CN103724042B - A kind of lamination mixes the preparation method of solar heat protection sandwich - Google Patents
A kind of lamination mixes the preparation method of solar heat protection sandwich Download PDFInfo
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- CN103724042B CN103724042B CN201310412273.2A CN201310412273A CN103724042B CN 103724042 B CN103724042 B CN 103724042B CN 201310412273 A CN201310412273 A CN 201310412273A CN 103724042 B CN103724042 B CN 103724042B
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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, adopts CVI legal system for SiC matrix, forms C/SiC matrix material.At the carbon cloth of wooden model surface wrap preimpregnation modified alkyd resin glue liquid, then with porous C/C prefabricated component minor diameter fit, after hot-press solidifying, the demoulding forms phenolic resin-base composite, namely obtains lamination and mixes solar heat protection sandwich.Adopt in chemical gaseous phase permeation process and fiber reinforcement is not damaged, ensure that integrity and the intensity of matrix material.Base material C/C matrix material vesicular structure has heat-blocking action, and outer C/SiC ceramic matric composite is that base material C/C matrix material plays oxidation protection effect, and internal layer phenolic resin-base composite 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 base and ceramic matrix hybrid composite material, particularly relate to the preparation method that a kind of lamination mixes solar heat protection sandwich.
Background technology
Carbon/carbon (hereinafter referred to as C/C) matrix material 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 matrix material high temperature, oxidation can make its hole increase, structural weakening, the rapid reduction that causes intensity and other mechanical propertys, and oxidation weight loss 1%, its strength degradation reaches 10%, and (Throat Materials for Solid Rocket Motors, guided missile nose cone etc. as Gao Chongzhi ratio) C/C matrix material does not then have required high temperature resistance ablation energy ability in extreme environment.Therefore, the high-temp antioxidizing ablation problem of C/C matrix material 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 antioxygenation, the SiO of generation
2be the most oxidation resistant known material, protect C/C matrix material not to be oxidized by external environment when high temperature.And high temperature resistant problem, by improving in conjunction with phenolic resin-base composite, resol good heat resistance, the instantaneous ultrahigh-temperature of ability, and also more excellent through its resistance to elevated temperatures of resol 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 oxidation resistant coating, is mixed to get powder A by silica flour and Graphite Powder 99; 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 plumbago crucible, and add embedding powder C, plumbago crucible is put into vertical vacuum furnace, passes into argon gas and be down to room temperature as after protective atmosphere reacting by heating, after cleaning up in ultrasonic wave with dehydrated alcohol, obtain carbon/carbon compound material silicon carbide transition layer; 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 silicon carbide transition layer, sealing water heating kettle also puts it in ultrasonic-microwave producer, deposit rear taking-up sample, dry carbon/carbon composite wood SiC/C-AlPO
4-mullite anti-oxidation composite coating.The compound coating of preparation can protect C/C matrix materials 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 matrix material is embedded in powder, put into plumbago 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 layer, and preparation is had SiC/MoSi
2high Temperature Furnaces Heating Apparatus put into by the C/C matrix material of coating, heat-treats 2 ~ 6 hours at 1200 ~ 1400 DEG C.The C/C matrix material 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.
Matrix material prepared by above-mentioned two kinds of preparation methods improves the antioxidant property of C/C matrix material, 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 lamination is provided to mix the preparation method of solar heat protection sandwich, it is characterized in that 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, adopts CVI legal system for SiC matrix, forms C/SiC matrix material.At the carbon cloth of wooden model surface wrap preimpregnation modified alkyd resin glue liquid, then with porous C/C prefabricated component minor diameter fit, after hot-press solidifying, the demoulding forms phenolic resin-base composite.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 Sweet natural gas as the source of the gas of carbon, the prefabricated component of fiber C described in step 1, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and temperature rise rate is 8 ~ 10 DEG C/min, depositing temperature is 950 ~ 1350 DEG C, and depositing 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 insert, then in 80 ~ 120 DEG C of baking ovens, dry 2 ~ 4h, until quality no longer changes;
4. at C/C precast body surface wrap carbon cloth or C prepreg cloth;
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 silicon carbide, CVI temperature is 1000 ~ 1300 DEG C, and the time is 100 ~ 350h;
6. use anhydrous alcohol solution modified phenolic resins and solidifying agent, uniform stirring resin glue, the carbon fiber of oven dry is laid as in steeping vat, the resin adhesive liquid configured evenly is brushed on carbon cloth;
7. at wooden model surface wrap fiber C prepreg cloth, then with porous C/C prefabricated component minor diameter fit;
8. the porous C after then step 7 being processed/C precast body is 120 ~ 150 DEG C in temperature, and pressure is 5 ~ 15MPa, hot-press solidifying 30 ~ 60min;
9. after solidification terminates, the demoulding.
The advantage that the present invention has: 1. adopt in chemical gaseous phase permeation process and fiber reinforcement is not damaged, ensure that integrity and the intensity of matrix material; 2. base material C/C matrix material vesicular structure has heat-blocking action; 3. outer C/SiC ceramic matric composite is that base material C/C matrix material plays oxidation protection effect, and internal layer phenolic resin-base composite improves material monolithic structural stability; 4. preparation technology is simple, and cost is low.
Embodiment
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.
Embodiment 1
1. using graphite as liner, prefabricated component is formed at its surface wrap or braiding fiber C;
2. using methane or Sweet natural gas as the source of the gas of carbon, the prefabricated component of fiber C described in step 1, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and temperature rise rate is 8 DEG C/min, depositing temperature is 1150 DEG C, and depositing 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 insert, then in 100 DEG C of baking ovens, dry 2h, until quality no longer changes;
4. at C/C precast body surface wrap carbon cloth or C prepreg cloth;
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 silicon carbide, CVI temperature is 1100 DEG C, and the time is 250h;
6. use anhydrous alcohol solution modified phenolic resins and solidifying agent, uniform stirring resin glue, the carbon fiber of oven dry is laid as in steeping vat, the resin adhesive liquid configured evenly is brushed on carbon cloth;
7. at wooden model surface wrap fiber C prepreg cloth, then with porous C/C prefabricated component minor diameter fit;
8. the porous C after then step 7 being processed/C precast body is 130 DEG C in temperature, and pressure is 10MPa, hot-press solidifying 40min;
9. after solidification terminates, the demoulding.
Embodiment 2
1. using graphite as liner, prefabricated component is formed at its surface wrap or braiding fiber C;
2. using methane or Sweet natural gas as the source of the gas of carbon, the prefabricated component of fiber C described in step 1, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and temperature rise rate is 10 DEG C/min, depositing temperature is 1150 DEG C, and depositing 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 insert, then in 120 DEG C of baking ovens, dry 3h, until quality no longer changes;
4. at C/C precast body surface wrap carbon cloth or C prepreg cloth;
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 silicon carbide, CVI temperature is 1200 DEG C, and the time is 300h;
6. use anhydrous alcohol solution modified phenolic resins and solidifying agent, uniform stirring resin glue, the carbon fiber of oven dry is laid as in steeping vat, the resin adhesive liquid configured evenly is brushed on carbon cloth;
7. at wooden model surface wrap fiber C prepreg cloth, then with porous C/C prefabricated component minor diameter fit;
8. the porous C after then step 7 being processed/C precast body is 140 DEG C in temperature, and pressure is 12MPa, hot-press solidifying 50min;
9. after solidification terminates, the demoulding.
Above are only two embodiments 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. lamination mixes a preparation method for solar heat protection sandwich, 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 Sweet natural gas as the source of the gas of carbon, the prefabricated component of fiber C described in step 1, as diluent gas and carrier gas, is put into cvd furnace and is deposited pyrolysis C matrix by hydrogen or argon gas, and temperature rise rate is 8 ~ 10 DEG C/min, depositing temperature is 950 ~ 1350 DEG C, and depositing 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 insert, then in 80 ~ 120 DEG C of baking ovens, dry 2 ~ 4h, until quality no longer changes;
4. at C/C precast body surface wrap carbon cloth or C prepreg cloth;
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 silicon carbide, CVI temperature is 1000 ~ 1300 DEG C, and the time is 100 ~ 350h;
6. use anhydrous alcohol solution modified phenolic resins and solidifying agent, uniform stirring resin glue, the carbon fiber of oven dry is laid as in steeping vat, the resin adhesive liquid configured evenly is brushed on carbon cloth;
7. at wooden model surface wrap fiber C prepreg cloth, then with porous C/C prefabricated component minor diameter fit;
8. the porous C after then step 7 being processed/C precast body is 120 ~ 150 DEG C in temperature, and pressure is 5 ~ 15MPa, hot-press solidifying 30 ~ 60min;
9. after solidification terminates, the demoulding.
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| CN201310412273.2A CN103724042B (en) | 2013-09-11 | 2013-09-11 | A kind of lamination mixes the preparation method of solar heat protection sandwich |
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| CN201310412273.2A CN103724042B (en) | 2013-09-11 | 2013-09-11 | A kind of lamination mixes the preparation method of solar heat protection sandwich |
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| CN103724042A CN103724042A (en) | 2014-04-16 |
| CN103724042B true CN103724042B (en) | 2015-08-26 |
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| CN103954131B (en) * | 2014-04-17 | 2015-06-03 | 四川科达节能技术有限公司 | Inner liner material for industrial kiln furnace |
| TWI602794B (en) * | 2016-03-14 | 2017-10-21 | National Chung-Shan Institute Of Science And Tech | Ceramic composite materials production methods |
| CN107417277B (en) * | 2017-07-24 | 2020-06-16 | 西北工业大学 | Method for synergistically preparing heat insulation and antioxidation of porous carbon material |
| FR3071830B1 (en) * | 2017-10-02 | 2021-03-12 | Safran Ceram | PROCESS FOR MAKING A HOLLOW PART IN COMPOSITE MATERIAL WITH CERAMIC MATRIX |
| 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 |
| CN108794040B (en) * | 2018-06-29 | 2021-02-09 | 航天材料及工艺研究所 | Composite material based on melt siliconizing process, carbon/carbon porous body and preparation method thereof |
| CN111875402B (en) * | 2020-07-23 | 2023-04-07 | 西安超码科技有限公司 | Fiber winding reinforced graphite heating tube structure and preparation method thereof |
| CN113149684A (en) * | 2021-04-29 | 2021-07-23 | 上海骐杰碳素材料有限公司 | Carbon-carbon or carbon-ceramic composite material winding preform, product and preparation method thereof |
| CN113979771B (en) * | 2021-10-19 | 2022-10-11 | 中国航发沈阳黎明航空发动机有限责任公司 | Sandwich structure ceramic matrix composite containing heat conduction layer 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. |