CN110004408A - A kind of CO resistant to high temperature2Laser anti-reflection film and preparation method thereof - Google Patents

A kind of CO resistant to high temperature2Laser anti-reflection film and preparation method thereof Download PDF

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CN110004408A
CN110004408A CN201910296990.0A CN201910296990A CN110004408A CN 110004408 A CN110004408 A CN 110004408A CN 201910296990 A CN201910296990 A CN 201910296990A CN 110004408 A CN110004408 A CN 110004408A
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layer
yttrium fluoride
zinc selenide
resistant
high temperature
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CN110004408B (en
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李全民
陈莉
朱敏
王国力
吴玉堂
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Nanjing Wavelength Optoelectronics Technology Co Ltd
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Nanjing Wavelength Optoelectronics Technology Co Ltd
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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
    • C23C14/0623—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
    • C23C14/0694—Halides
    • 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
    • C23C14/221—Ion beam deposition
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Surface Treatment Of Optical Elements (AREA)
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Abstract

The invention discloses a kind of CO resistant to high temperature2Laser anti-reflection film and preparation method thereof, CO resistant to high temperature2Laser anti-reflection film, including basal layer, the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer have been sequentially depositing on basal layer, wherein, the area coverage of the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer is 95% or more of substrate surface area.Present invention CO resistant to high temperature2Laser anti-reflection film, structure is simple, deft design, first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and four layers of the second yttrium fluoride layer, which are combined, has the characteristics that high temperature resistant, high transmittance, film layer are secured, the mutual stress complementation of film layer, film layer are not easily broken, can meet element continuously under the high temperature conditions operation the case where；Each layer material therefor is "dead", will not be to operator and environmental concerns.

Description

A kind of CO resistant to high temperature2Laser anti-reflection film and preparation method thereof
Technical field
The present invention relates to a kind of CO resistant to high temperature2Laser anti-reflection film and preparation method thereof, belongs to CO2Laser anti-reflection film field.
Background technique
Recently as the development of information industry, the materials such as ceramics, glass, printed circuit board, organic matter have been obtained largely Use, for the hot spot for being processed into research of these materials, CO thus2Laser technology is by pay attention to day by day.
Laser film is both link most weak in critical elements and all elements in laser system, laser film Performance superiority and inferiority be largely fixed laser output performance.Laser is to limit laser to Gao Gong to the destruction of optical element The bottleneck that rate, high-energy develop, and the main reason for influence element service life.Therefore, the anti-laser of film is continuously improved Intensity has very important significance.
Optical element, especially optical film layer are lacked in film layer there are various due to material itself with coating process It falls into, in film layer in some way and Density Distribution, these defects are often to lead to the main original of optic element damage to defect Cause.Temperature tolerance difference is current CO2The generally existing defect of laser anti-reflection film, and at present about CO2The high temperature resistant of antireflective coating is reported It is very few.
Summary of the invention
The present invention provides a kind of CO resistant to high temperature2Laser anti-reflection film and preparation method thereof, by optimizing Film Design structure, To reach the promotion of film layer performance resistant to high temperature, and then extend element service life by promoting threshold for resisting laser damage； Further, by the improvement of preparation process, reduce film layer defect, the comprehensive performance of film layer is made to be significantly improved.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
A kind of CO resistant to high temperature2Laser anti-reflection film, including basal layer, be sequentially depositing on basal layer the first yttrium fluoride layer, It is fluorinated ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer, wherein the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and second The area coverage of yttrium fluoride layer is 95% or more of substrate surface area.
It is deposited with the first yttrium fluoride layer of low-refraction on the application basal layer, is deposited with low-refraction on yttrium fluoride layer It is fluorinated ytterbium calcium layer, the zinc selenide layer for being deposited with high refractive index in ytterbium calcium layer is fluorinated, is deposited with the second yttrium fluoride layer on zinc selenide layer.
Coating materials requires: 1, itself not absorbing or seldom absorb laser output light；2, it is inhaled under conditions of actual use It is as small as possible to receive coefficient variation with temperature；3, should have preferable thermal conductivity, so as to can if necessary operating condition it is severe Or high-power output) take measures effectively to cool down and worked normally with assuring element；4, there should be certain intensity.Applicant's warp Research is found: in infrared band, in contrast the absorption of ZnSe is minimum, other characteristics are preferable, and suitable low-index material has YF3(yttrium fluoride), YBF3- Ca (fluorination ytterbium calcium), ThF4(thorium fluoride), BaF2Different materials such as (barium fluorides), but due to Th member It is known as radioactivity, therefore has selected YF3And YBF3- Ca, in this two kinds of coating materials, YF3With the variation of temperature, absorbing state changes very Greatly, stress in thin film is caused to happen the phenomenon that changing and then breaking, YBF3- Ca is comparatively more stable, but answers Tensile stress is presented in power, in conjunction with substrate loosely, and two kinds of materials is used in combination, not only stability is good, and far infrared 10.6um The transmitance of wave band reaches 99.5%, and can bear 300 degree of high temperature, and effectively increase lens element application uses the longevity Life.
In first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer, it is fluorinated the physical thickness of ytterbium calcium layer The thickness of maximum, zinc selenide layer takes second place, and the thickness of the first yttrium fluoride layer and the second yttrium fluoride layer is minimum, and such film layer is answered each other Power complementary effect is good, and film layer is not easily broken, and the transmitance of anti-reflection film is high, temperature tolerance is good.
It is preferred that the physical thickness of fluorination ytterbium calcium layer is 8-9.5 times of the first yttrium fluoride layer physical thickness, the object of zinc selenide layer It manages with a thickness of 2-3 times of the first yttrium fluoride layer physical thickness, the physical thickness of the second yttrium fluoride layer is the first yttrium fluoride layer physics 0.95-1.05 times of thickness.The complementary effect between each film layer can further be promoted in this way, improve the stability of anti-reflection film and resistance to Warm nature.
The transmitance, stability and temperature tolerance of anti-reflection film in order to balance, it is preferable that the physical thickness of the first yttrium fluoride layer is 95-100 nanometers.
The transmitance, stability and temperature tolerance of anti-reflection film in order to balance, it is preferable that the physical thickness of fluorination ytterbium calcium layer is 860- 870 nanometers.
The transmitance, stability and temperature tolerance of anti-reflection film in order to balance, it is preferable that the physical thickness of zinc selenide layer is 240- 250 nanometers.
The transmitance, stability and temperature tolerance of anti-reflection film in order to balance, it is preferable that the physical thickness of the second yttrium fluoride layer is 95-100 nanometers.
In order to ensure the transmitance of anti-reflection film, it is preferable that basal layer is zinc selenide basal layer.Applicant it has been investigated that, selenium Change the absorption coefficient that zinc has good infrared transmission performance and very little, is the optimal selection of basal layer.Zinc selenide basal layer Thickness is preferably 3 ± 0.1mm.
Above-mentioned CO resistant to high temperature2The preparation method of laser anti-reflection film, is successively sunk on the base layer in a manner of vacuum evaporation The first yttrium fluoride layer of product, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer.
In order to reduce film defect, it is preferable that above-mentioned CO resistant to high temperature2The preparation method of laser anti-reflection film, including be connected in order Following steps:
1) independent fritting processing is carried out to yttrium fluoride, fluorination ytterbium calcium and zinc selenide coating materials, removes the impurity (packet inside coating materials Include bubble, steam etc.)；
2) it after cleaning basal layer, is placed in vacuum chamber, is by force (1.8 ± 0.2) × 10 in vacuum intraventricular pressure-3Pa, baking Under conditions of temperature is 100 ± 5 DEG C, the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer are sequentially depositing on the surface of basal layer With the second yttrium fluoride layer.
In order to further ensure that the fastness of film layer, in step 2), the first yttrium fluoride layer, fluorination ytterbium calcium layer and the second fluorine Change in yttrium layer evaporation process and needs ion assisted deposition.
In order to further ensure that the fastness of film layer, in step 2), when depositing the first yttrium fluoride layer, the evaporation of yttrium fluoride Rate is 0.28 ± 0.02nm/S, and ion source line is 20A；
When depositing fluorinated ytterbium calcium layer, the evaporation rate of fluorination ytterbium calcium is 0.28 ± 0.02nm/S, and ion source line is 20A, This layer only uses ion source in preceding 100nm；
When depositing zinc selenide layer, zinc selenide evaporation rate is 0.17 ± 0.02nm/S, does not use ion source；
When depositing the second yttrium fluoride layer, the evaporation rate of yttrium fluoride is 0.28 ± 0.02nm/S, and ion source line is 20A.
The present invention is in order to improve the use temperature of CO2 laser condensing lens, the side such as selection and Stress match from film material It is optimized in face of film structure, using the electron beam evaporation process of ion assisted deposition, is prepared for the Hao ﹑ attachment of optical property Xing can high temperature resistant anti-reflection film of the You Liang ﹑ based on zinc selenide substrate.The membrane system has to be reached in the transmitance of far infrared 10.6um wave band To 99.5%, and 300 DEG C or more of high temperature can be born, effectively increase the service life of lens element application.
The unmentioned technology of the present invention is referring to the prior art.
Present invention CO resistant to high temperature2Laser anti-reflection film, structure is simple, deft design, the first yttrium fluoride layer, fluorination ytterbium calcium Layer, zinc selenide layer and four layers of the second yttrium fluoride layer, which combine, has that high temperature resistant, high transmittance, film layer be secured, the mutual stress of film layer The features such as complementary, film layer is not easily broken, can meet element continuously under the high temperature conditions operation the case where；Each equal nothing of layer material therefor Radioactivity, will not be to operator and environmental concerns.
Detailed description of the invention
Fig. 1 is CO resistant to high temperature in embodiment 12The structural schematic diagram of laser anti-reflection film；
Fig. 2 is CO resistant to high temperature in embodiment 12Laser anti-reflection film single side reflectance curve figure (abscissa be wavelength/ Nm, ordinate are reflectivity/%)；
Fig. 3 is CO common in comparative example 12The structural schematic diagram of laser anti-reflection film；
Fig. 4 is CO common in comparative example 12The single side reflectance curve figure of laser anti-reflection film；
In figure, 1 is basal layer, and 2 be the first yttrium fluoride layer, and 3 be fluorination ytterbium calcium layer, and 4 be zinc selenide layer, and 5 be the second fluorination Yttrium layer, 6 be air, and 7 be the second zinc sulfide layer.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention Content is not limited solely to the following examples.
Using 800 type coating machine of southern light in lower example, crystalline substance control uses INFICON SQC-310 controller, is to utilize quartz Crystal oscillation frequency changes to measure film quality thickness.The Kaufman ion source of nine chapter development of section, leads in ion source use Rationally control ion energy is crossed, the consistency of deposition film can be improved, improves optically and mechanically performance.
Embodiment 1
As shown in Figure 1, a kind of CO resistant to high temperature2Laser anti-reflection film, including basal layer have been sequentially depositing first on basal layer Yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer, wherein the first yttrium fluoride layer, fluorination ytterbium calcium layer, selenizing Zinc layers and the area coverage of the second yttrium fluoride layer are the 98% of substrate surface area.
The physical thickness of first yttrium fluoride layer is 96 nanometers；The physical thickness for being fluorinated ytterbium calcium layer is 866 nanometers；Zinc selenide layer Physical thickness be 242 nanometers；The physical thickness of second yttrium fluoride layer is 97 nanometers；Basal layer is with a thickness of 3mm selenizing zinc-base Bottom.
Above-mentioned CO resistant to high temperature2The preparation method of laser anti-reflection film, including the following steps being connected in order:
1) independent fritting processing is carried out to yttrium fluoride, fluorination ytterbium calcium, zinc selenide coating materials, removes the impurity inside coating materials；
2) it after cleaning basal layer, is placed in vacuum chamber, is by force 1.8 × 10 in vacuum intraventricular pressure-3Pa, baking temperature are Under conditions of 100 DEG C, the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second fluorine are sequentially depositing on the surface of basal layer Change yttrium layer；When depositing the first yttrium fluoride layer, the evaporation rate of yttrium fluoride is 0.28nm/S, ion source: acceleration voltage 250V, screen Pole tension is 400V, line 20A；When depositing fluorinated ytterbium calcium layer, fluorination ytterbium calcium evaporation rate be 0.28nm/S, ion source: Acceleration voltage is 250V, plate voltage 400V, line 20A, this layer only uses ion source in preceding 100nm；Deposit zinc selenide When layer, zinc selenide evaporation rate is 0.17nm/S, does not use ion source；When depositing the second yttrium fluoride layer, the evaporation speed of yttrium fluoride Rate is 0.28nm/S, ion source: acceleration voltage 250V, plate voltage 400V, line 20A.Gained CO resistant to high temperature2Swash Light anti-reflection film reaches 99.5% in the transmitance of far infrared 10.6um wave band.
Embodiment 2
As shown in Figure 1, a kind of CO resistant to high temperature2Laser anti-reflection film, including basal layer have been sequentially depositing first on basal layer Yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer, wherein the first yttrium fluoride layer, fluorination ytterbium calcium layer, selenizing Zinc layers and the area coverage of the second yttrium fluoride layer are the 98% of substrate surface area.
The physical thickness of first yttrium fluoride layer is 98 nanometers；The physical thickness for being fluorinated ytterbium calcium layer is 863 nanometers；Zinc selenide layer Physical thickness be 246 nanometers；The physical thickness of second yttrium fluoride layer is 99 nanometers；Basal layer is the zinc selenide with a thickness of 3mm Basal layer.
Above-mentioned CO resistant to high temperature2The preparation of laser anti-reflection film is referring to embodiment 1.Gained CO resistant to high temperature2Laser anti-reflection film exists The transmitance of far infrared 10.6um wave band reaches 99.5%.
Film obtained by above-mentioned each example is performed the following performance tests, reference standard is that American army mark MIL-48497A film environment can By the standard of property test, concrete outcome is as follows:
1) high temperature resistant is tested: after plated film print is toasted 6 hours at 300 DEG C, being down to room temperature, it is further heated up to 300 DEG C baking 6 hours, film layer without peeling, blistering, crackle, demoulding phenomena such as；
2) water resistance test: after being impregnated 24 hours in the water at being 50 DEG C in temperature by plated film print, film layer without fragmentation, And with width be 2cm, the adhesive tape of peel strength I > 2.94N/cm is cemented in film surface, by adhesive tape from the edge of part towards table After the rapid pull-up of the vertical direction in face, film layer nothing falls off, is not damaged；
3) adhesive force is tested；It is close to coated surface with 1 inch of width of 3M special adhesive tape, it is then fast along film surface vertical direction Fast pull-up is pullled 10 times, repeatedly without stripping phenomenon.
Comparative example 1
As shown in Figure 3, a kind of common CO2Laser anti-reflection film, including basal layer have been sequentially depositing the first fluorine on basal layer Change yttrium layer and the second zinc sulfide layer, wherein the first yttrium fluoride layer, the second zinc sulfide layer area coverage be substrate surface face Long-pending 98%.
The physical thickness of first yttrium fluoride layer is 967 nanometers；Second layer zinc sulfide layer is 308 nanometers, and basal layer is thickness For the zinc selenide basal layer of 3mm.
Above-mentioned common CO2The preparation method of laser anti-reflection film, including the following steps being connected in order:
1) independent fritting processing is carried out to yttrium fluoride, zinc sulphide coating materials, removes the impurity inside coating materials；
2) it after cleaning basal layer, is placed in vacuum chamber, is by force 1.8 × 10 in vacuum intraventricular pressure-3Pa, baking temperature are Under conditions of 100 DEG C, the first yttrium fluoride layer and the second zinc sulfide layer are sequentially depositing on the surface of basal layer；Deposit the first yttrium fluoride When layer, the evaporation rate of yttrium fluoride is 0.28nm/S, and ion source: acceleration voltage 250V, plate voltage 400V, line are 20A, this layer only use ion source in preceding 100nm；When depositing zinc sulfide layer, zinc sulphide evaporation rate is 0.17nm/S, is not used Ion source；The common CO of gained2Laser anti-reflection film reaches 99.5% in the transmitance of far infrared 10.6um wave band.
Film obtained by above-mentioned each example is performed the following performance tests, reference standard is that American army mark MIL-48497A film environment can By the standard of property test, concrete outcome is as follows:
1) high temperature resistant is tested: after plated film print is toasted 6 hours at 300 DEG C, being down to room temperature, it is further heated up to 300 DEG C baking 6 hours, there is phenomena such as peeling, blistering, crackle, demoulding in film layer；
2) water resistance test: after being impregnated 24 hours in the water at being 50 DEG C in temperature by plated film print, film layer without fragmentation, And with width be 2cm, the adhesive tape of peel strength I > 2.94N/cm is cemented in film surface, by adhesive tape from the edge of part towards table After the rapid pull-up of the vertical direction in face, film layer nothing falls off, is not damaged；
3) adhesive force is tested；It is close to coated surface with 1 inch of width of 3M special adhesive tape, it is then fast along film surface vertical direction Fast pull-up is pullled 10 times, repeatedly without stripping phenomenon.

Claims (10)

1. a kind of CO resistant to high temperature2Laser anti-reflection film, it is characterised in that: including basal layer, the first fluorine has been sequentially depositing on basal layer Change yttrium layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer, wherein the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide The area coverage of layer and the second yttrium fluoride layer is 95% or more of substrate surface area.
2. CO resistant to high temperature according to claim 12Laser anti-reflection film, it is characterised in that: the physical thickness of fluorination ytterbium calcium layer Greater than the physical thickness of zinc selenide layer.
3. CO resistant to high temperature according to claim 22Laser anti-reflection film, it is characterised in that: the physics of the first yttrium fluoride layer is thick The physical thickness of degree and the second yttrium fluoride layer is respectively less than the physical thickness of zinc selenide layer.
4. CO resistant to high temperature according to claim 32Laser anti-reflection film, it is characterised in that: the physical thickness of fluorination ytterbium calcium layer It is 8-9.5 times of the first yttrium fluoride layer physical thickness, the physical thickness of zinc selenide layer is the 2-3 of the first yttrium fluoride layer physical thickness Times, the physical thickness of the second yttrium fluoride layer is 0.95-1.05 times of the first yttrium fluoride layer physical thickness.
5. CO resistant to high temperature according to any one of claims 1-42Laser anti-reflection film, it is characterised in that: the first yttrium fluoride The physical thickness of layer is 95-100 nanometers；The physical thickness for being fluorinated ytterbium calcium layer is 860-870 nanometers；The physical thickness of zinc selenide layer It is 240-250 nanometers；The physical thickness of second yttrium fluoride layer is 95-100 nanometers.
6. CO resistant to high temperature according to any one of claims 1-42Laser anti-reflection film, it is characterised in that: basal layer is thickness Degree is the zinc selenide basal layer of 3 ± 0.1mm；CO resistant to high temperature2Laser anti-reflection film is reached in the transmitance of far infrared 10.6um wave band To 99.5%, temperature tolerance is greater than 300 DEG C.
7. CO resistant to high temperature as claimed in any one of claims 1 to 62The preparation method of laser anti-reflection film, it is characterised in that: with true The mode of sky evaporation is sequentially depositing the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the second yttrium fluoride layer on the base layer.
8. preparation method according to claim 7, it is characterised in that: including the following steps being connected in order:
1) independent fritting processing is carried out to yttrium fluoride, fluorination ytterbium calcium and zinc selenide coating materials, removes the impurity inside coating materials；
2) it after cleaning basal layer, is placed in vacuum chamber, is by force (1.8 ± 0.2) × 10 in vacuum intraventricular pressure-3Pa, baking temperature Under conditions of 100 ± 5 DEG C, the first yttrium fluoride layer, fluorination ytterbium calcium layer, zinc selenide layer and the are sequentially depositing on the surface of basal layer Bifluoride yttrium layer.
9. preparation method according to claim 8, it is characterised in that: in step 2), the first yttrium fluoride layer, fluorination ytterbium calcium layer And second need ion assisted deposition in yttrium fluoride layer evaporation process.
10. preparation method according to claim 9, it is characterised in that: in step 2), when depositing the first yttrium fluoride layer, fluorine The evaporation rate for changing yttrium is 0.28 ± 0.02nm/S, and ion source line is 20A；
When depositing fluorinated ytterbium calcium layer, the evaporation rate of fluorination ytterbium calcium is 0.28 ± 0.02nm/S, and ion source line is 20A, this layer Only ion source is used in preceding 100nm；
When depositing zinc selenide layer, zinc selenide evaporation rate is 0.17 ± 0.02nm/S, does not use ion source；
When depositing the second yttrium fluoride layer, the evaporation rate of yttrium fluoride is 0.28 ± 0.02nm/S, and ion source line is 20A.
CN201910296990.0A 2019-04-15 2019-04-15 High-temperature-resistant CO 2 Laser antireflection film and preparation method thereof Active CN110004408B (en)

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CN113900165A (en) * 2021-11-16 2022-01-07 天津津航技术物理研究所 Barium fluoride substrate composite antireflection film and structure design method thereof

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Publication number Priority date Publication date Assignee Title
CN113900165A (en) * 2021-11-16 2022-01-07 天津津航技术物理研究所 Barium fluoride substrate composite antireflection film and structure design method thereof
CN113900165B (en) * 2021-11-16 2023-09-22 天津津航技术物理研究所 Barium fluoride substrate composite antireflection film and structural design method thereof

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