CN103924443A - Preparation method of carbon fiber surface antioxidation coating - Google Patents
Preparation method of carbon fiber surface antioxidation coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon fiber surface antioxidation coating, which belongs to the technical field of inorganic non-metallic material. The preparation method comprises the following steps: using an organic solvent to remove a glue layer and an attachment on the surface of the carbon fiber, taking a silane coupling agent as a precursor to prepare a coating slurry; coating the obtained coating slurry on the surface of the carbon fiber product and drying; in 99.999% of inert atmosphere, and processing the dried carbon fiber product under high temperature of 800-1600 DEG C for 30-360 minutes to obtain the carbon fiber surface antioxidation coating. According to the invention, the silane coupling agent is taken as a precursor, and is easily infiltrated with carbon fiber to form an uniform coating, the enhanced particles can improve the defects of poor clunging of the coating and cracking of the coating; the solidification time is short, the solidification temperature is low, and automation mechanical equipment is cooperated for easily realizing the continuous coating of the coating.
Description
Technical field
The present invention relates to a kind of preparation method of carbon fiber surface ORC, the preparation method of especially a kind of technique carbon fiber surface ORC simple, with low cost, belongs to technical field of inorganic nonmetallic materials.
Background technology
Carbon fibre reinforced ceramics or carbon fiber reinforced carbon matrix composite material have the feature of high specific stiffness, specific strength, and have good high-temperature behavior, in inert environments, exceeding 2000 DEG C still can keep the mechanical properties such as intensity not reduce, having good fracture toughness and ABRASION RESISTANCE, is very potential high-temperature structural material in the industries such as military affairs, the energy and communications and transportation.But the oxidation resistance of carbon fiber is poor, in oxidizing atmosphere, will be oxidized higher than 400 DEG C of carbon fibers, cause material property to reduce even and lost efficacy.In addition, because carbon fiber surface activity is lower, poor without processing with the adhesion of matrix, also can reduce the performance of composite.
Prepare ORC at carbon fiber surface and can effectively solve carbon fiber problem of oxidation.In addition, select suitable coating can also play the object of fiber surface modification, the adhesion of fortifying fibre and matrix material.At present, method for preparing antioxidant coating can be divided into four classes substantially: (1), based on chemical vapour deposition (CVD) principle at carbon fiber surface deposited coatings.On August 14th, 2013, Chinese invention patent CN102505101B discloses a kind of carbon fiber surface C/Si composite coating and preparation method thereof, adopts SiCl
4and CH
4as raw material, Ar is as protective gas and current-carrying gas, H
2as reducibility gas, use the preparation of negative pressure chemical vapour deposition technique, making pyrocarbon coating and Si is external coating; On May 24th, 2006, Chinese invention patent CN1257308C discloses a kind of preparation method of corundum-mullite complex phase ceramic coating, adopt certain precursor gassy system to prepare γ-Al2O3 by rpcvd method at the temperature of 450 DEG C-650 DEG C and check oxide coating in conjunction with unformed SiO2, then can obtain coating 1250 DEG C of left and right heat treatments.Said method needs special gaseous phase deposition stove, consersion unit costliness, and in course of reaction, can produce environment harmful gas as hydrogen chloride etc.(2), reaction in-situ generates coating.On July 25th, 2007, Chinese invention patent application CN 200610151216.3 discloses a kind of method of preparing coat of silicon carbide at carbon fiber surface, first raw material is packed in vacuum sphere grinding jar, makes mixed powder; Then prepare slurry; Final drying is processed and sintering, obtains surface and have the carbon fibre of coat of silicon carbide.These class methods need highly purified nanometer silicon carbide powder and carbon dust, raw material costliness, and complex technical process, and coating quality influence factor is many, is difficult to control the quality of coating.(3), electrophoresis.On April 17th, 2013, Chinese invention patent CN102220621B discloses a kind of method of carrying out coat of silicon carbide at carbon fiber surface, first prepare carborundum electrophoresis liquid, then in tiselius apparatus, fix graphite-pipe and carbon fiber is installed, secondly connect power supply and carry out carborundum electrophoretic deposition, finally carry out forced air drying and obtain the finished product carbon fiber of coating silicon carbide coating.The method need to be carried out surface modification to silicon-carbide particle, makes its grafting polar group.The method of modification normally adopts strong acid treatment, but also need in electrophoresis liquid, add charge adjuvant.The introducing of strong acid treatment and charge adjuvant has been introduced plurality of impurities at carbon fiber surface undoubtedly, is unfavorable for carbon-fiber high-temperature environment stability inferior.(4), presoma cracking process.On April 17th, 2013, Chinese invention patent application CN103046315A discloses the preparation method of the full carbon coating of a kind of carbon fiber surface, adopts phenolic resins to produce the method for pyrocarbon coating at carbon fiber surface as presoma.First this technology carries out acidification to carbon fiber surface, then applies phenolic resins, by solidifying and high temperature cabonization technique acquisition pyrocarbon coating; Thesis for the doctorate " carbon fiber is prepared the micromechanism of damage research in ceramic matric composite process in PIP technique " (author: Wang Jianfang, PLA University of Science and Technology for National Defense, 2003) introduce the method that adopts the toluene solution that applies Polycarbosilane at fiber surface to prepare coat of silicon carbide, come unstuck carbon fiber (400 DEG C, N in tube furnace
2protection) remove surperficial epoxy resin, then ultrasonic immersing coating solution, cracking in high temperature sintering furnace again after being dried, being cross-linked (1100 DEG C, Ar protection), can obtain coated fiber.In the method, between carbon fiber and presoma, do not have chemical bond to be connected, presoma is not easy to infiltrate and form uniform coating with carbon fiber.Document " Carbothermal Synthesis of Boron Nitride Coating o n PAN Carbon Fiber " ([J] Journal o f the European Ceramic Society, 2009,29:2129-2134.) introduce employing nitric acid PAN carbon fiber has been carried out to preliminary treatment, prepare boron nitride pellicle by infusion process.Boric acid is formed to boron nitride pellicle 1 200 DEG C of nitrogen nitrogenize.Reaction mechanism is original position carbothermic reduction reaction, and coating comprises carbon, fibre strength 15% left and right that declined.Document " preparation of carbon fiber surface boron nitride coating " ([J] sufacing,, the 40th volume in 2011, the fourth phase, 1-7 page) taking boric acid as raw material, by the dip-coating of carbon fiber process precursor solution, heat treatment again, has prepared the boron nitride pellicle coating of continuous uniform at carbon fiber surface.The method that " Carbothermal Synthesis of Boron Nitride Coating o n PAN Carbon Fiber " and " preparation method of the full carbon coating of carbon fiber surface " introduces need to be carried out acidification to carbon fiber, can reduce the mechanical property of carbon fiber." Formation of BN Films on Carbon Fibers by Dip-coating " ([J] Surface and Coating Technology, 2002,150:269-276.) adopt the methanol solution infusion process of boric acid and urea, under 1000 DEG C of ammonia nitrogen treatment, successfully on carbon fiber, prepare turbine stratiform BN coating.The method show that coating is inhomogeneous, and treatment temperature is high, Exhaust Gas contaminated air.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned defect, and the preparation method of the carbon fiber surface ORC that a kind of technique is simple, with low cost, coating adhesion is good is provided.
In order to solve the problems of the technologies described above, the invention provides a kind of carbon fiber surface method for preparing antioxidant coating, comprise the following steps:
1), utilize organic solvent to remove glue-line and other attached crops on carbon fiber product surface;
2), by weight 1-2 part silane coupler is joined in 95-100 part water-alcohol solvent and forms mixed solution, add again glacial acetic acid that the pH value of mixed solution is adjusted to 0.1-0.3, stir and within 50-80 minute, form coupling agent solution, then in coupling agent solution, add 4-6 part to strengthen particle, stir again 50-80 minute, obtain coating paste;
3), by step 2) coating paste that obtains is coated on carbon fiber product surface;
4), by step 3) carbon fiber product that applied coating paste is dried, coating paste solidified under 20-150 DEG C of condition;
5), by step 4) carbon fiber product after coating paste solidifies inserts in 99.999% inert atmosphere, under temperature 800-1600 DEG C condition after high-temperature process 30-360 minute, obtain carbon fiber surface ORC.
In the present invention, step 1) described in organic solvent be acetone, ethanol or chloroform.
In the present invention, step 1) glue-line and other the attached crops that adopt soxhlet extraction to remove carbon fiber surface.
In the present invention, step 2) described in silane coupler be silane coupling A 151, silane coupler K570 or silane coupler K550.
In the present invention, step 2) described in water-alcohol solvent mixed by the ethanol of 75-95wt% and the isopropyl alcohol of 5-25wt% distilled water or 75-95wt% and 5-25wt% distilled water.
In the present invention, step 2) described in to strengthen particle be silicon carbide powder, powdered graphite or boron nitride powder.
In the present invention, described carbon fiber product is carbon fiber bundle, carbon cloth and three-dimensional carbon fiber preform.
Beneficial effect of the present invention is: (1), the present invention are using silane coupler as presoma, the hydroxyl forming after silane coupler hydrolysis not only with carbon fiber surface hydroxyl reaction, form firm chemical bond, also can there is polycondensation reaction in the hydroxyl between coupling agent molecule simultaneously, form linear polymeric material, easy and carbon fiber infiltrates and forms uniform coating; Strengthen particle can to have improved coating adhesion poor and overcome coating cracking and peel off defect simultaneously; (2), using silane coupler as presoma, its hardening time is short, solidification temperature is low, coordinates automated machine equipment, easily realizes the continuous coating of coating; (3), technique of the present invention is simple, raw material are easy to obtain, and easily realize.
Brief description of the drawings
Fig. 1 is carbon fiber surface method for preparing antioxidant coating process chart of the present invention;
Fig. 2 is the structural representation of the embodiment of the present invention 1 coating unit used;
Number in the figure title: 1-take-up pulley, 2-heating furnace, 3-derives wheel, 4-impregnating bath, 5-first is to Kun, 6-carbon fiber bundle, 7-second is to Kun, and 8-imports wheel, 9-actinobacillus wheel.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
embodiment 1
The first step, adopts acetone as solvent, by soxhlet extraction Treatment of Carbon, removes glue-line and other attached crops on carbon fiber bundle 6 surfaces;
Second step, get by weight 1 part of silane coupling A 151 as presoma, join in 98 parts of water-alcohol solutions that formed by 75wt% ethanol and 25wt% distilled water and form mixed solution, add again glacial acetic acid that the ph value of mixed solution is adjusted to 0.1-0.3, fully stir 60 minutes, then add 5 parts of silicon carbide powders as strengthening particle, fully stir 60 minutes, form coating paste;
The 3rd step, coating paste is injected to impregnating bath 4, by the carbon fiber bundle 6 except after glue from being arranged on the actinobacillus wheel 9 of impregnating bath 4 tops, successively through importing wheel 8 and being arranged on second couple of Kun in impregnating bath 47, first couple of Kun 5, take turns 3 through the derivation of impregnating bath 4 tops again, carbon fiber bundle 6 is entered from heating furnace 2 one end, pass from the other end of heating furnace 2, finally carbon fiber bundle 6 front ends are fixed on take-up pulley 1.Simultaneously, in impregnating bath 4, put into agitating device, then switch on power, start traction motor and heating furnace 2, keeping heating-up temperature is 100 DEG C, makes the speed of carbon fiber bundle 6 with 0.001m/s, first in impregnating bath, flood, then in heating furnace, be heating and curing, take-up pulley obtains the carbon fiber bundle semi-finished product that apply cure pastes, as shown in Figure 2;
The 4th step, is woven into precast body by carbon fiber bundle as required, by precast body under 99.999% inert atmosphere 1000 DEG C process 60 minutes, can obtain carbon fiber bundle surface oxidation-resistant coating.
embodiment 2
The first step, adopts ethanol as solvent, by soxhlet extraction Treatment of Carbon cloth, removes glue-line and other attached crops on carbon cloth surface;
Second step, get 2 parts of silane coupler K570 as presoma, join in 100 parts of water-alcohol solutions that formed by 95wt% ethanol and 5wt% distilled water and form mixed solution, add again glacial acetic acid that the ph value of mixed solution is adjusted to 0.1-0.3, fully stir 80 minutes, then add 4 parts of boron nitride powders as strengthening particle, fully stir 80 minutes, form coating paste;
The 3rd step, injects impregnating bath coating paste, will put into impregnating bath except the carbon cloth after glue, and then ultrasonic processing 30 minutes, fully immerses in carbon cloth slurry; Take out, erase gently unnecessary maceration extract on carbon cloth surface with glass bar, then in heating furnace 150 DEG C be dried 30 minutes;
The 4th step, finally by carbon cloth under 99.999% inert atmosphere 800 DEG C process 360 minutes, can obtain carbon cloth surface oxidation-resistant coating.
embodiment 3
The first step, adopts chloroform as solvent, processes 3 D weaving carbon fiber precast body by soxhlet extraction, removes glue-line and other attached crops on 3 D weaving carbon fiber precast body surface;
Second step, gets 2 parts of silane coupler K550 as presoma, joins in 95 parts of water-alcohol solutions that are made up of 95wt% isopropyl alcohol and 5wt% distilled water and forms mixed solution, fully stir 50 minutes, then add 6 parts of silicon carbide powders as strengthening particle, then stir 50 minutes, form coating paste;
The 3rd step, injects impregnating bath coating paste, will put into impregnating bath except the 3 D weaving carbon fiber precast body after glue, and then ultrasonic processing 30 minutes, fully immerses in 3 D weaving carbon fiber precast body slurry; Take out, after draining in heating furnace 150 degrees Celsius dry 30 minutes;
The 4th step, finally by carbon cloth under 99.999% inert atmosphere 1600 DEG C process 200 minutes, can obtain carbon fiber bundle surface oxidation-resistant coating.
embodiment 4
The first step, adopts acetone as solvent, by soxhlet extraction Treatment of Carbon cloth, removes glue-line and other attached crops on carbon cloth surface;
Second step, get 1 part of silane coupler K570 as presoma, join in 99 parts of water-alcohol solutions that formed by 85wt% ethanol and 15wt% distilled water and form mixed solution, add again glacial acetic acid that the ph value of mixed solution is adjusted to 0.1-0.3, fully stir 70 minutes, then add 6 parts of silicon carbide powders as strengthening particle, fully stir 70 minutes, form coating paste;
The 3rd step, injects impregnating bath coating paste, will put into impregnating bath except the carbon cloth after glue, and then ultrasonic processing 30 minutes, fully immerses in carbon cloth slurry; Take out, erase gently unnecessary maceration extract with glass bar on carbon cloth surface, then under 20 DEG C of environment, be dried 150 minutes;
The 4th step, finally by carbon cloth under 99.999% inert atmosphere 800 DEG C process 360 minutes, can obtain carbon cloth surface oxidation-resistant coating.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, can also make under the premise without departing from the principles of the invention some improvement, and these improve and also should be considered as protection scope of the present invention.
Claims (7)
1. a carbon fiber surface method for preparing antioxidant coating, is characterized in that comprising the following steps:
1), utilize organic solvent to remove glue-line and other attached crops on carbon fiber product surface;
2), by weight 1-2 part silane coupler is joined in 95-100 part water-alcohol solvent and forms mixed solution, add again glacial acetic acid that the pH value of mixed solution is adjusted to 0.1-0.3, stir and within 50-80 minute, form coupling agent solution, then in coupling agent solution, add 4-6 part to strengthen particle, stir again 50-80 minute, obtain coating paste;
3), by step 2) coating paste that obtains is coated on carbon fiber product surface;
4), by step 3) carbon fiber product that applied coating paste is dried, coating paste solidified under 20-150 DEG C of condition;
5), by step 4) carbon fiber product after coating paste solidifies inserts in 99.999% inert atmosphere, under temperature 800-1600 DEG C condition after high-temperature process 30-360 minute, obtain carbon fiber surface ORC.
2. carbon fiber surface method for preparing antioxidant coating according to claim 1, is characterized in that: step 1) described in organic solvent be acetone, ethanol or chloroform.
3. carbon fiber surface method for preparing antioxidant coating according to claim 1 and 2, is characterized in that: step 1) adopt soxhlet extraction glue-line and other attached crops of removing carbon fiber surface.
4. carbon fiber surface method for preparing antioxidant coating according to claim 3, is characterized in that: step 2) described in silane coupler be silane coupling A 151, silane coupler K570 or silane coupler K550.
5. carbon fiber surface method for preparing antioxidant coating according to claim 4, is characterized in that: step 2) described in water-alcohol solvent mixed by the ethanol of 75-95wt% and the isopropyl alcohol of 5-25wt% distilled water or 75-95wt% and 5-25wt% distilled water.
6. carbon fiber surface method for preparing antioxidant coating according to claim 5, is characterized in that: step 2) described in to strengthen particle be silicon carbide powder, powdered graphite or boron nitride powder.
7. carbon fiber surface method for preparing antioxidant coating according to claim 6, is characterized in that: described carbon fiber product is carbon fiber bundle, carbon cloth and three-dimensional carbon fiber preform.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532551A (en) * | 2014-12-12 | 2015-04-22 | 哈尔滨工业大学 | Method for in-situ preparing silicon-boron-carbon-nitrogen ceramic coating on surface of carbon fiber |
| CN105948821A (en) * | 2016-04-27 | 2016-09-21 | 航天材料及工艺研究所 | Lightweight carbon fiber thermal insulation material surface pore-sealing method |
| CN107880494A (en) * | 2016-09-30 | 2018-04-06 | 比亚迪股份有限公司 | A kind of carbon fibre initial rinse fabric and preparation method thereof and metal fiber composite |
| CN108238799A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院上海应用物理研究所 | A kind of preparation method of silicon-containing ceramic coating |
| CN108950739A (en) * | 2017-12-29 | 2018-12-07 | 海南梵思科技有限公司 | A kind of preparation method of carbon fiber and high-temperature nylon composite material containing it |
| CN109824380A (en) * | 2019-03-28 | 2019-05-31 | 山东众途复合材料有限公司 | A kind of preparation method of the carbon fiber thermal insulating material coated with anti-oxidant shock resistance coating |
| CN110820323A (en) * | 2019-10-31 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of Si-C-O ceramic antioxidant coating on surface of carbon fiber |
| CN113185856A (en) * | 2021-04-25 | 2021-07-30 | 仲恺农业工程学院 | Preparation method and application of coating material for oil sludge cracking treatment |
| CN113897784A (en) * | 2021-11-11 | 2022-01-07 | 江苏瑞洋安泰新材料科技有限公司 | Washable environment-friendly stiffening agent and preparation method thereof |
| CN114717491A (en) * | 2022-04-29 | 2022-07-08 | 中国科学院合肥物质科学研究院 | High-toughness Wf/W composite material and preparation method thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104532551A (en) * | 2014-12-12 | 2015-04-22 | 哈尔滨工业大学 | Method for in-situ preparing silicon-boron-carbon-nitrogen ceramic coating on surface of carbon fiber |
| CN105948821A (en) * | 2016-04-27 | 2016-09-21 | 航天材料及工艺研究所 | Lightweight carbon fiber thermal insulation material surface pore-sealing method |
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| CN107880494A (en) * | 2016-09-30 | 2018-04-06 | 比亚迪股份有限公司 | A kind of carbon fibre initial rinse fabric and preparation method thereof and metal fiber composite |
| CN108238799A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院上海应用物理研究所 | A kind of preparation method of silicon-containing ceramic coating |
| CN108950739A (en) * | 2017-12-29 | 2018-12-07 | 海南梵思科技有限公司 | A kind of preparation method of carbon fiber and high-temperature nylon composite material containing it |
| CN108950739B (en) * | 2017-12-29 | 2021-09-14 | 海南梵思科技有限公司 | Preparation method of carbon fiber and high-temperature nylon composite material containing carbon fiber |
| CN109824380A (en) * | 2019-03-28 | 2019-05-31 | 山东众途复合材料有限公司 | A kind of preparation method of the carbon fiber thermal insulating material coated with anti-oxidant shock resistance coating |
| CN109824380B (en) * | 2019-03-28 | 2021-09-14 | 山东众途复合材料有限公司 | Preparation method of carbon fiber thermal insulation material coated with antioxidant impact-resistant coating |
| CN110820323B (en) * | 2019-10-31 | 2022-08-09 | 哈尔滨工业大学 | Preparation method of Si-C-O ceramic antioxidant coating on surface of carbon fiber |
| CN110820323A (en) * | 2019-10-31 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of Si-C-O ceramic antioxidant coating on surface of carbon fiber |
| CN113185856A (en) * | 2021-04-25 | 2021-07-30 | 仲恺农业工程学院 | Preparation method and application of coating material for oil sludge cracking treatment |
| CN113185856B (en) * | 2021-04-25 | 2024-04-09 | 仲恺农业工程学院 | Preparation method and application of coating material for oil sludge cracking treatment |
| CN113897784A (en) * | 2021-11-11 | 2022-01-07 | 江苏瑞洋安泰新材料科技有限公司 | Washable environment-friendly stiffening agent and preparation method thereof |
| CN114717491A (en) * | 2022-04-29 | 2022-07-08 | 中国科学院合肥物质科学研究院 | High-toughness Wf/W composite material and preparation method thereof |
| CN114717491B (en) * | 2022-04-29 | 2022-12-02 | 中国科学院合肥物质科学研究院 | High-toughness W f /W composite material and preparation method thereof |
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