CN114774855B - AR film and AF film, and preparation methods and applications thereof - Google Patents
AR film and AF film, and preparation methods and applications thereof Download PDFInfo
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- CN114774855B CN114774855B CN202210303084.0A CN202210303084A CN114774855B CN 114774855 B CN114774855 B CN 114774855B CN 202210303084 A CN202210303084 A CN 202210303084A CN 114774855 B CN114774855 B CN 114774855B
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- 238000002360 preparation method Methods 0.000 title abstract description 4
- 239000000758 substrate Substances 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 45
- 238000007747 plating Methods 0.000 claims abstract description 25
- 238000000151 deposition Methods 0.000 claims abstract description 15
- 238000012545 processing Methods 0.000 claims abstract description 4
- DFUYAWQUODQGFF-UHFFFAOYSA-N 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane Chemical compound CCOC(F)(F)C(F)(F)C(F)(F)C(F)(F)F DFUYAWQUODQGFF-UHFFFAOYSA-N 0.000 claims description 20
- 239000012528 membrane Substances 0.000 claims description 14
- 238000007731 hot pressing Methods 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- SQEGLLMNIBLLNQ-UHFFFAOYSA-N 1-ethoxy-1,1,2,3,3,3-hexafluoro-2-(trifluoromethyl)propane Chemical compound CCOC(F)(F)C(F)(C(F)(F)F)C(F)(F)F SQEGLLMNIBLLNQ-UHFFFAOYSA-N 0.000 claims description 9
- 229940045180 ethyl perfluoroisobutyl ether Drugs 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims 1
- 238000004140 cleaning Methods 0.000 description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 28
- 229910052786 argon Inorganic materials 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000011550 stock solution Substances 0.000 description 10
- 230000007935 neutral effect Effects 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000012752 auxiliary agent Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000012459 cleaning agent Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 210000002268 wool Anatomy 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 230000003666 anti-fingerprint Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
Classifications
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
- C23C14/0641—Nitrides
- C23C14/0652—Silicon nitride
-
- 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
- C23C14/12—Organic material
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- 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
- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- 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
- C23C14/58—After-treatment
- C23C14/5886—Mechanical treatment
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/18—Coatings for keeping optical surfaces clean, e.g. hydrophobic or photo-catalytic films
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to the technical field of film plating, and discloses an AR film and an AF film as well as preparation methods and applications thereof, wherein the method comprises the following steps: (1) Introducing a substrate to be coated into a first processing chamber for pretreatment to obtain a pretreated substrate; (2) Introducing the pretreated substrate into an AR chamber to form an AR film, thereby obtaining a substrate containing the AR film; (3) Introducing a substrate containing an AR film into an AF chamber containing an AF film material, and depositing the AF film material on the surface of the AR film to obtain a substrate containing the AR film and the AF film; (4) The substrate containing the AR film and the AF film was subjected to a hot press treatment in an AF chamber. The AR film and the AF film prepared by the method have the characteristics of high surface hardness and friction resistance.
Description
Technical Field
The invention relates to the technical field of film plating, in particular to an AR film and an AF film as well as preparation methods and applications thereof.
Background
At present, an AR film and an AF film are basically plated on the surface of a screen of a consumer electronic product, wherein the AR film is an abbreviation of Anti-reflection film, and is also called an Anti-reflection film and an Anti-reflection film; AF film is an abbreviation of Anti-Fingerprint film.
Because the AR film is plated on the surface of the touch cover plate, the AR film is often touched in the use process, and the AR film is easy to be rubbed and fallen off in some application scenes with higher touch. In the industry, an AF film is generally plated on the surface of an AR film, so that a surface film layer has both the anti-reflection property of the AR film and the antifouling and wear-resistant properties of the AF film.
The existing film forming process is usually to lead out the substrate containing the AR+AF film to be subjected to standing treatment or baking and curing treatment after leading out after finishing the plating of the AR+AF film.
However, because the surface hardness of the AR film layer is lower than that of glass, the quality and reliability of the AR+AF film layer are reduced, so that the problems of low surface hardness and low friction resistance of the AR film and the AF film formed by the existing film forming process are solved, and the requirement that the water drop angle of the steel wool after 1000g/4000 times of friction resistance is more than or equal to 100 DEG cannot be met.
Disclosure of Invention
The invention aims to solve the problems of low surface hardness and low friction resistance of a touch cover plate in the prior art.
The inventor finds that in the research process, after the AF film plating is finished in an AF film plating machine by the existing AR+AF film forming process, a substrate containing an AF film is led out and then subjected to standing treatment or baking curing treatment, and the AF film material cannot effectively exert the wear resistance, oil stain resistance and corrosion resistance of AF stock solution, so that the AF film layer has the problem of low surface hardness and friction resistance; the inventors have also found that an AF film layer excellent in performance can be obtained by directly carrying out vacuum hot-pressing treatment in an AF film plating machine after the AF film plating is completed by blending an AF film material containing ethoxynonafluorobutane in a specific ratio. Based on this, the inventors completed the present scheme.
In order to achieve the above object, a first aspect of the present invention provides a method of preparing an AR film and an AF film, the method comprising:
(1) Introducing a substrate to be coated into a first processing chamber for pretreatment to obtain a pretreated substrate;
(2) Introducing the pretreated substrate into an AR chamber to form an AR film, so as to obtain a substrate containing the AR film;
(3) Introducing the substrate containing the AR film into an AF chamber containing AF film material, and depositing the AF film material on the surface of the AR film to obtain the substrate containing the AR film and the AF film;
(4) Carrying out hot pressing treatment on the substrate containing the AR film and the AF film in an AF chamber; the conditions of the hot press treatment at least comprise: vacuum degree no more than 5 x 10 -3 Pa, the temperature is 120-180 ℃ and the time is 3-10min;
wherein the AF membrane material contains ethoxy nonafluorobutane, and the content of the ethoxy nonafluorobutane accounts for 82-90% of the total volume of the AF membrane material.
Preferably, in step (4), the conditions of the autoclave include at least: vacuum degree no more than 5 x 10 -3 Pa, the temperature is 140-160 ℃, and the time is 5-8min.
Preferably, in the step (3), the content of the ethoxy nonafluorobutane accounts for 86-90% of the total volume of the AF film material.
Preferably, in step (1), the pretreatment includes: and sequentially carrying out preheating treatment and vacuumizing treatment on the substrate to be coated.
Preferably, in step (1), the conditions of the preheating treatment include at least: the temperature is 100-120 ℃.
Preferably, in step (1), the conditions of the vacuuming treatment include at least: vacuum degree no more than 5 x 10 -3 Pa。
Preferably, in step (2), the AR film is plated using magnetron sputtering, and the plating method of the AR film includes: sequentially depositing a first layer of SiO on the surface of the pretreated substrate 2 First layer Si 3 N 4 SiO of the second layer 2 Second layer Si 3 N 4 And a third layer of SiO 2 。
Preferably, in step (2), the conditions of the magnetron sputtering include at least: vacuum degree no more than 1.5×10 -3 Pa, the flow rate of the protective atmosphere is 500-700mL/min, and the sputtering power is 8-12kw.
Preferably, in the step (3), the amount of the AF film material is controlled so that the average thickness of the AF film is 12-26nm.
The second aspect of the present invention provides an AR film and an AF film prepared by the method of the first aspect.
A third aspect of the present invention provides the use of the AR film and AF film of the second aspect in an optical device.
According to the invention, the AF film material containing the ethoxy nonafluorobutane with a specific proportion is used in the AF film plating process, and the AF film material is directly subjected to vacuum hot-pressing treatment in an AF film plating machine after AF film plating is finished, so that the AR film and the AF film with high surface hardness and excellent friction resistance can be obtained.
In particular, the AR film and the AF film prepared by the method can meet the requirement that the water drop angle is more than or equal to 100 degrees after 1000g/4000 times of friction resistance of steel wool.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
As described above, the first aspect of the present invention provides a method of preparing an AR film and an AF film, the method comprising:
(1) Introducing a substrate to be coated into a first processing chamber for pretreatment to obtain a pretreated substrate;
(2) Introducing the pretreated substrate into an AR chamber to form an AR film, so as to obtain a substrate containing the AR film;
(3) Introducing the substrate containing the AR film into an AF chamber containing AF film material, and depositing the AF film material on the surface of the AR film to obtain the substrate containing the AR film and the AF film;
(4) Carrying out hot pressing treatment on the substrate containing the AR film and the AF film in an AF chamber; said heatThe conditions of the press treatment at least include: vacuum degree no more than 5 x 10 -3 Pa, the temperature is 120-180 ℃ and the time is 3-10min;
wherein the AF membrane material contains ethoxy nonafluorobutane, and the content of the ethoxy nonafluorobutane accounts for 82-90% of the total volume of the AF membrane material.
Preferably, in step (4), the conditions of the autoclave include at least: vacuum degree no more than 5 x 10 -3 Pa, the temperature is 140-160 ℃, and the time is 5-8min. The inventors found that the friction resistance of the AF film layer can be significantly improved by adopting this preferred embodiment.
Preferably, the content of the ethoxy nonafluorobutane accounts for 86-90% of the total volume of the AF film material.
In the invention, the AF film material is formed by mixing AF stock solution and AF auxiliary agent, the dosage proportion of the AF stock solution and the AF auxiliary agent is not particularly required, and the content of ethoxy nonafluorobutane in the AF film material only needs to be 82-90% of the total volume of the AF film material, preferably 86-90% by volume, and the dosage volume ratio of the AF stock solution to the AF auxiliary agent is 1:0.4-1, and both the AF stock solution and the AF aid are purchased from DAIKIN OPTOOL company.
In the invention, the ethoxy nonafluorobutane consists of two substances of ethyl perfluoro-isobutyl ether and ethyl nonafluoro-n-butyl ether, and the structural formula of the ethyl perfluoro-isobutyl ether is as followsThe structural formula of the ethyl nonafluoro-n-butyl ether is +.>
Preferably, in step (1), the substrate is a glass cover plate.
Preferably, in step (1), the method further comprises: and before the pretreatment is carried out, cleaning the substrate to be coated with the film.
The specific operation of the cleaning I is not particularly limited, and may be performed by methods known in the art, and the present invention uses a cleaning machine to clean the substrate to be coated.
Preferably, in step (1), the pretreatment includes: and sequentially carrying out preheating treatment and vacuumizing treatment on the substrate to be coated.
Preferably, in step (1), the conditions of the preheating treatment include at least: the temperature is 100-120 ℃.
Preferably, in step (1), the conditions of the vacuuming treatment include at least: vacuum degree no more than 5 x 10 -3 Pa。
Preferably, in step (2), the method further comprises: the pretreated substrate is subjected to a cleaning II prior to forming the AR film.
According to a particularly preferred embodiment, in step (2), the cleaning II employs plasma cleaning, and the conditions of the cleaning II include at least: the argon flow is 250-350mL/min, the power is 3-5kw, and the time is 1-3min.
Preferably, in step (2), the AR film is plated using magnetron sputtering, and the plating method of the AR film includes: sequentially depositing a first layer of SiO on the surface of the pretreated substrate 2 First layer Si 3 N 4 SiO of the second layer 2 Second layer Si 3 N 4 And a third layer of SiO 2 。
Preferably, in step (2), the conditions of the magnetron sputtering include at least: vacuum degree no more than 1.5×10 -3 Pa, the flow rate of the protective atmosphere is 500-700mL/min, and the sputtering power is 8-12kw.
The invention is not particularly limited to the specific process of magnetron sputtering and may be carried out by processes known in the art, illustratively by twin target intermediate frequency sputtering.
Specifically, in the step (2), the specific operation of the magnetron sputtering includes: at a vacuum degree of no more than 1.5X10 -3 Bombarding and sputtering a silicon target with power of 8-12kw under the conditions of Pa and argon flow of 500-700mL/min, respectively reacting silicon atoms with oxygen and nitrogen to generate silicon dioxide and silicon tetranitride, and according to a first methodLayer SiO 2 First layer Si 3 N 4 SiO of the second layer 2 Second layer Si 3 N 4 And a third layer of SiO 2 Is deposited on the pretreated substrate in sequence.
According to a particularly preferred embodiment, in step (2), the flow ratio of argon to oxygen is 0.9-1.1:1 and the flow ratio of argon to nitrogen is 1.5-2:1 during the magnetron sputtering.
According to a particularly preferred embodiment, in step (2), the first layer of SiO 2 The thickness of the first layer Si is 18-21nm 3 N 4 Is 14-16nm thick, the second layer of SiO 2 Is 20-22nm thick, the second layer Si 3 N 4 The thickness of the third layer SiO is 98-100nm 2 Is 84-86nm thick.
Preferably, in step (3), the method further comprises: before the AF film is plated, the substrate containing the AR film is heated I and cleaned III.
According to a particularly preferred embodiment, in step (3), the conditions for heating I comprise at least: vacuum degree no more than 5 x 10 -3 Pa, and the temperature is 100-150 ℃.
According to another particularly preferred embodiment, in step (3), the cleaning III employs plasma cleaning, and the conditions of the cleaning III include at least: the argon flow is 250-350mL/min, the power is 2-4kw, and the time is 2-8min.
The present invention is not particularly limited to the method of plating the AF film, and may be performed by methods known in the art, and illustratively, the present invention employs a resistance evaporation heating method to plate the AF film.
Preferably, in step (3), the conditions for plating the AF film include at least: the temperature is 300-450 ℃ and the time is 8-12min.
Preferably, in the step (3), the amount of the AF film material is controlled so that the average thickness of the AF film is 12-26nm.
Preferably, in step (4), the method further comprises: and sequentially carrying out standing treatment and IV cleaning on the substrate subjected to the hot pressing treatment.
Preferably, in step (4), the conditions of the standing treatment include at least: the time is 4-6h.
The invention is not particularly limited to the specific operation of the cleaning IV, which may be carried out using methods known in the art, and is exemplified by neutral cleaners. Illustratively, the neutral detergent is at least one selected from the group consisting of fatty alcohol alkoxy surfactants, fatty alcohol polyoxyethylene ether surfactants, polyether surfactants, and linear sodium alkylbenzene sulfonate.
It should be noted that "I", "II", "III", "IV" in the cleaning I, cleaning II, cleaning III, cleaning IV, and the like in the present invention are only used to indicate that this involves two heats, not the same cleaning, but this does not represent a sequential order unless specifically described.
As described above, the second aspect of the present invention provides an AR film and an AF film prepared by the method of the first aspect.
As described above, the third aspect of the present invention provides the use of the AR film and the AF film of the second aspect in an optical device.
The invention will be described in detail below by way of examples. In the following examples, all of the raw materials used were commercial products unless otherwise specified.
AF stock solution: the major components included 50% by volume ethyl perfluoroisobutyl ether and 30% by volume ethyl nonafluoro n-butyl ether, available from DAIKIN OPTOOL corporation;
AF auxiliary agent: the main components were 50% by volume ethyl perfluoroisobutyl ether and 50% by volume ethyl nonafluoro n-butyl ether, available from DAIKIN OPTOOL company;
AF film material 1: mixing AF stock solution and AF auxiliary agent according to the volume ratio of 1:1, wherein the content of ethoxy nonafluorobutane in AF film material 1 is 90 percent of the total volume of AF film material 1, wherein the content of ethyl perfluoro isobutyl ether is 50 percent by volume, and the content of ethyl nonafluoro n-butyl ether is 40 percent by volume;
AF film material 2: mixing AF stock solution and AF auxiliary agent according to a volume ratio of 3:2, wherein the content of ethoxy nonafluorobutane in AF membrane material 2 accounts for 88% of the total volume of AF membrane material 2, wherein the content of ethyl perfluoro isobutyl ether is 50% by volume, and the content of ethyl nonafluoro n-butyl ether is 38% by volume;
AF film material 3: mixing AF stock solution and AF auxiliary agent according to the volume ratio of 7:3, wherein the content of ethoxy nonafluorobutane in AF membrane material 3 accounts for 86 percent of the total volume of AF membrane material 3, wherein the content of ethyl perfluoro isobutyl ether is 50 percent by volume, and the content of ethyl nonafluoro n-butyl ether is 36 percent by volume;
AF film material 4: mixing AF stock solution and AF auxiliary agent according to the volume ratio of 2:3, wherein the content of ethoxy nonafluorobutane in AF membrane material 4 accounts for 92% of the total volume of AF membrane material 4, wherein the content of ethyl perfluoro isobutyl ether is 50% by volume, and the content of ethyl nonafluoro n-butyl ether is 42% by volume;
neutral cleaning agent: g-18 neutral cleaner available from Guangdong Fuxing detergent technology Co., ltd;
a substrate: a glass cover plate.
Example 1
The present embodiment provides a method of preparing an AR film and an AF film, the method comprising:
(1) Placing the cleaned substrate on a coating jig, introducing into a vacuum chamber, and vacuumizing at 100deg.C until the vacuum degree is 5×10 -3 Pa, obtaining a pretreated substrate;
(2) The pretreated substrate obtained is subjected to first plasma cleaning, and then the cleaned substrate is introduced into an AR chamber, and a first layer of SiO is deposited on the surface of the pretreated substrate in sequence by adopting a magnetron sputtering method 2 First layer Si 3 N 4 SiO of the second layer 2 Second layer Si 3 N 4 And a third layer of SiO 2 Obtaining a substrate containing an AR film;
wherein, the conditions of the first plasma cleaning are as follows: argon flow is 300mL/min, power is 4kw, and time is 2min;
deposition of a first layer of SiO 2 The conditions of (2) are: argon gasThe flow rate is 600mL/min, the oxygen flow rate is 600mL/min, the power of the silicon target is 10kw, and the film thickness is 20nm;
depositing a first layer of Si 3 N 4 The conditions of (2) are: argon flow is 600mL/min, nitrogen flow is 320mL/min, silicon target power is 10kw, and film thickness is 14.32nm;
deposition of a second layer of SiO 2 The conditions of (2) are: argon flow is 600mL/min, oxygen flow is 600mL/min, silicon target power is 10kw, and film thickness is 21.86nm;
depositing a second layer of Si 3 N 4 The conditions of (2) are: argon flow is 600mL/min, nitrogen flow is 320mL/min, silicon target power is 10kw, and film thickness is 99.54nm;
deposition of a third layer of SiO 2 The conditions of (2) are: argon flow is 600mL/min, oxygen flow is 600mL/min, silicon target power is 10kw, and film thickness is 85.23nm;
(3) Introducing the substrate containing the AR film into an AF chamber, and vacuum-pumping at 150deg.C until the vacuum degree is 5×10 -3 Pa, then carrying out secondary plasma cleaning on the substrate, plating an AF film by adopting a resistance evaporation heating method, uniformly depositing 4mL of AF film material 1 on the surface of the AR film to obtain the substrate containing the AR film and the AF film, wherein the thickness of the AF film on the substrate is 26nm;
wherein, the conditions of the second plasma cleaning are as follows: argon flow is 300mL/min, power is 3kw, and time is 5min;
conditions for plating the AF film are as follows: the temperature is 300 ℃ and the time is 10min;
(4) Carrying out hot pressing treatment on the obtained substrate containing the AR film and the AF film in an AF chamber, taking out the substrate plated with the AR film and the AF film from a film plating jig, standing for 4 hours, and cleaning with a neutral cleaning agent;
wherein, the conditions of the hot pressing treatment are as follows: vacuum degree of 5X 10 -3 Pa, the temperature is 150 ℃ and the time is 5min.
Example 2
The present embodiment provides a method of preparing an AR film and an AF film, the method comprising:
(1) The pretreated substrate was obtained in the same manner as in step (1) of example 1;
(2) As in step (2) in example 1, a substrate containing an AR film was obtained;
(3) Introducing the substrate containing the AR film into an AF chamber, and vacuum-pumping at 150deg.C until the vacuum degree is 5×10 -3 Pa, then carrying out secondary plasma cleaning on the substrate, plating an AF film by adopting a resistance evaporation heating method, and uniformly depositing 4mL of AF film material 2 on the surface of the AR film to obtain the substrate containing the AR film and the AF film, wherein the thickness of the AF film on the substrate is 26nm;
wherein, the conditions of the second plasma cleaning are as follows: argon flow is 300mL/min, power is 3kw, and time is 5min;
conditions for plating the AF film are as follows: the temperature is 300 ℃ and the time is 10min;
(4) Carrying out hot pressing treatment on the obtained substrate containing the AR film and the AF film in an AF chamber, taking out the substrate plated with the AR film and the AF film from a film plating jig, standing for 4 hours, and cleaning with a neutral cleaning agent;
wherein, the conditions of the hot pressing treatment are as follows: vacuum degree of 5X 10 -3 Pa, the temperature is 150 ℃ and the time is 6min.
Example 3
The present embodiment provides a method of preparing an AR film and an AF film, the method comprising:
(1) The pretreated substrate was obtained in the same manner as in step (1) of example 1;
(2) As in step (2) in example 1, a substrate containing an AR film was obtained;
(3) Introducing the substrate containing the AR film into an AF chamber, and vacuum-pumping at 150deg.C until the vacuum degree is 5×10 -3 Pa, then carrying out secondary plasma cleaning on the substrate, plating an AF film by adopting a resistance evaporation heating method, and uniformly depositing 4mL of AF film material 3 on the surface of the AR film to obtain the substrate containing the AR film and the AF film, wherein the thickness of the AF film on the substrate is 26nm;
wherein, the conditions of the second plasma cleaning are as follows: argon flow is 300mL/min, power is 3kw, and time is 5min;
conditions for plating the AF film are as follows: the temperature is 300 ℃ and the time is 10min;
(4) Carrying out hot pressing treatment on the obtained substrate containing the AR film and the AF film in an AF chamber, taking out the substrate plated with the AR film and the AF film from a film plating jig, standing for 4 hours, and cleaning with a neutral cleaning agent;
wherein, the conditions of the hot pressing treatment are as follows: vacuum degree of 5X 10 -3 Pa, the temperature is 150 ℃ and the time is 8min.
Example 4
This example prepares an AR film and an AF film according to the method of example 1, except that in step (4), the temperature of the heat press treatment is 180 ℃.
The rest of the procedure is the same as in example 1.
Example 5
This example prepares an AR film and an AF film according to the method of example 1, except that in step (4), the temperature of the heat press treatment is 120 ℃.
The rest of the procedure is the same as in example 1.
Example 6
This example prepares an AR film and an AF film according to the method of example 1, except that in step (3), the AF film material 1 is replaced with an equal volume of AF film material 4.
The rest of the procedure is the same as in example 1.
Comparative example 1
This comparative example AR film and AF film were prepared in the same manner as in example 1 except that in step (4), no heat press treatment was performed;
specifically, the operation method of the step (4) includes: taking out the substrate plated with the AR film and the AF film from the film plating jig, standing for 4 hours, and cleaning with a neutral cleaning agent.
The rest of the procedure is the same as in example 1.
Comparative example 2
This comparative example AR film and AF film were prepared as in example 1, except that in step (4), the substrate containing AR film and AF film was taken out of the AF chamber, then placed in an oven at 150 ℃ for drying treatment for 30min, and then cooled and left to stand for 4 hours, and then washed with a neutral detergent.
The rest of the procedure is the same as in example 1.
Comparative example 3
This comparative example AR film and AF film were prepared in the same manner as in example 1 except that in step (4), the temperature of the heat press treatment was 100 ℃.
The rest of the procedure is the same as in example 1.
Comparative example 4
This comparative example AR film and AF film were prepared as in example 1, except that in step (3), AF film stock 1 was replaced with an equal volume of AF stock, i.e., AF film stock was all AF stock.
The rest of the procedure is the same as in example 1.
Test case
The substrates containing the AR film and the AF film prepared in the examples and comparative examples were subjected to performance test, mainly to detect the initial water drop angle of the substrates, and the water drop angle after 4000 times of rubbing was measured using a 1000g weight and daily steel wool (model 0000#, purchased from Bon Star company), and the specific results are shown in table 1.
The method for testing the water drop angle comprises the following steps: the substrates containing the AR film and the AF film obtained for each example were tested for 3 pieces, and the water drop angle of 4 points was measured for each piece, and averaged.
TABLE 1
| Examples numbering | Initial drop angle/° | Water drop angle/° after 1000g/4000 times steel wool friction |
| Example 1 | 117.943 | 102.007 |
| Example 2 | 117.114 | 101.332 |
| Example 3 | 116.833 | 101.759 |
| Example 4 | 116.758 | 98.794 |
| Example 5 | 115.135 | 95.526 |
| Example 6 | 113.175 | 84.103 |
| Comparative example 1 | 114.947 | 86.470 |
| Comparative example 2 | 116.344 | 92.722 |
| Comparative example 3 | 114.818 | 95.284 |
| Comparative example 4 | 111.467 | 82.763 |
As can be seen from the results of table 1, the AR film and the AF film prepared by the method of the present invention have excellent abrasion resistance; in particular, the AR film and the AF film prepared by the method can meet the requirement that the water drop angle is more than or equal to 100 degrees after 1000g/4000 times of friction resistance of steel wool.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. A method of preparing an AR film and an AF film, the method comprising:
(1) Introducing a substrate to be coated into a first processing chamber for pretreatment to obtain a pretreated substrate;
(2) Introducing the pretreated substrate into an AR chamber to form an AR film, so as to obtain a substrate containing the AR film;
(3) Introducing the substrate containing the AR film into an AF chamber containing AF film material, and depositing the AF film material on the surface of the AR film to obtain the substrate containing the AR film and the AF film;
(4) Carrying out hot pressing treatment on the substrate containing the AR film and the AF film in an AF chamber; the conditions of the hot press treatment at least comprise: vacuum degree no more than 5 x 10 -3 Pa, the temperature is 140-160 ℃ and the time is 5-8min;
wherein the AF membrane material contains ethoxy nonafluorobutane, and the content of the ethoxy nonafluorobutane accounts for 82-90% of the total volume of the AF membrane material;
the ethoxy nonafluorobutane consists of two substances, namely ethyl perfluoro isobutyl ether and ethyl nonafluoro n-butyl ether, and the content of the ethyl nonafluoro n-butyl ether accounts for 36-40% of the total volume of the AF membrane material.
2. The method according to claim 1, wherein the content of the ethoxy nonafluorobutane is 86-90% of the total volume of the AF membrane material.
3. The method according to claim 1 or 2, wherein in step (1), the pre-treatment comprises: and sequentially carrying out preheating treatment and vacuumizing treatment on the substrate to be coated.
4. A method according to claim 3, wherein in step (1), the conditions of the preheating treatment include at least: the temperature is 100-120 ℃.
5. A method according to claim 3, wherein in step (1), the conditions of the vacuuming treatment include at least: vacuum degree no more than 5 x 10 -3 Pa。
6. The method according to claim 1 or 2, wherein in step (2), the AR film is plated using magnetron sputtering, and the plating method of the AR film comprises: sequentially depositing a first layer of SiO on the surface of the pretreated substrate 2 First layer Si 3 N 4 SiO of the second layer 2 Second layer Si 3 N 4 And a third layer of SiO 2 。
7. The method of claim 6, wherein in step (2), the conditions of the magnetron sputtering include at least: vacuum degree no more than 1.5×10 -3 Pa, the flow rate of the protective atmosphere is 500-700mL/min, and the sputtering power is 8-12kw.
8. A method according to claim 1 or 2, wherein in step (3), the amount of the AF film material is controlled so that the AF film has an average thickness of 12-26nm.
9. An AR film and an AF film prepared by the method of any one of claims 1 to 8.
10. Use of the AR film and AF film of claim 9 in an optical device.
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