CN103722784B - A kind of laminated resin fills the preparation method of hybrid composite - Google Patents
A kind of laminated resin fills the preparation method of hybrid composite Download PDFInfo
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- CN103722784B CN103722784B CN201310412156.6A CN201310412156A CN103722784B CN 103722784 B CN103722784 B CN 103722784B CN 201310412156 A CN201310412156 A CN 201310412156A CN 103722784 B CN103722784 B CN 103722784B
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Abstract
Lamination mixes a preparation method for solar heat protection sandwich, it is characterized in that using graphite as liner, forms prefabricated component at its surface wrap or braiding fiber C, and on prefabricated component, deposit pyrolysis C formation porous C/C precast body.Remove graphite core, at precast body surface wrap carbon cloth or C prepreg cloth, deposition skim pyrolysis C interface, 1100 ~ 1300 DEG C of chemical vapor infiltration SiC matrix, forms C/SiC composite.Liner C/C precast body is immersed in deployed resin adhesive liquid, obtains lamination after hot-press solidifying and mix solar heat protection sandwich.Adopt in chemical gaseous phase permeation process and fiber reinforcement is not damaged, ensure that integrality and the intensity of composite.Base material C/C composite loose structure has heat-blocking action, and outer C/SiC ceramic matric composite is that base material C/C composite plays oxidation protection effect, and potting resin improves material monolithic structural stability.Preparation technology is simple, and cost is low.
Description
Technical field
The present invention relates to the preparation method of a kind of resin-based and ceramic matrix hybrid composite material, particularly relate to the preparation method that a kind of laminated resin fills hybrid composite.
Background technology
Carbon/carbon (hereinafter referred to as C/C) composite has because of it characteristic that mechanical property under mechanical behavior under high temperature, particularly high temperature of low-density and excellence goes up not down, and becomes the preferred material of the thermojunction component of advanced aircraft.But, very easily be oxidized under C/C composite high temperature, oxidation can make its hole increase, structural weakening, the rapid reduction that causes intensity and other mechanical performances, and oxidation weight loss 1%, its intensity declines and reaches 10%, and (Throat Materials for Solid Rocket Motors, guided missile nose cone etc. as Gao Chongzhi ratio) C/C composite does not then have required high temperature resistance ablation energy ability in extreme environment.Therefore, the high-temp antioxidizing ablation problem of C/C composite is the bottleneck realizing its practical application.For this reason by the mechanical property of comprehensive carbon fiber excellence and good heat, the chemical stability of ceramic matrix, prepare a kind of by thermal protection, structural bearing and the anti-oxidant new function integrated composite combined.For anti-oxidation problem, realized by preparation SiC coating, SiC is outstanding oxidation-resistant material, has good antioxidation, the SiO of generation
2be the most oxidation resistant known material, protect C/C composite not to be oxidized by external environment when high temperature.And high temperature resistant problem, by improving in conjunction with phenolic resin-base composite, phenolic resins good heat resistance, the instantaneous superhigh temperature of ability, and also more excellent through its resistance to elevated temperatures of phenolic resins of modification, be widely used in heat-resisting ablator.And its raw material is sufficient, low price.
Application number be 201210149453.1 Chinese patent disclose a kind of carbon/carbon compound material SiC/C-AlPO
4the preparation method of-mullite ORC, is mixed to get powder A by silica flour and graphite powder; By Al
2o
3powder, WO
3powder and B
2o
3powder is mixed to get powder material B; Powder A and powder material B are mixed to get and embed powder C; Sample is put into graphite crucible, and add embedding powder C, graphite crucible is put into vertical vacuum furnace, passes into after argon gas adds thermal response as protective atmosphere and be down to room temperature, after cleaning up in ultrasonic wave with absolute ethyl alcohol, obtain carbon/carbon compound material carborundum transition zone; By C-AlPO
4join methyl alcohol with mullite powder to add iodine again and obtain suspension, this suspension is placed in water heating kettle, negative electrode selects the carbon/carbon compound material having prepared carborundum transition zone, sealing water heating kettle also puts it in ultrasonic-microwave generator, deposit rear taking-up sample, dry carbon/carbon composite wood SiC/C-AlPO
4-mullite anti-oxidation composite coating.The composite coating of preparation can protect C/C composites 322 hours at 1500 DEG C of still airs, and oxidation weight loss is less than 2%.
Application number be 200910022719.4 Chinese patent disclose a kind of preparation method of Improvement of The Oxidation Protective Coating For C/c Composites, treated C/C composite is embedded in powder, put into graphite crucible, carry out process in 1 ~ 3 hour at 1800 ~ 2200 DEG C, utilize Supersonic Plasma Spraying equipment by MoSi
2powder sprays to the C/C composite material surface with SiC transition zone, and preparation is had SiC/MoSi
2high temperature furnace put into by the C/C composite of coating, heat-treats 2 ~ 6 hours at 1200 ~ 1400 DEG C.The C/C composite that the method prepares more than 1650 DEG C in still air anti-oxidization time within 200 hours, bring up to 300 ~ 400 hours by prior art.
Composite prepared by above-mentioned two kinds of preparation methods improves the antioxygenic property of C/C composite, but high temperature protection problem unresolved.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, a kind of laminated resin is provided to fill the preparation method of hybrid composite, using graphite as liner, form prefabricated component at its surface wrap or braiding fiber C, and on prefabricated component, deposit pyrolysis C formation porous C/C precast body.Remove graphite core, at precast body surface wrap carbon cloth or C prepreg cloth, deposition skim pyrolysis C interface, chemical vapor infiltration prepares C matrix, forms C/SiC composite.Liner C/C precast body is immersed in deployed resin adhesive liquid, obtains lamination after hot-press solidifying and mix solar heat protection sandwich.It is characterized in that, comprise the preparation process of following order:
(1) using graphite as liner, prefabricated component is formed at its surface wrap or braiding fiber C;
(2) using methane or natural gas as the source of the gas of carbon, above-mentioned fiber C prefabricated component, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and heating rate is 8 ~ 10 DEG C/min, depositing temperature is 950 ~ 1350 DEG C, and sedimentation time is 50 ~ 150h;
(3) remove graphite core, obtain porous C/C precast body, and cleaned by ultrasonic vibration is carried out 2 ~ 4 times to porous body, then in 80 ~ 120 DEG C of baking ovens, dry 2 ~ 4h, until quality no longer changes;
(4) at precast body surface wrap carbon cloth or C prepreg cloth, deposition skim pyrolysis C interface;
(5) adopt CVI legal system for SiC matrix, using trichloromethyl silane as the source of the gas of SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature is 1000 ~ 1300 DEG C, and the time is 100 ~ 300h;
(6) with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immersed in resin adhesive liquid by liner C/C precast body, infiltrating time is 20 ~ 40min;
(7) the liner porous C/C precast body after then step 6 being processed is 120 ~ 150 DEG C in temperature, and pressure is 5 ~ 15MPa, hot-press solidifying 30 ~ 60min.
The advantage that the present invention has: 1. adopt in chemical gaseous phase permeation process and fiber reinforcement is not damaged, ensure that integrality and the intensity of composite; 2. base material C/C composite loose structure has heat-blocking action; 3. outer C/SiC ceramic matric composite is that base material C/C composite plays oxidation protection effect, and potting resin improves material monolithic structural stability; 4. preparation technology is simple, and cost is low.
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
Accompanying drawing explanation
Fig. 1 is that laminated resin fills hybrid composite longitdinal cross-section diagram
Diagram [10] porous C/C composite; [20] C/SiC composite; [30] phenolic resins
Embodiment 1
1, using graphite as liner, prefabricated component is formed at its surface wrap or braiding fiber C;
2, using methane or natural gas as the source of the gas of carbon, above-mentioned fiber C prefabricated component, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and heating rate is 8 DEG C/min, and depositing temperature is 1400 DEG C, and sedimentation time is 100h;
3, remove graphite core, obtain porous C/C precast body, and cleaned by ultrasonic vibration is carried out 2 times to porous body, then in 100 DEG C of baking ovens, dry 2.5h, until quality no longer changes;
4, at precast body surface wrap carbon cloth or C prepreg cloth, deposition skim pyrolysis C interface;
5, adopt CVI legal system for SiC matrix, using trichloromethyl silane as the source of the gas of SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature 1200 DEG C, the time is 200h;
6, with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immersed in resin adhesive liquid by liner C/C precast body, infiltrating time is 20min;
7, the liner porous C/C precast body after then step 6 being processed is 140 DEG C in temperature, and pressure is 10MPa, hot-press solidifying 40min.
Embodiment 2
1, using graphite as liner, prefabricated component is formed at its surface wrap or braiding fiber C;
2, using methane or natural gas as the source of the gas of carbon, above-mentioned fiber C prefabricated component, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and heating rate is 10 DEG C/min, and depositing temperature is 1000 DEG C, and sedimentation time is 150h;
3, remove graphite core, obtain porous C/C precast body, and cleaned by ultrasonic vibration is carried out 3 times to porous body, then in 120 DEG C of baking ovens, dry 3h, until quality no longer changes;
4, at precast body surface wrap carbon cloth or C prepreg cloth, deposition skim pyrolysis C interface;
5, adopt CVI legal system for SiC matrix, using trichloromethyl silane as the source of the gas of SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature is 1300 DEG C, and the time is 250h;
6, with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immersed in resin adhesive liquid by liner C/C precast body, infiltrating time is 30min;
7, the liner porous C/C precast body after then step 6 being processed is 130 DEG C in temperature, and pressure is 8MPa, hot-press solidifying 45min.
Above are only two detailed description of the invention of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. laminated resin fills a preparation method for hybrid composite, it is characterized in that the preparation process comprising following order:
(1) using graphite as liner, prefabricated component is formed at its surface wrap or braiding fiber C;
(2) using methane or natural gas as the source of the gas of carbon, above-mentioned fiber C prefabricated component, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and heating rate is 8 ~ 10 DEG C/min, depositing temperature is 950 ~ 1350 DEG C, and sedimentation time is 50 ~ 150h;
(3) remove graphite core, obtain porous C/C precast body, and cleaned by ultrasonic vibration is carried out 2 ~ 4 times to porous body, then in 80 ~ 120 DEG C of baking ovens, dry 2 ~ 4h, until quality no longer changes;
(4) at precast body surface wrap carbon cloth or C prepreg cloth, deposition skim pyrolysis C interface;
(5) adopt CVI legal system for SiC matrix, using trichloromethyl silane as the source of the gas of SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature is 1000 ~ 1300 DEG C, and the time is 100 ~ 300h;
(6) with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immersed in resin adhesive liquid by liner C/C precast body, infiltrating time is 20 ~ 40min;
(7) the liner porous C/C precast body after then step 6 being processed is 120 ~ 150 DEG C in temperature, and pressure is 5 ~ 15MPa, hot-press solidifying 30 ~ 60min.
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| CN106567246A (en) * | 2016-10-31 | 2017-04-19 | 航天材料及工艺研究所 | Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration |
| CN108484135A (en) * | 2018-04-17 | 2018-09-04 | 苏州宏久航空防热材料科技有限公司 | A kind of growth in situ ceramics reinforcing fiber resin composite materials |
| CN116039173B (en) * | 2023-02-26 | 2023-12-29 | 西北工业大学 | Carbon fiber powder reinforced carbon cloth-polyimide resin composite material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583671A (en) * | 2004-06-15 | 2005-02-23 | 深圳大学 | Method for preparing ceramic or ceramic-base composite materials |
| CN102718539A (en) * | 2012-07-05 | 2012-10-10 | 湖南金博复合材料科技有限公司 | Carbon/carbon/silicon carbide composite material thermal-insulation barrel and preparation method |
| CN102944320A (en) * | 2012-12-03 | 2013-02-27 | 中国航空工业集团公司北京长城计量测试技术研究所 | Cooling-free type high temperature sensor based on composite material |
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| US20070054103A1 (en) * | 2005-09-07 | 2007-03-08 | General Electric Company | Methods and apparatus for forming a composite protection layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583671A (en) * | 2004-06-15 | 2005-02-23 | 深圳大学 | Method for preparing ceramic or ceramic-base composite materials |
| CN102718539A (en) * | 2012-07-05 | 2012-10-10 | 湖南金博复合材料科技有限公司 | Carbon/carbon/silicon carbide composite material thermal-insulation barrel and preparation method |
| CN102944320A (en) * | 2012-12-03 | 2013-02-27 | 中国航空工业集团公司北京长城计量测试技术研究所 | Cooling-free type high temperature sensor based on composite material |
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