CN108840697A - A kind of carbon/carbon compound material honeycomb and preparation method thereof - Google Patents
A kind of carbon/carbon compound material honeycomb and preparation method thereof Download PDFInfo
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- CN108840697A CN108840697A CN201810697631.1A CN201810697631A CN108840697A CN 108840697 A CN108840697 A CN 108840697A CN 201810697631 A CN201810697631 A CN 201810697631A CN 108840697 A CN108840697 A CN 108840697A
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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
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- 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 kind of carbon/carbon compound material honeycomb and preparation method thereof, belongs to carbon/carbon compound material technical field.The carbon/carbon compound material honeycomb, including carbon fiber reinforcement and the carbon base body for being covered on the carbon fiber reinforcement surface, wherein the carbon fiber reinforcement is honeycomb, and L is to continuous carbon fibre in the honeycomb, and W is to also with continuous carbon fibre.Carbon/carbon compound material honeycomb of the invention has excellent thermal stability and mechanical property, and meets space industry lightweight requirements；Honeycomb Specifeca tion speeification meets flat crushing strength >=8MPa, concora crush modulus >=900MPa, L to shear strength >=6.7MPa, L to modulus of shearing >=1500MPa, W to shear strength >=4.5MPa, and W is to modulus of shearing >=730MPa, thermal expansion coefficient 0~0.2 × 10‑6/K。
Description
Technical field
This patent is related to a kind of High Accuracy Observation platform low-density, high stable, high strength monolithic carbon/carbon composite bee
Nest belongs to carbon/carbon compound material technical field.
Background technique
Traditional spacecraft structure generally only requires high specific strength, high ratio modulus etc. with composite material, to its dimensionally stable
Property it is of less demanding.But the high-precisions such as satellite spacecraft with composite structure develop field, have high stability, lightweight,
The composite material of the features such as high intensity is its important development direction.Advanced country has begun one's study the space flight of zero thermal expansion, high stable
Device composite structure is mainly used for the optical instruments such as space telescope support construction, gravity gradiometer support base, antenna
Reflector Panel etc..For the operating accuracy for guaranteeing spaceborne high-precision optical instrument and detecting devices, it is necessary to provide height for it
Stability, high-intensitive light composite material structure platform.
In the prior art, domestic space industry is usually using carbon/carbon compound material block, carbon/composite material of silicon carbide block
The support construction of body or carbon fiber enhancement resin base honeycomb as precision instrument, so that it keeps good stability；Due to carbon/
Carbon composite block either carbon/composite material of silicon carbide block is solid construction, is unfavorable for space industry lightweight and wants
It asks；Carbon fiber enhancement resin base honeycomb heat expansion system is about 10-4Magnitude, thermal stability are poor.
Summary of the invention
To solve problems of the prior art, the embodiment of the present invention provide a kind of carbon/carbon compound material honeycomb and its
Preparation method, carbon/carbon compound material honeycomb has excellent thermal stability and mechanical property, and meets space industry lightweight and want
It asks.
For achieving the above object, the present invention provides the following technical solutions：
A kind of carbon/carbon compound material honeycomb including carbon fiber reinforcement and is covered on the carbon fiber reinforcement surface
Carbon base body, wherein the carbon fiber reinforcement is honeycomb, and in the honeycomb L to continuous carbon fibre, W to
With continuous carbon fibre.
In an alternative embodiment, the carbon fiber reinforcement by T300-1K, T300-3K, T300-6K, T300-12K,
One of T700-6K, T700-12K, T800-6K or T800-12K polyacrylonitrile-based carbon fibre or more than one combinations are made.
In an alternative embodiment, with the continuous fiber in 30-60 ° of direction on the honeycomb wall of the carbon fiber reinforcement.
In an alternative embodiment, the cellular core lattice side length is 2.75mm~15mm, and honeycomb wall is with a thickness of 0.17mm
~2mm.
In an alternative embodiment, the carbon/carbon compound material cellular densities are 100kg/m3~220kg/m3。
A kind of cellular preparation method of carbon/carbon compound material, includes the following steps：
Step 1, the carbon fiber reinforcement for preparing honeycomb, in the honeycomb L to continuous carbon fibre, W to
Also there is continuous carbon fibre；
Step 2 is impregnated using carbon fiber reinforcement of the phenolic resin to the honeycomb, is solidified, and is solidified
The carbon fiber reinforcement of d type；
Step 3 is carbonized to the carbon fiber reinforcement for solidifying d type, densification, and carbon/carbon composite wood is obtained
Expect honeycomb.
In an alternative embodiment, the carbon fiber reinforcement for solidifying d type is carried out at carbonization described in step 3
Before reason, further include：
Core model is inserted into the honeycomb core lattice of the carbon fiber reinforcement for solidifying d type, the core model side wall is equipped with edge
The airflow channel that honeycomb thickness direction extends.
In an alternative embodiment, the airflow channel, and the gas are equipped on six side walls of each core model
The width of circulation road and the carbon fiber reinforcement connecting position for solidifying d type is the 60-80% of the core model sidewall width,
Depth is the 20-30% of the distance of opposite two side walls of the core model.
In an alternative embodiment, phenolic resin described in step 2 is the diluted phenolic resin of volatile organic solvent,
Described in volatile organic solvent mass percent be 10%~50%
In an alternative embodiment, carbonization described in step 3, including：
First at 280~320 DEG C, 1.5~3h is kept the temperature, then at 540~560 DEG C, 1.5~3h is kept the temperature, later in 800-900
DEG C, 2-4h is kept the temperature, room temperature is down to.
In an alternative embodiment, 180~220 DEG C are warming up to the heating rate of 40-60 DEG C/h, with the liter of 5-15 DEG C/h
Warm rate is warming up to 280~320 DEG C, 540~560 DEG C is warming up to the heating rate of 5~10 DEG C/h, with the liter of 5~10 DEG C/h
Warm rate is warming up to 640~660 DEG C；It is warming up to 800-900 DEG C with the heating rate of 10-20 DEG C/h, no more than 100 DEG C/h's
Rate of temperature fall is down to room temperature.In an alternative embodiment, densification described in step 3, including：
Densification is carried out using gas-phase deposition is learned, wherein carbon-source gas is one in methane, propylene or propane
Kind or more than one combinations, Ventilation Rate is 5~50L/min, pressure is 0.6~0.7kPa, sedimentation time 100-400h.
Compared with prior art, the present invention having the advantages that：
(1) carbon/carbon compound material honeycomb provided in an embodiment of the present invention, by make the L of carbon fiber reinforcement to W to equal
With continuous carbon fibre, it is ensured that carbon/carbon compound material honeycomb is not easy delamination splitting, fine and close chemical industry in carbonization and densification process
Skill adaptability is excellent, and the carbon/carbon compound material honeycomb of preparation has excellent thermal stability and mechanical property, and meets space flight neck
Domain lightweight requirements；
(2) honeycomb Specifeca tion speeification meet flat crushing strength >=8MPa, concora crush modulus >=900MPa, L to shear strength >=
6.7MPa, L are to modulus of shearing >=730MPa, thermal expansion to modulus of shearing >=1500MPa, W to shear strength >=4.5MPa, W
Number 0~0.2 × 10-6/K；
(3) it is densified using chemical vapor deposition process, it is ensured that the nearly size of honeycomb efficiently densifies；
(4) carbon/carbon honeycomb densification process process is simple, and densification cycle is short, it is easy to accomplish engineering application.
Detailed description of the invention
Fig. 1 is a kind of carbon/carbon compound material honeycomb outside drawing provided in an embodiment of the present invention；
Fig. 2 is two pieces of carbon cloth combinations signals provided in an embodiment of the present invention when preparing carbon fiber reinforcement with carbon cloth
Figure；
Fig. 3 is densification graphite core mould structural schematic diagram provided in an embodiment of the present invention.
Specific embodiment
Explanation is further explained to a specific embodiment of the invention below with reference to specific embodiment.
As shown in Figure 1, the embodiment of the invention provides a kind of carbon/carbon compound material honeycomb, including carbon fiber reinforcement and
It is covered on the carbon base body on the carbon fiber reinforcement surface, wherein the carbon fiber reinforcement is honeycomb, and the honeycomb
L is to continuous carbon fibre in structure, and W is to also with continuous carbon fibre.
Specifically, in the embodiment of the present invention, carbon fiber reinforcement honeycomb can be realized in such a way that carbon cloth splices suture
The L of structure to W to all having continuous fiber, wherein for L to for the continuous fiber in layer of cloth, W is fine to the suture for cloth interlayer
Dimension, specifically, as shown in Fig. 2, carbon cloth according to cell layout size is first cut into predetermined shape and in the position that sutures of needs
It makes marks, then docks adjacent carbon cloth, and interface is sutured by suture；
Carbon/carbon compound material honeycomb provided in an embodiment of the present invention, by make the L of carbon fiber reinforcement to W to having
There is continuous carbon fibre, it is ensured that there is continuity, effect in honeycomb interior all directions as carbon/carbon honeycomb skeleton carbon fiber
External applied load on carbon/carbon honeycomb can efficiently be transmitted by continuous fiber in different honeycomb core compartments, sufficiently raising carbon/carbon honeycomb
Mechanical property；Carbon/carbon compound material honeycomb provided in an embodiment of the present invention has excellent thermal stability and mechanical property, and
Meet space industry lightweight requirements；Carbon/carbon compound material honeycomb is not easy delamination splitting in carbonization and densification process, fine and close
It is excellent to change Technological adaptability；Honeycomb Specifeca tion speeification meets flat crushing strength >=8MPa, concora crush modulus >=900MPa, L to shearing
For intensity >=6.7MPa, L to modulus of shearing >=1500MPa, W to shear strength >=4.5MPa, W is warm to modulus of shearing >=730MPa
The coefficient of expansion 0~0.2 × 10-6/K。
In an alternative embodiment, the carbon fiber reinforcement is preferably by T300-1K, T300-3K, T300-6K, T300-
One of 12K, T700-6K, T700-12K, T800-6K or T800-12K polyacrylonitrile-based carbon fibre or more than one combinations
It is made.
In an alternative embodiment, there is the continuous fiber in 30-60 ° of direction on the honeycomb wall of the carbon fiber reinforcement,
Ensure that carbon/carbon honeycomb has stronger anti-shear performance.
In an alternative embodiment, the cellular core lattice side length is 2.75mm~15mm, and honeycomb wall is with a thickness of 0.17mm
~2mm had not only ensured honeycomb specific strength with higher, but also guarantee honeycomb wall by preferred different honeycomb core lattice side lengths and wall thickness
It is smooth, it avoids causing since honeycomb wall is rough generating carbon distribution or demoulding damage honeycomb wall during densification process.
In an alternative embodiment, the carbon/carbon compound material honeycomb, density 100kg/m3~220kg/m3, it is ensured that
While carbon/carbon honeycomb meets light-weight design, also meet mechanical performance index requirement.
The embodiment of the invention also provides a kind of cellular preparation methods of carbon/carbon compound material, include the following steps：
Step 1, the carbon fiber reinforcement for preparing honeycomb, in the honeycomb L to continuous carbon fibre, W to
Also there is continuous carbon fibre；
Specifically, in the embodiment of the present invention, carbon fiber reinforcement honeycomb can be realized in such a way that carbon cloth splices suture
The L of structure to W to continuous fiber is all had, specifically, as shown in Fig. 2, first carbon cloth m is cut into according to cell layout size
Predetermined shape is simultaneously needing the position sutured to make marks, and then by two pieces of cloth m fitting docking of carbon, interface is stitched by suture n
It closes, after suture, when being inserted into core model in non-suture, is demoulded after solidification dimension shape, honeycomb as shown in Figure 2 can be obtained；
The carbon base body includes that the resin carbon that resin carbonation is formed and densification (chemical vapor deposition) are formed
Pyrolytic carbon.
Step 2 is impregnated using carbon fiber reinforcement of the phenolic resin to the honeycomb, is solidified, and is solidified
The carbon fiber reinforcement of d type；
Specifically, in the embodiment of the present invention, phenolic resin described in step 2 is ethyl alcohol, ethyl acetate, methanol, acetone etc.
The diluted phenolic resin of volatile organic solvent, wherein the mass percent of the volatile organic solvent is 10%~50%；
Solidification described in step 2 is preferably warming up to 60~80 DEG C with the heating rate of 20~40 DEG C/h, keeps the temperature 1~3h；With 5~20 DEG C/
The heating rate of h is warming up to 90~110 DEG C, keeps the temperature 0.5~2h；120~130 DEG C are warming up to the heating rate of 5~20 DEG C/h,
Keep the temperature 0.5~2h；150~170 DEG C are warming up to the heating rate of 5~20 DEG C/h, keeps the temperature 5~7h；With the cooling of≤25 DEG C/h
Rate is cooled to 80 DEG C hereinafter, then freely cooling down；
Step 3 is carbonized to the carbon fiber reinforcement for solidifying d type, densification, and carbon/carbon composite wood is obtained
Expect honeycomb.
In an alternative embodiment, the carbon fiber reinforcement for solidifying d type is carried out at carbonization described in step 3
Before reason, further include：
Core model is inserted into the honeycomb core lattice of the carbon fiber reinforcement for solidifying d type, the core model side wall is equipped with edge
The airflow channel that honeycomb thickness direction d extends.By the way that airflow channel is arranged, it is ensured that carbon-source gas can be entered unimpededly in honeycomb
Portion realizes the efficient uniform densification of honeycomb wall.
As shown in figure 3, it is logical to be equipped with the air-flow on six side walls of each core model in an alternative embodiment
Road, and the width a of the airflow channel and the carbon fiber reinforcement connecting position for solidifying d type is that the core model side wall is wide
The 60-80% of degree, depth b are the 20-30% of the distance of opposite two side walls of the core model.By controlling airflow channel
Size, it is ensured that into the carbon-source gas flow inside airflow channel, while minimizing honeycomb wall and core model external form face contact
Area demoulds after facilitating densification, reduces the demoulding to honeycomb wall and damages.
In an alternative embodiment, carbonization described in step 3, including：180 are warming up to the heating rate of 40~60 DEG C/h
~220 DEG C；280~320 DEG C are warming up to the heating rate of 5~15 DEG C/h, keeps the temperature 1.5~3h；With the heating speed of 5~10 DEG C/h
Rate is warming up to 540~560 DEG C, keeps the temperature 1.5~3h；640~660 DEG C are warming up to the heating rate of 5~10 DEG C/h；With 10~20
DEG C/heating rate of h is warming up to 800~900 DEG C, 1.5~3h is kept the temperature, resin carbonation is completed.Pass through the carbonization technique, mid-term liter
Warm rate is slow, can reduce deformation internal stress of the honeycomb in carbonisation, it is ensured that the nearly size molding of honeycomb.In an alternative embodiment
In, densification described in step 3, including：After completing carbonization technique in cvd furnace, the heating of 10~20 DEG C/h is directly pressed
Rate is warming up to 900~1000 DEG C from carbonization technique maximum temperature, keeps the temperature 1~3h, starts to be passed through carbon-source gas, gas flow 5
~50L/min, 0.6~0.7kPa of pressure in the burner hearth, 100~400h of sedimentation time, to ensure that the nearly size of honeycomb efficiently densifies.
The present embodiment can prepare the carbon/carbon compound material honeycomb in above-mentioned honeycomb embodiment, about carbon/carbon compound material
Cellular specific descriptions are referring to above-mentioned honeycomb embodiment, and details are not described herein.
The following are several specific embodiments of the invention：
Embodiment 1
Present embodiments provide a kind of overall size 200mm × 200mm × 80mm, honeycomb core lattice side length 5mm, thickness of honeycomb wall
The satellite of 0.8mm carbon/carbon compound material honeycomb, preparation method include：
1) general purpose grade T300-3K polyacrylonitrile-based carbon fibre is selected to be woven into surface density 240g/cm3Plain weave carbon cloth, longitude and latitude
Close 6/cm × 6 piece/cm.The carbon cloth block that carbon cloth is then cut into certain specification by honeycomb wall developed dimension is spare；It is cutting
In the process with warp yarn direction for 0 °, rotation forms+45 ° of carbon cloths counterclockwise, rotates clockwise to form -45 ° of carbon cloths.
2) the carbon cloth block in step 1) is subjected to cloth lamination according to the ply stacking-sequence of design, adjacent carbon cloth is according to+45/-
The arrangement of 45 ply stacking-sequences；Carbon cloth is sutured two-by-two, honeycomb thickness direction sutures spacing 4mm, and the direction honeycomb L sutures spacing 5mm, seam
Zygonema is T300-1K carbon fiber, and yarn tooling diameter 1.3mm is drawn in suture；Carbon cloth suture is accumulated to honeycomb products design requirement laying
After number, it is inserted into hexahedron metal impregnation-solidification tooling and impregnates the phenol resin solution of ethyl alcohol mass content 20%；It is heating and curing
After demould, form carbon fiber reinforcement, wherein resin solidification temperature increasing schedule is：Room temperature~80 DEG C, 25 DEG C/h；80 DEG C of heat preservation 2h；
80 DEG C~100 DEG C, 10 DEG C/h；100 DEG C of heat preservation 1h；100 DEG C~120 DEG C, 10 DEG C/h；120 DEG C of heat preservation 1h；120 DEG C~160 DEG C,
10℃/h；160 DEG C of heat preservation 6h；160 DEG C~70 DEG C ,≤25 DEG C/h；70 DEG C~room temperature, freely cool down.
3) full carbonaceous anti-deformation is prepared according to the carbon fiber reinforcement of the solidification d type prepared in step 2) and densifies tooling,
Tooling is made of graphite core mould and clamping plate.Graphite core mould is prism structure, and fluted 1 is processed on each side wall, is formed
Airflow channel, graphite core mould cross section are hexagonal structure as shown in Figure 3, further groove 1 and the carbon fiber for solidifying d type
The width a for tieing up reinforcement connecting position is 3mm, and depth b is 2mm.
4) carbonaceous tooling complete in step 3) is assemblied in step 2) and is solidified on the carbon fiber reinforcement of d type, it will be with tooling
The carbon fiber reinforcement of solidification d type be vertically placed in cylindrical vertical cvd furnace；Heating treatment is carried out to cvd furnace, is risen
Warm curve be room temperature~200 DEG C, 50 DEG C/h；200 DEG C~300 DEG C, 10 DEG C/h；300 DEG C of heat preservation 2h；300 DEG C~550 DEG C, 5 DEG C/
h；550 DEG C of heat preservation 2h；550 DEG C~650 DEG C, 10 DEG C/h；650 DEG C~850 DEG C, 15 DEG C/h；850 DEG C of heat preservation 2h complete resin carbon
Change；Continue to heat up, 850 DEG C~930 DEG C, 15 DEG C/h；930 DEG C of heat preservation 2h；Start logical propylene, gas flow 20L/min keeps furnace
0.6~0.7kPa of breech pressure, sedimentation time 200h；After completing deposition, stop ventilation.930 DEG C~room temperature, freely cool down.
6) demounting procedure 4) in full carbonaceous tooling, honeycomb is machined to predetermined size, obtains final products.
Process through the invention realizes 200mm magnitude carbon/carbon honeycomb and passes through the density of 200h chemical vapor deposition
To density 0.19g/cm3, five increments, density variation ± 0.003g/cm are taken from different location3；Test its flat crushing strength
10.28MPa, concora crush modulus 1052MPa, L are to shear strength 6.79MPa, and L is to modulus of shearing 1670MPa, and W is to shear strength
5.26MPa, W are to modulus of shearing 831MPa, thermal expansion coefficient 0.18 × 10-6/K；Thickness of honeycomb wall 0.78mm~0.82mm, honeycomb wall
Surface is without carbon distribution；10 honeycomb core lattice opposite side distance 8.63mm~8.71mm of random measurement, core lattice deformation control effect are good.
Embodiment 2
Present embodiments provide a kind of overall size 400mm × 400mm × 80mm, honeycomb core lattice side length 5mm, thickness of honeycomb wall
0.8mm carbon/carbon compound material honeycomb, preparation method include：
1) general purpose grade T300-3K polyacrylonitrile-based carbon fibre is selected to be woven into surface density 240g/cm3Plain weave carbon cloth, longitude and latitude
Close 6/cm × 6 piece/cm.The carbon cloth block that carbon cloth is then cut into certain specification by honeycomb wall developed dimension is spare；It is cutting
In the process with warp yarn direction for 0 °, rotation forms+45 ° of carbon cloths counterclockwise, rotates clockwise to form -45 ° of carbon cloths.
2) the carbon cloth block in step 1) is subjected to cloth lamination according to the ply stacking-sequence of design, adjacent carbon cloth is according to+45/-
The arrangement of 45 ply stacking-sequences；Carbon cloth is sutured two-by-two, honeycomb thickness direction sutures spacing 4mm, and the direction honeycomb L sutures spacing 5mm, seam
Zygonema is T300-1K carbon fiber, and yarn tooling diameter 1.3mm is drawn in suture；Carbon cloth suture is accumulated to honeycomb products design requirement laying
After number, it is inserted into hexahedron metal impregnation-solidification tooling and impregnates the phenol resin solution of ethyl alcohol mass content 20%；It is heating and curing
After demould, form carbon fiber reinforcement, wherein resin solidification temperature increasing schedule is：Room temperature~80 DEG C, 25 DEG C/h；80 DEG C of heat preservation 2h；
80 DEG C~100 DEG C, 10 DEG C/h；100 DEG C of heat preservation 1h；100 DEG C~120 DEG C, 10 DEG C/h；120 DEG C of heat preservation 1h；120 DEG C~160 DEG C,
10℃/h；160 DEG C of heat preservation 6h；160 DEG C~70 DEG C ,≤25 DEG C/h；70 DEG C~room temperature, freely cool down.
3) full carbonaceous anti-deformation is prepared according to the carbon fiber reinforcement of the solidification d type prepared in step 2) and densifies tooling,
Tooling is made of graphite core mould and clamping plate.Graphite core is prism structure, and processing forms gas by groove 1 on each side wall
Circulation road, graphite core mould cross section are hexagonal structure as shown in Figure 3, further groove 1 and the carbon fiber for solidifying d type
The width a of reinforcement connecting position is 3mm, and depth b is 2mm.
4) carbonaceous tooling complete in step 3) is assemblied in step 2) and is solidified on the carbon fiber reinforcement of d type, it will be with tooling
The carbon fiber reinforcement of solidification d type be vertically placed in cylindrical vertical cvd furnace；Heating treatment is carried out to cvd furnace, is risen
Warm curve be room temperature~200 DEG C, 50 DEG C/h；200 DEG C~300 DEG C, 10 DEG C/h；300 DEG C of heat preservation 2h；300 DEG C~550 DEG C, 5 DEG C/
h；550 DEG C of heat preservation 2h；550 DEG C~650 DEG C, 10 DEG C/h；650 DEG C~850 DEG C, 15 DEG C/h；850 DEG C of heat preservation 2h complete resin carbon
Change；Continue to heat up, 850 DEG C~930 DEG C, 15 DEG C/h；930 DEG C of heat preservation 2h；Start logical propylene, gas flow 20L/min keeps furnace
0.6~0.7kPa of breech pressure, sedimentation time 200h；After completing deposition, stop ventilation.930 DEG C~room temperature, freely cool down.
6) demounting procedure 4) in full carbonaceous tooling, honeycomb is machined to predetermined size, obtains final products.
Process through the invention realizes 400mm magnitude carbon/carbon honeycomb and passes through the density of 200h chemical vapor deposition
To density 0.185g/cm3, five increments, density variation ± 0.005g/cm are taken from different location3；Test its flat crushing strength
10.03MPa, concora crush modulus 1027MPa, L are to shear strength 6.55MPa, and L is to modulus of shearing 1606MPa, and W is to shear strength
5.01MPa, W are to modulus of shearing 798MPa, thermal expansion coefficient 0.18 × 10-6/K；Thickness of honeycomb wall 0.79mm~0.83mm, honeycomb wall
Surface is without carbon distribution；10 honeycomb core lattice opposite side distance 8.58mm~8.64mm of random measurement, core lattice deformation control effect are good.Together
When, the dimension scale honeycomb and 200mm honeycomb similar performance, carbon/carbon honeycomb described in this patent and preparation method thereof stability is good.
Embodiment 3
Present embodiments provide a kind of overall size 400mm × 400mm × 50mm, honeycomb core lattice side length 4mm, thickness of honeycomb wall
0.3mm carbon/carbon compound material honeycomb, preparation method include：
1) general purpose grade T700-12K polyacrylonitrile-based carbon fibre is selected to be woven into surface density 200g/cm3Broaden cloth, fiber exhibition
Open width 8mm.The carbon cloth block that carbon cloth is then cut into certain specification by honeycomb wall developed dimension is spare；During the cutting process with
Warp yarn direction is 0 °, and rotation forms+45 ° of carbon cloths counterclockwise, rotates clockwise to form -45 ° of carbon cloths.
2) the carbon cloth block in step 1) is subjected to cloth lamination according to the ply stacking-sequence of design, adjacent carbon cloth is according to+45/-
The arrangement of 45 ply stacking-sequences；Carbon cloth is sutured two-by-two, honeycomb thickness direction sutures spacing 3mm, and the direction honeycomb L sutures spacing 4mm, seam
Zygonema is T300-1K carbon fiber, and yarn tooling diameter 1.3mm is drawn in suture；Carbon cloth suture is accumulated to honeycomb products design requirement laying
After number, it is inserted into hexahedron metal impregnation-solidification tooling and impregnates the phenol resin solution of ethyl alcohol mass content 15%；It is heating and curing
After demould, form carbon fiber reinforcement, wherein resin solidification temperature increasing schedule is：Room temperature~80 DEG C, 25 DEG C/h；80 DEG C of heat preservation 2h；
80 DEG C~100 DEG C, 10 DEG C/h；100 DEG C of heat preservation 1h；100 DEG C~120 DEG C, 10 DEG C/h；120 DEG C of heat preservation 1h；120 DEG C~160 DEG C,
10℃/h；160 DEG C of heat preservation 6h；160 DEG C~70 DEG C ,≤25 DEG C/h；70 DEG C~room temperature, freely cool down.
3) full carbonaceous anti-deformation is prepared according to the carbon fiber reinforcement of the solidification d type prepared in step 2) and densifies tooling,
Tooling is made of graphite core mould and clamping plate.Graphite core is prism structure, and processing forms gas by groove 1 on each side wall
Circulation road, graphite core mould cross section are hexagonal structure as shown in Figure 3, further groove 1 and the carbon fiber for solidifying d type
The width a of reinforcement connecting position is 2.5mm, and depth b is 1.5mm.
4) carbonaceous tooling complete in step 3) is assemblied in step 2) and is solidified on the carbon fiber reinforcement of d type, it will be with tooling
The carbon fiber reinforcement of solidification d type be vertically placed in cylindrical vertical cvd furnace；Heating treatment is carried out to cvd furnace, is risen
Warm curve be room temperature~200 DEG C, 50 DEG C/h；200 DEG C~300 DEG C, 10 DEG C/h；300 DEG C of heat preservation 2h；300 DEG C~550 DEG C, 5 DEG C/
h；550 DEG C of heat preservation 2h；550 DEG C~650 DEG C, 10 DEG C/h；650 DEG C~850 DEG C, 15 DEG C/h；850 DEG C of heat preservation 2h complete resin carbon
Change；Continue to heat up, 850 DEG C~930 DEG C, 15 DEG C/h；930 DEG C of heat preservation 2h；Start logical propylene, gas flow 20L/min keeps furnace
0.6~0.7kPa of breech pressure, sedimentation time 300h；After completing deposition, stop ventilation.930 DEG C~room temperature, freely cool down.
6) demounting procedure 4) in full carbonaceous tooling, honeycomb is machined to predetermined size, obtains final products.
Process through the invention realizes 400mm magnitude carbon/carbon honeycomb and passes through the density of 300h chemical vapor deposition
To density 0.18g/cm3, five increments, density variation ± 0.005g/cm are taken from different location3；Test its flat crushing strength
8.93MPa, concora crush modulus 967MPa, L are to shear strength 6.32MPa, and L is to modulus of shearing 1583MPa, and W is to shear strength
4.89MPa, W are to modulus of shearing 795MPa, thermal expansion coefficient 0.16 × 10-6/K；Thickness of honeycomb wall 0.29mm~0.33mm, honeycomb wall
Surface is without carbon distribution；10 honeycomb core lattice opposite side distance 6.90mm~7.05mm of random measurement, core lattice deformation control effect are good.
The content that description in the present invention is not described in detail belongs to the well-known technique of professional and technical personnel in the field.
Claims (12)
1. a kind of carbon/carbon compound material honeycomb, which is characterized in that including carbon fiber reinforcement and be covered on the fibre reinforced
The carbon base body in body surface face, wherein the carbon fiber reinforcement be honeycomb, and in the honeycomb L to continuous carbon fiber
Dimension, W is to also with continuous carbon fibre.
2. carbon/carbon compound material honeycomb according to claim 1, which is characterized in that the carbon fiber reinforcement is by T300-
1K, T300-3K, T300-6K, T300-12K, T700-6K, T700-12K, T800-6K or T800-12K polyacrylonitrile-radical carbon fiber
One of dimension or more than one combinations are made.
3. carbon/carbon compound material honeycomb according to claim 1, which is characterized in that the honeycomb of the carbon fiber reinforcement
With the continuous fiber in 30-60 ° of direction on wall.
4. carbon/carbon compound material honeycomb according to claim 1, which is characterized in that the cellular core lattice side length is
2.75mm~15mm, honeycomb wall is with a thickness of 0.17mm~2mm.
5. carbon/carbon compound material honeycomb according to claim 1, which is characterized in that density 100kg/m3~220kg/
m3。
6. a kind of cellular preparation method of carbon/carbon compound material, which is characterized in that include the following steps：
Step 1, the carbon fiber reinforcement for preparing honeycomb, L is to continuous carbon fibre in the honeycomb, and W is to also having
There is continuous carbon fibre；
Step 2 is impregnated using carbon fiber reinforcement of the phenolic resin to the honeycomb, is solidified, and solidification d type is obtained
Carbon fiber reinforcement；
Step 3 is carbonized to the carbon fiber reinforcement for solidifying d type, densification, and carbon/carbon compound material bee is obtained
Nest.
7. the cellular preparation method of carbon/carbon compound material according to claim 6, which is characterized in that described in step 3
Before carrying out carbonization treatment to the carbon fiber reinforcement for solidifying d type, further include：
Core model is inserted into the honeycomb core lattice of the carbon fiber reinforcement for solidifying d type, the core model side wall is equipped with along honeycomb
The airflow channel that thickness direction extends.
8. the cellular preparation method of carbon/carbon compound material according to claim 7, which is characterized in that each core model
Six side walls on be equipped with the airflow channel, and the airflow channel connects with the carbon fiber reinforcement for solidifying d type
The width of position is the 60-80% of the core model sidewall width, and depth is the distance of opposite two side walls of the core model
20-30%.
9. the cellular preparation method of carbon/carbon compound material according to claim 6, which is characterized in that phenol described in step 2
Urea formaldehyde is the diluted phenolic resin of volatile organic solvent, wherein the mass percent of the volatile organic solvent is 10%
~50%.
10. the cellular preparation method of carbon/carbon compound material according to claim 6, which is characterized in that described in step 3
Carbonization, including：
First at 280~320 DEG C, 1.5~3h is kept the temperature, then at 540~560 DEG C, keeps the temperature 1.5~3h, later at 800-900 DEG C,
2-4h is kept the temperature, room temperature is down to.
11. the cellular preparation method of carbon/carbon compound material according to claim 10, which is characterized in that with 40-60 DEG C/h
Heating rate be warming up to 180~220 DEG C, 280~320 DEG C are warming up to the heating rate of 5-15 DEG C/h, with 5~10 DEG C/h's
Heating rate is warming up to 540~560 DEG C, is warming up to 640~660 DEG C with the heating rate of 5~10 DEG C/h；With 10-20 DEG C/h's
Heating rate is warming up to 800-900 DEG C, is down to room temperature with the rate of temperature fall no more than 100 DEG C/h.
12. the cellular preparation method of carbon/carbon compound material according to claim 6, which is characterized in that described in step 3
Densification, including：
Carry out densification using gas-phase deposition is learned, wherein carbon-source gas be one of methane, propylene or propane or
More than one combinations, Ventilation Rate is 5~50L/min, pressure is 0.6~0.7kPa, sedimentation time 100-400h.
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| 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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|---|---|---|---|---|
| CN110039792A (en) * | 2018-11-22 | 2019-07-23 | 阜宁云逸航空复合材料有限公司 | The cellular production method and device of continuous fiber reinforcement side wall |
| CN110282994A (en) * | 2019-06-24 | 2019-09-27 | 湖南东映碳材料科技有限公司 | A kind of cellular preparation method of carbon fiber reinforced carbon based composites |
| 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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