CN107326655B - Method for modifying surface of carbon fiber - Google Patents
Method for modifying surface of carbon fiber Download PDFInfo
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- CN107326655B CN107326655B CN201710559667.9A CN201710559667A CN107326655B CN 107326655 B CN107326655 B CN 107326655B CN 201710559667 A CN201710559667 A CN 201710559667A CN 107326655 B CN107326655 B CN 107326655B
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
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Abstract
The invention discloses a method for modifying the surface of carbon fiber, in particular relates to a preparation method for generating boron nitride grains on the surface of the carbon fiber, and belongs to the field of interface modification of composite materials. The invention relates to a method for modifying the surface of carbon fiber, which comprises the following steps: 1. removing glue, 2, generating boron nitride crystal grains, and 3, aging at low temperature. The invention optimizes the reaction condition, leads boron carbide to generate crystal grains in the hydrothermal environment, coats the boron nitride crystal on the surface of the carbon fiber to achieve the purpose of modifying the carbon fiber, not only can improve the surface roughness and the surface activity of the carbon fiber, but also can play a role of mechanical meshing in a resin matrix to improve the mechanical property of the composite material.
Description
Technical Field
The invention belongs to the field of interface modification of composite materials, relates to a method for modifying the surface of carbon fibers, and particularly relates to a preparation method for generating boron nitride grains on the surface of the carbon fibers.
Background
Carbon fiber composites are widely used in the fields of aerospace, automobiles, weaponry, and sporting goods due to their advantages of high specific strength, low density, and high specific modulus. The carbon fiber resin matrix composite material is the most widely applied composite material, and the epoxy resin matrix is the most representative of the resin matrix composite material.
The carbon fiber resin matrix composite material has good mechanical properties. However, with the higher and higher requirements for the mechanical properties of structural materials in modern society, the mechanical properties of composite materials still need to be improved continuously. In the aspect of mechanical properties of the modified composite material, research is mainly carried out from three angles: firstly, the performance of a base material is improved; secondly, the performance of the reinforced material is improved; and thirdly, the interface bonding performance of the matrix and the reinforcing material is improved. Wherein, the interface performance of the matrix and the reinforced material has great effect on the overall performance of the composite material. The performance improvement of the matrix material and the reinforced material has great limitation, and as the production processes of the matrix material and the reinforced material are mature and belong to batch production, the stability of the performance and the breakthrough performance improvement are more pursued. Therefore, the research on the performance improvement of the composite material is based on the interface energy of the matrix and the reinforcing material, the process is easy to operate and execute in a laboratory, and is quick and convenient, the efficiency is improved, and the effect is more remarkable. The improvement of the interfacial bonding properties of carbon fiber composites is based on the surface modification of carbon fibers. Since carbon fibers have a low surface roughness and are chemically inert, they are not suitable for bonding to a resin matrix. The surface treatment method of carbon fiber can be roughly classified into an oxidation treatment method and a non-oxidation treatment method. Among them, the method of non-oxidation treatment is highly preferred by researchers because it causes little damage to carbon fibers themselves and requires little equipment. In recent years, a carbon fiber surface whisker treatment has become a novel treatment method, for example, a carbon nanotube is obtained on the surface of a carbon fiber by chemical vapor deposition, or silica nanoparticles are formed on the surface of a carbon fiber by a sol-gel method, and further, an inorganic whisker such as titanium dioxide, copper oxide, manganese oxide, or the like is grown on the surface of a carbon fiber by a hydrothermal method.
Boron nitride has high melting point, chemical stability, excellent dielectric property and other excellent performances, can be used as a coating to improve the mechanical property of a material and increase the oxidation resistance of the material, and is the first of the surface modification of carbon fibers.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a modification method for generating boron nitride grains on the surface of carbon fiber, which can improve the mechanical property of a composite material and simultaneously improve the heat resistance and oxidation resistance of the material.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a carbon fiber surface modification method, which comprises the following steps:
step one, removing glue from carbon fiber
Putting carbon fibers into an organic solvent, removing a sizing agent and impurities on the surfaces of the carbon fibers, soaking the carbon fibers in the solution, and finally drying the carbon fibers to obtain carbon fibers with clean surfaces;
step two, generating boron nitride crystal grains
(1) Placing the carbon fiber in a reaction kettle filled with a mixed solution of a boric acid solution and a sodium azide solution, and then placing the reaction kettle in a thermostat to obtain the carbon fiber with boron nitride grains on the surface;
(2) repeating the step two (1) for 2-3 times to obtain carbon fibers with uniformly distributed boron nitride;
step three, low-temperature aging
And (4) cleaning the carbon fiber obtained in the second step, removing the growth liquid on the surface of the carbon fiber, and then placing the carbon fiber in a vacuum drying oven for constant-temperature drying to finally obtain the carbon fiber with the surface coated with the boron nitride particles.
The invention relates to a carbon fiber surface modification method, which comprises the step one, wherein an organic solvent is a mixed solution of ethanol, acetone and tetrahydrofuran, and the volume ratio of ethanol to acetone to tetrahydrofuran is 1:1: 1-1: 5: 5.
The invention relates to a method for modifying the surface of carbon fiber, which comprises the following steps of firstly, placing an organic solvent in a Soxhlet extractor, and extracting at a certain temperature; the extraction temperature is 50-80 ℃; the extraction time is 15-24 h.
The invention relates to a carbon fiber surface modification method, which comprises the step one of sequentially soaking in an ethanol solution and an aqueous solution for 5-10 min.
In the second step, the concentration of the boric acid solution is 0.01-0.03M, and the concentration of the sodium azide solution is 0.005-0.01M. Preferably, the concentration of the boric acid solution is 0.02-0.03M, and the concentration of the sodium azide solution is 0.008-0.01M.
In the second step, the volume ratio of the boric acid solution to the sodium azide solution is 1: 1-1: 5. Preferably, the volume ratio of the boric acid solution to the sodium azide solution is 1: 1.5-1: 2. In a further preferred embodiment, the volume ratio of boric acid to sodium azide is 1: 2.
The invention relates to a carbon fiber surface modification method, in the second step, the preparation method of the mixed solution is as follows: firstly, respectively preparing a boric acid solution and a sodium azide solution, then adding the sodium azide solution into the boric acid solution, and uniformly stirring in a mechanical stirrer.
In the second step, the mixing time of the mixed solution is 1-2 hours, the mixing temperature is 15-35 ℃, and the rotating speed is 100-1000 r/min. Preferably, the stirring time of the mixed solution is 1-2 h, the stirring temperature is 20-35 ℃, and the rotating speed is 750-1000 r/min.
The invention relates to a carbon fiber surface modification method, wherein in the second step, the heat preservation temperature of a constant temperature box is 100-500 ℃; the heat preservation time is 1-24 h. As a preferred scheme, the constant temperature of the constant temperature box is 350-390 ℃; the constant temperature time is 12-24 h.
The invention relates to a method for modifying the surface of carbon fiber, which comprises the following steps: placing the carbon fiber in secondary distilled water, and ultrasonically vibrating; the volume of the secondary distilled water is 50-1000 ml; the time of ultrasonic vibration is 10-60 min.
The invention relates to a carbon fiber surface modification method, which comprises the following steps of in the third step, keeping the temperature of the drying oven at constant temperature for aging at 100-300 ℃; the time of constant temperature aging is 0.5-12 h. As a preferred scheme, the temperature of constant-temperature aging in the drying oven is 250-300 ℃; the time for constant temperature aging is 10-12 h. The interface bonding capability of the boron nitride crystal grains and the carbon fibers can be enhanced through constant temperature drying.
The invention has the beneficial effects that:
according to the invention, the boron nitride crystal grains are used for carrying out surface modification on the carbon fibers, and the boron nitride crystal grains are embedded on the surfaces of the carbon fibers, so that the surface roughness and the surface activity of the carbon fibers can be improved, the mechanical property of the composite material can be obviously improved after the boron nitride crystal grains are combined with a resin matrix, and the interface shear strength of the composite material can be improved by 35%. Due to the high temperature resistance and the oxidation resistance of the boron nitride, the boron nitride has a good effect on the stability of the high-temperature performance of the composite material, wherein the performance of the composite material at high temperature is 95-98% of the retention rate at low temperature.
In general, it is considered that it is difficult to produce boron nitride crystal grains by hydrothermal reaction, and therefore, it takes a long time to carry out the hydrothermal reaction, and the conversion rate of the obtained boron nitride is not high. In the experimental process, the invention discovers that when the concentration of the boric acid solution is 0.02-0.03M, the concentration of the sodium azide solution is 0.008-0.01M, and the volume ratio of the addition of the boric acid solution and the sodium azide solution is 1: 1.5-1: 2, the conversion rate of the boron nitride can be more than or equal to 30% within 12-24 h at the low temperature of 350-390 ℃.
The hydrothermal reaction of the invention has low temperature and short time, can obviously reduce the energy consumption in the aspect of boron nitride synthesis, and effectively improves the modification efficiency of the carbon fiber.
The invention introduces the low-temperature aging process and the treatment method in the technical aspect of modifying the carbon fiber, can obviously improve the interface bonding strength of the boron nitride and the carbon fiber, and ensures that the boron nitride is not easy to fall off.
Detailed Description
The technical solutions of the present invention are further described below, but not limited thereto, and modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
The first embodiment is as follows: the embodiment provides a carbon fiber surface modification method, which is specifically completed according to the following steps: first, remove glue
Putting 5g of carbon fiber into a Soxhlet extractor filled with an ethanol/acetone/tetrahydrofuran mixed solution with a volume ratio of 1:1:1, extracting for 15h at 60 ℃, removing a sizing agent and impurities on the surface of the carbon fiber, then respectively soaking for 10min in an ethanol solution and a distilled water solution, and drying for 30min after cleaning in a blast drying box at 100 ℃ to obtain carbon fiber with a clean surface;
secondly, generating boron nitride crystal grains
(1) Respectively preparing 0.01M boric acid solution and 0.005M sodium azide solution, and then adding the boric acid solution into the sodium azide solution, wherein the volume ratio of the boric acid solution to the sodium azide solution is 1: 1; stirring for 1h at 25 ℃ and the rotating speed is 750 r/min;
(2) placing the carbon fiber obtained in the step one in the mixed solution obtained in the step two (1), then placing the reaction kettle in a constant temperature environment, wherein the constant temperature is 350 ℃, the constant temperature time is 12 hours, and then taking out the carbon fiber;
(3) repeating the step two (2) for 2-3 times to obtain carbon fibers with boron nitride grains on the surfaces;
the conversion rate of the boron nitride is calculated to be 32%.
Third, low temperature aging
(1) Placing the carbon fiber with the boron nitride grains on the surface obtained in the step two (3) in 100ml of secondary distilled water, and ultrasonically vibrating for 10min to clean residual growth liquid on the surface of the sample;
(2) and (2) drying the carbon fiber obtained in the step (1) in a vacuum drying oven at constant temperature to enhance the interface bonding capability of the boron nitride crystal grains and the carbon fiber. The constant temperature is 250 ℃, the constant temperature time is 10 hours, and then the carbon fiber with the surface embedded with the boron nitride grains is obtained after being taken out.
The carbon fiber epoxy resin composite material is prepared from the modified carbon fiber, and the interface shear strength is 102 MPa.
The second embodiment is as follows: the embodiment provides a carbon fiber surface modification method, which is specifically completed according to the following steps:
first, remove glue
Putting 5g of carbon fibers into a Soxhlet extractor filled with an ethanol/acetone/tetrahydrofuran mixed solution with a volume ratio of 1:2:1, extracting for 15 hours at 50 ℃ by using the mixed solution, removing a sizing agent and impurities on the surfaces of the carbon fibers, then respectively soaking for 5min in an ethanol solution and a distilled water solution, and drying the cleaned carbon fibers for 50min in a blast drying box at 120 ℃ to obtain carbon fibers with clean surfaces;
secondly, generating boron nitride crystal grains
(1) Respectively preparing 0.02M boric acid solution and 0.01M sodium azide solution, then adding the boric acid solution into the sodium azide solution, wherein the volume ratio of the boric acid solution to the sodium azide solution is 1:2, stirring for 1.5h at 35 ℃, and rotating speed is 800 r/min;
(2) placing the carbon fiber obtained in the step one in the mixed solution obtained in the step two (1), then placing the reaction kettle in a constant temperature environment, wherein the constant temperature is 380 ℃, the constant temperature time is 18 hours, and then taking out the carbon fiber;
(3) repeating the step two (2) for 2-3 times to obtain carbon fibers with boron nitride grains on the surfaces;
the conversion rate of the boron nitride is calculated to be 40%.
Third, low temperature aging
(1) Placing the carbon fiber with the boron nitride grains on the surface obtained in the step two (3) in 200ml of secondary distilled water, and ultrasonically vibrating for 15min to clean residual growth liquid on the surface of the sample;
(2) and (2) drying the carbon fiber obtained in the step (1) in a vacuum drying oven at constant temperature to enhance the interface bonding capability of the boron nitride crystal grains and the carbon fiber. The constant temperature is 280 ℃, the constant temperature time is 11 hours, and then the carbon fiber with the surface embedded with the boron nitride crystal grains is obtained after being taken out.
The carbon fiber epoxy resin composite material prepared from the modified carbon fiber is detected to have the interface shear strength of 122 MPa.
The third concrete implementation mode: the embodiment provides a carbon fiber surface modification method, which is specifically completed according to the following steps: first, remove glue
Putting 5g of carbon fiber into a Soxhlet extractor filled with an ethanol/acetone/tetrahydrofuran mixed solution with a volume ratio of 1:2:2, extracting for 24 hours at 70 ℃ by using the mixed solution, removing a sizing agent and impurities on the surface of the carbon fiber, then respectively soaking for 8min in an ethanol solution and a distilled water solution, and drying the cleaned carbon fiber in a blast drying box at 150 ℃ for 60min to obtain carbon fiber with a clean surface;
secondly, generating boron nitride crystal grains
(1) Respectively preparing 0.03M boric acid solution and 0.008M sodium azide solution, then adding the boric acid solution into the sodium azide solution, wherein the volume ratio of the boric acid solution to the sodium azide solution is 1:5, stirring for 2h at 20 ℃, and the rotating speed is 1000 r/min;
(2) placing the carbon fiber obtained in the step one in the mixed solution obtained in the step two (1), then placing the reaction kettle in a constant temperature environment, wherein the constant temperature is 390 ℃, and the constant temperature time is 24 hours, and then taking out the carbon fiber;
(3) repeating the step two (2) for 2-3 times to obtain carbon fibers with boron nitride grains on the surfaces;
the conversion rate of boron nitride is calculated to be 36%.
Third, low temperature aging
(1) Placing the carbon fiber with the boron nitride grains on the surface obtained in the step two (3) in 300ml of secondary distilled water, and ultrasonically vibrating for 20min to clean residual growth liquid on the surface of the sample;
(2) and (2) drying the carbon fiber obtained in the step (1) in a vacuum drying oven at constant temperature to enhance the interface bonding capability of the boron nitride crystal grains and the carbon fiber. The constant temperature is 300 ℃, the constant temperature time is 12 hours, and then the carbon fiber with the surface embedded with the boron nitride grains is obtained after being taken out.
The carbon fiber epoxy resin composite material is prepared from the modified carbon fiber, and the interface shear strength of the carbon fiber epoxy resin composite material is 118 MPa.
Comparative example embodiment one: the embodiment provides a carbon fiber surface modification method, which is specifically completed according to the following steps:
first, remove glue
Putting 5g of carbon fibers into a Soxhlet extractor filled with an ethanol/acetone/tetrahydrofuran mixed solution with a volume ratio of 1:2:1, extracting for 15 hours at 50 ℃ by using the mixed solution, removing a sizing agent and impurities on the surfaces of the carbon fibers, then respectively soaking for 5min in an ethanol solution and a distilled water solution, and drying the cleaned carbon fibers for 50min in a blast drying box at 120 ℃ to obtain carbon fibers with clean surfaces;
secondly, generating boron nitride crystal grains
(1) Respectively preparing 0.02M boric acid solution and 0.01M sodium azide solution, then adding the boric acid solution into the sodium azide solution, wherein the volume ratio of the boric acid solution to the sodium azide solution is 1:0.5, stirring for 0.5h at 35 ℃, and rotating speed is 50 r/min;
(2) placing the carbon fiber obtained in the step one into the mixed solution obtained in the step two (1), then placing the reaction kettle in a constant temperature environment, wherein the constant temperature is 300 ℃, the constant temperature time is 10 hours, and then taking out the carbon fiber;
(3) repeating the step two (2) for 2-3 times to obtain carbon fibers with boron nitride grains on the surfaces;
the conversion rate of the boron nitride is calculated to be 29 percent.
Third, low temperature aging
(1) Placing the carbon fiber with the boron nitride grains on the surface obtained in the step two (3) in 300ml of secondary distilled water, and soaking and cleaning the residual growth liquid on the surface of the sample;
(2) and (2) drying the carbon fiber obtained in the step (1) in a vacuum drying oven at constant temperature to enhance the interface bonding capability of the boron nitride crystal grains and the carbon fiber. The constant temperature is 280 ℃, the constant temperature time is 10 hours, and then the carbon fiber with the surface embedded with the boron nitride crystal grains is obtained after being taken out.
The carbon fiber epoxy resin composite material prepared from the modified carbon fiber is detected to have the interface shear strength of 89 MPa.
Comparative example embodiment two: the embodiment provides a carbon fiber surface modification method, which is specifically completed according to the following steps:
first, remove glue
Putting 5g of carbon fibers into a Soxhlet extractor filled with an ethanol/acetone/tetrahydrofuran mixed solution with a volume ratio of 1:2:1, extracting for 15 hours at 50 ℃ by using the mixed solution, removing a sizing agent and impurities on the surfaces of the carbon fibers, then respectively soaking for 5min in an ethanol solution and a distilled water solution, and drying the cleaned carbon fibers for 50min in a blast drying box at 120 ℃ to obtain carbon fibers with clean surfaces;
secondly, generating boron nitride crystal grains
(1) Respectively preparing 0.01M boric acid solution and 0.02M sodium azide solution, then adding the boric acid solution into the sodium azide solution, wherein the volume ratio of the boric acid solution to the sodium azide solution is 1:2, stirring for 1.5h at 35 ℃, and rotating speed is 800 r/min;
(2) placing the carbon fiber obtained in the step one in the mixed solution obtained in the step two (1), then placing the reaction kettle in a constant temperature environment, wherein the constant temperature is 420 ℃, the constant temperature time is 18 hours, and then taking out the carbon fiber;
(3) repeating the step two (2) for 2-3 times to obtain carbon fibers with boron nitride grains on the surfaces;
the conversion rate of the boron nitride is calculated to be 28 percent.
Third, low temperature aging
(1) Placing the carbon fiber with the boron nitride grains on the surface obtained in the step two (3) in 200ml of secondary distilled water, and ultrasonically vibrating for 15min to clean residual growth liquid on the surface of the sample;
(2) and (2) drying the carbon fiber obtained in the step (1) in a vacuum drying oven at constant temperature to enhance the interface bonding capability of the boron nitride crystal grains and the carbon fiber. The constant temperature is 280 ℃, the constant temperature time is 11 hours, and then the carbon fiber with the surface embedded with the boron nitride crystal grains is obtained after being taken out.
The carbon fiber epoxy resin composite material prepared from the modified carbon fiber is detected to have the interface shear strength of 93 MPa.
Comparative example embodiment three: the embodiment provides a carbon fiber surface modification method, which is specifically completed according to the following steps:
first, remove glue
Putting 5g of carbon fiber into a Soxhlet extractor filled with an ethanol/acetone/tetrahydrofuran mixed solution with a volume ratio of 1:2:2, extracting for 24 hours at 70 ℃ by using the mixed solution, removing a sizing agent and impurities on the surface of the carbon fiber, then respectively soaking for 8min in an ethanol solution and a distilled water solution, and drying the cleaned carbon fiber in a blast drying box at 150 ℃ for 60min to obtain carbon fiber with a clean surface;
secondly, generating boron nitride crystal grains
(1) Respectively preparing 0.03M boric acid solution and 0.008M sodium azide solution, then adding the boric acid solution into the sodium azide solution, wherein the volume ratio of the boric acid solution to the sodium azide solution is 1:5, stirring for 2h at 20 ℃, and the rotating speed is 1000 r/min;
(2) placing the carbon fiber obtained in the step one in the mixed solution obtained in the step two (1), then placing the reaction kettle in a constant temperature environment, wherein the constant temperature is 390 ℃, and the constant temperature time is 24 hours, and then taking out the carbon fiber;
(3) repeating the step two (2) for 2-3 times to obtain carbon fibers with boron nitride grains on the surfaces;
the conversion rate of boron nitride is calculated to be 36%.
Third, low temperature aging
(1) Placing the carbon fiber with the boron nitride grains on the surface obtained in the step two (3) in 300ml of secondary distilled water, and ultrasonically vibrating for 20min to clean residual growth liquid on the surface of the sample;
(2) and (2) drying the carbon fiber obtained in the step (1) in a vacuum drying oven at constant temperature to enhance the interface bonding capability of the boron nitride crystal grains and the carbon fiber. The constant temperature is 100 ℃, the constant temperature time is 10 hours, and then the carbon fiber with the surface embedded with the boron nitride grains is obtained after being taken out.
The carbon fiber epoxy resin composite material is prepared from the modified carbon fiber, and the interface shear strength of the carbon fiber epoxy resin composite material is detected to be 100 MPa.
Claims (4)
1. A method for modifying the surface of carbon fibers is characterized by comprising the following steps:
step one, removing glue from carbon fiber
Putting carbon fibers into an organic solvent, removing a sizing agent and impurities on the surfaces of the carbon fibers, soaking the carbon fibers in the solution, and finally drying the carbon fibers to obtain carbon fibers with clean surfaces;
step two, generating boron nitride crystal grains
(1) Placing carbon fibers in a reaction kettle filled with a mixed solution of a boric acid solution and a sodium azide solution, wherein the mixed solution is prepared in a way that: firstly, respectively preparing a boric acid solution and a sodium azide solution, then adding the sodium azide solution into the boric acid solution, and uniformly stirring in a mechanical stirrer; then placing the reaction kettle in a constant temperature box, wherein the constant temperature in the constant temperature box is 350-390 ℃, and the constant temperature time is 12-24 hours, so as to obtain carbon fibers with boron nitride grains on the surfaces; the concentration of the boric acid solution is 0.02-0.03M, the concentration of the sodium azide solution is 0.008-0.01M, and the volume ratio of the boric acid solution to the sodium azide solution is 1: 1.5-1: 2;
(2) repeating the step two (1) for 2-3 times to obtain carbon fibers with uniformly distributed boron nitride;
step three, low-temperature aging
And (4) cleaning the carbon fiber obtained in the second step, removing the growth liquid on the surface of the carbon fiber, and then placing the carbon fiber in a vacuum drying oven for constant-temperature drying to finally obtain the carbon fiber with the surface coated with the boron nitride particles.
2. The method for surface modification of carbon fiber according to claim 1, wherein: the stirring time of the mixed solution is 1-2 h, the stirring temperature is 20-35 ℃, and the rotating speed is 750-1000 r/min.
3. The method for surface modification of carbon fiber according to claim 1, wherein: in the third step, the constant temperature drying temperature in the vacuum drying oven is 100-300 ℃; the time is 0.5-12 h.
4. A method of surface modification of carbon fibres as claimed in claim 3, characterised in that: the constant-temperature drying temperature in the vacuum drying oven is 250-300 ℃; the time is 10-12 h.
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| CN110453495B (en) * | 2019-09-24 | 2021-05-25 | 吉林大学 | Method for plating boron carbide on surface of carbon fiber |
| CN112724699A (en) * | 2021-01-19 | 2021-04-30 | 天津泰吉诺新材料科技有限公司 | Preparation process of multifunctional high-thermal-conductivity composite resin with structural orientation |
| CN114261111A (en) * | 2021-12-27 | 2022-04-01 | 西安理工大学 | Method for regulating and controlling micro-area tissue of carbon fiber reinforced resin matrix composite interface |
| CN114481600B (en) * | 2021-12-27 | 2024-05-03 | 西安理工大学 | Carbon fiber surface modification method |
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| CN1173879C (en) * | 2002-02-07 | 2004-11-03 | 山东大学 | Process for preparing nitride ultromicro powder and nitride crystal wunder hydrothermal condition |
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