CN114488361B - Ultra-low stress 8-12 mu m infrared broadband antireflection film and preparation method thereof - Google Patents
Ultra-low stress 8-12 mu m infrared broadband antireflection film and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 230000003287 optical effect Effects 0.000 claims abstract description 9
- 238000002834 transmittance Methods 0.000 claims abstract description 8
- 238000002310 reflectometry Methods 0.000 claims abstract description 7
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 7
- 239000010980 sapphire Substances 0.000 claims abstract description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 238000010894 electron beam technology Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 230000001133 acceleration Effects 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000007888 film coating Substances 0.000 claims description 2
- 238000009501 film coating Methods 0.000 claims description 2
- 230000003667 anti-reflective effect Effects 0.000 claims 2
- 239000012528 membrane Substances 0.000 claims 2
- 238000000869 ion-assisted deposition Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 230000003595 spectral effect Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 96
- 238000012360 testing method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000005566 electron beam evaporation Methods 0.000 description 2
- 239000012788 optical film Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
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- 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
-
- 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
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- 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
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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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
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
- C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
- C23C14/546—Controlling the film thickness or evaporation rate using measurement on deposited material using crystal oscillators
-
- 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
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Abstract
The invention discloses an ultra-low stress 8-12 mu m infrared broadband anti-reflection film and a preparation method thereof, the ultra-low stress 8-12 mu m infrared broadband anti-reflection film has a film system structure of SUB/aHbLcHdLeH/air, wherein SUB represents a sapphire substrate, air represents air, H represents a ZnSe layer, L represents a Yb-A layer, and Yb-A layer is YF 3 1 to 8 weight percent of YbF doped with calcium 3 A mixed film layer with the volume ratio of 1:1-5:1; a-e represent coefficients of quarter reference wavelength optical thickness for each layer. According to the ultra-low stress infrared broadband antireflection film with the thickness of 8-12 mu m and the preparation method thereof, the antireflection film layer with small stress change is obtained through the collocation of mixed film materials, the surface shape of the film layer after the finished product is maintained at the original surface shape of the substrate, so that the better film firmness is obtained, the problems of large stress between film layers and small film adhesion are effectively solved, the obtained film layer has good spectral performance and better mechanical stability, the average single-sided reflectivity of 8-12 mu m is not more than 0.3%, the average double-sided transmittance is not less than 99.3%, and the film stress is close to 0.
Description
Technical Field
The invention relates to an ultra-low stress 8-12 mu m infrared broadband anti-reflection film and a preparation method thereof, belonging to the technical field of infrared broadband anti-reflection films.
Background
Optical films are extremely widely used, but almost all films have different levels of stress, especially in the infrared range, due to their relatively thick film layers and poor strength. The existence of stress can directly lead to phenomena such as film shedding, color splitting and the like, and seriously influence the performances of various aspects of products. The property and the size of the film stress are closely related to a substrate, a film material, a deposition process, a deposition condition and the like; for many years, several documents have reported electron beam evaporation and various influencing factors, but no related report for eliminating stress through film material matching exists at present.
Disclosure of Invention
The invention provides an ultra-low stress 8-12 mu m infrared broadband antireflection film and a preparation method thereof, wherein an antireflection film layer with small stress change is obtained through proportioning, selection and film material matching among film layers, and the surface shape of the film layer after finished products is maintained at the original surface shape of a substrate, so that good film firmness is obtained, the problems of high stress among the film layers and small film layer adhesive force are effectively solved, and the obtained film layer has good spectral performance and good mechanical stability.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
an ultra-low stress infrared broadband anti-reflection film with the thickness of 8-12 μm has a film system structure of SUB/aHbLcHdLeH/air, wherein SUB represents a sapphire substrate, air represents air, H represents a ZnSe layer, L represents a Yb-A layer, and Yb-A layer is YF 3 1 to 8 weight percent of YbF doped with calcium 3 A mixed film layer with the volume ratio of 1:1-5:1; a-e represent coefficients of quarter reference wavelength optical thickness for each layer.
The high refractive index material ZnSe in the infrared band has the light transmission range of 0.5-15 mu m, extremely low scattering loss and high bearing capacity on thermal shock. The ZnSe and Yb-A are adopted as high-refractive index film materials and low-refractive index film materials respectively, the film system is optimally designed and compared through different schemes, the film system structure SUB/aHbLcHdLeH/A is generated, the stress problem between film layers is effectively solved, the compactness of the film layer is improved, the film layer is firmer, and the service life is longer.
YF 3 And YbF 3 The inventor researches that the two film materials are greatly influenced by the process conditions during deposition, and the film materials are usually expressed as tensile stress and moderately calcium-doped YbF 3 May exhibit compressive stress; and YbF 3 In contrast, YF 3 With lower refractive index, in film system design, is easyObtaining lower single-sided reflectivity; using YF 3 1 to 8 weight percent of YbF doped with calcium 3 The mixed film layer and the ZnSe layer with the volume ratio of 1:1-5:1 are alternately arranged according to a specific thickness, and the 8-12 mu m infrared broadband anti-reflection film with the film stress (overall comprehensive stress) close to 0Gpa is obtained.
The values of a to e are related to the reference wavelength lambda, and preferably, a has a value of 1.00 to 1.60, b has a value of 1.70 to 2.30, c has a value of 13.00 to 13.60, d has a value of 12.70 to 13.30, and e has a value of 2.55 to 3.15. Further preferably, a is 1.30 to 1.34, b is 1.98 to 2.02, c is 13.28 to 13.32, d is 12.98 to 13.02, and e is 2.83 to 2.87. More preferably, a has a value of 1.32, b has a value of 2.00, c has a value of 13.30, d has a value of 13.00, and e has a value of 2.85.
In order to better consider the optical performance and mechanical performance of the antireflection film, aH is a first ZnSe layer, bL is a first Yb-A layer, cH is a second ZnSe layer, dL is a second Yb-A layer, and eH is a third ZnSe layer; the physical thickness of the first ZnSe layer is 400+/-50 nm, the physical thickness of the first Yb-A layer is 140+/-20 nm, the physical thickness of the second ZnSe layer is 600+/-50 nm, the physical thickness of the second Yb-A layer is 1200+/-100 nm, and the physical thickness of the third ZnSe layer is 200+/-30 nm.
The transparent film is plated on both sides, and the film system structure is air/eHdLcHbLaH/SUB/aHbLcHdLeH/air. The average single-sided reflectivity of the film system structure of 8-12 mu m is not more than 0.3%, the average double-sided transmission is not less than 99.3%, and the film stress is calculated to be close to 0 through the surface type.
The application adopts the Newton's ring method formulaCalculating film stress, when the film surface diameter is more than 50 times larger than the thickness, measuring the curvature radius r of interference seasoning to derive the film stress sigma, wherein ts is not the thickness of the substrate, t f Where Es is the Young's modulus of elasticity of the substrate and v is the Poisson's ratio of the substrate. />
The ultra-low stress infrared broadband antireflection film with the thickness of 8-12 mu m is deposited by ion assistance in the film coating process; before coating, the sapphire substrate is baked for 0.5 to 1 hour at the temperature of between 90 and 100 ℃; the initial vacuum degree is (0.8-1.2) 10-3Pa, and the ion source parameters are set as follows: acceleration voltage is 200V, screen voltage is 450+ -50V, and beam current is 40+ -20 mA.
In order to further increase the density of the deposited film and improve the optical and mechanical properties, znSe is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.8+/-0.1 nm/s. The Yb-A layer is evaporated by adopting a graphite crucible electron beam, and the evaporation rate is controlled to be 0.8+/-0.1 nm/s. During the evaporation of Yb-A layer, YF is first deposited 3 1 to 8 weight percent of YbF doped with calcium 3 Mixing according to the volume ratio of 1:1-5:1, and then adopting a graphite crucible to carry out electron beam evaporation.
According to the method, various process parameters are reasonably controlled by effectively selecting the coating materials, and the multilayer film is coated on the substrate, so that the film index meets the transmittance requirement of 8-12 mu m, and meanwhile, the residual stress of the film is close to zero, thereby effectively solving the defects of film layer insecurity and the like in the wave band.
The technology not mentioned in the present invention refers to the prior art.
According to the ultra-low stress infrared broadband antireflection film with the thickness of 8-12 mu m and the preparation method thereof, the antireflection film layer with small stress change is obtained through the collocation of mixed film materials, the surface shape of the film layer after the finished product is maintained at the original surface shape of the substrate, so that the better film firmness is obtained, the problems of large stress between film layers and small film adhesion are effectively solved, the obtained film layer has good spectral performance and better mechanical stability, the average single-sided reflectivity of 8-12 mu m is not more than 0.3%, the average double-sided transmittance is not less than 99.3%, and the film stress is close to 0Gpa.
Drawings
FIG. 1 is a schematic structural diagram of an ultra-low stress 8-12 μm infrared broadband antireflection film in example 1 of the present invention;
FIG. 2 is a theoretical design single-sided reflection curve diagram of an ultra-low stress 8-12 μm infrared broadband anti-reflection film in example 1 of the present invention;
FIG. 3 is a graph of the single-sided reflection of an ultra-low stress 8-12 μm infrared broadband antireflection film in example 1 of the present invention;
FIG. 4 is a graph showing the double-sided transmission of an ultra-low stress, 8-12 μm infrared broadband antireflection film in example 1 of the present invention;
FIG. 5 is a comparative diagram of the transformation of the front and rear sides of a single-sided coating on a substrate (a is before coating, b is after coating) in example 1 of the present invention;
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
Example 1
As shown in FIG. 1, the ultra-low stress infrared broadband anti-reflection film with the thickness of 8-12 μm has a film system structure of air/eHdLcHbLaH/SUB/aHbLcHdLeH/air, wherein SUB represents a sapphire substrate, air represents air, H represents a ZnSe layer, L represents a Yb-A layer, and Yb-A layer is YF 3 3wt% of YbF doped with calcium 3 A mixed film layer with a volume ratio of 2:1; a-e represents the coefficient of quarter reference wavelength optical thickness of each layer, a has a value of 1.32, b has a value of 2.00, c has a value of 13.30, d has a value of 13.00, and e has a value of 2.85; aH is a first ZnSe layer, bL is a first Yb-A layer, cH is a second ZnSe layer, dL is a second Yb-A layer, and eH is a third ZnSe layer; the physical thickness of the first ZnSe layer is 400nm, the physical thickness of the first Yb-A layer is 140nm, the physical thickness of the second ZnSe layer is 600nm, the physical thickness of the second Yb-A layer is 1200nm, and the physical thickness of the third ZnSe layer is 200nm;
film forming apparatus: the wafer control adopts INFICON IC6 controller by using a Wittman light 1100 type film plating machine, and the quality and thickness of the film are measured by using the oscillation frequency change of quartz crystals. The ion source adopts koufman ion source developed by Jiu chapter in Zhongke. The vacuum chamber is matched with a diffusion pump and a cryogenic unit system by a mechanical pump to obtain the vacuum degree required by a film system, and a thermocouple meter is used for measuring the vacuum degree.
And (3) carrying out ultrasonic cleaning on the sapphire substrate before coating, removing residual dirt on the surface, and baking for 0.5h at a baking temperature of 100 ℃, wherein the initial vacuum degree during film deposition is about 1.0 x 10 < -3 > Pa. The ion source parameters were set as: acceleration voltage is 200V, screen voltage is 450V, and beam current is about 40 mA. In the film deposition process, a kofmann ion source is used for assisting deposition, so that the aggregation density is increased, the structural integrity is improved, the performance and the service time of the film are improved, the optical thickness is controlled by adopting a light control method, and the evaporation rate is controlled by adopting a crystal control method. ZnSe is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.8nm/s; yb-A is evaporated by adopting a graphite crucible electron beam, and the evaporation rate is controlled to be 0.8nm/s.
Test results:
optical performance test: the single-sided reflectivity and the double-sided transmissivity of the film are tested by adopting an infrared spectrophotometer Spectrum100, and the obtained Spectrum curve meets the design requirement: as shown in FIGS. 3 to 4, the average single-sided reflectance of 8 to 12 μm was less than 0.3% and the average double-sided transmittance was more than 99.3%, and the film stress was calculated to be-0.04 Gpa according to the Newton's ring method formula by the surface shape shown in FIG. 5.
Film performance test
In order to ensure the reliability of the optical element, the following environmental test is carried out on the broadband antireflection film sample according to the requirements of the general specification of the GJB2485-95 optical film layer:
(1) Abrasion resistance test: 2 layers of dry absorbent gauze are wrapped outside the rubber friction head, the film layers are rubbed along the same track under the pressure of 9.8N, the film layers are reciprocated for 1000 times, and the film layers are free of scratches and other damages.
(2) Salt spray test: at 35 ℃ environment temperature, 5% NaCl is continuously sprayed for 12 hours for two cycles, and the total time is 24 hours, so that the film layer is free from abnormality.
(3) Soaking test: the sample was completely immersed in distilled or deionized water, and after 96 hours, the film layer was free of anomalies.
(4) High-low temperature test: the temperature is kept at-65 ℃ for 2 hours, the temperature is quickly switched from-65 ℃ to 80 ℃ for 2 hours, and the temperature is kept from 80 ℃ to-65 ℃ for 2 hours, and the film layer is free from abnormality.
(5) Adhesion experiments: the adhesive tape is firmly adhered on the surface of the film layer by using a 3M adhesive tape with the width of 1cm, and the film layer is free from falling off and damage after the adhesive tape paper is rapidly pulled up from the edge of the part to the vertical direction of the surface, and the process is repeated for 30 times, so that the film layer is free from falling off and damage.
Comparative example 1
Replacement of Yb-A layer in example 1 with YF 3 The remainder were referred to example 1. The average single-sided reflectivity of 8-12 μm is 0.28%, the average double-sided transmittance is 99.22%, and the film stress is 21.57Gpa as calculated by the surface type, so that the film stress is larger, and the film stripping phenomenon is easy to occur.
Comparative example 2
Replacement of Yb-A layer in example 1 with YbF 3 The remainder were referred to example 1. The average single-sided reflectance of 8-12 μm is 0.7%, the average double-sided transmittance is 98.5%, and the film stress is 13.83GPa as calculated by the surface type, so that the film stress and the film firmness are slightly improved, but the film system index is poor.
Comparative example 3
The Yb-A layer of example 1 was replaced with 3wt% calcium-doped YbF 3 The remainder were referred to example 1. The average single-sided reflection of 8-12 μm was 0.5% and the average double-sided transmittance was 98.8%, and the film stress and film firmness were slightly improved by calculating the film stress as-2.3 Gpa by the surface type, but the film stress and film firmness were not enough as compared with example 1.
Claims (6)
1. An ultra-low stress 8-12 mu m infrared broadband antireflection film is characterized in that: the membrane system structure is SUB/aHbLcHdLeH/air, wherein SUB represents a sapphire substrate, air represents air, H represents a ZnSe layer, L represents a Yb-A layer, and Yb-A layer is YF 3 1 to 8 weight percent of YbF doped with calcium 3 A mixed film layer with the volume ratio of 1:1-5:1; a-e represent coefficients of quarter reference wavelength optical thickness for each layer;
aH is a first ZnSe layer, bL is a first Yb-A layer, cH is a second ZnSe layer, dL is a second Yb-A layer, and eH is a third ZnSe layer; the physical thickness of the first ZnSe layer is 400+/-50 nm, the physical thickness of the first Yb-A layer is 140+/-20 nm, the physical thickness of the second ZnSe layer is 600+/-50 nm, the physical thickness of the second Yb-A layer is 1200+/-100 nm, and the physical thickness of the third ZnSe layer is 200+/-30 nm.
2. The ultra-low stress, 8-12 μm infrared broadband antireflective film of claim 1, wherein: the membrane system structure is air/eHdLcHbLaH/SUB/aHbLcHdLeH/air.
3. The ultra-low stress, 8-12 μm infrared broadband antireflective film of claim 1 or 2, wherein: the average single-sided reflectivity of 8-12 μm is not more than 0.3%, the average double-sided transmittance is not less than 99.3%, and the film stress is 0.
4. A method for preparing an ultra-low stress 8-12 μm infrared broadband antireflection film according to any one of claims 1-3, which is characterized in that: ion-assisted deposition is adopted in the film coating process; before coating, the sapphire substrate is baked for 0.5 to 1 hour at the temperature of between 90 and 100 ℃; the initial vacuum degree is (0.8-1.2) 10 -3 Pa, ion source parameters are set as: acceleration voltage is 200V, screen voltage is 450+ -50V, and beam current is 40+ -20 mA.
5. The method of manufacturing according to claim 4, wherein: znSe was electron beam evaporated using a copper crucible with an evaporation rate controlled at 0.8.+ -. 0.1nm/s.
6. The method of claim 4 or 5, wherein: yb-A is evaporated by adopting a graphite crucible electron beam, and the evaporation rate is controlled to be 0.8+/-0.1 nm/s.
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| CN202210072105.2A CN114488361B (en) | 2022-01-21 | 2022-01-21 | Ultra-low stress 8-12 mu m infrared broadband antireflection film and preparation method thereof |
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| CN202210072105.2A CN114488361B (en) | 2022-01-21 | 2022-01-21 | Ultra-low stress 8-12 mu m infrared broadband antireflection film and preparation method thereof |
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| CN114488361A CN114488361A (en) | 2022-05-13 |
| CN114488361B true CN114488361B (en) | 2024-02-09 |
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| CN202210072105.2A Active CN114488361B (en) | 2022-01-21 | 2022-01-21 | Ultra-low stress 8-12 mu m infrared broadband antireflection film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07331412A (en) * | 1994-06-10 | 1995-12-19 | Sumitomo Electric Ind Ltd | Optical parts for infrared ray and their production |
| CN204331075U (en) * | 2014-12-24 | 2015-05-13 | 南京波长光电科技股份有限公司 | A kind of infrared glass GASIR1 anti-reflection film |
| CN206920633U (en) * | 2017-07-13 | 2018-01-23 | 南京波长光电科技股份有限公司 | A kind of near-infrared is to middle ultra-wideband anti-reflection film |
| CN111164463A (en) * | 2017-07-31 | 2020-05-15 | 康宁股份有限公司 | Hard antireflective coatings |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07331412A (en) * | 1994-06-10 | 1995-12-19 | Sumitomo Electric Ind Ltd | Optical parts for infrared ray and their production |
| CN204331075U (en) * | 2014-12-24 | 2015-05-13 | 南京波长光电科技股份有限公司 | A kind of infrared glass GASIR1 anti-reflection film |
| CN206920633U (en) * | 2017-07-13 | 2018-01-23 | 南京波长光电科技股份有限公司 | A kind of near-infrared is to middle ultra-wideband anti-reflection film |
| CN111164463A (en) * | 2017-07-31 | 2020-05-15 | 康宁股份有限公司 | Hard antireflective coatings |
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