CN110863341A - Preparation method of PA66 grafted carbon fiber - Google Patents
Preparation method of PA66 grafted carbon fiber Download PDFInfo
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- CN110863341A CN110863341A CN201911217033.0A CN201911217033A CN110863341A CN 110863341 A CN110863341 A CN 110863341A CN 201911217033 A CN201911217033 A CN 201911217033A CN 110863341 A CN110863341 A CN 110863341A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention discloses a preparation method of PA66 grafted carbon fibers, and particularly relates to a preparation method of PA66 grafted carbon fibers, which is characterized by comprising the following steps: firstly, removing the epoxy coating on the surface of the carbon fiber, then activating the surface of the carbon fiber by adopting a plasma technology, improving oxygen-containing functional groups on the surface of the carbon fiber, performing infiltration treatment on the treated activated carbon fiber, and finally reacting PA66 with the activated carbon fiber to obtain the PA66 grafted carbon fiber. The carbon fiber surface modification method adopted by the invention is simple, the structure of the carbon fiber body is maintained more completely, the compatibility of the carbon fiber and a PA66 matrix is improved, and the mechanical property and the antistatic property of the PA66 resin are obviously improved.
Description
[ technical field ]
The invention relates to a preparation method of a high-molecular composite material, and particularly relates to a preparation method of PA66 grafted carbon fibers.
[ background art ]
Polyamide 66 is commonly called nylon 66, and is a high-performance engineering plastic with chemical resistance, wear resistance and high temperature resistance. The PA66 has excellent mechanical properties, good self-lubricating property, good toughness and other excellent properties, and is widely applied to the fields of machinery industry, automobiles, instruments and meters and the like. However, the PA66 resin has high resistance, and static electricity is accumulated due to friction during use, so that the PA66 product is easy to adsorb dust and even to cause electric sparks. Meanwhile, in the process of using the PA66 resin as a structural member to replace metal, the mechanical strength of the PA66 resin cannot meet the requirements of the structural member. Therefore, in the process of using the PA66 resin as a structural member metal substitute, the mechanical property of the PA66 resin needs to be enhanced and antistatic treatment is needed.
Carbon fiber as a novel inorganic material has a series of excellent performances such as high specific strength, high specific modulus, high temperature resistance and the like, and is widely applied to reinforcement of advanced composite materials. Meanwhile, the carbon fiber also has excellent conductivity, and the problem of poor antistatic performance of the polymer can be obviously improved. However, carbon fibers have low surface energy, few reactive functional groups, and chemically inert surfaces, which makes them less compatible with resin matrices. Therefore, how to increase the surface energy of the carbon fiber greatly helps to improve the antistatic property and the mechanical property of the PA66 resin.
[ summary of the invention ]
Aiming at the defects in the prior art, the invention provides a preparation method of PA66 grafted carbon fibers, and aims to solve the problem that the compatibility of the carbon fibers and a PA66 lipid matrix is poor.
The preparation method of the PA66 grafted carbon fiber is realized according to the following steps:
step one, removing the epoxy coating on the surface of the carbon fiber
Putting the carbon fiber bundle into a Soxhlet extractor, using acetone as a solvent, heating to 75-85 ℃, and continuously cleaning impurities on the surface of the carbon fiber in distilled acetone for 30-40 h; then taking out the carbon fiber, and drying in an oven at the temperature of 80-90 ℃ for 4-6 h;
step two, preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the gas flow of 1.5L/min-2L/min for 5min-8 min; then introducing pure oxygen with the gas flow of l0mL/min-15mL/min for 5min-8 min; performing plasma modification in the plasma reaction cavity to prepare plasma activated carbon fibers;
step three, preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
Dissolving hyperbranched polyglycerol into N, N-dimethylformamide solution, and preparing the N, N-dimethylformamide solution of hyperbranched polyglycerol with the mass concentration of 0.5% -1%;
step four, modification of activated carbon fibers
And (3) adding the plasma activated carbon fiber obtained in the step (2) into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step (3), and carrying out ultrasonic treatment for 15-30 min. Modifying the obtained solution at 90-100 ℃ for 24-36 h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber;
step five, grafting modified carbon fiber by PA66
Dissolving PA66 in a formic acid solution, then adding activated carbon fiber into a PA66 solution, stirring for reaction for 2 hours, centrifuging a product after reaction, washing with the formic acid solution, washing with ethanol, and then drying to obtain PA66 graft modified carbon fiber;
further, the carbon fiber in the first step is PAN-based carbon fiber.
Further, the power of the plasma processor in the second step is 60W-80W, and the discharge processing time is 80s-100 s.
Further, the concentration of the hyperbranched polyglycerol N, N-dimethylformamide solution in the third step is 0.5-1%.
Further, the mass-to-volume ratio of the addition amount of the plasma activated carbon fibers to the hyperbranched polyglycerol N, N-dimethylformamide solution in the fourth step is (5-10) g: 0.1L.
Further, the adding mass ratio of the activated carbon fibers in the fifth step is 1-50%.
The invention has the beneficial effects that:
(1) the plasma technology adopted by the invention is used for treating the surface depth of the carbon fiber to be not more than 100 mu m, so that the strength of the carbon fiber body is not damaged;
(2) the modified carbon fiber prepared by the method has good compatibility in a PA66 matrix, and provides a better solution for improving the antistatic property and the mechanical property of PA 66;
(3) the carbon fiber surface modification method adopted by the invention is simpler, the structure of the carbon fiber body is maintained more completely, the compatibility of the carbon fiber and a PA66 matrix is improved, and the mechanical property and the antistatic property of PA66 resin are obviously improved;
(4) the carbon fiber surface modification method adopted by the invention greatly improves the compatibility of the carbon fiber in a PA66 matrix, and provides a scheme for effectively improving the antistatic property and the mechanical property of PA 66. Meanwhile, the method also has the advantages of low cost, short preparation period, environmental protection and the like.
[ detailed description of the invention ]
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
The first embodiment is as follows: this example, a method for grafting carbon fibers with PA66, was carried out as follows:
(1) removal of epoxy coating on carbon fiber surface
Putting the carbon fiber bundle into a Soxhlet extractor, heating to 75 ℃ by using acetone as a solvent to continuously clean impurities on the surface of the carbon fiber in distilled acetone for 30 hours; the carbon fibers were then removed and dried in an oven at 80 ℃ for 4 h.
(2) Preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the gas flow of 1.5L/min for 5 min; then introducing pure oxygen with the air flow of l0mL/min for 5 min; and (4) performing discharge treatment for 80s at the power of 60W to prepare the plasma activated carbon fiber.
(3) Preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
Dissolving hyperbranched polyglycerol into N, N-dimethylformamide solution, and preparing the N, N-dimethylformamide solution of hyperbranched polyglycerol with the mass concentration of 0.5%.
(4) Modification of activated carbon fibers
Adding the plasma activated carbon fiber obtained in the step (2) into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step (3) and carrying out ultrasonic treatment for 15min, wherein the mass-to-volume ratio of the adding amount of the plasma activated carbon fiber to the hyperbranched polyglycerol N, N-dimethylformamide solution is 5 g: 0.1L. And modifying the obtained solution at 90 ℃ for 24h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber.
(5) PA66 graft modified carbon fiber
Dissolving 10g of PA66 in a formic acid solution, then adding 1g of activated carbon fiber into the PA66 solution, stirring and reacting for 2h, centrifuging the product after reaction, washing with the formic acid solution, washing with ethanol, and drying to obtain the PA66 graft modified carbon fiber.
The second embodiment is as follows: this example, a method for grafting carbon fibers with PA66, was carried out as follows:
(1) removal of epoxy coating on carbon fiber surface
Putting the carbon fiber bundle into a Soxhlet extractor, heating to 80 ℃ by using acetone as a solvent, and continuously cleaning impurities on the surface of the carbon fiber in distilled acetone for 35 hours; the carbon fibers were then removed and dried in an oven at 80 ℃ for 6 h.
(2) Preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the flow rate of 2L/min for 5 min; then introducing pure oxygen with the air flow of l5mL/min for 5 min; and (4) discharging at the power of 70W for 90s to prepare the plasma activated carbon fiber.
(3) Preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
Dissolving hyperbranched polyglycerol into N, N-dimethylformamide solution, and preparing the N, N-dimethylformamide solution of hyperbranched polyglycerol with the mass concentration of 0.5%.
(4) Modification of activated carbon fibers
Adding the plasma activated carbon fiber obtained in the step (2) into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step (3) and carrying out ultrasonic treatment for 20min, wherein the mass-to-volume ratio of the addition amount of the plasma activated carbon fiber to the hyperbranched polyglycerol N, N-dimethylformamide solution is 6 g: 0.1L. And modifying the obtained solution at 100 ℃ for 24h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber.
(5) PA66 graft modified carbon fiber
Dissolving 10g of PA66 in a formic acid solution, then adding 2g of activated carbon fiber into the PA66 solution, stirring and reacting for 2h, centrifuging the product after reaction, washing with the formic acid solution, washing with ethanol, and drying to obtain the PA66 grafted modified carbon fiber.
The third concrete implementation mode: this example, a method for grafting carbon fibers with PA66, was carried out as follows:
(1) removal of epoxy coating on carbon fiber surface
Putting the carbon fiber bundle into a Soxhlet extractor, heating to 85 ℃ by using acetone as a solvent, and continuously cleaning impurities on the surface of the carbon fiber in distilled acetone for 40 h; the carbon fibers were then removed and dried in an oven at 80 ℃ for 6 h.
(2) Preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the flow rate of 2L/min for 8 min; then introducing pure oxygen with the gas flow of 12mL/min for 7 min; and (4) performing discharge treatment for 100s under the power of 60W to prepare the plasma activated carbon fiber.
(3) Preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
Dissolving hyperbranched polyglycerol into N, N-dimethylformamide solution, and preparing the N, N-dimethylformamide solution of hyperbranched polyglycerol with the mass concentration of 0.6%.
(4) Modification of activated carbon fibers
Adding the plasma activated carbon fiber obtained in the step (2) into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step (3) and carrying out ultrasonic treatment for 30min, wherein the mass-to-volume ratio of the adding amount of the plasma activated carbon fiber to the hyperbranched polyglycerol N, N-dimethylformamide solution is 10 g: 0.1L. And modifying the obtained solution at 90 ℃ for 24h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber.
(5) PA66 graft modified carbon fiber
Dissolving 10g of PA66 in a formic acid solution, then adding 3.5g of activated carbon fiber into the PA66 solution, stirring and reacting for 2 hours, centrifuging a product after reaction, washing with the formic acid solution, washing with ethanol, and drying to obtain the PA66 graft modified carbon fiber.
The fourth concrete implementation mode: this example, a method for grafting carbon fibers with PA66, was carried out as follows:
(1) removal of epoxy coating on carbon fiber surface
Putting the carbon fiber bundle into a Soxhlet extractor, heating to 85 ℃ by using acetone as a solvent, and continuously cleaning impurities on the surface of the carbon fiber in distilled acetone for 35 hours; the carbon fibers were then removed and dried in an oven at 80 ℃ for 5 h.
(2) Preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the gas flow of 1.8L/min for 5 min; then introducing pure oxygen with the gas flow of 10mL/min for 7 min; and (4) discharging at the power of 65W for 85s to prepare the plasma activated carbon fiber.
(3) Preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
Dissolving hyperbranched polyglycerol into N, N-dimethylformamide solution, and preparing the N, N-dimethylformamide solution of hyperbranched polyglycerol with the mass concentration of 1%.
(4) Modification of activated carbon fibers
Adding the plasma activated carbon fiber obtained in the step (2) into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step (3) and carrying out ultrasonic treatment for 15min, wherein the mass-to-volume ratio of the addition amount of the plasma activated carbon fiber to the hyperbranched polyglycerol N, N-dimethylformamide solution is 8 g: 0.1L. And modifying the obtained solution at 100 ℃ for 30h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber.
(5) PA66 graft modified carbon fiber
Dissolving 10g of PA66 in a formic acid solution, then adding 4g of activated carbon fiber into the PA66 solution, stirring and reacting for 2h, centrifuging the product after reaction, washing with the formic acid solution, washing with ethanol, and drying to obtain the PA66 graft modified carbon fiber.
The fifth concrete implementation mode: this example, a method for grafting carbon fibers with PA66, was carried out as follows:
(1) removal of epoxy coating on carbon fiber surface
Putting the carbon fiber bundle into a Soxhlet extractor, heating to 85 ℃ by using acetone as a solvent, and continuously cleaning impurities on the surface of the carbon fiber in distilled acetone for 35 hours; the carbon fibers were then removed and dried in an oven at 80 ℃ for 5 h.
(2) Preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the flow rate of 2L/min for 5 min; then introducing pure oxygen with the air flow of l5mL/min for 7 min; and (4) discharging at the power of 70W for 85s to prepare the plasma activated carbon fiber.
(3) Preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
And dissolving the hyperbranched polyglycerol into an N, N-dimethylformamide solution to prepare the N, N-dimethylformamide solution of the hyperbranched polyglycerol with the mass concentration of 0.7%.
(4) Modification of activated carbon fibers
Adding the plasma activated carbon fiber obtained in the step (2) into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step (3) and carrying out ultrasonic treatment for 25min, wherein the mass-to-volume ratio of the addition amount of the plasma activated carbon fiber to the hyperbranched polyglycerol N, N-dimethylformamide solution is 8 g: 0.1L. And modifying the obtained solution at 90 ℃ for 24h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber.
(5) PA66 graft modified carbon fiber
Dissolving 10g of PA66 in a formic acid solution, then adding 1.5g of activated carbon fiber into the PA66 solution, stirring and reacting for 2 hours, centrifuging a product after reaction, washing with the formic acid solution, washing with ethanol, and drying to obtain the PA66 graft modified carbon fiber.
Table 1 shows the surface resistance and mechanical properties of the composite material obtained by grafting PA66 with carbon fibers. As can be seen from Table 1, after the PA66 is grafted with the carbon fibers, the surface resistance of the composite material is obviously reduced, and the antistatic effect of the material is obviously improved. Meanwhile, the tensile strength of the composite material obtained by grafting the carbon fibers with the PA66 is improved to 165-191 MPa, the flexural modulus and the flexural strength are obviously improved, the impact strength is obviously improved, and the thermal deformation temperature of the material reaches 204-248 ℃, which is far higher than that of pure PA66 resin at 90 ℃. The modified carbon fiber provided by the invention can be successfully grafted with PA66, has excellent compatibility, and can greatly improve the antistatic property of PA66 and obviously enhance the mechanical property of PA 66.
TABLE 1 surface resistance and mechanical Properties of composites made from PA66 grafted carbon fibers
The above-mentioned embodiments of the present invention are intended to better explain the present invention, but the above-mentioned embodiments do not limit the scope of the present invention. Other variations or modifications may be made on the basis of the above description, which is not intended to be exhaustive, and all other variations or modifications encompassed by the present invention are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (6)
1. A preparation method of PA66 grafted carbon fibers is characterized by comprising the following steps:
step one, removing the epoxy coating on the surface of the carbon fiber
Putting the carbon fiber bundle into a Soxhlet extractor, using acetone as a solvent, heating to 75-85 ℃, and continuously cleaning impurities on the surface of the carbon fiber in distilled acetone for 30-40 h; then taking out the carbon fiber, and drying in an oven at the temperature of 80-90 ℃ for 4-6 h;
step two, preparation of plasma activated carbon fiber
Placing carbon fiber in a plasma reaction cavity, and introducing high-purity argon with the gas flow of 1.5L/min-2L/min for 5min-8 min; then introducing pure oxygen with the gas flow of l0mL/min-15mL/min for 5min-8 min; performing plasma modification in the plasma reaction cavity to prepare plasma activated carbon fibers;
step three, preparation of hyperbranched polyglycerol N, N-dimethylformamide solution
Dissolving hyperbranched polyglycerol into N, N-dimethylformamide solution to prepare N, N-dimethylformamide solution of hyperbranched polyglycerol;
step four, modification of activated carbon fibers
And (3) adding the plasma activated carbon fiber obtained in the step two into the hyperbranched polyglycerol N, N-dimethylformamide solution obtained in the step three, and carrying out ultrasonic treatment for 15-30 min. Modifying the obtained solution at 90-100 ℃ for 24-36 h, extracting the modified carbon fiber with acetone for 24h, and drying to obtain the hyperbranched polyglycerol-modified carbon fiber;
step five, grafting modified carbon fiber by PA66
Dissolving PA66 in a formic acid solution, then adding activated carbon fiber into a PA66 solution, stirring for reaction for 2 hours, centrifuging a product after reaction, washing with the formic acid solution, washing with ethanol, and then drying to obtain the PA66 graft modified carbon fiber.
2. The method for preparing PA66 grafted carbon fiber according to claim 1, wherein: the carbon fiber in the first step is PAN-based carbon fiber.
3. The method for preparing PA66 grafted carbon fiber according to claim 1, wherein: and in the step two, the power of the plasma processor is 60W-80W, and the discharge processing time is 80s-100 s.
4. The method for preparing PA66 grafted carbon fiber according to claim 1, wherein: the concentration of the hyperbranched polyglycerol N, N-dimethylformamide solution in the third step is 0.5-1%.
5. The method for preparing PA66 grafted carbon fiber according to claim 1, wherein: the mass-to-volume ratio of the addition amount of the plasma activated carbon fibers to the hyperbranched polyglycerol N, N-dimethylformamide solution in the fourth step is (5-10) g: 0.1L.
6. The method for preparing PA66 grafted carbon fiber according to claim 1, wherein: and the mass ratio of the activated carbon fibers in the fifth step is 1-50%.
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| CN113338027A (en) * | 2021-05-12 | 2021-09-03 | 北京化工大学 | Surface treatment method of carbon fiber |
| CN115490987A (en) * | 2022-09-18 | 2022-12-20 | 西北工业大学 | Amino-terminated hyperbranched polymer modified carbon cloth reinforced resin-based friction material and preparation method thereof |
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