CN103243548A - Preparation method of high-temperature-resistant SiBN(C) carbon fiber coating - Google Patents
Preparation method of high-temperature-resistant SiBN(C) carbon fiber coating Download PDFInfo
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- CN103243548A CN103243548A CN2013101936777A CN201310193677A CN103243548A CN 103243548 A CN103243548 A CN 103243548A CN 2013101936777 A CN2013101936777 A CN 2013101936777A CN 201310193677 A CN201310193677 A CN 201310193677A CN 103243548 A CN103243548 A CN 103243548A
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Abstract
The invention relates to a preparation method of high-temperature-resistant SiBN(C) carbon fiber coating. The preparation method comprises the following steps of: (1) preparing polyborosilazane anhydrous toluene solution; (2) performing glue-removing treatment on the carbon fiber at 100 to 600 DEG C and soaking the carbon fiber into 40 to 70 percent nitric acid to obtain the treated carbon fiber; (3) under the protection of nitrogen, soaking the treated carbon fiber into the polyborosilazane anhydrous toluene solution for 0.1 to 5 hours and standing; and (4) under the atmosphere of nitrogen flow, crosslinking the soaked carbon fiber obtained in the step (3), heating to 1,000 to 1,600 DEG C at the rate of 0.05 to 5 DEG C/min, cracking and cooling to obtain the high-temperature-resistant SiBN(C) carbon fiber coating. The preparation method is simple and has strong actionability; and the surface of the obtained SiBN(C) carbon fiber coating is uniform and compact, the original mechanical property of the carbon fiber is maintained, and the high-temperature oxidation resistance is improved.
Description
Technical field
The invention belongs to the preparation field of modified carbon fiber, particularly a kind of high temperature resistant SiBN(C) preparation method of carbon fiber coating.
Background technology
Since the sixties in this century come out as commodity, carbon fiber (hereinafter to be referred as CF) is with its high specific strength, specific modulus, good heat conduction, electric conductivity and the good thermal stability in inert atmosphere, to the stiff stability that acid, alkalization learn to be corroded, cause people's extensive concern and be applied to many fields of high-tech sector such as Aeronautics and Astronautics and civilian industry rapidly.
But the high-temperature oxidation resistance of carbon fiber is poor, will begin to descend in the mechanical property of 450 ℃ of following carbon fibers, and this shortcoming has limited the application of carbon fiber under extreme environment greatly.In order to overcome this shortcoming, need carry out stabilization processes to carbon fiber, improve its heat endurance and high-temperature oxidation resistance.At present, the maximum of research are to apply one deck exotic material at carbon fiber surface, play the effect of starvation, strengthen its resistance to elevated temperatures.
The technology of preparing of carbon fiber coating will cause very big influence to the performance of final material.On the one hand coating evenly, is closely sticked on the carbon fiber, to reach the effect of starvation; The form that will make the fracture mechanism of material come unstuck, extract based on fiber on the other hand so just can not make the material fragility fracture.
Summary of the invention
Technical problem to be solved by this invention provides a kind of high temperature resistant SiBN(C) preparation method of carbon fiber coating, this method technology is simple, and exploitativeness is strong, the SiBN(C of the carbon fiber surface that obtains) the coating even compact, no microcrack, high-temperature oxidation resistance and mechanical property excellence.
A kind of high temperature resistant SiBN(C of the present invention) preparation method of carbon fiber coating comprises:
(1) under nitrogen atmosphere, disposes the poly-borosilicate azane anhydrous toluene solution of SiBN (C) presoma;
(2) under the nitrogen protection, the 100-600 ℃ of processing of removing photoresist, the time is 1-6 hour with carbon fiber, placing concentration then is that the nitric acid of 40-70% soaked 0.1-5 hour, it is carried out surface treatment, and remove impurity, clean oven dry, the carbon fiber after obtaining handling again;
(3) under the nitrogen protection, the carbon fiber after the above-mentioned processing with poly-borosilicate azane anhydrous toluene solution dipping 0.1-5 hour, is left standstill after dipping is good to toluene and volatilizees;
(4) under the nitrogen stream atmosphere, the carbon fiber behind the dipping that step (3) is obtained is warmed up to 50-400 ℃ with the speed of 0.02-2 ℃/min and carries out crosslinkedly earlier, is incubated 10-30 hour; And then be warming up to 1000-1600 ℃ with the speed of 0.05-5 ℃/min and carry out cracking, be incubated 1-6 hour; Speed with 0.05-5 ℃/min drops to 100-600 ℃ at last, namely obtains SiBN(C) the carbon fiber coating.
The mass concentration of the poly-borosilicate azane anhydrous toluene solution described in the step (1) is 0.01-20%.
Clean employing described in the step (2) be deionized water.
Operation described in the step (3) is to finish in being full of the glove box of pure nitrogen gas.
The mass fraction of SiBN (C) is 40-70% in the resulting SiBN of step (4) (C) the carbon fiber coating.
The heat resisting temperature of the resulting SiBN of step (4) (C) carbon fiber coating in oxidizing atmosphere is 400-800 ℃.
SiBN(C) have high strength, high-modulus, excellent properties such as high temperature resistant and anti-oxidant, and the thermal coefficient of expansion of SiBN (C) and carbon fiber is close, can well be coated in carbon fiber surface, play the effect of starvation, thereby strengthen the heat-resisting ability of carbon fiber greatly, satisfy the application requirements of high-tech sectors such as Aero-Space.
Beneficial effect:
(1) preparation method's operation of the present invention, no especial equipment requirements, exploitativeness is strong;
(2) the SiBNC coating even compact of the carbon fiber surface that obtains of the present invention is non-microcracked, high-temperature oxidation resistance and mechanical property excellence.
Description of drawings
Fig. 1 is the carbon fiber SEM figure of not coating;
Fig. 2 is SiBN(C) SEM of coat carbon fiber figure.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1:
The preparation mass fraction is 0.01% poly-borosilicate azane anhydrous toluene solution; Under the nitrogen atmosphere, it is to remove photoresist in 100 ℃ the tube furnace to handle 1 hour that carbon fiber is put into temperature; Be to take out behind the nitric acid dousing 0.1h of 40-70% with concentration then, clean and dry with deionized water.Under the nitrogen atmosphere, pretreated carbon fiber is put into dipping forwarded in the tube furnace after 0.1 hour in 0.01% the poly-borosilicate azane anhydrous toluene solution that configures.Flow down at nitrogen, be warming up to 100 ℃ with the speed of 0.02 ℃/min, make carbon fiber carry out polymerization crosslinking, be incubated 2 hours; Then be warming up to 1000 ℃ with the speed of 0.05/min and carry out cracking, be incubated that the speed with 0.05 ℃/min is cooled to 600 ℃ after 2 hours, obtain SiBN (C) carbon fiber.Heat resisting temperature under its oxidizing atmosphere is 600 ℃, coating even compact, no microcrack.
Embodiment 2:
The preparation mass fraction is 10% poly-borosilicate azane anhydrous toluene solution; Under the nitrogen atmosphere, it is to remove photoresist in 300 ℃ the tube furnace to handle 3 hours that carbon fiber is put into temperature; Be to take out behind the nitric acid dousing 0.5h of 40-70% with concentration then, clean and dry with deionized water.Under the nitrogen atmosphere, pretreated carbon fiber is put into dipping forwarded in the tube furnace after 0.5 hour in 10% the poly-borosilicate azane anhydrous toluene solution that configures.Flow down at nitrogen, be warming up to 200 ℃ with the speed of 0.2 ℃/min, make carbon fiber carry out polymerization crosslinking, be incubated 4 hours, then be warming up to 1300 ℃ with the speed of 0.5/min and carry out cracking, be incubated that the speed with 3 ℃/min is cooled to 400 ℃ after 4 hours, obtain SiBN (C) carbon fiber.Heat resisting temperature under its oxidizing atmosphere is 700 ℃, coating even compact, no microcrack.
Embodiment 3:
The preparation mass fraction is 20% poly-borosilicate azane anhydrous toluene solution.Under the nitrogen atmosphere, it is to remove photoresist in 600 ℃ the tube furnace to handle 6 hours that carbon fiber is put into temperature; Be to take out behind the nitric acid dousing 5h of 40-70% with concentration then, clean and dry with deionized water.Under the nitrogen atmosphere, pretreated carbon fiber is put into dipping forwarded in the tube furnace after 5 hours in 20% the poly-borosilicate azane anhydrous toluene solution that configures.Flow down at nitrogen, be warming up to 400 ℃ with the speed of 2 ℃/min, make carbon fiber carry out polymerization crosslinking, be incubated 6 hours; Then be warming up to 1000 ℃ with the speed of 5/min and carry out cracking, be incubated that the speed with 5 ℃/min is cooled to 200 ℃ after 6 hours, obtain SiBN (C) carbon fiber.Heat resisting temperature under its oxidizing atmosphere is 800 ℃, coating even compact, no microcrack.
Claims (6)
1. the preparation method of carbon fiber coating high temperature resistant SiBN(C) comprises:
(1) the poly-borosilicate azane anhydrous toluene solution of configuration under nitrogen atmosphere;
(2) under the nitrogen protection, the 100-600 ℃ of processing of removing photoresist, the time is 1-6 hour with carbon fiber, and placing concentration then is that the nitric acid of 40-70% soaked 0.1-5 hour, cleans oven dry, the carbon fiber after obtaining handling again;
(3) under the nitrogen protection, the carbon fiber after the above-mentioned processing was flooded 0.1-5 hour with poly-borosilicate azane anhydrous toluene solution, leave standstill after dipping is good;
(4) under the nitrogen stream atmosphere, the carbon fiber behind the dipping that step (3) is obtained is warmed up to 50-400 ℃ with the speed of 0.02-2 ℃/min and carries out crosslinkedly earlier, is incubated 10-30 hour; And then be warming up to 1000-1600 ℃ with the speed of 0.05-5 ℃/min and carry out cracking, be incubated 1-6 hour; Speed with 0.05-5 ℃/min drops to 100-600 ℃ at last, namely obtains SiBN(C) the carbon fiber coating.
2. the preparation method of carbon fiber coating a kind of high temperature resistant SiBN(C according to claim 1), it is characterized in that: the mass concentration of the poly-borosilicate azane anhydrous toluene solution described in the step (1) is 0.01-20%.
3. the preparation method of carbon fiber coating a kind of high temperature resistant SiBN(C according to claim 1) is characterized in that: the clean employing described in the step (2) be deionized water.
4. the preparation method of carbon fiber coating a kind of high temperature resistant SiBN(C according to claim 1), it is characterized in that: the operation described in the step (3) is to finish in being full of the glove box of pure nitrogen gas.
5. the preparation method of carbon fiber coating a kind of high temperature resistant SiBN(C according to claim 1), it is characterized in that: the mass fraction of SiBN (C) is 40-70% in the resulting SiBN of step (4) (C) the carbon fiber coating.
6. the preparation method of carbon fiber coating a kind of high temperature resistant SiBN(C according to claim 1), it is characterized in that: the heat resisting temperature of the resulting SiBN of step (4) (C) carbon fiber coating in oxidizing atmosphere is 400-800 ℃.
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Cited By (9)
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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 |
| CN104878357A (en) * | 2015-06-11 | 2015-09-02 | 桂林理工大学 | Method for preparing SiC coating layers on surfaces of carbon fibers by radio-frequency (RF) magnetron sputtering |
| CN105622119A (en) * | 2015-12-31 | 2016-06-01 | 中物功能材料研究院有限公司 | Ceramic-based composite coating and preparation method thereof |
| CN106192371A (en) * | 2016-06-30 | 2016-12-07 | 东华大学 | A kind of high temperature resistant 3Al2o32SiO2the preparation method of SiBNC carbon fiber composite coating |
| CN109400168A (en) * | 2018-12-03 | 2019-03-01 | 航天特种材料及工艺技术研究所 | It is a kind of comprising the SiC fiber and its preparation method and application of the SiBCN coating and SiC coating that are alternatively formed |
| CN110318253A (en) * | 2019-08-11 | 2019-10-11 | 西南石油大学 | A kind of preparation method of carbon fiber surface modification anti-oxidation composite coating |
| CN110721889A (en) * | 2019-10-16 | 2020-01-24 | 厦门欧势复材科技有限公司 | Method for preparing high-temperature-resistant coating by using high-impact-resistance carbon fibers |
| CN112961647A (en) * | 2021-02-09 | 2021-06-15 | 航天材料及工艺研究所 | Polyborosilazane high-temperature-resistant adhesive and preparation method and use method thereof |
| CN115028457A (en) * | 2022-06-24 | 2022-09-09 | 中国人民解放军国防科技大学 | Si-containing alloy 2 N 2 SiBN fiber with O-microcrystal in-situ coating and preparation method and application thereof |
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| 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 |
| CN104878357A (en) * | 2015-06-11 | 2015-09-02 | 桂林理工大学 | Method for preparing SiC coating layers on surfaces of carbon fibers by radio-frequency (RF) magnetron sputtering |
| CN105622119A (en) * | 2015-12-31 | 2016-06-01 | 中物功能材料研究院有限公司 | Ceramic-based composite coating and preparation method thereof |
| CN106192371A (en) * | 2016-06-30 | 2016-12-07 | 东华大学 | A kind of high temperature resistant 3Al2o32SiO2the preparation method of SiBNC carbon fiber composite coating |
| CN106192371B (en) * | 2016-06-30 | 2018-08-03 | 东华大学 | A kind of high temperature resistant 3Al2O3-2SiO2The preparation method of-SiBNC carbon fiber composite coatings |
| CN109400168A (en) * | 2018-12-03 | 2019-03-01 | 航天特种材料及工艺技术研究所 | It is a kind of comprising the SiC fiber and its preparation method and application of the SiBCN coating and SiC coating that are alternatively formed |
| CN109400168B (en) * | 2018-12-03 | 2022-02-08 | 航天特种材料及工艺技术研究所 | SiC fiber containing SiBCN coating and SiC coating which are alternately formed, and preparation method and application thereof |
| CN110318253A (en) * | 2019-08-11 | 2019-10-11 | 西南石油大学 | A kind of preparation method of carbon fiber surface modification anti-oxidation composite coating |
| CN110721889A (en) * | 2019-10-16 | 2020-01-24 | 厦门欧势复材科技有限公司 | Method for preparing high-temperature-resistant coating by using high-impact-resistance carbon fibers |
| CN112961647A (en) * | 2021-02-09 | 2021-06-15 | 航天材料及工艺研究所 | Polyborosilazane high-temperature-resistant adhesive and preparation method and use method thereof |
| CN115028457A (en) * | 2022-06-24 | 2022-09-09 | 中国人民解放军国防科技大学 | Si-containing alloy 2 N 2 SiBN fiber with O-microcrystal in-situ coating and preparation method and application thereof |
| CN115028457B (en) * | 2022-06-24 | 2022-12-30 | 中国人民解放军国防科技大学 | Si-containing alloy 2 N 2 SiBN fiber with O-microcrystal in-situ coating and preparation method and application thereof |
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Application publication date: 20130814 |