CN112609158A - Visible infrared window antireflection film based on magnetron sputtering and preparation method - Google Patents
Visible infrared window antireflection film based on magnetron sputtering and preparation method Download PDFInfo
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- CN112609158A CN112609158A CN202011310042.7A CN202011310042A CN112609158A CN 112609158 A CN112609158 A CN 112609158A CN 202011310042 A CN202011310042 A CN 202011310042A CN 112609158 A CN112609158 A CN 112609158A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3485—Sputtering using pulsed power to the target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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Abstract
The invention discloses a visible infrared window antireflection film based on magnetron sputtering and a preparation method thereof, and belongs to the technical field of optical films. The method mainly uses a magnetron sputtering plating method, abandons the use of soft film materials such as ytterbium fluoride and zinc sulfide with low hardness in the conventional high-efficiency antireflection film, uses hard oxide protective films such as yttrium oxide, titanium oxide and aluminum oxide, and forms the visible, low-light and infrared common-window high-strength antireflection film which can be used in a zinc sulfide base through design optimization. The film system can have the reflectivity of 5 percent in the wave band range of 0.4-0.75 um and 1.57um and the transmittance of more than 92 percent in the wave band range of 7.4-10.7 um, has good surface quality and firmness of the film layer, and can resist the test requirements of friction test specified in GJB2485-95, temperature, damp and hot, salt fog and the like specified in GJB 150A-2009.
Description
Technical Field
The invention relates to the technical field of optical films, in particular to a visible infrared window antireflection film based on magnetron sputtering and a preparation method thereof.
Background
The CVD ZnS has wide transmission waveband (0.6-13 Lm), can be cheap and large-sized, is the best material for visible and infrared windows of military photoelectric sightseeing instruments, but has low surface hardness, and the optical surface is easy to be damaged during high-speed running so that the infrared transmittance is reduced, so that the surface needs to be plated with a protective film; the protective film applied to the infrared window is mainly focused on a diamond film, a diamond-like film, a boron phosphide film, a germanium carbide film, a hafnium oxynitride film and the like.
1. The conventional high-efficiency antireflection film uses materials with lower hardness, such as ytterbium fluoride, zinc sulfide and the like, and can meet the optical use requirement, but the film layer is easy to damage in severe environments, such as desert, rainforest and the like;
2. the diamond-like film is commonly used as an infrared protection material as a conventional hard protection film, but has high internal stress and large absorption, and is difficult to deposit a thick film;
3. the diamond film is the most ideal choice for the protective film, but has great problems in the aspects of large-area deposition, thermal mismatch, cost and the like at present;
4. the reported hafnium oxynitride film can be used for protecting an infrared zinc sulfide material, but the refractive index of the film is closer to that of the zinc sulfide material, and the reported single-layer hafnium oxynitride film cannot meet the multispectral antireflection requirement.
Disclosure of Invention
The invention aims to provide a visible infrared window antireflection film based on magnetron sputtering and a preparation method thereof, and mainly adopts a magnetron sputtering plating method, and a visible, dim light and infrared common-window high-strength antireflection film which can be used for a zinc sulfide base is formed by design optimization by using hard oxide protective films such as yttrium oxide, titanium oxide, aluminum oxide and the like instead of using soft film materials such as ytterbium fluoride and zinc sulfide and the like with low hardness as a conventional high-efficiency antireflection film.
In order to solve the technical problems, the invention provides a method for preparing a visible infrared window antireflection film based on magnetron sputtering, which comprises the following steps:
the method comprises the following steps: cleaning a cathode target material, and sequentially filling a No. 1 Al target material, a No. 2 Ti target material and a No. 3Y target material;
step two: putting the cleaned part to be plated into a processed plating fixture, placing the fixture in a part tray of a plating machine, pressing a vacuum chamber door tightly, and starting to vacuumize;
step three: background vacuum degree rP is less than or equal to 3.0 multiplied by 10-6When torr, starting a coating program;
step four: and (3) pre-sputtering the target material, wherein the pre-sputtering time of each target is preferably determined according to the surface state until no splashing point exists.
Step five: sputtering Y2O3A film layer, wherein the cathode power is 3.8kw, argon gas is 60-70 sccm, the ion source power is 2kw, oxygen gas is 25sccm, and the deposition rate is 0.23 nm/s;
step six: sputtering of TiO2A film layer, wherein the cathode power is 4kw, the argon gas is 50-60 sccm, the ion source power is 3.5kw, the oxygen gas is 30-40 sccm, and the deposition rate is 0.05 nm/s;
step seven: repeating the fifth step and the sixth step according to the actual spectrum requirement;
step eight: sputtering of Al2O3A film layer, wherein the cathode power is 3.8kw, the argon gas is 60-70 sccm, the ion source power is 3kw, the oxygen gas is 30-40 sccm, and the sputtering rate is 0.18 nm/s;
step nine: and (5) after the plating is finished, taking the workpiece after 10 minutes.
Optionally, the ion source in the fourth step uses an ICP plasma source.
Optionally, in the fourth step, the sputtering cathode is driven by a direct current pulse direct current power supply.
Optionally, the ion source ionized gas in step four uses oxygen of 99.99% purity.
Another object of the present invention is to provide a visible infrared window antireflection film obtained by the above production method.
The invention provides a visible infrared window antireflection film based on magnetron sputtering and a preparation method thereof, which mainly use a magnetron sputtering plating method, abandon the use of soft film materials such as ytterbium fluoride and zinc sulfide with low hardness in the conventional high-efficiency antireflection film, use hard oxide protective films such as yttrium oxide, titanium oxide and aluminum oxide, and form the visible, glimmer and infrared common-window high-strength antireflection film used for a zinc sulfide base through design optimization. The film system can have the reflectivity of 5 percent in the wave band range of 0.4-0.75 um and 1.57um and the transmittance of more than 92 percent in the wave band range of 7.4-10.7 um, has good surface quality and firmness of the film layer, and can resist the test requirements of friction test specified in GJB2485-95, temperature, damp and hot, salt fog and the like specified in GJB 150A-2009.
Drawings
FIG. 1 is a microscopic comparison of a visible infrared window antireflection film provided by the present invention after a rubbing test with a high strength film;
FIG. 2 is a microscopic comparison graph of a visible infrared window antireflection film provided by the present invention after 240h damp heat test with a high strength film;
FIG. 3 is a graph of the transmittance of a visible infrared window antireflection film provided by the present invention;
FIG. 4 is a graph of the transmittance of a visible laser window antireflection film provided by the present invention.
Detailed Description
The visible infrared window antireflection film based on magnetron sputtering and the preparation method thereof provided by the invention are further described in detail with reference to specific examples. Advantages and features of the present invention will become apparent from the following description and from the claims. It is to be noted that the drawings are in a very simplified form and are not to precise scale, which is merely for the purpose of facilitating and distinctly claiming the embodiments of the present invention.
Example one
The invention provides a method for preparing a visible infrared window antireflection film based on magnetron sputtering, which comprises the following steps:
the method comprises the following steps: cleaning a cathode target material, and sequentially filling a No. 1 Al target material, a No. 2 Ti target material and a No. 3Y target material;
step two: putting the cleaned part to be plated into a processed plating fixture, placing the fixture in a part tray of a plating machine, pressing a vacuum chamber door tightly, and starting to vacuumize;
step three: background vacuum degree rP is less than or equal to 3.0 multiplied by 10-6When torr, starting a coating program;
step four: and (3) pre-sputtering the target material, wherein the pre-sputtering time of each target is preferably determined according to the surface state until no splashing point exists.
Step five: sputtering Y2O3A film layer, wherein the cathode power is 3.8kw, argon gas is 60-70 sccm, the ion source power is 2kw, oxygen gas is 25sccm, and the deposition rate is 0.23 nm/s;
step six: sputtering of TiO2A film layer, wherein the cathode power is 4kw, the argon gas is 50-60 sccm, the ion source power is 3.5kw, the oxygen gas is 30-40 sccm, and the deposition rate is 0.05 nm/s;
step seven: repeating the fifth step and the sixth step according to the actual spectrum requirement;
step eight: sputtering of Al2O3A film layer, wherein the cathode power is 3.8kw, the argon gas is 60-70 sccm, the ion source power is 3kw, the oxygen gas is 30-40 sccm, and the sputtering rate is 0.18 nm/s;
step nine: and (5) after the plating is finished, taking the workpiece after 10 minutes.
Specifically, the workbench used by the coating machine is an ultra-clean workbench, and a spectrophotometer is used for testing a spectrum; meanwhile, the requirement on the environment is clean; the temperature is 20-25 ℃; the relative humidity is 30-50%.
Specifically, the crystal structure of ZnS is related to the growth temperature, the ZnS material as a far infrared material is a cubic structure (sphalerite structure), and ZnS is a wide band gap material (E ═ 3.58eV), is not easily excited by electromagnetic waves, has low electrical conductivity and good optical transmittance, and has a refractive index n of 2.2 (at a wavelength of 10 μm) and a theoretical transmittance of 75.342%. A single base material (such as ZnS) hardly meets the requirements of the above-mentioned application conditions, especially for infrared photoelectric systems; the window material is generally not composed of an optical system, but composed of two or more optical elements, the optical elements are selected and designed to have high light energy which is expected to be transmitted, the higher the transmitted light energy is, the farther the detected signal distance is, the higher the resolution is, and the clearer the imaging is; however, most far infrared materials have high refractive index, so that the theoretical transmittance is low, the application requirements of optical elements cannot be met, and the far infrared materials have low hardness and are extremely easy to be damaged by the environment in a severe working environment; therefore, it is necessary to plate one or more layers of anti-reflection protective materials with low refractive index, high hardness and small absorption coefficient on the surface of the far infrared material.
The formed visible infrared window antireflection films based on ZnS substrates were evaluated by the following methods 1 to 6, and the results thereof are shown in the following table.
1. Friction test
The film layer is not worn out after being rubbed for 40 times (20 times back and forth) by a rubber rubbing head with the pressure of 9.8N, thereby meeting the requirement.
2. Tape peeling test
The adhesive tape with the width not less than 2cm and the peeling strength not less than 2.74N/cm is firmly adhered to the surface of the film layer, and after the adhesive tape is vertically and rapidly pulled up, the film stripping phenomenon does not occur, so that the requirements are met.
3. Damp-heat test
The temperature is 50 +/-2 ℃, the relative humidity is 95-100%, the temperature is kept for ten days, the total time is 240 hours, the film layer does not fall off, and the requirements are met.
4. Salt spray test
Continuously spraying for 48 hours in salt fog with the temperature of 35 ℃ plus or minus 2 ℃, the concentration of 4.9-5.1% and the pH value of 6.5-7.2, wherein the film layer does not fall off, and the requirement is met.
6. Temperature change test
Keeping the temperature at minus 62 +/-2 ℃ and 70 +/-2 ℃ for 2 hours respectively, and after the temperature returns to the room temperature, the film layer does not fall off, thereby meeting the requirements.
The above description is only for the purpose of describing the preferred embodiments of the present invention, and is not intended to limit the scope of the present invention, and any variations and modifications made by those skilled in the art based on the above disclosure are within the scope of the appended claims.
Claims (5)
1. A preparation method of a visible infrared window antireflection film based on magnetron sputtering is characterized by comprising the following steps:
the method comprises the following steps: cleaning a cathode target material, and sequentially filling a No. 1 Al target material, a No. 2 Ti target material and a No. 3Y target material;
step two: putting the cleaned part to be plated into a processed plating fixture, placing the fixture in a part tray of a plating machine, pressing a vacuum chamber door tightly, and starting to vacuumize;
step three: background vacuum degree rP is less than or equal to 3.0 multiplied by 10-6When torr, starting a coating program;
step four: and (3) pre-sputtering the target material, wherein the pre-sputtering time of each target is preferably determined according to the surface state until no splashing point exists.
Step five: sputtering Y2O3A film layer, wherein the cathode power is 3.8kw, argon gas is 60-70 sccm, the ion source power is 2kw, oxygen gas is 25sccm, and the deposition rate is 0.23 nm/s;
step six: sputtering of TiO2A film layer, wherein the cathode power is 4kw, the argon gas is 50-60 sccm, the ion source power is 3.5kw, the oxygen gas is 30-40 sccm, and the deposition rate is 0.05 nm/s;
step seven: repeating the fifth step and the sixth step according to the actual spectrum requirement;
step eight: sputtering of Al2O3A film layer, wherein the cathode power is 3.8kw, the argon gas is 60-70 sccm, the ion source power is 3kw, the oxygen gas is 30-40 sccm, and the sputtering rate is 0.18 nm/s;
step nine: and (5) after the plating is finished, taking the workpiece after 10 minutes.
2. The method for preparing a visible infrared window antireflection film based on magnetron sputtering of claim 1, wherein the ion source in the fourth step uses an ICP plasma source.
3. The method for preparing a visible infrared window antireflection film based on magnetron sputtering of claim 1, wherein the sputtering cathode in the fourth step is driven by a direct current pulse direct current power supply.
4. The method of claim 1, wherein the ionizing gas of the ion source in the fourth step uses oxygen with a purity of 99.99%.
5. The visible infrared window antireflection film obtained by the production method according to any one of claims 1 to 4.
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| CN202011310042.7A CN112609158B (en) | 2020-11-20 | 2020-11-20 | Visible infrared window antireflection film based on magnetron sputtering and preparation method |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003202407A (en) * | 2001-10-25 | 2003-07-18 | Hoya Corp | Optical member with antireflection film and manufacturing method therefor |
| US20040005482A1 (en) * | 2001-04-17 | 2004-01-08 | Tomio Kobayashi | Antireflection film and antireflection layer-affixed plastic substrate |
| CN1985190A (en) * | 2004-05-26 | 2007-06-20 | 株式会社腾龙 | Anti-reflection film |
| CN101806508A (en) * | 2010-02-26 | 2010-08-18 | 北京天瑞星真空技术开发有限公司 | High temperature solar energy selective absorption coating and preparation method thereof |
| CN109073785A (en) * | 2016-05-04 | 2018-12-21 | 依视路国际公司 | It include the optical goods of the anti-reflective coating near infrared region (NIR) with high reflection |
| CN110275230A (en) * | 2018-03-13 | 2019-09-24 | 唯亚威通讯技术有限公司 | The optical device stacked including the optical layer with function treatment |
-
2020
- 2020-11-20 CN CN202011310042.7A patent/CN112609158B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040005482A1 (en) * | 2001-04-17 | 2004-01-08 | Tomio Kobayashi | Antireflection film and antireflection layer-affixed plastic substrate |
| JP2003202407A (en) * | 2001-10-25 | 2003-07-18 | Hoya Corp | Optical member with antireflection film and manufacturing method therefor |
| CN1985190A (en) * | 2004-05-26 | 2007-06-20 | 株式会社腾龙 | Anti-reflection film |
| CN101806508A (en) * | 2010-02-26 | 2010-08-18 | 北京天瑞星真空技术开发有限公司 | High temperature solar energy selective absorption coating and preparation method thereof |
| CN109073785A (en) * | 2016-05-04 | 2018-12-21 | 依视路国际公司 | It include the optical goods of the anti-reflective coating near infrared region (NIR) with high reflection |
| CN110275230A (en) * | 2018-03-13 | 2019-09-24 | 唯亚威通讯技术有限公司 | The optical device stacked including the optical layer with function treatment |
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