CN108840697B - Carbon/carbon composite material honeycomb and preparation method thereof - Google Patents
Carbon/carbon composite material honeycomb and preparation method thereof Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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- C04B35/83—Carbon fibres in a carbon matrix
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
A carbon/carbon composite material honeycomb and a preparation method thereof belong to the technical field of carbon/carbon composite materials. The carbon/carbon composite material honeycomb comprises a carbon fiber reinforcement body and a carbon matrix covering the surface of the carbon fiber reinforcement body, wherein the carbon fiber reinforcement body is of a honeycomb structure, continuous carbon fibers are arranged in the L direction and continuous carbon fibers are arranged in the W direction of the honeycomb structure. The carbon/carbon composite material honeycomb has excellent thermal stability and mechanical property, and meets the lightweight requirement in the aerospace field; the main performance parameters of the honeycomb meet the conditions that the flat compression strength is more than or equal to 8MPa, the flat compression modulus is more than or equal to 900MPa, the L-direction shear strength is more than or equal to 6.7MPa, the L-direction shear modulus is more than or equal to 1500MPa, the W-direction shear strength is more than or equal to 4.5MPa, the W-direction shear modulus is more than or equal to 730MPa, and the thermal expansion coefficient is 0-0.2 multiplied by 10‑6/K。
Description
Technical Field
The patent relates to a high accuracy is whole carbon/carbon composite material honeycomb of low density, high stability, high strength for observation platform belongs to carbon/carbon composite material technical field.
Background
The traditional composite material for the spacecraft structure generally only requires high specific strength, high specific modulus and the like, and has low requirement on the dimensional stability. However, in the field of development of composite material structures for high-precision spacecrafts such as satellites and the like, composite materials with the characteristics of high stability, light weight, high strength and the like are an important development direction. Advanced countries have started to research zero-expansion and high-stability composite material structures for spacecraft, and the composite material structures are mainly used for optical instrument supporting structures such as space telescopes and the like, gravity gradiometer supporting bases, antenna reflecting panels and the like. In order to ensure the working accuracy of high-accuracy optical instruments and detection equipment on the spacecraft, a light composite material structure platform with high stability and high strength must be provided for the spacecraft.
In the prior art, carbon/carbon composite material blocks, carbon/silicon carbide composite material blocks or carbon fiber reinforced resin-based honeycombs are generally used as a support structure of a precision instrument in the domestic aerospace field so as to keep good stability; the carbon/carbon composite material block or the carbon/silicon carbide composite material block is of a solid structure, so that the lightweight requirement of the aerospace field is not facilitated; the carbon fiber reinforced resin-based honeycomb thermal expansion system is about 10-4Magnitude, poor thermal stability.
Disclosure of Invention
In order to solve the problems in the prior art, the embodiment of the invention provides a carbon/carbon composite material honeycomb and a preparation method thereof, wherein the carbon/carbon composite material honeycomb has excellent thermal stability and mechanical property and meets the lightweight requirement in the aerospace field.
In order to achieve the above purpose, the invention provides the following technical scheme:
a carbon/carbon composite material honeycomb comprises a carbon fiber reinforcement body and a carbon matrix covering the surface of the carbon fiber reinforcement body, wherein the carbon fiber reinforcement body is of a honeycomb structure, and continuous carbon fibers are arranged in the L direction and continuous carbon fibers are also arranged in the W direction of the honeycomb structure.
In an alternative embodiment, the carbon fiber reinforcement is made of one or more of T300-1K, T300-3K, T300-6K, T300-12K, T700-6K, T700-12K, T800-6K or T800-12K polyacrylonitrile-based carbon fibers.
In an alternative embodiment, the carbon fiber reinforcement has continuous fibers oriented at 30-60 ° on the honeycomb walls.
In an optional embodiment, the length of the core grid side of the honeycomb is 2.75 mm-15 mm, and the thickness of the honeycomb wall is 0.17 mm-2 mm.
In an alternative embodiment, the carbon/carbon composite honeycomb density is 100kg/m3～220kg/m3。
A preparation method of a carbon/carbon composite material honeycomb comprises the following steps:
step 1, preparing a carbon fiber reinforcement body with a honeycomb structure, wherein continuous carbon fibers are arranged in the L direction and continuous carbon fibers are also arranged in the W direction of the honeycomb structure;
step 2, impregnating and curing the carbon fiber reinforcement with the honeycomb structure by adopting phenolic resin to obtain a cured dimensional carbon fiber reinforcement;
and 3, carbonizing and densifying the cured dimensional carbon fiber reinforcement to obtain the carbon/carbon composite material honeycomb.
In an alternative embodiment, before the carbonizing treatment of the carbon fiber reinforcement in the cured dimensional form in step 3, the method further includes:
and a core mold is inserted into the honeycomb core grid of the curing dimensional carbon fiber reinforcement, and an airflow channel extending along the thickness direction of the honeycomb is arranged on the side wall of the core mold.
In an alternative embodiment, the airflow channels are arranged on six side walls of each core mold, and the width of the position where the airflow channels are connected with the carbon fiber reinforcement of the curing dimensional form is 60-80% of the width of the side wall of the core mold, and the depth of the airflow channels is 20-30% of the distance between two opposite side walls of the core mold.
In an optional embodiment, the phenolic resin in the step 2 is phenolic resin diluted by a volatile organic solvent, wherein the mass percentage of the volatile organic solvent is 10-50%
In an alternative embodiment, the carbonizing of step 3 includes:
the temperature is maintained at 280-320 ℃ for 1.5-3 h, then at 540-560 ℃ for 1.5-3 h, and then at 800-900 ℃ for 2-4h, and then the temperature is reduced to room temperature.
In an optional embodiment, the temperature is increased to 180-220 ℃ at a temperature increase rate of 40-60 ℃/h, to 280-320 ℃ at a temperature increase rate of 5-15 ℃/h, to 540-560 ℃ at a temperature increase rate of 5-10 ℃/h, and to 640-660 ℃ at a temperature increase rate of 5-10 ℃/h; heating to 800-900 ℃ at a heating rate of 10-20 ℃/h, and cooling to room temperature at a cooling rate of not more than 100 ℃/h. In an alternative embodiment, the densification process of step 3 includes:
performing densification treatment by chemical vapor deposition, wherein the carbon source gas is one or more of methane, propylene or propane, the aeration rate is 5-50L/min, the pressure is 0.6-0.7 kPa, and the deposition time is 100-400 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the carbon/carbon composite material honeycomb provided by the embodiment of the invention, continuous carbon fibers are arranged in the L direction and the W direction of the carbon fiber reinforcement, so that the carbon/carbon composite material honeycomb is not easy to delaminate and crack in the carbonization and densification processes, the densification process has excellent adaptability, and the prepared carbon/carbon composite material honeycomb has excellent thermal stability and mechanical property and meets the lightweight requirement in the aerospace field;
(2) the main performance parameters of the honeycomb meet the conditions that the flat compression strength is more than or equal to 8MPa, the flat compression modulus is more than or equal to 900MPa, the L-direction shear strength is more than or equal to 6.7MPa, the L-direction shear modulus is more than or equal to 1500MPa, the W-direction shear strength is more than or equal to 4.5MPa, the W-direction shear modulus is more than or equal to 730MPa, and the thermal expansion coefficient is 0-0.2 multiplied by 10-6/K；
(3) The densification is carried out by adopting a chemical vapor deposition process, so that the near-size efficient densification of the honeycomb is ensured;
(4) the carbon/carbon honeycomb densification process flow is simple, the densification period is short, and the engineered application is easy to realize.
Drawings
Fig. 1 is an appearance diagram of a carbon/carbon composite honeycomb according to an embodiment of the present invention;
FIG. 2 is a schematic view of a manner of bonding two carbon cloths when a carbon fiber reinforcement is prepared using the carbon cloths according to an embodiment of the present invention;
fig. 3 is a schematic structural view of a graphite core mold for densification according to an embodiment of the present invention.
Detailed Description
The following further explains embodiments of the present invention with reference to specific examples.
As shown in fig. 1, an embodiment of the present invention provides a carbon/carbon composite honeycomb, including a carbon fiber reinforcement and a carbon matrix covering a surface of the carbon fiber reinforcement, where the carbon fiber reinforcement is a honeycomb structure, and an L direction of the honeycomb structure has continuous carbon fibers, and a W direction of the honeycomb structure also has continuous carbon fibers.
Specifically, in the embodiment of the invention, the carbon fiber reinforcement honeycomb structure can be provided with continuous fibers in the L direction and the W direction in a splicing and sewing manner through carbon cloth, wherein the L direction is the continuous fibers in a cloth layer, and the W direction is the sewing fibers between the cloth layers, specifically, as shown in fig. 2, the carbon cloth is cut into a preset shape according to the honeycomb design size and marked at the position needing sewing, then adjacent carbon cloths are butted, and the butted surfaces are sewn through a sewing line;
according to the carbon/carbon composite material honeycomb provided by the embodiment of the invention, continuous carbon fibers are arranged in the L direction and the W direction of the carbon fiber reinforcement, so that the carbon fibers serving as a carbon/carbon honeycomb framework are ensured to have continuity in all directions in the honeycomb, external loads acting on the carbon/carbon honeycomb can be efficiently transferred among different honeycomb core cells through the continuous fibers, and the mechanical property of the carbon/carbon honeycomb is fully improved; the carbon/carbon composite material honeycomb provided by the embodiment of the invention has excellent thermal stability and mechanical property, and meets the lightweight requirement in the aerospace field; the carbon/carbon composite material honeycomb is not easy to delaminate and crack in the carbonization and densification processes, and the densification process is suitableThe performance is excellent; the main performance parameters of the honeycomb meet the conditions that the flat compression strength is more than or equal to 8MPa, the flat compression modulus is more than or equal to 900MPa, the L-direction shear strength is more than or equal to 6.7MPa, the L-direction shear modulus is more than or equal to 1500MPa, the W-direction shear strength is more than or equal to 4.5MPa, the W-direction shear modulus is more than or equal to 730MPa, and the thermal expansion coefficient is 0-0.2 multiplied by 10-6/K。
In an alternative embodiment, the carbon fiber reinforcement is preferably made of one or more of T300-1K, T300-3K, T300-6K, T300-12K, T700-6K, T700-12K, T800-6K or T800-12K polyacrylonitrile-based carbon fibers.
In an alternative embodiment, the carbon fiber reinforcement has continuous fibers oriented at 30-60 degrees on the honeycomb walls to ensure that the carbon/carbon honeycomb has strong shear resistance.
In an optional embodiment, the side length of the core lattice of the honeycomb is 2.75 mm-15 mm, the thickness of the honeycomb wall is 0.17 mm-2 mm, and by optimizing the side length and the wall thickness of different honeycomb core lattices, the honeycomb is ensured to have higher specific strength, the honeycomb wall is ensured to be smooth and flat, and carbon deposition generated in the densification process or the honeycomb wall damaged by demolding due to the unsmooth honeycomb wall is avoided.
In an alternative embodiment, the carbon/carbon composite honeycomb has a density of 100kg/m3～220kg/m3And the carbon/carbon honeycomb can meet the requirement of mechanical property index while meeting the lightweight design.
The embodiment of the invention also provides a preparation method of the carbon/carbon composite material honeycomb, which comprises the following steps:
step 1, preparing a carbon fiber reinforcement body with a honeycomb structure, wherein continuous carbon fibers are arranged in the L direction and continuous carbon fibers are also arranged in the W direction of the honeycomb structure;
specifically, in the embodiment of the present invention, continuous fibers are provided in both the L direction and the W direction of the carbon fiber reinforced honeycomb structure by splicing and sewing carbon cloth, specifically, as shown in fig. 2, the carbon cloth m is cut into a predetermined shape according to the honeycomb design size and marked at the position to be sewn, then the two carbon cloths m are attached and butted, the butted surface is sewn by a sewing thread n, after sewing, when a core mold is inserted at the position where the core mold is not sewn, and after the fiber shape is cured, the core mold is removed from the mold, so that the honeycomb structure shown in fig. 2 can be obtained;
the carbon matrix comprises resin carbon formed by carbonizing a resin and pyrolytic carbon formed by densification treatment (chemical vapor deposition).
Step 2, impregnating and curing the carbon fiber reinforcement with the honeycomb structure by adopting phenolic resin to obtain a cured dimensional carbon fiber reinforcement;
specifically, in the embodiment of the present invention, the phenolic resin in step 2 is phenolic resin diluted by volatile organic solvents such as ethanol, ethyl acetate, methanol, acetone, and the like, wherein the mass percentage of the volatile organic solvents is 10% to 50%; curing in the step 2, preferably heating to 60-80 ℃ at a heating rate of 20-40 ℃/h, and keeping the temperature for 1-3 h; heating to 90-110 ℃ at a heating rate of 5-20 ℃/h, and keeping the temperature for 0.5-2 h; heating to 120-130 ℃ at a heating rate of 5-20 ℃/h, and keeping the temperature for 0.5-2 h; heating to 150-170 ℃ at a heating rate of 5-20 ℃/h, and preserving heat for 5-7 h; cooling to below 80 ℃ at a cooling rate of less than or equal to 25 ℃/h, and then freely cooling;
and 3, carbonizing and densifying the cured dimensional carbon fiber reinforcement to obtain the carbon/carbon composite material honeycomb.
In an alternative embodiment, before the carbonizing treatment of the carbon fiber reinforcement in the cured dimensional form in step 3, the method further includes:
and a core mold is inserted into the honeycomb core grid of the curing dimensional carbon fiber reinforcement, and an airflow channel extending along the thickness direction d of the honeycomb is arranged on the side wall of the core mold. By arranging the gas flow channel, the carbon source gas can smoothly enter the honeycomb, and the efficient and uniform densification of the honeycomb wall is realized.
In an alternative embodiment, as shown in fig. 3, the air flow channels are formed in six side walls of each mandrel, and the air flow channels are connected with the carbon fiber reinforcement of the curing dimensional form at positions having a width a of 60-80% of the width of the side wall of the mandrel and a depth b of 20-30% of the distance between the two opposite side walls of the mandrel. The size of the airflow channel is controlled to ensure the flow of the carbon source gas entering the airflow channel, and meanwhile, the contact area of the honeycomb wall and the outer surface of the core mold is reduced as much as possible, so that the demolding after densification is facilitated, and the demolding damage to the honeycomb wall is reduced.
In an alternative embodiment, the carbonizing of step 3 includes: heating to 180-220 ℃ at a heating rate of 40-60 ℃/h; heating to 280-320 ℃ at a heating rate of 5-15 ℃/h, and preserving heat for 1.5-3 h; heating to 540-560 ℃ at a heating rate of 5-10 ℃/h, and preserving heat for 1.5-3 h; heating to 640-660 ℃ at a heating rate of 5-10 ℃/h; heating to 800-900 ℃ at a heating rate of 10-20 ℃/h, and preserving heat for 1.5-3 h to finish resin carbonization. Through the carbonization process, the temperature rise rate in the middle period is low, the deformation internal stress of the honeycomb in the carbonization process can be reduced, and the near-size forming of the honeycomb is ensured. In an alternative embodiment, the densification process of step 3 includes: after the carbonization process is completed in the deposition furnace, directly heating to 900-1000 ℃ from the highest temperature of the carbonization process at a heating rate of 10-20 ℃/h, preserving heat for 1-3 h, introducing a carbon source gas, wherein the gas flow is 5-50L/min, the pressure in a hearth is 0.6-0.7 kPa, and the deposition time is 100-400h, so as to ensure the near-size efficient densification of the honeycomb.
In this embodiment, the carbon/carbon composite material honeycomb in the honeycomb embodiment may be prepared, and for specific description of the carbon/carbon composite material honeycomb, reference is made to the honeycomb embodiment, and details are not repeated here.
The following are several specific embodiments of the invention:
example 1
The embodiment provides a carbon/carbon composite material honeycomb for a satellite, which has the overall dimension of 200mm multiplied by 80mm, the side length of a honeycomb core grid of 5mm and the wall thickness of the honeycomb of 0.8mm, and the preparation method comprises the following steps:
1) universal grade T300-3K polyacrylonitrile-based carbon fiber is selected to weave into the material with the surface density of 240g/cm3Plain carbon cloth with 6 warp and weft threads/cm multiplied by 6 threads/cm. Then cutting the carbon cloth into carbon cloth blocks with certain specifications according to the expansion size of the honeycomb wall for later use; in the cutting process, the warp yarn direction is 0 degree, the carbon cloth is rotated anticlockwise to form +45 degrees, and the carbon cloth is rotated clockwise to form-45 degrees.
2) Laminating the carbon cloth blocks in the step 1) according to a designed layering sequence, and arranging adjacent carbon cloth according to a +45/-45 layering sequence; sewing the carbon cloth pairwise, wherein the sewing distance in the thickness direction of the honeycomb is 4mm, the sewing distance in the L direction of the honeycomb is 5mm, the sewing line is T300-1K carbon fiber, and the diameter of the sewing yarn-leading tool is 1.3 mm; after the carbon cloth is sewn and stacked to the number of layers required by the design of the honeycomb product, inserting a hexagonal metal impregnation-solidification tool and impregnating a phenolic resin solution with the mass content of ethanol being 20%; and (3) demolding after heating and curing to form the carbon fiber reinforcement, wherein the resin curing temperature rising system is as follows: the room temperature is between 80 ℃ and 25 ℃/h; keeping the temperature at 80 ℃ for 2 h; 10 ℃/h at the temperature of 80-100 ℃; keeping the temperature at 100 ℃ for 1 h; 10 ℃/h at 100-120 ℃; preserving heat for 1h at 120 ℃; 120-160 ℃ and 10 ℃/h; keeping the temperature at 160 ℃ for 6 h; 160-70 ℃ and less than or equal to 25 ℃/h; and (5) freely cooling at 70-room temperature.
3) Preparing a full-carbon deformation-preventing densification tool according to the curing dimensional carbon fiber reinforcement prepared in the step 2), wherein the tool consists of a graphite core mold and a clamping plate. The graphite core mold is of a prism structure, grooves 1 are machined in all side walls to form airflow channels, the cross section of the graphite core mold is of a hexagonal structure as shown in figure 3, the width a of the position where the grooves 1 are connected with the carbon fiber reinforcement of the curing dimensional type is 3mm, and the depth b of the grooves is 2 mm.
4) Assembling the full-carbon tool in the step 3) on the curing dimensional carbon fiber reinforcement in the step 2), and vertically placing the curing dimensional carbon fiber reinforcement with the tool in a cylindrical vertical deposition furnace; heating the deposition furnace at 50 deg.c/h to 200 deg.c; 200-300 ℃ and 10 ℃/h; keeping the temperature at 300 ℃ for 2 h; 300-550 ℃ and 5 ℃/h; preserving heat for 2 hours at 550 ℃; 550-650 ℃ and 10 ℃/h; 650-850 ℃ and 15 ℃/h; keeping the temperature at 850 ℃ for 2h to finish resin carbonization; continuously heating to 850-930 ℃ at 15 ℃/h; keeping the temperature at 930 ℃ for 2 h; feeding propylene at the beginning, wherein the gas flow is 20L/min, the pressure in the hearth is kept at 0.6-0.7 kPa, and the deposition time is 200 h; after deposition was completed, the aeration was stopped. 930 deg.c to room temperature and free cooling.
6) Disassembling the all-carbon tool in the step 4), and processing the honeycomb to a preset size to obtain a final product.
By the process method, the carbon with the magnitude of 200mm is realizedThe carbon honeycomb is densified to the density of 0.19g/cm by chemical vapor deposition for 200h3Taking five subsamples from different positions, the density deviation being. + -. 0.003g/cm3(ii) a The flat compression strength is 10.28MPa, the flat compression modulus is 1052MPa, the L-direction shear strength is 6.79MPa, the L-direction shear modulus is 1670MPa, the W-direction shear strength is 5.26MPa, the W-direction shear modulus is 831MPa, and the thermal expansion coefficient is 0.18 multiplied by 10-6K; the thickness of the honeycomb wall is 0.78 mm-0.82 mm, and carbon deposition does not exist on the surface of the honeycomb wall; the distance between the opposite sides of 10 honeycomb core grids is randomly measured to be 8.63 mm-8.71 mm, and the deformation control effect of the core grids is good.
Example 2
The embodiment provides a carbon/carbon composite material honeycomb with the overall size of 400mm multiplied by 80mm, the side length of a honeycomb core grid of 5mm and the wall thickness of the honeycomb of 0.8mm, and the preparation method comprises the following steps:
1) universal grade T300-3K polyacrylonitrile-based carbon fiber is selected to weave into the material with the surface density of 240g/cm3Plain carbon cloth with 6 warp and weft threads/cm multiplied by 6 threads/cm. Then cutting the carbon cloth into carbon cloth blocks with certain specifications according to the expansion size of the honeycomb wall for later use; in the cutting process, the warp yarn direction is 0 degree, the carbon cloth is rotated anticlockwise to form +45 degrees, and the carbon cloth is rotated clockwise to form-45 degrees.
2) Laminating the carbon cloth blocks in the step 1) according to a designed layering sequence, and arranging adjacent carbon cloth according to a +45/-45 layering sequence; sewing the carbon cloth pairwise, wherein the sewing distance in the thickness direction of the honeycomb is 4mm, the sewing distance in the L direction of the honeycomb is 5mm, the sewing line is T300-1K carbon fiber, and the diameter of the sewing yarn-leading tool is 1.3 mm; after the carbon cloth is sewn and stacked to the number of layers required by the design of the honeycomb product, inserting a hexagonal metal impregnation-solidification tool and impregnating a phenolic resin solution with the mass content of ethanol being 20%; and (3) demolding after heating and curing to form the carbon fiber reinforcement, wherein the resin curing temperature rising system is as follows: the room temperature is between 80 ℃ and 25 ℃/h; keeping the temperature at 80 ℃ for 2 h; 10 ℃/h at the temperature of 80-100 ℃; keeping the temperature at 100 ℃ for 1 h; 10 ℃/h at 100-120 ℃; preserving heat for 1h at 120 ℃; 120-160 ℃ and 10 ℃/h; keeping the temperature at 160 ℃ for 6 h; 160-70 ℃ and less than or equal to 25 ℃/h; and (5) freely cooling at 70-room temperature.
3) Preparing a full-carbon deformation-preventing densification tool according to the curing dimensional carbon fiber reinforcement prepared in the step 2), wherein the tool consists of a graphite core mold and a clamping plate. The graphite core is in a prism structure, grooves 1 are machined in all side walls to form airflow channels, the cross section of the graphite core is in a hexagonal structure as shown in figure 3, the width a of the position where the grooves 1 are connected with the curing dimensional carbon fiber reinforcement is 3mm, and the depth b of the grooves is 2 mm.
4) Assembling the full-carbon tool in the step 3) on the curing dimensional carbon fiber reinforcement in the step 2), and vertically placing the curing dimensional carbon fiber reinforcement with the tool in a cylindrical vertical deposition furnace; heating the deposition furnace at 50 deg.c/h to 200 deg.c; 200-300 ℃ and 10 ℃/h; keeping the temperature at 300 ℃ for 2 h; 300-550 ℃ and 5 ℃/h; preserving heat for 2 hours at 550 ℃; 550-650 ℃ and 10 ℃/h; 650-850 ℃ and 15 ℃/h; keeping the temperature at 850 ℃ for 2h to finish resin carbonization; continuously heating to 850-930 ℃ at 15 ℃/h; keeping the temperature at 930 ℃ for 2 h; feeding propylene at the beginning, wherein the gas flow is 20L/min, the pressure in the hearth is kept at 0.6-0.7 kPa, and the deposition time is 200 h; after deposition was completed, the aeration was stopped. 930 deg.c to room temperature and free cooling.
6) Disassembling the all-carbon tool in the step 4), and processing the honeycomb to a preset size to obtain a final product.
By the process method, the densification of the 400 mm-magnitude carbon/carbon honeycomb to the density of 0.185g/cm through 200h chemical vapor deposition is realized3Taking five subsamples from different positions, the density deviation is + -0.005 g/cm3(ii) a The flat compression strength is 10.03MPa, the flat compression modulus is 1027MPa, the L-direction shear strength is 6.55MPa, the L-direction shear modulus is 1606MPa, the W-direction shear strength is 5.01MPa, the W-direction shear modulus is 798MPa, and the thermal expansion coefficient is 0.18 multiplied by 10-6K; the thickness of the honeycomb wall is 0.79 mm-0.83 mm, and no carbon deposition exists on the surface of the honeycomb wall; the distance between the opposite sides of 10 honeycomb core grids is randomly measured to be 8.58 mm-8.64 mm, and the deformation control effect of the core grids is good. Meanwhile, the performance of the size-order honeycomb is similar to that of a 200mm honeycomb, and the carbon/carbon honeycomb and the preparation method thereof are good in stability.
Example 3
The embodiment provides a carbon/carbon composite material honeycomb with the overall size of 400mm multiplied by 50mm, the side length of a honeycomb core grid of 4mm and the wall thickness of the honeycomb of 0.3mm, and the preparation method comprises the following steps:
1) universal grade T700-12K polyacrylonitrile-based carbon fiber is selected to weave into the material with the surface density of 200g/cm3And (5) widening the cloth, wherein the fiber unfolding width is 8 mm. Then cutting the carbon cloth into carbon cloth blocks with certain specifications according to the expansion size of the honeycomb wall for later use; in the cutting process, the warp yarn direction is 0 degree, the carbon cloth is rotated anticlockwise to form +45 degrees, and the carbon cloth is rotated clockwise to form-45 degrees.
2) Laminating the carbon cloth blocks in the step 1) according to a designed layering sequence, and arranging adjacent carbon cloth according to a +45/-45 layering sequence; sewing the carbon cloth pairwise, wherein the sewing distance in the thickness direction of the honeycomb is 3mm, the sewing distance in the L direction of the honeycomb is 4mm, the sewing line is T300-1K carbon fiber, and the diameter of the sewing yarn guiding tool is 1.3 mm; after the carbon cloth is sewn and stacked to the number of layers required by the design of the honeycomb product, inserting a hexagonal metal impregnation-solidification tool and impregnating a phenolic resin solution with the mass content of ethanol being 15%; and (3) demolding after heating and curing to form the carbon fiber reinforcement, wherein the resin curing temperature rising system is as follows: the room temperature is between 80 ℃ and 25 ℃/h; keeping the temperature at 80 ℃ for 2 h; 10 ℃/h at the temperature of 80-100 ℃; keeping the temperature at 100 ℃ for 1 h; 10 ℃/h at 100-120 ℃; preserving heat for 1h at 120 ℃; 120-160 ℃ and 10 ℃/h; keeping the temperature at 160 ℃ for 6 h; 160-70 ℃ and less than or equal to 25 ℃/h; and (5) freely cooling at 70-room temperature.
3) Preparing a full-carbon deformation-preventing densification tool according to the curing dimensional carbon fiber reinforcement prepared in the step 2), wherein the tool consists of a graphite core mold and a clamping plate. The graphite core is in a prism structure, grooves 1 are machined in all side walls to form airflow channels, the cross section of the graphite core is in a hexagonal structure as shown in figure 3, the width a of the position where the grooves 1 are connected with the curing dimensional carbon fiber reinforcement is 2.5mm, and the depth b of the grooves is 1.5 mm.
4) Assembling the full-carbon tool in the step 3) on the curing dimensional carbon fiber reinforcement in the step 2), and vertically placing the curing dimensional carbon fiber reinforcement with the tool in a cylindrical vertical deposition furnace; heating the deposition furnace at 50 deg.c/h to 200 deg.c; 200-300 ℃ and 10 ℃/h; keeping the temperature at 300 ℃ for 2 h; 300-550 ℃ and 5 ℃/h; preserving heat for 2 hours at 550 ℃; 550-650 ℃ and 10 ℃/h; 650-850 ℃ and 15 ℃/h; keeping the temperature at 850 ℃ for 2h to finish resin carbonization; continuously heating to 850-930 ℃ at 15 ℃/h; keeping the temperature at 930 ℃ for 2 h; feeding propylene at the beginning, wherein the gas flow is 20L/min, the pressure in the hearth is kept at 0.6-0.7 kPa, and the deposition time is 300 h; after deposition was completed, the aeration was stopped. 930 deg.c to room temperature and free cooling.
6) Disassembling the all-carbon tool in the step 4), and processing the honeycomb to a preset size to obtain a final product.
By the process method, the densification of the 400 mm-magnitude carbon/carbon honeycomb to the density of 0.18g/cm through 300h chemical vapor deposition is realized3Taking five subsamples from different positions, the density deviation is + -0.005 g/cm3(ii) a The flat compression strength is 8.93MPa, the flat compression modulus is 967MPa, the L-direction shear strength is 6.32MPa, the L-direction shear modulus is 1583MPa, the W-direction shear strength is 4.89MPa, the W-direction shear modulus is 795MPa, and the thermal expansion coefficient is 0.16 multiplied by 10-6K; the thickness of the honeycomb wall is 0.29 mm-0.33 mm, and no carbon deposition exists on the surface of the honeycomb wall; the distance between the opposite sides of 10 honeycomb core grids is measured at random to be 6.90 mm-7.05 mm, and the deformation control effect of the core grids is good.
Those skilled in the art will appreciate that the invention may be practiced without these specific details.
Claims (1)
1. A preparation method of a carbon/carbon composite material honeycomb for a high-precision observation platform is characterized by comprising the following steps: the carbon/carbon composite material honeycomb is a carbon/carbon composite material honeycomb for a satellite, the outline dimension of which is 200mm multiplied by 80mm, the side length of a honeycomb core grid is 5mm, and the wall thickness of the honeycomb is 0.8mm, and the steps comprise:
1) universal grade T300-3K polyacrylonitrile-based carbon fiber is selected to weave into the material with the surface density of 240g/cm3Plain carbon cloth with the warp and weft density of 6 pieces/cm multiplied by 6 pieces/cm is cut into carbon cloth blocks with set specifications for later use according to the expansion size of the honeycomb wall; in the cutting process, the warp direction is 0 degree, the carbon cloth is rotated anticlockwise to form +45 degrees, and the carbon cloth is rotated clockwise to form-45 degrees;
2) laminating the carbon cloth blocks in the step 1) according to a designed layering sequence, and arranging adjacent carbon cloth according to a +45 DEG/45 DEG layering sequence; sewing the carbon cloth pairwise, wherein the sewing distance in the thickness direction of the honeycomb is 4mm, the sewing distance in the L direction of the honeycomb is 5mm, the sewing line is T300-1K carbon fiber, and the diameter of the sewing yarn-leading tool is 1.3 mm; after the carbon cloth is sewn and stacked to the number of layers required by the design of the honeycomb product, inserting a hexagonal metal impregnation-solidification tool and impregnating a phenolic resin solution with the mass content of ethanol being 20%; and (3) demolding after heating and curing to form the carbon fiber reinforcement, wherein the resin curing temperature rising system is as follows: the temperature is between room temperature and 80 ℃, and the speed is 25 ℃/h; keeping the temperature at 80 ℃ for 2 h; 10 ℃/h at the temperature of 80-100 ℃; keeping the temperature at 100 ℃ for 1 h; 10 ℃/h at the temperature of 100-120 ℃; preserving heat for 1h at 120 ℃; at the temperature of 120-160 ℃, 10 ℃/h; keeping the temperature at 160 ℃ for 6 h; 160-70 ℃ and less than or equal to 25 ℃/h; freely cooling at 70-room temperature;
3) preparing a full-carbon deformation-preventing densification tool according to the curing dimensional carbon fiber reinforcement prepared in the step 2), wherein the tool comprises a graphite core mold and a clamping plate, the graphite core mold is of a prism structure, grooves are processed on each side wall to form an airflow channel, the cross section of the graphite core mold is of a hexagonal structure, the width a of the position where the grooves are connected with the curing dimensional carbon fiber reinforcement is 3mm, and the depth b of the grooves is 2 mm;
4) assembling the full-carbon tool in the step 3) on the curing dimensional carbon fiber reinforcement in the step 2), and vertically placing the curing dimensional carbon fiber reinforcement with the tool in a cylindrical vertical deposition furnace; heating the deposition furnace at 50 ℃/h with a heating curve of room temperature-200 ℃; the temperature is 200-300 ℃, and the temperature is 10 ℃/h; keeping the temperature at 300 ℃ for 2 h; at the temperature of 300-550 ℃, 5 ℃/h; preserving heat for 2 hours at 550 ℃; 550-650 ℃, 10 ℃/h; at the temperature of 650-850 ℃, 15 ℃/h; keeping the temperature at 850 ℃ for 2h to finish resin carbonization; continuously heating at 850-930 ℃ for 15 ℃/h; keeping the temperature at 930 ℃ for 2 h; feeding propylene at the beginning, wherein the gas flow is 20L/min, the pressure in the hearth is kept at 0.6-0.7 kPa, and the deposition time is 200 h; after deposition is finished, stopping ventilation, and freely cooling at 930-room temperature;
6) disassembling the all-carbon tool in the step 4), and processing the honeycomb to a preset size to obtain a final product;
by the preparation method, the densification of the 200 mm-magnitude carbon/carbon honeycomb to the density of 0.19g/cm through 200h chemical vapor deposition is realized3Taking five subsamples from different positions, the density deviation being. + -. 0.003g/cm3(ii) a The flat compression strength is 10.28MPa, the flat compression modulus is 1052MPa, and the L-direction shear is testedShear strength of 6.79MPa, L-direction shear modulus of 1670MPa, W-direction shear strength of 5.26MPa, W-direction shear modulus of 831MPa, and thermal expansion coefficient of 0.18 × 10-6K; the thickness of the honeycomb wall is 0.78 mm-0.82 mm, and carbon deposition does not exist on the surface of the honeycomb wall; the distance between the opposite sides of 10 honeycomb core grids is randomly measured to be 8.63 mm-8.71 mm, and the deformation control effect of the core grids is good.
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| CN110282994B (en) * | 2019-06-24 | 2021-08-17 | 湖南东映碳材料科技有限公司 | Preparation method of carbon fiber reinforced carbon-based composite material honeycomb |
| CN114920576A (en) * | 2022-05-06 | 2022-08-19 | 北京理工大学 | Preparation method of novel carbon/silicon carbide honeycomb sandwich structure |
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