CN105645966B - A kind of preparation method of C/C SiC ceramic matrix composite materials vacuum insulation panel - Google Patents
A kind of preparation method of C/C SiC ceramic matrix composite materials vacuum insulation panel Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 37
- 238000009413 insulation Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011153 ceramic matrix composite Substances 0.000 title abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 20
- 239000004917 carbon fiber Substances 0.000 claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 238000001291 vacuum drying Methods 0.000 claims abstract description 16
- 230000008595 infiltration Effects 0.000 claims abstract description 10
- 238000001764 infiltration Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910003978 SiClx Inorganic materials 0.000 claims description 2
- 238000009954 braiding Methods 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 19
- 239000011162 core material Substances 0.000 abstract description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 abstract description 5
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000002296 pyrolytic carbon Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 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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- 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
- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
- C04B35/573—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 carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention discloses a kind of preparation method of C/C SiC ceramic matrix composite materials vacuum insulation panel, prepares one layer of carbon fiber precast body on the heat insulation core material surface for being coated with graphite paper first;One layer of pyrolytic carbon is prepared in carbon fiber surface using chemical vapor infiltration again;Then molten silicon method of impregnation is used, the sample prepared is put into graphite crucible, embedded with Si powder, crucible is put into vacuum drying oven and heated, reaction temperature is 1,450 1550 DEG C, fills out the remaining micro-crack of envelope using chemical vapor infiltration depositing silicon carbide layers, a small sircle hole is finally opened in material shell bottom, envelope aperture is filled out with melt under vacuum conditions, obtains C/C SiC ceramic matrix composite material vacuum insulation panels.It can be used by the C/SiC composite vacuum heat-insulations plate material obtained by this method under 1500 DEG C of environment above, there is low thermal conductivity coefficient.
Description
Technical field
The present invention relates to a kind of preparation method of thermal insulation board, more particularly to a kind of C/C-SiC composites vacuum heat-insulation
The preparation method of plate.
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 " composite, Yin Hongfeng, Wei Jian metallurgical industry publishing house " describes what is prepared by chemical liquid phase method of impregnation
2D C/SiC composites are respectively 14~20.6W/m with the thermal conductivity factor in vertical carbon fiber direction in parallel carbon fiber direction
K and 5.9~7W/mK.Document " calculating of unidirectional C/C thermal conductivity of composite materials, Chen Jie, Xiong Xiang, Xiao Peng charcoal element technologies,
2008,27 (2):1-4 " describes heat conduction system of the unidirectional C/C composites in parallel carbon fiber direction with vertical carbon fiber direction
Number is respectively 40.65~51.12W/mK and 3.83~5.96W/mK.Foreign literature " OrtonaA, 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-layer ceramic based composites layer and middle carbon
SiClx froth bed is formed.The material has lower thermal conductivity factor than C/C and C/SiC composites, but is used for inside it simultaneously
It is antivacuum, therefore its thermal conductivity is still relatively large, so to ensure its using effect, then will increase the thickness of sic foam layer
Degree, to reach effect of heat insulation, this will just cause the weight of material to increase.From data above, answered for a kind of solid
Condensation material, can not meet the requirement of extremely low thermal conductivity factor, and invention is a kind of with extremely low thermal conductivity factor and can superhigh temperature resistant
Material then seems extremely urgent.
The content of the invention
The technical problem to be solved in the present invention is to overcome traditional vacuum heat-insulating plate can not be in hot environment
The problem of lower use, there is provided it is a kind of to use at high temperature, and C/C-SiC composite vacuum that thermal conductivity factor is extremely low
The preparation method of thermal insulation board.
Technical scheme is used by realize the purpose of the present invention:(1) in the outer surface of low thermal conductivity material core
One layer of graphite paper is coated, graphite paper thickness is 30-100 μm, and core is ceramic foam, ceramic fiber blanket, carbon fiber felt, core gas
Porosity is 70%~90%;(2) prefabricated component is formed in graphite paper surface wrap carbon fiber skin, carbon fiber skin is pre- by carbon fiber
Cloth composition is soaked, carbon fiber skin can also be made up of the carbon fiber by braiding, and prefabricated body thickness is 2-20mm;(3) will be prefabricated
Part is put into chemical vapor deposition stove, is warming up to 900-1200 DEG C, is passed through propylene, methane, hydrogen, argon gas, nitrogen, is passed through
Chemical vapor infiltration penetrates into carbon caused by propylene, methane decomposition in shell, shell is become C/C composite skeletons,
The porosity of shell is 5%~20%;(4) molten silicon method of impregnation is used, the sample prepared is put into graphite crucible, with Si powder
Embedding, crucible is put into vacuum drying oven and heated, and vacuum drying oven programming rate be 1-10 DEG C/min, and vacuum is 10 in stove-1- 10Pa,
Reaction temperature is 1450-1550 DEG C, reaction time 1-2h, and fine and close C/C-SiC material shells are made;(5) using chemistry
Vapor infiltration method, obtained fine and close C/C-SiC material shells in (4) step are continued into depositing silicon carbide layers, sedimentation time
For 10-30h, the remaining micro-crack of envelope, the C/C-SiC material shells being fully sealed are filled out;(6) at material shell bottom
Open a small sircle hole, hole diameter 0.1-2mm in portion;(7) sample is kept flat in vacuum drying oven, perforate is face-up, aperture upper part
One block of melt is placed, the volume of melt is 0.5-1 cubic centimetres;(8) vacuumize, vacuum in stove is reached below 1Pa, temperature
900-1750 DEG C is raised to, vacuum drying oven programming rate is 1-10 DEG C/min, is incubated 1-2h, is taken out after cooling, it is compound to obtain C/C-SiC
Material vacuum thermal insulation board.
Wherein:
Silica flour particle diameter described in step (4) is 10-500 μm.
Melt described in step (7) is buik silicon, one kind in simple glass, bulk silica.
The invention has the advantages that:1. material prepared by can use under 1500 DEG C of environment above;Material prepared by 2.
Material has extremely low thermal conductivity coefficient.
Brief description of the drawings
Fig. 1 is a kind of sectional view of C/SiC composites vacuum insulation panel;
10 be C/SiC material shells;20 be heat insulation core material;30 be melt.
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 ceramic fibre core, graphite paper thickness is 100 μm, the core porosity
For 90%:
(2) prefabricated component being formed in graphite paper surface wrap carbon fiber skin, carbon fiber skin is made up of carbon fibre initial rinse fabric,
Prefabricated body thickness is 3mm;
(3) prefabricated component is put into chemical vapor deposition stove, is warming up to 1100 DEG C, be passed through propylene, hydrogen, argon gas,
By chemical vapor infiltration, shell is set to become C/C composite skeletons, the porosity of shell is 10%;
(4) molten silicon method of impregnation is used, the sample prepared is put into graphite crucible, is embedded with Si powder, crucible is put into
Heated in vacuum drying oven, vacuum drying oven programming rate is 10 DEG C/min, and vacuum is 10Pa in stove, and reaction temperature is 1500 DEG C, reaction
Time is 1h, and fine and close C/C-SiC material shells are made;
(5) chemical vapor infiltration is used, obtained fine and close C/C-SiC material shells in (4) step are continued to sink
Product silicon carbide layer, sedimentation time 20h, fill out the remaining micro-crack of envelope, the C/C-SiC material shells being fully sealed;
(6) small sircle hole, hole diameter 1mm are opened in material shell bottom;
(7) sample is kept flat in vacuum drying oven, perforate is face-up, and aperture upper part places a buik silicon, and volume is 1 cube
Centimetre;
(8) vacuumize, vacuum in stove is reached 10-1Pa, temperature are raised to 1500 DEG C, and vacuum drying oven programming rate is 5 DEG C/
Min, 1h is incubated, is taken out after cooling, obtains C/C-SiC composite vacuum insulation panels.
Embodiment 2
(1) one layer of graphite paper is coated in the outer surface of ceramic fibre core, graphite paper thickness is 50 μm, and the core porosity is
80%;
(2) prefabricated component is formed in graphite paper surface weave carbon fiber skin, prefabricated body thickness is 5mm;
(3) prefabricated component is put into chemical vapor deposition stove, is warming up to 1000 DEG C, be passed through methane, hydrogen, argon gas,
By chemical vapor infiltration, shell is set to become C/C composite skeletons, the porosity of shell is 10%;
(4) molten silicon method of impregnation is used, the sample prepared is put into graphite crucible, is embedded with Si powder, crucible is put into
Heated in vacuum drying oven, vacuum drying oven programming rate is 10 DEG C/min, and vacuum is 1Pa in stove, and reaction temperature is 1500 DEG C, during reaction
Between be 1h, be made fine and close C/C-SiC material shells;
(5) chemical vapor infiltration is used, obtained fine and close C/C-SiC material shells in (4) step are continued to sink
Product silicon carbide layer, sedimentation time 30h, fill out the remaining micro-crack of envelope, the C/C-SiC material shells being fully sealed;
(6) small sircle hole, hole diameter 2mm are opened in material shell bottom;
(7) sample is kept flat in vacuum drying oven, perforate is face-up, and aperture upper part places one block of simple glass, volume 1
Cubic centimetre;
(8) vacuumize, vacuum in stove is reached 10-1Pa, temperature are raised to 900 DEG C, and vacuum drying oven programming rate is 10 DEG C/
Min, 1h is incubated, is taken out after cooling, obtains C/C-SiC composite vacuum insulation panels.
The single embodiment of the present invention is above are only, but the design concept of the present invention is not limited thereto, all profits
The change of unsubstantiality is carried out to the present invention with this design, the behavior for invading the scope of protection of the invention all should be belonged to.In every case it is
Any type of letter made without departing from the content of technical solution of the present invention, the technical spirit according to the present invention to above example
Single modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (3)
1. a kind of preparation method of C/C-SiC composites vacuum insulation panel, it is characterised in that including following sequential steps:
(1) one layer of graphite paper is coated in the outer surface of low thermal conductivity material core, graphite paper thickness is 30-100 μm, and core is
Ceramic foam, ceramic fiber blanket, carbon fiber felt, the core porosity are 70%~90%;
(2) graphite paper surface wrap carbon fiber skin formed prefabricated component, carbon fiber skin be made up of carbon fibre initial rinse fabric or
It is made up of the carbon fiber by braiding, prefabricated component thickness is 2-20mm;
(3) 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, nitrogen, carbon caused by propylene, methane decomposition is penetrated into carbon fiber skin by chemical vapor infiltration, makes carbon fine
Dimension shell becomes C/C composite skeletons, and the porosity of C/C composite skeletons is 5%~20%;
(4) molten silicon method of impregnation is used, the sample prepared is put into graphite crucible, is embedded with Si powder, crucible is put into vacuum
Heated in stove, vacuum drying oven programming rate is 1-10 DEG C/min, and vacuum is 10 in stove-1- 10Pa, reaction temperature 1450-1550
DEG C, reaction time 1-2h, fine and close C/C-SiC material shells are made;
(5) chemical vapor infiltration is used, obtained fine and close C/C-SiC material shells in (4) step are continued to deposit carbon
SiClx layer, sedimentation time 10-30h, fill out the remaining micro-crack of envelope, the C/C-SiC material shells being fully sealed;
(6) small sircle hole, hole diameter 0.1-2mm are opened in material shell bottom;
(7) sample is kept flat in vacuum drying oven, perforate is face-up, and aperture upper part places one block of melt, and the volume of melt is
0.5-1 cubic centimetres;
(8) vacuumize, vacuum in stove is reached below 1Pa, temperature is raised to 900-1750 DEG C, and vacuum drying oven programming rate is 1-10
DEG C/min, 1-2h is incubated, is taken out after cooling, obtains C/C-SiC composite vacuum insulation panels.
2. preparation method according to claim 1, it is characterised in that the Si powders footpath described in step (4) is 10-500 μm.
3. preparation method according to claim 1, it is characterised in that the melt described in step (7) is buik silicon, common glass
One kind in glass, bulk silica.
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CN108516858A (en) * | 2018-04-20 | 2018-09-11 | 苏州宏久航空防热材料科技有限公司 | A kind of high-temperature vacuum heat insulation composite material with ceramic fibre shell |
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US11624287B2 (en) * | 2020-02-21 | 2023-04-11 | Raytheon Technologies Corporation | Ceramic matrix composite component having low density core and method of making |
CN113045325B (en) * | 2021-03-31 | 2022-10-14 | 西北工业大学 | Preparation method of high-strength carbon/carbon-silicon carbide composite material |
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 |
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JP3120884B2 (en) * | 1991-12-13 | 2000-12-25 | 東芝セラミックス株式会社 | SiC coated C / C composite |
JP2010254484A (en) * | 2009-04-21 | 2010-11-11 | Mitsubishi Electric Corp | C/SiC HONEYCOMB COMPOSITE BODY AND METHOD FOR PRODUCING THE SAME |
CN102718539B (en) * | 2012-07-05 | 2014-06-04 | 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 |
CN103121858A (en) * | 2013-01-23 | 2013-05-29 | 西北工业大学 | Method for improving connection performance of carbon/carbon composites |
CN103342561B (en) * | 2013-06-26 | 2014-11-05 | 中国人民解放军国防科学技术大学 | C/ZrC composite material prepared on basis of vapor infiltration reaction, preparation method thereof and equipment for process |
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