CN111996491A - Thermal control coating with designable solar absorptivity and preparation method thereof - Google Patents

Thermal control coating with designable solar absorptivity and preparation method thereof Download PDF

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Publication number
CN111996491A
CN111996491A CN202010950599.0A CN202010950599A CN111996491A CN 111996491 A CN111996491 A CN 111996491A CN 202010950599 A CN202010950599 A CN 202010950599A CN 111996491 A CN111996491 A CN 111996491A
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layer
coating
thermal control
thickness
control coating
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丁良兵
董中林
李磊
佟文清
杨鑫鑫
曹立荣
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CETC 38 Research Institute
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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
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • 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
    • C23C14/081Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • 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
    • C23C14/34Sputtering

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
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Abstract

The invention discloses a thermal control coating with a designable solar absorptivity and a preparation method thereof.A first coating, a second coating and a third coating are sequentially arranged on the surface of a substrate from inside to outside, wherein the first coating is a pure aluminum layer, the second coating is an aluminum nitride layer, and the third coating is an aluminum oxide layer; the thermal control coating prepared on the surface of the aluminum alloy base material by the preparation method can realize the adjustment of the solar absorptivity of the thermal control coating within the range of 0.10 to 0.92 through the thickness design of the coating film layer.

Description

Thermal control coating with designable solar absorptivity and preparation method thereof
Technical Field
The invention relates to the technical field of surface engineering, in particular to a thermal control coating with designable solar absorptivity and a preparation method thereof.
Background
The thermal control coating is a functional coating for adjusting the optical and thermal properties of the surface of a solid so as to achieve the aim of thermal control, and is a very important material adopted by a thermal control system of a spacecraft. The thermal control coating maintains the balance of energy absorption and radiation of the outer surface by adjusting the thermal radiation property of the surface of the object, thereby achieving the purpose of controlling the temperature of the object. The two most important parameters are solar absorptance and solar absorptance.
With the development of the demands of miniaturization, high integration and function diversification of the spacecraft in the future, higher requirements are put forward on the thermal control performance indexes of the thermal control coating on the surfaces of the spacecraft and related equipment. The thermal control coating must achieve the requirements of precise temperature control, long service life, high performance and the like. Meanwhile, aiming at different space environments and spacecraft index requirements, the thermal control performance of the thermal control coating needs to be flexibly changed.
At present, thermal control coatings used by domestic spacecrafts mainly comprise: organic white paint, black paint, OSR, a chemical oxide film, an aluminum alloy anodic oxide layer and the like, but the solar absorptance can only meet the requirements of lower solar absorptance and higher solar absorptance, and the solar absorptance of the thermal control coating can not be designed within a certain range.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
In order to solve the technical defects, the invention adopts the technical scheme that a thermal control coating with a designable solar absorptivity is provided, wherein a first coating layer, a second coating layer and a third coating layer are sequentially arranged on the surface of a base material from inside to outside, the first coating layer is a pure aluminum layer, the second coating layer is an aluminum nitride layer, and the third coating layer is an aluminum oxide layer.
Preferably, the base material is an aluminum alloy base, and the thickness of the first coating is 0 nm-300 nm; the thickness of the first coating is 0 nm-250 nm; the thickness of the third plating layer is 0 nm-20 nm, and the solar absorptivity of the thermal control coating is 0.10-0.92.
Preferably, the base material is polyimide, and the thickness of the first coating is 0 nm-300 nm; the thickness of the first coating is 0 nm-250 nm; the thickness of the third coating is 0 nm-20 nm, and the solar absorptivity of the thermal control coating is 0.10-0.90.
Preferably, the thickness of the first layer coating is not less than 100 nm.
Preferably, in the method for preparing the thermal control coating with a programmable solar absorptivity, the first plating layer, the second plating layer and the third plating layer are prepared by vacuum coating.
Preferably, the process parameters of the first layer of plating layer plating are as follows: vacuum degree of 6X 10-1Pa~8×10-1Pa; the air inflow of the argon is 120sccm, and the voltage is 550V; the current is 3A; the sputtering time was 500 s.
Preferably, the plating process parameters of the second plating layer are as follows: vacuum degree of 6X 10-1Pa~8×10-1Pa; the air inflow of argon is 120 sccm; the nitrogen gas inflow is 45 sccm; the voltage is 550V; the current is 3A; the sputtering time was 250 s.
Preferably, the plating process parameters of the third plating layer are as follows: vacuum degree of 6X 10-1Pa~8×10-1Pa; the air inflow of argon is 120 sccm; the power was 1200W and the sputtering time was 400 s.
Compared with the prior art, the invention has the beneficial effects that: 1, the thermal control coating prepared on the surface of the aluminum alloy substrate by the preparation method of the invention, and the solar absorptivity of the thermal control coating can be adjusted within the range of 0.10 to 0.92 by designing the thickness of a coating film layer; 2, the thermal control coating prepared on the surface of the polyimide substrate by the preparation method of the invention has the solar absorptivity capable of being adjusted within the range of 0.10 to 0.90 by designing the thickness of the coating film layer; 3, the composite thermal control coating prepared by the preparation method has good performance of resisting space atomic oxygen, protons, electrons and ultraviolet radiation. After space atomic oxygen, proton, electron and ultraviolet irradiation tests, the solar absorptivity index of the thermal control coating does not change more than 0.02; 4, the substrate material of the method can be popularized to metal, plastic, ceramic or composite materials.
Drawings
FIG. 1 is a schematic perspective view of the solar absorptance programmable thermal control coating;
FIG. 2 is a graph of solar absorptance versus aluminum nitride layer thickness for different substrate surfaces;
FIG. 3 is a sample object diagram according to the first embodiment, the second embodiment and the third embodiment;
FIG. 4 is a scanning electron microscope image of the surface morphology of the samples of the first, second, and third embodiments.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
As shown in fig. 1, fig. 1 is a schematic perspective view of the solar absorptance programmable thermal control coating; the invention relates to a preparation method of a thermal control coating with designable solar absorptivity, which is characterized in that a composite film system structure is designed, and a first plating layer on the surface of a substrate is a pure aluminum layer and is used as a low-absorptivity metal layer; the second coating is an aluminum nitride layer and is used as a high-absorptivity ceramic layer; the third layer is an alumina layer as a protective layer and an antireflection layer.
The preparation method of the thermal control coating with the designable solar absorptivity is characterized by comprising the following steps of: the adopted vacuum coating equipment is vacuum equipment capable of ionizing the target into plasma, and the preferred equipment is vacuum magnetron sputtering equipment or ion beam reactive sputtering equipment.
According to the preparation method of the thermal control coating with the designable solar absorptivity, for an aluminum alloy substrate, a first pure aluminum layer is plated to be 0-300 nm in thickness; the second aluminum nitride layer is plated to a thickness of 0nm to 250 nm; the third alumina layer is plated to a thickness of 0nm to 20 nm; the solar absorptivity of the thermal control coating prepared on the surface of the aluminum alloy material through plating thickness adjustment can be designed from 0.10 to 0.92.
The preparation method of the thermal control coating with the designable solar absorptivity comprises the steps of coating a first pure aluminum layer on a polyimide substrate to a thickness of 0-300 nm; the second aluminum nitride layer is plated to a thickness of 0nm to 250 nm; the third alumina layer is plated to a thickness of 0nm to 20 nm; the solar absorptivity of the thermal control coating prepared on the surface of the polyimide material through plating thickness adjustment can be designed from 0.10 to 0.90.
The composite thermal control coating prepared by the thermal control coating preparation method with the designable solar absorptivity can resist the irradiation environment of space atomic oxygen, protons, electrons and ultraviolet rays. After space atomic oxygen, proton, electron and ultraviolet irradiation tests, the solar absorptivity index of the thermal control coating does not change more than 0.02.
The metal ceramic composite coating is an aluminum layer-aluminum nitride layer-aluminum oxide layer. As the volume fraction of metal particles in the material increases, the film properties change from insulating to metallic, and the refractive index and extinction coefficient also change in a gradient manner. Therefore, the composite coating can optimize the selectivity of the coating by selecting proper film thickness, particle concentration, particle shape and size. The metal ceramic composite absorption coating mainly comprises an antireflection layer (aluminum oxide plays a role in antireflection of sunlight) on the outermost layer, a metal infrared reflection layer (aluminum layer plays a role in high reflection of long-wavelength infrared light) on the bottommost layer and an absorption layer (aluminum nitride) in the middle. The metal ceramic composite absorption coating uses the multilayer gradual change type and the principle of destructive interference of light for reference, and can obtain higher solar absorptivity along with the increase of the thickness of the middle absorption layer.
The equipment and materials used in the following examples: one magnetron sputtering deposition device; metallic aluminum target (99%); nitrogen (purity: 99.999%); oxygen (purity: 99.999%); argon (purity: 99.999%).
The thickness of the pure aluminum layer plated on the first layer on the surface of the polyimide and aluminum alloy substrate cannot be lower than 100nm, otherwise the adjustment of low solar absorptivity (less than 0.14) cannot be realized.
As shown in fig. 2, fig. 2 is a graph of solar absorptance versus aluminum nitride layer thickness for different substrate surfaces.
The invention establishes the correlation between the solar absorptivity of different base material surfaces and the thickness of the aluminum nitride layer through a large amount of experimental data. When the thickness of the first pure aluminum layer is 100nm and the thickness of the third alumina layer is 10nm, the thickness of the AlN film layer and the solar absorptivity of the sample piece are governed as shown in the following table.
AlN thickness (nm) Polyimide sample solar absorptivity Solar absorptivity of aluminum alloy sample
0 0.11 0.1
10 0.23 0.31
20 0.43 0.51
40 0.59 0.62
60 0.69 0.72
80 0.75 0.8
100 0.81 0.85
120 0.85 0.89
140 0.87 0.9
160 0.89 0.91
180 0.9 0.92
200 0.9 0.92
Example one
And (3) placing the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) into magnetron sputtering deposition equipment for film coating. Wherein the thickness of the first pure aluminum layer is 100nm, the thickness of the second aluminum nitride layer is 0nm, and the thickness of the third aluminum oxide layer is 10 nm.
The aluminum layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas is fed into the furnace at 120sccm and the voltage is 550V; current 3A; the sputtering time was 500 s. In this example, the aluminum nitride layer was not plated. The aluminum oxide plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; power 1200W, sputtering time 10 s.
Thermal radiation performance index test
Example a test piece solar absorptance test results are given in the following table:
numbering Polyimide sample solar absorptivity Solar absorptivity of aluminum alloy sample
1 0.11 0.10
2 0.11 0.10
3 0.10 0.11
4 0.10 0.10
5 0.10 0.11
After the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) are subjected to space atomic oxygen, proton, electron and ultraviolet irradiation tests, the solar absorptivity index change of the thermal control coating does not exceed 0.02.
Example two
And (3) placing the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) into magnetron sputtering deposition equipment for film coating. Wherein the thickness of the first pure aluminum layer is 100nm, the thickness of the second aluminum nitride layer is 10nm, and the thickness of the third aluminum oxide layer is 10 nm.
The aluminum layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas is fed into the furnace at 120sccm and the voltage is 550V; current 3A; the sputtering time was 500 s. The aluminum nitride layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; the nitrogen gas inflow is 45 sccm; the voltage is 550V; current 3A; the sputtering time was 250 s. The aluminum oxide plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; power 1200W, sputtering time 400 s.
Thermal radiation performance index test
Example two test pieces solar absorptance test results are given in the following table:
numbering Polyimide sample solar absorptivity Solar absorptivity of aluminum alloy sample
1 0.25 0.34
2 0.26 0.33
3 0.24 0.32
4 0.25 0.33
5 0.27 0.34
After the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) are subjected to space atomic oxygen, proton, electron and ultraviolet irradiation tests, the solar absorptivity index change of the thermal control coating does not exceed 0.02.
EXAMPLE III
And (3) placing the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) into magnetron sputtering deposition equipment for film coating. Wherein the thickness of the first pure aluminum layer is 100nm, the thickness of the second aluminum nitride layer is 80nm, and the thickness of the third aluminum oxide layer is 10 nm.
The aluminum layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas is fed into the furnace at 120sccm and the voltage is 550V; current 3A; the sputtering time was 500 s. The aluminum nitride layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; the nitrogen gas inflow is 45 sccm; the voltage is 550V; current 3A; the sputtering time was 500 s. The aluminum oxide plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; power 1200W, sputtering time 400 s.
Thermal radiation performance index test
Example three test pieces solar absorptance test results are given in the following table:
numbering Polyimide sample solar absorptivity Solar absorptivity of aluminum alloy sample
1 0.75 0.80
2 0.74 0.80
3 0.76 0.82
4 0.75 0.81
5 0.74 0.79
After the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) are subjected to space atomic oxygen, proton, electron and ultraviolet irradiation tests, the solar absorptivity index change of the thermal control coating does not exceed 0.02.
As shown in fig. 3 and 4, (a) in fig. 3 is a sample object diagram of the first embodiment, (b) is a sample object diagram of the second embodiment, and (c) is a sample object diagram of the third embodiment; FIG. 4 is a scanning electron microscope image of the surface morphology of the sample of example one (a), a scanning electron microscope image of the surface morphology of the sample of example two (b), and a scanning electron microscope image of the surface morphology of the sample of example three (c).
Example four
And (3) placing the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) into magnetron sputtering deposition equipment for film coating. Wherein the thickness of the first pure aluminum layer is 100nm, the thickness of the second aluminum nitride layer is 160nm, and the thickness of the third aluminum oxide layer is 10 nm.
The aluminum layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas is fed into the furnace at 120sccm and the voltage is 550V; current 3A; the sputtering time was 500 s. The aluminum nitride layer plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; the nitrogen gas inflow is 45 sccm; the voltage is 550V; current 3A; the sputtering time is 1250 s. The aluminum oxide plating process parameters are as follows: degree of vacuum of 6X 10-1Pa~8×10-1Pa; the argon gas inflow is 120 sccm; power 1200W, sputtering time 400 s.
Thermal radiation performance index test
Example four test pieces solar absorptance test results are given in the following table:
numbering Polyimide sample solar absorptivity Solar absorptivity of aluminum alloy sample
1 0.90 0.92
2 0.88 0.91
3 0.91 0.93
4 0.89 0.90
5 0.89 0.92
After the aluminum alloy test piece (5 pieces) and the polyimide test piece (5 pieces) are subjected to space atomic oxygen, proton, electron and ultraviolet irradiation tests, the solar absorptivity index change of the thermal control coating does not exceed 0.02.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (8)

1. The utility model provides a thermal control coating that solar absorptivity designable, its characterized in that sets gradually first layer cladding material, second floor cladding material and third layer cladding material from inside to outside at the substrate surface, first layer cladding material is pure aluminium layer, the second floor cladding material is the aluminium nitride layer, third layer cladding material is the aluminium oxide layer.
2. The solar absorptance programmable thermal control coating of claim 1, wherein the substrate is an aluminum alloy based, and the first layer is from 0nm to 300nm thick; the thickness of the first coating is 0 nm-250 nm; the thickness of the third plating layer is 0 nm-20 nm, and the solar absorptivity of the thermal control coating is 0.10-0.92.
3. The solar absorptance programmable thermal control coating of claim 1, wherein the substrate is polyimide, and the first layer is deposited to a thickness of 0nm to 300 nm; the thickness of the first coating is 0 nm-250 nm; the thickness of the third coating is 0 nm-20 nm, and the solar absorptivity of the thermal control coating is 0.10-0.90.
4. The solar absorptance programmable thermal control coating of claim 2 or 3, wherein the first layer is deposited to a thickness of no less than 100 nm.
5. A method for producing a solar absorptance programmable thermal control coating according to any one of claims 1-3, wherein the first, second and third coating layers are vacuum coated.
6. The method of claim 5, wherein the first layer plating layer is plated according to the following process parameters: vacuum degree of 6X 10-1Pa~8×10-1Pa; the air inflow of the argon is 120sccm, and the voltage is 550V; the current is 3A; the sputtering time was 500 s.
7. The method of claim 5, wherein the second plating layer has plating process parameters of: vacuum degree of 6X 10-1Pa~8×10-1Pa; the air inflow of argon is 120 sccm; the nitrogen gas inflow is 45 sccm; the voltage is 550V; the current is 3A; the sputtering time was 250 s.
8. The method of claim 5, wherein the third plating layer has plating process parameters of: vacuum degree of 6X 10-1Pa~8×10-1Pa; the air inflow of argon is 120 sccm; the power was 1200W and the sputtering time was 400 s.
CN202010950599.0A 2020-09-10 2020-09-10 Thermal control coating with designable solar absorptivity and preparation method thereof Pending CN111996491A (en)

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CN112899632A (en) * 2021-05-07 2021-06-04 上海陛通半导体能源科技股份有限公司 Vacuum coating process equipment and method capable of realizing convenient temperature control
CN112899632B (en) * 2021-05-07 2021-12-28 上海陛通半导体能源科技股份有限公司 Vacuum coating process equipment and method capable of realizing convenient temperature control
CN114192363A (en) * 2021-12-23 2022-03-18 上海卫星装备研究所 Preparation method and system of solar absorption ratio adjustable thermal control coating and heat insulation assembly

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Application publication date: 20201127