CN110004408B - High-temperature-resistant CO 2 Laser antireflection film and preparation method thereof - Google Patents

High-temperature-resistant CO 2 Laser antireflection film and preparation method thereof Download PDF

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CN110004408B
CN110004408B CN201910296990.0A CN201910296990A CN110004408B CN 110004408 B CN110004408 B CN 110004408B CN 201910296990 A CN201910296990 A CN 201910296990A CN 110004408 B CN110004408 B CN 110004408B
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yttrium fluoride
fluoride layer
zinc selenide
yttrium
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CN110004408A (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
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    • 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
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    • 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
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Abstract

The invention discloses a high-temperature resistant CO 2 Laser antireflection film and preparation method thereof, and high-temperature-resistant CO (carbon monoxide) 2 The laser antireflection film comprises a substrate layer, wherein a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer are sequentially deposited on the substrate layer, and the coverage areas of the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are more than 95% of the surface area of the substrate layer. The invention is resistant to high temperature CO 2 The laser antireflection film has the characteristics of simple structure, exquisite design, high temperature resistance, high transmittance, firm film layers, mutual stress complementation of the film layers, difficult rupture of the film layers and the like, and can meet the condition that the element continuously operates under the high temperature condition when the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are combined; the materials used in each layer are non-radioactive and do not cause damage to operators and the environment.

Description

High-temperature-resistant CO 2 Laser antireflection film and preparation method thereof
Technical Field
The invention relates to a high temperature resistant CO 2 Laser antireflection film and preparation method thereof, belonging to CO 2 Laser antireflection film field.
Background
In recent years, with the development of information industry, materials such as ceramics, glass, printed circuit boards, organic matters and the like have been used in large amounts, and the processing of these materials has become a hot spot for research, and this has been CO 2 Laser technology is increasingly gaining importance.
The laser film is not only an important element in a laser system, but also the weakest link in all elements, and the performance of the laser film determines the performance of laser output to a great extent. Damage to optical components by laser light is a bottleneck limiting the development of laser light to high power and high energy and is also a major cause of affecting the useful life of the components. Therefore, the laser resistance of the film is continuously improved, and the film has very important significance.
Optical elements, in particular optical films, due to the material itself andthe film coating process causes various defects in the film layer, and the defects are distributed in the film layer in a certain mode and density, and the defects are often the main causes of damage to the optical element. Poor temperature resistance is CO 2 The laser anti-reflection film has common defects, and at present, the laser anti-reflection film relates to CO 2 The high temperature resistance of the antireflection film layer is rarely reported.
Disclosure of Invention
The invention provides a high-temperature resistant CO 2 According to the laser antireflection film and the preparation method thereof, the high temperature resistance of the film layer is improved by optimizing the design structure of the film system, and the service life of the element is prolonged by improving the laser damage resistance threshold; further, by improving the preparation process, the defects of the film layer are reduced, and the comprehensive performance of the film layer is obviously improved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
high-temperature-resistant CO 2 The laser antireflection film comprises a substrate layer, wherein a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer are sequentially deposited on the substrate layer, and the coverage areas of the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are more than 95% of the surface area of the substrate layer.
The first yttrium fluoride layer with the low refractive index is deposited on the substrate layer, the ytterbium calcium fluoride layer with the low refractive index is deposited on the yttrium fluoride layer, the zinc selenide layer with the high refractive index is deposited on the ytterbium calcium fluoride layer, and the second yttrium fluoride layer is deposited on the zinc selenide layer.
The requirements of the film material are as follows: 1. does not or hardly absorb the laser output light itself; 2. the change of the absorption coefficient with temperature is as small as possible under the condition of practical use; 3. better thermal conductivity so as to be capable of operating under severe conditions or high power output when necessary) to be effectively cooled to ensure proper operation of the components; 4. should have a certain strength. The applicant found through research that: in the infrared band, znSe has minimal absorption, and other good properties, and suitable low refractive index materials are YF 3 (yttrium fluoride), YBF 3 Ca (ytterbium calcium fluoride), thF 4 (thorium fluoride), baF 2 (barium fluoride) and the like, YF is selected because Th element has radioactivity 3 And YBF 3 Ca, YF of these two membranes 3 With the change of temperature, the absorption condition is greatly changed, so that the film stress condition is changed and then the phenomenon of breakdown occurs, and YBF is generated 3 Ca is relatively stable, but the stress shows tensile stress, and is not firmly combined with the substrate, so that the two materials are combined for use, the stability is good, the transmittance of the far infrared 10.6um wave band reaches 99.5%, the high temperature of 300 ℃ can be born, and the service life of the application of the lens element is effectively prolonged.
Among the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer, the physical thickness of the ytterbium calcium fluoride layer is the largest, the thickness of the zinc selenide layer is the next largest, and the thickness of the first yttrium fluoride layer and the second yttrium fluoride layer is the smallest, so that the mutual stress complementation effect of the film layers is good, the film layers are not easy to break, and the anti-reflection film has high transmittance and good temperature resistance.
Preferably, the physical thickness of the ytterbium calcium fluoride layer is 8-9.5 times of that of the first yttrium fluoride layer, the physical thickness of the zinc selenide layer is 2-3 times of that of the first yttrium fluoride layer, and the physical thickness of the second yttrium fluoride layer is 0.95-1.05 times of that of the first yttrium fluoride layer. Therefore, the complementary effect among the film layers can be further promoted, and the stability and the temperature resistance of the antireflection film are improved.
In order to achieve the transmittance, stability and temperature resistance of the antireflection film, the physical thickness of the first yttrium fluoride layer is preferably 95-100 nanometers.
In order to achieve the transmittance, stability and temperature resistance of the antireflection film, the physical thickness of the ytterbium fluoride calcium layer is preferably 860-870 nanometers.
In order to achieve the transmittance, stability and temperature resistance of the antireflection film, the physical thickness of the zinc selenide layer is preferably 240-250 nanometers.
In order to achieve the transmittance, stability and temperature resistance of the antireflection film, the physical thickness of the second yttrium fluoride layer is preferably 95-100 nanometers.
In order to ensure the transmittance of the antireflection film, the underlayer is preferably a zinc selenide underlayer. The applicant finds that zinc selenide has good infrared transmission performance and small absorption coefficient, and is the best choice of the basal layer. The thickness of the zinc selenide base layer is preferably 3±0.1mm.
The high temperature resistant CO 2 The preparation method of the laser antireflection film comprises the step of sequentially depositing a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer on a basal layer in a vacuum evaporation mode.
In order to reduce film defects, it is preferable that the above-mentioned high temperature resistant CO 2 The preparation method of the laser antireflection film comprises the following steps of:
1) Performing independent premelting treatment on yttrium fluoride, ytterbium calcium fluoride and zinc selenide membrane materials to remove impurities (including bubbles, water vapor and the like) in the membrane materials;
2) Cleaning the substrate layer, placing in a vacuum chamber with pressure of (1.8+ -0.2) ×10 -3 And under the conditions of Pa and baking temperature of 100+/-5 ℃, sequentially depositing a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer on the surface of the basal layer.
In order to further ensure the firmness of the film layer, in step 2), ion-assisted deposition is required during the evaporation of the first yttrium fluoride layer, the ytterbium calcium fluoride layer and the second yttrium fluoride layer.
In order to further ensure the firmness of the film layer, in the step 2), when the first yttrium fluoride layer is deposited, the evaporation rate of yttrium fluoride is 0.28+/-0.02 nm/S, and the ion source beam current is 20A;
when the ytterbium calcium fluoride layer is deposited, the evaporation rate of the ytterbium calcium fluoride is 0.28+/-0.02 nm/S, the beam current of the ion source is 20A, and the ion source is only used at the first 100 nm;
when depositing the zinc selenide layer, the evaporation rate of the zinc selenide is 0.17+/-0.02 nm/S, and an ion source is not used;
when the second yttrium fluoride layer is deposited, the evaporation rate of yttrium fluoride is 0.28+/-0.02 nm/S, and the ion source beam current is 20A.
In order to improve the service temperature of the CO2 laser focusing mirror, the film system structure is optimized in the aspects of material selection, stress matching and the like of a film layer material, and the high-temperature-resistant antireflection film with good optical performance and excellent adhesion performance based on a zinc selenide substrate is prepared by adopting an electron beam evaporation process of ion-assisted deposition. The film system has the transmittance reaching 99.5% in the far infrared 10.6um wave band, can bear the high temperature of more than 300 ℃, and effectively prolongs the service life of the application of the lens element.
The technology not mentioned in the present invention refers to the prior art.
The invention is resistant to high temperature CO 2 The laser antireflection film has the characteristics of simple structure, exquisite design, high temperature resistance, high transmittance, firm film layers, mutual stress complementation of the film layers, difficult rupture of the film layers and the like, and can meet the condition that the element continuously operates under the high temperature condition when the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are combined; the materials used in each layer are non-radioactive and do not cause damage to operators and the environment.
Drawings
FIG. 1 is a high temperature CO resistant of example 1 2 A structural schematic diagram of the laser antireflection film;
FIG. 2 is a high temperature CO resistant of example 1 2 A single-sided reflectance graph (wavelength/nm on the abscissa and reflectance/%);
FIG. 3 is a common CO of comparative example 1 2 A structural schematic diagram of the laser antireflection film;
FIG. 4 is a graph of the common CO of comparative example 1 2 A single-sided reflectivity curve of the laser antireflection film;
in the figure, 1 is a basal layer, 2 is a first yttrium fluoride layer, 3 is a ytterbium calcium fluoride layer, 4 is a zinc selenide layer, 5 is a second yttrium fluoride layer, 6 is air, and 7 is a second zinc sulfide layer.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
In the following example, a south light 800 type film plating machine is adopted, an INFICON SQC-310 controller is adopted for crystal control, and the quality and thickness of the film are measured by utilizing the change of the oscillation frequency of a quartz crystal. The ion source adopts the koufman ion source developed by the Ming dynasty chapter, and the density of the deposited film can be improved and the optical and mechanical properties can be improved by reasonably controlling the ion energy.
Example 1
As shown in FIG. 1, a high temperature resistant CO 2 The laser antireflection film comprises a substrate layer, wherein a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer are sequentially deposited on the substrate layer, and the coverage areas of the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are 98% of the surface area of the substrate layer.
The physical thickness of the first yttrium fluoride layer is 96 nanometers; the physical thickness of the ytterbium fluoride calcium layer is 866 nanometers; the physical thickness of the zinc selenide layer is 242 nanometers; the physical thickness of the second yttrium fluoride layer is 97 nanometers; the basal layer is zinc selenide basal layer with the thickness of 3 mm.
The high temperature resistant CO 2 The preparation method of the laser antireflection film comprises the following steps of:
1) Performing independent premelting treatment on yttrium fluoride, ytterbium calcium fluoride and zinc selenide membrane materials to remove impurities in the membrane materials;
2) After cleaning the substrate layer, it was placed in a vacuum chamber at a pressure of 1.8X10 -3 Under the conditions of Pa and baking temperature of 100 ℃, sequentially depositing a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer on the surface of the basal layer; when depositing the first yttrium fluoride layer, the evaporation rate of yttrium fluoride is 0.28nm/S, and the ion source is as follows: the accelerating voltage is 250V, the screen electrode voltage is 400V, and the beam current is 20A; when the ytterbium fluoride calcium layer is deposited, the evaporation rate of ytterbium fluoride calcium is 0.28nm/S, and the ion source is as follows: the accelerating voltage is 250V, the screen electrode voltage is 400V, the beam current is 20A, and the layer only uses an ion source at the first 100 nm; when depositing the zinc selenide layer, the evaporation rate of the zinc selenide is 0.17nm/S, and an ion source is not used; when depositing the second yttrium fluoride layer, the evaporation rate of yttrium fluoride is 0.28nm/S, and the ion source is as follows: the acceleration voltage was 250V, the screen voltage was 400V, and the beam current was 20A. The obtained CO with high temperature resistance 2 The transmittance of the laser antireflection film in the far infrared 10.6um wave band reaches 99.5 percent.
Example 2
As shown in FIG. 1, a high temperature resistant CO 2 The laser antireflection film comprises a substrate layer, wherein a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer are sequentially deposited on the substrate layer, and the coverage areas of the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are 98% of the surface area of the substrate layer.
The physical thickness of the first yttrium fluoride layer is 98 nanometers; the physical thickness of the ytterbium fluoride calcium layer is 863 nanometers; the physical thickness of the zinc selenide layer was 246 nanometers; the physical thickness of the second yttrium fluoride layer is 99 nanometers; the basal layer is zinc selenide basal layer with thickness of 3 mm.
The high temperature resistant CO 2 The preparation of the laser antireflection film is described in example 1. The obtained CO with high temperature resistance 2 The transmittance of the laser antireflection film in the far infrared 10.6um wave band reaches 99.5 percent.
The films obtained in each example were subjected to the following performance tests, with reference to the standard of the environmental reliability test of the film of the army standard MILs-48497 a, and the specific results are as follows:
1) High temperature resistance test: baking the film-coated sample wafer at 300 ℃ for 6 hours, cooling to normal temperature, and continuously heating to 300 ℃ for 6 hours, wherein the film layer has no phenomena of peeling, foaming, cracking, stripping and the like;
2) And (3) water resistance test: after the film-coated sample piece is soaked in water at 50 ℃ for 24 hours, the film layer is not broken, and adhesive tape paper with the width of 2cm and the peel strength I of more than 2.94N/cm is firmly adhered to the surface of the film layer, and after the adhesive tape paper is rapidly pulled up from the edge of a part to the vertical direction of the surface, the film layer is not fallen off and damaged;
3) Testing adhesive force; the film is tightly attached to the surface of the film by using a 3M special adhesive tape with the width of 1 inch, then is quickly pulled up along the vertical direction of the film surface, and is repeatedly pulled for 10 times, so that the film stripping phenomenon is avoided.
Comparative example 1
As shown in fig. 3, a common CO 2 The laser antireflection film comprises a substrate layer, wherein a first yttrium fluoride layer and a second zinc sulfide layer are sequentially deposited on the substrate layer, and the coverage areas of the first yttrium fluoride layer and the second zinc sulfide layer are 98% of the surface area of the substrate layer.
The physical thickness of the first yttrium fluoride layer is 967 nanometers; the second zinc sulfide layer is 308 nanometers, and the basal layer is zinc selenide basal layer with the thickness of 3 mm.
The above-mentioned common CO 2 The preparation method of the laser antireflection film comprises the following steps of:
1) Performing independent premelting treatment on yttrium fluoride and zinc sulfide membrane materials to remove impurities in the membrane materials;
2) After cleaning the substrate layer, it was placed in a vacuum chamber at a pressure of 1.8X10 -3 Under the conditions of Pa and baking temperature of 100 ℃, sequentially depositing a first yttrium fluoride layer and a second zinc sulfide layer on the surface of the basal layer; when depositing the first yttrium fluoride layer, the evaporation rate of yttrium fluoride is 0.28nm/S, and the ion source is as follows: the accelerating voltage is 250V, the screen electrode voltage is 400V, the beam current is 20A, and the layer only uses an ion source at the first 100 nm; when depositing the zinc sulfide layer, the evaporation rate of the zinc sulfide is 0.17nm/S, and an ion source is not used; the common CO is obtained 2 The transmittance of the laser antireflection film in the far infrared 10.6um wave band reaches 99.5 percent.
The films obtained in each example were subjected to the following performance tests, with reference to the standard of the environmental reliability test of the film of the army standard MILs-48497 a, and the specific results are as follows:
1) High temperature resistance test: baking the film-coated sample piece at 300 ℃ for 6 hours, cooling to normal temperature, and continuously heating to 300 ℃ for 6 hours, wherein the film layer has the phenomena of peeling, foaming, cracking, stripping and the like;
2) And (3) water resistance test: after the film-coated sample piece is soaked in water at 50 ℃ for 24 hours, the film layer is not broken, and adhesive tape paper with the width of 2cm and the peel strength I of more than 2.94N/cm is firmly adhered to the surface of the film layer, and after the adhesive tape paper is rapidly pulled up from the edge of a part to the vertical direction of the surface, the film layer is not fallen off and damaged;
3) Testing adhesive force; the film is tightly attached to the surface of the film by using a 3M special adhesive tape with the width of 1 inch, then is quickly pulled up along the vertical direction of the film surface, and is repeatedly pulled for 10 times, so that the film stripping phenomenon is avoided.

Claims (10)

1. High-temperature-resistant CO 2 A laser antireflection film is characterized in thatIn the following steps: the composite material comprises a basal layer, wherein a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer are sequentially deposited on the basal layer, and the coverage areas of the first yttrium fluoride layer, the ytterbium calcium fluoride layer, the zinc selenide layer and the second yttrium fluoride layer are more than 95% of the surface area of the basal layer.
2. The high temperature resistant CO of claim 1 2 The laser antireflection film is characterized in that: the physical thickness of the ytterbium calcium fluoride layer is greater than that of the zinc selenide layer.
3. A high temperature resistant CO according to claim 2 2 The laser antireflection film is characterized in that: the physical thickness of the first yttrium fluoride layer and the physical thickness of the second yttrium fluoride layer are both less than the physical thickness of the zinc selenide layer.
4. A high temperature CO according to claim 3 2 The laser antireflection film is characterized in that: the physical thickness of the ytterbium calcium fluoride layer is 8-9.5 times of that of the first yttrium fluoride layer, the physical thickness of the zinc selenide layer is 2-3 times of that of the first yttrium fluoride layer, and the physical thickness of the second yttrium fluoride layer is 0.95-1.05 times of that of the first yttrium fluoride layer.
5. A high temperature CO according to any one of claims 1-4 2 The laser antireflection film is characterized in that: the physical thickness of the first yttrium fluoride layer is 95-100 nanometers; the physical thickness of the ytterbium fluoride calcium layer is 860-870 nanometers; the physical thickness of the zinc selenide layer is 240-250 nanometers; the physical thickness of the second yttrium fluoride layer is 95-100 nanometers.
6. A high temperature CO according to any one of claims 1-4 2 The laser antireflection film is characterized in that: the basal layer is zinc selenide basal layer with the thickness of 3+/-0.1 mm; high temperature resistant CO 2 The transmittance of the laser antireflection film in the far infrared 10.6um wave band reaches 99.5 percent, and the temperature resistance is more than 300 ℃.
7. Weight(s)The high temperature CO of any one of claims 1 to 6 2 The preparation method of the laser antireflection film is characterized by comprising the following steps: and sequentially depositing a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer on the substrate layer in a vacuum evaporation mode.
8. The method of manufacturing according to claim 7, wherein: the method comprises the following steps of:
1) Performing independent premelting treatment on yttrium fluoride, ytterbium calcium fluoride and zinc selenide membrane materials to remove impurities in the membrane materials;
2) Cleaning the substrate layer, placing in a vacuum chamber with pressure of (1.8+ -0.2) ×10 -3 And under the conditions of Pa and baking temperature of 100+/-5 ℃, sequentially depositing a first yttrium fluoride layer, a ytterbium calcium fluoride layer, a zinc selenide layer and a second yttrium fluoride layer on the surface of the basal layer.
9. The method of manufacturing according to claim 8, wherein: in step 2), ion-assisted deposition is required during evaporation of the first yttrium fluoride layer, the ytterbium calcium fluoride layer, and the second yttrium fluoride layer.
10. The method of manufacturing according to claim 9, wherein: in the step 2), when the first yttrium fluoride layer is deposited, the evaporation rate of yttrium fluoride is 0.28+/-0.02 nm/S, and the beam current of the ion source is 20A;
when the ytterbium calcium fluoride layer is deposited, the evaporation rate of the ytterbium calcium fluoride is 0.28+/-0.02 nm/S, the beam current of the ion source is 20A, and the ion source is only used at the first 100 nm;
when depositing the zinc selenide layer, the evaporation rate of the zinc selenide is 0.17+/-0.02 nm/S, and an ion source is not used;
when the second yttrium fluoride layer is deposited, the evaporation rate of yttrium fluoride is 0.28+/-0.02 nm/S, and the ion source beam current 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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CN110004408B true CN110004408B (en) 2023-05-23

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