CN112941460A - High-reliability optical filter manufacturing method - Google Patents

High-reliability optical filter manufacturing method Download PDF

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Publication number
CN112941460A
CN112941460A CN202110138713.4A CN202110138713A CN112941460A CN 112941460 A CN112941460 A CN 112941460A CN 202110138713 A CN202110138713 A CN 202110138713A CN 112941460 A CN112941460 A CN 112941460A
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glass substrate
coating
film forming
cleaning
coating jig
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CN202110138713.4A
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Chinese (zh)
Inventor
陈国彦
刁兆俊
蔡喜斌
华秀菊
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Shenzhen Smartidea Co ltd
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Shenzhen Smartidea Co ltd
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Priority to CN202110138713.4A priority Critical patent/CN112941460A/en
Publication of CN112941460A publication Critical patent/CN112941460A/en
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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
    • 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
    • C23C14/021Cleaning or etching treatments
    • 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
    • C23C14/58After-treatment
    • C23C14/584Non-reactive treatment

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention provides a method for manufacturing a high-reliability optical filter, which comprises the following steps: selecting quartz glass with high hardness, high temperature resistance, low expansion coefficient and good chemical stability; cleaning, drying and storing the glass substrate; before coating, extracting high vacuum from a coating jig to ensure that the vacuum degree of the coating jig is stabilized between 1.0E and 3Pa, simultaneously heating a cavity in the coating jig and a cleaned and dried glass substrate to 220 ℃ at constant temperature, loading the glass substrate heated at constant temperature onto an umbrella stand of the coating jig, and carrying out evaporation coating on the glass substrate by using a Ti3O5 material with a high refractive index and a SiO2 material with a low refractive index; and naturally cooling the coated glass substrate, and filling high-purity nitrogen into the cavity of the coating jig to solidify the cooled glass substrate. Compared with the prior art, the invention can improve the mechanical property of the product, manufacture the optical filter with high reliability and solve the problems of low product yield, easy demoulding, edge breakage and corner breakage of the optical filter in the prior art.

Description

High-reliability optical filter manufacturing method
Technical Field
The invention relates to the technical field of optical thin films, in particular to a method for manufacturing a high-reliability optical filter.
Background
Filters are optical devices used to select a desired wavelength band of radiation. One common property of filters is that no filter can make the imaging of celestial objects brighter, since all filters absorb certain wavelengths, thereby making the object darker.
Under the drive of the rapid development of the optical communication industry, the demand of the optical filter is greatly increased. In addition to certain optical characteristics, the optical film should have mechanical characteristics suitable for its application, such as sufficient mechanical strength, good adhesion to a glass substrate, proper internal stress state, etc., and the microstructure of the film plays an important role in influencing its mechanical properties. The traditional process for preparing the optical filter mainly adopts normal-temperature evaporation type film forming, and requires low vacuum degree and low material deposition rate; the phenomenon of large internal stress and poor adhesive force can be caused to the optical filter with a thick film layer. The above process has the following defects: the internal stress of the product is large, and the product can cause film falling and glass edge breakage due to poor adhesion and internal stress release of the film in the cutting process.
In the film forming process of the optical filter, due to the difference of the material and the film system of the glass substrate, good adhesive force is lacked between the film layer and the substrate. The internal stress is caused by the vacuum degree of the cavity in the coating process and the difference of the thermal expansion coefficients between the film layer and the substrate, the evaporation of the film material can generate heat, and when the film material is switched and evaporated, the temperatures of the cavity and the glass substrate are difficult to control, so that the temperature of the cavity can generate large fluctuation, and the internal stress is not well controlled. The optical filter can be subjected to demoulding, edge breakage and corner cracking in the process of cutting into small particles, the reliability is poor, the yield of the product is reduced by 23%, and the requirements of customers cannot be met.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention can improve the mechanical property of the product, so that the optical filter is not easy to demould, break edges and crack corners, the optical filter with high reliability is manufactured, and the yield of the optical filter is improved.
A method for manufacturing a high-reliability optical filter adopts the following specific technical scheme:
a method for manufacturing a high-reliability optical filter comprises the following steps:
selecting the material of the glass substrate: selecting quartz glass with hardness up to Mohs seven grade, high temperature resistance, low expansion coefficient, good chemical stability and size of 40 X40X0.88mm;
cleaning and drying treatment: cleaning, drying and storing the glass substrate;
coating treatment: before coating, extracting high vacuum from a coating jig to ensure that the vacuum degree of the coating jig is stabilized between 1.0E and 3Pa, simultaneously heating a cavity in the coating jig and the cleaned and dried glass substrate to 220 ℃ at constant temperature, loading the glass substrate heated at constant temperature onto an umbrella stand of the coating jig, and performing evaporation coating on the glass substrate by using a Ti3O5 material with a high refractive index and a SiO2 material with a low refractive index;
cooling and solidifying: and naturally cooling the glass substrate after the film coating is finished for a preset time, and filling high-purity nitrogen into the cavity of the film coating jig to solidify the cooled glass substrate.
In a specific embodiment, the method of the "coating treatment" includes:
firstly plating the SiO2 material to generate a SiO2 film layer, and then plating the Ti3O5 material to generate a Ti3O5 film layer;
when the SiO2 material is plated, an ion source is used for thoroughly pre-cleaning the glass substrate, and then a SiO2 bonding layer with the thickness of 0.15um is pre-plated, wherein the film forming rate of the SiO2 material is 8.5A/s, the film forming oxygen is 50sccm, the film forming argon is 10sccm, the film forming temperature is 220 ℃, and the film forming vacuum degree is 1.0E-3 Pa;
when the Ti3O5 material is plated, the film forming rate of the Ti3O5 material is 4.5A/s, the film forming oxygen is 60sccm, the film forming argon is 10sccm, the film forming temperature is 220 ℃, and the film forming vacuum degree is 1.0E-2 Pa.
In a specific embodiment, the method of the "cleaning and drying process" includes:
loading optical quartz glass into a cleaning basket, further placing the cleaning basket on a full-automatic ultrasonic cleaning line, cleaning the glass for removing oil and dust, and after cleaning, placing the glass into a full-automatic dust-free high-temperature oven for drying and storing.
In a specific embodiment, the method of "cooling and solidifying" includes:
and after the film forming is finished, placing the glass substrate in a cavity in the film coating jig for natural cooling for a preset time, and filling high-purity nitrogen into the cavity in the film coating jig after the natural cooling to solidify the glass substrate.
Compared with the prior art, the invention has the following beneficial effects:
according to the manufacturing method of the technical scheme, high vacuum is extracted from the coating jig before coating, the vacuum degree of the coating jig is stabilized to be 1.0E-3Pa, meanwhile, a cavity in the coating jig and the cleaned and dried glass substrate are heated to 220 ℃ at constant temperature, the glass substrate heated at constant temperature is loaded onto an umbrella stand of the coating jig, and Ti3O5 material with high refractive index and SiO2 material with low refractive index are used for evaporation coating of the glass substrate. And naturally cooling the glass substrate after the film coating is finished for a preset time, and filling high-purity nitrogen into the cavity of the film coating jig to solidify the cooled glass substrate. Further improves the mechanical property of the product, ensures that the optical filter is not easy to demould, edge breakage and corner cracking, manufactures the optical filter with high reliability and improves the yield of the optical filter.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of a method for fabricating an optical filter according to an embodiment;
fig. 2 is a structural view of the optical filter in the embodiment.
Description of the main element symbols:
1-a glass substrate; a 2-SiO2 bonding layer; 3-SiO2 film layer; 4-Ti3O5 film layer; 5-curing the layer with nitrogen.
Detailed Description
According to the manufacturing method of the high-reliability optical filter, high vacuum is extracted from the coating jig before coating, so that the vacuum degree of the coating jig is stabilized between 1.0E-3Pa, meanwhile, a cavity in the coating jig and the cleaned and dried glass substrate are heated to 220 ℃ at a constant temperature, the glass substrate heated at the constant temperature is loaded on an umbrella stand of the coating jig, and the glass substrate is subjected to evaporation coating by using a Ti3O5 material with a high refractive index and a SiO2 material with a low refractive index. And naturally cooling the glass substrate after the film coating is finished for a preset time, and filling high-purity nitrogen into the cavity of the film coating jig to solidify the cooled glass substrate. Further, the mechanical property of the product is improved, so that the optical filter is not easy to demould, break edges and crack corners, the optical filter with high reliability is manufactured, and the yield of the optical filter is improved.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Examples
As shown in fig. 1-2, the embodiment provides a method for manufacturing a high-reliability optical filter, and the specific technical solution is as follows:
a method for manufacturing a high-reliability optical filter comprises the following steps:
selecting the material of the glass substrate 1: the quartz glass with hardness up to Mohs seven grade, high temperature resistance, low expansion coefficient, good chemical stability and size of 40X40X0.88mm is selected.
In particular, the quartz glass has the hardness of reaching Mohs seven grades, has high temperature resistance, the frequent use temperature of 1100 ℃ to 1200 ℃, the short-term use temperature of 1400 ℃ and low expansion coefficient, and is 1/10 to 1/20 of common BK7 glass. The heat shock resistance, the chemical stability and the electrical insulation performance are good, and ultraviolet rays and infrared rays can be transmitted;
cleaning and drying treatment: and cleaning, drying and storing the glass substrate 1.
Coating treatment: before coating, the coating jig is pumped to high vacuum, so that the vacuum degree of the coating jig is stabilized between 1.0E-3Pa, and simultaneously, the cavity in the coating jig and the cleaned and dried glass substrate 1 are heated to 220 ℃ at constant temperature, because the high vacuum degree and the higher substrate temperature are favorable for mutual diffusion between the film material and the substrate, and firm diffusion adhesion is formed. And then loading the glass substrate 1 heated at the constant temperature on an umbrella stand of a coating jig, and performing evaporation coating on the glass substrate 1 by using a Ti3O5 material with a high refractive index and an SiO2 material with a low refractive index.
Cooling and solidifying: and naturally cooling the glass substrate 1 after the film coating is finished for a preset time, and filling high-purity nitrogen into the cavity of the film coating jig to solidify the cooled glass substrate 1.
In this embodiment, the method of "cleaning and drying" includes:
loading optical quartz glass into a cleaning basket, further placing the cleaning basket on a full-automatic ultrasonic cleaning line, cleaning the glass for removing oil and dust, and after cleaning, placing the glass into a full-automatic dust-free high-temperature oven for drying and storing. The cleaning and storage of the glass substrate 1 directly affects the surface state of the glass, on the one hand, the adhesion is greatly affected, and on the other hand, the magnitude of the internal stress is also affected.
In this embodiment, the method of "plating treatment" includes:
firstly plating SiO2 material to generate SiO2 film layer 3, and then plating Ti3O5 material to generate Ti3O5 film layer 4.
Specifically, since the physical properties of the SiO2 material are close to those of the quartz substrate, the SiO2 material plated first can further increase the adhesion between the film and the glass substrate 1 compared with the Ti3O5 material plated first.
When the SiO2 material is plated, the glass substrate 1 is thoroughly pre-cleaned by the ion source, and the adsorption layer on the surface of the contaminated glass substrate 1 will destroy the physical and chemical bonding force required for adhesion. And pre-plating a SiO2 bonding layer 2 with the thickness of 0.15um, wherein the film forming rate of the SiO2 material is 8.5A/s, the film forming oxygen is 50sccm, the film forming argon is 10sccm, the film forming temperature is 220 ℃, and the film forming vacuum degree is 1.0E-3 Pa.
When the Ti3O5 material is plated, the film forming rate of the Ti3O5 material is 4.5A/s, the film forming oxygen is 60sccm, the film forming argon is 10sccm, the film forming temperature is 220 ℃, and the film forming vacuum degree is 1.0E-2 Pa.
Specifically, the generation of the internal stress of the optical filter is mainly the influence of the deposition process of the film material, and the influence of the film forming temperature, the film forming rate, the film forming vacuum degree and the like on the film layer stress needs to be specifically researched according to the type of the film material, the material of the glass substrate 1 and the film forming process.
In the present embodiment, the method of "cooling and solidifying" includes:
after the film forming is finished, the glass substrate 1 is placed in a cavity in a film coating jig for natural cooling for a preset time, high-purity nitrogen is filled into the cavity in the film coating jig after the natural cooling to solidify the glass substrate 1, and a nitrogen solidified layer 5 is generated on the surface of the glass substrate 1.
Specifically, the internal stress of the film often shows timeliness, and the internal stress can be slowly changed under different environments and temperatures, and the cooling scheme can effectively release the internal stress of the film.
Specifically, the glass substrate 1 is placed in a cavity in the coating jig and naturally cooled for 1 hour and 30 minutes, and the time period of 1 hour and 30 minutes is only one preferable mode of the embodiment, and other preferable modes are provided.
Compared with the prior art, the manufacturing method adopting the technical scheme of the invention has the advantages that high vacuum is extracted from the coating jig before coating, so that the vacuum degree of the coating jig is stabilized between 1.0E-3Pa, meanwhile, the cavity in the coating jig and the cleaned and dried glass substrate are heated to 220 ℃ at constant temperature, the glass substrate heated at constant temperature is loaded on the umbrella stand of the coating jig, and the Ti3O5 material with high refractive index and the SiO2 material with low refractive index are used for evaporation coating of the glass substrate. And naturally cooling the glass substrate after the film coating is finished for a preset time, and filling high-purity nitrogen into the cavity of the film coating jig to solidify the cooled glass substrate. Further improves the mechanical property of the product, ensures that the optical filter is not easy to demould, edge breakage and corner cracking, manufactures the optical filter with high reliability and improves the yield of the optical filter.
Those skilled in the art will appreciate that the figures are merely schematic representations of one preferred implementation scenario and that the blocks or flow diagrams in the figures are not necessarily required to practice the present invention.
Those skilled in the art will appreciate that the modules in the devices in the implementation scenario may be distributed in the devices in the implementation scenario according to the description of the implementation scenario, or may be located in one or more devices different from the present implementation scenario with corresponding changes. The modules of the implementation scenario may be combined into one module, or may be further split into a plurality of sub-modules.
The above-mentioned invention numbers are merely for description and do not represent the merits of the implementation scenarios.
The above disclosure is only a few specific implementation scenarios of the present invention, however, the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.

Claims (4)

1. A method for manufacturing a high-reliability optical filter is characterized by comprising the following steps:
selecting the material of the glass substrate: selecting quartz glass with hardness up to Mohs seven grade, high temperature resistance, low expansion coefficient, good chemical stability and size of 40 X40X0.88mm;
cleaning and drying treatment: cleaning, drying and storing the glass substrate;
coating treatment: before coating, extracting high vacuum from a coating jig to ensure that the vacuum degree of the coating jig is stabilized between 1.0E and 3Pa, simultaneously heating a cavity in the coating jig and the cleaned and dried glass substrate to 220 ℃ at constant temperature, loading the glass substrate heated at constant temperature onto an umbrella stand of the coating jig, and performing evaporation coating on the glass substrate by using a Ti3O5 material with a high refractive index and a SiO2 material with a low refractive index;
cooling and solidifying: and naturally cooling the glass substrate after the film coating is finished for a preset time, and filling high-purity nitrogen into the cavity of the film coating jig to solidify the cooled glass substrate.
2. The method of claim 1, wherein the coating process comprises:
firstly plating the SiO2 material to generate a SiO2 film layer, and then plating the Ti3O5 material to generate a Ti3O5 film layer;
when the SiO2 material is plated, an ion source is used for thoroughly pre-cleaning the glass substrate, and then a SiO2 bonding layer with the thickness of 0.15um is pre-plated, wherein the film forming rate of the SiO2 material is 8.5A/s, the film forming oxygen is 50sccm, the film forming argon is 10sccm, the film forming temperature is 220 ℃, and the film forming vacuum degree is 1.0E-3 Pa;
when the Ti3O5 material is plated, the film forming rate of the Ti3O5 material is 4.5A/s, the film forming oxygen is 60sccm, the film forming argon is 10sccm, the film forming temperature is 220 ℃, and the film forming vacuum degree is 1.0E-2 Pa.
3. The method of manufacturing an optical filter according to claim 1, wherein the "cleaning and drying process" method comprises:
loading optical quartz glass into a cleaning basket, further placing the cleaning basket on a full-automatic ultrasonic cleaning line, cleaning the glass for removing oil and dust, and after cleaning, placing the glass into a full-automatic dust-free high-temperature oven for drying and storing.
4. A method for manufacturing an optical filter according to claim 1, wherein the "cooling and solidifying" method comprises:
and after the film forming is finished, placing the glass substrate in a cavity in the film coating jig for natural cooling for a preset time, and filling high-purity nitrogen into the cavity in the film coating jig after the natural cooling to solidify the glass substrate.
CN202110138713.4A 2021-02-01 2021-02-01 High-reliability optical filter manufacturing method Pending CN112941460A (en)

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