CN101560728A - Method for generating silicon carbide coating on surface of carbon fiber - Google Patents
Method for generating silicon carbide coating on surface of carbon fiber Download PDFInfo
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- CN101560728A CN101560728A CNA2009100983312A CN200910098331A CN101560728A CN 101560728 A CN101560728 A CN 101560728A CN A2009100983312 A CNA2009100983312 A CN A2009100983312A CN 200910098331 A CN200910098331 A CN 200910098331A CN 101560728 A CN101560728 A CN 101560728A
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Abstract
The invention discloses a method for generating a silicon carbide coating on the surface of a carbon fiber. The method is used to synthesize the SiC coating on the surface of a polyacrylonitrile carbon fiber. The method comprises the following steps: placing silicon powder or fragments of silicon briquets into the bottom of a graphite crucible, and placing the carbon fiber horizontally on the top of the crucible; inversely placing a crucible with the same size on the crucible in which the carbon fiber is placed in order to increase the contact between the carbon fiber and silicon vapor as much as possible and fix the carbon fiber, and always keeping a distance between the fragments of the silicone briquets and the carbon fiber; placing the device into a high temperature vacuum sintering furnace, carrying out forvacuum pumping to 1 to 5 Pa by a mechanical pump, then charging shielding gas argon, carrying out vacuum pumping again to 10<-4> to 10<-2> Pa by the mechanical pump and a diffusion pump, then charging the shielding gas argon again, and turning off an argon source; and then raising the temperature above the melting point of silicon, holding the temperature for 1 to 9 hours, turning off power supply, and taking out the fiber after cooling down to find the silicone carbide coating generated on the surface of the fiber. The method has a series of advantages of simple device, no precursor gas such as chlorosilane or polycarbosilane needed, no hydrogen needed, and the like.
Description
Technical field
The present invention relates to a kind of method of generating silicon carbide coating on surface of carbon fiber.
Background technology
Carbon fiber is the material of firing in inert atmosphere with high specific strength and high ratio modulus, but has strong oxidation sensitive under the high temperature, has limited its application in fields such as Aeronautics and Astronautics, military projects.Apply the high-temperature oxidation resistance that ORC can improve carbon fiber at carbon fiber surface.Characteristics such as the SiC material has low-density, infusibility, thermal coefficient of expansion is low and antioxygenic property is good, carbon fiber surface applies SiC and solves carbon fiber non-oxidizability, inhibition interfacial reaction, again can assurance and light metals such as Al, Mg have compound good result, make it become the preferred material of ORC.Trichloromethyl silane commonly used or chlorosilane prepare the SiC coating for the precursor chemical vapour deposition technique both at home and abroad, also have to adopt low temperature radio frequency method, physical sputtering method to carry out the technology of SiC coating on carbon fiber.By the brushing carborundum sol-gel precursor, and carborundum is formed from the teeth outwards in order to the protection material with carbon element.But original carbon fiber surface prepares the method for SiC coating and needs special equipment PECVD or LPCVD and precursor gases (chlorosilane or Polycarbosilane), causes cost to increase.The present invention adopts the method for simple thermal evaporation silicon under high vacuum environment, form fine and close coat of silicon carbide at carbon fiber surface.This method is compared with traditional method, have equipment simple, need not chlorosilane or series of advantages such as Polycarbosilane precursor gases and hydrogen.
Summary of the invention
The object of the present invention is to provide a kind of method of generating silicon carbide coating on surface of carbon fiber, this method is directly under high vacuum environment, adopt the method for simple thermal evaporation silicon, silicon melt evaporation under the high temperature, generate carborundum with the carbon generation gas-solid reaction on carbon fiber top layer, form fine and close coat of silicon carbide at carbon fiber surface.
The technical solution used in the present invention is as follows:
Silica flour or silico briquette fragment are put into the black-fead crucible bottom; the poly-third Chi nitrile carbon fiber is horizontally placed on the crucible port; in order to increase contacting and the fixing third Chi nitrile carbon fiber that gathers of the poly-third Chi nitrile carbon fiber and silicon steam; be inverted onesize crucible on the crucible of having shelved the poly-third Chi nitrile carbon fiber; with silica flour or silico briquette fragment and the poly-third Chi nitrile carbon fibre separation; this device is put into the high-temperature vacuum sintering furnace; mechanical pump forvacuum 1～5Pa; charge into argon shield gas then, be evacuated to 10 with mechanical pump and diffusion pump once more
-4～10
-2Pa, and then charge into argon shield gas closes argon gas source, is warmed up to then on the fusing point of silicon, is incubated 1～9 hour, turns off power supply, takes out the poly-third Chi nitrile fiber after being cooled to room temperature, has promptly generated one deck coat of silicon carbide at the poly-third Chi nitrile carbon fiber surface.
The present invention compares with background technology, and the useful effect that has is:
The present invention adopts the method for simple thermal evaporation silicon under high vacuum environment, form fine and close coat of silicon carbide at carbon fiber surface.Do not need special equipment and precursor gases in the preparation process, make preparation cost than original method.This method is compared with traditional method, have equipment simple, need not chlorosilane or series of advantages such as Polycarbosilane precursor gases and hydrogen.
Description of drawings
Fig. 1 is the surface sweeping electromicroscopic photograph of embodiment 1 carbon fiber surface coat of silicon carbide.
Fig. 2 is the surface sweeping electromicroscopic photograph of embodiment 2 carbon fiber surface coat of silicon carbide.
Fig. 3 is the surface sweeping electromicroscopic photograph of embodiment 3 carbon fiber surface coat of silicon carbide.
The specific embodiment
Embodiment 1:
The present invention adopts the method for simple thermal evaporation silicon melt, in the synthetic SiC coating of the poly-third Chi nitrile carbon fiber surface.Silica flour is put into the black-fead crucible bottom, the poly-third Chi nitrile carbon fiber is horizontally placed on the crucible top, in order to increase contacting and the fixing third Chi nitrile carbon fiber that gathers of the poly-third Chi nitrile carbon fiber and silicon steam as far as possible, be inverted onesize crucible on the crucible of having shelved the poly-third Chi nitrile carbon fiber, maintain a certain distance between silica flour and the poly-third Chi nitrile carbon fiber.This device is put into the high-temperature vacuum sintering furnace, and mechanical pump forvacuum 1Pa charges into argon shield gas then, is evacuated to vacuum 1 * 10 with mechanical pump and diffusion pump once more
-4Pa, and then charge into argon shield gas, close argon gas source.Be warmed up to then on the fusing point of silicon, be incubated 5 hours, turn off power supply, sample is taken out in the cooling back, and the poly-third Chi nitrile carbon fiber surface of black has become bright green.Directly adopt the phase composition of X-ray diffraction analysis product, its pattern of scanning electron microscope analysis.The result shows that the poly-third Chi nitrile fiber surface has generated one deck coat of silicon carbide, as shown in Figure 1.
Embodiment 2:
The present invention adopts the method for simple thermal evaporation silicon melt, in the synthetic SiC coating of the poly-third Chi nitrile carbon fiber surface.The silico briquette fragment is put into the black-fead crucible bottom, the poly-third Chi nitrile carbon fiber is horizontally placed on the crucible top, in order to increase contacting and the fixing third Chi nitrile carbon fiber that gathers of the poly-third Chi nitrile carbon fiber and silicon steam as far as possible, be inverted onesize crucible on the crucible of having shelved the poly-third Chi nitrile carbon fiber, remain certain distance between silico briquette fragment and the poly-third Chi nitrile carbon fiber.This device is put into the high-temperature vacuum sintering furnace, and mechanical pump forvacuum 3Pa charges into argon shield gas then, is evacuated to different vacuum 1 * 10 with mechanical pump and diffusion pump once more
-2Pa, and then charge into argon shield gas, close argon gas source.Be warmed up to then on the fusing point of silicon, be incubated 9 hours, turn off power supply, sample is taken out in the cooling back, and the poly-third Chi nitrile carbon fiber surface of black has become bright green.Directly adopt the phase composition of X-ray diffraction analysis product, its pattern of scanning electron microscope analysis.The result shows that the poly-third Chi nitrile fiber surface has generated one deck coat of silicon carbide, is also shown in a spot of silicon carbide whisker and generates, as shown in Figure 2 under the lower vacuum.
Embodiment 3:
The present invention adopts the method for simple thermal evaporation silicon melt, in the synthetic SiC coating of the poly-third Chi nitrile carbon fiber surface.Silica flour is put into the black-fead crucible bottom, the poly-third Chi nitrile carbon fiber is horizontally placed on the crucible top, in order to increase contacting and the fixing third Chi nitrile carbon fiber that gathers of the poly-third Chi nitrile carbon fiber and silicon steam as far as possible, be inverted onesize crucible on the crucible of having shelved the poly-third Chi nitrile carbon fiber, remain certain distance between silica flour and the poly-third Chi nitrile carbon fiber.This device is put into the high-temperature vacuum sintering furnace, and mechanical pump forvacuum 5Pa charges into argon shield gas then, is evacuated to different vacuum 1 * 10 with mechanical pump and diffusion pump once more
-3Pa, and then charge into argon shield gas, close argon gas source.Be warmed up to then on the fusing point of silicon, be incubated 1 hour, turn off power supply, sample is taken out in the cooling back, and the poly-third Chi nitrile carbon fiber surface of black has become bright green.Directly adopt the phase composition of X-ray diffraction analysis product, its pattern of scanning electron microscope analysis.The result shows that the poly-third Chi nitrile fiber surface has generated one deck coat of silicon carbide, as shown in Figure 3.
Claims (1)
1; a kind of method of generating silicon carbide coating on surface of carbon fiber; it is characterized in that: silica flour or silico briquette fragment are put into the black-fead crucible bottom; the poly-third Chi nitrile carbon fiber is horizontally placed on the crucible port; in order to increase contacting and the fixing third Chi nitrile carbon fiber that gathers of the poly-third Chi nitrile carbon fiber and silicon steam; be inverted onesize crucible on the crucible of having shelved the poly-third Chi nitrile carbon fiber; with silica flour or silico briquette fragment and the poly-third Chi nitrile carbon fibre separation; this device is put into the high-temperature vacuum sintering furnace; mechanical pump forvacuum 1～5Pa; charge into argon shield gas then, be evacuated to 10 with mechanical pump and diffusion pump once more
-4～10
-2Pa, and then charge into argon shield gas closes argon gas source, is warmed up to then on the fusing point of silicon, is incubated 1～9 hour, turns off power supply, takes out the poly-third Chi nitrile fiber after being cooled to room temperature, has promptly generated one deck coat of silicon carbide at the poly-third Chi nitrile carbon fiber surface.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100983312A CN101560728A (en) | 2009-05-07 | 2009-05-07 | Method for generating silicon carbide coating on surface of carbon fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100983312A CN101560728A (en) | 2009-05-07 | 2009-05-07 | Method for generating silicon carbide coating on surface of carbon fiber |
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| CN101560728A true CN101560728A (en) | 2009-10-21 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021817A (en) * | 2010-11-11 | 2011-04-20 | 中国人民解放军国防科学技术大学 | Silicon carbide fiber solid fabric for in-situ growing carbon nano tubes, composite material and preparation method thereof |
| CN103993475A (en) * | 2014-05-27 | 2014-08-20 | 哈尔滨工业大学 | Preparation method for coating carbon fiber surface with SiC nanowire |
| CN103993474A (en) * | 2014-04-23 | 2014-08-20 | 大连理工高邮研究院有限公司 | Preparation method of silicon carbide coating on surface of hard carbon fiber felt |
| CN105130498A (en) * | 2015-07-02 | 2015-12-09 | 甘肃郝氏炭纤维有限公司 | Method for preparing silicon carbide coating on carbon material by employing reaction diffusion process |
| CN107059129A (en) * | 2017-04-05 | 2017-08-18 | 西北工业大学 | Co-precipitation and the preparation method of thermal evaporation techniques fabricated in situ taper SiC whiskers |
-
2009
- 2009-05-07 CN CNA2009100983312A patent/CN101560728A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021817A (en) * | 2010-11-11 | 2011-04-20 | 中国人民解放军国防科学技术大学 | Silicon carbide fiber solid fabric for in-situ growing carbon nano tubes, composite material and preparation method thereof |
| CN102021817B (en) * | 2010-11-11 | 2012-03-21 | 中国人民解放军国防科学技术大学 | Silicon carbide fiber solid fabric for in-situ growing carbon nano tubes, composite material and preparation method thereof |
| CN103993474A (en) * | 2014-04-23 | 2014-08-20 | 大连理工高邮研究院有限公司 | Preparation method of silicon carbide coating on surface of hard carbon fiber felt |
| CN103993475A (en) * | 2014-05-27 | 2014-08-20 | 哈尔滨工业大学 | Preparation method for coating carbon fiber surface with SiC nanowire |
| CN105130498A (en) * | 2015-07-02 | 2015-12-09 | 甘肃郝氏炭纤维有限公司 | Method for preparing silicon carbide coating on carbon material by employing reaction diffusion process |
| CN107059129A (en) * | 2017-04-05 | 2017-08-18 | 西北工业大学 | Co-precipitation and the preparation method of thermal evaporation techniques fabricated in situ taper SiC whiskers |
| CN107059129B (en) * | 2017-04-05 | 2019-04-19 | 西北工业大学 | The preparation method of co-precipitation and thermal evaporation techniques fabricated in situ cone cell SiC whisker |
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Open date: 20091021 |