CN111041413A - Method for improving surface shape precision of large-aperture reflector coating film - Google Patents

Method for improving surface shape precision of large-aperture reflector coating film Download PDF

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CN111041413A
CN111041413A CN201911268270.XA CN201911268270A CN111041413A CN 111041413 A CN111041413 A CN 111041413A CN 201911268270 A CN201911268270 A CN 201911268270A CN 111041413 A CN111041413 A CN 111041413A
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substrate
coated
refractive
coating
film layer
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CN111041413B (en
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潘峰
王健
刘民才
吴倩
罗晋
唐明
王震
张飞
张清华
卫耀伟
李树刚
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Laser Fusion Research Center China Academy of Engineering Physics
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10Glass or silica
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process
    • C23C14/548Controlling the composition
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements

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Abstract

The invention discloses a method for improving the precision of the surface shape of a large-aperture reflector coating film, which adopts a comprehensive control method of the surface shape of a substrate and a film layer with high and low refractive indexes in the coating process: aiming at the deformation of the substrate in the film coating process before film coating, the change of the surface shape of the substrate caused by heating in the film coating process is controlled and offset by adopting a substrate pre-turnover annealing method; the residual stress of the film layers in the reflector is controlled by adopting a method of adjusting oxygen charging amount and ion-assisted deposition, so that the residual stress of each film layer is basically close to zero stress. The invention discloses a method for improving the surface shape precision of a large-aperture reflector coating film, which has the advantages of high surface shape precision, simplicity, practicability, wide application range and suitability for reflector surface shape control of different film layers and substrate combinations.

Description

Method for improving surface shape precision of large-aperture reflector coating film
Technical Field
The invention relates to the technical field of thin film optics, in particular to a method for improving the surface shape accuracy of a large-aperture reflector coating film.
Background
The large-aperture laser reflector is one of the key optical elements of various large-scale laser devices, and the surface shape precision of the reflector is one of the key factors influencing the quality of laser transmission beams. Electron beam evaporation is a common method for preparing a large-aperture reflector coating film at present, and has the advantages of low cost, good uniformity of a large-aperture film layer and high laser damage resistance threshold. The electron beam evaporation mode is to deposit a high refractive index film layer and a low refractive index film layer on a substrate to be coated alternately according to a set thickness to form a reflector.
One of the key difficulties in coating a film on a large-aperture reflector film layer is the control of the shape of the mirror surface, and in the existing research, aiming at the fact that the control of the surface shape is more the influence rule of the research process factors on the residual stress of the film layer, the commonly used reflector surface shape control technology is usually adopted to adjust the residual stress of the film layer (such as silicon oxide) by changing the oxygen charging amount in the coating process, so that the residual stress is matched and offset with the residual stress of the high-refractive-index film layer, and the purpose of improving the surface shape precision is. Obviously, the existing reflector surface shape improving technology does not consider the substrate deformation in the coating process of the large-aperture reflector, only considers the reflector surface shape deformation factor caused by the residual stress of a single film layer, and has limited surface shape control precision improving effect; and the high-low refractive index film stress counteracting method is adopted, the thickness of each film is limited to a certain extent, the surface shape regulation range is limited, and the requirement of high-precision surface shape regulation of the large-caliber reflector cannot be met.
Therefore, how to provide a method for improving the accuracy of the coating surface shape of the large-aperture reflector is a problem that needs to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for improving the surface shape accuracy of a large-aperture reflector, which adopts a method of combining a substrate annealing process and film stress active regulation and control to greatly reduce the surface shape change in the film coating process of the large-aperture reflector, thereby improving the surface shape accuracy of the large-aperture reflector.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for improving the accuracy of the surface shape of a coating film of a large-aperture reflector comprises the following steps:
s1, before film coating, placing the substrate to be coated on a film coating station of an electron beam evaporation film coating machine, keeping the film coating surface of the substrate to be coated upward, and simultaneously, positioning the film coating station in a vacuum chamber, and vacuumizing the vacuum chamber;
s2, heating the substrate to be coated to a coating temperature through a heating module of the electron beam evaporation coating machine, then carrying out annealing treatment, and taking down the substrate after cooling to a natural temperature;
s3, placing a high-refraction material and a low-refraction material in the electron beam evaporation coating machine;
s4, cleaning the substrate to be coated;
s5, placing the film-coated surface of the substrate to be film-coated on a film-coating station of the electron beam evaporation film-coating machine downwards, and vacuumizing the substrate to be film-coated again through a vacuum chamber of the electron beam evaporation film-coating machine;
s6, heating the substrate to be coated to the coating temperature again through a heating module of the electron beam evaporation coating machine, and carrying out heat preservation treatment;
s7, depositing the low-refractive-index material on the substrate to be coated by a first electron gun on the electron beam evaporation coating machine to form a low-refractive-index film layer on the substrate to be coated, simultaneously spraying oxygen on the low-refractive-index film layer by an oxygen spraying mechanism on the electron beam evaporation coating machine, and simultaneously bombarding the low-refractive-index film layer by an auxiliary ion source;
s8, depositing the high-refractive-index material on the low-refractive-index film layer in the step 5 through a second electron gun of the electron beam evaporation coating machine to form a high-refractive-index film layer on the low-refractive-index film layer, simultaneously spraying oxygen on the high-refractive-index film layer through an oxygen spraying mechanism on the electron beam evaporation coating machine, and simultaneously bombarding the high-refractive-index film layer through an auxiliary ion source;
s9, sequentially circulating the steps S7 and S8 to enable the low-refractive-index film layer and the high-refractive-index film layer to be formed on the substrate to be coated at intervals until the coating is finished to form a reflector;
and S10, cooling the reflector formed after the film coating is finished to room temperature, and taking out the reflector to obtain a large-aperture reflector sample.
Before film coating, the film coating surface of a substrate to be coated is upwards placed on a film coating station of an electron beam evaporation film coating machine so as to heat and anneal the substrate to be coated with the upward film coating surface, thereby compensating the deformation quantity of the substrate to be coated in the film coating process in the subsequent steps so as to offset the heated deformation of the substrate in the state that the film coating surface is downwards in the film coating process from S6 to S10, and effectively controlling the surface shape of a reflector substrate The residual stress of each film layer of the reflector is basically close to zero stress. Obviously, the invention adopts the method of pre-turning and annealing the substrate to be coated to control and offset the surface shape change caused by the heating of the substrate in the coating process and combines the methods of adjusting the oxygen charging amount and ion auxiliary deposition to control the residual stress of the film layer in the reflector, thereby improving the surface shape precision of the large-caliber reflector.
Preferably, the vacuum degree of the vacuum chamber in the step S1 reaches 1 × 10-3Pa or less, the background vacuum degree of the vacuum chamber in the step S5 reaches 1 × 10-4Pa or less.
Preferably, the plating temperature in each of the step S2 and the step S6 is 80 to 200 ℃.
The coating temperature in the step S2 is determined according to the coating temperature in the step S6, so that the coating temperatures in the step S2 and the step S6 are ensured to be the same, and the thermal deformation of the substrate can be effectively counteracted. The coating temperature of 80-200 ℃ is based on the requirements of reducing the optical loss and absorption of the film, improving the adhesive force and density of the film and the like, and the proper coating temperature in the temperature range is selected.
Preferably, in the annealing process of step S2, the substrate to be coated is kept at the coating temperature of 140-150 minutes, the heat preservation time in step S6 is 50-60 minutes, and the heat preservation temperature is 80-200 ℃.
The invention can counteract the thermal deformation of the substrate in the coating process from S6 to S10 in the state that the coating surface of the substrate faces downwards to the greatest extent by controlling the time of keeping the coating temperature of the substrate to be coated in the annealing process to be 140-150 minutes, the heat preservation time in the step S6 to be 50-60 minutes and the heat preservation temperature to be 80-200 ℃, thereby further improving the shape accuracy of the large-caliber reflecting mirror surface.
Preferably, in step S7, an ion-assisted electron beam evaporation method is adopted to deposit the low refractive index material onto the substrate to be coated by the first electron gun of the electron beam evaporation coater, so as to form a low refractive index film layer on the substrate to be coated.
Preferably, in the step S7, when the first electron gun is controlled to deposit the low refractive index film, the flow rate of the oxygen gas is controlled to be 10-30sccm, the ion auxiliary voltage of the auxiliary ion source is controlled to be 300-800V, and the ion auxiliary current is controlled to be 300-1000 mA, so that the residual stress of the low refractive index film is less than 10 MPa.
The flow rate of the oxygen gas charged in the step S7 is controlled to be 10-30sccm, the ion auxiliary voltage is 300-800V, and the ion auxiliary current is 300-1000 mA, so that the residual stress of the low-refractive-index film layer in the reflecting mirror to be coated is controlled while the loss absorption of the film layer is reduced by adjusting the oxygen charging amount and by an ion auxiliary deposition method, and the residual stress of each film layer is basically close to zero stress.
Preferably, in step S8, an ion-assisted electron beam evaporation method is adopted to deposit the high refractive index material on the low refractive index film layer by the second electron gun of the electron beam evaporation coater, so that the high refractive index film layer is formed on the low refractive index film layer.
Preferably, when the second electron gun is controlled to deposit the high refractive index film in step S8, the flow rate of the oxygen gas is controlled to be 50-200sccm, the ion auxiliary voltage of the auxiliary ion source is controlled to be 300-1000V, and the ion auxiliary current is controlled to be 300-1500 mA, so that the residual stress of the high refractive index film is less than 10 MPa.
The oxygen flow in the step S8 is controlled to be 50-200sccm, the ion auxiliary voltage is 300-1000V, and the ion auxiliary current is 300mA-1500mA, so that the residual stress of the high-refractive-index film layer in the reflecting mirror to be coated is controlled by adjusting the oxygen charging amount and the ion auxiliary deposition method while the loss absorption of the film layer is reduced, and the residual stress of each film layer is basically close to zero stress.
Compared with the prior art, the invention discloses a method for improving the surface shape precision of a large-aperture reflector coating film, which can realize the following technical effects:
before film coating, the film coating surface of a substrate to be coated is upwards placed on a film coating station of an electron beam evaporation film coating machine so as to heat and anneal the substrate to be coated with the upward film coating surface, thereby compensating the deformation quantity of the substrate to be coated in the film coating process in the subsequent steps so as to offset the heated deformation of the substrate in the state that the film coating surface is downwards in the film coating process from S6 to S10, and effectively controlling the surface shape of a reflector substrate The residual stress of each film layer of the reflector is basically close to zero stress. Obviously, the invention adopts the method of pre-turning and annealing the substrate to be coated to control and offset the surface shape change caused by the heating of the substrate in the coating process and combines the methods of adjusting the oxygen charging amount and ion auxiliary deposition to control the residual stress of the film layer in the reflector, thereby improving the surface shape precision of the large-caliber reflector.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a method for improving the surface shape precision of a coating film of a large-aperture reflector, which comprises the following steps:
s1, before film coating, the substrate to be coated is placed on a film coating station of an electron beam evaporation film coating machine, the film coating surface of the substrate to be coated is kept upward, the film coating station is positioned in a vacuum chamber, and the vacuum chamber is vacuumized;
s2, heating the substrate to be coated to a coating temperature through a heating module of the electron beam evaporation coating machine, then carrying out annealing treatment, cooling to a natural temperature, and then taking down;
s3, placing a high-refraction material and a low-refraction material in the electron beam evaporation coating machine;
s4, cleaning the substrate to be coated;
s5, placing the substrate to be coated with the film coating surface facing downwards on a film coating station of an electron beam evaporation film coating machine, and vacuumizing the substrate to be coated again through a vacuum chamber of the electron beam evaporation film coating machine;
s6, heating the substrate to be coated again to the coating temperature through a heating module of the electron beam evaporation coating machine, and carrying out heat preservation treatment;
s7, depositing a low-refractive-index material on the substrate to be coated by a first electron gun on an electron beam evaporation coating machine to form a low-refractive-index film layer on the substrate to be coated, simultaneously spraying oxygen on the low-refractive-index film layer by an oxygen spraying mechanism on the electron beam evaporation coating machine, and simultaneously bombarding the low-refractive-index film layer by an auxiliary ion source;
s8, depositing a high-refractive-index material on the low-refractive-index film layer in the step 5 through a second electron gun of the electron beam evaporation coating machine to form a high-refractive-index film layer on the low-refractive-index film layer, simultaneously spraying oxygen on the high-refractive-index film layer through an oxygen spraying mechanism on the electron beam evaporation coating machine, and simultaneously bombarding the high-refractive-index film layer through an auxiliary ion source;
s9, sequentially circulating the steps S7 and S8 to enable the low-refractive-index film layer and the high-refractive-index film layer to be formed on the substrate to be coated at intervals until the coating is finished to form the reflector;
and S10, cooling the reflector formed after the film coating is finished to room temperature, and taking out the reflector to obtain a large-aperture reflector sample.
In order to further optimize the above technical solution, the vacuum degree of the vacuum chamber in step S1 reaches 1 × 10-3Pa or less, the background vacuum degree of the vacuum chamber in step S5 reaches 1 × 10-4Pa or less.
In order to further optimize the technical scheme, the coating temperature in the steps S2 and S6 is 80-200 ℃.
In order to further optimize the technical scheme, in the annealing process of the step S2, the temperature of the substrate to be coated is kept at 120-150 minutes, the heat preservation time in the step S6 is 50-60 minutes, and the heat preservation temperature is 80-200 ℃.
In order to further optimize the above technical solution, in step S7, an ion-assisted electron beam evaporation method is adopted to deposit a low refractive index material on the substrate to be coated by a first electron gun of an electron beam evaporation coating machine, so that a low refractive index film layer is formed on the substrate to be coated.
In order to further optimize the above technical solution, in step S7, when the first electron gun is controlled to deposit the low refractive index film, the flow rate of the oxygen gas is controlled to be 10-30sccm, the ion auxiliary voltage of the auxiliary ion source is controlled to be 300-800V, and the ion auxiliary current is controlled to be 300-1000 mA, so that the residual stress of the low refractive index film is less than 10 MPa.
In order to further optimize the above technical solution, in step S8, an ion-assisted electron beam evaporation method is adopted to deposit a high refractive index material on the low refractive index film layer by using a second electron gun of an electron beam evaporation coating machine, so that the high refractive index film layer is formed on the low refractive index film layer.
In order to further optimize the above technical solution, in step S8, when the second electron gun is controlled to deposit the high refractive index film, the flow rate of the oxygen gas is 50-200sccm, the ion auxiliary voltage of the auxiliary ion source is controlled to be 300-1000V, and the ion auxiliary current is controlled to be 300-1500 mA, so that the residual stress of the high refractive index film is less than 10 MPa.
Example 1:
the method comprises the following steps:
s1, before coating, the height difference between the highest point and the lowest point of the K9 glass substrate surface shape is 106nm, the substrate to be coated is firstly placed on a coating station of an electron beam evaporation coating machine, the coating surface of the substrate to be coated is kept upward, the coating station is positioned in a vacuum chamber, the vacuum chamber is vacuumized, and the vacuum degree reaches 1 x 10-3Pa below;
s2, heating the K9 glass substrate to be coated to a coating temperature of 80 ℃ through a heating module of an electron beam evaporation coating machine, cooling the glass substrate to a natural temperature after the K9 glass substrate to be coated keeps the coating temperature (80 ℃) for 150 minutes, and taking down the glass substrate to be coated, wherein the height difference between the highest point and the lowest point of the surface shape of the substrate to be coated is 403 nm;
s3, placing a high-refraction material hafnium oxide and a low-refraction material silicon oxide in the electron beam evaporation coating machine;
s4, cleaning the substrate to be coated;
s5, placing the glass substrate to be coated with the film-coated surface of the k9 facing downwards on a film-coating station of an electron beam evaporation film-coating machine, and vacuumizing the vacuum chamber again to make the background vacuum degree of the vacuum chamber reach 1 x 10-4Pa below;
s6, heating the k9 glass substrate to be coated to 80 ℃ again through a heating module of the electron beam evaporation coating machine, and keeping the temperature of the substrate to be coated at 80 ℃ for 60 minutes;
s7, depositing a low-refractive-index material silicon oxide on a substrate to be coated by an ion-assisted electron beam evaporation method through a first electron gun on an electron beam evaporation coating machine to form a low-refractive-index film layer on the substrate to be coated, controlling the flow of oxygen to be 10sccm when the first electron gun deposits the low-refractive-index film layer, controlling the ion-assisted voltage of an auxiliary ion source to be 400V and the ion-assisted current to be 420mA, and enabling the residual stress of the low-refractive-index film layer to be less than 10 MPa;
s8, depositing a high-refractive-index material on the low-refractive-index film layer in the step 5 through a second electron gun of the electron beam evaporation coating machine to form the high-refractive-index film layer on the low-refractive-index film layer, controlling the flow rate of oxygen gas filled in the low-refractive-index film layer to be 160sccm when the second electron gun deposits the high-refractive-index film layer, controlling the ion auxiliary voltage of the auxiliary ion source to be 300-1000V and the ion auxiliary current to be 300-1500 mA, and enabling the residual stress of the high-refractive-index film layer to be less than 10 MPa;
s9, sequentially circulating the steps S7 and S8 to enable the low-refractive-index film layer and the high-refractive-index film layer to be formed on the substrate to be coated at intervals until the coating is finished to form the reflector;
and S10, cooling the mirror formed after the coating is finished to room temperature, and taking out the mirror to obtain a coated mirror sample, wherein the height difference between the highest point and the lowest point of the surface shape is 123 nm.
The result of the coating method by utilizing the traditional large-aperture reflector film layer is as follows: the surface shape variation of the reflector is more than 100 nm;
as a result of the plating method in example 1 of the present invention, the amount of deformation after plating was controlled to 17 nm.
Example 2:
the method comprises the following steps:
s1, before coating, the height difference between the highest point and the lowest point of the K9 glass substrate surface shape is 130nm, the substrate to be coated is firstly placed on a coating station of an electron beam evaporation coating machine, the coating surface of the substrate to be coated is kept upward, the coating station is positioned in a vacuum chamber, the vacuum chamber is vacuumized, and the vacuum degree reaches 1 x 10-3Pa below;
s2, heating the K9 glass substrate to be coated to a coating temperature of 120 ℃ through a heating module of an electron beam evaporation coating machine, cooling the glass substrate to a natural temperature after the K9 glass substrate to be coated keeps the coating temperature (120 ℃) for 120 minutes, and taking down the glass substrate, wherein the height difference between the highest point and the lowest point of the surface shape of the substrate to be coated is 620 nm;
s3, placing a high-refraction material hafnium oxide and a low-refraction material silicon oxide in the electron beam evaporation coating machine;
s4, cleaning the substrate to be coated;
s5, placing the glass substrate to be coated with the film-coated surface of the k9 facing downwards on a film-coating station of an electron beam evaporation film-coating machine, and vacuumizing the vacuum chamber again to make the background vacuum degree of the vacuum chamber reach 1 x 10-4Pa below;
s6, heating the k9 glass substrate to be coated to 120 ℃ again through a heating module of the electron beam evaporation coating machine, and keeping the temperature of the substrate to be coated at 120 ℃ for 60 minutes;
s7, depositing a low-refractive-index material silicon oxide on a substrate to be coated by an ion-assisted electron beam evaporation method through a first electron gun on an electron beam evaporation coating machine to form a low-refractive-index film layer on the substrate to be coated, controlling the flow of oxygen to be 10sccm when the first electron gun deposits the low-refractive-index film layer, controlling the ion-assisted voltage of an auxiliary ion source to be 400V and the ion-assisted current to be 420mA, and enabling the residual stress of the low-refractive-index film layer to be less than 10 MPa;
s8, depositing a high-refractive-index material on the low-refractive-index film layer in the step 5 through a second electron gun of the electron beam evaporation coating machine to form the high-refractive-index film layer on the low-refractive-index film layer, controlling the flow rate of oxygen gas filled in the low-refractive-index film layer to be 160sccm when the second electron gun deposits the high-refractive-index film layer, controlling the ion auxiliary voltage of the auxiliary ion source to be 300-1000V and the ion auxiliary current to be 300-1500 mA, and enabling the residual stress of the high-refractive-index film layer to be less than 10 MPa;
s9, sequentially circulating the steps S7 and S8 to enable the low-refractive-index film layer and the high-refractive-index film layer to be formed on the substrate to be coated at intervals until the coating is finished to form the reflector;
and S10, cooling the reflector formed after the coating is finished to room temperature, and taking out the reflector to obtain a coated reflector sample, wherein the height difference between the highest point and the lowest point of the surface shape is 149 nm.
The result of the coating method by utilizing the traditional large-aperture reflector film layer is as follows: the surface shape variation of the reflector is more than 100 nm;
as a result of the plating method in example 1 of the present invention, the amount of deformation after plating was controlled to 19 nm.
Example 3:
the method comprises the following steps:
s1, before coating, the height difference between the highest point and the lowest point of the K9 glass substrate surface shape is 210nm, the substrate to be coated is firstly placed on a coating station of an electron beam evaporation coating machine, the coating surface of the substrate to be coated is kept upward, the coating station is positioned in a vacuum chamber, the vacuum chamber is vacuumized, and the vacuum degree reaches 1 x 10-3Pa below;
s2, heating the K9 glass substrate to be coated to a coating temperature of 200 ℃ through a heating module of an electron beam evaporation coating machine, cooling the glass substrate to a natural temperature after the K9 glass substrate to be coated keeps the coating temperature (200 ℃) for 120 minutes, and taking down the glass substrate, wherein the height difference between the highest point and the lowest point of the surface shape of the substrate to be coated is 720 nm;
s3, placing a high-refraction material hafnium oxide and a low-refraction material silicon oxide in the electron beam evaporation coating machine;
s4, cleaning the substrate to be coated;
s5, placing the glass substrate to be coated with the film-coated surface of the k9 facing downwards on a film-coating station of an electron beam evaporation film-coating machine, and vacuumizing the vacuum chamber again to make the background vacuum degree of the vacuum chamber reach 1 x 10-4Pa below;
s6, heating the k9 glass substrate to be coated to 200 ℃ again through a heating module of the electron beam evaporation coating machine, and keeping the temperature of the substrate to be coated at 200 ℃ for 60 minutes;
s7, depositing a low-refractive-index material silicon oxide on a substrate to be coated by an ion-assisted electron beam evaporation method through a first electron gun on an electron beam evaporation coating machine to form a low-refractive-index film layer on the substrate to be coated, controlling the flow of oxygen to be 10sccm when the first electron gun deposits the low-refractive-index film layer, controlling the ion-assisted voltage of an auxiliary ion source to be 400V and the ion-assisted current to be 420mA, and enabling the residual stress of the low-refractive-index film layer to be less than 10 MPa;
s8, depositing a high-refractive-index material on the low-refractive-index film layer in the step 5 through a second electron gun of the electron beam evaporation coating machine to form the high-refractive-index film layer on the low-refractive-index film layer, controlling the flow rate of oxygen gas filled in the low-refractive-index film layer to be 160sccm when the second electron gun deposits the high-refractive-index film layer, controlling the ion auxiliary voltage of the auxiliary ion source to be 300-1000V and the ion auxiliary current to be 300-1500 mA, and enabling the residual stress of the high-refractive-index film layer to be less than 10 MPa;
s9, sequentially circulating the steps S7 and S8 to enable the low-refractive-index film layer and the high-refractive-index film layer to be formed on the substrate to be coated at intervals until the coating is finished to form the reflector;
and S10, cooling the reflector formed after the coating is finished to room temperature, and taking out the reflector to obtain a coated reflector sample, wherein the height difference between the highest point and the lowest point of the surface shape is 225 nm.
The result of the coating method by utilizing the traditional large-aperture reflector film layer is as follows: the surface shape variation of the reflector is more than 100 nm;
as a result of the plating method in example 1 of the present invention, the amount of deformation after plating was controlled to 15 nm.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (7)

1. A method for improving the accuracy of the coating surface shape of a large-aperture reflector is characterized by comprising the following steps:
s1, before film coating, placing the substrate to be coated on a film coating station of an electron beam evaporation film coating machine, keeping the film coating surface of the substrate to be coated upward, and simultaneously, positioning the film coating station in a vacuum chamber, and vacuumizing the vacuum chamber;
s2, heating the substrate to be coated to a coating temperature through a heating module of the electron beam evaporation coating machine, then carrying out annealing treatment, and taking down the substrate after cooling to a natural temperature;
s3, placing a high-refraction material and a low-refraction material in the electron beam evaporation coating machine;
s4, cleaning the substrate to be coated;
s5, placing the film-coated surface of the substrate to be film-coated on a film-coating station of the electron beam evaporation film-coating machine downwards, and vacuumizing the substrate to be film-coated again through a vacuum chamber of the electron beam evaporation film-coating machine;
s6, heating the substrate to be coated to the coating temperature again through a heating module of the electron beam evaporation coating machine, and carrying out heat preservation treatment;
s7, depositing the low-refractive-index material on the substrate to be coated by a first electron gun on the electron beam evaporation coating machine to form a low-refractive-index film layer on the substrate to be coated, simultaneously spraying oxygen on the low-refractive-index film layer by an oxygen spraying mechanism on the electron beam evaporation coating machine, and simultaneously bombarding the low-refractive-index film layer by an auxiliary ion source;
s8, depositing the high-refractive-index material on the low-refractive-index film layer in the step 5 through a second electron gun of the electron beam evaporation coating machine to form a high-refractive-index film layer on the low-refractive-index film layer, simultaneously spraying oxygen on the high-refractive-index film layer through an oxygen spraying mechanism on the electron beam evaporation coating machine, and simultaneously bombarding the high-refractive-index film layer through an auxiliary ion source;
s9, sequentially circulating the steps S7 and S8 to enable the low-refractive-index film layer and the high-refractive-index film layer to be formed on the substrate to be coated at intervals until the coating is finished to form a reflector;
and S10, cooling the reflector formed after the film coating is finished to room temperature, and taking out the reflector to obtain a large-aperture reflector sample.
2. The method of claim 1, wherein the coating temperature in each of the steps S2 and S6 is 80 to 200 degrees Celsius.
3. The method as claimed in claim 2, wherein in the annealing step of step S2, the substrate to be coated is kept at the coating temperature of 140-150 minutes, the heat-preserving time in step S6 is 50-60 minutes, and the heat-preserving temperature is 80-200 ℃.
4. The method of claim 1, wherein in step S7, an ion-assisted electron beam evaporation method is used to deposit the low refractive index material on the substrate to be coated by the first electron gun of the electron beam evaporation coater to form a low refractive index film layer on the substrate to be coated.
5. The method as claimed in claim 4, wherein in step S7, when the first electron gun is controlled to deposit the low refractive index film, the flow rate of the oxygen gas is controlled to be 10-30sccm, the ion-assisted voltage of the auxiliary ion source is controlled to be 300-800V, and the ion-assisted current is controlled to be 300-1000 mA, so that the residual stress of the low refractive index film is less than 10 MPa.
6. The method of claim 1, wherein an ion assisted electron beam evaporation method is used in step S8 to deposit the high refractive index material on the low refractive index film layer by the second electron gun of the electron beam evaporation coater to form the high refractive index film layer on the low refractive index film layer.
7. The method as claimed in claim 6, wherein in step S8, when the second electron gun is controlled to deposit the high refractive index film, the flow rate of the oxygen gas is controlled to be 50-200sccm, the ion assist voltage of the auxiliary ion source is controlled to be 300-1000V, and the ion assist current is controlled to be 300-1500 mA, so that the residual stress of the high refractive index film is less than 10 MPa.
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