A coupled ion beam preparation device and method for antigen-antigen oxygen polymer composite film

By using coupled ion beam preparation equipment and methods, the degradation problem of polymer films caused by atomic oxygen corrosion in the low-Earth orbit space environment was solved. The prepared composite film has high adhesion strength and flexibility, which improves the service life of the material.

CN119736600BActive Publication Date: 2025-10-03BEIJING SCI & TECH PATENT OFFICE
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Patent Information

Application Number
CN202411919978.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-25
Publication Date
2025-10-03
Estimated Expiration
2044-12-25

AI Technical Summary

Technical Problem

Existing polymer film materials suffer from degradation and failure due to atomic oxygen corrosion in the low-Earth orbit space environment, especially material mass loss, increased surface roughness, and macroscopic gloss loss, discoloration, and powdering. Existing protection strategies are difficult to strike a balance between maintaining material performance and environmental stability.

Method used

Using a coupled ion beam preparation device, Hall ion source etching, MEVVA ion implantation, magnetic filtered cathode vacuum arc deposition and high-power pulsed magnetron sputtering deposition technology, composite films resistant to antigenic oxygen are prepared on polymer substrates to achieve interface structure regulation and film layer design.

Benefits of technology

The prepared composite film has excellent interface adhesion strength and membrane-base synergistic deformation ability, which effectively alleviates film cracking caused by space debris collisions and hot and cold cycles, and improves the service life of polymer components.

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Abstract

The present invention discloses a coupled ion beam preparation device and method for an antigen-antigen oxygen polymer composite film. The device comprises a winding and unwinding system, a Hall ion source etching system, a MEVVA ion implantation system, a magnetically filtered cathode vacuum arc deposition system, and a high-power pulsed magnetron sputtering deposition system. The systems are connected via oxygen-free copper O-rings. The polymer film substrate is transported within the device, and the prepared composite film layer structure is shown in Figure 1. The composite film prepared using this technology exhibits excellent interfacial adhesion strength and film-substrate cooperative deformation capability, effectively alleviating AO erosion and degradation induced by cracking of the protective film caused by space debris collisions and thermal cycling, significantly improving the service life of polymer components.
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Description

Technical Field

[0001] The present invention relates to the technical field of polymer surface / interface modification, and more particularly to a coupled ion beam preparation device and method for an antigen-oxidation polymer composite film. Background Art

[0002] Kapton-type polyimide films have excellent thermal stability, mechanical properties, corrosion resistance, dielectric properties, radiation resistance, heat and flame retardancy, and biocompatibility. They have been successfully used in spacecraft thermal control systems and flexible solar cell arrays. However, the low-Earth orbit space environment, 200-700 km above the Earth's surface, is harsh and complex. In particular, the atomic oxygen erosion effect can directly lead to the degradation and failure of polymer film materials. AO has high reactivity and intrinsic kinetic energy, which can directly break the polymer backbone and cause oxidation reactions, releasing volatile small molecular products. The release of these volatile products from the polymer surface directly causes material quality loss, increased surface roughness, and macroscopic loss of gloss, discoloration, and powdering, which significantly reduces material stability.

[0003] Currently, single polymer film materials with excellent performance are unable to meet the requirements of service in harsh operating conditions. The development of new polymer films is complex and requires significant time and financial investment. To alleviate the damage problem of polymer films, researchers have constructed protective barriers on polymer surfaces through coating or vapor deposition to achieve the preparation of high-performance flexible composite films. This has been proven to be an effective means of improving the service stability of polymer films in space environments.

[0004] Flexible composite film preparation technologies are mainly divided into wet chemical method, thermoforming method and vapor deposition method. However, at this stage, organic protective films prepared based on wet chemical method or thermoforming method may have problems such as low film density (micro defects and micro holes), easy aging and falling off in coupling environment, and pollution of optoelectronic facilities. Inorganic protective films prepared based on traditional vapor deposition technology may have problems such as poor film base adhesion strength, large differences in flexibility and thermal expansion coefficient. Long-term service in a space environment may cause the protective film to crack, delaminate or even fall off, ultimately leading to failure of the polymer matrix. The protection strategies currently developed by the mainstream single vapor deposition technology are mainly divided into bulk material modification method and composite film protection method.

[0005] The bulk modification method is to change the molecular structure of the polymer material by doping it with specific element groups or nanoparticles, thereby enhancing the environmental stability of the polymer matrix. Its protection mechanism is that the modified polymer material grows an inert layer in situ on the surface when exposed to extreme environments to prevent further degradation of the material. The advantage of the bulk modification method is that in the process of introducing protective groups into the polymer molecular skeleton, the chelation effect provides a strong chemical bond between the two, which overcomes some of the shortcomings of the composite film protection method, namely stress-induced film cracking, delamination and even shedding during service. However, the bulk modification method is difficult to strike a balance between improving the environmental stability of polymer materials and maintaining their initial performance.

[0006] Composite thin film protection involves depositing an inert thin film material onto a polymer substrate using a specific film-forming technique to isolate the device from extreme environments. Depending on the deposition method and the film material used, this technology is categorized into organic and inorganic thin film protection methods.

[0007] The organic thin film protection method mainly uses plasma polymerization, hot pressing or coating to prepare a flexible precursor organic thin film on the polymer surface. Since the physical and chemical properties of the organic film are similar to those of the polymer substrate and the thermal expansion coefficient is close, it solves the shortcomings of inorganic thin films that are easy to crack and has good interfacial adhesion. At present, organic thin films still face many problems. The coupling effect of AO and ultraviolet radiation may cause the film to age and fall off. These organosilicon materials may also produce darker deposits when they serve in this coupled environment for a long time, thereby contaminating nearby optical instruments and reflectors in solar power generation systems. In addition, due to the influence of the coating process, a large number of small holes may be introduced in the preparation process of the organic film, thereby causing corrosion of the polymer substrate.

[0008] Inorganic thin film protection methods primarily utilize deposition techniques such as sol-gel, magnetron sputtering, evaporation, liquid phase deposition, and ALD to deposit metal or non-volatile oxide films on polymer surfaces. Currently, inorganic thin film protection methods face the following three main challenges. First, micro-defects and micro-voids are inevitably introduced during the thin film deposition process. Furthermore, inorganic thin films are subject to their poor flexibility, and collisions with orbiting space debris or micrometeoroids may cause the film to crack or even penetrate. Furthermore, the large difference in thermal expansion coefficients between the inorganic thin film and the polymer substrate can easily cause the film to crack, delaminate, or even fall off under the coupled effects of AO erosion and thermal cycling. Because AO is extremely sensitive to surface defects in thin films, these defects become channels for AO to diffuse inward, ultimately leading to erosion and degradation of the polymer substrate. Customized control of composite thin films through interface construction with the polymer substrate is difficult to achieve. Summary of the Invention

[0009] In light of this, the present invention provides a coupled ion beam fabrication apparatus and method for producing an anti-oxidant-oxygen polymer composite film. The composite film produced using this technology exhibits excellent interfacial adhesion strength and membrane-substrate synergistic deformation capability. This effectively mitigates AO erosion degradation caused by cracking of protective films due to space debris collisions and thermal cycling, significantly extending the service life of polymer components. The resulting composite film can be used in the field of aerospace composite film materials.

[0010] In order to achieve the above object, the present invention adopts the following technical solutions:

[0011] A coupled ion beam preparation device for an antigen-antigen oxygen polymer composite film, comprising:

[0012] a vacuum chamber, a first guide chamber, a first isolation chamber, a second guide chamber, a second isolation chamber, a third guide chamber, and a third isolation chamber;

[0013] Wherein, the vacuum chamber, the first guide chamber, the first isolation chamber, the second guide chamber, the second isolation chamber, the third guide chamber and the third isolation chamber are connected in sequence through oxygen-free copper O-rings;

[0014] The vacuum chamber is provided with a first unwinding roller, a second unwinding roller, a third unwinding roller and a Hall ion source etching system, wherein the first unwinding roller and the second unwinding roller are arranged vertically; the third unwinding roller is arranged on one side below the two unwinding rollers and is higher than the first unwinding roller; the Hall ion source etching system is arranged between the second unwinding roller and the third unwinding roller;

[0015] A first guide roller and a second guide roller are provided in the first guide chamber, the first guide roller is arranged parallel to the third unwinding roller, and the second guide roller is arranged above the first guide roller.

[0016] A fourth unwinding roller, a fifth unwinding roller and a MEVVA ion implantation system are provided in the first isolation chamber, wherein the fourth unwinding roller is arranged parallel to the second guide roller, and the fifth unwinding roller is arranged on one side below the fourth guide roller; the MEVVA ion implantation system is arranged between the fourth unwinding roller and the fifth unwinding roller;

[0017] A third guide roller and a fourth guide roller are provided in the second guide chamber, the third guide roller is arranged parallel to the fifth unwinding roller, and the fourth guide roller is arranged on one side above the third guide roller;

[0018] A sixth unwinding roller, a seventh unwinding roller, and a magnetic filtration cathode vacuum arc deposition system are provided in the second isolation chamber, wherein the sixth unwinding roller is arranged parallel to the fourth guide roller, and the seventh unwinding roller is arranged on one side below the sixth unwinding roller; the magnetic filtration cathode vacuum arc deposition system is arranged between the sixth unwinding roller and the seventh unwinding roller;

[0019] A fifth guide roller and a sixth guide roller are provided in the third guide chamber, the fifth guide roller is arranged parallel to the seventh unwinding roller, and the sixth guide roller is arranged on one side above the fifth guide roller;

[0020] An eighth unwinding roller, a ninth unwinding roller, a tenth unwinding roller and a high-power pulsed magnetron sputtering deposition system are arranged in the third isolation chamber. The eighth unwinding roller is arranged parallel to the sixth guide roller, and the ninth unwinding roller is arranged on the side below the eighth unwinding roller; the tenth unwinding roller is arranged above the eighth unwinding roller and vertically arranged with the ninth unwinding roller; the high-power pulsed magnetron sputtering deposition system is arranged between the eighth unwinding roller and the ninth unwinding roller.

[0021] Preferably, molecular pumps are provided on the outer tops and outer bottoms of the vacuum chamber, the first isolation chamber, the second isolation chamber, and the third isolation chamber.

[0022] Preferably, the side wall of the vacuum chamber is provided with an observation window.

[0023] Preferably, the first isolation chamber, the second isolation chamber and the third isolation chamber are all provided with heating components and cryogenic systems; wherein the heating components and cryogenic systems in the first isolation chamber are arranged at the top, and the heating components and cryogenic systems in the second isolation chamber and the third isolation chamber are arranged at the bottom.

[0024] Another object of the present invention is to provide a method for preparing an antigen-antigen oxygen polymer composite film by coupled ion beam, using the above-mentioned device, and the specific steps are as follows:

[0025] S01 Unwinding

[0026] The polymer is degassed in an oven, placed in a vacuum chamber, and the unwinding process begins;

[0027] S02 Hall ion source etching system

[0028] Use Hall ion source system to perform low energy and large beam current etching on polymer substrates;

[0029] S03 MEVVA ion implantation system

[0030] The polymer matrix is ​​implanted with low-energy, high-current metal ions using the MEVVA ion implantation system. After implantation, the metal element content in the subsurface layer within 30 nm is not less than 3%, and the defect density is not less than 10 16 cm -3 ;

[0031] S04 Magnetic Filtered Cathodic Vacuum Arc Deposition System

[0032] A magnetic filtered cathode vacuum arc deposition system is used to deposit an alloy buffer layer on a polymer matrix. Arc discharge is used to regulate the plasma transport through a magnetic field. The arc spot movement rate and range are controlled by a pulsed magnetic field.

[0033] The introduction of a pulsed magnetic field can significantly increase the area and movement rate of the arc spot on the cathode target. The plasma generated during the arc spot movement is more uniform; the effective area of ​​the magnetic filtration plasma drawn by a single magnetic filtration system can be increased by 2-3 times to 350mm.

[0034] S05 high power pulsed magnetron sputtering deposition system

[0035] The oxide barrier layer was deposited using a high-power pulsed magnetron sputtering deposition system. A high-density plasma (peak current density of 10 17 -10 19 Am -2 ); The extremely high current density promotes the collision process between electrons and target atoms, thereby significantly enhancing the target ionization rate (>70%);

[0036] S06 Rolling

[0037] After the treatment is completed, the polymer is wound up for treatment.

[0038] The present invention achieves surface and interface structure control of polymer substrates and film layer structure design by coupling the advantages of four ion beam technologies to solve key technical bottlenecks such as poor adhesion of the membrane base and easy cracking of inorganic films, thereby greatly improving the AO corrosion resistance of the composite film in complex space environments.

[0039] Preferably, the degassing temperature in step S01 is 60-120°C.

[0040] Preferably, the parameters of the Hall ion source etching system in step S02 include: surface etching beam current 500-2000mA, voltage 200-500V; cleaning temperature 20-40°C, etching speed 2-10m·min -1 , the surface roughness after etching is between 100-300nm.

[0041] Preferably, the MEVVA ion implantation system parameters in step S03 include: ion energy 7-30keV, beam current intensity 3-10mA; processing speed 2-10m·min -1 The treatment dose was 5×10 15 -1×10 16 atoms cm -2 .

[0042] Preferably, the parameters of the magnetic filtered cathode vacuum arc deposition system in step S04 include: arc discharge current 80-120A, pulse current 5-30A, pulse frequency 10-100Hz; deposition thickness 10-30nm, and deposited metal CuNi or NiCr.

[0043] Preferably, the high-power pulsed magnetron sputtering deposition system parameters in step S05 include: pulse power 2-5kW, pulse width 20-50μs, modulation pulse frequency 800-1000Hz; deposition thickness is 200nm, deposition structure is equiaxed crystal structure, and deposition metal is Al2O3, Cr2O3 or ZnO.

[0044] It can be seen from the above technical solutions that compared with the prior art, the present invention has the following beneficial effects:

[0045] 1. The prepared composite film has good AO resistance and the erosion rate can be as low as 5×10 -26 cm 3 atom -1 (Land-based atomic oxygen exposure test);

[0046] 2. The prepared composite film has high interface adhesion strength, greater than 1.5N mm -1 (45° peel test);

[0047] 3. The prepared composite film has good flexibility and the residual stress is less than -100MPa (the residual stress is calculated by the film curvature radius);

[0048] 4. The preparation temperature is less than 50°C, and the film density is high (the bulk density is calculated by the film refractive index);

[0049] 5. High preparation efficiency, low cost, and travel speed of 2-10m·min -1 . BRIEF DESCRIPTION OF THE DRAWINGS

[0050] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are merely embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0051] Figure 1 Schematic diagram of the composite film structure prepared by the present invention;

[0052] Figure 2 Schematic diagram of the coupled ion beam preparation device of the present invention;

[0053] Figure 3This is a flow chart for preparing the composite film of the present invention;

[0054] in, Figure 1 middle:

[0055] 101- low stress oxide protective layer; 102- flexible alloy buffer layer; 103- Ni ion pinning mixed layer; 104- polymer matrix;

[0056] Figure 2 middle:

[0057] 201-Observation window; 2021-First unwinding roller; 2022-Second unwinding roller; 2023-Third unwinding roller; 2024-Fourth unwinding roller; 2025-Fifth unwinding roller; 2026-Sixth unwinding roller; 2027-Seventh unwinding roller; 2028-Eighth unwinding roller; 2029-Ninth unwinding roller; 2030-Tenth unwinding roller; 203-Molecular pump; 204-Hall ion source etching system; 2051-First guide roller; 2052-Second guide roller; 2053-Third guide roller Roller; 2054-fourth guide roller; 2055-fifth guide roller; 2056-sixth guide roller; 206-MEVVA ion implantation system; 207-magnetic filtered cathode vacuum arc deposition system; 208-high power pulsed magnetron sputtering deposition system; 209-heating assembly; 210-deep cooling system; 211-vacuum chamber; 212-first isolation chamber; 213-second isolation chamber; 214-third isolation chamber; 215-first guide chamber; 216-second guide chamber; 217-third guide chamber. DETAILED DESCRIPTION

[0058] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0059] Example 1

[0060] This embodiment provides a coupled ion beam preparation device for an antigen-antigen oxygen polymer composite film, comprising:

[0061] Vacuum chamber 211, first guide chamber 215, first isolation chamber 212, second guide chamber 216, second isolation chamber 213, third guide chamber 217 and third isolation chamber 214;

[0062] Among them, the vacuum chamber 211, the first guide chamber 215, the first isolation chamber 212, the second guide chamber 216, the second isolation chamber 213, the third guide chamber 217 and the third isolation chamber 214 are connected in sequence through oxygen-free copper O-rings;

[0063] A first unwinding roller 2021, a second unwinding roller 2022, a third unwinding roller 2023, and a Hall ion source etching system 204 are provided in the vacuum chamber 211. The first unwinding roller 2021 and the second unwinding roller 2022 are arranged vertically; the third unwinding roller 2022 is provided below the second unwinding roller 2022 and is higher than the first unwinding roller 2021; the Hall ion source etching system 204 is provided between the second unwinding roller 2022 and the third unwinding roller 2023;

[0064] A first guide roller 2051 and a second guide roller 2052 are provided in the first guide chamber 215. The first guide roller 2051 is provided in parallel with the third unwinding roller 2023. The second guide roller 2052 is provided above the first guide roller 2051.

[0065] A fourth unwinding roller 2024, a fifth unwinding roller 2025, and a MEVVA ion implantation system 206 are provided in the first isolation chamber 212. The fourth unwinding roller 2024 is provided in parallel with the second guide roller 2052, and the fifth unwinding roller 2025 is provided below the fourth guide roller 2054. The MEVVA ion implantation system 206 is provided between the fourth unwinding roller 2024 and the fifth unwinding roller 2025.

[0066] A third guide roller 2053 and a fourth guide roller 2054 are provided in the second guide chamber 216. The third guide roller 2053 is provided in parallel with the fifth unwinding roller 2024. The fourth guide roller 2054 is provided above the third guide roller 2023.

[0067] The second isolation chamber 213 is provided with a sixth unwinding roller 2026, a seventh unwinding roller 2027, and a magnetic filtration cathode vacuum arc deposition system 207. The sixth unwinding roller 2026 is arranged parallel to the fourth guide roller 2054, and the seventh unwinding roller 2027 is arranged below the sixth unwinding roller 2026. The magnetic filtration cathode vacuum arc deposition system 207 is arranged between the sixth unwinding roller 2026 and the seventh unwinding roller 2027.

[0068] A fifth guide roller 2055 and a sixth guide roller 2056 are provided in the third guide chamber 217. The fifth guide roller 2055 is provided in parallel with the seventh unwinding roller 2027. The sixth guide roller 2056 is provided above the fifth guide roller 2055.

[0069] The third isolation chamber 214 is provided with an eighth unwinding roller 2028, a ninth unwinding roller 2029, a tenth unwinding roller 2010 and a high-power pulsed magnetron sputtering deposition system 208. The eighth unwinding roller 2028 is arranged parallel to the sixth guide roller 2056, and the ninth unwinding roller 2029 is arranged on the side below the eighth unwinding roller 2028; the tenth unwinding roller 2010 is arranged above the eighth unwinding roller 2028 and is arranged vertically with the ninth unwinding roller 2029; the high-power pulsed magnetron sputtering deposition system 208 is arranged between the eighth unwinding roller 2028 and the ninth unwinding roller 2029.

[0070] In this embodiment, molecular pumps 203 are provided on the outer tops and outer bottoms of the vacuum chamber 211 , the first isolation chamber 212 , the second isolation chamber 213 , and the third isolation chamber 214 .

[0071] An observation window 201 is provided on the side wall of the vacuum chamber 211 .

[0072] The first isolation chamber 211, the second isolation chamber 212 and the third isolation chamber 213 are all equipped with a heating component 209 and a cryogenic system 210; the heating component 209 and the cryogenic system 210 in the first isolation chamber 211 are arranged at the top, and the heating component 209 and the cryogenic system 210 in the second isolation chamber 212 and the third isolation chamber 213 are arranged at the bottom.

[0073] Example 2

[0074] This embodiment provides a coupled ion beam preparation method for an antigen-oxygen polymer composite film, comprising the following steps:

[0075] S01 Unwinding

[0076] The polymer was degassed in an oven at 80°C, placed in a vacuum chamber, and unwinding was started;

[0077] S02 Hall ion source etching;

[0078] The polymer substrate was etched with a Hall ion source system using a low-energy, high-beam current. The surface etching beam current was 1000 mA and the voltage was 300 V. The cleaning temperature was 35°C and the etching speed was 6 m / min. -1 , the surface roughness after etching is 150nm.

[0079] S03 MEVVA ion implantation;

[0080] Low-energy, high-current Ni ion implantation was performed on the polymer matrix using the MEVVA ion implantation system; the ion energy was 9 keV, the beam current was 4.5 mA, and the processing speed was 4.5 m / min. -1 The treatment dose was 6×10 15 atoms cm -2, the Ni content of the subsurface layer within 30nm after injection is 3.8%, and the defect density is about 10 16 cm -3 ;

[0081] S04 magnetic filtered cathode vacuum arc deposition;

[0082] The NiCr alloy buffer layer was deposited on the polymer matrix using a magnetic filtered cathode vacuum arc deposition system with an arc discharge current of 100A, a pulse current of 25A, a pulse frequency of 80Hz, and a processing speed of 4.0mmin. -1 The deposition thickness is 25 nm, and the interfacial adhesion strength between NiCr and polymer substrate is about 1.6 N mm by 45° peel test. -1 ;

[0083] S05 high power pulsed magnetron sputtering deposition;

[0084] The Al2O3 barrier layer was deposited using a high-power pulsed magnetron sputtering deposition system with a pulse power of 4kW, a pulse width of 40μs, a modulation pulse frequency of 900Hz, and a processing speed of 4.0mmin. -1 The deposition thickness is 200 nm, the film structure is an equiaxed crystal structure, the residual stress of the film is calculated to be -85 MPa by the radius of curvature method, and the film packing density is measured by ellipsometry to be 0.9788;

[0085] S06 Rolling

[0086] After the treatment, the polymer was rolled up and the AO erosion rate of the composite film was measured by land-based atomic oxygen exposure test to be 6.69×10 -26 cm 3 atom -1 .

[0087] Example 3

[0088] This embodiment provides a coupled ion beam preparation method for an antigen-oxygen polymer composite film, comprising the following steps:

[0089] S01 Unwinding

[0090] The polymer was degassed in an oven at 80°C, placed in a vacuum chamber, and unwinding was started;

[0091] S02 Hall ion source etching;

[0092] The polymer substrate was etched with a Hall ion source system using a low-energy, high-beam current. The surface etching beam current was 1000 mA and the voltage was 300 V. The cleaning temperature was 35°C and the etching speed was 6 m / min. -1 , the surface roughness after etching is 150nm.

[0093] S03 MEVVA ion implantation;

[0094] Low-energy, high-current Ni ion implantation was performed on the polymer matrix using the MEVVA ion implantation system; the ion energy was 9 keV, the beam current was 4.5 mA, and the processing speed was 4.5 m / min. -1 , the treatment dose is 10 16 atoms cm -2 After injection, the Ni content in the subsurface layer within 30 nm is 6.3%, and the defect density is about 1.7×10 16 cm -3 ;

[0095] S04 magnetic filtered cathode vacuum arc deposition;

[0096] The NiCr alloy buffer layer was deposited on the polymer matrix using a magnetic filtered cathode vacuum arc deposition system with an arc discharge current of 100A, a pulse current of 25A, a pulse frequency of 80Hz, and a processing speed of 4.0mmin. -1 The deposition thickness is 25 nm, and the interfacial adhesion strength between NiCr and polymer substrate is about 1.8 N mm by 45° peel test. -1 ;

[0097] S05 high power pulsed magnetron sputtering deposition;

[0098] The Al2O3 barrier layer was deposited using a high-power pulsed magnetron sputtering deposition system with a pulse power of 4kW, a pulse width of 40μs, a modulation pulse frequency of 900Hz, and a processing speed of 4.0mmin. -1 The deposition thickness is 200 nm, the film structure is an equiaxed crystal structure, the residual stress of the film is calculated to be -67 MPa by the radius of curvature method, and the film packing density is measured by ellipsometry to be 0.9779;

[0099] S06 Rolling

[0100] After the treatment, the polymer was rolled up and the AO erosion rate of the composite film was measured by land-based atomic oxygen exposure test to be 5.38×10 -26 cm 3 atom -1 .

[0101] Example 4

[0102] This embodiment provides a coupled ion beam preparation method for an antigen-oxygen polymer composite film, comprising the following steps:

[0103] S01 Unwinding

[0104] The polymer was degassed in an oven at 80°C, placed in a vacuum chamber, and unwinding was started;

[0105] S02 Hall ion source etching;

[0106] The polymer substrate was etched with a Hall ion source system using a low-energy, high-beam current. The surface etching beam current was 1000 mA and the voltage was 300 V. The cleaning temperature was 35°C and the etching speed was 6 m / min. -1 , the surface roughness after etching is 150nm.

[0107] S03 MEVVA ion implantation;

[0108] Low-energy, high-current Ni ion implantation was performed on the polymer matrix using the MEVVA ion implantation system; the ion energy was 9 keV, the beam current was 4.5 mA, and the processing speed was 4.5 m / min. -1 The treatment dose was 6×10 15 atoms cm -2 , the Ni content of the subsurface layer within 30nm after injection is 3.8%, and the defect density is about 10 16 cm -3 ;

[0109] S04 magnetic filtered cathode vacuum arc deposition;

[0110] The NiCr alloy buffer layer was deposited on the polymer matrix using a magnetic filtered cathode vacuum arc deposition system with an arc discharge current of 100A, a pulse current of 25A, a pulse frequency of 80Hz, and a processing speed of 4.0mmin. -1 The deposition thickness is 25 nm, and the interfacial adhesion strength between NiCr and polymer substrate is about 1.6 N mm by 45° peel test. -1 ;

[0111] S05 high power pulsed magnetron sputtering deposition;

[0112] The Cr2O3 barrier layer was deposited using a high-power pulsed magnetron sputtering deposition system with a pulse power of 4kW, a pulse width of 40μs, a modulation pulse frequency of 800Hz, and a processing speed of 4.0mmin. -1 The deposition thickness is 200 nm, the film structure is an equiaxed crystal structure, the residual stress of the film is calculated to be -92 MPa by the radius of curvature method, and the film packing density is measured by ellipsometry to be 0.9842;

[0113] S06 Rolling

[0114] After the treatment, the polymer was rolled up and the AO erosion rate of the composite film was measured by land-based atomic oxygen exposure test to be 6.28×10 -26 cm 3atom -1 .

[0115] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. Reference can be made to the common and similar parts between the various embodiments. For the devices disclosed in the embodiments, since they correspond to the methods disclosed in the embodiments, the description is relatively simple, and the relevant parts can be referred to the method description.

[0116] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A coupled ion beam preparation device for an antigen-antigen oxygen polymer composite film, characterized in that: include: a vacuum chamber, a first guide chamber, a first isolation chamber, a second guide chamber, a second isolation chamber, a third guide chamber, and a third isolation chamber; Wherein, the vacuum chamber, the first guide chamber, the first isolation chamber, the second guide chamber, the second isolation chamber, the third guide chamber and the third isolation chamber are connected in sequence through oxygen-free copper O-rings; The vacuum chamber is provided with a first unwinding roller, a second unwinding roller, a third unwinding roller and a Hall ion source etching system, wherein the first unwinding roller and the second unwinding roller are arranged vertically; the third unwinding roller is arranged on one side below the two unwinding rollers and is higher than the first unwinding roller; the Hall ion source etching system is arranged between the second unwinding roller and the third unwinding roller; A first guide roller and a second guide roller are provided in the first guide chamber, the first guide roller is arranged parallel to the third unwinding roller, and the second guide roller is arranged above the first guide roller. A fourth unwinding roller, a fifth unwinding roller and a MEVVA ion implantation system are provided in the first isolation chamber, wherein the fourth unwinding roller is arranged parallel to the second guide roller, and the fifth unwinding roller is arranged on one side below the fourth guide roller; the MEVVA ion implantation system is arranged between the fourth unwinding roller and the fifth unwinding roller; A third guide roller and a fourth guide roller are provided in the second guide chamber, the third guide roller is arranged parallel to the fifth unwinding roller, and the fourth guide roller is arranged on one side above the third guide roller; A sixth unwinding roller, a seventh unwinding roller, and a magnetic filtration cathode vacuum arc deposition system are provided in the second isolation chamber, wherein the sixth unwinding roller is arranged parallel to the fourth guide roller, and the seventh unwinding roller is arranged on one side below the sixth unwinding roller; the magnetic filtration cathode vacuum arc deposition system is arranged between the sixth unwinding roller and the seventh unwinding roller; A fifth guide roller and a sixth guide roller are provided in the third guide chamber, the fifth guide roller is arranged parallel to the seventh unwinding roller, and the sixth guide roller is arranged on one side above the fifth guide roller; An eighth unwinding roller, a ninth unwinding roller, a tenth unwinding roller and a high-power pulsed magnetron sputtering deposition system are arranged in the third isolation chamber. The eighth unwinding roller is arranged parallel to the sixth guide roller, and the ninth unwinding roller is arranged on the side below the eighth unwinding roller; the tenth unwinding roller is arranged above the eighth unwinding roller and vertically arranged with the ninth unwinding roller; the high-power pulsed magnetron sputtering deposition system is arranged between the eighth unwinding roller and the ninth unwinding roller.

2. The coupled ion beam preparation device for an antigen-antioxidant polymer composite film according to claim 1, characterized in that: Molecular pumps are provided on the outer tops and outer bottoms of the vacuum chamber, the first isolation chamber, the second isolation chamber and the third isolation chamber.

3. The coupled ion beam preparation device for an antigen-antioxidant polymer composite film according to claim 2, characterized in that: The side wall of the vacuum chamber is provided with an observation window.

4. The coupled ion beam preparation device for an antigen-antioxidant polymer composite film according to claim 3, characterized in that: The first isolation chamber, the second isolation chamber and the third isolation chamber are all provided with a heating component and a cryogenic system; wherein the heating component and the cryogenic system in the first isolation chamber are arranged at the top, and the heating component and the cryogenic system in the second isolation chamber and the third isolation chamber are arranged at the bottom.

5. A method for preparing an antigen-antigen oxygen polymer composite film by coupled ion beam, characterized in that: Using the device described in claim 4, the specific steps are as follows: S01 Unwinding The polymer is degassed in an oven, placed in a vacuum chamber, and the unwinding process begins; S02 Hall ion source etching system Use Hall ion source system to perform low energy and large beam current etching on polymer substrates; S03 MEVVA ion implantation system The polymer matrix is ​​implanted with low-energy, high-current metal ions using the MEVVA ion implantation system. After implantation, the metal element content in the subsurface layer within 30 nm is not less than 3%, and the defect density is not less than 10 16 cm -3 ; S04 Magnetic Filtered Cathodic Vacuum Arc Deposition System A magnetic filtered cathode vacuum arc deposition system is used to deposit an alloy buffer layer on a polymer matrix. Arc discharge is used to regulate the plasma transport through a magnetic field. The arc spot movement rate and range are controlled by a pulsed magnetic field. S05 high power pulsed magnetron sputtering deposition system The oxide barrier layer is deposited using a high-power pulsed magnetron sputtering deposition system. Using glow discharge, a pulsed power supply with a duty cycle of 1%-30% and a discharge time of 10-500μs is used to obtain an extremely high-density plasma. S06 Rolling After the treatment is completed, the polymer is wound up for treatment.

6. The method for preparing an antigen-antiproto-oxygen polymer composite film by coupled ion beam according to claim 5, characterized in that: The degassing temperature in step S01 is 60-120°C.

7. The method for preparing an antigen-antiproto-oxygen polymer composite film by coupled ion beam according to claim 5, characterized in that: The parameters of the Hall ion source etching system in step S02 include: surface etching beam current 500-2000mA, voltage 200-500V; cleaning temperature 20-40℃, etching speed 2-10m·min -1 , the surface roughness after etching is between 100-300nm.

8. The method for preparing an antigen-antiproto-oxygen polymer composite film by coupled ion beam according to claim 5, characterized in that: The MEVVA ion implantation system parameters in step S03 include: ion energy 7-30keV, beam current 3-10mA; processing speed 2-10m·min -1 The treatment dose was 5×10 15 -1×10 16 atoms cm -2 .

9. The method for preparing an antigen-antiproto-oxygen polymer composite film by coupled ion beam according to claim 5, characterized in that: The parameters of the magnetic filtered cathode vacuum arc deposition system in step S04 include: arc discharge current 80-120A, pulse current 5-30A, pulse frequency 10-100Hz; deposition thickness 10-30nm, and deposition metal CuNi or NiCr.

10. The method for preparing an antigen-antioxidant polymer composite film by coupled ion beam according to claim 5, characterized in that: The high power pulsed magnetron sputtering deposition system parameters in step S05 include: The pulse power is 2-5kW, the pulse width is 20-50μs, and the modulation pulse frequency is 800-1000Hz; the deposition thickness is 200nm, the deposition structure is an equiaxed crystal structure, and the deposited metal is Al2O3, Cr2O3 or ZnO.

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