CN114276574B - High-temperature-resistant polyimide/polyaryletherketone composite membrane and interface strengthening method thereof - Google Patents
High-temperature-resistant polyimide/polyaryletherketone composite membrane and interface strengthening method thereof Download PDFInfo
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Abstract
A high temperature resistant polyimide/polyaryletherketone composite membrane and an interface strengthening method thereof belong to the technical field of material preparation. The interface strengthening method of the high-temperature resistant polyimide/polyaryletherketone composite membrane comprises the following steps: spraying an active grafting agent (4-alkynyl imidoyl terminated PAEK oligomer) solution on the surface of the PI film after impurity removal; etching and grafting by adopting a low-temperature plasma surface treatment method; spraying PAEK aqueous emulsion on the surface of the grafted and modified PI film in an atomizing manner, heating and drying, continuously heating to 350-420 ℃, keeping the temperature to ensure that the PAEK is fully melted, and cooling to room temperature at the cooling rate of 1-5 ℃/min to obtain a high-temperature-resistant polyimide/polyaryletherketone composite film; the composite film has excellent interface bonding strength, can be used as a wrapping insulating layer, and can be widely applied to the field of high-temperature resistant electromagnetic wires with harsh service environments.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a high-temperature-resistant polyimide/polyaryletherketone composite membrane and an interface strengthening method thereof.
Background
The Polyimide (PI) film has excellent electrical insulation performance, has excellent tolerance to common organic solvents, mineral oil, aviation kerosene and the like, and is widely used as a wrapping insulation layer of an electromagnetic wire. The high-performance PI film is prepared by dehydrating and ring-closing aromatic heterocyclic structured polyamic acid at high temperature, and besides ring-closing dehydration in a molecular chain, dehydration among molecular chains can also occur to form a high-rigidity cross-linked network structure; therefore, the PI film cannot be dissolved in an organic solvent and is difficult to melt even at high temperatures. This results in PI film lapped wires that cannot be formed into hermetic insulation by the heat melt-cool consolidation mechanism as do other thermoplastic resin film lapped wires. At present, the PI film lapped wire mainly adopts F46 resin as a bonding agent, and fills a gap between layers of a PI film winding structure to form an integrally sealed lapped insulating layer. However, the melting point of the F46 resin is 240-260 ℃, when the using temperature of the winding is higher than 260 ℃, the bonding performance is reduced to cause debonding, and the structure of the insulating layer is changed.
The Polyaryletherketone (PAEK) comprises polyetheretherketone, polyetherketoneketone, polyetheretherketoneketone and the like, is a high-performance thermoplastic resin, has a melting point of 340-410 ℃, and can regulate and control the crystallinity, melting point, melt viscosity and high-temperature thermal decomposition performance of the PAEK by changing the relative content, bonding sequence and molecular weight of aromatic ether bonds and aromatic ketone bonds. The temperature resistance of the PAEK is far better than that of F46, and the use temperature of the PAEK is obviously improved by replacing the adhesive of the F46 used as the insulating layer of the PI lapping wire. The PAEK is a semi-crystalline polymer material, the cohesion among molecular chains is strong, and the mechanical property is very excellent; the compatibility between the PAEK semi-crystalline structure and the PI film amorphous crosslinking structure is poor, so that the interface bonding strength between the PAEK and the PI film is relatively low, and debonding and peeling are easy to occur between the PAEK and the PI film after the PAEK and the PI film are subjected to high-low temperature cyclic fatigue. Therefore, improving the interface bonding performance between the PI/PAEK composite films is a key technical way for improving the working temperature of the PI lapping wire.
The plasma is a mixture of electrons, ions, atoms, atomic groups and the like generated by ionizing gas molecules, and is known as a fourth state of a substance; the low-temperature plasma is a non-equilibrium plasma, the temperature of electrons is far lower than that of heavy particles, and the whole system is in a low-temperature state. The surface treatment method of the low-temperature plasma is characterized in that a large number of active particles such as ions, electrons, excited atoms, free radicals and the like in the plasma collide with the surface of an object to generate a physical and chemical reaction, the surface is etched to form a nano-grade uneven shape, and meanwhile, a plurality of novel groups or molecular chain segments are introduced to the surface through a grafting reaction; the technology does not need a solvent and a post-treatment process, has simple process, is green and efficient, and is a very promising surface/interface modification technology.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-temperature resistant polyimide/polyaryletherketone composite membrane and an interface strengthening method thereof. The high-temperature resistant polyimide/polyaryletherketone composite membrane prepared by the method has excellent interface bonding strength and bright application prospect in the field of high-temperature resistant electromagnetic wire insulation.
The invention relates to a method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane, which comprises the following steps of:
s1: surface pretreatment of PI film
Removing impurities on the surface of the PI film, spraying an active grafting agent solution with the mass percentage concentration of 0.5-5%, heating and drying to remove the solvent in the solution, and obtaining a pretreated PI film;
the active grafting agent is one or a mixture of more than one of PAEK oligomer terminated by 4-alkynyl imido group:
the structural formula is as follows:
wherein R is a hydrogen atom or a benzene ring;
n is a positive integer less than 10;
x is
A structure of (1);
s2: etching graft treatment by low-temperature plasma surface treatment method
Etching and grafting the surface of the pretreated PI film by adopting a low-temperature plasma surface treatment method, and grafting an active grafting agent to obtain a graft modified PI film;
s3: high-temperature-resistant polyimide/polyaryletherketone composite membrane
Spraying PAEK aqueous emulsion on the surface of a grafted and modified PI film in an atomizing manner by adopting a spraying method, heating and drying, continuously heating to 350-420 ℃, preserving the temperature to ensure that the PAEK is fully melted, and cooling to room temperature at the cooling rate of 1-5 ℃/min to obtain the high-temperature resistant polyimide/polyaryletherketone composite film.
In the step S1, the method for removing impurities comprises: wiping with solvent, preferably one or more of methanol, ethanol, acetone, and ethyl acetate.
In the step S1, the spraying thickness is 50-200 nm.
In S1, the solvent adopted by the active grafting agent solution is one or a mixture of more of dichloromethane, chloroform, dimethylformamide, dimethylacetamide and N-methylpyrrolidone.
And in the S1, heating and drying are carried out, wherein the heating temperature is 30-200 ℃.
In S2, the distance between the low-temperature plasma electrode and the surface of the pretreated PI film is 0.5-2 cm, the discharge power is 10W-1000W, and the treatment time is 1-10S;
in S3, the heating and drying temperature is 120-150 ℃.
In the S3, the PAEK aqueous emulsion is an emulsified dispersion of PAEK particles in water, the mass percentage concentration of the PAEK aqueous emulsion is 15-50%, and the particle size of the PAEK particles is 100-1000 meshes.
In S3, the heat preservation time is preferably 1-5 min.
In S3, the thickness of the polyaryletherketone film of the high-temperature resistant polyimide/polyaryletherketone composite film is 0.01-0.2 mm.
In S3, the PAEK is one or a mixture of polyether ether ketone (PEEK), polyether ether ketone (PEEKK), polyether ketone (PEKK), and polyether ketone ether ketone (PEKK).
The high-temperature-resistant polyimide/polyaryletherketone composite membrane is prepared by adopting the interface strengthening method of the high-temperature-resistant polyimide/polyaryletherketone composite membrane, and the PI/PAEK interface bonding strength of the obtained high-temperature-resistant polyimide/polyaryletherketone composite membrane is 35-40 MPa.
The invention relates to a high temperature resistant polyimide/polyaryletherketone composite membrane and an interface strengthening method thereof, which have the following beneficial effects:
1) The thermal decomposition temperature of both PI and PAEK is more than 500 ℃; the melting temperature of the PAEK is more than 340 ℃; the lapping insulating layer formed by the PI/PAEK composite film can not be decomposed and carbonized at the high temperature of 300-400 ℃, and the high temperature resistance of the electromagnetic wire is obviously improved.
2) Aiming at the molecular characteristics of PI and PAEK, a plasma surface treatment method is adopted to modify the surface of the PI film, and the active particle impact in the plasma improves the roughness of the PI film; meanwhile, the active free radicals in the plasma are utilized to initiate the grafting reaction of the PAEK oligomer terminated by 4-alkynyl imide, so that the chemical characteristics of the surface of the PI film are changed; both mechanisms are beneficial to improving the wetting property of the surface of the PI film, and further improving the interface bonding property between the PI film and the PAEK coating.
3) The grafting agent is a 4-alkynyl imide terminated PAEK oligomer, alkynyl can generate free radical polymerization reaction, and can be trimerized to form an aromatic heterocyclic structure at high temperature, so that the high-temperature chemical stability of the PI/PAEK composite membrane is maintained; the imide group has good compatibility with the molecular chain of the PI film, and the aryl ether ketone framework has good compatibility with the PAEK resin adhesive.
4) The spraying amount of the spraying method can be accurately controlled, the repeatability is good, the operation is simple, and the industrial amplification is easy.
5) The high-temperature-resistant PI/PAEK composite film provided by the invention has important influence on improving the heat-resistant grade, reliability/durability and service life of an electromagnetic wire, and has bright application prospect in various fields such as oil exploitation, aviation and aerospace, machinery, nuclear energy and the like.
Drawings
FIG. 1 is a schematic structural diagram of a PI/PAEK composite membrane.
FIG. 2 is a surface topography of the PI/PEEK composite film.
Detailed Description
In the following examples, the active grafting agent (4-alkynylimidyl terminated PAEK oligomer) was synthesized by a two-step process:
4,4 '-difluorobenzophenone and dihydric phenol (one or a mixture of resorcinol, hydroquinone, 4,4' -biphenol, 1,4-naphthalenediol, 2,6-naphthalenediol, 2,7-naphthalenediol and hexafluorobisphenol A) are used as raw materials, 4-aminophenol is used as an end capping agent, carbonate (one or a mixture of potassium carbonate, sodium carbonate and magnesium carbonate) is used as a catalyst, and the raw materials are reacted in a high-boiling aprotic polar solvent (one or a mixture of dimethylformamide, dimethylacetamide and N-methylpyrrolidone) at 150-210 ℃ for 6-12 hours to obtain the amino-terminated PAEK oligomer. Wherein, according to the mol ratio, 4,4' -difluorobenzophenone, dihydric phenol, 4-aminophenol: catalyst = (1.1-2): 1, (0.2-1): 2.
Dissolving the amino-terminated PAEK oligomer and 4-alkynyl phthalic anhydride in an aprotic polar solvent (one of dimethylformamide, dimethylacetamide and N-methylpyrrolidone), and stirring at room temperature for 4-8 hours; heating to 60-80 ℃, adding a dehydrating agent (acetic anhydride and/or propionic anhydride) and an acetate catalyst (sodium acetate and/or cobalt acetate) to react for 4-10 hours to obtain the 4-alkynyl imido group-terminated PAEK oligomer. Wherein, the usage amount of the 4-alkynyl phthalic anhydride, the dehydrating agent and the acetate catalyst is 2 to 2.2 times of that of the amino-terminated PAEK oligomer according to the mol ratio.
The following further describes the specific embodiments of the present invention in combination with the technical solutions.
In the following examples, the preparation of corresponding composite membranes was performed according to the PAEK type, and the schematic structure thereof is shown in fig. 1.
Example 1
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by using acetone to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 3% on the surface, spraying the active grafting agent solution with the thickness of 50nm, heating to 30 ℃ and drying to obtain a pretreated PI film;
in the active grafting agent solution used in this example, the molecular structure of the active grafting agent is:
the solvent used was dichloromethane.
(2) And (3) carrying out etching grafting treatment on the surface of the pretreated PI film by using low-temperature plasma, wherein the distance between a low-temperature plasma electrode and the surface of the PI film is 1.5cm, the discharge power is 650W, and the treatment time is 3s, so that the graft modified PI film is obtained.
(3) Spraying 25% of PEEK aqueous emulsion with solid content of 500 meshes on the surface of the graft modified PI film in an atomizing manner by adopting a spraying method, and heating at 150 ℃ for 30min to remove moisture; and then heating to 350 ℃, preserving the heat for 5min to fully melt the PEEK, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEEK composite film, wherein the thickness of the PEEK film is 0.01mm.
(4) The interfacial bonding strength of the PI/PEEK composite film is 35.5MPa, the surface topography of the PI/PEEK composite film prepared by the embodiment is shown in figure 2, most PEEK particles are melted, expanded and uniformly adhered to the surface of the PI film, and no layering phenomenon occurs.
Example 2
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by using acetone to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 4% on the surface, and spraying the active grafting agent solution with the thickness of 50nm; heating to 50 ℃ and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the molecular structural formula of the active grafting agent is:
chloroform is used as solvent.
(2) And (3) carrying out etching grafting treatment on the surface of the pretreated PI film by using low-temperature plasma, wherein the distance between a low-temperature plasma electrode and the surface of the PI film is 2cm, the discharge power is 1000W, and the treatment time is 1s, so that the graft modified PI film is obtained.
(3) Spraying 15% of PEEK aqueous emulsion with solid content of 1000 meshes on the surface of the graft modified PI film in an atomizing manner by adopting a spraying method, and heating at 150 ℃ for 30min to remove moisture; and then heating to 380 ℃, preserving heat for 1min to fully melt the PEEK, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEEK composite film, wherein the thickness of the PEEK film is 0.05mm.
(4) The interface bonding strength of the PI/PEEK composite film is 36.3MPa.
Example 3
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by using acetone to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 0.5% on the surface, spraying the active grafting agent solution with the thickness of 100nm, heating to 50 ℃ and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the molecular structural formula of the active grafting agent is:
the solvent used was a 4:1 mixed solution of dichloromethane and chloroform.
(2) And (3) etching and grafting the surface of the pretreated PI film by using low-temperature plasma, so that the surface roughness of the PI is increased, and an active grafting agent (4-alkynyl imido terminated PAEK oligomer) is grafted. The distance between the low-temperature plasma electrode and the surface of the PI film is 1cm, the discharge power is 400W, and the treatment time is 10s, so that the grafted and modified PI film is obtained.
(3) Spraying PEKK aqueous emulsion with 15% solid content and 500 meshes on the surface of the grafted and modified PI film in an atomizing way by adopting a spraying method, and heating at 150 ℃ for 30min to remove water; and then heating to 410 ℃, keeping the temperature for 5min to fully melt the PEKK, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEKK composite membrane, wherein the thickness of the PEKK membrane is 0.1mm.
(4) The interface bonding strength of the PI/PEKK composite membrane is 38.2MPa.
Example 4
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by adopting ethanol to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 1% on the surface, spraying the active grafting agent solution with the thickness of 100nm, heating to 150 ℃, and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the molecular structural formula of the active grafting agent is:
the solvent used was dimethylformamide.
(2) And (3) carrying out etching grafting treatment on the surface of the pretreated PI film by using low-temperature plasma, wherein the distance between a low-temperature plasma electrode and the surface of the PI film is 0.5cm, the discharge power is 10W, and the treatment time is 10s, so that the grafted and modified PI film is obtained.
(3) Spraying PEKK aqueous emulsion with 30% solid content and 300-mesh particle size on the surface of the grafted and modified PI film in an atomizing manner by adopting a spraying method, heating at 150 ℃ for 30min, and drying to remove moisture; and then heating to 420 ℃, preserving heat for 2min to enable the PEEK to be fully melted, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEKK composite membrane, wherein the thickness of the PEKK membrane is 0.05mm.
(4) The interface bonding strength of the PI/PEKK composite membrane is 36.9MPa.
Example 5
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by using acetone to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 1% on the surface, spraying the active grafting agent solution with the thickness of 100nm, heating to 160 ℃, and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the molecular structural formula of the active grafting agent is:
the solvent used is dimethylacetamide.
(2) And (3) etching and grafting the surface of the pretreated PI film by using low-temperature plasma, so that the surface roughness of the PI is increased, and an active grafting agent (4-alkynyl imido terminated PAEK oligomer) is grafted. The distance between the low-temperature plasma electrode and the surface of the PI film is 1.5cm, the discharge power is 650W, and the treatment time is 2s, so that the grafted and modified PI film is obtained.
(3) Spraying PEKK aqueous emulsion with 50% solid content and 100-mesh particle size on the surface of the grafted and modified PI film in an atomizing manner by adopting a spraying method, and heating at 150 ℃ for 30min to remove water; and then heating to 380 ℃, preserving the heat for 5min to fully melt the PAEK, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEKK composite membrane, wherein the thickness of the PEKK membrane is 0.05mm.
(4) The interface bonding strength of the PI/PEKK composite membrane is 36.8MPa.
Example 6
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by adopting ethyl acetate to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 5% on the surface, spraying the active grafting agent solution with the thickness of 150nm, heating to 60 ℃, and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the molecular structural formula of the active grafting agent is:
the solvent used was dichloromethane.
(2) And (3) carrying out etching grafting treatment on the surface of the pretreated PI film by adopting low-temperature plasma, wherein the distance between a low-temperature plasma electrode and the surface of the PI film is 2cm, the discharge power is 1000W, and the treatment time is 1s.
(3) Spraying PEEKK aqueous emulsion with 20% solid content and 500 meshes on the surface of the grafted and modified PI film in an atomizing way by adopting a spraying method, and heating at 150 ℃ for 30min to remove water; and then heating to 380 ℃, preserving the heat for 5min to fully melt the PEEKK, and cooling at the cooling rate of 5 ℃/min to obtain the PI/PEEKK composite membrane, wherein the thickness of the PEEKK membrane is 0.15mm. .
(4) The interface bonding strength of the PI/PEEKK composite membrane is 38.7MPa.
Example 7
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by adopting methanol to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 3% on the surface, spraying the active grafting agent solution with the thickness of 200nm, heating to 200 ℃ and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the molecular structural formula of the active grafting agent is:
the solvent used is N-methyl pyrrolidone.
(2) And (3) carrying out etching grafting treatment on the surface of the pretreated PI film by using low-temperature plasma, wherein the distance between a low-temperature plasma electrode and the surface of the PI film is 1.5cm, the discharge power is 300W, and the treatment time is 8s, so that the graft modified PI film is obtained.
(3) Spraying PEKEKK aqueous emulsion with the solid content of 15% and the particle size of 500 meshes on the surface of the grafted and modified PI film in an atomizing manner by adopting a spraying method, and heating the surface of the grafted and modified PI film at 150 ℃ for 30min to remove water; and then heating to 400 ℃, keeping the temperature for 5min to fully melt the PEKEKK, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEKEKK composite membrane, wherein the thickness of the PEKEKK membrane is 0.2mm. .
(4) The interface bonding strength of the PI/PEKEKK composite membrane is 39.5MPa.
Example 8
A method for strengthening an interface of a high-temperature-resistant polyimide/polyaryletherketone composite membrane specifically comprises the following steps:
(1) And (3) pretreating the surface of the PI film by adopting methanol to remove surface stains and dust. Then, spraying an active grafting agent solution with the mass percentage concentration of 3% on the surface, spraying the active grafting agent solution with the thickness of 200nm, heating to 200 ℃ and drying to obtain a pretreated PI film;
in the active grafting agent solution adopted in this example, the active grafting agent is a mixture of two molecular structural formulas, which are respectively:
the molar ratio of the two is 1:1, and the solvent is N-methyl pyrrolidone.
(2) And (3) carrying out etching grafting treatment on the surface of the pretreated PI film by using low-temperature plasma, wherein the distance between a low-temperature plasma electrode and the surface of the PI film is 1.5cm, the discharge power is 800W, and the treatment time is 6s, so that the graft modified PI film is obtained.
(3) Spraying the mixture of PEKEKK and PEKK with 30% solid content and 300 meshes on the surface of the grafted and modified PI film by adopting a spraying method, heating at 150 ℃ for 30min, and drying to remove water; and then heating to 400 ℃, keeping the temperature for 5min to fully melt the PEKEKK, and cooling at a cooling rate of 5 ℃/min to obtain the PI/PEKEKK/PEKK composite membrane, wherein the thickness of the PEKEKK/PEKK membrane is 0.15mm.
(4) The interface bonding strength of the PI/PEKEKK/PEKK composite membrane is 39.2MPa.
Comparative example 1
A preparation method of a composite membrane is the same as that of the embodiment 1, and is different in that the steps (1) to (2) are omitted, 25% of PEEK aqueous emulsion with the solid content of 500 meshes is directly sprayed on the surface of the PI, drying is carried out to remove water, then the temperature is raised to 350 ℃, the temperature is kept for 5min to enable the PEEK to be fully melted, the temperature is reduced at the cooling rate of 5 ℃/min, and the PEEK membrane is stripped from the surface of the PI in the temperature reduction process.
Comparative example 2
The preparation method of the composite film is the same as that in the example 1, except that the step (2) is omitted, the microstructure of the obtained composite film shows that the PEEK melt is not spread sufficiently, the surface is irregularly distributed with a plurality of bulges, and the interface bonding strength is lower than 20MPa.
Claims (10)
1. A method for strengthening the interface of a high-temperature resistant polyimide/polyaryletherketone composite membrane is characterized by comprising the following steps:
s1: surface pretreatment of PI film
Spraying an active grafting agent solution with the mass percentage concentration of 0.5-5% on the surface of the PI film after impurity removal, and heating and drying to remove the solvent in the solution to obtain a pretreated PI film;
the active grafting agent is one or a mixture of more than one of PAEK oligomer terminated by 4-alkynyl imido group:
the structural formula is as follows:
wherein R is a hydrogen atom or a benzene ring;
n is a positive integer less than 10;
x is
A structure of (1);
s2: etching grafting treatment by low-temperature plasma surface treatment method
Etching and grafting the surface of the pretreated PI film by adopting a low-temperature plasma surface treatment method, and grafting an active grafting agent to obtain a graft modified PI film;
s3: high-temperature-resistant polyimide/polyaryletherketone composite membrane
Spraying PAEK aqueous emulsion on the surface of a grafted and modified PI film in an atomizing manner by adopting a spraying method, heating and drying, continuously heating to 350-420 ℃, preserving the temperature to ensure that the PAEK is fully melted, and cooling to room temperature at the cooling rate of 1-5 ℃/min to obtain the high-temperature resistant polyimide/polyaryletherketone composite film.
2. The interface strengthening method of the high-temperature-resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S1, the impurity removal method comprises the following steps: wiping with solvent, wherein the solvent is one or more of methanol, ethanol, acetone, and ethyl acetate.
3. The method for strengthening the interface of the high-temperature-resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S1, the spraying thickness is 50-200 nm.
4. The method for strengthening the interface of the high-temperature-resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S1, the solvent adopted by the active grafting agent solution is one or a mixture of more of dichloromethane, chloroform, dimethylformamide, dimethylacetamide and N-methylpyrrolidone.
5. The method for strengthening the interface of the high-temperature-resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S1, the polyimide/polyaryletherketone composite membrane is heated and dried at a temperature of 30-200 ℃.
6. The method for strengthening the interface of the high-temperature-resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S2, the distance between the low-temperature plasma electrode and the surface of the pretreated PI film is 0.5-2 cm, the discharge power is 10W-1000W, and the treatment time is 1-10S.
7. The method for strengthening the interface of the high temperature resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S3, PAEK is one or a mixture of polyether ether ketone, polyether ether ketone, polyether ketone, and polyether ketone ether ketone.
8. The method for strengthening the interface of the high-temperature-resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in the step S3, the PAEK aqueous emulsion is an emulsified dispersion of PAEK particles in water, the mass percentage concentration of the PAEK aqueous emulsion is 15-50%, and the particle size of the PAEK particles is 100-1000 meshes.
9. The interface strengthening method of the high temperature resistant polyimide/polyaryletherketone composite membrane according to claim 1, wherein in S3, the heating and drying temperature is 120-150 ℃; the heat preservation time is 1-5 min.
10. A high temperature resistant polyimide/polyaryletherketone composite membrane is characterized in that the high temperature resistant polyimide/polyaryletherketone composite membrane interface strengthening method is adopted to obtain the high temperature resistant polyimide/polyaryletherketone composite membrane, the thickness of the polyaryletherketone membrane of the high temperature resistant polyimide/polyaryletherketone composite membrane is 0.01-0.2 mm, and the PI/PAEK interface bonding strength of the obtained high temperature resistant polyimide/polyaryletherketone composite membrane is 35-40 MPa.
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|---|---|---|---|---|
| JP2011245856A (en) * | 2010-04-26 | 2011-12-08 | Ube Industries Ltd | Laminated film |
| CN113105620A (en) * | 2021-04-13 | 2021-07-13 | 吉林大学 | Amino-terminated soluble polyaryletherketone and preparation method and application thereof |
| CN113488224A (en) * | 2021-06-16 | 2021-10-08 | 上海申茂电磁线有限公司 | PEEK crowded package polyimide film is around chartered line |
| CN113963861A (en) * | 2021-10-28 | 2022-01-21 | 沈阳方舟石油科技发展有限公司 | PI/PEEK composite insulation lapped wire and preparation method thereof |
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| EP3765283A4 (en) * | 2018-03-13 | 2021-11-10 | Arkema, Inc. | Film laminates based on polyaryletherketones |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011245856A (en) * | 2010-04-26 | 2011-12-08 | Ube Industries Ltd | Laminated film |
| CN113105620A (en) * | 2021-04-13 | 2021-07-13 | 吉林大学 | Amino-terminated soluble polyaryletherketone and preparation method and application thereof |
| CN113488224A (en) * | 2021-06-16 | 2021-10-08 | 上海申茂电磁线有限公司 | PEEK crowded package polyimide film is around chartered line |
| CN113963861A (en) * | 2021-10-28 | 2022-01-21 | 沈阳方舟石油科技发展有限公司 | PI/PEEK composite insulation lapped wire and preparation method thereof |
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