CN114541136A - Modified silicon carbide sizing agent for improving wave absorption performance of carbon fiber and preparation method thereof - Google Patents
Modified silicon carbide sizing agent for improving wave absorption performance of carbon fiber and preparation method thereof Download PDFInfo
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- CN114541136A CN114541136A CN202210097044.5A CN202210097044A CN114541136A CN 114541136 A CN114541136 A CN 114541136A CN 202210097044 A CN202210097044 A CN 202210097044A CN 114541136 A CN114541136 A CN 114541136A
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- silicon carbide
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- sizing agent
- emulsifier
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 55
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 53
- 238000004513 sizing Methods 0.000 title claims abstract description 43
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 30
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 47
- 239000003607 modifier Substances 0.000 claims description 28
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 19
- 235000019441 ethanol Nutrition 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 13
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 9
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 9
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 9
- 229920000053 polysorbate 80 Polymers 0.000 claims description 9
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 9
- 239000001587 sorbitan monostearate Substances 0.000 claims description 9
- 235000011076 sorbitan monostearate Nutrition 0.000 claims description 9
- 229940035048 sorbitan monostearate Drugs 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000001804 emulsifying effect Effects 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 2
- 229960000583 acetic acid Drugs 0.000 claims 1
- 239000012362 glacial acetic acid Substances 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 12
- 239000000835 fiber Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011208 reinforced composite material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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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
- D06M11/77—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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- 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
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- 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
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- 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
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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Abstract
The invention discloses a modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers and a preparation method thereof, wherein the sizing agent consists of modified silicon carbide, an emulsifier, alcohol and thermosetting resin, and the weight percentage of the modified silicon carbide, the emulsifier, the alcohol and the thermosetting resin is 0.1-10 wt%: 10-20 wt%: 40-70wt%: 10-40wt%, and the sizing agent can be directly used for carbon fibers, so that the carbon fibers have certain wave absorption on the basis of improving the bonding property of the carbon fibers, and the carbon fiber composite material product has the wave absorption.
Description
Technical Field
The invention belongs to the field of production of carbon fiber composite materials, and particularly relates to a modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers and a preparation method thereof.
Background
The carbon fiber has the characteristics of high temperature resistance, light weight, high strength, high modulus and the like, and has excellent reinforcing and toughening effects, so that the purposes of reducing weight and improving mechanical properties can be effectively achieved by using the carbon fiber reinforced composite material, and common carbon fiber reinforced resin-based prepreg is widely concerned and applied to aerospace and military products. At present, the development trend of composite materials is structural function integration, and carbon fiber reinforced composite materials are excellent in mechanical properties and general in functional properties. The concrete aspects are as follows:
(1) the binding property is poor: the common carbon fiber has larger brittleness and serious static electricity, is not easy to bundle in the production, weaving and transportation processes, and is easy to generate broken filaments and even break; in addition, the carbon fiber has smooth surface and low surface energy, which is not beneficial to the infiltration of resin and the interface combination of the composite material;
(2) poor wave absorption: the carbon fiber composite material applied to the fields of aerospace, military industry and the like has corresponding requirements on how to ensure the product performance and improve the electromagnetic shielding capability. At present, only carbon fibers with special-shaped cross sections and carbon fiber composites with special-shaped structures have a wave absorbing function, and ordinary carbon fibers serving as reflectors of electromagnetic waves do not have wave absorbing performance, so that the ordinary carbon fiber composites have poor wave absorbing performance. At present, in order to make a carbon fiber composite material product have or improve its wave absorption, a metal material such as a copper mesh or a foam material such as PET or PMI is generally added in the process of preparing the carbon fiber composite material. These methods may reduce the overall mechanical properties of the carbon fiber composite material to some extent.
In order to solve the above two problems, a new sizing agent is urgently needed in the market, on one hand, the bonding property of carbon fiber and resin can be improved; on the other hand, the carbon fiber can have a certain electromagnetic wave absorption capacity, and the carbon fiber composite material further has an electromagnetic shielding capacity.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a sizing agent which can improve the wave absorption of carbon fibers and meet the bonding performance of the carbon fibers.
The specific technical scheme is as follows:
a modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers comprises 0.1-10wt% of modified silicon carbide, 10-20wt% of emulsifier, 40-70wt% of alcohol and 10-40wt% of thermosetting resin;
furthermore, the weight percentage of the modified silicon carbide is 3-8wt%.
Further, the emulsifier is composed of 30-50wt% of sorbitan monostearate, 30-50wt% of polyoxyethylene sorbitan monooleate and 0-30 wt% of sodium dodecyl benzene sulfonate.
Further, the thermosetting resin is any one or more of unsaturated resin, epoxy resin, phenolic resin and urea resin.
Further, the modified silicon carbide is silane coupling agent modified silicon carbide, and the crystal whisker is 500nm-2 um.
A preparation method of modified silicon carbide sizing agent for improving the wave absorption performance of carbon fiber comprises the following steps:
step one, preparing an emulsifier: mixing 30-50wt% of sorbitan monostearate, 30-50wt% of polyoxyethylene sorbitan monooleate and 0-30 wt% of sodium dodecyl benzene sulfonate;
step two, preparing a silicon carbide modifier: 40-70wt% of: 20-40wt%:0.1-20wt% of silane coupling agent, absolute ethyl alcohol and hydrolytic agent are prepared, after the absolute ethyl alcohol and the hydrolytic agent are mixed, the silane coupling agent is added, and after full mixing, the silicon carbide modifier is obtained;
step three, preparing modified silicon carbide: according to the weight percentage of 0.1-10 wt%: preparing 90-99.9wt% of silicon carbide modifier and silicon carbide powder, fully stirring and heating the silicon carbide powder to 110 ℃ in a high-temperature stirrer, preserving heat for 10min, dropwise adding the silicon carbide modifier into the stirrer at 1-2ml/s, after the silicon carbide and the silicon carbide modifier are fully reacted, continuously heating in the stirrer to 135 ℃ at 130 ℃, preserving heat for 20-40min, and preparing modified silicon carbide powder;
step four, mixing the emulsifier, the alcohol and the thermosetting resin which are compounded in the step one according to the weight percentage of 10-20 wt%: 40-70wt%: 10-40wt% of the mixture is put into a vacuum emulsifying machine for mixing, and the mixture is stirred for 50-60min at the stirring speed of 600-1000rpm to prepare a uniform mixed solution;
step five, mixing the modified silicon carbide powder prepared in the step three with the mixed solution prepared in the step four according to the weight percentage of 0.1-10 wt%: 90-99.9wt%, and then placing the mixture into a constant temperature water bath kettle, controlling the temperature at 60-80 ℃, and stirring the mixture for 6-10h at the stirring speed of 400-600rpm to obtain the modified silicon carbide sizing agent with uniform dispersion.
Further, the silane coupling agent in the second step is a silane coupling agent containing vinyl.
In the invention, the silicon carbide has relatively wider forbidden bandwidth, and the impedance of the silicon carbide can be changed along with the adjustable conductivity of the silicon carbide, so that the silicon carbide is a novel wave-absorbing material in the existing electromagnetic shielding field, but the silicon carbide is applied to the carbon fiber, so that the silicon carbide is difficult to combine with the carbon fiber, in addition, the adopted silicon carbide has smaller particle size and is easy to agglomerate, and the carbon fiber can be influenced finally, after the silicon carbide is modified by the silane coupling agent, the dispersibility of the modified silicon carbide on the surface of the fiber is greatly improved, in addition, the surface roughness of the carbon fiber is also improved, the diffusion of the surface defects of the fiber is prevented, the mechanical meshing action of an interface is improved, on the other hand, the nano powder plays a role of steric hindrance, the mutual transmission of heat is effectively isolated, the heat resistance of the fiber is improved, and meanwhile, the water resistance of the sizing agent is improved by the hydrophobic silicon-carbon bond (Si-C-Si), the steric hindrance effect can also effectively enhance the damp-heat resistant strength of the fiber material.
Has the advantages that: (1) excellent wave-absorbing performance: the common carbon fiber does not have wave-absorbing capacity and cannot meet the fixed requirements of space flight and aviation, but the silicon carbide serving as a wide-band-gap semiconductor material can provide excellent wave-absorbing performance; (2) good interfacial compatibility: the carbon fiber coated with the modified silicon carbide sizing agent can be well combined with a resin matrix, so that the surface wettability of the carbon fiber bundle is improved, the chemical bonding of the carbon fiber and the corresponding resin is greatly improved, and the corresponding layer shearing capacity is improved; (3) the simple manufacturing process comprises the following steps: compared with the traditional electromagnetic shielding material which is usually a composite material subjected to high-temperature graphitization or designed with an opposite structure, the silicon carbide nano particle sizing agent can greatly reduce the process difficulty, improve the yield and is more suitable for industrial production; (4) compared with the traditional fiber sizing agent, the modified silicon carbide nanoparticle sizing agent has obvious enhancement in improving the interface effect between resin and fiber or improving the wave-absorbing performance of the fiber, has a simpler production process compared with the traditional carbon fiber electronic shielding composite material, and is suitable for the production of aerospace products with large batch, high repeatability and complex structure.
Drawings
FIG. 1 is an SEM comparison of plates prepared before and after carbon fibers are coated with a modified silicon carbide sizing agent.
Detailed Description
Example 1
A modified sizing agent for improving the wave absorption performance of carbon fibers comprises the following components:
3.6wt% of modified silicon carbide;
12.05wt% of emulsifier;
64.11wt% of alcohol;
20.24wt% of thermosetting resin.
The preparation method of the modified silicon carbide sizing agent comprises the following steps:
step one, preparing an emulsifier: mixing 40wt% of sorbitan monostearate, 40wt% of polyoxyethylene sorbitan monooleate and 20wt% of sodium dodecyl benzene sulfonate;
step two, preparing a silicon carbide modifier: adding 62.5wt% of silane coupling agent into a mixed solution consisting of 28.1 wt% of absolute ethyl alcohol and 9.4wt% of hydrolytic agent to obtain a silicon carbide modifier; the silane coupling agent is a commercially available product, and the specific model is the silane coupling agent M611.
Step three, preparing modified silicon carbide: the silicon carbide and the silicon carbide modifier prepared in the second step are 5wt% in weight percentage: 95wt% preparation, namely, putting the silicon carbide powder into a high-temperature stirrer, fully stirring and heating to 100 ℃, preserving heat for 10min, then dropwise adding the silicon carbide modifier into the stirrer at 1.5ml/s to fully react with the silicon carbide powder, continuously heating to 133 ℃, and preserving heat for 30min to prepare the modified silicon carbide powder.
Step four, mixing the emulsifier, the alcohol and the thermosetting resin which are compounded in the step one according to the weight percentage of 12.5 percent: 66.5 wt%: mixing 21wt% in a vacuum emulsifying machine, and stirring at a certain speed for 56min to obtain a uniform mixed solution;
step five, mixing the modified silicon carbide powder prepared in the step three with the mixed solution prepared in the step four according to the weight percentage of 3.6 percent: 96.4wt% of the raw materials are mixed, and then the mixture is put into a constant-temperature water bath kettle and stirred at medium speed for 8 hours to obtain the modified silicon carbide sizing agent with uniform dispersion.
Example 2
A modified sizing agent for improving the wave absorption performance of carbon fibers comprises the following components:
10wt% of modified silicon carbide;
11.25wt% of emulsifier;
59.85wt% of alcohol;
thermosetting resin, 18.9 wt%.
The preparation method of the modified silicon carbide sizing agent comprises the following steps:
step one, preparing an emulsifier: mixing 40wt% of sorbitan monostearate, 40wt% of polyoxyethylene sorbitan monooleate and 20wt% of sodium dodecyl benzene sulfonate;
step two, preparing a silicon carbide modifier: adding 62.5wt% of silane coupling agent into a mixed solution consisting of 28.1 wt% of absolute ethyl alcohol and 9.4wt% of hydrolytic agent to obtain a silicon carbide modifier; the silane coupling agent is a commercially available product, and the specific model is the silane coupling agent M611.
Step three, preparing modified silicon carbide: the silicon carbide and the silicon carbide modifier prepared in the second step are 5wt% in weight percentage: 95wt% preparation, namely, putting the silicon carbide powder into a high-temperature stirrer, fully stirring and heating to 100 ℃, preserving heat for 10min, then dropwise adding the silicon carbide modifier into the stirrer at 1.5ml/s to fully react with the silicon carbide powder, continuously heating to 133 ℃, and preserving heat for 30min to prepare the modified silicon carbide powder.
Step four, mixing the emulsifier, the alcohol and the thermosetting resin which are compounded in the step one according to the weight percentage of 12.5 percent: 66.5 wt%: mixing 21wt% in a vacuum emulsifying machine, and stirring at a certain speed for 56min to obtain a uniform mixed solution;
step five, mixing the modified silicon carbide powder prepared in the step three with the mixed solution prepared in the step four according to the weight percentage of 10 percent: mixing 90wt%, putting into a constant-temperature water bath kettle, and stirring at medium speed for 8h to obtain the uniformly dispersed modified silicon carbide sizing agent.
Example 3
A modified sizing agent for improving the wave absorption performance of carbon fibers comprises the following components:
3.6wt% of modified silicon carbide;
12.05wt% of emulsifier;
64.11wt% of alcohol;
20.24wt% of thermosetting resin.
The preparation method of the modified silicon carbide sizing agent comprises the following steps:
step one, preparing an emulsifier: mixing 40wt% of sorbitan monostearate, 40wt% of polyoxyethylene sorbitan monooleate and 20wt% of sodium dodecyl benzene sulfonate;
step two, preparing a silicon carbide modifier: adding 20wt% of silane coupling agent into a mixed solution consisting of 70wt% of absolute ethyl alcohol and 10wt% of hydrolytic agent to obtain a silicon carbide modifier; the silane coupling agent is a commercially available product, and the specific model is the silane coupling agent M611.
Step three, preparing modified silicon carbide: the silicon carbide and the silicon carbide modifier prepared in the second step are 5wt% in weight percentage: 95wt% preparation, namely, putting the silicon carbide powder into a high-temperature stirrer, fully stirring and heating to 100 ℃, preserving heat for 10min, then dropwise adding the silicon carbide modifier into the stirrer at 1.5ml/s to fully react with the silicon carbide powder, continuously heating to 133 ℃, and preserving heat for 30min to prepare the modified silicon carbide powder.
Step four, mixing the emulsifier, the alcohol and the thermosetting resin which are compounded in the step one according to the weight percentage of 12.5 percent: 66.5 wt%: mixing 21wt% in a vacuum emulsifying machine, and stirring at a certain speed for 56min to obtain a uniform mixed solution;
step five, mixing the modified silicon carbide powder prepared in the step three with the mixed solution prepared in the step four according to the weight percentage of 3.6 percent: 96.4wt% of the raw materials are mixed, and then the mixture is put into a constant-temperature water bath kettle and stirred at medium speed for 8 hours to obtain the modified silicon carbide sizing agent with uniform dispersion.
Example 4
A modified sizing agent for improving the wave absorption performance of carbon fibers comprises the following components:
3.6wt% of modified silicon carbide;
12.05wt% of emulsifier;
64.11wt% of alcohol;
20.24wt% of thermosetting resin.
The preparation method of the modified silicon carbide sizing agent comprises the following steps:
step one, preparing an emulsifier: mixing 40wt% of sorbitan monostearate, 40wt% of polyoxyethylene sorbitan monooleate and 20wt% of sodium dodecyl benzene sulfonate;
step two, preparing a silicon carbide modifier: adding 62.5wt% of silane coupling agent into a mixed solution consisting of 28.1 wt% of absolute ethyl alcohol and 9.4wt% of hydrolytic agent to obtain a silicon carbide modifier; the silane coupling agent is a commercially available product, and the specific model is the silane coupling agent M611.
Step three, preparing modified silicon carbide: 1wt% of silicon carbide and the silicon carbide modifier prepared in the second step: 99wt% preparation, namely, putting the silicon carbide powder into a high-temperature stirrer, fully stirring and heating to 110 ℃, preserving heat for 5min, dropwise adding a silicon carbide modifier into the stirrer at 2ml/s to fully react with the silicon carbide powder, continuously heating to 130 ℃, and preserving heat for 50min to obtain the modified silicon carbide powder.
Step four, mixing the emulsifier, the alcohol and the thermosetting resin which are compounded in the step one according to the weight percentage of 12.5 percent: 66.5 wt%: mixing 21wt% in a vacuum emulsifying machine, and stirring at a certain speed for 56min to obtain a uniform mixed solution;
step five, mixing the modified silicon carbide powder prepared in the step three with the mixed solution prepared in the step four according to the weight percentage of 3.6 percent: 96.4wt% of the raw materials are mixed, and then the mixture is put into a constant-temperature water bath kettle and stirred at medium speed for 8 hours to obtain the modified silicon carbide sizing agent with uniform dispersion.
Example 5
A modified sizing agent for improving the wave absorption performance of carbon fibers comprises the following components:
3.6wt% of modified silicon carbide;
emulsifier, 14.46 wt%;
57.84wt% of alcohol;
thermosetting resin, 24.1 wt%.
The preparation method of the modified silicon carbide sizing agent comprises the following steps:
step one, preparing an emulsifier: mixing 40wt% of sorbitan monostearate, 40wt% of polyoxyethylene sorbitan monooleate and 20wt% of sodium dodecyl benzene sulfonate;
step two, preparing a silicon carbide modifier: adding 62.5wt% of silane coupling agent into a mixed solution consisting of 28.1 wt% of absolute ethyl alcohol and 9.4wt% of hydrolytic agent to obtain a silicon carbide modifier; the silane coupling agent is a commercially available product, and the specific model is the silane coupling agent M611.
Step three, preparing modified silicon carbide: the silicon carbide and the silicon carbide modifier prepared in the second step are 5wt% in weight percentage: 95wt% preparation, namely, putting the silicon carbide powder into a high-temperature stirrer, fully stirring and heating to 100 ℃, preserving heat for 10min, then dropwise adding the silicon carbide modifier into the stirrer at 1.5ml/s to fully react with the silicon carbide powder, continuously heating to 133 ℃, and preserving heat for 30min to prepare the modified silicon carbide powder.
Step four, mixing the emulsifier, the alcohol and the thermosetting resin which are compounded in the step one in a weight percentage of 18 percent: 68 wt%: putting 17wt% of the mixture into a vacuum emulsifying machine for mixing, and stirring for 80min at a certain speed to prepare a uniform mixed solution;
step five, the modified silicon carbide powder prepared in the step three and the mixed solution prepared in the step four are 3.6wt% in percentage by weight: 96.4wt% of the raw materials are mixed, and then the mixture is put into a constant-temperature water bath kettle and stirred at medium speed for 8 hours to obtain the modified silicon carbide sizing agent with uniform dispersion.
The modified silicon carbide sizing agent prepared according to example 1 is coated on carbon fibers according to a conventional sizing agent, and an SEM image of a prepared carbon fiber plate is shown in an attached figure 1 (b). SEM images of plates prepared from carbon fibers not coated with modified silicon carbide sizing agent are shown in the attached figure 1 (a), and comparison shows that: (a) in the figure, the surface of the carbon fiber dry filament in the plate is smoother, and no other substances except the fixed fiber bundle exist; (b) in the figure, a large number of SiC particles are uniformly distributed on the surface of carbon fiber filaments in the composite board, and the SiC sizing agent prepared by the invention on the surface has better bonding property with carbon fibers.
Claims (10)
1. The modified silicon carbide sizing agent for improving the wave absorption performance of the carbon fiber is characterized by comprising modified silicon carbide, an emulsifier, alcohol and thermosetting resin, wherein the weight percentage of the modified silicon carbide, the emulsifier, the alcohol and the thermosetting resin is 0.1-10 wt%: 10-20 wt%: 40-70wt%: 10-40 wt%.
2. The modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers according to claim 1, wherein the weight percentage of the modified silicon carbide, the emulsifier, the alcohol and the thermosetting resin is 3-8 wt%: 10-20 wt%: 40-70wt%: 10-40 wt%.
3. The modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers according to claim 1, wherein the modified silicon carbide is silane coupling agent modified silicon carbide, and the whiskers of the modified silicon carbide are between 500nm and 2 um.
4. The modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers according to claim 1, wherein the emulsifier is prepared from 30-50 wt%: 30-50 wt%: 0-30 wt% of sorbitan monostearate, polyoxyethylene sorbitan monooleate and sodium dodecyl benzene sulfonate.
5. The modified silicon carbide sizing agent for improving the wave absorption performance of carbon fibers according to claim 1, wherein the thermosetting resin is any one or more of unsaturated resin, epoxy resin, phenolic resin and urea resin.
6. The preparation method of the modified silicon carbide sizing agent for improving the wave absorption performance of the carbon fiber according to any one of claims 1 to 5, characterized by comprising the following steps:
step one, preparing an emulsifier: 30-50wt% of sorbitan monostearate, polyoxyethylene sorbitan monooleate and sodium dodecyl benzene sulfonate: 30-50 wt%: 0-30 wt% to obtain an emulsifier;
step two, preparing a silicon carbide modifier: preparing a silane coupling agent, absolute ethyl alcohol and a hydrolytic agent according to the weight percentage of 40-70wt% to 20-40wt% to 0.1-20wt%, fully mixing the absolute ethyl alcohol and the hydrolytic agent, then adding the silane coupling agent, and fully mixing to obtain a silicon carbide modifier;
step three, preparing modified silicon carbide: the silicon carbide modifier prepared in the second step and the silicon carbide are 0.1-10wt% in percentage by weight: 90-99.9wt% preparation, namely, putting the silicon carbide powder into a high-temperature stirrer, fully stirring and heating to 110 ℃ for 100-;
step four, mixing the emulsifier compounded in the step one with alcohol and thermosetting resin according to the weight percentage of 10-20 wt%: 40-70wt%: 10-40wt% of the mixture is put into a vacuum emulsifying machine and stirred for 50-60min at a certain stirring speed to prepare a uniform mixed solution;
step five, mixing the modified silicon carbide powder obtained in the step three with the mixed solution prepared in the step four according to the weight percentage of 0.1-10: 90-99.9wt%, then putting into a constant temperature water bath kettle for heat preservation and stirring at low speed for 6-10h to obtain the modified silicon carbide sizing agent with uniform dispersion.
7. The method according to claim 6, wherein the silane coupling agent in the second step is a silane coupling agent containing a vinyl group, and the hydrolyzing agent is glacial acetic acid.
8. The method according to claim 6, wherein the thermosetting resin in the fourth step is any one or more of unsaturated resin, epoxy resin, phenolic resin and urea resin.
9. The method according to claim 6, wherein the stirring speed in the fourth step is 600-1000 rpm.
10. The method according to claim 6, wherein the temperature in step five is 60-80 ℃, and the stirring speed is 400-600 rpm.
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| JP2008258253A (en) * | 2007-04-02 | 2008-10-23 | Technes Co Ltd | Material excellent in electromagnetic wave shielding property and heat dissipation and molded good |
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