CN104446585B - The method that batch quickly prepares high-density carbon/carbon composite material - Google Patents
The method that batch quickly prepares high-density carbon/carbon composite material Download PDFInfo
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- CN104446585B CN104446585B CN201310438377.0A CN201310438377A CN104446585B CN 104446585 B CN104446585 B CN 104446585B CN 201310438377 A CN201310438377 A CN 201310438377A CN 104446585 B CN104446585 B CN 104446585B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 41
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003345 natural gas Substances 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 238000005336 cracking Methods 0.000 claims abstract description 3
- 239000003085 diluting agent Substances 0.000 claims abstract description 3
- 238000004062 sedimentation Methods 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000002296 pyrolytic carbon Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000151 deposition Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000011112 process operation Methods 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract 1
- 230000001131 transforming effect Effects 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical class [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 206010051986 Pneumatosis Diseases 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The present invention relates to a kind of method that batch quickly prepares high-density carbon/carbon composite material, after its method is by transforming furnace chamber inside, precast body is put into stove, cracked gas natural gas and diluent gas nitrogen are passed through gas tank after proportioning, enter cvd furnace after mixing, again by the preheating and diffusion of preheating zone, it is heated evenly mixed gas, natural gas reaches critical cracking temperature, interim operation is carried out by inputting the gentle voltage-controlled processing procedure sequence of temperature control program, gas flow control program so that the deposition efficiency of gas is high.The method can carry out industrialization production, and the technique of preparation is simple, process operation intelligent control.Product short preparation period, density is high, stable quality, and qualification rate is high.
Description
Technical field
The present invention relates to carbon-carbon composites technical field, and it is compound particularly quickly to prepare high-density carbon/carbon/charcoal in batches
The method of material.
Background technology
Carbon/carbon composite is the composite material of carbon fiber reinforced carbon matrix, in high temperature environments with high specific strength and
Specific modulus, and good resistance to ablation, ermal physics, friction and wear behavior and mechanical behavior under high temperature, are uniquely can so far
Meet these rigors and most promising hi tech and new material.It has been successfully applied to guided missile nose cone, rocket engine
The military, aerospace field such as jet pipe throat lining, space shuttle nose cone and the leading edge of a wing and aeroplane brake discs and chemical industry, metallurgy,
Automobile, nuclear energy etc. is civilian and medical domain.But since external long-term technology blocks, China is prepared in carbon-carbon composites at present
Fall behind in technique also in developing stage, equipment, complex process, long preparation period, deposition efficiency is low, unstable product quality one
It is directly the present situation of China's carbon/carbon composite.The present invention be directed to insufficient present in charcoal/charcoal compound heat treating preparation process, into
Substantial amounts of experimental exploration is gone, significant improvement has been carried out to deposition furnace apparatus, by carrying out the stage to temperature, air pressure and gas flow
Property control, design a kind of new process, device is simple, easy to operate, is applicable to variously-shaped precast body, with this work
The carbon/carbon composite cycle prepared by skill is short, and cost is low, and deposition efficiency is high, and product quality is stablized.
By retrieval, the related invention that domestic batch quickly prepares the method for high-density carbon/carbon composite material at present exists
Complex process, the problems such as cost is excessive, can not produce in enormous quantities, and quality is unstable.Such as domestic Patent No.
Pneumatosis method of flow control is oozed in a kind of 200910093946.6 high-performance carbon-based composite material slewing, its graphite Fixture Design
Ring-like precast body can only be adapted to, template or special-shaped precast body cannot be oriented and ooze product, and not to air pressure, temperature
If degree and gas flow carry out stage control, the effect of quick densifying is not reached.Such as domestic Patent No.
200410026035.9 thermal gradient chemical vapor deposition method for preparing carbon/carbon/carbon composite heavy wall plate, this patent is described
Method can quickly prepare highdensity carbon/carbon composite really, but the structure of common product is that there is some difference, need
Special fixture, only suitable single-piece production, it is difficult to industrialized production.
The content of the invention
The purpose of the present invention is the deficiency for existing technology both at home and abroad, and a kind of batch is provided and quickly prepares high density
The method of carbon/carbon composite.
To achieve the above object, the technical solution adopted in the present invention is：It is multiple that a kind of batch quickly prepares high-density carbon/carbon/charcoal
The method of condensation material, it is characterised in that this method comprises the following steps：
(1) precast body and frock clamp are put into cvd furnace, close bell, to carrying out being evacuated to pressure ＜ in stove
10Pa, starts heating schedule, is warming up to 800-1100 DEG C；
(2) cracked gas natural gas and diluent gas nitrogen are passed through gas tank after proportioning, it is heavy to enter after mixing
Product stove；
(3) above-mentioned mixed gas is diffused gas by cvd furnace preheating zone, graphite cover, mixed gas is heated
Uniformly, and it is rapidly heated to 800-1100 DEG C, reaches the critical cracking temperature of natural gas, so improves the utilization rate of gas and sink
Long-pending speed；
(4) two kinds of mixed gas of natural gas and nitrogen are equal by pyrolytic carbon by three graphite cylinders and porous graphite plectane
Even is deposited in precast body internal clearance, by input temperature control program, gas flow control the gentle voltage-controlled processing procedure sequence of program into
The interim operation of row so that the utilization rate of gas is high, sedimentation time 300h, extrudate density >=1.70g/cm3。
It is of the invention to be had the following advantages compared with existing domestic technique：
(1) the method can carry out industrialization production.
(2) the method is unrestricted to the geomery of precast body.
(3) technique prepared is simple, process operation intelligent control.
(4) product short preparation period, density is high, stable quality, and qualification rate is high.
Brief description of the drawings
Fig. 1 is the device structure schematic diagram of the present invention.
Symbol description is as follows in figure：
(1)-gas outlet；(2)-graphite ring pads；(3)-precast body；
(4)-porous graphite plectane；(5)-graphite cylinder；(6)-preheating coil；
(7)-graphite cover；(8)-air inlet.
Embodiment
With reference to example, the present invention will be further described：
Example 1
Using intermediate frequency power supply chemical vapor deposition stove (a diameter of 650MM of furnace chamber, is highly 1600MM), 12 prefabricated
Body size is 4001mm × 400mm × 30mm, and 12 graphite ring pads outside diameters are 600mm, are highly 80mm, 12 porous graphite circles
Plate outside diameter is 600mm, thickness 30mm, and the through hole of 100 diameter 15mm is evenly distributed on plectane.Its step is as follows：
(1) precast body and frock clamp are put into cvd furnace, close bell, to carrying out being evacuated to pressure ＜ in stove
10Pa, starts heating schedule, is warming up to 800-1100 DEG C；Gas valve, natural gas and nitrogen is opened to mix by gas tank
Enter cvd furnace after even.
(2) input the gentle voltage-controlled processing procedure sequence of temperature control program, gas flow control program and carry out interim operation：Preheating gas
Temperature is 920 DEG C in 0-100h, and sedimentation time is 870 DEG C in 100-200h, and sedimentation time is 820 in 200-300h
℃.In-furnace temperature is 950 DEG C when sedimentation time is in 0-200h, and sedimentation time is 1000 DEG C in 200-300h.Natural gas and
The flow of nitrogen is 2L/min and 6L/min when sedimentation time is in 0-100h, sedimentation time in 100-200h for 2L/min and
5L/min, sedimentation time are 2L/min and 4L/min in 200-300h.Air pressure is 5Pa when sedimentation time is in 0-100h, is sunk
The product time is 60Pa in 100-200h, and sedimentation time is 120Pa in 200-300h.
(3) after being vapor-deposited when 300 is small, power supply is closed, gas valve is closed, cools to room temperature, thus obtain
Density is 1.75g/cm3Product.
Example 2
Using intermediate frequency power supply chemical vapor deposition stove (a diameter of 650MM of furnace chamber, is highly 1600MM), 12 prefabricated
Body size is 400mm × 400mm × 20mm, and 12 graphite ring pads outside diameters are 600mm, are highly 80mm, 12 porous graphite circles
Plate outside diameter is 600mm, thickness 30mm, and the through hole of 100 diameter 15mm is evenly distributed on plectane.Its step is as follows：
(1) precast body and frock clamp are put into cvd furnace, close bell, to carrying out being evacuated to pressure ＜ in stove
10Pa, starts heating schedule, is warming up to 800-1100 DEG C；Gas valve, natural gas and nitrogen is opened to mix by gas tank
Enter cvd furnace after even.
(2) input the gentle voltage-controlled processing procedure sequence of temperature control program, gas flow control program and carry out interim operation：Preheating gas
Temperature is 900 DEG C in 0-100h, and sedimentation time is 850 DEG C in 100-200h, and sedimentation time is 800 in 200-300h
℃.In-furnace temperature is 980 DEG C when sedimentation time is in 0-200h, and sedimentation time is 1050 DEG C in 200-300h.Natural gas and
The flow of nitrogen is 2L/min and 6L/min when sedimentation time is in 0-100h, sedimentation time in 100-200h for 2L/min and
5L/min, sedimentation time are 2L/min and 4L/min in 200-300h.Air pressure is 5Pa when sedimentation time is in 0-100h, is sunk
The product time is 50Pa in 100-200h, and sedimentation time is 110Pa in 200-300h.
(3) after being vapor-deposited when 300 is small, power supply is closed, gas valve is closed, cools to room temperature, thus obtain
Density is 1.75g/cm3Product.
The tensile strength of its product is 150-200MPa, compressive strength 180-250MPa, bending strength 140-
280MPa, its property indices reach requirement.
Claims (3)
1. the method that batch quickly prepares high-density carbon/carbon composite material, this method comprise the following steps：
(1) precast body and frock clamp are put into cvd furnace, close bell, to carrying out being evacuated to pressure ＜ 10Pa in stove,
Start heating schedule, be warming up to 800~1100 DEG C；
(2) cracked gas natural gas and diluent gas nitrogen are passed through gas tank after proportioning, after mixing into cvd furnace；
(3) above-mentioned mixed gas is diffused gas by cvd furnace preheating zone, graphite cover, mixed gas is heated
It is even, and be rapidly heated to 800~1100 DEG C, reach the critical cracking temperature of natural gas, so improve the utilization rate of gas and sink
Long-pending speed；
(4) two kinds of mixed gas of natural gas and nitrogen pass sequentially through three graphite cylinders and porous graphite plectane, and pyrolytic carbon is equal
Even is deposited in precast body internal clearance, by input temperature control program, gas flow control the gentle voltage-controlled processing procedure sequence of program into
The interim operation of row so that the utilization rate of gas is high, sedimentation time 300h, extrudate density >=1.70g/cm3；Sedimentation time exists
During 0~100h, the flow-rate ratio of natural gas and nitrogen is 1:3, air pressure is 0~10Pa, and pre-heated gas temperature is 900-950 DEG C；It is heavy
The product time, the flow-rate ratio of natural gas and nitrogen was 1 in 100~200h:2.5, air pressure is 50~100Pa, pre-heated gas temperature
For 850~900 DEG C；For sedimentation time in 200~300h, the flow-rate ratio of natural gas and nitrogen is 1:2, air pressure for 100~
150Pa, pre-heated gas temperature are 800~850 DEG C；When sedimentation time is in 0~200h, in-furnace temperature is 900~1000 DEG C, is sunk
The product time, in-furnace temperature was 1000~1100 DEG C in 200~300h.
2. the method that batch according to claim 1 quickly prepares high-density carbon/carbon composite material, it is characterised in that institute
State a diameter of 50~80mm of graphite cylinder in step (4).
3. the method that batch according to claim 1 quickly prepares high-density carbon/carbon composite material, it is characterised in that institute
The thickness for stating the graphite disk in step (4) is 30~50mm, a diameter of 450-500mm, EDS maps on the graphite disk
Hole count is 70~100.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558427B (en) * | 2018-05-22 | 2020-11-13 | 中南大学 | Method for batch preparation of carbon/carbon composite material flat plate with uniform density by using confined reactor |
| CN109400198A (en) * | 2018-12-13 | 2019-03-01 | 上海康碳复合材料科技有限公司 | A kind of carbon/carbon (pottery) composite material brake disc Preparation equipment and preparation method thereof based on quick sedimentation process |
| CN111574237A (en) * | 2020-05-22 | 2020-08-25 | 中南大学 | Oversized carbon/carbon composite material sheet and equipment for preparing same |
| CN112628326A (en) * | 2020-11-13 | 2021-04-09 | 甘肃新西北碳素科技有限公司 | Preparation method of aircraft brake disc made of carbon/carbon composite material |
| CN113293356A (en) * | 2021-04-09 | 2021-08-24 | 郭李梁 | Device for preparing carbon-carbon composite material |
| CN114249601B (en) * | 2021-11-15 | 2022-10-28 | 西安航空制动科技有限公司 | Densification method of brake disc made of carbon/carbon composite material |
| CN115231940A (en) * | 2022-08-01 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | Production process of carbon thermal insulation cylinder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5578255A (en) * | 1989-10-26 | 1996-11-26 | Mitsubishi Chemical Corporation | Method of making carbon fiber reinforced carbon composites |
| CN101671189A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Method for using domestic carbon fiber to prepare high-performance carbon-based composite material through rapid directional infiltration |
| CN101671188A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Gas flow control method of rapid directional infiltration for high-performance carbon-based composite material |
-
2013
- 2013-09-24 CN CN201310438377.0A patent/CN104446585B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5578255A (en) * | 1989-10-26 | 1996-11-26 | Mitsubishi Chemical Corporation | Method of making carbon fiber reinforced carbon composites |
| CN101671189A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Method for using domestic carbon fiber to prepare high-performance carbon-based composite material through rapid directional infiltration |
| CN101671188A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Gas flow control method of rapid directional infiltration for high-performance carbon-based composite material |
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Effective date of registration: 20190315 Address after: Room 502, Venture Building No. 18, High-tech Second Road, Nanchang High-tech Industrial Development Zone, Nanchang City, Jiangxi Province Patentee after: JIANGXI JIAJIE XINDA NEW MATERIAL TECHNOLOGY CO.,LTD. Address before: 529164 No. 1 Beach Wai Industrial Zone, Zhoujun Village, Tangxia Town, Pengjiang District, Jiangmen City, Guangdong Province Patentee before: Jiangmen Shuopu Science And Technology Develop Co.,Ltd. |
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Effective date of registration: 20240125 Address after: 330513 Hongshan Avenue, Industrial Park, Anyi County, Nanchang City, Jiangxi Province Patentee after: Jiangxi Xinda Hangke New Material Technology Co.,Ltd. Country or region after: China Address before: Room 502, Venture Building No. 18, High-tech Second Road, Nanchang High-tech Industrial Development Zone, Nanchang City, Jiangxi Province Patentee before: JIANGXI JIAJIE XINDA NEW MATERIAL TECHNOLOGY CO.,LTD. Country or region before: China |