A molding process for atomic oxygen resistant composite materials

Atomic oxygen-resistant composite materials were prepared by acid pickling and vacuum pressure rolling technology, which solved the problem of composite materials being intolerant to atomic oxygen in spacecraft. This achieved long-term durability and non-debonding bubble performance of the materials, thus extending the life of spacecraft.

CN119329176BActive Publication Date: 2026-06-30HARBIN FRP INST +1

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
HARBIN FRP INST
Filing Date
2024-11-27
Publication Date
2026-06-30

Smart Images

  • Figure CN119329176B_ABST
    Figure CN119329176B_ABST
Patent Text Reader

Abstract

A molding process for atomic oxygen-resistant composite materials. This invention belongs to the field of aerospace materials technology. This invention solves the problems of composite materials being susceptible to atomic oxygen in aerospace environments, and the tendency for debonding and air bubbles to form during bonding processes. This invention involves first coating an alloy material and a resin-based carbon fiber composite material separately with adhesive, and then bonding the alloy material and the resin-based carbon fiber composite material together to obtain an atomic oxygen-resistant composite material. The use of pressure rollers in this invention effectively ensures uniform adhesive layer thickness. A uniform adhesive layer allows for better adhesion of the metal protective layer to the surface of the resin-based carbon fiber composite material. The molding process of this invention ensures that the atomic oxygen-resistant composite material does not debond in aerospace environments, effectively extending the service life of aerospace equipment.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of aerospace materials technology, specifically relating to a molding process for atomic oxygen resistant composite materials. Background Technology

[0002] Atomic oxygen is formed by the photodecomposition of oxygen molecules under solar radiation. On the one hand, atomic oxygen has strong oxidizing properties and can react directly with materials, causing severe oxidation and erosion of organic and some metallic materials on spacecraft surfaces. This leads to material thinning, changes in surface morphology, alterations in thermal / electrical properties, and even complete failure. On the other hand, when a spacecraft travels at high speeds, the energy of atomic oxygen impacting its surface is extremely high. When these highly oxidizing, high-flux, and high-energy atomic oxygen particles interact with the spacecraft surface, they cause erosion and performance degradation of the surface materials, thus affecting the normal operation and lifespan of the spacecraft. For resin composites and carbon fiber composites, the space environment is susceptible to the effects of atomic oxygen and ultraviolet radiation, leading to a decline in their physicochemical properties and poor survivability, thus affecting the normal operation of the spacecraft. To ensure the long-term reliable operation of spacecraft in orbit, and considering the atomic oxygen resistance requirements for domestic low-Earth orbit long-life spacecraft, necessary protection needs to be provided for the external components of the spacecraft.

[0003] Composite materials account for a significantly increased proportion of the structural weight of aircraft and spacecraft, and their applications are more widespread. However, composite materials lack resistance to atomic oxygen. Current technologies typically address this deficiency by painting, coating, or bonding methods to cover the composite material with an anti-atomic material. However, painting and coating methods suffer from severe wear and tear and have a short service life. While bonding methods have less wear and tear and a longer service life, they are prone to problems such as detachment or air bubbles, further wasting material and affecting usability. Therefore, a new process is urgently needed to solve the problems of atomic oxygen attack on composite materials and the detachment and air bubble issues associated with bonding methods, thereby extending the service life of aerospace equipment. This is of great significance for the sustainable development of aerospace. Summary of the Invention

[0004] The purpose of this invention is to solve the problems of composite materials being intolerant to atomic oxygen in aerospace environments, the tendency of bonding processes to debond and bubble, and the need to extend the service life of aerospace equipment. This invention provides a molding process for atomic oxygen-resistant composite materials.

[0005] The technical solution of the present invention is as follows:

[0006] One objective of this invention is to provide a molding process for atomic oxygen-resistant composite materials, wherein the molding process is as follows:

[0007] S1: Treatment of the metal protective layer: The metal protective layer is pickled;

[0008] S2: Surface treatment of resin-based carbon fiber composite material: Lightly polish the resin-based carbon fiber composite material with 800-1000 grit sandpaper;

[0009] S3: Adhesive preparation: Mix epoxy adhesive components A and B at a mass ratio of 5:1 until homogeneous, then place in a vacuum chamber to remove gas;

[0010] S4: Metal protective layer adhesive coating: Cut the metal protective layer into several strips 100-500mm long and 50-100mm wide. Make a Ф2mm vent hole every 100mm along the center line of the wide side. Squeeze the adhesive evenly onto the metal protective layer and roll it evenly.

[0011] S5: Coating of resin-based carbon fiber composite material with adhesive layer: Place the resin-based carbon fiber composite material on the platform, add the adhesive liquid evenly in small amounts multiple times to the coating area on the surface of the resin-based carbon fiber composite material, and roll it evenly;

[0012] S6: Metal protective layer is laid on the surface of resin-based carbon fiber composite material: The metal protective layer is laid on the surface of resin-based carbon fiber composite material and rolled evenly. After rolling, the next metal protective layer is laid. The metal protective layers are overlapped with each other. After laying, a soft film is laid on top, put into a vacuum bag, vacuum pressurize, and then put into an autoclave for curing to obtain atomic oxygen resistant composite material.

[0013] Further specifying, the metal protective layer in S1 is made of aluminum foil or aluminum alloy material, with a thickness of 25-50 μm.

[0014] Further specified, the vacuum tank pressure in S3 is -80 to -90 kPa, and the degassing time is 15-20 min.

[0015] Further specified, the coating thickness in S4 is 10-20μm, and the coating thickness in S5 is 30-40μm.

[0016] Further specified, the autoclave temperature in S6 is 45-85℃, the pressure is 200±5Kpa, and the curing time is 1-3h.

[0017] Furthermore, the overlap width between the metal protective layers in S6 is 2-10mm.

[0018] Further specified, the soft film in S6 is made of silicone rubber, with a thickness of 1-2 mm, a hardness of 40-80 HB, a tensile strength of 5-10 MPa, and an elongation of 200-300%.

[0019] Furthermore, all the above steps are to be performed in an environment with a temperature of 15-35℃ and a relative humidity of 30%-60%.

[0020] The second objective of this invention is to provide an atomic oxygen resistant composite material, which is prepared by the above-mentioned molding process.

[0021] The third objective of this invention is to provide an atomic oxygen-resistant composite material for use in aerospace.

[0022] The beneficial effects of this invention are as follows:

[0023] This invention effectively ensures uniform adhesive layer thickness through specialized roller application and rolling. Uniform adhesive layer allows for better bonding of the metal protective layer to the surface of the composite material, achieving resistance to atomic oxygen. It also overcomes the problem of air bubbles forming when the metal protective layer and composite material are bonded in a vacuum environment. This application has undergone tens of thousands of high and low temperature cycles, and the metal protective layer and composite material have not debonded or generated air bubbles, meeting the 15-year service life requirement for spacecraft in orbit. Attached Figure Description

[0024] Figure 1 It is a vacuum autoclave;

[0025] Figure 2 The image shows the atomic oxygen resistant composite material of Example 1 after a vacuum autoclave test;

[0026] Figure 3 Image of the atomic oxygen resistant composite material used in Comparative Example 1 after a vacuum autoclave test.

[0027] Figure 4 The graphs show the mass loss of atomic oxygen stripping in Example 1 and Comparative Example 1.

[0028] Figure 5 This is a diagram of the experimental bonding process. Detailed Implementation

[0029] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0030] The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used in the following embodiments, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such a composition, step, method, article, or apparatus.

[0031] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1 to 5” is disclosed, the described range should be interpreted as including ranges “1 to 4”, “1 to 3”, “1 to 2”, “1 to 2 and 4 to 5”, “1 to 3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range. In this specification and claims, range definitions may be combined and / or interchanged, unless otherwise stated, these ranges include all subranges contained therein.

[0032] The indefinite articles “a” and “an” preceding an element or component of this invention do not impose any limitation on the quantity (i.e., number of times) of the element or component. Therefore, “an” or “a” should be interpreted as including one or at least one, and the singular form of an element or component also includes the plural form, unless the quantity clearly refers only to the singular form.

[0033] In this invention, "an embodiment" or "embodiment" refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the invention. The phrase "in one embodiment" appearing in different places in this specification does not necessarily refer to the same embodiment, nor is it a single or selective embodiment that excludes other embodiments.

[0034] The endpoints and any values ​​of the ranges disclosed in this invention are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0035] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, the materials, reagents, methods, and instruments used are all conventional materials, reagents, methods, and instruments in the art, and can be obtained commercially by those skilled in the art.

[0036] Example 1:

[0037] S1: Treatment of the metal protective layer: Select aluminum foil with a thickness of 50μm and perform surface phosphate anodizing treatment for 2 hours;

[0038] S2: Surface treatment of resin-based carbon fiber composite material (carbon fiber volume ratio 60%, resin volume ratio 40%): lightly polish the surface of the composite material with 1000-grit sandpaper.

[0039] S3: Adhesive preparation: Mix 100g of component A and 20g of component B of HB01 adhesive solution evenly, then place it in a vacuum tank to degas. The pressure of the vacuum tank is -90kpa, and the degassing time is 20min.

[0040] S4: Metal Protective Layer Adhesive Coating: Cut the metal protective layer into several strips 500mm long and 100mm wide. Make a Ф2mm vent hole every 100mm along the central axis of the wide side. Adhere green high-temperature resistant pressure-sensitive adhesive tape to both sides of the metal protective layer. Place the metal protective layer on the metal plate so that the side with the pressure-sensitive adhesive tape is in contact with the metal plate. Squeeze the adhesive evenly onto the metal protective layer. The adhesive thickness is 20μm. Roll it evenly.

[0041] S5: Coating of resin-based carbon fiber composite material: Place the resin-based carbon fiber composite material on the platform, add HB01 adhesive in two equal portions to the surface of the resin-based carbon fiber composite material, roll it evenly, and the coating thickness is 40μm.

[0042] S6: Metal protective layer is laid on the surface of resin-based carbon fiber composite material: The metal protective layer is placed on the surface of the resin-based carbon fiber composite material and rolled with a 100mm rubber roller. After rolling, the pressure-sensitive tape is removed, and the next metal protective layer is laid. The metal protective layers are overlapped with a width of 5mm. After laying, a soft film material is laid on top, placed in a vacuum bag, vacuum pressurized, and then placed in a hot autoclave for curing. The temperature of the hot autoclave is 80℃, the pressure is 200±5KPa, and the curing time is 2h to obtain an atomic oxygen resistant composite material.

[0043] All of the above steps were completed in a Class 100,000 cleanroom with an ambient temperature of 26°C and a relative humidity of 40%.

[0044] Comparative Example 1:

[0045] S1: Treatment of the metal protective layer: Select aluminum foil with a thickness of 15μm and perform surface polishing;

[0046] S2: Surface treatment of resin-based carbon fiber composite material: Lightly polish the surface of the composite material with 600-grit sandpaper;

[0047] S3: Adhesive preparation: Mix 100g of component A and 20g of component B of HB01 adhesive solution evenly.

[0048] S4: Metal protective layer adhesive coating: The adhesive is evenly squeezed onto the metal protective layer, with a coating thickness of 100μm, and rolled evenly.

[0049] S5: Coating of resin-based carbon fiber composite material adhesive layer (carbon fiber volume ratio 60%, resin volume ratio 40%): Place the resin-based carbon fiber composite material on the platform, add HB01 adhesive to the surface of the resin-based carbon fiber composite material in one go, roll it evenly, and the coating thickness is 100μm.

[0050] S6: Metal protective layer is laid on the surface of resin-based carbon fiber composite material: The metal protective layer is placed on the surface of resin-based carbon fiber composite material. After the laying is completed, it is put into a vacuum bag, the vacuum bag is pressurized, the vacuum pressure is maintained at -85 kPa, and the curing time is 24 hours to obtain atomic oxygen resistant composite material.

[0051] All of the above steps were completed in a Class 100,000 cleanroom with an ambient temperature of 26°C and a relative humidity of 40%.

[0052] Vacuum autoclave test:

[0053] The experimental conditions were ±100℃ and a vacuum degree of 10. -4 The cycle repeats 12 times.

[0054] Depend on Figure 2 and Figure 3 It can be seen that after the thermal vacuum test, the surface of Example 1, which has undergone the process of this experiment, remains flat, without bubbles or protrusions, and exhibits excellent material properties. In contrast, the test piece of Comparative Example 1, which has not undergone the process of this experiment, has many bubbles and wrinkles on its surface.

[0055] Atomic oxygen stripping mass loss test:

[0056] Experimental conditions: The atomic oxygen irradiation experiment was conducted on a plasma-type atomic oxygen ground simulation facility. The oxygen plasma was generated by a magnetic mirror configuration microwave ECR method. The atomic oxygen energy was 5 eV; the flux rate was 5.0 × 10¹⁵ O / (cm²). 2 ·s); when the irradiation dose reaches 10.0×1020O / cm 2 At that time, performance tests were conducted on the materials. The test results are as follows: Figure 4 As shown, by Figure 4 It can be seen that the atomic oxygen stripping mass loss in Example 1 is only 0.1%, while the atomic oxygen stripping mass loss in Comparative Example 1 is 0.8%. This shows that the atomic oxygen resistant composite material treated by this experimental process can effectively resist the erosion of space atomic oxygen and meet the requirements for use in spacecraft materials.

[0057] The above description is merely a preferred embodiment of the present invention. These specific embodiments are different implementations based on the overall concept of the present invention, and the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A molding process for atomic oxygen-resistant composite materials, characterized in that, The molding process includes the following steps: S1: Treatment of the metal protective layer: The metal protective layer is pickled; S2: Surface treatment of resin-based carbon fiber composite material: Lightly polish the resin-based carbon fiber composite material with 800-1000 grit sandpaper; S3: Adhesive preparation: Mix epoxy adhesive components A and B at a mass ratio of 5:1 until homogeneous, then place in a vacuum chamber to remove gas; S4: Metal protective layer adhesive coating: Cut the metal protective layer into several strips 100-500mm long and 50-100mm wide. Make a Ф2mm vent hole every 100mm along the center line of the wide side. Squeeze the adhesive evenly onto the metal protective layer and roll it evenly. S5: Coating of resin-based carbon fiber composite material with adhesive layer: Place the resin-based carbon fiber composite material on the platform, add the adhesive liquid evenly in small amounts multiple times to the coating area on the surface of the resin-based carbon fiber composite material, and roll it evenly; S6: Metal protective layer is laid on the surface of resin-based carbon fiber composite material: The metal protective layer is laid on the surface of resin-based carbon fiber composite material and rolled evenly. After rolling, the next metal protective layer is laid. The metal protective layers are overlapped. After laying, a soft film is laid on top, put into a vacuum bag, vacuum pressurize, and then put into a thermostatic precipitator for curing to obtain atomic oxygen resistant composite material. The coating thickness in S4 is 10-20μm, and the coating thickness in S5 is 30-40μm. The metal protective layer in S1 is made of aluminum foil or aluminum alloy, with a thickness of 25-50 μm.

2. The molding process according to claim 1, characterized in that, The vacuum tank pressure in S3 is -80~-90kPa, and the degassing time is 15-20min.

3. The molding process according to claim 1, characterized in that, The S6 autoclave temperature is 45-85℃, the pressure is 200±5kPa, and the curing time is 1-3h.

4. The molding process according to claim 1, characterized in that, The overlap width between metal protective layers in S6 is 2-10mm.

5. The molding process according to claim 1, characterized in that, The soft film in S6 is made of silicone rubber, with a thickness of 1-2 mm, a tensile strength of 5-10 MPa, and an elongation of 200-300%.

6. The molding process according to claim 1, characterized in that, All of the above steps were performed in an environment with a temperature of 15-35℃ and a relative humidity of 30%-60%.

7. A composite material resistant to atomic oxygen, characterized in that, It is prepared by the molding process described in any one of claims 1-6.

8. The atomic oxygen resistant composite material according to claim 7 is used in aerospace.