CN113846482A - Preparation method of carbon fiber/rare earth oxide nanowire mixed reinforcement, material obtained by preparation method and application of material - Google Patents
Preparation method of carbon fiber/rare earth oxide nanowire mixed reinforcement, material obtained by preparation method and application of material Download PDFInfo
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- 239000004917 carbon fiber Substances 0.000 title claims abstract description 96
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 95
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000002070 nanowire Substances 0.000 title claims abstract description 84
- 230000002787 reinforcement Effects 0.000 title claims abstract description 64
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title abstract description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 4
- 239000011153 ceramic matrix composite Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- -1 rare earth salt Chemical class 0.000 claims description 22
- 230000015572 biosynthetic process Effects 0.000 claims description 20
- 238000003786 synthesis reaction Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012295 chemical reaction liquid Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 230000010355 oscillation Effects 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000011065 in-situ storage Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 4
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 3
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 29
- 239000000243 solution Substances 0.000 description 22
- 229910000420 cerium oxide Inorganic materials 0.000 description 17
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 17
- 239000002041 carbon nanotube Substances 0.000 description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229910052684 Cerium Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000002679 ablation Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002249 LaCl3 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement, and an obtained material and application thereof. The preparation method avoids using reagents with high cost and environmental pollution, has simple and controllable preparation process and low reaction temperature, and can control the composition, content and the like of the rare earth oxide nanowires through the design of the proportion of a reaction solution and reaction conditions; the mixed reinforcement prepared by the invention can give consideration to the advantages of the carbon fiber and the nano wire in the interface and the cross-scale cooperative reinforcement of the matrix and the modification effect of the rare earth on the surface of the carbon fiber, and can be used for reinforcing polymers, carbon and ceramic matrix composite materials.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement, and an obtained material and application thereof.
Background
Carbon fiber is widely used as a reinforcement of polymer-based, carbon-based and ceramic-based composite materials due to the characteristics of high specific strength and specific modulus, small thermal expansion coefficient, excellent high-temperature mechanical properties and the like. However, the chemical inertness of the surface of the carbon fiber causes the interface bonding between the carbon fiber and a matrix to be weaker, particularly, when the carbon prepared at high temperature and a ceramic matrix are reinforced, the functional group of surface modification is eliminated, the interface bonding depends on mechanical meshing, the interlayer strength is low, and the reinforcing potential performance and the overall structural performance of the composite material are limited. The cross-micron and nano-scale mixed reinforcement body of the carbon fiber surface loaded with the nano material is an effective way for improving the interface bonding and mechanical properties of the composite material, and the carbon nanotube is most applied at present. The rare earth nano material has obvious application effect in catalysis, luminescence, permanent magnetism, microelectronics and composite materials due to unique physical and chemical properties.
Patent documents CN104231605, CN1587319, CN1597774, CN1597765, CN109693424 and CN1807496 describe that the strength and friction performance of polymer matrix composite material are improved by carbon fiber/rare earth compound particle mixed reinforcement by soaking carbon fiber cloth in ethanol solution containing one or more of lanthanum chloride, cerium chloride, lanthanum oxide and cerium oxide.
Patent document No. CN102351556 discloses a preparation method of rare earth toughened carbon/carbon composite material, which utilizes rare earth compound particles loaded on the surface of carbon fiber to improve the strength and toughness of the C/C composite material.
Literature [ Materials Science&Engineering A529 (2011)177-]Research shows that the carbon fiber/LaCl3The particle mixed reinforcement improves the interface combination and the matrix structure of the C/C composite material and catalyzes the growth of the carbon nano tube, thereby improving the mechanical property, the heat conduction property, the friction property and the ablation resistance property.
The literature "The effects of addition of La2O3 on The microstructure and mechanical properties of C/C compositions [ Materials Science&Engineering A,610(2014)350-354]", by using La on the surface of carbon fibers2O3The particles improve the mechanical property of the C/C composite material.
The rare earth compounds disclosed in the above documents are in the form of particles, and do not relate to the formation of a cross-scale mixed reinforcement by using rare earth oxide nanowires and carbon fibers, and the particles and the carbon fibers are weak in combination, easy to fall off, and limited in reinforcing effect on a composite material interface and a matrix. In addition, the preparation method uses solvents such as ethanol, ammonium chloride, nitric acid and the like, so that the cost is high and the environment is polluted.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body and an obtained material and application thereof. The method utilizes the aqueous solution containing rare earth ions to grow the rare earth oxide nanowires on the surfaces of the prefabricated carbon fibers, thereby avoiding the use of reagents with high cost and environmental pollution. The mixed reinforcement has the functions of cross-scale coordination and reinforcement of the carbon fibers and the nanowires and modification of the surfaces of the carbon fibers by the rare earth, and the rare earth oxide has high melting point and great potential in the aspects of improving the high-temperature mechanics and ablation resistance of the composite material. The carbon fiber/rare earth carbide nanowire/carbon nanotube mixed reinforcement can be further prepared by utilizing the advantages of the rare earth oxide nanowire in the catalytic growth of the carbon nanotube.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body comprises the following steps:
1) placing the carbon fiber preform in an atmosphere protection furnace, carrying out heat treatment for 2-5 h at 500-1000 ℃, then carrying out ultrasonic oscillation cleaning by using deionized water, and drying for later use at 80-120 ℃;
2) preparing a water solution from dried rare earth salt, dripping a surfactant, stirring for a period of time at 30-50 ℃, and dripping a sodium hydroxide solution to adjust the pH value to 10-13 to obtain a reaction solution;
3) placing the reaction liquid obtained in the step 2) and the carbon fiber preform obtained in the step 1) into a reaction kettle, and carrying out in-situ synthesis on the rare earth oxide nanowire after ultrasonic oscillation for a period of time to obtain a treated carbon fiber preform;
4) soaking the carbon fiber preform obtained in the step 3) with deionized water, cleaning, drying and weighing, calculating the content of the rare earth oxide nanowire, and repeating the steps 3) and 4) to obtain a crude product of the carbon fiber/rare earth oxide nanowire mixed reinforcement with the content of the rare earth oxide nanowire of 2-10 wt%;
5) calcining the crude mixed reinforcement product obtained in the step 4) for 1-5 hours at the temperature of 300-600 ℃ under the protection of nitrogen to obtain a mixed reinforcement product which optimizes the shape of the rare earth oxide nanowire and removes residual organic matters.
Further, the preparation method of the carbon fiber/rare earth oxide nanowire mixed reinforcement body as described above, in step 1)The carbon fiber preform is any one of carbon fiber cloth, a carbon fiber integral felt, a carbon fiber needling and a woven preform, and the density of the carbon fiber felt, the carbon fiber needling or the woven preform is 0.20-0.70 g/cm3。
Further, in the preparation method of the carbon fiber/rare earth oxide nanowire mixed reinforcement, in the step 2), the rare earth salt is at least one of cerium chloride, lanthanum chloride, cerium sulfate, lanthanum sulfate, cerium nitrate and lanthanum nitrate.
Further, in the preparation method of the carbon fiber/rare earth oxide nanowire hybrid reinforcement, in the step 2), the surfactant is any one of cetyl trimethyl ammonium bromide, urea, ethylene glycol and alkylphenol polyoxyethylene.
Further, in the preparation method of the carbon fiber/rare earth oxide nanowire mixed reinforcement, in the step 2), the concentration of rare earth ions in the reaction solution is 0.1-0.6 mol/L, the concentration of the surfactant is 0.05-0.15 mol/L, and the concentration ratio of the rare earth ions to the sodium hydroxide is 1: 2-1: 5.
Further, in the preparation method of the carbon fiber/rare earth oxide nanowire hybrid reinforcement, in step 3), the in-situ synthesis conditions are as follows: the synthesis temperature is 120-200 ℃, the synthesis time is 5-10 h, the pressure is 1-3 MPa, and the reaction liquid is magnetically stirred in the whole process.
A carbon fiber/rare earth oxide nanowire mixed reinforcement is prepared by the preparation method. The carbon fiber/rare earth oxide nanowire hybrid reinforcement can be used for reinforcing polymers, carbon and ceramic matrix composite materials.
The invention has the beneficial effects that:
1. the preparation method provided by the invention is scientific and reasonable in design, and the carbon fiber/rare earth oxide nanowire mixed reinforcement with the rare earth oxide nanowire content of 2-10% is obtained by placing the carbon fiber preform in a rare earth salt reaction solution, performing magnetic stirring, high-temperature and high-pressure in-situ synthesis reaction, cleaning, drying and calcining.
2. The preparation method avoids using reagents with high cost and environmental pollution, has simple and controllable preparation process and low reaction temperature, has the nanowire yield of more than 80 percent, and can control the composition, the content and the like of the rare earth oxide nanowire through the design of the proportion of a reaction solution and the reaction conditions. In addition, based on the advantages of the rare earth oxide nanowires for catalytic growth of the carbon nanotubes, the carbon fiber/rare earth carbide nanowire/carbon nanotube mixed reinforcement can be prepared, and the mechanical properties, ablation resistance, frictional wear resistance and other properties of the composite material are further improved.
3. The mixed reinforcement prepared by the invention can give consideration to the cross-scale synergistic reinforcement advantages of the carbon fiber and the nano wire to the interface and the matrix and the modification effect of the rare earth to the surface of the carbon fiber, particularly the melting point of the rare earth oxide is high, the bonding and mechanical properties of the composite material interface are improved, the high-temperature strength, the high-temperature ablation resistance and the frictional wear resistance are improved, and the requirements of harsh service environment on the combination of the structure and the function of the composite material are met.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an X-ray diffraction pattern of cerium oxide nanowires in a hybrid reinforcement prepared in example 1;
FIG. 2 is a transmission electron micrograph of cerium oxide nanowires in the hybrid reinforcement prepared in example 1;
FIG. 3 is a scanning electron micrograph of the carbon fiber/lanthanum oxide nanowire hybrid reinforcement prepared in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body specifically comprises the following steps:
1) and (3) placing the carbon fiber preform in an atmosphere protection furnace, carrying out heat treatment for 2-5 h at 500-1000 ℃, then carrying out ultrasonic oscillation cleaning by using deionized water, and drying for later use at 80-120 ℃.
2) Preparing a water solution from dried rare earth salt, dripping a surfactant, stirring for 30min at 30-50 ℃ by using a magnetic stirrer, and dripping a sodium hydroxide solution to adjust the pH value to 10-13 to obtain a reaction solution, wherein the concentration of rare earth ions is 0.1-0.6 mol/L, the concentration of the activator is 0.05-0.15 mol/L, and the concentration ratio of the rare earth ions to the sodium hydroxide is 1: 2-1: 5.
3) And (3) placing the reaction liquid and the treated carbon fiber preform into a reaction kettle, carrying out ultrasonic oscillation for 30min, then carrying out in-situ synthesis on the rare earth oxide nanowire, wherein the synthesis temperature is 120-200 ℃, the synthesis time is 5-10 h, the pressure is 1-3 MPa, and the whole process is carried out on the reaction liquid through magnetic stirring.
4) Soaking the treated carbon fiber preform in deionized water, cleaning, drying and weighing, calculating the content of the rare earth oxide nanowire, and repeating the step 3) and the step 4) to obtain a crude product of the carbon fiber/rare earth oxide nanowire mixed reinforcement with the nanowire content of 2-10 wt%.
5) And calcining the mixed reinforcement for 1-5 hours at 300-600 ℃ under the protection of nitrogen, optimizing the shape of the rare earth oxide nanowire and removing residual organic matters to obtain a carbon fiber/rare earth oxide nanowire mixed reinforcement finished product.
The specific embodiment of the invention is as follows:
example 1
A preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body comprises the following steps:
1) arranging the carbon fiber in a vacuum atmosphere protection furnace, carrying out heat treatment at 500 ℃ for 5h, then carrying out ultrasonic oscillation cleaning by using deionized water, and drying at 80 ℃ for later use.
2) Preparing dried cerium chloride into an aqueous solution, dropwise adding cetyl trimethyl ammonium bromide, stirring for 30min at 30 ℃ by using a magnetic stirrer, and simultaneously dropwise adding a sodium hydroxide solution to adjust the pH value to 10 to obtain a reaction solution, wherein the concentration of cerium ions is 0.1mol/L, the concentration of cetyl trimethyl ammonium bromide is 0.05mol/L, and the concentration ratio of cerium to sodium hydroxide is 1: 2.
3) And (3) arranging the reaction liquid and the treated carbon fiber in a reaction kettle, carrying out in-situ synthesis on the cerium oxide nanowire after ultrasonic oscillation for 30min, wherein the synthesis temperature is 120 ℃, the time is 7h, the pressure is 1MPa, and the whole process is used for magnetically stirring the reaction liquid. The X-ray diffraction results of the prepared cerium oxide nanowires are shown in fig. 1, and the transmission electron microscope results are shown in fig. 2.
4) Soaking the treated carbon fiber cloth in deionized water, cleaning, drying and weighing, calculating the content of the cerium oxide nanowire, and repeating the step 3) and the step 4) to obtain a crude product of the carbon fiber/cerium oxide nanowire mixed reinforcement with the cerium oxide nanowire content of 2 wt%.
5) And calcining the mixed reinforcement body for 3 hours at 300 ℃ under the protection of nitrogen, optimizing the appearance of the cerium oxide nanowire and removing residual organic matters to obtain a carbon fiber/cerium oxide nanowire mixed reinforcement body finished product.
Example 2
A preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body comprises the following steps:
1) the density is 0.20g/cm3The carbon fiber integrated felt is placed in an atmosphere protection furnace and is subjected to heat treatment at 700 ℃ for 4 hours, and then is cleaned by ultrasonic oscillation of deionized water and is dried at 90 ℃ for later use.
2) Preparing dried lanthanum chloride into an aqueous solution, dripping ethylene glycol, stirring for 30min at 40 ℃ by using a magnetic stirrer, and dripping sodium hydroxide solution to adjust the pH value to 11 to obtain a reaction solution, wherein the concentration of lanthanum ions is 0.3mol/L, the concentration of ethylene glycol is 0.1mol/L, and the concentration ratio of cerium to sodium hydroxide is 1: 3.
3) And (3) placing the reaction liquid and the treated carbon fiber integral felt in a reaction kettle, carrying out ultrasonic oscillation for 30min, then carrying out in-situ synthesis on the lanthanum oxide nanowire, wherein the synthesis temperature is 200 ℃, the time is 5h, the pressure is about 3MPa, and the whole process is carried out for magnetically stirring the reaction liquid.
4) Soaking the treated carbon fiber whole felt in deionized water, cleaning, drying and weighing, calculating the content of the lanthanum oxide nanowire, and repeating the step 3) and the step 4) to obtain a crude carbon fiber/lanthanum oxide nanowire mixed reinforcement product with the lanthanum oxide nanowire content of 5 wt%.
5) And calcining the mixed reinforcement body for 5 hours at 400 ℃ under the protection of nitrogen to optimize the shape of the lanthanum oxide nanowire and remove residual organic matters to obtain a finished product of the carbon fiber/lanthanum oxide nanowire mixed reinforcement body, wherein the scanning electron microscope result of the finished product is shown in figure 3.
Example 3
A preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body comprises the following steps:
1) the density is 0.50g/cm3The carbon fiber needling preform is placed in an atmosphere protection furnace and is subjected to heat treatment at 850 ℃ for 3h, then is cleaned by ultrasonic oscillation of deionized water, and is dried at 100 ℃ for later use.
2) Preparing dried cerium sulfate into an aqueous solution, dripping a urea solution, stirring for 30min at 50 ℃ by using a magnetic stirrer, and dripping a sodium hydroxide solution to adjust the pH value to 12 to obtain a reaction solution, wherein the concentration of cerium ions is 0.4mol/L, the concentration of urea is 0.12mol/L, and the concentration ratio of cerium to sodium hydroxide is 1: 4.
3) And (3) placing the reaction liquid and the treated carbon fiber needling preform in a reaction kettle, carrying out in-situ synthesis on the cerium oxide nanowire after ultrasonic oscillation is carried out for 30min, wherein the synthesis temperature is 160 ℃, the time is 8h, the pressure is 2MPa, and the whole process is carried out on the magnetic stirring of the reaction liquid.
4) Soaking the treated carbon fiber needled preform in deionized water, cleaning, drying and weighing, calculating the content of the cerium oxide nanowire, and repeating the step 3) and the step 4) to obtain a carbon fiber/cerium oxide nanowire mixed reinforcement crude product with the cerium oxide nanowire content of 7 wt%.
5) And calcining the carbon fiber/cerium oxide nanowire mixed reinforcement for 1h at 500 ℃ under the protection of nitrogen, optimizing the appearance of the cerium oxide nanowire and removing residual organic matters to obtain a carbon fiber/cerium oxide nanowire mixed reinforcement finished product.
Example 4
A preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body comprises the following steps:
1) the density is 0.70g/cm3The carbon fiber woven preform is placed in an atmosphere protection furnace and is subjected to heat treatment at 1000 ℃ for 2 hours, then is subjected to ultrasonic oscillation cleaning by deionized water, and is dried at 120 ℃ for later use.
2) Preparing a water solution from dried lanthanum nitrate, dripping alkylphenol ethoxylates, stirring for 30min at 30 ℃ by using a magnetic stirrer, and dripping a sodium hydroxide solution to adjust the pH value to 13 to obtain a reaction solution, wherein the concentration of lanthanum ions is 0.6mol/L, the concentration of the alkylphenol ethoxylates is 0.15mol/L, and the concentration ratio of lanthanum to sodium hydroxide is 1: 5.
3) And (3) placing the reaction liquid and the treated carbon fiber woven preform in a reaction kettle, carrying out in-situ synthesis on the lanthanum oxide nanowire after ultrasonic oscillation for 30min, wherein the synthesis temperature is 140 ℃, the time is 10h, the pressure is 2MPa, and the whole process is carried out by magnetically stirring the reaction liquid.
4) Soaking the treated carbon fiber woven preform in deionized water, cleaning, drying and weighing, calculating the content of the lanthanum oxide nanowire, and repeating the step 3) and the step 4) to obtain a crude carbon fiber/lanthanum oxide nanowire mixed reinforcement product with the lanthanum oxide nanowire content of 10 wt%.
5) And calcining the mixed reinforcement body for 4 hours at the temperature of 600 ℃ under the protection of nitrogen, optimizing the shape of the lanthanum oxide nanowire and removing residual organic matters to obtain a carbon fiber/lanthanum oxide nanowire mixed reinforcement body finished product.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A preparation method of a carbon fiber/rare earth oxide nanowire mixed reinforcement body is characterized by comprising the following steps:
1) placing the carbon fiber preform in an atmosphere protection furnace, carrying out heat treatment for 2-5 h at 500-1000 ℃, then carrying out ultrasonic oscillation cleaning by using deionized water, and drying for later use at 80-120 ℃;
2) preparing a water solution from dried rare earth salt, dripping a surfactant, stirring for a period of time at 30-50 ℃, and dripping a sodium hydroxide solution to adjust the pH value to 10-13 to obtain a reaction solution;
3) placing the reaction liquid obtained in the step 2) and the carbon fiber preform obtained in the step 1) into a reaction kettle, and carrying out in-situ synthesis on the rare earth oxide nanowire after ultrasonic oscillation for a period of time to obtain a treated carbon fiber preform;
4) soaking the carbon fiber preform obtained in the step 3) with deionized water, cleaning, drying and weighing, calculating the content of the rare earth oxide nanowire, and repeating the steps 3) and 4) to obtain a crude product of the carbon fiber/rare earth oxide nanowire mixed reinforcement with the content of the rare earth oxide nanowire of 2-10 wt%;
5) calcining the crude mixed reinforcement product obtained in the step 4) for 1-5 hours at the temperature of 300-600 ℃ under the protection of nitrogen to obtain a mixed reinforcement product which optimizes the shape of the rare earth oxide nanowire and removes residual organic matters.
2. The method for preparing the carbon fiber/rare earth oxide nanowire hybrid reinforcement according to claim 1, characterized in that: in the step 1), the carbon fiber preform is any one of carbon fiber cloth, a carbon fiber integral felt, carbon fiber needling and a woven preform, and the density of the carbon fiber felt, the carbon fiber needling or the woven preform is 0.20-0.70 g/cm3。
3. The method for preparing the carbon fiber/rare earth oxide nanowire hybrid reinforcement according to claim 1, characterized in that: in the step 2), the rare earth salt is at least one of cerium chloride, lanthanum chloride, cerium sulfate, lanthanum sulfate, cerium nitrate and lanthanum nitrate.
4. The method for preparing the carbon fiber/rare earth oxide nanowire hybrid reinforcement according to claim 1, characterized in that: in the step 2), the surfactant is any one of cetyl trimethyl ammonium bromide, urea, ethylene glycol and alkylphenol polyoxyethylene.
5. The method for preparing the carbon fiber/rare earth oxide nanowire hybrid reinforcement according to claim 1, characterized in that: in the step 2), the concentration of rare earth ions in the reaction liquid is 0.1-0.6 mol/L, the concentration of a surfactant is 0.05-0.15 mol/L, and the concentration ratio of the rare earth ions to sodium hydroxide in the reaction liquid is 1: 2-1: 5.
6. The method for preparing the carbon fiber/rare earth oxide nanowire hybrid reinforcement according to claim 1, characterized in that: in the step 3), the in-situ synthesis conditions are as follows: the synthesis temperature is 120-200 ℃, the synthesis time is 5-10 h, the pressure is 1-3 MPa, and the reaction liquid is magnetically stirred in the whole process.
7. A carbon fiber/rare earth oxide nanowire hybrid reinforcement prepared by the preparation method of any one of claims 1 to 6.
8. Use of the hybrid reinforcement of claim 7 for reinforcing polymer, carbon and ceramic matrix composites.
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