.76nm; the second layer is zinc sulfide, and the thickness of the film layer is 281.9nm; the third layer is germanium, the thickness of the film layer is 665.15nm, the fourth layer is M1, the thickness of the film layer is 157.21nm, the fifth layer is germanium, and the thickness of the film layer is 150nm; the sixth layer is DLC, and the thickness of the film layer is 950nm.
(2) Plating a front 5-layer medium film by adopting a 1350-layer vacuum optical coating machine, wherein the equipment is provided with a 6-bit crystal control probe, a 6-steric hindrance steamer, a single e-type electron gun and a koufman ion source, and a vacuum system consists of a mechanical pump and a cold pump; DLC film is plated by LWT700-VI type radio frequency plasma chemical vapor deposition equipment which is provided with a radio frequency power supply, and a vacuum system consists of a mechanical pump and a molecular pump.
(3) Before plating the film, the chalcogenide glass substrate needs to be wiped, so that the phenomenon that the deposited film is not firm due to scratch, residual water vapor and dust is avoided, and the wiping cloth is used for dipping the reagent for treatment: alcohol-acetone-alcohol-polishing liquid-alcohol-acetone.
(4) Placing the wiped substrate on a male tray, vacuumizing the device, setting the temperature to 85deg.C, and when the initial vacuum degree reaches 2.0X10 -3 Pa, cleaning the substrate by adopting an ion source for 5 minutes, cleaning the surface of the substrate and improving the ion activity of the surface of the substrate.
(5) Germanium is evaporated by adopting an electron beam, the evaporation rate is 0.3nm/s, zinc sulfide is evaporated by adopting an evaporation blocking mode, the evaporation rate is 0.8nm/s, and when an M1 material is evaporated, the ytterbium fluoride rate is 0.4nm/s, and the zinc sulfide rate is 0.6nm/s.
(6) After the film system plating is completed, when the temperature is cooled to below 70 ℃, the chalcogenide glass substrate can be put into chemical vapor deposition equipment to start vacuumizing, and when the vacuum degree is 5 multiplied by 10 -3 Pa, the radio frequency power is 400W, a constant voltage mode is adopted to be 3Pa, 35SCCM argon is filled, and the substrate is cleaned for 300S. When the vacuum degree is pumped to 3 multiplied by 10 -3 pa, the radio frequency power is 600W, the reaction gas is methane, argon is used as carrier gas, and the ratio is CH 4:Ar=149: 10, vacuum pressure of 10Pa and deposition time of 2800S. After the preparation is completed, the substrate is cooled for 20 minutes, and the preparation of the protective film is completed.
And (3) carrying out environmental test on the film:
the film layer using performance is tested by the film layer firmness, salt fog, high and low temperature and friction test in the GBJ2485-1995 standard test, wherein the salt fog, the high and low temperature and the abrasion resistance test can meet the using requirements, but the film layer firmness is weakened compared with the film layer in the embodiment 1, and the film layer firmness and the plating process prove that the material composition of the M1 film layer and the plating process are complementary and indispensable.
In the description of the specification, reference to the term "one embodiment," "a particular embodiment," "an example," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or by similar arrangements, by those skilled in the art, without departing from the scope of the invention or beyond the scope of the appended claims.
Claims (10)
1. The salt spray resistant composite film system taking the chalcogenide glass as the substrate is characterized by sequentially comprising a first germanium film layer, a zinc sulfide film layer, a second germanium film layer, an M1 film layer, a third germanium film layer and a DLC film layer from the chalcogenide glass substrate, wherein the M1 film layer is a mixed film layer obtained by co-evaporating zinc sulfide and fluoridation through a physical vapor deposition technology.
2. The composite film system according to claim 1, wherein in the plating of the M1 film layer, ytterbium fluoride has an evaporation rate of 0.5 to 0.6nm/s and zinc sulfide has an evaporation rate of 0.5 to 0.6nm/s.
3. The composite film system of claim 1, wherein the first, zinc sulfide, second, and third germanium films are plated by physical vapor deposition techniques.
4. The composite film system of claim 1 wherein co-evaporating zinc sulfide and fluorinated by physical vapor deposition techniques comprises co-evaporating zinc sulfide and electron gun deposited fluorinated .
5. The composite film system of claim 1, wherein the DLC film layer is plated by chemical vapor deposition techniques.
6. The composite film system according to any one of claims 1 to 5, wherein the initial vacuum level of the vapor deposited film layer is 1.0X10 -4 Pa～2.0×10 -3 Pa。
7. The composite film system of claim 1, wherein the DLC film layer has a thickness of less than 1000nm.
8. A method of preparing a salt spray resistant composite film system based on chalcogenide glass, the method comprising the steps of:
1) The chalcogenide glass substrate is cleaned and the glass substrate is cleaned,
2) Plating a first germanium film layer, a zinc sulfide film layer and a second germanium film layer on the surface of the chalcogenide glass substrate in sequence by a physical vapor deposition technology,
3) The second germanium film layer is plated with an M1 film layer by co-evaporating zinc sulfide and fluoridation through a physical vapor deposition technology,
4) Plating a third germanium film layer on the M1 film layer by physical vapor deposition technology, and
5) And plating a DLC film layer on the third germanium film layer by a chemical vapor deposition technology.
9. The method of claim 8, wherein co-evaporating zinc sulfide and fluoride by physical vapor deposition techniques in step 3) comprises co-evaporating zinc sulfide and electron gun deposited fluoride .
10. The method according to claim 8, wherein the cleaning in step 1) preferably comprises an ion assisted cleaning process,
preferably, in the plating of the M1 film layer, the ytterbium fluoride has an evaporation rate of 0.5-0.6nm/s, the zinc sulfide has an evaporation rate of 0.5-0.6nm/s,
preferably, the initial vacuum degree of the evaporation coating film layer is 1.0X10 -4 Pa～2.0×10 -3 Pa，
Preferably, the DLC film layer has a thickness of less than 1000nm.
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