CN107504325A - A kind of preparation method of high temperature VIP composites - Google Patents
A kind of preparation method of high temperature VIP composites Download PDFInfo
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- CN107504325A CN107504325A CN201710656015.7A CN201710656015A CN107504325A CN 107504325 A CN107504325 A CN 107504325A CN 201710656015 A CN201710656015 A CN 201710656015A CN 107504325 A CN107504325 A CN 107504325A
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- high temperature
- carbon fiber
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- composites
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L59/00—Thermal insulation in general
- F16L59/02—Shape or form of insulating materials, with or without coverings integral with the insulating materials
- F16L59/028—Composition or method of fixing a thermally insulating material
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- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
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Abstract
The present invention discloses a kind of preparation method of high temperature VIP composites, first one layer of graphite paper is coated in the outer surface of high temperature resistant low thermal conductivity material core, then wind carbon fiber skin in the core outer surface for being surrounded by graphite paper and form prefabricated component, prefabricated component is put into chemical vapor deposition stove, deposit pyrolytic carbon and carry out density, form C/C shells, sedimentation time is 100 200h, vacuum is 0.1Pa~10Pa in cvd furnace, the ceramic crucible for filling silica flour or silico briquette is placed in the bottom of vacuum high temperature furnace, the sample deposited is suspended on above ceramic crucible at 5 10cm, it is warming up to 1,500 1600 DEG C, it is incubated 10 50h, vacuum is 0.01 1Pa in holding furnace, obtain high temperature VIP composites.The material can be used at high temperature, and have extremely low thermal conductivity coefficient, and the silicon carbide layer of even compact is formed in C/C case surfaces, and secondary encapsulation effect is played to compact outer shell, prevents ambient atmos and penetrates into inside core.
Description
Technical field
The present invention relates to a kind of heat-insulating material preparation method, more particularly to a kind of preparation side of high temperature VIP composites
Method.
Background technology
Novel high speed aerospace craft have the characteristics that the reaction time it is short, it is global it is quick reach, be each Aero-Space in the world
One of space technology research focus that big country competitively carries out.The flying speed of some novel high speed aerospace crafts is up to 10 horses
Conspicuous, the flight time, the Aerodynamic Heating on aircraft fuselage surface was extremely serious, and its superhigh temperature spot temperature up to dozens of minutes
Up to more than 1600 DEG C, this harsh thermal environment limits plus the space that compact housing construction is brought, to thermal protection system
Propose thundering challenge.The heat-barrier material used in thermal protection system must be provided simultaneously with superhigh temperature resistant, ultralow thermal conductivity
The performance characteristics such as rate and sufficient intensity, the heat that could effectively obstruct fuselage surface or superhigh temperature position are propagated toward fuselage interior,
It can just bear superhigh temperature, the drastically harsh heating power environment such as thermal shock, judder simultaneously.Ceramic matric composite has intensity
Height, can high temperature resistant the features such as, but these materials all have higher thermal conductivity factor, if being used as heat-insulating material certainly will increase
The thickness and weight of material.If by ceramic matric composite as shell, adiabatic core is filled in inside, then make it that material can be
Used under high temperature, not only weight substantially reduces, while also has low thermal conductivity coefficient.This is by with huge application prospect, spy
It is not in national defense industry, Aero-Space etc..
Document " Chinese patent of Application No. 200520112605.6 " discloses a kind of vacuum heat-insulating plate.The material includes
There is one layer of nylon protective layer barrier film layer and warming plate, the outer surface of described barrier film layer, and its inner surface has layer of polyethylene
Hot sealing layer.Document " Chinese patent of Application No. 201010235788.6 " discloses another vacuum heat-insulating plate.Protected in tabular
Being set among adiabator through the cavity of warming plate, the inwall in cavity is covered with reflectance coating, and getter is put into cavity,
Vacuumized after being wrapped up with high-resistant diaphragm, form cavity type vacuum heat-insulating plate.Both the above vacuum heat-insulating plate is former using vacuum insulation
Reason is made, and completely cuts off heat transfer by improving internal vacuum to greatest extent, has extremely low thermal conductivity coefficient, but the material is only
It can be used under low temperature environment, can not use in the case of a high temperature.Document " publish by composite, Yin Hongfeng, Wei Jian metallurgical industry
Society " is described by 2D C/SiC composites prepared by chemical liquid phase method of impregnation in parallel carbon fiber direction and vertical carbon fiber side
To thermal conductivity factor be respectively 14~20.6W/mK and 5.9~7W/mK.Document be " unidirectional C/C thermal conductivity of composite materials
Calculate, Chen Jie, Xiong Xiang, Xiao Peng charcoal element technologies, 2008,27 (2)：1-4 " describes unidirectional C/C composites in parallel carbon fiber
Direction is respectively 40.65~51.12W/mK and 3.83~5.96W/mK with the thermal conductivity factor in vertical carbon fiber direction.It is external
Document " Ortona A, Gianella S, Pusterla S.An integrated assembly method of sandwich
structured ceramic matrix composites[J].Journal of the European Ceramic
Society, 2011,31 (9)：1821-1826. " disclose a kind of sandwich structure composite.The material is by upper and lower two layers
Ceramic matric composite layer and middle carborundum froth bed are formed.The material has lower lead than C/C and C/SiC composites
Hot coefficient, but it is internal and antivacuum for it, and heat radiation heat transfer is serious under high temperature, therefore its thermal conductivity is still relatively large, institute
To ensure its using effect, then it will increase the thickness of sic foam layer, to reach effect of heat insulation, this will just cause material
The weight increase of material.From data above, for a kind of solid composite, extremely low thermal conductivity factor can not be met
It is required that a kind of material with extremely low thermal conductivity factor and energy superhigh temperature resistant of invention then seems extremely urgent.
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 high temperature VIP composites,
It is characterized in that comprise the following steps：
A kind of preparation method of high temperature VIP composites, it is characterised in that comprise the following steps：
(1) one layer of graphite paper is coated in the outer surface of high temperature resistant low thermal conductivity material core, the thickness of graphite paper is 0.1
~0.5mm, core are ceramic foam, ceramic fiber blanket, any of carbon fiber felt or several, the core porosity is 70%~
90%；
(2) wind carbon fiber skin in the core outer surface for being surrounded by graphite paper and form prefabricated component, carbon fiber skin is fine by carbon
Prepreg cloth composition is tieed up, carbon fiber skin can also be formed by the carbon fiber by braiding, and carbon fiber skin thickness is 2~4mm；
(4) prefabricated component is put into chemical vapor deposition stove, is warming up to 900-1200 DEG C, be passed through propylene, methane, hydrogen
Gas, argon gas, carbon caused by propylene, methane decomposition is penetrated into by chemical vapor infiltration density is carried out in shell, form C/C
Shell, sedimentation time 100-200h, vacuum is 0.1Pa~10Pa in cvd furnace；
(5) ceramic crucible for filling silica flour or silico briquette is placed in the bottom of vacuum high temperature furnace, will be deposited in step (4)
Sample be suspended on 5-10cm places above ceramic crucible, be warming up to 1500-1600 DEG C, insulation 10-50h, vacuum in holding furnace
For 0.01-1Pa；
(6) high temperature VIP composites are obtained, material internal vacuum is 0.01Pa~1Pa.
The invention has the advantages that：1st, prepared material surface is coat of silicon carbide so that the material can be at 1500 DEG C
Used under environment above；2nd, prepared material internal low pressure, heat transfer and the thermal convection current of material internal gas are effectively alleviated, because
This has extremely low thermal conductivity coefficient；3rd, silica flour melts and produces silicon steam under high temperature, may penetrate into inside C/C outer shells, and
The coat of silicon carbide to form even compact is reacted with the pyrolytic carbon deposited, the compactness of outer shell is improved, to compact outer shell
Secondary encapsulation effect is played, prevents ambient atmos and penetrates into inside core.
Brief description of the drawings
Fig. 1 is a kind of high temperature VIP composite sectional views.
10 be C/C material shells in diagram；20 be low thermal conductivity material core；30 be SiC external coatings.
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) one layer of graphite paper is coated in the outer surface of high temperature resistant low thermal conductivity material core, the thickness of graphite paper is
0.1mm, core are ceramic foam, and the core porosity is 85%；
(2) wind carbon fiber skin in the core outer surface for being surrounded by graphite paper and form prefabricated component, carbon fiber skin is fine by carbon
Prepreg cloth composition is tieed up, carbon fiber skin thickness is 3mm；
(4) prefabricated component is put into chemical vapor deposition stove, is warming up to 900-1200 DEG C, be passed through propylene, methane, hydrogen
Gas, argon gas, carbon caused by propylene, methane decomposition is penetrated into by chemical vapor infiltration density is carried out in shell, form C/C
Shell, sedimentation time 150h, vacuum is 5Pa in cvd furnace；
(5) placed in the bottom of vacuum high temperature furnace and fill silica flour alumina crucible, the sample deposited is suspended on ceramics
Above crucible at 5cm, 1550 DEG C are warming up to, is incubated 20h, vacuum is 0.1Pa in holding furnace；
(6) high temperature VIP composites, thermal conductivity factor 0.047W/mK are obtained.
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 preparation method of high temperature VIP composites, it is characterised in that comprise the following steps：
(1) coat one layer of graphite paper in the outer surface of high temperature resistant low thermal conductivity material core, the thickness of graphite paper for 0.1~
0.5mm, core are ceramic foam, ceramic fiber blanket, any of carbon fiber felt or several, the core porosity is 70%~
90%；
(2) wind carbon fiber skin in the core outer surface for being surrounded by graphite paper and form prefabricated component, carbon fiber skin is pre- by carbon fiber
Cloth composition is soaked, carbon fiber skin can also be formed by the carbon fiber by braiding, and carbon fiber skin thickness is 2~4mm；
(4) prefabricated component is put into chemical vapor deposition stove, is warming up to 900-1200 DEG C, be passed through propylene, methane, hydrogen,
Argon gas, carbon caused by propylene, methane decomposition is penetrated into by chemical vapor infiltration density is carried out in shell, formed outside C/C
Shell, sedimentation time 100-200h, vacuum is 0.1Pa~10Pa in cvd furnace；
(5) ceramic crucible for filling silica flour or silico briquette, the sample that will have been deposited in step (4) are placed in the bottom of vacuum high temperature furnace
Product are suspended on above ceramic crucible at 5-10cm, are warming up to 1500-1600 DEG C, are incubated 10-50h, and vacuum is in holding furnace
0.01-1Pa；
(6) high temperature VIP composites are obtained, material internal vacuum is 0.01Pa~1Pa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113045325A (en) * | 2021-03-31 | 2021-06-29 | 西北工业大学 | Preparation method of high-strength carbon/carbon-silicon carbide composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030135A (en) * | 2013-01-05 | 2013-04-10 | 航天材料及工艺研究所 | Preparation method of antioxidant high-heat-conductivity foamy carbon material |
| CN103193514A (en) * | 2013-04-07 | 2013-07-10 | 山东国晶新材料有限公司 | Silicon steam corrosion resistant internal coating for directly protecting carbon fiber and in-situ preparation method thereof |
| CN105645966A (en) * | 2015-12-30 | 2016-06-08 | 南京航空航天大学 | Preparation method of C/C-SiC (carbon/carbon-silicon carbide) composite material vacuum heat insulation plate |
| CN106145989A (en) * | 2015-03-26 | 2016-11-23 | 北京赛恩高科技有限公司 | A kind of preparation method of polycrystalline ingot furnace thermal field cover plate |
-
2017
- 2017-07-29 CN CN201710656015.7A patent/CN107504325A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030135A (en) * | 2013-01-05 | 2013-04-10 | 航天材料及工艺研究所 | Preparation method of antioxidant high-heat-conductivity foamy carbon material |
| CN103193514A (en) * | 2013-04-07 | 2013-07-10 | 山东国晶新材料有限公司 | Silicon steam corrosion resistant internal coating for directly protecting carbon fiber and in-situ preparation method thereof |
| CN106145989A (en) * | 2015-03-26 | 2016-11-23 | 北京赛恩高科技有限公司 | A kind of preparation method of polycrystalline ingot furnace thermal field cover plate |
| CN105645966A (en) * | 2015-12-30 | 2016-06-08 | 南京航空航天大学 | Preparation method of C/C-SiC (carbon/carbon-silicon carbide) composite material vacuum heat insulation plate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113045325A (en) * | 2021-03-31 | 2021-06-29 | 西北工业大学 | Preparation method of high-strength carbon/carbon-silicon carbide composite material |
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Application publication date: 20171222 |