CN108265269B - Coating method for improving environmental stability of multilayer laser film element - Google Patents

Coating method for improving environmental stability of multilayer laser film element Download PDF

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CN108265269B
CN108265269B CN201810140020.7A CN201810140020A CN108265269B CN 108265269 B CN108265269 B CN 108265269B CN 201810140020 A CN201810140020 A CN 201810140020A CN 108265269 B CN108265269 B CN 108265269B
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electron beam
multilayer
laser
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CN108265269A (en
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朱美萍
曾婷婷
邵建达
易葵
尹超奕
许诺
孙建
李静平
王胭脂
王建国
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Shanghai Institute of Optics and Fine Mechanics of CAS
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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
    • C23C14/24—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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • 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
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/46—Sputtering by ion beam produced by an external ion source
    • 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
    • G02B1/14—Protective coatings, e.g. hard coatings

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  • Mechanical Engineering (AREA)
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  • Engineering & Computer Science (AREA)
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Abstract

A film coating method for improving the environmental stability of multi-layer laser film element features that the ion beam aided deposition technique is combined with the electron beam evaporation technique. According to the designed film system, depositing a plurality of films except the outermost layer by using an electron beam evaporation technology to obtain a high laser damage resistance threshold; and depositing the outermost layer by using an ion beam assisted deposition technology to obtain a compact water vapor barrier layer and prevent water molecules from rapidly entering and exiting the surface of the multilayer laser thin film element. The invention can improve the environmental stability of the multilayer laser film element prepared by the electron beam evaporation technology while keeping the higher laser damage resistance threshold of the element.

Description

Coating method for improving environmental stability of multilayer laser film element
Technical Field
The invention belongs to the technical field of optical films, and particularly relates to a film coating method for improving the environmental stability of a multilayer laser film element.
Background
The electron beam evaporation deposition technology is widely applied to the preparation of laser thin film elements because of the easy acquisition of a high laser damage threshold and the easy expansion of the electron beam evaporation deposition technology for preparing large-size thin film elements. However, the performance change of the large-caliber laser thin-film component prepared by the electron beam deposition technology under different environments, such as the change of spectral performance and transmission wave surface quality, is one of the main reasons influencing the stable operation of the laser system. For example: the problems of spectral shift and the like of thin film elements caused by moisture absorption due to the change of environmental humidity are encountered in the operation process of large high-power laser devices such as national super-luminescent devices (GSP) and National Ignition (NIF). This is because the influence of the use environment of the thin film element on the performance of the thin film element is mainly that the thin film prepared by electron beam evaporation has a porous structure and is likely to interact with polar molecules such as water vapor in the environment. Therefore, reducing the porosity of the thin film element can suppress the environmental influence to some extent. At present, an ion beam assisted deposition technology or an ion beam sputtering deposition technology is often adopted to prepare an optical thin film element with higher density, the prepared thin film element has higher environmental stability but higher stress, and for a thicker optical thin film element, film cracking is easily caused to further cause failure of the thin film element; and the laser damage resistance threshold of the film element is generally lower than that of a film element prepared by an electron beam evaporation technology.
Disclosure of Invention
The present invention provides a coating method for improving environmental stability of a multilayer laser thin film element, which can maintain a high laser damage threshold performance of an optical thin film element prepared by an electron beam evaporation technique, control the stress within a small range, and improve the environmental stability of the laser thin film element.
The technical solution of the invention is as follows:
a coating method for improving the environmental stability of a multilayer laser film element is characterized in that the essence of the method is that on the basis of preparing a multilayer film by adopting an electron beam deposition technology to obtain a high laser damage resistance threshold, the outermost layer of a film system is prepared by adopting an ion beam assisted deposition technology to obtain a high-density moisture barrier film layer, and the method comprises the following steps:
1) designing a membrane system:
designing the film system according to the required optical performance requirement: s | MN | A, wherein S represents a substrate, M represents a multilayer film, A represents air, N represents a dense outermost protective layer which prevents water molecules from rapidly entering and exiting the surface of the multilayer laser thin film element, and the thickness of N:
Figure BDA0001577334830000021
(for high-reflective films, Z-1, 2,3 …),
wherein λ is the design wavelength of the multilayer film system; n is the refractive index of the medium, here the refractive index of the dense protective layer prepared by ion beam assisted deposition technology; θ is the angle of incidence of the light;
2) substrate cleaning: cleaning and airing the substrate;
3) preparing a film:
⑴ according to the designed film system, the multilayer film M is deposited by electron beam evaporation technique by heating the substrate to 120-250 deg.C, and when the vacuum degree is better than 9.0 × 10-4When Pa, opening an electron gun, and preparing a high-refractive-index film layer and a low-refractive-index film layer by adopting an electron beam evaporation technology according to the designed film system sequence;
⑵ plating a dense protective layer on the outermost layer by ion beam assisted deposition technology:
after the deposition of the multilayer film M is finished, the plasma source is opened, the plasma bias voltage is set to be 100V-200V, the N layer is plated, and the plasma source and the electron gun are closed after the film layer is plated;
⑶ and finishing the coating.
The substrate is optical glass or crystal.
The invention has the technical effects that:
1. the invention adopts electron beam evaporation technology and ion beam assisted deposition technology to prepare multilayer film: the outermost layer is prepared by adopting an ion beam assisted deposition technology to obtain a compact film layer; the remaining layers are electron beam deposited to achieve a high laser damage threshold.
2. The invention can solve the problem of environmental instability of the film element prepared by the electron beam evaporation technology due to the porous characteristic of the film element, namely moisture absorption and desorption, and adopts the ion-assisted deposition technology to deposit the outermost protective layer of the film system on the basis of the electron beam evaporation technology to obtain the high-density plated moisture barrier layer and prevent water molecules from rapidly entering and exiting the surface of the multilayer laser film element, thereby improving the environmental stability of the laser film element.
3. The method is simple and easy to implement, and has the characteristics of strong pertinence and high efficiency. Is very suitable for preparing laser film elements with high requirements on environmental stability.
Drawings
FIG. 1 is a schematic view of a film system of a multilayer high-reflective film prepared by a conventional electron beam evaporation technique and a multilayer high-reflective film prepared by the method of the present invention, respectively, wherein a is prepared by a conventional electron beam evaporation technique and b is prepared by the method of the present invention.
FIG. 2 is a graph of spectral environmental stability of a multilayer highly reflective film prepared by a conventional electron beam evaporation technique and a multilayer highly reflective film prepared by the method of the present invention, respectively, wherein a is prepared by a conventional electron beam evaporation technique and b is prepared by the method of the present invention.
Detailed Description
The invention is further illustrated by the following examples and figures.
Referring to FIG. 1, FIG. 1 is a schematic diagram of a film system of a multi-layer high-reflective film prepared by conventional electron beam evaporation and by the method of the present invention, in which the high-refractive index material is HfO2The low refractive index material is SiO2The film system is designed into a multi-layer high-reflection film with S | M B | A, S | M N | A as an example, and the invention is used for describing the film coating technology for improving the environmental stability of a multi-layer laser film element, wherein M ═ 4L (HL)12H, B ═ N ═ 4L, the technique includes the following steps:
1) designing a membrane system:
according to the spectral performance requirements: 0 DEG R is more than or equal to 99.5% @1064nm, and the designed film system is as follows: s |4L (HL)12H4L | A, wherein L represents a low refractive index material SiO2H represents a high refractive index material HfO2The 4L layer is a protective layer;
2) substrate cleaning: cleaning and airing the substrate;
3) preparing a film:
⑴ conventional electron beam evaporation technique:
① according to the designed film system, the film layer except the outermost protective layer is deposited by electron beam evaporation technology:
heating the substrate to 200 ℃; when the vacuum degree is better than 9.0 multiplied by 10-4And when Pa is needed, opening the electron gun, and preparing the high-refractive-index film layer M and the low-refractive-index film layer M by adopting an electron beam evaporation technology according to the designed film system sequence. If the layer is HfO2Layer of oxygen partial pressure of 2X 10- 2Pa, deposition rate of 0.2 nm/s; if the layer is SiO2Layer, oxygen partial pressure 5.0X 10-3Pa, deposition rate of 0.4 nm/s.
② depositing the outermost protective layer by electron beam evaporation:
multilayer film M ═ 4L (HL)12And after H is deposited, continuing to deposit the protective layer N-4L by adopting an electron beam evaporation technology. In this case the layer is SiO2Layer of oxygen partial pressure of 1.5X 10-2Pa, deposition rate of 0.4 nm/s. And closing the electron gun after the film layer is plated.
③ and finishing the coating.
⑵ the method comprises preparing the outermost layer by ion beam assisted deposition to obtain a dense film, and preparing the other layers by electron beam deposition to obtain high laser damage threshold:
① according to the designed film system, the film layer except the outermost protective layer is deposited by electron beam evaporation technology:
heating the substrate to 200 ℃; when the vacuum degree is better than 9.0 multiplied by 10-4And when Pa is needed, opening the electron gun, and preparing the high-refractive-index film layer M and the low-refractive-index film layer M by adopting an electron beam evaporation technology according to the designed film system sequence. If the layer is HfO2Layer of oxygen partial pressure of 2X 10- 2Pa, deposition rate of 0.2 nm/s; if the layer is SiO2Layer, oxygen partial pressure 5.0X 10-3Pa, deposition rate of 0.4 nm/s.
② deposition of the outermost protective layer using an ion beam assisted deposition process:
multilayer film M ═ 4L (HL)12After H deposition is finished, turning on the plasma source to bias the plasmaThe pressure was set at 150V, APS was fixed oxygenated at 5sccm, and deposition of protective layer N was started at 4L. In this case the layer is SiO2Layer, deposition rate 0.4 nm/s. After the film is plated, the plasma source and the electron gun are turned off.
③ and finishing the coating.
4) The transmission spectra of the high-reflection film prepared by the conventional electron beam evaporation technology and the high-reflection film prepared by the method are respectively measured by a spectrometer along with the change of the use environment (under the isothermal condition, the higher the vacuum degree is, the lower the relative humidity is):
① spectral measurement in atmospheric environment, the high reflection film prepared by conventional electron beam evaporation technology and the method of the invention is respectively placed in a vacuum device for spectral transmittance measurement, at this time, the vacuum device is not vacuumized, the pressure, the environmental temperature and the humidity are consistent with the atmospheric environment, the test angle is 0 degree, and the test range is 300nm-1400 nm.
② Spectrum measurement in vacuum environment is carried out by putting high reflective films prepared by conventional electron beam evaporation and method in vacuum device, connecting with coating apparatus, and vacuumizing until vacuum degree is better than 3.0 × 10-4Pa (vacuum environment a), evacuation was stopped and the spectral transmittance measurement was immediately performed. In order to verify that the high-reflection film prepared by the method has higher environmental stability, the high-reflection film is further subjected to a vacuum-pumping experiment, and when the vacuum degree is superior to 1.0 multiplied by 10-5The spectral change was measured immediately Pa (vacuum environment B). Testing and testing angles: 0 degree, and the testing range is 300nm-1400 nm. Fig. 2 is a graph of spectral environmental stability of a highly reflective film.
Multiple experiments show that: the outermost layer of the method is prepared by adopting an ion beam assisted deposition technology to obtain a compact film layer and prevent water molecules from rapidly entering and exiting the surface of the multilayer laser film element; the remaining layers are electron beam deposited to achieve a high laser damage threshold. On the premise of not increasing the difficulty of film system design and film coating process, the problems of unstable optical performance and the like of a porous film prepared by an electron beam evaporation technology due to moisture absorption and desorption can be effectively solved, and thus the environmental stability of a multilayer film element is improved.

Claims (2)

1. A coating method for improving the environmental stability of a multilayer laser film element is characterized in that the essence of the method is that on the basis of preparing a multilayer film by adopting an electron beam deposition technology to obtain a high laser damage resistance threshold, the outermost layer of a film system is prepared by adopting an ion beam assisted deposition technology to obtain a high-density moisture barrier film layer, and the method comprises the following steps:
1) designing a membrane system:
designing the film system according to the required optical performance requirement: s | MN | A, where S denotes a substrate, M denotes a multilayer film, A denotes air, and N denotes a dense outermost protective layer, i.e., SiO2Layer, preventing water molecules from rapidly entering and exiting the surface of the multilayer laser thin film element, thickness of N:
Figure FDA0002383421620000011
wherein λ is the design wavelength of the multilayer film system; n is the refractive index of the medium, here the refractive index of the dense protective layer prepared by ion beam assisted deposition technology; θ is the angle of incidence of the light;
2) substrate cleaning: cleaning and airing the substrate;
3) preparing a film:
⑴ according to the designed film system, the multilayer film M is deposited by electron beam evaporation technique by heating the substrate to 120-250 deg.C, and when the vacuum degree is better than 9.0 × 10-4When Pa, opening an electron gun, and preparing a high-refractive-index film layer and a low-refractive-index film layer by adopting an electron beam evaporation technology according to the designed film system sequence;
⑵ plating a dense protective layer on the outermost layer by ion beam assisted deposition technology:
after the deposition of the multilayer film M is finished, the plasma source is opened, the plasma bias voltage is set to be 100V-200V, the N layer is plated, and the plasma source and the electron gun are closed after the film layer is plated;
⑶ and finishing the coating.
2. The method according to claim 1, wherein the substrate is an optical glass or a crystal.
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CN110079778B (en) * 2019-05-06 2021-07-06 成都精密光学工程研究中心 Low defect optical film and method of making same
CN110441844A (en) * 2019-06-24 2019-11-12 东莞理工学院 10 kW semiconductor laser high-reflecting films of one kind and preparation method thereof
CN111286700B (en) * 2020-03-18 2020-10-16 中国科学院上海光学精密机械研究所 Surface shape compensation method of optical coating element based on mixture single-layer film
CN111378934B (en) * 2020-03-30 2021-03-30 中国科学院上海光学精密机械研究所 Coating method for improving spectrum and stress aging stability of electron beam evaporation film element
CN111575657B (en) * 2020-04-23 2022-04-05 中国科学院上海光学精密机械研究所 Method for solving cracking of electron beam deposition film based on ion beam assisted nano lamination
CN112379472B (en) * 2020-11-13 2022-08-16 上海卫星装备研究所 Optical solar reflecting mirror with low radiation absorption ratio and preparation method thereof

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