CN103722784A - Preparation method of laminated hybrid composite filled with resin - Google Patents
Preparation method of laminated hybrid composite filled with resin Download PDFInfo
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- CN103722784A CN103722784A CN201310412156.6A CN201310412156A CN103722784A CN 103722784 A CN103722784 A CN 103722784A CN 201310412156 A CN201310412156 A CN 201310412156A CN 103722784 A CN103722784 A CN 103722784A
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Abstract
A preparation method of laminated hybrid composite filled with resin is characterized in that graphite is taken as a liner, a C fiber is wound or woven on the surface of the graphite to form a prefabricated part, and C is subjected to deposition and pyrolysis on the prefabricated part so as to form a C/C prefabricated body; a graphite core is removed, carbon cloth or C prepreg is wound on the surface of the prefabricated body, a thin-film pyrolysis C interface is deposited, a SiC matrix is prepared with a CVI (chemical vapor infiltration) method at the temperature of 1,100-1,300 DEG C, and a C/SiC composite is formed; and the liner C/C prefabricated part is impregnated in a blended resin adhesive, and the laminated hybrid heatproof composite structured material is obtained after hot-press solidification. According to the preparation method, a fiber framework is not damaged during the CVI process, and the integrity and strength of the composite are guaranteed; the substrate C/C composite with a porous structure has a heat insulating function, an outer-layer C/SiC ceramic matrix composite performs an oxidation protection function for the substrate C/C composite, and filled resin improves the overall structural stability of the material; and the preparation technology is simple, and the cost is low.
Description
Technical field
The present invention relates to the preparation method of a kind of resin-based and ceramic base hybrid composite, particularly relate to a kind of preparation method of lamination resin filling hybrid composite.
Background technology
Carbon/carbon (hereinafter to be referred as C/C) composite, because it has the characteristic that under low-density and excellent mechanical behavior under high temperature, particularly high temperature, mechanical property goes up not down, becomes the preferred material of the thermojunction member of advanced aircraft.But, very easily oxidation under C/C composite high temperature, oxidation can make its hole increase, structure weaken, cause the rapid reduction of intensity and other mechanical performances, and oxidation weight loss 1%, its intensity declines and reaches 10%, and (as the Throat Materials for Solid Rocket Motors of Gao Chongzhi ratio, guided missile nose cone etc.) C/C composite does not 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 of realizing its practical application.Good heat, the chemical stability of mechanical property by comprehensive carbon fiber excellence and ceramic matrix, prepares a kind of by thermal protection, structural bearing and the anti-oxidant new function integrated composite combining for this reason.For anti-oxidation problem, by preparation SiC coating, realize, SiC is outstanding oxidation-resistant material, has good antioxidation, the SiO of generation
2be the most oxidation resistant known material, protect C/C composite by external environment, not to be oxidized 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 abundance, low price.
Application number is that 201210149453.1 Chinese patent discloses 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 to embedding powder C; Sample is put into graphite crucible, and add embedding powder C, graphite crucible is put into vertical vacuum furnace, pass 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
4joining methyl alcohol with mullite powder adds iodine to obtain suspension again, this suspension is placed in water heating kettle, negative electrode is selected the carbon/carbon compound material of having prepared carborundum transition zone, sealing water heating kettle also puts it in ultrasonic-microwave generator, deposit rear taking-up sample, be dried to obtain carbon/carbon composite wood SiC/C-AlPO
4-mullite anti-oxidation composite coating.The composite coating of preparation can be protected C/C composites 322 hours at 1500 ℃ of still airs, and oxidation weight loss is less than 2%.
Application number is the preparation method that 200910022719.4 Chinese patent discloses a kind of Improvement of The Oxidation Protective Coating For C/c Composites, treated C/C composite is embedded in powder, put into graphite crucible, at 1800～2200 ℃, carry out processing for 1～3 hour, utilize Supersonic Plasma Spraying equipment by MoSi
2powder sprays to the C/C composite material surface with SiC transition zone, will be prepared with SiC/MoSi
2the C/C composite of coating is put into high temperature furnace, at 1200～1400 ℃, heat-treats 2～6 hours.The C/C composite that the method prepares more than 1650 ℃ in still air anti-oxidization time by prior art, within 200 hours, bring up to 300～400 hours.
Composite prepared by above-mentioned two kinds of preparation methods has improved 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 is to overcome the deficiencies in the prior art, a kind of preparation method of lamination resin filling hybrid composite is provided, using graphite as liner, on its surface, be wound around or braiding C fiber formation prefabricated component, and on prefabricated component, deposit pyrolysis C formation porous C/C precast body.Remove graphite core, on precast body surface, be wound around carbon cloth or C preimpregnation cloth, deposition skim pyrolysis C interface, chemical vapor infiltration is prepared C matrix, forms C/SiC composite.Liner C/C precast body is immersed in deployed resin adhesive liquid, after hot-press solidifying, obtain lamination and mix solar heat protection sandwich.It is characterized in that, comprise the preparation process of following order:
(1), using graphite as liner, on its surface, be wound around or braiding C fiber formation prefabricated component;
(2) source of the gas using methane or natural gas as carbon, hydrogen or argon gas, as diluent gas and carrier gas, are put into cvd furnace by above-mentioned C fiber preform and are deposited pyrolysis C matrix, and heating rate is 8～10 ℃/min, depositing temperature is 950～1350 ℃, and sedimentation time is 50～150h;
(3) remove graphite core, obtain porous C/C precast body, and porous body is carried out to cleaned by ultrasonic vibration 2～4 times, then in 80～120 ℃ of baking ovens, dry 2～4h, until quality no longer changes;
(4) on precast body surface, be wound around carbon cloth or C preimpregnation cloth, deposition skim pyrolysis C interface;
(5) adopt CVI legal system for SiC matrix, the source of the gas using trichloromethyl silane as SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature is 1000～1300 ℃, the time is 100～300h;
(6) with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immerses liner C/C precast body in resin adhesive liquid, and infiltrating time is 20～40min;
(7) by liner porous C/C precast body after treatment step 6, in temperature, be then 120～150 ℃, pressure is 5～15MPa, hot-press solidifying 30～60min.
The present invention has advantages of: 1. adopt in chemical gaseous phase permeation process fiber reinforcement is not damaged, guaranteed 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, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
Accompanying drawing explanation
Fig. 1 is lamination resin filling 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, on its surface, be wound around or braiding C fiber formation prefabricated component;
2, the source of the gas using methane or natural gas as carbon, hydrogen or argon gas, as diluent gas and carrier gas, are put into cvd furnace by above-mentioned C fiber preform and are deposited pyrolysis C matrix, and heating rate is 8 ℃/min, and depositing temperature is 1400 ℃, and sedimentation time is 100h;
3, remove graphite core, obtain porous C/C precast body, and porous body is carried out to cleaned by ultrasonic vibration 2 times, then in 100 ℃ of baking ovens, dry 2.5h, until quality no longer changes;
4, on precast body surface, be wound around carbon cloth or C preimpregnation cloth, deposition skim pyrolysis C interface;
5, adopt CVI legal system for SiC matrix, the source of the gas using trichloromethyl silane as SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, 1200 ℃ of CVI temperature, the time is 200h;
6, with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immerses liner C/C precast body in resin adhesive liquid, and infiltrating time is 20min;
7, by liner porous C/C precast body after treatment step 6, in temperature, be then 140 ℃, pressure is 10MPa, hot-press solidifying 40min.
Embodiment 2
1,, using graphite as liner, on its surface, be wound around or braiding C fiber formation prefabricated component;
2, the source of the gas using methane or natural gas as carbon, hydrogen or argon gas, as diluent gas and carrier gas, are put into cvd furnace by above-mentioned C fiber preform and are deposited pyrolysis C matrix, and heating rate is 10 ℃/min, and depositing temperature is 1000 ℃, and sedimentation time is 150h;
3, remove graphite core, obtain porous C/C precast body, and porous body is carried out to cleaned by ultrasonic vibration 3 times, then in 120 ℃ of baking ovens, dry 3h, until quality no longer changes;
4, on precast body surface, be wound around carbon cloth or C preimpregnation cloth, deposition skim pyrolysis C interface;
5, adopt CVI legal system for SiC matrix, the source of the gas using trichloromethyl silane as SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature is 1300 ℃, the time is 250h;
6, with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immerses liner C/C precast body in resin adhesive liquid, and infiltrating time is 30min;
7, by liner porous C/C precast body after treatment step 6, in temperature, be then 130 ℃, pressure is 8MPa, hot-press solidifying 45min.
Above are only two specific embodiment of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for lamination resin filling hybrid composite, is characterized in that comprising the preparation process of following order:
(1), using graphite as liner, on its surface, be wound around or braiding C fiber formation prefabricated component;
(2) source of the gas using methane or natural gas as carbon, hydrogen or argon gas, as diluent gas and carrier gas, are put into cvd furnace by above-mentioned C fiber preform and are deposited pyrolysis C matrix, and heating rate is 8～10 ℃/min, depositing temperature is 950～1350 ℃, and sedimentation time is 50～150h;
(3) remove graphite core, obtain porous C/C precast body, and porous body is carried out to cleaned by ultrasonic vibration 2～4 times, then in 80～120 ℃ of baking ovens, dry 2～4h, until quality no longer changes;
(4) on precast body surface, be wound around carbon cloth or C preimpregnation cloth, deposition skim pyrolysis C interface;
(5) adopt CVI legal system for SiC matrix, the source of the gas using trichloromethyl silane as SiC, using hydrogen or argon gas as diluent gas and carrier gas, chemical vapor infiltration carborundum, CVI temperature is 1000～1300 ℃, the time is 100～300h;
(6) with anhydrous alcohol solution phenol-formaldehyde resin modified and curing agent, uniform stirring resin glue, immerses liner C/C precast body in resin adhesive liquid, and infiltrating time is 20～40min;
(7) by liner porous C/C precast body after treatment step 6, in temperature, be then 120～150 ℃, pressure is 5～15MPa, hot-press solidifying 30～60min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116039173A (en) * | 2023-02-26 | 2023-05-02 | 西北工业大学 | Carbon fiber powder reinforced carbon cloth-polyimide resin composite material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116039173A (en) * | 2023-02-26 | 2023-05-02 | 西北工业大学 | Carbon fiber powder reinforced carbon cloth-polyimide resin composite material and preparation method thereof |
| 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 |
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Address after: 215400 Chengxiang City, Taicang Province town of the People South Road, No. 162, No. Patentee after: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. Address before: 215400 people's road, Jiangsu, Taicang Hua Xu apartment C412 Patentee before: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. |