CN110820323B - Preparation method of Si-C-O ceramic antioxidant coating on surface of carbon fiber - Google Patents
Preparation method of Si-C-O ceramic antioxidant coating on surface of carbon fiber Download PDFInfo
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- CN110820323B CN110820323B CN201911053729.4A CN201911053729A CN110820323B CN 110820323 B CN110820323 B CN 110820323B CN 201911053729 A CN201911053729 A CN 201911053729A CN 110820323 B CN110820323 B CN 110820323B
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- 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
- D06M11/77—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 silicon or compounds thereof
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Abstract
The invention discloses a preparation method of a Si-C-O ceramic antioxidant coating on the surface of carbon fiber, and relates to a preparation method of a carbon fiber antioxidant coating. The invention aims to solve the technical problem that the material performance is reduced due to the fact that an oxidation-resistant coating on the surface of carbon fiber prepared by a precursor impregnation cracking method has pores and cracks. The method comprises the following steps: adding a mixed monomer of propyl trimethoxy silane and phenyl trimethoxy silane into a potassium hydroxide aqueous solution for reaction, then filtering and drying a filter cake to obtain a precursor; dissolving the precursor in xylene to obtain a precursor solution; and repeatedly dipping and drying the polyacrylonitrile-based carbon fiber in the precursor solution, then sintering in an argon atmosphere, and then repeatedly dipping, drying and sintering to obtain the antioxidant Si-C-O ceramic coating on the surface of the carbon fiber. The anti-oxidation Si-C-O ceramic coating obtained on the surface of the carbon fiber by the method has no cracks and pores, and can be used in the fields of high temperature resistant and anti-oxidation materials.
Description
Technical Field
The invention relates to a preparation method of a carbon fiber antioxidant coating.
Background
With the rapid development of scientific technology, the industrial production has more and more urgent needs for novel ultralight, high temperature resistant, oxidation resistant and thermal shock resistant composite materials. The carbon fiber material is widely concerned by researchers by virtue of the characteristics of light weight, high strength and the like, is widely applied to various fields of human activities as a reinforcing material, and becomes a new high-tech industry in China. However, some lattice defects exist on the surface of the carbon fiber and active points caused by the defects caused by internal stress in the material preparation process, the active points are oxidized when the temperature of the active points exceeds 400 ℃ under the air condition, the comprehensive performance is greatly reduced due to low oxidation resistance, and the application of the carbon fiber composite material is greatly limited. Therefore, the research on the oxidation resistant coating of the carbon fiber material and the improvement of the oxidation resistance of the carbon fiber composite material at high temperature are the key points in the current research on the carbon fiber composite material.
At present, the surface of carbon fiber is modified by surface coating, and the methods generally comprise a sol-gel method, a plasma spraying method, a precursor impregnation pyrolysis method and the like. The precursor impregnation cracking method is to impregnate organic polymer precursor solution or melt containing Si (such as polycarbosilane, polymethylsilane and the like) into a carbon fiber preform, and then to crack at high temperature under inert gasification protection after drying and curing to obtain the carbon fiber composite material with the surface covered with SiC. The method can prepare a complicated special-shaped member, but the porosity is very high due to the overflow of a large amount of small molecules in the cracking process, and the carbon fiber ceramic composite material with high coating density is difficult to obtain; and the material has large volume shrinkage in the process of converting the organic precursor into the inorganic ceramic, and the performance of the material is reduced by microcrack and internal stress generated by shrinkage. For example, the article "cross-linking and cracking polysiloxane used as a ceramic precursor" published in 2004-198 of the science and engineering of polymer materials by Pinus massoniana discloses that hydrogen-containing polysiloxane is used as a raw material, and a precursor impregnation cracking method is utilized to prepare a continuous carbon fiber reinforced Si-C-O ceramic matrix composite through cross-linking and cracking of the hydrogen-containing polysiloxane and vinyl-containing polysiloxane, wherein a surface coating of the composite has pores and cracks.
Disclosure of Invention
The invention provides a preparation method of a Si-C-O ceramic antioxidant coating on the surface of carbon fiber, aiming at solving the technical problem that the material performance is reduced due to the pores and cracks of the antioxidant coating on the surface of carbon fiber prepared by the existing precursor impregnation cracking method.
The preparation method of the Si-C-O ceramic antioxidant coating on the surface of the carbon fiber comprises the following steps:
firstly, weighing 40-90% of propyl trimethoxy silane and 10-60% of phenyl trimethoxy silane according to the mass percentage, and uniformly mixing to obtain a mixed monomer;
secondly, adding potassium hydroxide into water to prepare a solution to obtain a potassium hydroxide solution, heating the potassium hydroxide solution to 55-75 ℃, dripping the mixed monomer into the potassium hydroxide solution under the stirring condition, continuously stirring for 4-6 hours under the condition of 55-75 ℃ after dripping is finished to ensure that silane is completely hydrolyzed, then filtering, and drying a filter cake to obtain a precursor;
dissolving the precursor in xylene to obtain a precursor solution;
fourthly, immersing the polyacrylonitrile-based carbon fibers into a precursor solution at the temperature of 110-150 ℃ for 3-5 hours, and taking out the polyacrylonitrile-based carbon fibers for drying; repeating the operations of soaking and drying to obtain the precursor-loaded carbon fiber;
placing the carbon fiber loaded with the precursor in a tube furnace, vacuumizing the tube furnace, then filling argon, and heating to 800-1500 ℃ in an argon atmosphere for 2-6 hours;
sixthly, repeating the operation of the fourth step and the operation of the fifth step to obtain the oxidation resistant Si-C-O ceramic coating on the surface of the carbon fiber.
The invention adopts propyl trimethoxy silane and phenyl trimethoxy silane as monomers for preparing the precursor, and the quantity of generated escaped micromolecule substances is greatly reduced when the precursor is organized at high temperature due to the influence of benzene rings in the monomers, thereby reducing the generation of cracks and pores and meeting the requirements of materials on high temperature resistance and oxidation resistance.
Drawings
FIG. 1 is a SEM photograph of a precursor obtained in step two of example 1;
FIG. 2 is a thermogravimetric plot of the precursor obtained in step two of example 1;
FIG. 3 is a scanning electron micrograph of precursor-supporting carbon fibers (i.e., carbon fiber ceramic coatings before oxidation) obtained in step four of example 1;
FIG. 4 is an XRD spectrum of the antioxidant Si-C-O ceramic coating obtained on the surface of the carbon fiber through step six in example 1;
FIG. 5 is a scanning electron microscope photograph of the oxidation-resistant Si-C-O ceramic coating on the surface of the carbon fiber obtained in step six of example 1.
Detailed Description
The first embodiment is as follows: the preparation method of the Si-C-O ceramic antioxidant coating on the surface of the carbon fiber comprises the following steps:
firstly, weighing 40-90% of propyl trimethoxy silane and 10-60% of phenyl trimethoxy silane according to the mass percentage, and uniformly mixing to obtain a mixed monomer;
secondly, adding potassium hydroxide into water to prepare a solution to obtain a potassium hydroxide solution, heating the potassium hydroxide solution to 55-75 ℃, dripping the mixed monomer into the potassium hydroxide solution under the stirring condition, continuously stirring for 4-6 hours under the condition of 55-75 ℃ after dripping is finished to ensure that silane is completely hydrolyzed, then filtering, and drying a filter cake to obtain a precursor;
dissolving the precursor in xylene to obtain a precursor solution;
fourthly, immersing the polyacrylonitrile-based carbon fibers into a precursor solution at the temperature of 110-150 ℃ for 3-5 hours, and taking out the polyacrylonitrile-based carbon fibers for drying; repeating the operations of soaking and drying to obtain the precursor-loaded carbon fiber;
placing the carbon fiber loaded with the precursor in a tube furnace, vacuumizing the tube furnace, then filling argon, and heating to 800-1500 ℃ in an argon atmosphere for 2-6 hours;
sixthly, repeating the operation of the fourth step and the operation of the fifth step to obtain the oxidation resistant Si-C-O ceramic coating on the surface of the carbon fiber.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the concentration of the potassium hydroxide solution in the second step is 0.025-0.1 mol/L; the rest is the same as the first embodiment.
The third concrete implementation mode: the second embodiment is different from the first or second embodiment in that the water in the second step is ultrapure water; the other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is that the mass percentage concentration of the precursor in the precursor solution in the third step is 10% to 15%; the others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between the present embodiment and one of the first to fourth embodiments is that the number of times of repeated soaking and drying operations in the fourth step is 3-5 times; the other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between the present embodiment and one of the first to fifth embodiments is that in the sixth embodiment, the number of times of repeating the operations of the fourth and fifth steps is 3 to 5 times; the other is the same as one of the first to fifth embodiments.
The following examples are used to demonstrate the beneficial effects of the present invention:
example 1: the preparation method of the Si-C-O ceramic antioxidant coating on the surface of the carbon fiber provided by the embodiment comprises the following steps:
firstly, weighing 64 g of propyl trimethoxy silane and 16 g of phenyl trimethoxy silane, and uniformly mixing to obtain a mixed monomer; wherein the mass percent of the propyl trimethoxy silane is 80 percent, and the mass percent of the phenyl trimethoxy silane is 20 percent;
secondly, adding 0.37g of potassium hydroxide into 266.77g of ultrapure water to prepare a solution to obtain a potassium hydroxide solution with the concentration of 0.025mol/L, heating the potassium hydroxide solution to 55 ℃, dripping the mixed monomer into the potassium hydroxide solution under the stirring condition, continuously stirring for 5 hours under the temperature of 55 ℃ after dripping is finished to ensure that silane is completely hydrolyzed, then filtering, and drying a filter cake to obtain a precursor; the precursor is white powder;
thirdly, dissolving the precursor in dimethylbenzene according to the mass percentage concentration of the precursor of 10 percent to obtain a precursor solution;
fourthly, the polyacrylonitrile-based carbon fiber is immersed into a precursor solution at the temperature of 110 ℃ for 3 hours, and the polyacrylonitrile-based carbon fiber is taken out and dried; repeating the operations of soaking and drying for 3 times to obtain carbon fibers loaded with precursors;
placing the carbon fiber loaded with the precursor in a tube furnace, vacuumizing the tube furnace, then filling argon, and heating to 1400 ℃ in the argon atmosphere for 4 hours;
sixthly, repeating the operation of the fourth step and the operation of the fifth step for 3 times to obtain the oxidation resistant Si-C-O ceramic coating on the surface of the carbon fiber.
The scanning electron micrograph of the precursor obtained in the second step of this example 1 is shown in fig. 1, and it can be seen from fig. 1 that the precursor resin is spherical particles, and the particle diameter is uniform and is 400 to 600 nm.
The thermogravimetric curve of the precursor obtained in step two of this example 1 is shown in fig. 2, and it can be seen from fig. 2 that the process of cracking the precursor resin into the derived ceramic body can be roughly divided into three stages: the first stage is at room temperature to 370 ℃, and the weight loss of the sample in the process is very small (about 4%), mainly the escape of uncrosslinked small molecules in the sample. The second stage is 370-600 ℃, the weight loss of the sample is obvious in the process, mainly the cracking and rearrangement reaction between Si-O, Si-C and Si-H occurs in the sample, silane escapes, organic-inorganic conversion is carried out, and a large amount of small molecule gas (such as CH) is released 4 、H 2 Etc.). The third stage is>At 600 ℃. During this process, mainly some other impurities are completely decomposed and the extensive breaking of C-H, Si-C and Si-O bonds proceed to ceramming, the composition of the resulting ceramic body being free carbon and amorphous [ Si (O, C) ] 4 ]Phase, the ceramming weight loss rate of the precursor prepared in this example was calculated to be only 26%.
The scanning electron micrograph of the precursor-supporting carbon fiber obtained in step four of example 1 (i.e., before oxidation of the carbon fiber ceramic coating) is shown in fig. 3, and it can be seen from fig. 3 that the precursor resin is uniformly supported on the carbon fiber.
The XRD spectrum of the antioxidant Si-C-O ceramic coating obtained on the surface of the carbon fiber in the sixth step of example 1 is shown in fig. 4, and it can be seen from fig. 4 that the ceramic body has no distinct diffraction peak and is in an amorphous structure.
In this example 1, a scanning electron microscope photograph of the oxidation-resistant Si-C-O ceramic coating on the surface of the carbon fiber after the six steps is shown in fig. 5, and it can be seen from fig. 5 that the oxidation-resistant Si-C-O ceramic coating on the surface of the carbon fiber has no cracks and no pores.
Example 2: the preparation method of the Si-C-O ceramic antioxidant coating on the surface of the carbon fiber provided by the embodiment comprises the following steps:
weighing 40 g of propyl trimethoxy silane and 40 g of phenyl trimethoxy silane, and uniformly mixing to obtain a mixed monomer; wherein the mass percent of the propyl trimethoxy silane is 50 percent, and the mass percent of the phenyl trimethoxy silane is 50 percent;
secondly, adding 0.37g of potassium hydroxide into 266.77g of ultrapure water to prepare a solution to obtain a potassium hydroxide solution with the concentration of 0.025mol/L, heating the potassium hydroxide solution to 60 ℃, dripping the mixed monomer into the potassium hydroxide solution under the stirring condition, continuously stirring for 5 hours under the condition of 60 ℃ after dripping is finished to ensure that silane is completely hydrolyzed, then filtering, and drying a filter cake to obtain a precursor; the precursor is white powder;
dissolving the precursor in xylene according to the mass percentage concentration of the precursor of 20% to obtain a precursor solution;
fourthly, immersing the polyacrylonitrile-based carbon fiber into a precursor solution at the temperature of 110 ℃ for 3 hours, and taking out and drying the polyacrylonitrile-based carbon fiber; repeating the operations of soaking and drying for 3 times to obtain carbon fibers loaded with precursors;
placing the carbon fiber loaded with the precursor in a tube furnace, vacuumizing the tube furnace, then filling argon, and heating to 900 ℃ in the argon atmosphere for 4 hours;
sixthly, repeating the operation of the fourth step and the operation of the fifth step for 3 times to obtain the oxidation resistant Si-C-O ceramic coating on the surface of the carbon fiber.
The anti-oxidation Si-C-O ceramic coating on the surface of the carbon fiber obtained in the embodiment 2 has no cracks and no pores, and can meet the requirements of materials on high temperature resistance and oxidation resistance.
Claims (1)
1. A preparation method of a Si-C-O ceramic anti-oxidation coating on the surface of carbon fiber is characterized by comprising the following steps:
firstly, weighing 64 g of propyl trimethoxy silane and 16 g of phenyl trimethoxy silane, and uniformly mixing to obtain a mixed monomer; wherein the mass percent of the propyl trimethoxy silane is 80 percent, and the mass percent of the phenyl trimethoxy silane is 20 percent;
secondly, adding 0.37g of potassium hydroxide into 266.77g of ultrapure water to prepare a solution to obtain a potassium hydroxide solution with the concentration of 0.025mol/L, heating the potassium hydroxide solution to 55 ℃, dripping the mixed monomer into the potassium hydroxide solution under the stirring condition, continuously stirring for 5 hours under the temperature of 55 ℃ after dripping is finished to ensure that silane is completely hydrolyzed, then filtering, and drying a filter cake to obtain a precursor; the precursor is white powder;
thirdly, dissolving the precursor in dimethylbenzene according to the mass percentage concentration of the precursor of 10 percent to obtain a precursor solution;
fourthly, immersing the polyacrylonitrile-based carbon fiber into a precursor solution at the temperature of 110 ℃ for 3 hours, and taking out and drying the polyacrylonitrile-based carbon fiber; repeating the operations of soaking and drying for 3 times to obtain carbon fibers loaded with precursors;
placing the carbon fiber loaded with the precursor in a tube furnace, vacuumizing the tube furnace, then filling argon, and heating to 1400 ℃ in the argon atmosphere for 4 hours;
sixthly, repeating the operation of the fourth step and the operation of the fifth step for 3 times to obtain the oxidation resistant Si-C-O ceramic coating on the surface of the carbon fiber.
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