CN115787288A - Polyimide fiber surface modification method and application thereof - Google Patents
Polyimide fiber surface modification method and application thereof Download PDFInfo
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- CN115787288A CN115787288A CN202211624832.1A CN202211624832A CN115787288A CN 115787288 A CN115787288 A CN 115787288A CN 202211624832 A CN202211624832 A CN 202211624832A CN 115787288 A CN115787288 A CN 115787288A
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- 239000004642 Polyimide Substances 0.000 title claims abstract description 90
- 238000002715 modification method Methods 0.000 title claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 29
- 229910052786 argon Inorganic materials 0.000 claims abstract description 23
- 238000012986 modification Methods 0.000 claims abstract description 23
- 230000004048 modification Effects 0.000 claims abstract description 23
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- -1 argon ions Chemical class 0.000 claims abstract description 10
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- 239000013077 target material Substances 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 6
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- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims description 18
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- 239000011159 matrix material Substances 0.000 claims description 8
- 230000002787 reinforcement Effects 0.000 claims description 6
- 229920006231 aramid fiber Polymers 0.000 claims description 3
- 239000000805 composite resin Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920001230 polyarylate Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims description 2
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims description 2
- 229920003192 poly(bis maleimide) Polymers 0.000 claims description 2
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Abstract
The present invention relates to a polyimideThe surface modification method of the imine fiber and the application thereof, the method comprises the following steps: depositing silicon dioxide on the surface of the polyimide fiber by adopting magnetron sputtering to perform surface modification, cleaning the polyimide fiber for 2-10 min by using argon ions for magnetron sputtering, taking the polyimide fiber as a base material, and taking SiO as a material 2 Using high-purity argon as working gas as target material, bombarding SiO with ionized argon ions 2 A target. After the polyimide fiber is subjected to surface modification by adopting the method disclosed by the invention, the interfacial shear strength of the fiber and the resin is obviously improved, and meanwhile, the compressive strength of the fiber is obviously improved.
Description
Technical Field
The invention relates to the technical field of high-performance fibers, in particular to a surface modification method of polyimide fibers.
Background
The polyimide fiber has the characteristics of outstanding mechanical property, high and low temperature resistance, aging resistance, low water absorption, low dielectric, high insulation and the like, can be used for preparing light high-strength composite materials, and has wide application prospects in the fields of aerospace, weaponry and the like. The composite material is composed of reinforced fibers and a resin matrix, and the mechanical property of the fibers and the interface state between the fibers and the resin matrix are important factors influencing the overall mechanical property and service behavior of the composite material.
The polyimide fiber has smooth and chemically inert surface, lacks chemical groups which react with the resin matrix, and is difficult to form effective bonding with the resin matrix during compounding. In addition, as an organic fiber, unlike the strong interlayer pi-pi interaction in carbon fibers, the intermolecular force is weak, and only weak van der waals force is used as lateral support between fibrils, so that the organic fiber is easy to lose efficacy under the action of a compressive load, thereby limiting the application of polyimide fibers in the field of composite materials.
The prior art researches the surface modification technology of polyimide fiber, improves the wettability between fiber and resin by adopting various physical or chemical means, and improves the interface bonding strength. CN104233777A discloses a method for modifying the surface of polyimide fiber, which comprises treating polyimide fiber with plasma, mixing with a solution containing a grafting agent to obtain the surface-modified polyimide fiber, and improving the shear strength of the fiber and resin. CN110284321A discloses a method for modifying polyimide fibers with glucose, nano carbon spheres are synthesized in situ on the surfaces of the polyimide fibers by a hydrothermal reaction method, and carboxyl and hydroxyl are arranged on the surfaces of the carbon spheres, so that the surface active groups of the fibers are increased. CN103966833A discloses a method for modifying the surface of a high-strength high-modulus polyimide fiber with plasma, which improves the wettability of the fiber after plasma treatment, increases the surface free energy, and improves the interlaminar shear strength of the composite material. CN108625163A and CN108660742A disclose methods for modifying graphene oxide and carbon nanotubes on the surface of polyimide fibers, respectively, in order to improve the surface roughness of the fibers, reduce the surface energy, and improve the hydrophilicity and specific surface area thereof, and can be used for enhancing modification of thermoplastics. CN106120304A discloses a continuous treatment method for activating the surface of a polyimide fiber, wherein the surface of the fiber is hydrolyzed and opened in an alkaline environment, then grafting modification is carried out, and active groups are introduced, so that the roughness of the surface of the fiber and the number of the active groups are improved, and the surface activity of the fiber is improved. CN108486888A discloses a method for biomimetic modification of polyimide fiber surface, which obtains a poly-dopamine coated polyimide fiber with high surface polarity and surface energy, and can be used as an enhancer in composite materials or functional materials.
However, in the above prior art, although the polyimide fiber is surface-modified by various physical or chemical methods to introduce active groups and improve the interface bonding strength between the fiber and the resin matrix, none of them can solve the problem of low compressive strength of the polyimide fiber.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide a novel method for modifying a surface of a polyimide fiber, which can improve the bonding strength between the polyimide fiber and a resin interface and further improve the compressive strength of the fiber, thereby solving the disadvantages in the prior art.
The invention also aims to provide application of the polyimide surface modification method.
According to the object of the present invention, the present invention provides a polyimide fiber surface modification method, which comprises the following steps:
depositing silicon dioxide on the surface of the polyimide fiber by adopting magnetron sputtering to carry out surface modification, and cleaning the polyimide fiber by using argon ions for 2-10 min by the magnetron sputtering so as toThe polyimide fiber is taken as a base material and SiO is used 2 Using high-purity argon as working gas as target material, bombarding SiO with ionized argon ions 2 A target.
The polyimide fiber modification method is based on magnetron sputtering, a silicon dioxide layer is deposited on the surface of the polyimide fiber by adopting the magnetron sputtering method, and the excellent wettability of silicon dioxide and resin and the excellent compression resistance of inorganic materials are utilized, so that the bonding strength of the polyimide fiber and the resin interface can be improved, and the compression strength of the fiber can be further improved.
The polyimide fiber used in the present invention is preferably a high-performance polyimide fiber, such as a high-strength high-modulus polyimide fiber.
Preferably, in the method of the present invention, the magnetron sputtering conditions include one or more of the following conditions: background vacuum degree of 1.3X 10 -3 Pa, magnetron sputtering power of 50-350W, magnetron sputtering pressure of 0.5-1.6 Pa, magnetron sputtering time of 5-60 min, room temperature-200 ℃, argon flow of 100sccm, and target base distance of 2-10 cm.
The method adopts magnetron sputtering to carry out surface modification on the polyimide fiber and deposit SiO on the surface of the fiber 2 The interface bonding strength between the fiber and the resin and the compressive strength of the fiber are regulated and controlled by changing the magnetron sputtering condition. The key indexes of regulation include target base distance, magnetron sputtering power, time, temperature and working pressure.
Preferably, in the method of the present invention, the substrate table is rotated at a speed of 5 to 30r/min during the magnetron sputtering. By controlling the rotation speed of the substrate table, siO on the surface of the fiber can be ensured 2 The deposition is uniform.
The surface of the polyimide fiber treated by the method of the invention is uniformly deposited with SiO 2 The layer not only can increase the interfacial shear strength between the fiber and the resin, but also can improve the fiber compression strength.
In addition, the magnetron sputtering method adopted by the invention does not damage the body structure and the mechanical property of the fiber, and is not only suitable for the surface modification of the polyimide fiber and the fabric thereof, but also suitable for the surface modification of other fibers and fabrics such as PBO (poly-p-phenylene benzobisoxazole), aramid fiber, polyarylate and the like.
According to another aspect of the present invention, the present invention provides a surface modified polyimide fiber, which is prepared by the above polyimide fiber modification method, and has an interfacial shear strength of 30MPa or more and a compressive strength of 380MPa or more. The polyimide fiber is excellent not only in the interface bonding strength with the resin matrix but also in the fiber compression strength.
In another aspect, the present invention provides the use of the surface-modified polyimide fiber described above in a composite material. The surface modified polyimide fiber obtained by the method can be used as a reinforcement for composite materials, such as polyimide fiber reinforced resin composite materials formed by resin.
In yet another aspect, the present invention provides a composite material having the above surface-modified polyimide fiber as a reinforcement. The composite material has wide application prospect in the fields of aerospace, weaponry and the like, and can be widely applied to a plurality of fields of rail transit, aerospace, ships, automobiles and the like.
Preferably, in the present invention, the composite material is a polyimide fiber reinforced resin composite material, which is obtained by compounding the surface-modified polyimide fiber as a reinforcement with a resin matrix.
In the present invention, the resin may be a different kind of resin, such as an epoxy resin, a cyanate resin, a bismaleimide resin, a benzoxazine resin, a polyimide resin, and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) After the polyimide fiber is subjected to surface modification by adopting the method disclosed by the invention, the interfacial shear strength of the fiber and the resin is obviously improved, and meanwhile, the compressive strength of the fiber is obviously improved.
(2) By changing the key parameters of target base distance, magnetron sputtering power, time, temperature and working pressure, siO can be effectively controlled 2 The deposition state on the fiber surface can meet different treatment requirements.
(3) The magnetron sputtering method adopted by the invention can not damage the body structure and the mechanical property of the fiber, and is not only suitable for the surface modification of the polyimide fiber and the fabric thereof, but also suitable for the surface modification of other fibers and fabrics such as PBO (poly-p-phenylene benzobisoxazole), aramid fiber, polyarylate and the like.
(4) The surface modified polyimide fiber obtained by the invention can be used as a reinforcement of different resins for composite materials.
Drawings
FIG. 1 is a scanning electron microscope photograph of a polyimide fiber in comparative example 1 of the present invention at a magnification of 1000.
FIG. 2 is a scanning electron microscope photograph of the polyimide fiber after surface modification in example 1 of the present invention at a magnification of 1000.
FIG. 3 is an XPS spectrum of the surface of the polyimide fiber in comparative example 1 of the present invention.
FIG. 4 is an XPS spectrum of the surface-modified polyimide fiber in example 1 of the present invention.
FIG. 5 is an AFM image of a polyimide fiber in comparative example 1 of the present invention.
FIG. 6 is an AFM image of the surface modified fiber in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available. The polyimide fibers used in the examples and comparative examples were high-strength high-modulus polyimide fibers provided by Jiangsu Deno New Material science and technology, inc.
The fiber property test methods and conditions in the following examples and comparative examples are as follows:
the mechanical properties of the fiber are as follows: the tensile breaking strength of the filaments of the fibers was tested according to GB/T14337-2022 "test methods for the tensile Properties of staple fibers for chemical fibers".
Fiber interface shear strength: testing by a composite material interface performance evaluation instrument, wherein the microsphere is formed by curing epoxy resin E51 and D400, and the diameter of the microsphere is 50-80 um;
fiber compressive strength: the tensile resilience is measured by a tensile resilience method, and specific method steps of the tensile resilience method are shown in the following documents: limalone, and the like, the tensile resilience method is used to measure the compressive strength [ J ] of carbon fibers, and the synthetic fiber industry, 2019 (stage 6): 82 to 87.
Example 1:
cleaning polyimide fiber with argon ion for 10min, and cleaning with SiO 2 Taking high-purity argon as working gas as a target material, and carrying out magnetron sputtering treatment on the polyimide fiber under the following conditions: background vacuum degree of 1.3X 10 -3 Pa, magnetron sputtering power of 100W, magnetron sputtering pressure of 0.5Pa, magnetron sputtering time of 60min, room temperature, argon flow of 100sccm, target base distance of 7cm, and substrate table rotation at 5 r/min.
Example 2:
cleaning polyimide fiber with argon ion for 10min, and cleaning with SiO 2 Taking high-purity argon as working gas as a target material, and carrying out magnetron sputtering treatment on the polyimide fiber under the following conditions: background vacuum degree of 1.3X 10 -3 Pa, magnetron sputtering power of 100W, magnetron sputtering pressure of 1.6Pa, magnetron sputtering time of 60min, temperature of 200 deg.C, argon flow of 100sccm, target substrate distance of 7cm, and substrate table rotation at 5 r/min.
Example 3:
cleaning polyimide fiber with argon ion for 10min, and cleaning with SiO 2 Taking high-purity argon as working gas as a target material, and carrying out magnetron sputtering treatment on the polyimide fiber under the following conditions: background vacuum degree of 1.3X 10 -3 Pa, magnetron sputtering power of 350W, magnetron sputtering pressure of 0.5Pa, magnetron sputtering time of 60min, room temperature, argon flow of 100sccm, target substrate distance of 2cm, and substrate table rotation at 10 r/min.
Example 4:
cleaning polyimide fiber with argon ion for 10min, and cleaning with SiO 2 As target material, high-purity argon as working gas, and polyimide fiberCarrying out magnetron sputtering treatment on the alloy material under the following conditions: background vacuum degree of 1.3X 10 -3 Pa, magnetron sputtering power of 50W, magnetron sputtering pressure of 0.5Pa, magnetron sputtering time of 5min, room temperature, argon flow of 100sccm, target substrate distance of 10cm, and substrate table rotation at 30 r/min.
Comparative example 1:
polyimide fibers which are not subjected to surface modification treatment.
The surface-modified polyimide fibers obtained in examples 1 to 4 and the polyimide fiber of comparative example 1, which was not subjected to the surface modification treatment, were measured for tensile breaking strength, interfacial shear strength (IFSS), and compressive strength of the monofilament, respectively, and the results are shown in table 1 below.
TABLE 1
| Tensile Strength at Break for monofilament (MPa) | Interfacial shear strength (MPa) | Compressive Strength (MPa) | |
| Example 1 | 3992±282.5 | 40.82±2.77 | 497 |
| Example 2 | 3976±254.8 | 46.57±2.67 | 586 |
| Example 3 | 3947±290.6 | 48.36±2.14 | 612 |
| Example 4 | 3983±307.4 | 33.43±4.73 | 446 |
| Comparative example 1 | 3923±300.3 | 27.45±5.77 | 341 |
As shown in Table 1, in examples 1 to 4, the interfacial shear strength of the fiber and the resin is significantly improved and the compressive strength of the fiber is significantly improved as compared with comparative example 1. This shows that the compressive strength of the polyimide fiber can be further improved while the interface bonding strength of the polyimide fiber and the resin is improved after the surface modification of the polyimide fiber by the magnetron sputtering method of the present invention.
FIG. 1 is a scanning electron microscope photograph of a polyimide fiber of comparative example 1 of the present invention at a magnification of 1000; FIG. 2 is a scanning electron microscope image of the polyimide fiber subjected to surface modification in example 1 of the present invention at a magnification of 1000; FIG. 3 is an XPS spectrum of the surface of a polyimide fiber in comparative example 1 of the present invention; FIG. 4 is an XPS spectrum of the surface of the polyimide fiber after surface modification in example 1 of the present invention; FIG. 5 is an AFM image of a polyimide fiber in comparative example 1 of the present invention; FIG. 6 is an AFM image of the surface modified fiber in example 1 of the present invention.
As can be seen from comparing FIG. 1 and FIG. 2, the SiO is deposited on the surface of the polyimide fiber by magnetron sputtering 2 Later, the fiber surface SiO 2 The layer deposition is uniform. As can be seen from a comparison of FIGS. 3 and 4, magnetron sputtering is used to form the polymerDeposition of SiO on the surface of imide fibers 2 After that, the silicon atom content on the fiber surface increases. As can be seen from the comparison between FIG. 5 and FIG. 6, the SiO is deposited on the surface of the polyimide fiber by magnetron sputtering 2 After that, the fiber surface roughness increases.
In addition, the same tests as in example 1 were carried out for the surface-modified polyimide fibers in examples 2 to 4 of the present invention, and the results of tests similar to those in FIGS. 2, 4 and 6 were obtained for all of them.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. A polyimide fiber surface modification method is characterized by comprising the following steps:
depositing silicon dioxide on the surface of the polyimide fiber by adopting magnetron sputtering to perform surface modification, cleaning the polyimide fiber for 2-10 min by using argon ions for magnetron sputtering, taking the polyimide fiber as a base material, and taking SiO as a material 2 Using high-purity argon as working gas as target material, bombarding SiO with ionized argon ions 2 A target.
2. The method of claim 1, wherein the magnetron sputtering conditions comprise: the magnetron sputtering power is 50-350W, the magnetron sputtering pressure is 0.5-1.6 Pa, the magnetron sputtering time is 5-60 min, and the temperature is room temperature-200 ℃; and/or
Background vacuum degree of 1.3X 10 -3 Pa, the target base distance is 2-10 cm, and the argon flow is 100sccm.
3. The method according to claim 1 or 2, characterized in that during the magnetron sputtering the substrate table is rotated at a speed of 5-30 r/min.
4. The method according to claim 1 or 2, characterized in that some or all of the polyimide fibers are replaced by PBO fibers, aramid fibers and/or polyarylate fibers.
5. A surface-modified polyimide fiber, which is obtained by the method according to any one of claims 1 to 3, and has an interfacial shear strength of not less than 30MPa and a compressive strength of not less than 380MPa.
6. Use of the surface-modified polyimide fiber of claim 5 in the preparation of a composite material.
7. A composite material comprising the surface-modified polyimide fiber according to claim 5 as a reinforcement.
8. The composite material according to claim 7, wherein the composite material is a polyimide fiber-reinforced resin composite material, and is obtained by compounding the surface-modified polyimide fiber as a reinforcement with a resin matrix.
9. Composite according to claim 8, characterized in that the resin is an epoxy resin, a cyanate ester resin, a bismaleimide resin, a benzoxazine resin and/or a polyimide resin.
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