CN112267098B - Preparation method of space laser film - Google Patents
Preparation method of space laser film Download PDFInfo
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- CN112267098B CN112267098B CN202010928969.0A CN202010928969A CN112267098B CN 112267098 B CN112267098 B CN 112267098B CN 202010928969 A CN202010928969 A CN 202010928969A CN 112267098 B CN112267098 B CN 112267098B
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/3442—Applying energy to the substrate during sputtering using an ion beam
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- 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
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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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
- C23C14/54—Controlling or regulating the coating process
Abstract
The invention belongs to the technical field of optical films, and particularly relates to a preparation method of a space laser film. The method provides a full-flow technical scheme for preparing the space laser film, which comprises the steps of removing pollutants and subsurface defects on the surface of a substrate, adding an anti-irradiation protective layer and coating a film on the substrate, and defines the technical scheme and the realization way of each link.
Description
Technical Field
The invention belongs to the technical field of optical films, and particularly relates to a preparation method of a space laser film.
Background
With the continuous and deep exploration of the space environment by human beings and the continuous development of lasers, the space laser system becomes an important tool in the space mission. The optical film is one of the weakest elements in the optical system, and cannot be repaired or replaced once being damaged during the track running, so that the stability and the service life of the optical film are very important for the whole system. The space has special environmental factors such as vacuum, high-low temperature alternation, high-energy particle irradiation and the like different from the ground, and the laser film applied to the space not only can resist laser damage, but also has good stability in the space environment, thereby putting higher requirements on the optical film.
The laser film prepared by the traditional electron beam evaporation is loose and porous in structure, and can generate serious atmospheric-vacuum effect and irradiation damage in the process from the ground to the space, so that the microstructure, stress and material thermodynamic parameters of the film material are changed, and the macroscopic spectral performance and the laser damage resistance performance are further influenced, therefore, the laser film is not suitable for the space environment.
In addition, the surface defects and subsurface defects of the substrate also greatly limit the laser damage threshold of the film, commonly used ultrasonic cleaning cannot effectively remove substrate impurities, and chemical etching methods such as HF (hydrogen fluoride) or ion beam etching methods are needed to effectively remove pollutants and subsurface defects.
Aiming at the defects of the traditional processing and preparation process, the invention provides a full-flow preparation technology from substrate cleaning to coating process, and the laser damage threshold and the space stability of the film are further improved.
Disclosure of Invention
The invention aims to provide a preparation method of a space laser film, provides a full-flow technical scheme including removing pollutants and subsurface defects on the surface of a substrate, adding an anti-irradiation protective layer and coating a film on the substrate, and effectively solves the problem of poor stability of the laser film in a space environment.
The technical solution of the invention is as follows:
(1) removing pollutants and subsurface defects on the surface of the substrate;
(2) selection of SiO2、Al2O3And MgF2One of them is used as an anti-radiation protective layer and is coated on the substrate.
In the invention, the specific steps of the step (1) are as follows:
(1.1) ultrasonically cleaning the substrate for 10-30 min, then flushing with deionized water, and finally drying with high-purity nitrogen;
(1.2) performing hydrofluoric acid etching or ion beam etching on the substrate, wherein the etching depth is 180-220 nm.
In the invention, the substrate material is a space irradiation resistant substrate material, such as quartz glass.
In the invention, the laser film is made of SiO2、Al2O3、MgF2、TiO2、Ta2O5、ZrO2、HfO2、Nb2O5A monolayer film or a multilayer film of one or more of (a).
In the invention, the anti-radiation protective layer in the step (2) is positioned on the incident medium layer, and SiO2、MgF2Suitable for ultraviolet band, Al2O3Suitable for use in the visible and infrared bands.
In the invention, the step (2) of coating the film on the substrate comprises the following specific steps:
(2.1) scrubbing a vacuum chamber in the coating machine, and performing vacuum pumping;
(2.2) putting the substrate and the target material into a film plating machine, closing the cabin door of the vacuum cabin, performing vacuum air suction again, and controlling the background vacuum degree of the vacuum chamber in the film plating machine to be 10-5-10-7Pa；
(2.3) heating the substrate to keep the temperature of the substrate between 80 and 120 ℃;
and (2.4) coating by using an ion source assisted physical vapor deposition method, wherein argon is used as an ion source gas, oxygen is filled in the argon, the oxygen is filled in the argon at an amount of 5-45sccm to fully oxidize target material atoms, and the deposition rate of film material molecules on a substrate is controlled to be 0.15-0.40 nm/s.
In the invention, the ion source assisted physical vapor deposition method in the step (2.4) is one of dual ion beam sputtering, ion beam assisted deposition and magnetron sputtering.
In the invention, the dual ion beam sputtering specifically comprises the following steps: argon is used as a main ion source gas, the voltage of the main ion source is 1150-1350V, argon and oxygen are used as auxiliary ion source gases, the voltage of the auxiliary ion source is 500-700V, and the flow ratio of the argon to the oxygen is 1:4-1: 6.
The invention has the following technical effects:
(1) the technical scheme of the whole process of removing pollutants and subsurface defects on the surface of a substrate, adding an anti-irradiation protective layer and coating on the substrate is provided, an optimized solution is provided for each link of film design, processing and preparation, and the laser irradiation stability and the space environment stability of the prepared film are obviously improved;
(2) the anti-irradiation protective layer is added, so that the prepared space laser film is not easy to be damaged by irradiation of space particles, has higher space stability, has no obvious change in the overall optical performance after being irradiated by Gamma rays, and has the transmittance change of less than 3 percent;
(3) by using acid etching or ion beam etching, the defects of the surface and the sub-surface of the substrate are greatly reduced, the defects of low threshold value and impurities are effectively removed, the defect density is reduced by about 10 times compared with ultrasonic cleaning, and the threshold value of the film is improved by about 10 times compared with ultrasonic cleaning;
(4) the refractive index of the prepared space laser film can reach the level of bulk material, the spectral offset is small in the atmosphere-vacuum environment, and the vacuum degree is lower than 10-3The spectral offset in the environment of mbar is less than 0.5 percent, and the environment with alternating vacuum and high and low temperature can be resisted.
Drawings
FIG. 1 is a transmittance spectrum of a film under the atmosphere and vacuum in the preferred embodiment 1 of the present invention.
FIG. 2 is a graph showing the probability of laser damage to a thin film in different substrate cleaning modes according to the preferred embodiment 1 of the present invention.
FIG. 3 is a spectrum curve of the thin film before and after Gamma ray irradiation in the preferred embodiment 2 of the present invention.
FIG. 4 is a graph showing the probability of 1-on-1 laser damage before and after Gamma ray irradiation of the thin film in the preferred embodiment 2 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Example 1: using quartz glass as substrate, Al2O3Is film layer material, SiO2And preparing a 1064nm antireflection film for the protective layer material.
Ultrasonically cleaning the substrate for 10-30 min, then flushing with deionized water, and finally drying with high-purity nitrogen; scrubbing a vacuum chamber in the coating machine, and performing vacuum pumping; putting the substrate into a film coating machine, closing the hatch door of the vacuum chamber, performing vacuum pumping again, and controlling the background vacuum degree of the vacuum chamber in the film coating machine to be 2 multiplied by 10-6Pa, heating the substrate to keep the temperature of the substrate at 80 ℃; before coating, ion beam etching is carried out on the substrate, an Ar ion source is used for bombarding the substrate, the voltage of the used Ar ion source is 650V, and the etching depth is 200 nm; and (3) coating a film on the treated substrate by using a double-ion-beam sputtering device, wherein the voltage of a main ion source is 1250V, argon is used as a main ion source gas, the voltage of an auxiliary ion source is 650V, the flow ratio of the argon to oxygen is 1:5, the oxygen charging amount is 15sccm, and the deposition rate of film material molecules on the substrate is controlled to be about 0.2 nm/s.
Performing spectrum test on the prepared space laser film under atmosphere and vacuum, wherein the test vacuum degree is about 10-3mbar, fig. 1 is the transmittance spectrum of the film in air and vacuum. Research shows that the spectral wavelength of the antireflection film is only slightly blue-shifted, the offset is reduced from 2.5% to 0.15% compared with a 1064nm antireflection film prepared by a traditional method, and the transmittance at 1064nm is hardly reduced.
The prepared space laser film is subjected to 1-on-1 laser damage test according to ISO 21254 standard, and FIG. 2 shows laser damage probability curves of the film under different substrate cleaning modes. The results show that after ion beam etching, radicalsImpurity elements such as Na, Ce, K, Fe and the like in the bottom are obviously reduced, the surface roughness is also obviously improved, and the defect density is 2.20mm obtained by ultrasonic cleaning-2Reduced to 0.22mm-2The film threshold was increased by about 10 times compared to the ultrasonic method, respectively.
Example 2: ta on quartz glass as substrate2O5Is film layer material, SiO2Preparing a high-reflection film for the protective layer material.
Ultrasonically cleaning the substrate for 10-30 min, then flushing with deionized water, and finally drying with high-purity nitrogen; scrubbing a vacuum chamber in the coating machine, and performing vacuum pumping; putting the substrate into a film coating machine, closing the hatch door of the vacuum chamber, performing vacuum pumping again, and controlling the background vacuum degree of the vacuum chamber in the film coating machine to be 2 multiplied by 10-6Pa, heating the substrate to keep the temperature of the substrate at 80 ℃; before coating, ion beam etching is carried out on the substrate, an Ar ion source is used for bombarding the substrate, the voltage of the Ar ion source is 650V, and the etching depth is 200 nm; and (3) coating a film on the treated substrate by using a double-ion-beam sputtering device, wherein the voltage of a main ion source is 1250V, argon is used as a main ion source gas, the voltage of an auxiliary ion source is 650V, the flow ratio of the argon to oxygen is 1:5, the oxygen charging amount is 40sccm, and the deposition rate of film material molecules on the substrate is controlled to be about 0.2 nm/s.
According to the result of an isodose irradiation experiment carried out by Gamma rays which are operated for 8 years on the track in practical application, the spectrum is not obviously changed before and after irradiation, the film has good irradiation resistance stability, and a graph 3 is a spectrum curve of the film before and after the Gamma ray irradiation.
And then performing 1-on-1 laser damage test on the irradiated film according to ISO 21254 standard, wherein FIG. 4 shows the 1-on-1 laser damage probability of the film before and after Gamma ray irradiation. The result shows that the laser damage threshold of the film prepared by the invention is basically unchanged after Gamma ray irradiation, and the film has good space irradiation resistance and laser damage resistance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The preparation method of the space laser film is characterized by comprising the following steps of:
(1) removing pollutants and subsurface defects on the surface of the substrate;
(2) selection of SiO2、Al2O3And MgF2One of the layers is used as an anti-radiation protective layer and is coated on the substrate, the anti-radiation protective layer is positioned on the incident medium layer, wherein SiO2、MgF2Suitable for ultraviolet band, Al2O3Suitable for visible and infrared wave band;
the specific steps of coating the film on the substrate are as follows:
(2.1) scrubbing a vacuum chamber in the coating machine, and performing vacuum pumping;
(2.2) putting the substrate and the target material into a film plating machine, closing the cabin door of the vacuum cabin, performing vacuum air suction again, and controlling the background vacuum degree of the vacuum chamber in the film plating machine to be 10-5-10-7Pa；
(2.3) heating the substrate to keep the temperature of the substrate between 80 and 120 ℃;
and (2.4) coating by using an ion source assisted physical vapor deposition method, wherein argon is used as an ion source gas, oxygen is filled in the argon, the oxygen is filled in the argon at an amount of 5-45sccm to fully oxidize target material atoms, and the deposition rate of film material molecules on a substrate is controlled to be 0.15-0.40 nm/s.
2. The method for preparing a space laser film according to claim 1, wherein: the specific step of the step (1) is
(1.1) ultrasonically cleaning the substrate for 10-30 min, then flushing with deionized water, and finally drying with high-purity nitrogen;
(1.2) performing hydrofluoric acid etching or ion beam etching on the substrate, wherein the etching depth is 180-220 nm.
3. The method for preparing a space laser film according to claim 1, wherein: the substrate material is a space irradiation resistant substrate material.
4. The method for preparing a space laser film according to claim 1, wherein: the laser film is made of SiO2、Al2O3、MgF2、TiO2、Ta2O5、ZrO2、HfO2、Nb2O5One or more of (a).
5. The method for preparing a space laser film according to claim 1, wherein the ion source assisted physical vapor deposition method in the step (2.4) is one of dual ion beam sputtering, ion beam assisted deposition and magnetron sputtering.
6. The method as claimed in claim 5, wherein the dual ion beam sputtering is performed by using argon as the main ion source gas, the main ion source voltage is 1150-1350V, argon and oxygen are used as the auxiliary ion source gas, the auxiliary ion source voltage is 500-700V, and the flow ratio of argon to oxygen is 1:4-1: 6.
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| KR101353264B1 (en) * | 2012-05-31 | 2014-01-27 | 현대자동차주식회사 | Plating method using a etching process of laser |
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