CN113292351B - Preparation method of quasi-isotropic carbon cloth needling carbon/carbon composite material - Google Patents
Preparation method of quasi-isotropic carbon cloth needling carbon/carbon composite material Download PDFInfo
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Abstract
The invention provides a preparation method of a quasi-isotropic carbon cloth needling carbon/carbon composite material, which comprises the following steps: (1) Selecting reinforcement fibers, laying the reinforcement fibers on a net tire to weave the reinforcement fibers into a reinforcement layer, layering the reinforcement layers layer by layer according to a set angle, and weaving the reinforcement layers into a fiber preform by adopting a needling technology; (2) carrying out chemical vapor deposition on the fiber preform; and (3) carrying out densification treatment on the carbon fiber preform. The material prepared by the method of the invention has more balanced mechanics and thermophysics in all directions of the plane, and the performance balance of each direction is improved to 1 compared with the prior carbon/carbon material by 0.3.
Description
Technical Field
The invention relates to a preparation method of a quasi-isotropic carbon/carbon composite material, which is mainly used for preparing parts with complex stress requirements.
Background
The hypersonic reentry accurate striking weapon which takes the distant accurate striking of the hypersonic reentry as the main technical characteristic becomes the world military hot spot, and brings a revolution to the future war concept and mode. Compared with the traditional weapon, the hypersonic weapon has great efficiency advantages, can effectively reduce defense response time, enhance the defense burst and defense resistance of the weapon, enlarge the range of a launching platform and improve the survivability, operational efficiency and efficiency of the weapon.
The space-based high-speed reentry precise striking aircraft flies in the atmosphere at a high speed and for a long time (more than 2000 s), the flying aircraft reenters at a high speed from hundreds of kilometers, and an abnormal harsh aerodynamic force/thermal load service environment is brought by the long-time hypersonic maneuvering flight in the atmosphere, and the large-area stagnation aerodynamic pressure at the front section of the aircraft body is gradually increased from 1.0kPa at the initial stage to 10kPa at the pressing stage and also needs to be subjected to airflow impact. In order to realize remote maneuvering flight and implement accurate striking and meet the requirement of lift-drag ratio to aerodynamic shape, a large-area heat-proof layer on the outer surface of an aircraft has the double functions of heat prevention and bearing, and the 'long-time heat prevention and bearing integrated heat-proof and heat insulation material technology' becomes a decisive factor for realizing the fighting function.
The carbon/carbon composite material has a series of excellent characteristics of good dimensional stability, strong designability and the like, particularly has outstanding advantages in the aspect of high-temperature specific strength, and is the best candidate material for accurately striking the ultra-high-temperature heat-proof structure of a near-space hypersonic weapon such as an aircraft and the like at high speed of a space base. According to the relevant data, similar hypersonic aircrafts under development in countries such as the United states and the Russia and the like also generally select carbon/carbon composite materials as thermal structural schemes. As a main material scheme of a thermal structure of a hypersonic aircraft, the performance level of the hypersonic aircraft directly determines a structural design scheme of the aircraft, the performance of a carbon/carbon composite material greatly depends on a carbon fiber reinforcement, and the mechanical performance of the carbon/carbon composite material is directly influenced by the structural form of the reinforcement. Because the existing material system has obvious anisotropic shape and cannot meet the requirement of uniform stress of the components in all directions, a quasi-isotropic carbon/carbon composite material suitable for the components with complex shapes needs to be further developed on the existing material system, and a key material technical support is provided for the development of a high-speed accurate hitting aircraft for the space-based flight.
Disclosure of Invention
The technical problem solved by the invention is as follows: the invention provides a method for preparing a quasi-isotropic carbon/carbon composite material by spreading a needle-punched preform at multiple angles by utilizing open fiber and widened high-performance carbon fiber/mesh tire unidirectional cloth, the prepared material is more balanced in mechanics and thermophysics in all directions of a plane, and the performance balance of each direction is improved to 1 compared with that of the existing carbon/carbon material by 0.3.
The technical scheme adopted by the invention is as follows: a preparation method of a quasi-isotropic carbon cloth needling carbon/carbon composite material comprises the following steps:
(1) Selecting reinforcement fibers to be laid on the net tire to be woven into a reinforcement layer, laminating layer by layer according to a set angle, and weaving into a fiber preform by adopting a needling technology;
(2) Carrying out chemical vapor deposition on the fiber preform;
the specific steps of the step (2) are as follows:
placing the fiber preform in a chemical vapor deposition furnace, firstly vacuumizing to below 40Pa, then heating to 900-1200 ℃, then mixing carbon source gas and argon gas, introducing into a furnace body, performing carbon deposition on the surface of the carbon fiber, stopping introducing the mixed gas after 2-5 h of deposition, vacuumizing to below 40Pa, cooling to below 100 ℃ along with the furnace, and taking the carbon fiber preform sample out of the furnace;
(3) The method comprises the following steps of:
placing the carbon fiber preform sample after being discharged and cooled in a pitch impregnation tank, firstly vacuumizing to 0 position of a vacuum gauge, then introducing molten pitch into the pitch impregnation tank, setting different impregnation pressure values in the pitch impregnation tank, and sequentially impregnating the carbon fiber preform for multiple times according to different impregnation pressure values to finally prepare the quasi-isotropic carbon cloth needling carbon/carbon composite material.
The method of each impregnation comprises the following steps: introducing a carbon source into the carbon fiber preform, then carbonizing the sample at the temperature rising rate of 50-100 ℃/h to 800 ℃, then raising the temperature to 2300-2500 ℃ at the temperature rising rate of 100-200 ℃/h, and finally cooling the sample to below 100 ℃ along with a furnace;
the reinforcing fiber is one or more of split and wide T300, T700, M40J, M50J, M60J, T700, T800 and T1000 carbon fiber.
The reinforced layer is one-way cloth formed by laying and applying the reinforced body fibers on the net tire according to different angles, the reinforced body fibers are woven into the one-way cloth, the one-way cloth selects a laying angle from 0 DEG every interval of alpha angles, and the prefabricated fabric is prepared by circularly laminating and needling; alpha ranges from 30 deg. to 45 deg..
The asphalt in the asphalt impregnation tank is medium-temperature coal asphalt.
Compared with the prior art, the invention has the technical effects that:
the invention provides a method for forming a quasi-isotropic carbon/carbon composite material, wherein a reinforcing layer of the prepared material is made of unidirectional cloth formed according to different angles, the unidirectional cloth is prepared into a prefabricated fabric by circularly laminating and needling a plurality of laying angles, the mechanical property and the thermophysical property of the unidirectional cloth are more balanced in each direction of a plane, the performance balance of each direction is improved to 1 compared with that of the existing carbon/carbon material, and the quasi-isotropic carbon/carbon composite material has a good application prospect in heat-proof parts such as large areas, side edges and the like of hypersonic aircrafts in China in future. The composite densification process adopted by the invention is an organic combination of low-pressure, medium-pressure and high-pressure impregnation and carbonization, and composite densification is carried out by adopting a targeted process according to the characteristics of pores at different stages.
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FIG. 1 is a flow chart of the preparation method of the present invention;
fig. 2 is a view of the unidirectional fabric of the present invention.
Detailed Description
The present invention will be described with reference to examples.
The invention provides a preparation method of a quasi-isotropic carbon cloth needling carbon/carbon composite material, which aims to improve the planar isotropic thermodynamic property balance of the carbon/carbon composite material.
The invention adopts split-fiber and widened high-performance carbon fiber (the tensile strength is more than or equal to 3.5GPa, the tensile modulus is more than or equal to 220 GPa)/net tire unidirectional cloth as a reinforcement, adopts the multi-angle laying and needling technology to prepare a prefabricated body, adopts Chemical Vapor Infiltration (CVI) to prepare an interface layer, and then combines the asphalt impregnation/carbonization, high-pressure impregnation/carbonization and other composite processes to complete later-stage densification, thereby manufacturing the quasi-isotropic carbon/carbon composite material.
As shown in fig. 1 and 2, a method for preparing a quasi-isotropic carbon cloth needle-punched carbon/carbon composite material comprises the following steps:
(1) Selecting reinforcement fibers to be laid on the net tire to be woven into a reinforcement layer, laminating layer by layer according to a set angle, and weaving into a fiber preform by adopting a needling technology;
(2) Carrying out chemical vapor deposition on the fiber preform;
the specific steps of the step (2) are as follows:
placing the fiber preform in a chemical vapor deposition furnace, firstly vacuumizing to below 40Pa, then heating to 900-1200 ℃, then mixing carbon source gas and argon gas, introducing into a furnace body, performing carbon deposition on the surface of the carbon fiber, stopping introducing the mixed gas after 2-5 h of deposition, vacuumizing to below 40Pa, cooling to below 100 ℃ along with the furnace, and taking the carbon fiber preform sample out of the furnace;
(3) The densification treatment of the carbon fiber preform comprises the following specific steps:
placing the carbon fiber preform sample after being discharged and cooled in a pitch impregnation tank, firstly vacuumizing to 0 position of a vacuum gauge, then introducing molten pitch into the pitch impregnation tank, setting different impregnation pressure values in the pitch impregnation tank, and sequentially impregnating the carbon fiber preform for multiple times according to different impregnation pressure values to finally prepare the quasi-isotropic carbon cloth needling carbon/carbon composite material.
The method of each impregnation comprises the following steps: introducing a carbon source into the carbon fiber preform, then carbonizing the sample at the temperature of 800 ℃ at the heating rate of 50-100 ℃/h, then heating at the temperature of 2300-2500 ℃ at the heating rate of 100-200 ℃/h, and finally cooling to the temperature below 100 ℃ along with a furnace and discharging the carbon fiber preform;
the reinforcing fiber is one or more of split and wide T300, T700, M40J, M50J, M60J, T700, T800 and T1000 carbon fiber.
The reinforcement layer is unidirectional cloth formed by laying and applying the reinforcement fibers on the net tire according to different angles, the unidirectional cloth is woven by the reinforcement fibers, a laying angle is selected from 0 DEG of the unidirectional cloth at every interval of alpha angles, and the prefabricated fabric is prepared by circularly laminating and needling; alpha ranges from 30 deg. to 45 deg..
The asphalt in the asphalt impregnating tank is medium-temperature coal asphalt.
Example 1
Selecting split and broadened T300 carbon fibers as a reinforcement, weaving into unidirectional cloth, and preparing a prefabricated fabric by circularly laminating and needling 0 degree, 30 degrees, 60 degrees, 90 degrees, 60 degrees and 30 degrees, then sequentially drying the fabric at 100 ℃ for 10 hours, pretreating at 1000 ℃ for 20 hours, and performing chemical vapor deposition on carbon source gas and argon at 950 ℃ according to the proportion of 1: introducing into a deposition furnace at a volume ratio of 0.5 for carbon deposition for 50h, impregnating pitch at normal pressure and medium pressure, carbonizing at normal pressure for 5 times, impregnating and carbonizing at high pressure (550 deg.C, 160MPa,10 hr), and heat treating at high temperature (1800 deg.C, 50 hr) for 6 times.
Finally, the quasi-isotropic carbon/carbon composite material is prepared, and the in-plane tensile strengths of 0 degree, 30 degrees, 60 degrees and 90 degrees are respectively 114MPa, 110MPa, 112MPa and 120MPa. Compared with carbon/carbon material with the same process, the mechanical property balance is improved by 60 percent.
Example 2
Selecting split and broadened T700 carbon fibers as a reinforcement, weaving into unidirectional cloth, and preparing a prefabricated fabric by circularly laminating and needling 0 degree, 30 degrees, 60 degrees, 90 degrees, 60 degrees and 30 degrees, then sequentially drying the fabric at 100 ℃ for 10 hours, pretreating at 1000 ℃ for 20 hours, and performing chemical vapor deposition on carbon source gas and argon at 950 ℃ according to the proportion of 1: introducing into a deposition furnace at a volume ratio of 0.5, performing carbon deposition for 50h, repeatedly impregnating pitch at normal pressure and medium pressure, carbonizing at normal pressure for 5 times, impregnating at high pressure for carbonization (550 deg.C, 160MPa,10 hr), and performing high temperature heat treatment (1800 deg.C, 50 hr) for 6 times.
Finally, the quasi-isotropic carbon/carbon composite material is prepared, and the in-plane tensile strengths of 0 degree, 30 degrees, 60 degrees and 90 degrees are respectively 125MPa, 115MPa, 120MPa and 130MPa. Compared with the carbon/carbon material with the same process, the mechanical property balance is improved by 58 percent.
Example 3
Selecting split and widened T700 carbon fibers as a reinforcement, weaving a unidirectional cloth, and preparing a prefabricated fabric by circularly laminating and needling 0 degrees, 45 degrees, 90 degrees and 45 degrees, then sequentially drying the fabric at 100 ℃ for 10 hours, pretreating the fabric at 1000 ℃ for 20 hours, and performing chemical vapor deposition to mix carbon source gas and argon gas at 950 ℃ according to the proportion of 1: introducing into a deposition furnace at a volume ratio of 0.5 for carbon deposition for 50h, impregnating pitch at normal pressure and medium pressure, carbonizing at normal pressure for 5 times, impregnating and carbonizing at high pressure (550 deg.C, 160MPa,10 hr), and heat treating at high temperature (1800 deg.C, 50 hr) for 6 times.
Finally, the quasi-isotropic carbon/carbon composite material is prepared, and the in-plane tensile strength of 0 degree, 45 degrees and 90 degrees is 150MPa, 125MPa and 160MPa respectively. Compared with the carbon/carbon material with the same process, the mechanical property balance is improved by 48 percent.
Example 4
Selecting split and widened T700 and M40J carbon fibers as a reinforcement, weaving a unidirectional cloth, preparing a prefabricated fabric by circularly laminating and needling 0 degree, 30 degrees, 60 degrees, 90 degrees, 60 degrees and 30 degrees, drying the fabric for 10 hours at 100 ℃, pretreating at high temperature of 1000 ℃ for 20 hours, and mixing carbon source gas and argon gas at 1000 ℃ according to the proportion of 1:1 for 50 hours, then impregnating pitch at normal pressure and medium pressure, carbonizing at normal pressure repeatedly for 5 times, then impregnating and carbonizing at high pressure (550 ℃, 160mpa,10 hours), and heat treating at high temperature (1800 ℃,50 hours) repeatedly for 6 times.
Finally, the quasi-isotropic carbon/carbon composite material is prepared, and the in-plane tensile strengths of 0 degree, 30 degrees, 60 degrees and 90 degrees are respectively 155MPa, 140MPa, 135MPa and 165MPa. Compared with the carbon/carbon material with the same process, the mechanical property balance is improved by 51 percent.
Example 5
Selecting split and broadened T800 carbon fibers as a reinforcement, weaving into unidirectional cloth, and preparing a prefabricated fabric by circularly laminating and needling 0 degree, 30 degrees, 60 degrees, 90 degrees, 60 degrees and 30 degrees, then sequentially drying the fabric at 100 ℃ for 10 hours, pretreating at 1000 ℃ for 20 hours, and performing chemical vapor deposition on carbon source gas and argon at 1000 ℃ according to the ratio of 1:1 for 50 hours, then impregnating pitch at normal pressure and medium pressure, carbonizing at normal pressure repeatedly for 5 times, then impregnating and carbonizing at high pressure (550 ℃, 160mpa,10 hours), and heat treating at high temperature (1800 ℃,50 hours) repeatedly for 6 times.
Finally, the quasi-isotropic carbon/carbon composite material is prepared, and the in-plane tensile strengths of 0 degree, 30 degrees, 60 degrees and 90 degrees are 135MPa, 120MPa, 125MPa and 138MPa respectively. Compared with the carbon/carbon material with the same process, the mechanical property balance is improved by 56 percent.
Those portions of the invention not described in detail are well within the skill of those in the art.
Claims (3)
1. A preparation method of a quasi-isotropic carbon cloth needling carbon/carbon composite material is characterized by comprising the following steps:
(1) Selecting reinforcement fibers to be laid on the net tire to be woven into a reinforcement layer, laminating layer by layer according to a set angle, and weaving into a fiber preform by adopting a needling technology;
(2) Carrying out chemical vapor deposition on the fiber preform;
the specific steps of the step (2) are as follows:
placing the fiber preform in a chemical vapor deposition furnace, firstly vacuumizing to below 40Pa, then heating to 900-1200 ℃, then mixing carbon source gas and argon gas, introducing into a furnace body, performing carbon deposition on the surface of the carbon fiber, stopping introducing the mixed gas after 2-5 h of deposition, vacuumizing to below 40Pa, cooling to below 100 ℃ along with the furnace, and taking the carbon fiber preform sample out of the furnace;
(3) Carrying out densification treatment on the carbon fiber preform to prepare a quasi-isotropic carbon cloth needling carbon/carbon composite material;
the specific steps of the step (3) are as follows:
placing the carbon fiber preform sample after being discharged and cooled in a pitch impregnation tank, firstly vacuumizing to 0 position of a vacuum gauge, then introducing molten pitch into the pitch impregnation tank, setting different impregnation pressure values in the pitch impregnation tank, and sequentially impregnating the carbon fiber preform for multiple times according to the different impregnation pressure values to finally prepare the quasi-isotropic carbon cloth needling carbon/carbon composite material; the asphalt in the asphalt impregnation tank is medium-temperature coal asphalt;
in the step (3), the method for dipping each time comprises the following steps: introducing a carbon source into the carbon fiber preform, then carbonizing the sample at the temperature rising rate of 50-100 ℃/h to 800 ℃, then raising the temperature at the temperature rising rate of 100-200 ℃/h to 2300-2500 ℃, and finally cooling the sample to below 100 ℃ along with the furnace and discharging the sample.
2. The method for preparing a quasi-isotropic carbon cloth needle-punched carbon/carbon composite material as claimed in claim 1, wherein: the reinforcing body fiber is one or more of split and wide T300, T700, M40J, M50J, M60J, T800 and T1000 carbon fiber.
3. The method for preparing a quasi-isotropic carbon cloth needle-punched carbon/carbon composite material according to claim 1 or 2, wherein: the reinforced layer is one-way cloth formed by laying and applying the reinforced body fibers on the net tire according to different angles, the reinforced body fibers are woven into the one-way cloth, the one-way cloth selects a laying angle from 0 DEG every interval of alpha angles, and the prefabricated fabric is prepared by circularly laminating and needling; alpha ranges from 30 deg. to 45 deg..
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| US5061414A (en) * | 1989-09-05 | 1991-10-29 | Engle Glen B | Method of making carbon-carbon composites |
| WO2009024045A1 (en) * | 2007-08-21 | 2009-02-26 | Hunan Kingbo Carbon-Carbon Composites Co. Ltd | A c/c composite crucible and a producing method thereof |
| CN104692823B (en) * | 2015-02-28 | 2017-07-04 | 中南大学 | A kind of pantograph preparation method of C/C composite draw runners |
| CN108314458B (en) * | 2018-02-09 | 2020-07-21 | 陕西天策新材料科技有限公司 | Preparation method of high-thermal-conductivity carbon/carbon composite material |
| CN109809828A (en) * | 2019-02-26 | 2019-05-28 | 航天材料及工艺研究所 | A kind of preparation method of the balanced thermally conductive carbon/carbon compound material of three-dimensional |
| CN110156485A (en) * | 2019-05-28 | 2019-08-23 | 中国科学院金属研究所 | A kind of method of short cycle, low cost preparation high-performance carbon/carbon compound material |
| CN111635242A (en) * | 2020-06-09 | 2020-09-08 | 中南大学 | Rapid preparation method and application of high-density revolving body carbon/carbon composite material |
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