CN107382355A - A kind of fine and close C/C composite material and preparation method thereofs - Google Patents
A kind of fine and close C/C composite material and preparation method thereofs Download PDFInfo
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- CN107382355A CN107382355A CN201710604398.3A CN201710604398A CN107382355A CN 107382355 A CN107382355 A CN 107382355A CN 201710604398 A CN201710604398 A CN 201710604398A CN 107382355 A CN107382355 A CN 107382355A
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- carbon
- precast body
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
Abstract
The present invention discloses a kind of preparation method of fine and close C/C composites, prepares the carbon fiber precast body of 3D or 2.5D braidings first；Prefabricated component is put into chemical vapor deposition stove again, it is passed through methane, hydrogen, by chemical vapor infiltration methane decompose caused by pyrolytic carbon penetrate into precast body, realize the densification between carbon fiber wire in precast body, precast body is become C/C composite skeletons；Then thermosetting resin solution is impregnated in obtained C/C composite skeletons using polymer infiltration and pyrolysis method, and carries out Pintsch process in vacuum drying oven and obtain glass carbon matrix；Last repetitive cycling step（3）, stop when the rate of body weight gain of material is less than 1%, be finally pyrolyzed obtained pyrolysis glass-like carbon and be filled in fiber interfascicular, realize the densification of fiber interfascicular, obtain a kind of fine and close C/C composites and prepare.The material has high density, low porosity, high specific strength, specific modulus, and good toughness；Possess higher compactness, wear-resisting, service life length.
Description
Technical field
The present invention relates to C/C composites, more particularly, to a kind of fine and close C/C composite material and preparation method thereofs, belong to material
Field.
Background technology
Carbon/carbon compound material is a kind of new type high temperature material of the unique properties to grow up in the 60's of 20th century, it
Combine the excellent mechanical property of fibre reinforced composites and the excellent high-temperature behavior of carbonaceous material, have high specific strength,
Specific modulus, a series of excellent properties such as excellent strength retention, creep resistance and anti-thermal shock under good toughness and high temperature.It
It is high-temperature structural material ideal under inert atmosphere known today.Under certain condition, pyrolytic carbon and carbon fiber are answered
Conjunction just can obtain carbon/carbon compound material, using chemical vapor infiltration（C V I）Technique is effective way that this may be achieved
Footpath.C V I techniques are a kind of chemical vapor deposition (C V D) special shapes, and its essence is the solid surface heterogeneouss of gas one
Learn reaction.Because pyrolysis carbon structure and performance have larger dispersiveness, so the formation of pyrolytic carbon rises certainly in C V I techniques
Qualitatively act on.Carry out the research to pyrocarbon mechanism, it will help the formulation of depositing operation is instructed, to realizing material
Structure has important practical significance to meet performance requirement needed for quick densifying and acquisition.
Document " research of pyrolytic carbon formation mechenism in carbon/carbon compound material CVI techniques " elaborates pyrolytic carbon formation mechenism
And deposit the complexity for reflecting pyrocarbon, also indicate that people also lack unified to the generating process and rule of pyrolytic carbon
Understanding.The main difference of each mechanism is in the determination of necessary intermediate product, and involved coherent function method.Pyrolytic carbon is given birth to
Influence factor into process is a lot, and different researchers is it is concluded that often not consistent, or even very big discrepancy be present.
The pyrolytic carbon of often several different tissues coexists in C/C composite, illustrates under same process conditions and more
Kind depositional mode coexists, and might have different deposition process influences the generation of pyrolytic carbon.
The patent of invention of Patent No. 200810150575.6 discloses a kind of preparation side of carbon/composite material of silicon carbide
Method, the deficiency that prior art shearing strength at intersection cuts poor performance is the method overcome, precast body combination CVI method systems are sutured using puncturing
A kind of standby preparation method of carbon/composite material of silicon carbide, improves shearing strength at intersection shearing stress.
The above two all ignore carbon fiber stomata is also easy to produce during CVI the defects of so that material compactness reduces.Nothing
C/C composites are prepared by the method only with CVI or PIP to be all difficult to reach high-compactness, because in carbon fiber precast body
Space very little between filament, the space between two fibre bundles are but very big.If only with CVI techniques, due to gaseous molecular
Scattering and permeating, then the densification between filament can be realized, but but can not be fine and close because of " bottleneck effect " between fibre bundle；
If readily permeable to the densification between fibre bundle, realizing fiber interfascicular because resin solution viscosity is big only with PIP techniques, but
It is difficult to penetrate between filament, so as to space that can not be between fiberfill fibers silk.The vitreous carbon prepared simultaneously using PIP techniques
It is a kind of fine and close carbon structure, there is the advantages that porosity is low, and thermal conductivity factor is small, and hardness is high, anti-oxidant, by the height of vitreous carbon
Permeability resistance, air impermeability improve the compactness of matrix.The present invention is combined technique using CVI and PIP, is compiled with 3D or 2.5D
The carbon fiber knitted body knitted is precast body, carries out CVI first, and the porosity of material is then reduced by PIP methods, obtains a kind of cause
Close C/C composites.
The content of the invention
The purpose of the present invention is intended to overcome the deficiencies in the prior art, there is provided a kind of preparation method of fine and close C/C composites,
Comprise the following steps that：
（1）The carbon fiber precast body of 3D or 2.5D braidings is prepared, carbon fibrous body fraction is 35-45%；
（2）Prefabricated component is put into chemical vapor deposition stove, furnace pressure 100Pa-104Pa, it is warming up to 900-1200
DEG C, be passed through methane, hydrogen, by chemical vapor infiltration methane decompose caused by pyrolytic carbon penetrate into precast body, deposit
Time is 100-200h, realizes the densification between carbon fiber wire in precast body, precast body is become C/C composite skeletons, C/C
The porosity of composite skeleton is 25% ~ 35%；
（3）Thermosetting resin solution is impregnated into by step using polymer infiltration and pyrolysis method（2）Resulting C/C composite bones
In frame, and carry out Pintsch process in vacuum drying oven and obtain glass carbon matrix, cracking temperature is 900-1200 DEG C, described thermosetting
Resin solution concentration is 30%-50%, and thermosetting resin is any of phenolic resin, furane resins, epoxy resin.
（4）Repetitive cycling step（3）, stop when the rate of body weight gain of material is less than 1%, be finally pyrolyzed obtained pyrolysis glass
Charcoal is filled in fiber interfascicular, realizes the densification of fiber interfascicular, obtains a kind of fine and close C/C composites and prepares.
The invention has the advantages that：1. material has high density, low porosity, high specific strength, specific modulus, and good toughness；2.
The advantages of combining CVI and PIP techniques；3. possess higher compactness, wear-resisting, service life length.
Brief description of the drawings
Fig. 1 is a kind of diagrammatic cross-section of C/C composites of the present invention, wherein 20 be carbon fiber bundle, 30 be that CVI is pyrolyzed
Carbon, 40 be PIP vitreous carbons.
Fig. 2 is the structural representation of carbon fiber bundle, wherein 10 be carbon fiber wire, 20 be CVI pyrolytic carbons.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention, after the present invention has been read, various equivalences of the those skilled in the art to the present invention
The modification of form falls within the application appended claims and limited.
Embodiment 1
（1）The carbon fiber precast body of 3D braidings is prepared, carbon fibrous body fraction is 37%；
（2）Prefabricated component is put into chemical vapor deposition stove, furnace pressure 1000Pa, 1000 DEG C is warming up to, is passed through first
Alkane, hydrogen, by chemical vapor infiltration methane decompose caused by pyrolytic carbon penetrate into precast body, sedimentation time is
120h, the densification between carbon fiber wire in precast body is realized, precast body is become C/C composite skeletons, C/C composite bones
The porosity of frame is 20%；
（3）Thermosetting resin solution is impregnated into by step using polymer infiltration and pyrolysis method（2）Resulting C/C composite bones
In frame, and carry out Pintsch process in vacuum drying oven and obtain glass carbon matrix, cracking temperature is 900 DEG C, described thermosetting resin
Solution concentration is 35%, and thermosetting resin is phenolic resin.
（4）Repetitive cycling step（3）, stop when the rate of body weight gain of material is less than 1%, be finally pyrolyzed obtained pyrolysis glass
Charcoal is filled in fiber interfascicular, realizes the densification of fiber interfascicular, obtains a kind of fine and close C/C composites and prepares.
Embodiment 2
（1）The carbon fiber precast body of 2.5D braidings is prepared, carbon fibrous body fraction is 45%；
（2）Prefabricated component is put into chemical vapor deposition stove, furnace pressure 104Pa, 1200 DEG C are warming up to, is passed through first
Alkane, hydrogen, by chemical vapor infiltration methane decompose caused by pyrolytic carbon penetrate into precast body, sedimentation time is
200h, the densification between carbon fiber wire in precast body is realized, precast body is become C/C composite skeletons, C/C composite bones
The porosity of frame is 35%；
（3）Thermosetting resin solution is impregnated into by step using polymer infiltration and pyrolysis method（2）Resulting C/C composite bones
In frame, and carry out Pintsch process in vacuum drying oven and obtain glass carbon matrix, cracking temperature is 1200 DEG C, described thermosetting resin
Solution concentration is 50%, and thermosetting resin is furane resins.
（4）Repetitive cycling step（3）, stop when the rate of body weight gain of material is less than 1%, be finally pyrolyzed obtained pyrolysis glass
Charcoal is filled in fiber interfascicular, realizes the densification of fiber interfascicular, obtains a kind of fine and close C/C composites and prepares.
The single embodiment of the present invention is above are only, but the design concept of the present invention is not limited thereto, all utilizations
This design carries out the change of unsubstantiality to the present invention, all should belong to the behavior for invading the scope of protection of the invention.In every case it is not
Depart from the content of technical solution of the present invention, the technical spirit according to the present invention is made any type of simple to above example
Modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (1)
1. a kind of fine and close C/C composite material and preparation method thereofs, it is characterised in that comprise the following steps：
（1）The carbon fiber precast body of 3D or 2.5D braidings is prepared, carbon fibrous body fraction is 35-45%；
（2）Prefabricated component is put into chemical vapor deposition stove, furnace pressure 100Pa-104Pa, it is warming up to 900-1200
DEG C, be passed through methane, hydrogen, by chemical vapor infiltration methane decompose caused by pyrolytic carbon penetrate into precast body, deposit
Time is 100-200h, realizes the densification between carbon fiber wire in precast body, precast body is become C/C composite skeletons, C/C
The porosity of composite skeleton is 25% ~ 35%；
（3）Thermosetting resin solution is impregnated into by step using polymer infiltration and pyrolysis method（2）Resulting C/C composite bones
In frame, and carry out Pintsch process in vacuum drying oven and obtain glass carbon matrix, cracking temperature is 900-1200 DEG C, described thermosetting
Resin solution concentration is 30%-50%, and thermosetting resin is any of phenolic resin, furane resins, epoxy resin；
（4）Repetitive cycling step（3）, stop when the rate of body weight gain of material is less than 1%, be finally pyrolyzed obtained pyrolysis glass-like carbon and fill out
The densification in fiber interfascicular, realizing fiber interfascicular is filled, a kind of fine and close C/C composites is obtained and prepares.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710604398.3A CN107382355A (en) | 2017-07-24 | 2017-07-24 | A kind of fine and close C/C composite material and preparation method thereofs |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108068432A (en) * | 2017-12-08 | 2018-05-25 | 南京航空航天大学 | A kind of preparation method of the low heat conduction high-temperature resistance carbon fiber enhancing carborundum/glass carbon composite vacuum heat-insulating plate of high densification |
| CN108709198A (en) * | 2018-06-06 | 2018-10-26 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of 3D printing SiC core materials and high-densit vitreous carbon encapsulation combustion chamber |
| CN110294632A (en) * | 2019-05-05 | 2019-10-01 | 上海大学 | A kind of preparation method of the carbon fiber three-dimensional fabric enhancing carbon-based double base matrix composite of polyimides- |
| CN112858034A (en) * | 2021-01-08 | 2021-05-28 | 航天材料及工艺研究所 | Method for testing high-temperature mechanical properties of carbon fibers |
| CN113354432A (en) * | 2021-06-25 | 2021-09-07 | 上海大学 | Composite material with carbon matrix combined with silicon-boron-carbon-nitrogen matrix and preparation method thereof |
| CN114230357A (en) * | 2021-12-22 | 2022-03-25 | 中国电子科技集团公司第三十八研究所 | Preparation method of composite material slot waveguide antenna |
| CN114455982A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | Carbon/carbon composite material crucible containing aluminum oxide coating and silicon carbide coating |
| CN115160007A (en) * | 2022-06-15 | 2022-10-11 | 浙江德鸿碳纤维复合材料有限公司 | Carbon-carbon composite structure and preparation method thereof |
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| CN1948224A (en) * | 2006-10-31 | 2007-04-18 | 西安航天复合材料研究所 | Preparation method of C/C composite material conductive threaded rod |
| CN101311143A (en) * | 2008-04-23 | 2008-11-26 | 西安超码科技有限公司 | Method for preparing charcoal/charcoal air supply nozzle of high temperature furnace |
| CN101805200A (en) * | 2010-03-17 | 2010-08-18 | 上海大学 | Method for producing carbon/carbone composite material for bearings |
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Patent Citations (3)
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| CN1948224A (en) * | 2006-10-31 | 2007-04-18 | 西安航天复合材料研究所 | Preparation method of C/C composite material conductive threaded rod |
| CN101311143A (en) * | 2008-04-23 | 2008-11-26 | 西安超码科技有限公司 | Method for preparing charcoal/charcoal air supply nozzle of high temperature furnace |
| CN101805200A (en) * | 2010-03-17 | 2010-08-18 | 上海大学 | Method for producing carbon/carbone composite material for bearings |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108068432A (en) * | 2017-12-08 | 2018-05-25 | 南京航空航天大学 | A kind of preparation method of the low heat conduction high-temperature resistance carbon fiber enhancing carborundum/glass carbon composite vacuum heat-insulating plate of high densification |
| CN108709198A (en) * | 2018-06-06 | 2018-10-26 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of 3D printing SiC core materials and high-densit vitreous carbon encapsulation combustion chamber |
| CN110294632A (en) * | 2019-05-05 | 2019-10-01 | 上海大学 | A kind of preparation method of the carbon fiber three-dimensional fabric enhancing carbon-based double base matrix composite of polyimides- |
| CN110294632B (en) * | 2019-05-05 | 2021-05-11 | 上海大学 | Carbon fiber three-dimensional fabric reinforced polyimide-carbon-based binary matrix composite material |
| CN112858034A (en) * | 2021-01-08 | 2021-05-28 | 航天材料及工艺研究所 | Method for testing high-temperature mechanical properties of carbon fibers |
| CN113354432A (en) * | 2021-06-25 | 2021-09-07 | 上海大学 | Composite material with carbon matrix combined with silicon-boron-carbon-nitrogen matrix and preparation method thereof |
| CN114230357A (en) * | 2021-12-22 | 2022-03-25 | 中国电子科技集团公司第三十八研究所 | Preparation method of composite material slot waveguide antenna |
| CN114230357B (en) * | 2021-12-22 | 2023-01-31 | 中国电子科技集团公司第三十八研究所 | Preparation method of composite material slot waveguide antenna |
| CN114455982A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | Carbon/carbon composite material crucible containing aluminum oxide coating and silicon carbide coating |
| CN114455982B (en) * | 2021-12-30 | 2023-08-11 | 西安超码科技有限公司 | Carbon/carbon composite material crucible containing aluminum oxide coating and silicon carbide coating |
| CN115160007A (en) * | 2022-06-15 | 2022-10-11 | 浙江德鸿碳纤维复合材料有限公司 | Carbon-carbon composite structure and preparation method thereof |
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