CN113341487A - ZnSe substrate 10.3-10.9 mu m high-strength antireflection film and plating method - Google Patents

ZnSe substrate 10.3-10.9 mu m high-strength antireflection film and plating method Download PDF

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Publication number
CN113341487A
CN113341487A CN202110617201.6A CN202110617201A CN113341487A CN 113341487 A CN113341487 A CN 113341487A CN 202110617201 A CN202110617201 A CN 202110617201A CN 113341487 A CN113341487 A CN 113341487A
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layer
thickness
znse substrate
film
antireflection film
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Inventor
张勇
张涛
郭浩宇
陈俊霞
王苗苗
苏颖
张恒华
张成群
白涛
张金豹
耿浩
张树盛
杨资阳
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Henan Pingyuan Optical & Electronic Co ltd
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Henan Pingyuan Optical & Electronic Co ltd
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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
    • C23C14/0694—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
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Physical Vapour Deposition (AREA)
  • Surface Treatment Of Optical Elements (AREA)

Abstract

The invention relates to the technical field of infrared optical coating, and provides a high-strength antireflection film with a ZnSe substrate of 10.3-10.9 mu m, wherein the structure of the film system is G/100L1010H901L10H933L 10H/A; the application also provides a plating method of the ZnSe substrate with the high strength and the antireflection film of 10.3-10.9 mu m, which adopts the high energy assistance of an APS ion source and the substrate heating film plating mode. The beneficial effect of this application does: after the high-strength antireflection film is plated on two sides of the ZnSe substrate, the average transmittance of 10.3-10.9 μm reaches more than 99%; and meets the requirements of abrasion resistance strength, constant damp and hot, low temperature and salt spray environment tests in the JB/T8226.1-1999 optical part coating standard.

Description

ZnSe substrate 10.3-10.9 mu m high-strength antireflection film and plating method
Technical Field
The invention relates to the technical field of infrared optical coating, in particular to a high-strength antireflection film with a ZnSe substrate of 10.3-10.9 mu m, and also relates to a coating method of the high-strength antireflection film with the ZnSe substrate of 10.3-10.9 mu m.
Background
With the development of military infrared technology, the application of infrared optical systems is increasing, and the requirements of optical elements indispensable to infrared systems, such as front windows or cowlings in airborne, shipboard and tank infrared imaging systems, are also greatly increased. The zinc selenide material is a yellow transparent polycrystalline material, the size of crystal particles is about 70 mu m, the light transmission range is 0.5-15 mu m, and the scattering loss is extremely low after impurity absorption. Because of the small absorption of 10.6 μm wavelength light, it is the preferred material for making optical devices in high power laser systems. And is also a commonly used material in different optical systems throughout its light transmission band. The zinc selenide material has high thermal shock resistance, so that the zinc selenide material becomes an optimal optical material in a high-power laser system and is widely applied to the fields of laser, medicine, astronomy, infrared night vision and the like. The zinc selenide material has larger refractive index, and the material is softer and is easy to scratch. Therefore, a high-strength antireflection film needs to be plated on the surface of the substrate to obtain high transmittance and protect the substrate to some extent.
Disclosure of Invention
The invention aims to provide a ZnSe substrate 10.3-10.9 μm high-strength antireflection film to solve the problems proposed in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a high-strength antireflection film with a ZnSe substrate of 10.3-10.9 μm is prepared by plating a front film system on the front surface of the ZnSe substrate and plating a back film system identical to the front film system on the back surface of the ZnSe substrate, wherein the front film system has the following structure:
G/100L1010H901L10H933L10H/A；
the reverse side film system structure is as follows:
G/100L1010H901L10H933L10H/A；
wherein: g: ZnSe; h: ZnS; l: YbF 3; a: air;
the number before the film layer is the physical thickness of the film layer in nm.
This application adds the thin layer ZnS isolation layer, with thick layer YbF3Separated into relatively thin two layers to reduce YbF3The layer creates a problem of film cracking due to thickness. YbF by first layer plating3And the problem of film layer mismatch caused by the reaction of ZnS and ZnSe is prevented.
The invention also provides a plating method of the high-strength antireflection film with the thickness of 10.3-10.9 mu m of the ZnSe substrate, which is used for preparing the high-strength antireflection film with the thickness of 10.3-10.9 mu m of the ZnSe substrate, and a YbF3 layer with the thickness of 100nm, a ZnS layer with the thickness of 1010nm, a YbF3 layer with the thickness of 901nm, a ZnS layer with the thickness of 10nm, a YbF3 layer with the thickness of 933nm and a ZnS layer with the thickness of 10nm are sequentially plated on the ZnSe substrate by adopting an APS ion source high-energy assistance and substrate heating film plating mode.
Preferably, the APS ion source assist energy control parameters are: the deflection voltage VB 100-120 v, the discharge current ID 45-55 mA, the temperature is controlled to be 18-26 ℃, the relative humidity is 30-70%, and the cleanliness is ten thousand. The APS ion source is adopted to assist in film coating, so that the compactness, firmness and abrasion resistance of the film layer can be improved. The auxiliary energy is controlled as follows: the deflection voltage VB (v) is 100-120, and the discharge current ID (mA) is 45-55. The film layer is easily damaged due to excessive energy. If the energy is too small, the auxiliary effect is reduced, and the due effect cannot be achieved.
The environmental requirements are as follows: changes of ambient temperature and humidity can cause changes of ZnSe substrate, and poor cleanliness can cause the surface defect grade of parts to be reduced.
Preferably, the substrate heating temperature is 150 ℃. The film obtained by plating at the temperature has relatively good strength and stability, improves the stress characteristic of the plated film layer, and reduces the problems of film cracking, film stripping and the like.
Preferably, the evaporation rate of ZnS is controlled to be between 0.6 and 0.8nm/s during the plating process, and YbF3The evaporation rate is controlled between 0.3nm/s and 0.5 nm/s. The evaporation rate can improve the compactness of the film layer and reduce defects. The problems of too low speed, easy incompact film layer, too high speed and easy defect generation are avoided.
The beneficial effect of this application does: after the high-strength antireflection film is plated on two sides of the ZnSe substrate, the average transmittance of 10.3-10.9 μm reaches more than 99%; and meets the requirements of abrasion resistance strength, constant damp and hot, low temperature and salt spray environment tests in the JB/T8226.1-1999 optical part coating standard.
The application solves the design problem of the high-strength antireflection film with the zinc selenide substrate in the prior art, and solves the problems of poor coating firmness, poor compactness and insufficient strength of the film layer.
The ZnSe substrate high-strength antireflection film with the thickness of 10.3-10.9 mu m and the plating method thereof can be widely applied to processing of infrared optical instruments, and products can be used for aerospace, aviation, laser beam-driving guidance systems, infrared product optical systems and the like.
Drawings
FIG. 1 is a single-side film structure diagram of a ZnSe substrate of the invention with a thickness of 10.3-10.9 μm.
FIG. 2 is a graph of the transmittance spectrum of a high-strength antireflection film of 10.3-10.9 μm on a ZnSe substrate plated according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following description of embodiments thereof, which is provided for helping those skilled in the art to more fully, accurately and deeply understand the concept and technical scheme of the present invention and to facilitate the implementation thereof.
A high-strength antireflection film with 10.3-10.9 μm of ZnSe substrate, wherein a front film system is plated on the front surface of the ZnSe substrate, and a back film system which is the same as the front film system is plated on the back surface of the ZnSe substrate, and the front film system has the structure shown in FIG. 1:
G/100L1010H901L10H933L10H/A；
the structure of the reverse side film system is shown in figure 1:
G/100L1010H901L10H933L10H/A；
wherein: g: ZnSe; h: ZnS; l: YbF 3; a: air;
the number before the film layer is the physical thickness of the film layer in nm.
A plating method of a ZnSe substrate with 10.3-10.9 μm high-strength antireflection film comprises the following steps: design and optimization of a film system → cleaning → ion beam cleaning → film coating → inspection of various technical requirements of parts → transfer to the next process.
In the coating process, YbF with the thickness of 100nm is sequentially coated on a ZnSe substrate by adopting an APS ion source high-energy auxiliary and substrate heating coating mode3Layer, ZnS layer of 1010nm thickness, YbF of 901nm thickness3Layer, ZnS layer of thickness 10nm, YbF of thickness 933nm3Layer, ZnS layer of 10nm thickness.
The APS ion source assist energy control parameters are: the deflection voltage VB 100-120 v, the discharge current ID 45-55 mA, the temperature is controlled to be 18-26 ℃, the relative humidity is 30-70%, and the cleanliness is ten thousand.
The substrate heating temperature was 150 ℃. In the plating process, the ZnS evaporation rate is controlled to be between 0.6 and 0.8nm/s, and YbF3The evaporation rate is controlled between 0.3nm/s and 0.5 nm/s.
The spectral law of the transmittance of the high-strength antireflection film with the thickness of 10.3-10.9 mu m on the ZnSe substrate plated by the application is shown in FIG. 2.
Example 1
Selecting a plane ZnSe substrate material with a certain specification, coating the substrate within the range of 10.3-10.9 mu m of wave band, and bombarding and cleaning the ZnSe substrate by adopting an APS ion source; at 150 ℃, adopting APS ion source to assist the deposition mode on ZnSeA YbF3 layer with the thickness of 100nm, a ZnS layer with the thickness of 1010nm and a YbF layer with the thickness of 901nm are plated on the substrate in sequence3Layer, ZnS layer of thickness 10nm, YbF of thickness 933nm3Layer, ZnS layer of 10nm thickness. The control parameters of the APS ion source are a deflection voltage VB 100-120 v and a discharge current ID 45-55 mA, the temperature is controlled to be 18-26 ℃, the relative humidity is 30-70%, and the cleanliness is ten thousand. The ZnS evaporation rate is controlled between 0.6nm/s, YbF3The evaporation rate is controlled between 0.3nm/s to obtain the high-strength antireflection film with the thickness of 10.3-10.9 mu m of the ZnSe substrate.
The transmittance of the obtained high-strength antireflection film with the ZnSe substrate of 10.3-10.9 μm is measured, and the average transmittance of the antireflection film is 99.50%.
Example 2
Selecting a plane ZnSe substrate material with a certain specification, coating the substrate within the range of 10.3-10.9 mu m of wave band, and bombarding and cleaning the ZnSe substrate by adopting an APS ion source; sequentially plating YbF with the thickness of 100nm on a ZnSe substrate by adopting an APS ion source assisted deposition mode at the temperature of 150 DEG C3Layer, ZnS layer of 1010nm thickness, YbF of 901nm thickness3Layer, ZnS layer of thickness 10nm, YbF of thickness 933nm3Layer, ZnS layer of 10nm thickness. The control parameters of the APS ion source are a deflection voltage VB 100-120 v and a discharge current ID 45-55 mA, the temperature is controlled to be 18-26 ℃, the relative humidity is 30-70%, and the cleanliness is ten thousand. The ZnS evaporation rate is controlled between 0.8nm/s, YbF3The evaporation rate is controlled between 0.5nm/s, and the high-strength antireflection film with the thickness of 10.3-10.9 mu m of the ZnSe substrate is obtained.
The transmittance of the obtained high-strength antireflection film with the ZnSe substrate of 10.3-10.9 μm is measured, and the average transmittance of the antireflection film is 99.70%.
Example 3
Selecting a plane ZnSe substrate material with a certain specification, coating the substrate within the range of 10.3-10.9 mu m of wave band, and bombarding and cleaning the ZnSe substrate by adopting an APS ion source; sequentially plating YbF with the thickness of 100nm on a ZnSe substrate by adopting an APS ion source assisted deposition mode at the temperature of 150 DEG C3Layer, ZnS layer of 1010nm thickness, YbF of 901nm thickness3Layer, ZnS layer of thickness 10nm, YbF3 of thickness 933nmLayer, ZnS layer of 10nm thickness. The control parameters of the APS ion source are a deflection voltage VB 100-120 v and a discharge current ID 45-55 mA, the temperature is controlled to be 18-26 ℃, the relative humidity is 30-70%, and the cleanliness is ten thousand. The ZnS evaporation rate is controlled between 0.7nm/s, YbF3The evaporation rate is controlled between 0.4nm/s, and the high-strength antireflection film with the thickness of 10.3-10.9 mu m of the ZnSe substrate is obtained.
The transmittance of the obtained high-strength antireflection film with the ZnSe substrate of 10.3-10.9 μm is measured, and the average transmittance of the antireflection film is 99.60%.
The invention is described above with reference to the accompanying drawings as an example, in so far as it is a insubstantial improvement in the method concept and technical solutions of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.

Claims (5)

1. A high-strength antireflection film with a ZnSe substrate of 10.3-10.9 μm is prepared by plating a front film system on the front surface of the ZnSe substrate and plating a back film system identical to the front film system on the back surface of the ZnSe substrate, and is characterized in that: the front film system structure is as follows:
G/100L1010H901L10H933L10H/A；
the reverse side film system structure is as follows:
G/100L1010H901L10H933L10H/A；
wherein: g: ZnSe; h: ZnS; l: YbF3(ii) a A: air;
the number before the film layer is the physical thickness of the film layer in nm.
2. A plating method of a ZnSe substrate 10.3 to 10.9 μm high-strength antireflection film for producing a ZnSe substrate 10.3 to 10.9 μm high-strength antireflection film as set forth in claim 1, characterized in that: sequentially plating YbF with the thickness of 100nm on a ZnSe substrate by adopting the high-energy assistance of an APS ion source and the substrate heating film plating mode3Layer, ZnS layer of 1010nm thickness, YbF of 901nm thickness3Layer, ZnS layer of thickness 10nm, YbF of thickness 933nm3Layer, ZnS layer of 10nm thickness.
3. The method for plating a high-strength antireflection film of ZnSe substrate 10.3 to 10.9 μm as set forth in claim 2, wherein: the APS ion source assist energy control parameters are: the deflection voltage VB 100-120 v, the discharge current ID 45-55 mA, the temperature is controlled to be 18-26 ℃, the relative humidity is 30-70%, and the cleanliness is ten thousand.
4. The method for plating a ZnSe substrate 10.3 to 10.9 μm high strength antireflection film according to claim 3, wherein: the substrate heating temperature was 150 ℃.
5. The method for plating a ZnSe substrate 10.3 to 10.9 μm high strength antireflection film according to claim 4, wherein: in the plating process, the ZnS evaporation rate is controlled to be between 0.6 and 0.8nm/s, and YbF3The evaporation rate is controlled between 0.3nm/s and 0.5 nm/s.
CN202110617201.6A 2021-06-03 2021-06-03 ZnSe substrate 10.3-10.9 mu m high-strength antireflection film and plating method Pending CN113341487A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114019591A (en) * 2021-09-23 2022-02-08 有研国晶辉新材料有限公司 Optical element comprising anti-reflection protective film and preparation method thereof
CN115494565A (en) * 2022-09-15 2022-12-20 安徽光智科技有限公司 Infrared antireflection film for protecting laser, preparation method and application

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105607159A (en) * 2016-01-12 2016-05-25 西南技术物理研究所 Preparation method for large-angle multiband infrared high antireflection film system
CN109696716A (en) * 2019-01-15 2019-04-30 西安应用光学研究所 A kind of film structure of ultra-wide multi-angle laser, the high-strength antireflective coating of LONG WAVE INFRARED two waveband
CN111090134A (en) * 2019-11-21 2020-05-01 天津津航技术物理研究所 Chalcogenide glass substrate laser, medium-wave infrared and long-wave infrared composite antireflection film
CN112505803A (en) * 2020-12-08 2021-03-16 云南北方驰宏光电有限公司 ZnSe substrate 7.7-9.5 mu m waveband high-durability antireflection film and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105607159A (en) * 2016-01-12 2016-05-25 西南技术物理研究所 Preparation method for large-angle multiband infrared high antireflection film system
CN109696716A (en) * 2019-01-15 2019-04-30 西安应用光学研究所 A kind of film structure of ultra-wide multi-angle laser, the high-strength antireflective coating of LONG WAVE INFRARED two waveband
CN111090134A (en) * 2019-11-21 2020-05-01 天津津航技术物理研究所 Chalcogenide glass substrate laser, medium-wave infrared and long-wave infrared composite antireflection film
CN112505803A (en) * 2020-12-08 2021-03-16 云南北方驰宏光电有限公司 ZnSe substrate 7.7-9.5 mu m waveband high-durability antireflection film and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114019591A (en) * 2021-09-23 2022-02-08 有研国晶辉新材料有限公司 Optical element comprising anti-reflection protective film and preparation method thereof
CN114019591B (en) * 2021-09-23 2023-08-01 有研国晶辉新材料有限公司 Optical element comprising anti-reflection protective film and preparation method thereof
CN115494565A (en) * 2022-09-15 2022-12-20 安徽光智科技有限公司 Infrared antireflection film for protecting laser, preparation method and application
CN115494565B (en) * 2022-09-15 2023-05-05 安徽光智科技有限公司 Laser-protected infrared antireflection film, preparation method and application

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