CN101392366A - Method for preparing rapid chemical vapor infiltration of carbon/carbon composite material flat plate - Google Patents

Method for preparing rapid chemical vapor infiltration of carbon/carbon composite material flat plate Download PDF

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Publication number
CN101392366A
CN101392366A CNA200810143540XA CN200810143540A CN101392366A CN 101392366 A CN101392366 A CN 101392366A CN A200810143540X A CNA200810143540X A CN A200810143540XA CN 200810143540 A CN200810143540 A CN 200810143540A CN 101392366 A CN101392366 A CN 101392366A
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carbon
compound material
base substrate
chemical vapor
vapor infiltration
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CNA200810143540XA
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CN101392366B (en
Inventor
张红波
熊翔
张福勤
周九宁
夏莉红
王蕾
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HUNAN BOYUN NEW MATERIALS CO Ltd
Central South University
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HUNAN BOYUN NEW MATERIALS CO Ltd
Central South University
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Abstract

The invention discloses a preparation method of fast chemical vapor infiltration of a carbon/carbon composite flat plate. The preparation method comprises the following steps that: (1) in a chemical vapor carburizing furnace, a heating unit of a flat plate is vertically arranged at the furnace bottom; (2) a fixed bearing platform is respectively arranged at both sides of the heating unit of the flat plate; and a carbon/carbon composite flat plate-shaped mold to be thickened and paralleling to the plane of the heating unit is respectively positioned on each bearing platform and the gas flow passes through the mold; (3) C3H6 is taken as gas of a carbon source and N2 as dilution gas; and the bulk factor of C3H6 to N2 is 1:0.5 to 3; and (4) the temperature of the furnace is controlled as 800 DEG C to 1300 DEG C and the pressure as 1kPa to 5kPa. The preparation method has the advantages of simpleness, convenient operation, high utilization ratio of the gas of the carbon source, high straightness of final products and short technological cycle, solves the long-standing problem which is pending in the field and also provides a practical method for the mass production of the carbon/carbon composite flat plate.

Description

The method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board
Technical field
The present invention relates to a kind of preparation method of carbon/carbon compound material, be meant a kind of method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board especially.
Background technology
Carbon/carbon compound material, promptly the carbon fiber reinforced carbon matrix composite material is a kind of thermal structure material of excellence.It not only has the matrix material excellent mechanical property, and has the property of carbon material, as: strength and stiffness height under the high temperature, thermal expansivity is low, dimensional stability is good etc., is at present unique 3000 ℃ of pyritous matrix materials that can be used for.Because above-mentioned special performance, carbon/carbon compound material flat board and workpiece the having a extensive future thereof of carbon/carbon compound material in fields such as hot-work.
Chemical vapor infiltration is the prefered method of preparation high-performance carbon/carbon compound material, and the material of this method preparation has even structure, complete, advantage such as compactness is good.But existing chemical gas phase cementation process is not suitable for the preparation of carbon/carbon compound material flat board.Its reason has two: one, existing chemical vapor infiltration process using drum type brake type of heating or column type type of heating, the carbon/carbon compound material base substrate place in the cylinder or the garden post around, in the chemical vapor infiltration process, flat board is heated buckling deformation can take place, and causes the planeness of product to be difficult to be guaranteed.The 2nd, owing to be subjected to the restriction of gas phase rate of diffusion and surface reaction speed, long (about 1000-1500h), carbon source gas utilising efficiency low (<5%) of chemical vapor infiltration thickening technology cycle causes the preparation cost height of product to be looked forward to.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide that a kind of processing method is simple, easy to operate, the method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board that carbon source gas utilising efficiency height, the planeness height of the finished product, process cycle are short.
The method for preparing rapid chemical vapor infiltration of the present invention---carbon/carbon compound material flat board is to adopt following proposal to realize:
1) in chemical gas phase carburizing stove, one flat-plate heating body is set perpendicular to furnace bottom;
2) in flat-plate heating body both sides one fixed bearing platform is set respectively, on each cushion cap, respectively be provided with one with the parallel plane density carbon/carbon compound material tabular base substrate for the treatment of of heating element, air-flow is worn base substrate and mistake;
3) with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is 1:0.5~3;
4) Control for Kiln Temperature is that 800~1300 ℃, furnace pressure are 1~5kPa.
Among the present invention, described flat-plate heating body can be a kind of in carbon/carbon compound material or the graphite.
Among the present invention, the described density carbon/carbon compound material tabular base substrate for the treatment of can be a kind of in the whole felt of tabular carbon felt or carbon fiber acupuncture, and the apparent density of tabular base substrate is 0.05g/cm 3~0.8g/cm 3
Among the present invention, described fixed bearing platform is the graphite manufacturing.
Among the present invention, describedly treat that density carbon/carbon compound material tabular base substrate and flat-plate heating surface spacing are 10~100mm.
The present invention is owing to adopt above-mentioned processing method, thereby, have following advantage and positively effect:
1, adopts fixedly base substrate of graphite fixed bearing platform, can reduce the temperature distortion of base substrate in technological process, guarantee the planeness of carbon/carbon compound material flat board.
2, carbon source gas passes base substrate and flows, and can shorten the chemical vapor infiltration thickening technology cycle, improves carbon source gas utilising efficiency.
3, adopt the present invention, through the 50h chemical vapor infiltration, the whole felt base substrate of acupuncture that can will be of a size of 300 * 300 * 15mm is by 0.5g/cm 3Density is to 1.52g/cm 3
In sum, the present invention--the method for preparing rapid chemical vapor infiltration of-carbon/carbon compound material flat board, processing method is simple, easy to operate, the planeness height of carbon source gas utilising efficiency height, the finished product, process cycle are short, solved for a long time this area and urgently wished to solve and unsolved problem, for the suitability for industrialized production of carbon/carbon compound material flat board provides a kind of practicable method.
Description of drawings
Accompanying drawing is the concrete structural principle synoptic diagram of implementing of the present invention.
Among the figure: 1---body of heater, 2---flat-plate heating body, 3---cushion cap, 4---are treated density carbon/carbon compound material tabular base substrate.
Embodiment
Embodiment 1
At first, choosing apparent density is 1.75g/cm 3, be of a size of 500 * 500 * 15mm the carbon/carbon compound material flat board as heating element, apparent density is 0.05g/cm 3, be of a size of the whole felt of carbon fiber acupuncture of 200 * 200 * 30mm as base substrate.Treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 10mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:0.5, total gas flow rate are that temperature is that 800 ℃, furnace pressure are 5kPa in the 25l/min, stove, and chemical vapor infiltration 200h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 2
At first, choosing apparent density is 1.75g/cm 3, be of a size of 500 * 500 * 15mm the carbon/carbon compound material flat board as heating element, apparent density is 0.6g/cm 3, be of a size of the whole felt of carbon fiber acupuncture of 300 * 300 * 20mm as base substrate.Treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 50mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 15l/min, sample surfaces temperature are that 1100 ℃, furnace pressure are 2.5kPa, and chemical vapor infiltration 150h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 3
At first, choosing apparent density is 1.75g/cm 3, be of a size of 500 * 500 * 15mm the carbon/carbon compound material flat board as heating element, apparent density is 0.8g/cm 3, be of a size of the whole felt of carbon fiber acupuncture of 400 * 400 * 15mm as base substrate.Treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 100mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:3, total gas flow rate are that 5l/min, sample surfaces temperature are that 1300 ℃, furnace pressure are 1kPa, and chemical vapor infiltration 100h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 4
At first, choosing apparent density is 1.75g/cm 3, be of a size of 500 * 500 * 15mm the carbon/carbon compound material flat board as heating element, apparent density is 0.25g/cm 3, be of a size of the whole felt of carbon fiber acupuncture of 500 * 500 * 15mm as base substrate.Treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 100mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 5l/min, sample surfaces temperature are that 1250 ℃, furnace pressure are 1kPa, and chemical vapor infiltration 50h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 5
At first, choosing apparent density is 1.8g/cm 3, be of a size of 500 * 500 * 15mm the graphite flat board as heating element, apparent density is 0.15g/cm 3, be of a size of the whole felt of carbon fiber acupuncture of 300 * 300 * 15mm as base substrate.Treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 100mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 20l/min, sample surfaces temperature are that 900 ℃, furnace pressure are 3kPa, and chemical vapor infiltration 150h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 6
At first, choosing apparent density is 1.8g/cm 3, be of a size of 500 * 500 * 15mm the graphite flat board as heating element, apparent density is 0.45g/cm 3, be of a size of the whole felt of carbon fiber acupuncture of 300 * 300 * 15mm as base substrate.Treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 100mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 10l/min, sample surfaces temperature are that 1000 ℃, furnace pressure are 2kPa, and chemical vapor infiltration 100h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 7
At first, choosing apparent density is 1.8g/cm 3, be of a size of 500 * 500 * 15mm the graphite flat board as heating element, apparent density is 0.55g/cm 3, be of a size of the carbon felt of 300 * 300 * 10mm as base substrate.Secondly, treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 20mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 5l/min, sample surfaces temperature are that 1150 ℃, furnace pressure are 1kPa, and chemical vapor infiltration 100h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 8
At first, choosing apparent density is 1.8g/cm 3, be of a size of 500 * 500 * 15mm the graphite flat board as heating element, apparent density is 0.8g/cm 3, be of a size of the carbon felt of 300 * 300 * 15mm as base substrate.Secondly, treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 20mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 15l/min, sample surfaces temperature are that 1000 ℃, furnace pressure are 3kPa, and chemical vapor infiltration 100h promptly gets carbon/carbon compound material flat board of the present invention.
Embodiment 9
At first, choosing apparent density is 1.8g/cm 3, be of a size of 500 * 500 * 15mm the graphite flat board as heating element, apparent density is 0.7g/cm 3, be of a size of the carbon felt of 300 * 300 * 10mm as base substrate.Secondly, treat the density carbon/carbon compound material base substrate heating element both sides that are placed in two, fix its position with the graphite fixed bearing platform, make plane, base substrate place and heating element place plane parallel, base substrate and heating element surface spacing are 50mm, and the carbon source air-flow is worn base substrate and mistake.At last, with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is that 1:1.5, total gas flow rate are that 25l/min, sample surfaces temperature are that 850 ℃, furnace pressure are 4kPa, and chemical vapor infiltration 150h promptly gets carbon/carbon compound material flat board of the present invention.

Claims (5)

1, the method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board comprises the steps:
1) in chemical gas phase carburizing stove, one flat-plate heating body is set perpendicular to furnace bottom;
2) in flat-plate heating body both sides one fixed bearing platform is set respectively, on each cushion cap, respectively be provided with one with the parallel plane density carbon/carbon compound material tabular base substrate for the treatment of of heating element, air-flow is worn base substrate and mistake;
3) with C 3H 6Be carbon source gas, N 2Be carrier gas, control C 3H 6: N 2Volume ratio is 1:0.5~3;
4) Control for Kiln Temperature is that 800~1300 ℃, furnace pressure are 1~5kPa.
2, the method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board according to claim 1 is characterized in that: described flat-plate heating body can be a kind of in carbon/carbon compound material or the graphite.
3, the method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board according to claim 1, it is characterized in that: the described density carbon/carbon compound material tabular base substrate for the treatment of can be a kind of in the whole felt of tabular carbon felt or carbon fiber acupuncture, and the apparent density of tabular base substrate is 0.05g/cm 3~0.8g/cm 3
4, the method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board according to claim 1 is characterized in that: described fixed bearing platform is the graphite manufacturing.
5, the method for preparing rapid chemical vapor infiltration of carbon/carbon compound material flat board according to claim 1 is characterized in that: describedly treat that density carbon/carbon compound material tabular base substrate and flat-plate heating surface spacing are 10~100mm.
CN200810143540XA 2008-11-07 2008-11-07 Method for preparing rapid chemical vapor infiltration of carbon/carbon composite material flat plate Expired - Fee Related CN101392366B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831621A (en) * 2010-04-08 2010-09-15 湖南金博复合材料科技有限公司 Chemical vapor densification furnace body
CN102211765A (en) * 2011-03-28 2011-10-12 航天材料及工艺研究所 Method for preparing carbon material with high heat conductivity by densifying gaps of graphite paper
CN108981534A (en) * 2018-09-11 2018-12-11 江苏擎弓科技股份有限公司 A kind of composite material plate spring detection device
CN109111239A (en) * 2018-10-30 2019-01-01 中南大学 A kind of preparation method of the device for preparing ultra-thin carbon/carbon compound material panel and panel
CN109279908A (en) * 2018-10-30 2019-01-29 中南大学 A kind of fixture preparing ultra-thin carbon/carbon compound material panel

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831621A (en) * 2010-04-08 2010-09-15 湖南金博复合材料科技有限公司 Chemical vapor densification furnace body
CN101831621B (en) * 2010-04-08 2012-10-17 湖南金博复合材料科技有限公司 Chemical vapor densification furnace body
CN102211765A (en) * 2011-03-28 2011-10-12 航天材料及工艺研究所 Method for preparing carbon material with high heat conductivity by densifying gaps of graphite paper
CN102211765B (en) * 2011-03-28 2013-06-26 航天材料及工艺研究所 Method for preparing carbon material with high heat conductivity by densifying gaps of graphite paper
CN108981534A (en) * 2018-09-11 2018-12-11 江苏擎弓科技股份有限公司 A kind of composite material plate spring detection device
CN108981534B (en) * 2018-09-11 2024-02-27 江苏擎弓科技股份有限公司 Detection device for composite plate spring
CN109111239A (en) * 2018-10-30 2019-01-01 中南大学 A kind of preparation method of the device for preparing ultra-thin carbon/carbon compound material panel and panel
CN109279908A (en) * 2018-10-30 2019-01-29 中南大学 A kind of fixture preparing ultra-thin carbon/carbon compound material panel
CN109111239B (en) * 2018-10-30 2021-11-16 中南大学 Device for preparing ultrathin carbon/carbon composite material panel and preparation method of panel

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