CN116751381B - Preparation method of high-performance carbon fiber reinforced PEEK prepreg and PEEK substrate material - Google Patents
Preparation method of high-performance carbon fiber reinforced PEEK prepreg and PEEK substrate material Download PDFInfo
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- CN116751381B CN116751381B CN202310210897.XA CN202310210897A CN116751381B CN 116751381 B CN116751381 B CN 116751381B CN 202310210897 A CN202310210897 A CN 202310210897A CN 116751381 B CN116751381 B CN 116751381B
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- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 134
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 134
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 107
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 107
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 title claims abstract 24
- 239000000463 material Substances 0.000 title claims description 41
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- 238000003892 spreading Methods 0.000 claims abstract description 13
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- 238000000748 compression moulding Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
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- 238000004804 winding Methods 0.000 claims abstract description 9
- 238000007598 dipping method Methods 0.000 claims abstract description 3
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- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 28
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000002048 multi walled nanotube Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 15
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- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
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- QVWTVJHDWLMMTC-UHFFFAOYSA-N fluoro octanoate Chemical compound CCCCCCCC(=O)OF QVWTVJHDWLMMTC-UHFFFAOYSA-N 0.000 claims description 3
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- 238000004519 manufacturing process Methods 0.000 claims description 2
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- 239000002131 composite material Substances 0.000 abstract description 15
- 239000002585 base Substances 0.000 description 23
- 239000000843 powder Substances 0.000 description 16
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- 230000000052 comparative effect Effects 0.000 description 9
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- 239000012456 homogeneous solution Substances 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 229920006351 engineering plastic Polymers 0.000 description 3
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- 239000004416 thermosoftening plastic Substances 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000004918 carbon fiber reinforced polymer Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
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- 229920005992 thermoplastic resin Polymers 0.000 description 2
- SNGREZUHAYWORS-UHFFFAOYSA-M 2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoate Chemical compound [O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-M 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011304 carbon pitch Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 239000011259 mixed solution Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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- 230000001376 precipitating effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- 238000007655 standard test method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/248—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using pre-treated fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K9/00—Use of pretreated ingredients
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention relates to a preparation method of a high-performance carbon fiber reinforced PEEK prepreg and a PEEK base plate, which comprise the following steps: s1, preparing a PEEK-containing suspension; s2, spreading the tows of the carbon fibers and then carrying out surface treatment to obtain pretreated carbon fibers; s3, immersing the pretreated carbon fiber into the suspension for dipping treatment, drying, extruding for molding, cooling and winding to obtain the carbon fiber reinforced polyether-ether-ketone prepreg; the PEEK base plate is obtained by compression molding after the carbon fiber reinforced PEEK prepreg is paved. The plate composite material has the advantages of good mechanical property, excellent wear resistance and low cost.
Description
Technical Field
The invention relates to the technical field of carbon fiber reinforced thermoplastic resin composite materials, in particular to a preparation method of a high-performance carbon fiber reinforced PEEK prepreg and a PEEK base plate.
Background
The specific strength and specific modulus of the carbon fiber reinforced thermoplastic resin matrix composite material are several times higher than those of pure engineering materials or short fiber reinforced engineering plastics. The composite material prepared by combining the composite material with a matrix is widely applied to various fields such as aerospace, national defense war industry, high-end civil industry, sports goods and the like.
Polyether ether ketone (PEEK) is made into semi-crystalline aromatic thermoplastic special engineering plastic by virtue of a rigid benzene ring, a flexible ether bond, carbonyl for improving intermolecular acting force and a regular structure on a macromolecular chain. Compared with other traditional engineering plastics, the plastic has the advantages of excellent comprehensive mechanical property, dimensional stability, heat resistance, chemical corrosion resistance, good self-lubricating property, peeling resistance, biocompatibility, good insulativity, easiness in processing and forming and the like. Due to the excellent characteristics, PEEK is widely applied to the fields of aerospace, military industry, automobiles, ships, instruments, medical treatment and the like. With the continuous increase of the requirements of various fields on the material performance, the application fields of the material are gradually expanding.
In industrial production or life, antifriction and wear-resistant materials are indispensable, and with the increase of use requirements, resin-based wear-resistant materials are actively developed with their unique advantages (light weight, self-lubrication, easy processing, etc.). The PEEK has good self-lubricity, so that the PEEK becomes an important antifriction and wear-resistant material, and can keep good wear resistance in a certain load, sliding speed and temperature range. And thus is widely used in various rotating and transmitting devices. However, with the rigor of equipment use environment and the continuous improvement of service life requirements, the requirements on materials are also higher and higher, and the pure PEEK resin is difficult to meet the complicated working condition requirements. The PEEK resin is reinforced by continuous fibers and modified by various fillers, and is an important way for improving the friction performance of PEEK resin and reducing the cost.
The prior art of the continuous carbon fiber reinforced polyether-ether-ketone composite material is as follows: the invention patent with application number 2021114043178 discloses a preparation method of a unidirectional prepreg tape of a high-temperature-resistant thermoplastic composite material, which comprises the steps of firstly preparing a resin solution, then carrying out precipitation treatment after fibers are fully soaked in the resin solution, precipitating the resin from the solution by using a precipitation agent to attach the resin on the fibers, realizing solvent recovery and preliminary shaping of the prepreg tape, and obtaining the unidirectional prepreg tape of the fiber-reinforced high-temperature-resistant thermoplastic composite material through drying, high-temperature shaping, cooling and winding.
The invention patent with application number 2022100802581 discloses a preparation method of a high-solid-content polyether-ether-ketone aqueous suspension and composite fibers, wherein the suspension comprises dispersed phase PEEK resin powder, a surfactant and continuous phase deionized water, and the solid content of the suspension is 10-40 mass%; the composite fiber comprises a carbon fiber reinforced PEEK composite fiber, and the preparation method comprises the following steps: uniformly dispersing a surfactant in deionized water, regulating the pH value of the solution to 2-12 by using an acid solution or an alkali solution, mixing the mixed solution dropwise with PEEK resin powder to form a suspension, coating the suspension on the surface of carbon fiber, drying, standing at constant temperature in a heat setting device, and cooling to obtain the modified PEEK resin.
The invention patent with application number 2022101912536 discloses a unidirectional prepreg tape of a carbon fiber-polyaryletherketone composite material and a preparation method thereof, wherein an amphipathic polyoxyethylene derivative is adopted to slurry carbon fibers, carbon fiber tows are subjected to expansion treatment at a certain lower temperature, then sizing agent is removed, and then the carbon fiber tows are subjected to hot melting compounding with the polyaryletherketone, and irradiation treatment and remelting treatment are carried out after the compounding, so that the interfacial interaction between the carbon fibers and the polyaryletherketone is further increased.
While some continuous carbon fiber reinforced PEEK prepregs or other types of composites have emerged, low cost, continuous carbon fiber reinforced PEEK prepregs or other forms of composites that are mechanically strong, excellent wear resistant are scarce. In view of the above, there is a need for a high-strength, abrasion-resistant and low-cost high-performance carbon fiber reinforced PEEK prepreg for use in manufacturing various products.
Disclosure of Invention
In order to solve the technical problems, a preparation method of the high-performance carbon fiber reinforced PEEK prepreg and a PEEK base plate are provided. The carbon fiber reinforced PEEK prepreg has good mechanical property, excellent wear resistance and low cost.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a preparation method of a high-performance carbon fiber reinforced PEEK prepreg comprises the following steps:
s1, preparing a PEEK-containing suspension;
s2, spreading the tows of the carbon fibers and then carrying out surface treatment to obtain pretreated carbon fibers;
and S3, immersing the pretreated carbon fiber into the suspension for immersion treatment, drying, extruding for molding, cooling and rolling to obtain the high-performance carbon fiber reinforced PEEK prepreg.
Further, the suspension comprises the following materials in parts by weight: 0.1-1 part of thickener, 0.01-0.2 part of surfactant, 0.01-0.3 part of nano carbon material, 0.5-5 parts of polytetrafluoroethylene, 5-50 parts of PEEK resin, 10-30 parts of aluminum oxide and 100 parts of water; wherein the PEEK resin is 10 times of the polytetrafluoroethylene resin in parts by weight.
Still further, the thickener is polyvinyl alcohol, for example, 1788, 1792, 1799, 2099 type PVA; the surfactant is one or more of fatty alcohol polyoxyethylene ether, sodium dodecyl sulfate and perfluoro caprylate; the nano carbon material is one or more of multi-wall carbon nano tubes, single-wall carbon nano tubes and graphene nano sheets; the conductivity of the water is 0.1-1 mu S/cm.
Further, the temperature of the surface treatment is 200-1000 ℃; the dipping treatment is carried out at room temperature; the temperature of the drying is 100-500 ℃; the extrusion molding temperature is 200-500 ℃; the winding speed is 0.1-5m/min.
Further, the carbon fiber accounts for 40-70wt% of the prepreg, and the balance is PEEK-based material, wherein the PEEK-based material comprises the following components in percentage by weight as 100 wt%: 30-60wt% of PEEK, 3-6wt% of polytetrafluoroethylene, 35-65wt% of aluminum oxide and 0.05-0.4wt% of multi-wall carbon nano tube; preferably, the carbon fiber accounts for 55-65wt% of the prepreg, and the balance is PEEK-based material.
Further, the carbon fiber is any one or a combination of a plurality of polyacrylonitrile-based carbon fibers, viscose-based carbon fibers and pitch-based carbon fibers, and the specification of the carbon fiber is 1K, 3K, 6K, 12K, 24K, 48K and the like.
The invention also provides a PEEK base plate, which is prepared by compression molding after the carbon fiber reinforced PEEK prepreg obtained by the preparation method is paved.
Further, the layers are laid in multiple layers according to any two or more angles of 0 degree, +45 degrees, -45 degrees and 90 degrees; the temperature of the compression molding is 350-380 ℃, the pressure is 0.5-1.2MPa, and the lamination time is 0.5-2h.
The beneficial technical effects are as follows:
according to the invention, PEEK is used as matrix resin, continuous carbon fiber is used as a reinforcement, carbon nano tube, aluminum oxide and polytetrafluoroethylene are used as modified materials to obtain high-performance carbon fiber reinforced PEEK prepreg, and the prepreg is used for multi-layer paving to obtain the high-performance PEEK base plate. The invention suspends the modified material and the matrix resin in the water solvent, and the suspending solution is kept stable by adding the auxiliary agent. The carbon fiber is soaked in the suspension liquid after high-temperature treatment, then baked to remove water and auxiliary agent, and then melted, extruded by a die, rolled and the like to prepare the prepreg. Compared with the prior art, the composite material has the advantages of good mechanical property, excellent wear resistance and low cost.
Drawings
FIG. 1 is a process flow diagram of the preparation of a high performance PEEK base sheet.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The numerical values set forth in these examples do not limit the scope of the present invention unless specifically stated otherwise. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values.
The experimental methods in the following examples, for which specific conditions are not noted, are generally determined according to national standards; if the national standard is not corresponding, the method is carried out according to the general international standard or the standard requirements set by related enterprises. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
The diameter of the carbon nano tube is 30-50nm, and the length is 0.5-50 mu m; the grain diameter of the polytetrafluoroethylene is 5-100 mu m; the particle size of PEEK resin powder is 300-2000 meshes, and the melt index under 5KG load at 380 ℃ is 50-200g/10min; the particle size of the aluminum oxide is 300-2000 meshes.
Example 1
A preparation method of a high-performance carbon fiber reinforced PEEK prepreg comprises the following steps:
s1, preparing a PEEK-containing suspension, wherein the suspension comprises the following materials in parts by weight: 17880.1 parts of PVA, 0.01 part of fatty alcohol polyoxyethylene ether AEO-3, 0.01 part of multi-wall carbon nano tube, 0.5 part of polytetrafluoroethylene, 5 parts of PEEK resin powder, 10 parts of aluminum oxide and 100 parts of deionized water;
the preparation process is as follows: PVA1788 and AEO-3 are dissolved in water to form a homogeneous solution, then multi-wall carbon nano tube, polytetrafluoroethylene, PEEK resin powder and aluminum oxide are added and stirred to form a suspension, and the suspension is placed in an impregnation tank for standby;
s2, placing 10 rolls of 6K (T700) carbon fibers on a creel, enabling each carbon fiber to pass through a ceramic yarn through hole and comb teeth so that each carbon fiber is not staggered and arranged in parallel after being discharged out of the creel, spreading carbon fiber tows by adopting a vibration yarn spreading device, and then carrying out high-temperature surface treatment at 200 ℃ to obtain pretreated carbon fibers;
s3, immersing the pretreated carbon fiber into the suspension in an immersion tank for immersion treatment at normal temperature, drying in an oven at 100 ℃, then putting into a die at 200 ℃ for extrusion molding, cooling, and winding at a speed of 0.1m/min to obtain the high-performance carbon fiber reinforced PEEK prepreg, wherein the carbon fiber accounts for 70wt% and the PEEK-based material accounts for 30wt% (wherein the PEEK-based material comprises PEEK32.24wt%, polytetrafluoroethylene 3.22wt%, multi-wall carbon nanotubes 0.07wt% and aluminum oxide 64.47 wt%).
High-performance PEEK base plate: the carbon fiber reinforced PEEK prepreg prepared by the method is subjected to layering according to 0 degree/90 degrees (namely, the lower layer paving angle is 0 degree, the upper layer paving angle is 90 degrees), and then subjected to compression molding at 360 ℃ and 1MPa pressure for 1h, so that the high-performance PEEK base plate is obtained.
Example 2
A preparation method of a high-performance carbon fiber reinforced PEEK prepreg comprises the following steps:
s1, preparing a PEEK-containing suspension, wherein the suspension comprises the following materials in parts by weight: 17920.3 parts of PVA, 0.03 part of sodium dodecyl sulfate, 0.08 part of multi-wall carbon nano tube, 1.5 parts of polytetrafluoroethylene, 15 parts of PEEK resin powder, 15 parts of aluminum oxide and 100 parts of deionized water;
the preparation process is as follows: PVA1792 and sodium dodecyl sulfate are dissolved in water to form a homogeneous solution, then multi-wall carbon nano tubes, polytetrafluoroethylene, PEEK resin powder and aluminum oxide are added, stirred to form a suspension, and placed in an impregnation tank for standby;
s2, placing 10 rolls of 12K (T700) carbon fibers on a creel, enabling each carbon fiber to pass through a ceramic yarn through hole and comb teeth so that each carbon fiber is not staggered and arranged in parallel after being discharged out of the creel, spreading carbon fiber tows by adopting a vibration yarn spreading device, and then carrying out high-temperature surface treatment at 400 ℃ to obtain pretreated carbon fibers;
s3, immersing the pretreated carbon fiber into the suspension liquid of an immersion tank for immersion treatment at normal temperature, then drying in an oven at 180 ℃, then performing extrusion molding in a die at 270 ℃, and winding at a speed of 1m/min after cooling to obtain carbon fiber reinforced PEEK prepreg; 62wt% of carbon fiber and 38wt% of PEEK base material in the prepreg (wherein PEEK base material comprises 47.50wt% of PEEK, 4.75wt% of polytetrafluoroethylene, 0.25wt% of multi-wall carbon nano tube and 47.50wt% of aluminum oxide).
High-performance PEEK base plate: the carbon fiber reinforced PEEK prepreg prepared by the method is subjected to layering according to 0 degree/90 degrees (namely, the lower layer paving angle is 0 degree, the upper layer paving angle is 90 degrees), and then subjected to compression molding at 360 ℃ and 1MPa pressure for 1h, so that the high-performance PEEK base plate is obtained.
Example 3
A preparation method of a high-performance carbon fiber reinforced PEEK prepreg comprises the following steps:
s1, preparing a PEEK-containing suspension, wherein the suspension comprises the following materials in parts by weight: 17990.5 parts of PVA, 0.1 part of fatty alcohol polyoxyethylene ether AEO-3, 0.15 part of multi-wall carbon nano tube, 2.8 parts of polytetrafluoroethylene, 28 parts of PEEK resin powder, 20 parts of aluminum oxide and 100 parts of deionized water;
the preparation process is as follows: PVA1799 and AEO-3 are dissolved in water to form a homogeneous solution, then multi-wall carbon nano tube, polytetrafluoroethylene, PEEK resin powder and aluminum oxide are added and stirred to form a suspension, and the suspension is placed in an impregnation tank for standby;
s2, placing 10 rolls of 12K (T700) carbon fibers on a creel, enabling each carbon fiber to pass through a ceramic yarn through hole and comb teeth so that each carbon fiber is not staggered and arranged in parallel after being discharged out of the creel, spreading carbon fiber tows by adopting a vibration yarn spreading device, and then carrying out high-temperature surface treatment at 600 ℃ to obtain pretreated carbon fibers;
s3, immersing the pretreated carbon fiber into the suspension liquid of an immersion tank for immersion treatment at normal temperature, then drying in an oven at 260 ℃, then performing extrusion molding in a mold at 350 ℃, and winding at a speed of 2m/min after cooling to obtain carbon fiber reinforced PEEK prepreg; the prepreg comprises 55wt% of carbon fiber and 45wt% of PEEK-based material (wherein the PEEK-based material comprises 54.97wt% of PEEK, 5.49wt% of polytetrafluoroethylene, 0.29wt% of multi-wall carbon nano tube and 39.25wt% of aluminum oxide).
High-performance PEEK base plate: the carbon fiber reinforced PEEK prepreg prepared by the method is subjected to layering according to 0 degree/90 degrees (namely, the lower layer paving angle is 0 degree, the upper layer paving angle is 90 degrees), and then subjected to compression molding at 360 ℃ and 1MPa pressure for 1h, so that the high-performance PEEK base plate is obtained.
Example 4
A preparation method of a high-performance carbon fiber reinforced PEEK prepreg comprises the following steps:
s1, preparing a PEEK-containing suspension, wherein the suspension comprises the following materials in parts by weight: 20990.8 parts of PVA, 0.15 part of perfluorooctanoate, 0.2 part of multi-wall carbon nano tube, 4 parts of polytetrafluoroethylene, 40 parts of PEEK resin powder, 25 parts of aluminum oxide and 100 parts of deionized water;
the preparation process is as follows: PVA2099 and perfluoro caprylate are dissolved in water to form a homogeneous solution, then multi-wall carbon nano tube, polytetrafluoroethylene, PEEK resin powder and aluminum oxide are added, stirred to form a suspension, and placed in an impregnation tank for standby;
s2, placing 10 rolls of 12K (T700) carbon fibers on a creel, enabling each carbon fiber to pass through a ceramic yarn through hole and comb teeth so that each carbon fiber is not staggered and arranged in parallel after being discharged out of the creel, spreading carbon fiber tows by adopting a vibration yarn spreading device, and then carrying out high-temperature surface treatment at 800 ℃ to obtain pretreated carbon fibers;
s3, immersing the pretreated carbon fiber into the suspension liquid of an immersion tank for immersion treatment at normal temperature, then drying in an oven at 350 ℃, then performing extrusion molding in a mold at 400 ℃, and winding at a speed of 3m/min after cooling to obtain carbon fiber reinforced PEEK prepreg; the prepreg comprises 50wt% of carbon fiber and 50wt% of PEEK-based material (wherein the PEEK-based material comprises 57.80wt% of PEEK, 5.78wt% of polytetrafluoroethylene, 0.29wt% of multi-wall carbon nano tube and 36.13wt% of aluminum oxide).
High-performance PEEK base plate: the carbon fiber reinforced PEEK prepreg prepared by the method is subjected to layering according to 0 degree/90 degrees (namely, the lower layer paving angle is 0 degree, the upper layer paving angle is 90 degrees), and then subjected to compression molding at 360 ℃ and 1MPa pressure for 1h, so that the high-performance PEEK base plate is obtained.
Example 5
A preparation method of a high-performance carbon fiber reinforced PEEK prepreg comprises the following steps:
s1, preparing a PEEK-containing suspension, wherein the suspension comprises the following materials in parts by weight: 17881 parts of PVA, 0.2 part of fatty alcohol polyoxyethylene ether AEO-3, 0.3 part of multi-wall carbon nano tube, 5 parts of polytetrafluoroethylene, 50 parts of PEEK resin powder, 30 parts of aluminum oxide and 100 parts of deionized water;
the preparation process is as follows: PVA1788 and AEO-3 are dissolved in water to form a homogeneous solution, then multi-wall carbon nano tube, polytetrafluoroethylene, PEEK resin powder and aluminum oxide are added and stirred to form a suspension, and the suspension is placed in an impregnation tank for standby;
s2, placing 10 rolls of 12K (T700) carbon fibers on a creel, enabling each carbon fiber to pass through a ceramic yarn through hole and comb teeth so that each carbon fiber is not staggered and arranged in parallel after being discharged out of the creel, spreading carbon fiber tows by adopting a vibration yarn spreading device, and then carrying out high-temperature surface treatment at 1000 ℃ to obtain pretreated carbon fibers;
s3, immersing the pretreated carbon fiber into the suspension liquid of an immersion tank for immersion treatment at normal temperature, then drying in an oven at 400 ℃, then performing extrusion molding in a mold at 400 ℃, and winding at a speed of 5m/min after cooling to obtain carbon fiber reinforced PEEK prepreg; the prepreg comprises 40wt% of carbon fiber and 60wt% of PEEK-based material (wherein the PEEK-based material comprises 58.62wt% of PEEK, 5.86wt% of polytetrafluoroethylene, 0.35wt% of multi-wall carbon nano tube and 35.17wt% of aluminum oxide).
High-performance PEEK base plate: the carbon fiber reinforced PEEK prepreg prepared by the method is subjected to layering according to 0 degree/90 degrees (namely, the lower layer paving angle is 0 degree, the upper layer paving angle is 90 degrees), and then subjected to compression molding at 360 ℃ and 1MPa pressure for 1h, so that the high-performance PEEK base plate is obtained.
Comparative example 1
The PEEK base sheet of this comparative example was prepared the same as in example 3 except that the PEEK suspension included the following materials in parts by weight: PVA 1799.5 parts, fatty alcohol polyoxyethylene ether AEO-3.1 parts, polytetrafluoroethylene 23 parts, PEEK resin powder 28 parts and deionized water 100 parts.
Comparative example 2
The PEEK base sheet of this comparative example was prepared the same as in example 3 except that the PEEK suspension included the following materials in parts by weight: PVA 1799.5 parts, fatty alcohol polyoxyethylene ether AEO-3.1 parts, multi-wall carbon nano tube 0.15 parts, polytetrafluoroethylene 22.8 parts, PEEK resin powder 28 parts and deionized water 100 parts.
Comparative example 3
The PEEK base sheet of this comparative example was prepared the same as in example 3 except that the PEEK suspension included the following materials in parts by weight: PVA 1799.5 parts, fatty alcohol polyoxyethylene ether AEO-3.1 parts, polytetrafluoroethylene 2.8 parts, PEEK resin powder 28 parts, aluminum oxide 20.15 parts and deionized water 100 parts.
The formulation of the carbon fiber reinforced PEEK prepreg of the above examples and comparative examples is shown in Table 1.
Table 1 example and comparative carbon fiber reinforced PEEK prepreg formulations
The PEEK base sheets of the above examples and comparative examples were tested for tensile strength according to ASTM D3039 (Standard test method for tensile Property of Polymer-based composites); the friction test uses 45 steel for the opposite grinding part, and the rotating speed is 346r/min and 132N; the experimental results are shown in table 2.
Table 2 experimental results
As can be seen from Table 2, the method of the invention uses carbon fiber as reinforcement, PEEK as base material, alumina as filler, a small amount of carbon nano tube and a small amount of PTFE as auxiliary materials to prepare carbon fiber reinforced PEEK prepreg, and the prepreg is layered to obtain the high-strength and wear-resistant PEEK base plate with the tensile strength of 350-645MPa and the friction coefficient of less than 0.37.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. The preparation method of the high-performance carbon fiber reinforced PEEK prepreg is characterized by comprising the following steps:
s1, preparing a PEEK-containing suspension;
the suspension comprises the following materials in parts by weight: 0.1-1 part of thickener, 0.01-0.2 part of surfactant, 0.01-0.3 part of nano carbon material, 0.5-5 parts of polytetrafluoroethylene, 5-50 parts of PEEK resin, 10-30 parts of aluminum oxide and 100 parts of water; wherein the PEEK resin is 10 times of polytetrafluoroethylene resin in parts by weight;
s2, spreading the tows of the carbon fibers and then carrying out surface treatment to obtain pretreated carbon fibers;
and S3, immersing the pretreated carbon fiber into the suspension for immersion treatment, drying, extruding for molding, cooling and rolling to obtain the high-performance carbon fiber reinforced PEEK prepreg.
2. The method for preparing the high-performance carbon fiber reinforced PEEK prepreg according to claim 1, wherein the thickener is polyvinyl alcohol; the surfactant is one or more of fatty alcohol polyoxyethylene ether, sodium dodecyl sulfate and perfluoro caprylate; the nano carbon material is one or more of multi-wall carbon nano tubes, single-wall carbon nano tubes and graphene nano sheets; the conductivity of the water is 0.1-1 mu S/cm.
3. The method for preparing the high-performance carbon fiber reinforced PEEK prepreg according to claim 1, wherein the diameter of the nano carbon material is 30-50nm, and the length of the nano carbon material is 0.5-50 μm; the grain diameter of the polytetrafluoroethylene is 5-100 mu m; the particle size of the PEEK resin is 300-2000 meshes, and the melt index of the PEEK resin under 5KG load at 380 ℃ is 50-200g/10min; the particle size of the aluminum oxide is 300-2000 meshes.
4. The method for preparing a high performance carbon fiber reinforced PEEK prepreg according to claim 1, wherein the surface treatment temperature is 200-1000 ℃; the dipping treatment is carried out at room temperature; the temperature of the drying is 100-500 ℃; the extrusion molding temperature is 200-500 ℃; the winding speed is 0.1-5m/min.
5. The method for preparing the high-performance carbon fiber reinforced PEEK prepreg according to claim 1, wherein the high-performance carbon fiber reinforced PEEK prepreg comprises 40-70wt% of carbon fiber and the balance of PEEK-based material, and the PEEK-based material comprises the following components in percentage by weight as 100% of the material: 30-60wt% of PEEK, 3-6wt% of polytetrafluoroethylene, 35-65wt% of aluminum oxide and 0.05-0.4wt% of multi-wall carbon nano tube.
6. The method for preparing the high-performance carbon fiber reinforced PEEK prepreg according to claim 1, wherein the carbon fiber is one or more of polyacrylonitrile-based carbon fiber, viscose-based carbon fiber and asphalt-based carbon fiber.
7. A PEEK-based sheet material, characterized in that it is produced by compression molding after being laid up by the carbon fiber-reinforced PEEK prepreg obtained by the production method according to any one of claims 1 to 6.
8. A PEEK based board according to claim 7, wherein said layers are laid in layers at any two or more angles of 0 °, +45°, -45 °, 90 °; the temperature of the compression molding is 350-380 ℃, the pressure is 0.5-1.2MPa, and the lamination time is 0.5-2h.
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| JP2013173812A (en) * | 2012-02-23 | 2013-09-05 | Toray Ind Inc | Prepreg and carbon fiber-reinforced composite material |
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| CN111057346A (en) * | 2020-01-09 | 2020-04-24 | 江苏韩塑新材料有限公司 | Carbon fiber reinforced PEEK unidirectional tape and preparation method thereof |
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| JP2013173812A (en) * | 2012-02-23 | 2013-09-05 | Toray Ind Inc | Prepreg and carbon fiber-reinforced composite material |
| CN109777036A (en) * | 2019-01-04 | 2019-05-21 | 扬州市维纳复合材料科技有限公司 | A kind of polyether-ether-ketone base wearing composite material and preparation method thereof |
| CN111057346A (en) * | 2020-01-09 | 2020-04-24 | 江苏韩塑新材料有限公司 | Carbon fiber reinforced PEEK unidirectional tape and preparation method thereof |
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Address after: 213100 no.7-16, Yangtze River Delta mold City, Wujin high tech Industrial Development Zone, Changzhou City, Jiangsu Province Patentee after: Jiangsu Junhua Special Polymer Materials Co.,Ltd. Patentee after: Changzhou Junhua Medical Technology Co.,Ltd. Address before: 213100 no.7-16, Yangtze River Delta mold City, Wujin high tech Industrial Development Zone, Changzhou City, Jiangsu Province Patentee before: JIANGSU JUNHUA HIGH PERFORMANCE SPECIALTY ENGINEERING PLASTICS (PEEK) PRODUCTS CO.,LTD. Patentee before: Changzhou Junhua Medical Technology Co.,Ltd. |