CN105130498A - Method for preparing silicon carbide coating on carbon material by employing reaction diffusion process - Google Patents
Method for preparing silicon carbide coating on carbon material by employing reaction diffusion process Download PDFInfo
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- CN105130498A CN105130498A CN201510380357.1A CN201510380357A CN105130498A CN 105130498 A CN105130498 A CN 105130498A CN 201510380357 A CN201510380357 A CN 201510380357A CN 105130498 A CN105130498 A CN 105130498A
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Abstract
The invention relates to the technical field of carbon fiber surface modification, and discloses a method for preparing silicon carbide coating on carbon material by employing reaction diffusion process. The method comprises firstly calculating and weighing a silicon powder with demanded mass according to the prepared silicon carbide coating on the carbon material surface; then putting the silicon powder and the carbon material in a furnace, vacuumizing the furnace to 1*10<2> Pa-1*10<-5> Pa, heating to 1000 DEG C-2000 DEG C stage by stage at a heating speed of 10-200 DEG C, keeping warm for 1-2 h, slowly cooling the raw materials along with the furnace, discharging from the furnace when the temperature decreases to 100 DEG C or below, and cooling in air, so as to obtain the uniform compact silicon carbide coating on the carbon material surface. According to the method, the demanded usage amount of the silicon powder is calculated, and the furnace internal temperature and the reaction time are adjusted and controlled, so that the thickness of the silicon carbide formed on the carbon fiber surface is precisely controlled, and the silicon carbide coating prepared on the carbon material surface is uniform and compact. The technology is simple in step and applicable to industrialized production.
Description
Technical field
The present invention relates to carbon material surface technical field of modification, specifically a kind of under elevated temperature in vacuo application response diffusion process prepare the method for coat of silicon carbide at carbon material surface.
Background technology
Carbon material is widely applied in all trades and professions because of numerous excellent properties such as its light weight, conduction, heat conduction, high-melting-point, high temperature resistant, resistance to ablation, high chemical stability, resistant to chemical media corrosion, however its numerous excellent properties especially high-temperature behavior advantage just can only embody in vacuum or non-oxygenated environment; In atmospheric environment, carbon material can only use below 400 DEG C, makes the continuous scaling loss of carbon material and rapid failure under higher temperature because carbon material can produce obviously oxidation.Therefore carbon material must carry out antioxidant defense when using in high temperature oxidation stability environment, preparing coat of silicon carbide at carbon material surface is the important channel of improving carbon material high temperature oxidation resistance.
The preparation method of carbon material surface coating mainly contains vapour deposition process, solid state diffusion method, entrapping method, squeegee process, sol-gel method, plasma spraying method, sputtering method, original position forming method, hydrothermal electrodeposition method and gel injection reaction sintering etc.Vapour deposition process is the most effective way preparing coat of silicon carbide at carbon material surface, and this method is not only suitable for overall carbon material, is also suitable for loose porous carbon material, as carbon fibre web tire, carbon felt etc.Conventional method easily occurs that when carbon material surface prepares coat of silicon carbide coating is prepared uneven, and coat-thickness is wayward, impact coating effect.
Summary of the invention
The object of this invention is to provide a kind of application response diffusion process prepares coat of silicon carbide method at carbon material surface, wayward with the thickness solving carbon material surface coat of silicon carbide, coating prepares uneven problem.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Application response diffusion process prepares a method for coat of silicon carbide at carbon material surface, and it comprises the following steps:
Step one, according to the coat of silicon carbide THICKNESS CALCULATION of drawing up standby at carbon material surface and weigh needed for silica flour quality;
Step 2, by silica flour and carbon material shove charge, in stove, be evacuated to 1 × 10
2pa ~ 1 × 10
-5pa, then be warming up to 1000 DEG C ~ 2000 DEG C stage by stage with the temperature rise rate of 10 ~ 200 DEG C/h, insulation 1 ~ 2h, then with stove Slow cooling, treat that temperature is reduced to less than 100 DEG C air coolings of coming out of the stove, carbon material surface obtains the coat of silicon carbide of even compact.
As a further improvement on the present invention, described carbon material comprises dense carbon material and goods, loose porous carbon material and goods thereof.
Silica flour quality m(unit in step one of the present invention: gram) and the carbon material surface of intending coating silicon carbide coating amass S(unit: square centimeter), coat-thickness t(unit: centimetre) between pass be:
Dense carbon material and goods thereof comprise carbon-carbon composite, graphite product etc.; Loose porous carbon material and goods thereof comprise carbon fibre web tire, carbon felt, carbon fiber knit body, carbon fiber acupuncture body etc.
Principle of the present invention silicon is heated in vacuum environment 1000 DEG C ~ 2000 DEG C high temperature, and the silicon steam utilizing the distillation of silicon under high-temperature vacuum or evaporation to produce reacts with carbon material and spreads, and at carbon material surface formation coat of silicon carbide, its reaction formula is:
The coat of silicon carbide that the method for the invention deposits at carbon material surface is even, fine and close, and only there is light spalling local, notes protection, almost do not peel off during operation.Coated component is carbon and silicon; Coating substance phase composite is α-SiC.
Beneficial effect of the present invention is:
(1) the method for the invention is by calculating the consumption of required silica flour, regulation and control reaction in-furnace temperature, reaction times, vacuum tightness, accurately can control the thickness of the coat of silicon carbide that carbon material surface is formed, the coat of silicon carbide even compact prepared by carbon material surface;
(2) processing step of the present invention is simple, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope microscopic appearance figure of original carbon felt;
Fig. 2 uses the scanning electron microscope shape appearance figure of processing method of the present invention after the carbon fiber surface depositing silicon silicon coating of carbon felt inside;
Fig. 3 is energy spectrum analysis region carbon felt shape appearance figure;
Fig. 4 is the energy spectrum analysis result at disbonding place;
Fig. 5 is the EDAX results at coating place;
Fig. 6 is the XRD spectra of coating carbon felt.
Embodiment
Be further described technical scheme of the present invention below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention again.
Embodiment 1
Be 40mm by diameter, thickness be the carbon felt sample of 10mm be placed in 1.5g silica flour is housed crucible in, be evacuated down to 1 × 10 after entering stove
2pa, is heated to 1000 DEG C of constant temperature 1 hour with the temperature rise rate of 10 DEG C/h, is then heated to 1300 DEG C with the temperature rise rate of 100 DEG C/h, then adjusts temperature rise rate and be heated to 2000 DEG C of degree constant temperature 2 hours with the temperature rise rate of 200 DEG C/h; Furnace cooling is to air cooling of being come out of the stove by material after 100 DEG C, and the thickness through inspection even compact at carbon felt internal carbon fibers surface deposition is the coat of silicon carbide of 0.29 μm.
Embodiment 2
Be 40mm by diameter, thickness be the carbon fibre web tire sample of 10mm be placed in 4.5g silica flour is housed crucible in, crucible is evacuated down to 1 × 10
-5pa, is heated to 1000 DEG C of constant temperature 1 hour with the temperature rise rate of 100 DEG C/h, is then heated to 1300 DEG C with the temperature rise rate of 50 DEG C/h, then adjusts temperature rise rate and be heated to 1600 DEG C of degree constant temperature 2 hours with the temperature rise rate of 30 DEG C/h; Furnace cooling is to air cooling of being come out of the stove by material after 100 DEG C, and the thickness through inspection even compact at carbon fibre web tire internal carbon fibers surface deposition is the coat of silicon carbide of 1.93 μm.
Embodiment 3
Be 40mm by diameter, thickness be the carbon felt sample of 10mm be placed in 5.5g silica flour is housed crucible in, be evacuated down to 1 × 10
-2below Pa, is heated to 1000 DEG C of constant temperature 1.5 hours with the temperature rise rate of 100 DEG C/h, is then heated to 1300 DEG C with the temperature rise rate of 80 DEG C/h, then adjusts temperature rise rate and be heated to 1800 DEG C of degree constant temperature 1.8 hours with the temperature rise rate of 60 DEG C/h; Furnace cooling is to air cooling of coming out of the stove after 100 DEG C, and at carbon felt internal carbon fibers surface deposition, the thickness of even compact is the coat of silicon carbide of 2.36 μm.
As shown in Figures 2 to 6, as seen from Figure 2, the coat of silicon carbide that carbon material internal carbon fibers surface deposits is even, fine and close, and only there is light spalling local for the coat of silicon carbide shape appearance figure of above-described embodiment prepared by carbon material surface; From Fig. 3, Fig. 4, Fig. 5, the composition of carbon fiber substrate is about the carbon of 98%, and coated component is carbon and silicon; As seen from Figure 6, coating substance phase composite is α-SiC.
The method of the invention, by calculating the consumption of required silica flour, regulation and control reaction in-furnace temperature, reaction times, accurately can control the thickness of the coat of silicon carbide that carbon fiber surface is formed, the coat of silicon carbide even compact prepared by carbon material surface.
Claims (2)
1. application response diffusion process prepares a method for coat of silicon carbide at carbon material surface, it is characterized in that: it comprises the following steps:
Step one, according to the coat of silicon carbide THICKNESS CALCULATION of drawing up standby at carbon material surface and weigh needed for silica flour quality;
Step 2, by silica flour and carbon material shove charge, in stove, be evacuated to 1 × 10
2pa ~ 1 × 10
-5pa, then be warming up to 1000 DEG C ~ 2000 DEG C stage by stage with the temperature rise rate of 10 ~ 200 DEG C/h, insulation 1 ~ 2h, then with stove Slow cooling, treat that temperature is reduced to less than 100 DEG C air coolings of coming out of the stove, carbon material surface obtains the coat of silicon carbide of even compact.
2. application response diffusion process according to claim 1 prepares the method for coat of silicon carbide at carbon material surface, it is characterized in that: described carbon material comprises dense carbon material and goods thereof, or loose porous carbon material and goods thereof.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114907144A (en) * | 2022-06-06 | 2022-08-16 | 吉林联科特种石墨材料有限公司 | Method for preparing SiC-C composite high-temperature coating by one-step method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003942A (en) * | 2006-12-29 | 2007-07-25 | 哈尔滨工业大学 | Method for preparing coat of silicon carbide on surface of carbon fiber |
| CN101560728A (en) * | 2009-05-07 | 2009-10-21 | 浙江理工大学 | Method for generating silicon carbide coating on surface of carbon fiber |
| CN102477694A (en) * | 2010-11-22 | 2012-05-30 | 大连创达技术交易市场有限公司 | Method for generating silicon carbide coating by using silicon thermal evaporation method |
| CN102850087A (en) * | 2012-09-29 | 2013-01-02 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| JP5166689B2 (en) * | 2005-10-17 | 2013-03-21 | 昭和電工株式会社 | Method for producing silica-coated carbon fiber |
| 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 |
-
2015
- 2015-07-02 CN CN201510380357.1A patent/CN105130498A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5166689B2 (en) * | 2005-10-17 | 2013-03-21 | 昭和電工株式会社 | Method for producing silica-coated carbon fiber |
| CN101003942A (en) * | 2006-12-29 | 2007-07-25 | 哈尔滨工业大学 | Method for preparing coat of silicon carbide on surface of carbon fiber |
| CN101560728A (en) * | 2009-05-07 | 2009-10-21 | 浙江理工大学 | Method for generating silicon carbide coating on surface of carbon fiber |
| CN102477694A (en) * | 2010-11-22 | 2012-05-30 | 大连创达技术交易市场有限公司 | Method for generating silicon carbide coating by using silicon thermal evaporation method |
| CN102850087A (en) * | 2012-09-29 | 2013-01-02 | 西安超码科技有限公司 | Method for preparing silicon carbide coating on graphite surface |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114907144A (en) * | 2022-06-06 | 2022-08-16 | 吉林联科特种石墨材料有限公司 | Method for preparing SiC-C composite high-temperature coating by one-step method |
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Application publication date: 20151209 |