CN113415054B - Resin-based composite material thermo-oxidative aging prevention structure and preparation method thereof - Google Patents
Resin-based composite material thermo-oxidative aging prevention structure and preparation method thereof Download PDFInfo
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- CN113415054B CN113415054B CN202110631900.6A CN202110631900A CN113415054B CN 113415054 B CN113415054 B CN 113415054B CN 202110631900 A CN202110631900 A CN 202110631900A CN 113415054 B CN113415054 B CN 113415054B
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
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- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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- B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
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- B32B2307/552—Fatigue strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/558—Impact strength, toughness
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
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Abstract
The invention relates to a thermal-oxidative-aging-resistant structure of a resin-based composite material and a forming method thereof, wherein the thermal-oxidative-aging-resistant structure comprises the resin-based composite material and a thermal-oxidative-aging-resistant film layer; the resin-based composite material and the thermal oxidation aging prevention film layer are both provided with a bonding surface, and the bonding surface of the thermal oxidation aging prevention film layer and the bonding surface of the resin-based composite material are bonded and cured into a whole; the thermal oxidation aging resistant mold layer is a polyimide film layer; and the joint surface of the thermal-oxidative-aging-resistant film layer is subjected to roughening treatment. The thermal oxidation protective polyimide film used in the invention has certain strength and toughness, has excellent thermal oxidation stability, and can effectively prevent the contact of oxygen functional resin matrix in the air, thereby reducing the aging rate of the composite material.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a thermal oxidation aging prevention structure of a resin matrix composite material and a preparation method thereof.
Background
The resin-based composite material has high specific strength, high specific modulus and good fatigue resistance, and is widely applied in the field of aerospace. At present, resin-based composite materials are mainly used for structural members of airplane fuselages in the field of aviation, the use temperature is generally not more than 200 ℃, and epoxy resin and bismaleimide resin are mostly used. Compared with aircraft structural materials, the temperature resistance of the materials of the aircraft engine is higher, the temperature resistance grade of the resin-based composite materials used for cold-end parts of the aircraft engine at present generally needs to be more than 200 ℃, and the service temperature of part of parts is more than 300 ℃ or higher.
Different from aerospace, the aeroengine not only requires the material to have better high-temperature performance, but also requires the material to have good mechanical property retention rate in a long-term high-temperature use process, namely, the material has longer service life, so as to achieve the safety and stability required by the aeroengine. The thermal aging is a problem that resin-based composite materials are difficult to avoid when applied to an aircraft engine, and the thermal aging can cause resin decomposition and reduction of mechanical properties of the composite materials, thereby causing material failure.
The thermal aging of the composite material is mainly that in a high-temperature environment, a resin matrix is oxidized and decomposed by oxygen in air to form microcracks on the surface of the material, and the air further enters the material, so that the decomposition of the resin is accelerated, and the mechanical property of the material is reduced. High temperature and oxygen are two major factors that cause thermal aging of the composite.
The problem of thermal aging of the composite material can be solved from multiple aspects, and the heat resistance of the resin matrix can be improved on the one hand, if polyimide resin with higher temperature resistance level is used, the method can fundamentally solve the problem of thermal aging, but the polyimide composite material has high molding difficulty, more defects and higher cost. On the other hand, the thermal stability of the material can be improved by a thermal protection method, for example, when a low-thermal-conductivity ceramic thermal barrier coating is used, the thermal barrier coating can prevent heat from being transferred to the composite material to a certain extent and reduce the temperature of the composite material, so that the thermal aging of the composite material is slowed down.
Disclosure of Invention
The purpose of the invention is: solves the technical problems of easy oxidation, low service life, fast reduction of mechanical property and high thermal weight loss of the resin-based material in a high-temperature environment. Particularly, the technical scheme of the invention can improve the long-term service temperature of the resin-based composite material by 30-50 ℃ on the original basis, or improve the service life of the resin-based composite material by 20-80% on the original basis, and can keep the structure of the composite material complete without layering, thereby ensuring that the composite material keeps higher mechanical property.
The technical scheme of the invention is as follows:
the invention provides a thermo-oxidative aging prevention structure for a resin matrix composite, which comprises the resin matrix composite and a thermo-oxidative aging prevention film layer; the resin-based composite material and the thermal-oxidative-aging-resistant film layer are both provided with a bonding surface, and the bonding surface of the thermal-oxidative-aging-resistant film layer and the bonding surface of the resin-based composite material are bonded and cured into a whole; the thermal oxidation aging resistant mold layer is a polyimide film layer; and the joint surface of the thermal-oxidative-aging-resistant film layer is subjected to roughening treatment.
Further, the thickness of the polyimide film layer is 25-75 micrometers.
Further, the elongation at break of the polyimide film is greater than 70%.
Further, the tensile strength of the polyimide film is greater than 200MPa.
Further, the polyimide film has a 5% weight loss temperature in nitrogen of greater than 550 ℃. Polyimide films are required to have high thermal stability.
Further, the roughening treatment is supercritical CO 2 And (5) spraying treatment.
Further, the resin-based composite material is an epoxy resin-based composite material or a bismaleimide resin-based composite material.
Further, the reinforcing material of the resin-based composite material is carbon fiber or glass fiber.
Further, the resin matrix of the resin-based composite material has a viscosity in a range of room temperature to 80 ℃.
Furthermore, volatile small molecules cannot be generated in the curing process of the resin-based composite material.
The invention also provides a preparation method of the resin matrix composite material thermo-oxidative aging prevention structure, which comprises the following steps:
step 1,
Subjecting polyimide film to supercritical CO 2 Carrying out spray treatment to realize roughening treatment;
step 2,
Sequentially paving and sticking the polyimide film and the prepreg in a mould, and carrying out vacuum packaging or die assembly;
step 3,
Placing the mould on an autoclave or a hot press, and curing at high temperature and high pressure according to a prepreg curing process;
step 4,
And (3) after the solidification, releasing pressure and demoulding to obtain the resin-based composite material part with the thermal oxidation aging prevention structure.
Furthermore, a polyimide film is firstly paved in the mould, at least one layer of prepreg is paved, and finally the polyimide film is paved. The resin-based composite material with the polyimide film on the surface is realized.
Furthermore, the polyimide film is spliced and paved, and a plurality of film sheets are spliced to form the whole polyimide film. Preferably, the width of the seam between the spliced films is below 1 mm.
Further, the supercritical CO 2 In the spraying treatment, the spraying pressure is more than 10 MPa, and the spraying area per unit time is not more than 0.1m 2 In terms of a/minute. Preferably, the spray angle is a vertical spray.
Further, when the prepreg is applied to a mold, the prepreg is applied in a heated state. The heating can improve the viscosity of the prepreg, so that the bonding effect of the prepreg and the polyimide film is better. Furthermore, the heating temperature for paving the prepreg in a heating state is 60-80 ℃.
Further, air between the polyimide film and the prepreg is removed while the polyimide film is paved in the mold;
further, when the polyimide film is spread in a mold, the polyimide film is subjected to flattening treatment. Wrinkles are eliminated.
Further, the resin in the prepreg is epoxy resin or bismaleimide resin.
Splicing in the invention is different from lapping, is strictly limited to butt joint, and can not be lapped. And the well polyimide film of this application is for tiling when spreading the subsides, can not appear the fold.
TABLE 1 comparison of the shear strength of the film before and after aging of the film-coated and film-uncoated specimens
The invention has the advantages that:
1. the thermal oxidation protection polyimide film used in the invention has certain strength and toughness and excellent thermal oxidation stability, and can effectively prevent the contact of oxygen functional resin matrix in the air, thereby reducing the aging rate of the composite material;
2. the thermal oxidation protective film used by the invention has a thermal expansion coefficient equivalent to that of the resin matrix, so that the protective film and the resin matrix composite material can be ensured to shrink synchronously when the thermal oxidation aging-resistant structure is cured, thermal stress does not exist, and debonding does not occur;
3. the high-temperature resistant film used in the invention uses supercritical CO before use 2 Surface treatment is carried out to remove surface impurities, the surface roughness of the film is increased, and the bonding strength between the film and resin can be improved, so that the overall strength and the service life of the composite material thermal-oxidation aging resistant structure are improved;
4. according to the invention, air between the protective film and the prepreg is eliminated as much as possible in the paving process, volatile micromolecules are generated at the part of the resin matrix during curing, the internal quality of the prepared composite material is good, the porosity is low, and the good mechanical property of the composite material is ensured;
5. the invention adopts co-curing technology, the thermo-oxidative aging resistant structure and the resin matrix composite material are synchronously cured and molded, the thermo-oxidative aging resistant performance of the composite material is improved, the interface problem of the matrix and the protective layer is not introduced, the post-treatment step is not needed, and the manufacturing cost is saved.
Drawings
FIG. 1 is a photograph of a composite crystalline phase with a heat protective film;
FIG. 2 is a graph of 192h weight loss of composites aged with and without heat protective film;
FIG. 3 is a graph of weight loss of a composite material with and without a heat protective film after aging for 600 h;
FIG. 4 is a scanning electron microscope image of the surface of a sample with a heat protective film after aging for 600 hours at 280 ℃;
FIG. 5 is a scanning electron micrograph of the surface of a sample aged 600h at 280 ℃ without a heat protecting film;
FIG. 6 is a circular structure of a resin-based composite material having a structure for preventing thermal-oxidative deterioration.
Detailed Description
The present invention is described in further detail below.
Embodiment 1 provides a thermal oxidation aging resistant structure of a resin-based composite material, which is a flat plate structure and comprises a resin-based composite material and a thermal oxidation aging resistant film layer; the resin-based composite material and the thermal-oxidative-aging-resistant film layer are both provided with a bonding surface, and the bonding surface of the thermal-oxidative-aging-resistant film layer and the bonding surface of the resin-based composite material are bonded and cured into a whole; the thermal oxidation aging resistant mold layer is a polyimide film layer; and the joint surface of the thermal-oxidative-aging-resistant film layer is subjected to roughening treatment.
The thickness of the polyimide film layer is 50 micrometers.
The elongation at break of the polyimide film was 80%.
The tensile strength of the polyimide film is 240MPa.
The polyimide film had a 5% weight loss in nitrogen at a temperature of 590 ℃. The roughening treatment is supercritical CO 2 And (5) spraying treatment.
The supercritical CO 2 In the spraying treatment, the spraying pressure is 12 MPa, and the spraying area per unit time is 0.05m 2 In terms of a/minute, the spray angle was vertical.
The resin-based composite material is a bismaleimide resin-based composite material.
The reinforcing material of the resin matrix composite material is carbon fiber.
The resin matrix of the resin-based composite material has viscosity at 80 ℃.
The resin-based composite material does not generate volatile micromolecules in the curing process.
The invention also provides a preparation method of the resin matrix composite material thermal oxidation aging resistant structure, which comprises the following steps:
step 1,
To polyimide filmSupercritical CO 2 Carrying out spray treatment to realize roughening treatment;
step 2,
Sequentially paving and sticking the polyimide film and the prepreg in a mould, and carrying out vacuum packaging;
the mold was first coated with a polyimide film, then 22 layers of prepreg were applied, and finally a polyimide film was applied. The resin-based composite material with the polyimide film on the surface is realized.
When the prepreg is laid in a mold, the prepreg is laid in a heated state. The heating can improve the viscosity of the prepreg, so that the bonding effect of the prepreg and the polyimide film is better. The heating temperature for laying the prepreg in a heating state is 80 ℃.
When the polyimide film is laid in a mould, air between the polyimide film and the prepreg is removed;
and when the polyimide film is paved in a mould, flattening the polyimide film. Wrinkles are eliminated.
Step 3,
Placing the mould in an autoclave, heating to 125 ℃, preserving heat for 30 minutes, then applying 0.6 MPa pressure, preserving heat for 1 hour at 180 ℃,2 hours at 230 ℃, 4 hours at 250 ℃ and 4 hours at 280 ℃ respectively, and finishing curing;
step 4,
After the solidification is finished, cooling to 60 ℃, releasing pressure and demolding to obtain the resin matrix composite flat plate with the thermal oxidation aging prevention structure.
The ultrasonic C-scanning results of the composite material flat plate with the heat protection film and the composite material without the heat protection film can be obtained, the internal quality of the composite material with the heat protection film prepared by the autoclave process is equivalent to that of a sample without the heat protection film, and no layering or dense pores exist.
The photo of the crystal phase of the composite material with the heat protection film is shown in figure 1, the porosity is less than 1%, and the internal quality of the composite material with the heat protection film is good.
The composite material sample with the heat protection film and the composite material sample without the heat protection film prepared in the same furnace are simultaneously placed in a 280 ℃ oven for aging test, the sizes of the samples are 36mm multiplied by 36mm, the weight loss curves of the two samples after aging for 192 hours are shown in figure 2, and the heat protection film can reduce the material aging rate by more than 50%.
The thermal weight loss curve of the above samples after 600 hours of aging in an oven at 280 ℃ is shown in FIG. 3, and it can be seen that the aging of the samples without the heat protective film is accelerated to about 200 hours, while the aging of the samples with the heat protective film is accelerated to about 500 hours, so that the heat protective film can slow down the aging acceleration of the composite material. When the weight loss of 5% is taken as the service life of the material, the heat protection film can increase the service life of the material from 250 hours to 450 hours, and the service life is prolonged by 80%.
The scanning electron microscope images of the surface of the sample after being aged for 600 hours in an oven at 280 ℃ are shown in fig. 4 and fig. 5, the sample with the heat protective film has a complete surface appearance without cracks after being aged for 600 hours, and the sample without the heat protective film has more micro cracks on the surface after being aged for 600 hours, so that the sample is seriously damaged. The heat protection film can better protect the composite material from being damaged in a high-temperature environment.
The layer shear performance ratio of the samples with the thermal protection films to the samples without the thermal protection films before and after aging for 600 hours at 280 ℃ is shown in table 1, and the layer shear performance of the two composite material samples before aging is equivalent to that of the samples without the thermal protection films, which shows that the thermal protection films and the prepreg have good bonding strength, and the thermal protection films do not reduce the mechanical properties of the materials.
TABLE 1 comparison of the shear strength of the film before and after aging of the film-coated and film-uncoated specimens
After the sample is aged for 600 hours at 280 ℃, the shear strength of the sample layer with the thermal protection film is 15.6MPa, the retention rate is 26%, the shear strength of the sample layer without the thermal protection film is 8.3MPa, the retention rate is only 15%, and both the absolute strength and the retention rate are far lower than those of the sample layer with the thermal protection film.
Embodiment 2 provides a thermal oxidation aging resistant structure of a resin matrix composite, which is a flat plate structure and comprises the resin matrix composite and a thermal oxidation aging resistant film layer; the resin-based composite material and the thermal oxidation aging prevention film layer are both provided with a bonding surface, and the bonding surface of the thermal oxidation aging prevention film layer and the bonding surface of the resin-based composite material are bonded and cured into a whole; the thermal oxidation aging resistant mold layer is a polyimide film layer; and the joint surface of the thermal-oxidative-aging-resistant film layer is subjected to roughening treatment.
The thickness of the polyimide film layer is 50 micrometers.
The elongation at break of the polyimide film was 80%.
The tensile strength of the polyimide film was 240MPa.
The polyimide film had a 5% weight loss in nitrogen at a temperature of 590 ℃.
The roughening treatment is supercritical CO 2 And (5) spraying treatment.
The supercritical CO 2 In the spraying treatment, the spraying pressure is 11 MPa, and the spraying area per unit time is 0.06m 2 In terms of a/minute, the spray angle was vertical.
The resin-based composite material is a bismaleimide resin-based composite material.
The reinforcing material of the resin matrix composite material is carbon fiber.
The resin matrix of the resin-based composite material has a viscosity at 80 ℃.
The resin-based composite material does not generate volatile micromolecules in the curing process.
The invention also provides a preparation method of the resin matrix composite material thermal oxidation aging resistant structure, which comprises the following steps:
step 1,
Subjecting polyimide film to supercritical CO 2 Carrying out spray treatment to realize roughening treatment;
step 2,
Successively paving and sticking the polyimide film and the prepreg in a mould, and closing the mould;
the polyimide film was laid in the mold first, then 22 layers of prepreg were laid, and finally the polyimide film was laid. The resin-based composite material with the polyimide film on the surface is realized.
When the prepreg is laid in a mold, the prepreg is laid in a heated state. The heating can improve the viscosity of the prepreg, so that the bonding effect of the prepreg and the polyimide film is better. The heating temperature for laying the prepreg in a heating state is 80 ℃.
When the polyimide film is laid in a mould, air between the polyimide film and the prepreg is removed;
and when the polyimide film is paved in a mould, flattening the polyimide film.
Step 3,
Placing the die on a hot press, preserving heat at 125 ℃ for 30 minutes, applying 2 tons of pressure, preserving heat at 180 ℃ for 1 hour, preserving heat at 230 ℃ for 2 hours, preserving heat at 250 ℃ for 4 hours, and preserving heat at 280 ℃ for 4 hours to finish curing;
step 4,
And after curing, cooling to 60 ℃, releasing pressure and demolding to obtain the resin-based composite material flat plate with the thermal-oxidative-aging-resistant structure, wherein the thickness of the flat plate is 2.8mm. The prepared composite material with the heat protection film has good appearance state, and the polyimide film can be completely attached to the prepreg. The composite material has good internal quality and no layering or dense pores.
Embodiment 3, the thermal oxidation aging resistant structure of the resin matrix composite provided by the invention is a circular ring structure, and comprises the resin matrix composite and a thermal oxidation aging resistant film layer; the resin-based composite material and the thermal oxidation aging prevention film layer are both provided with a bonding surface, and the bonding surface of the thermal oxidation aging prevention film layer and the bonding surface of the resin-based composite material are bonded and cured into a whole; the thermal oxidation aging resistant mold layer is a polyimide film layer; and the joint surface of the thermal-oxidative-aging-resistant film layer is subjected to roughening treatment.
The thickness of the polyimide film layer is 50 micrometers.
The elongation at break of the polyimide film was 80%.
The tensile strength of the polyimide film is 240MPa.
The polyimide film had a 5% weight loss in nitrogen at a temperature of 590 ℃.
The roughening treatment is supercritical CO 2 And (5) spraying treatment.
The supercritical CO 2 In the spraying treatment, the spraying pressure is 12 MPa, and the spraying area per unit time is 0.05m 2 In minutes, the spray angle is vertical.
The resin-based composite material is a bismaleimide resin-based composite material.
The reinforcing material of the resin-based composite material is carbon fiber.
The resin matrix of the resin-based composite material has a viscosity at 80 ℃.
The resin-based composite material does not generate volatile micromolecules in the curing process.
The invention also provides a preparation method of the resin matrix composite material thermal oxidation aging resistant structure, which comprises the following steps:
step 1,
Subjecting polyimide film to supercritical CO 2 Carrying out spray treatment to realize roughening treatment;
step 2,
Sequentially paving and sticking the polyimide film and the prepreg in a mould, and carrying out vacuum packaging;
the polyimide film was laid in the mold first, then 22 layers of prepreg were laid, and finally the polyimide film was laid. The resin-based composite material with the polyimide film on the surface is realized.
When the prepreg is laid in a mold, the prepreg is laid in a heated state. The heating can improve the viscosity of the prepreg, so that the bonding effect of the prepreg and the polyimide film is better. The heating temperature for laying the prepreg in a heated state was 80 ℃.
When the polyimide film is laid in a mould, air between the polyimide film and the prepreg is removed;
and when the polyimide film is paved in a mould, flattening the polyimide film. Wrinkles are eliminated.
The polyimide film is spliced and paved, and a plurality of film sheets are spliced to form the whole polyimide film. The width of the seam between the spliced films is less than 1 mm.
Step 3,
Placing the mould in an autoclave, preserving heat at 125 ℃ for 30 minutes, applying 0.6 MPa pressure, preserving heat at 180 ℃ for 1 hour, preserving heat at 230 ℃ for 2 hours, preserving heat at 250 ℃ for 4 hours, preserving heat at 280 ℃ for 4 hours, and finishing curing;
step 4,
After the solidification is finished, the temperature is reduced to 60 ℃, the pressure is released, and the mold is removed, so that the resin matrix composite material circular ring structure with the thermal oxidation aging prevention structure is obtained, and the figure 6 is shown. The diameter of the product is about 1000mm, and the height is about 300mm. And 4, nondestructive testing is carried out on the composite material part by using ultrasonic A-scanning equipment, and the tested composite material part has good internal quality and no layering or dense pores.
Claims (10)
1. Resin matrix combined material prevents ageing structure of thermal oxidation, its characterized in that: comprises a resin-based composite material and a thermal oxidation aging resistant film layer; the resin-based composite material and the thermal oxidation aging prevention film layer are both provided with a bonding surface, and the bonding surface of the thermal oxidation aging prevention film layer and the bonding surface of the resin-based composite material are bonded and cured into a whole; the thermal oxidation aging resistant mold layer is a polyimide film layer; the joint surface of the thermal-oxidative-aging-resistant film layer is subjected to roughening treatment;
the reinforcing material of the resin-based composite material is carbon fiber or glass fiber, the resin-based composite material is epoxy resin-based composite material or bismaleimide resin-based composite material, and volatile micromolecules cannot be generated in the curing process of the resin-based composite material;
the thickness of the polyimide film layer is 25-75 micrometers, the elongation at break of the polyimide film is more than 70%, the tensile strength of the polyimide film is more than 200MPa, and the weight loss of the polyimide film in nitrogen is 5% and the temperature is higher than 550 ℃;
the roughening treatment is supercritical CO 2 Spraying treatment;
when the resin-based composite material thermal oxidation aging prevention structure is prepared, a polyimide film is paved in a mould, at least one layer of prepreg is paved, and finally the polyimide film is paved.
2. The resin-based composite material thermo-oxidative aging resistant structure according to claim 1, wherein: the resin matrix of the resin-based composite material has viscosity in the range of room temperature to 80 ℃.
3. The method for preparing a thermo-oxidative aging resistant structure for resin-based composites as claimed in claim 1 or 2, comprising the steps of:
step 1,
Subjecting polyimide film to supercritical CO 2 Carrying out spray treatment to realize roughening treatment; the supercritical CO 2 In the spraying treatment, the spraying pressure is more than 10 MPa, and the spraying area per unit time is not more than 0.1m 2 A/min;
step 2,
Sequentially paving and pasting the polyimide film and the prepreg in a mould, paving and pasting the polyimide film in the mould, then paving and pasting at least one layer of prepreg, finally paving and pasting the polyimide film, and carrying out vacuum packaging or mould assembly; the resin in the prepreg is epoxy resin or bismaleimide resin;
step 3,
Placing the mould on an autoclave or a hot press, and curing at high temperature and high pressure according to a prepreg curing process;
step 4,
And (3) after the solidification, releasing pressure and demoulding to obtain the resin-based composite material part with the thermal oxidation aging prevention structure.
4. The method for preparing a thermo-oxidative aging resistant structure for resin-based composites as claimed in claim 3, wherein: the polyimide film is spliced and paved, and a plurality of film sheets are spliced to form the whole polyimide film.
5. The method for preparing a thermo-oxidative aging resistant structure for resin-based composites as claimed in claim 4, wherein: the width of the seam between the spliced films is less than 1 mm.
6. The method for preparing the thermo-oxidative aging resistant structure of the resin-based composite material as claimed in claim 3, wherein: the supercritical CO 2 In the spraying treatment, the spraying angle is vertical spraying.
7. The method for preparing a thermo-oxidative aging resistant structure for resin-based composites as claimed in claim 3, wherein: when the prepreg is laid in a mold, the prepreg is laid in a heated state.
8. The method for preparing a thermo-oxidative aging resistant structure for resin-based composites as claimed in claim 7, wherein: the heating temperature of the prepreg in a heating state in paving is 60-80 ℃.
9. The method for preparing a thermo-oxidative aging resistant structure for resin-based composites as claimed in claim 3, wherein: and (3) removing air between the polyimide film and the prepreg while paving in the mould.
10. The method for preparing the thermo-oxidative aging resistant structure of the resin-based composite material as claimed in claim 3, wherein: when the polyimide film is laid in a mold, the polyimide film is subjected to flattening treatment.
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| KR101912455B1 (en) * | 2018-04-10 | 2018-10-26 | (주)아이피아이테크 | Polyimide surface treated aerogel insulation materials and method of manufacturing the same |
| WO2020214871A1 (en) * | 2019-04-17 | 2020-10-22 | Cytec Industries Inc. | Light-weight sandwich structure with flame-retardant property and method of making the same |
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| CN1923506B (en) * | 2006-07-19 | 2010-08-04 | 中国航空工业第一集团公司北京航空材料研究院 | Toughening composite material lamination board and method for making same |
| CN104910881B (en) * | 2015-04-21 | 2017-02-22 | 中国石油大学(华东) | Supercritical carbon dioxide completion fluid |
| CN108099222A (en) * | 2017-12-21 | 2018-06-01 | 威海光威复合材料股份有限公司 | It is molded the forming method of phenolic board |
| CN110903507B (en) * | 2019-11-29 | 2022-05-03 | 航天特种材料及工艺技术研究所 | Polyimide composite material preform and preparation method thereof |
| CN211350792U (en) * | 2019-12-30 | 2020-08-25 | 湖南亿达电子材料有限公司 | Composite polyimide film |
| CN112724434A (en) * | 2020-12-23 | 2021-04-30 | 宁波长阳科技股份有限公司 | Transparent polyimide film and preparation method and application thereof |
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| KR101912455B1 (en) * | 2018-04-10 | 2018-10-26 | (주)아이피아이테크 | Polyimide surface treated aerogel insulation materials and method of manufacturing the same |
| WO2020214871A1 (en) * | 2019-04-17 | 2020-10-22 | Cytec Industries Inc. | Light-weight sandwich structure with flame-retardant property and method of making the same |
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