CN105506579A - Preparation method of graphene coated silicon carbide nanowire - Google Patents
Preparation method of graphene coated silicon carbide nanowire Download PDFInfo
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- CN105506579A CN105506579A CN201510933922.2A CN201510933922A CN105506579A CN 105506579 A CN105506579 A CN 105506579A CN 201510933922 A CN201510933922 A CN 201510933922A CN 105506579 A CN105506579 A CN 105506579A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
Abstract
The invention discloses a preparation method of a graphene coated silicon carbide nanowire. The technological process is easy to achieve, and the deposition temperature of the silicon carbide nanowire is relatively low, so that the preparation cost is reduced, and the preparation technology is simplified; the graphene coated silicon carbide nanowire obtained through the method is high in straightness and uniform in diameter distribution; when the product is utilized as a reinforcing phase of a ceramic material, the interface bonding between the silicon carbide nanowire and a ceramic matrix can be strengthened; and besides, the graphene on the surface of the silicon carbide nanowire has reinforcing and toughening effects.
Description
Technical field
The present invention relates to a kind of preparation method of graphene coated silicon carbide nanometer line.
Background technology
Silicon carbide is as third generation semiconductor material, there is excellent physical and chemical performance: as high thermostability, good heat conductivity, high rigidity and high-modulus, wide energy band, good anti-oxidant and corrosion resistance, these properties make SiC be used widely in fields such as aerospace, chemical industry, mechanical industry, metallurgical industry, frictional wear, optics, electronics and nuclear energy.And one dimension silicon carbide nano material is except having the good characteristic of silicon carbide block materials, also have outstanding electricity and mechanical property, therefore, silicon carbide nanometer line can be used as the desirable activeness and quietness materials'use of matrix material, has broad application prospects.
In recent years, scholars adopts diverse ways to prepare various informative silicon carbide nanometer line in succession, but the surface of most of silicon carbide nanometer line is smooth.And the silicon carbide nanometer line that document " G.Y.Zhang; J.Xin; E.G.Wang, Appl.Phys.Lett.84 (2004) 2646-2648. " report has complex surface structures can embed matrix better as activeness and quietness material, improve activeness and quietness effect.So far, investigators have successfully prepared the silicon carbide nanometer line of some complex constructions.Such as, document " J.Wei; K.Z.Li; H.J.Li; Q.G.Fu, L.Zhang, Mater.Chem.Phys.95 (2006) 140-144. " with silicon-dioxide and graphite for raw material, when 1400 DEG C of catalyst-frees are auxiliary, prepared the silicon carbide nanometer line of item chain by chemical gas-phase reaction method; Adopt chemical Vapor deposition process, by Si, SiO in document " J.Z.Guo, Y.Zuo, Z.J.Li, W.D.Gao, J.L.Zhang, PhysicaE39 (2007) 262-266. " report
2and CH
4issue biochemical reaction at 1350 DEG C and prepare the silicon carbide nanometer line with fin shape surface tissue; Document " J.Wei, K.Z.Li, J.Chen; H.D.Yuan, G.P.He, C.L.Yang; J.Am.Ceram.Soc.96 (2013) 627-633. " also adopts chemical Vapor deposition process, has prepared a kind of silicon carbide nanometer line of chain-like structure when catalyst-free.But the most complex process of these preparation methods, surface does not have graphene coated yet, also there is the shortcomings such as bonding force is not high, effect is not strong when using as strongthener.
Summary of the invention
For solving the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of graphene coated silicon carbide nanometer line.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A preparation method for graphene coated silicon carbide nanometer line, comprises the steps:
S1, pre-treatment is carried out to matrix sample: by clean with distilled water wash again after the carbon/carbon compound material sanding and polishing of porous, be placed in baking oven and dry;
S2, the matrix sample of drying is immersed in catalyzer nickel nitrate solution, be dipped to matrix specimen surface and no longer produce bubble, illustrate that the air in the vesicular structure of carbon/carbon compound material is discharged and is all filled with nickel nitrate solution, taking-up matrix sample is placed in baking oven dries;
S3, the carbon/carbon compound material immersion treatment crossed are as depositing base, and binding hangs in the deposition region of vertical gaseous phase deposition stove;
S4, cvd furnace is evacuated to 2kPa, the empty 30min of fidelity observes the reading of vacuumometer to determine whether gas leakage, more logical argon gas is to normal pressure, and repetitive operation three times, makes the oxygen content in cvd furnace drop to minimum;
S5, the furnace temperature of cvd furnace is risen to depositing temperature, in cvd furnace, continue logical argon gas in temperature-rise period, air outlet stays open state; After temperature; carrier gas hydrogen is passed in the bubbling bottle that METHYL TRICHLORO SILANE is housed; reactant gas source METHYL TRICHLORO SILANE is brought in the furnace of cvd furnace; regulate the flow of the dilution argon gas passing into burner hearth and dilution hydrogen simultaneously; control the dividing potential drop of reactant gases; after reactant gas source enters reaction flat-temperature zone reaction 10-120min; close dilution hydrogen; carrier gas hydrogen and reactant gas source is closed again after continuing reaction for some time; the cooling of power-off simultaneously; burner hearth is made to naturally cool to room temperature, logical argon shield in temperature-fall period.
In order to understand the present invention better, reaction mechanism of the present invention is presumed as follows: in earlier stage, METHYL TRICHLORO SILANE cracking when hydrogen participates in reaction generates silicon carbide nanometer line in reaction; In the reaction later stage, after closing dilution hydrogen, the cracking of METHYL TRICHLORO SILANE is the Graphene at surfactivity larger silicon carbide nanometer line Surface Creation preferentially, thus has obtained the silicon carbide nanometer line of graphene coated.
Preferably, aforementioned substrates sample is the carbon/carbon compound material of porous, and density is 1.68-1.75g/cm
3, be of a size of 20 × 10 × 5mm
3.
More preferably, in abovementioned steps S1, by No. 800 and No. 1000 sand paper, matrix sample is polished successively.
Again preferably, in aforementioned nickel nitrate solution, the mass percentage of nickelous nitrate is 5%-50%.
Further preferably, in abovementioned steps S3, the carbon/carbon compound material crossed by carbon fiber binding immersion treatment.
Again further preferably, in abovementioned steps S5, depositing temperature is 1050 DEG C-1300 DEG C, and the flow of described dilution argon gas, dilution hydrogen and carrier gas hydrogen is respectively 200-800sccm, 100-600sccm and 50-200sccm.
Preferably, in abovementioned steps S5, temperature rise rate is 10 DEG C/min.
Further, the purity of aforementioned dilution argon gas, dilution hydrogen and carrier gas hydrogen is all greater than 99.99%.
Usefulness of the present invention is: preparation method's technological process of the present invention is simple and easy to realize, the depositing temperature of silicon carbide nanometer line is lower, reduce preparation cost and simplify preparation technology, high and the uniform graphene coated silicon carbide nanometer line of diameter Distribution of linearity is obtained by the method, when this product uses as the wild phase of stupalith, can interface cohesion between strengthened silicon carbide nano wire and ceramic matrix; In addition, the Graphene on silicon carbide nanometer line surface also has activeness and quietness effect.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph figure of embodiments of the invention 1 product;
Fig. 2 is the XRD figure of embodiments of the invention 1 product;
Fig. 3 is the transmission electron microscope photo figure of embodiments of the invention 1 product, wherein, a () is for product transmission electron microscope photo and choose diffracting spectrum, b () is product high resolution photo, c () is the high resolution enlarged view in silicon carbide nanometer line bar portion, the high resolution photo that (d) is nanowire surface Graphene;
Fig. 4 is the energy spectrogram of embodiments of the invention 1 product, and wherein, (e) is bar portion power spectrum, and (f) is for being wrapped in the product power spectrum on bar;
Fig. 5 is the stereoscan photograph figure of embodiments of the invention 2 product;
Fig. 6 is the stereoscan photograph figure of embodiments of the invention 3 product.
Embodiment
Below in conjunction with the drawings and specific embodiments, concrete introduction is done to the present invention.
Embodiment 1
Density is about 1.70g/cm
3porous carbon/carbon compound material be processed into 20 × 10 × 5mm
3matrix sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after being placed in 120 DEG C of baking ovens oven dry, being soaked in mass percent is in the nickel nitrate solution of 10%, until matrix specimen surface no longer produces bubble, dry in 80 DEG C of baking ovens, as depositing base after taking out sample.
With a branch of carbon fiber, the carbon/carbon compound material after immersion is tied up rear overhang to be hung in the deposition region of vertical chemical vapor deposition stove.Cvd furnace is evacuated to 2kPa, and fidelity sky determines that cvd furnace sealing property is intact for 30 minutes, more logical argon gas is to normal pressure, this process in triplicate, with make the air in cvd furnace especially oxygen content be down to minimum; Then, with the speed of 10 DEG C/min, cvd furnace is warming up to 1100 DEG C, with the flow of 400sccm logical argon gas in cvd furnace in temperature-rise period, air outlet stays open state, remains atmospheric pressure state in cvd furnace furnace.After temperature; carrier gas hydrogen is passed in the bubbling bottle that METHYL TRICHLORO SILANE is housed; flow is 200sccm; reactant gas source METHYL TRICHLORO SILANE is brought in furnace; regulate dilution argon gas and dilute hydrogen airshed to be respectively 600sccm and 300sccm simultaneously; reactant gas source enters reaction flat-temperature zone and reacts closedown dilution hydrogen after 60 minutes; carrier gas hydrogen and reactant gas source is closed after 10 minutes; the cooling of power-off simultaneously; make burner hearth naturally cool to room temperature, the flow with 200sccm in temperature-fall period leads to argon shield.
Prepare after taking-up matrix sample through above process, obtained one deck black product at matrix specimen surface, be the silicon carbide nanometer line of graphene coated.
Embodiment 2
Density is about 1.75g/cm
3porous carbon/carbon compound material be processed into 20 × 10 × 5mm
3matrix sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after being placed in 120 DEG C of baking ovens oven dry, being soaked in mass percent is in the nickel nitrate solution of 8%, until specimen surface no longer produces bubble, dry in 80 DEG C of baking ovens, as depositing base after taking out sample.
With a branch of carbon fiber, the carbon/carbon compound material after immersion is tied up rear overhang to be hung in vertical chemical vapor deposition stove deposition region.Cvd furnace is evacuated to 2kPa, and fidelity sky determines that cvd furnace sealing property is intact for 30 minutes, more logical argon gas is to normal pressure, and this process in triplicate.Then with the speed of 10 DEG C/min, cvd furnace is warming up to 1100 DEG C, with the flow of 400sccm logical argon gas in cvd furnace in temperature-rise period, air outlet stays open state, remains atmospheric pressure state in deposition furnace.After temperature; carrier gas hydrogen is passed in the bubbling bottle that METHYL TRICHLORO SILANE is housed; flow is 100sccm; reactant gas source METHYL TRICHLORO SILANE is brought in furnace; regulate dilution argon gas and dilute hydrogen airshed to be respectively 600sccm and 450sccm simultaneously; reactant gas source enters reaction flat-temperature zone and reacts closedown dilution hydrogen after 60 minutes; carrier gas hydrogen and reactant gas source is closed after 10 minutes; the cooling of power-off simultaneously; make burner hearth naturally cool to room temperature, the flow with 200sccm in temperature-fall period leads to argon shield.
Prepare after taking-up sample through above process, obtained one deck black product at specimen surface, be the silicon carbide nanometer line of graphene coated.
Embodiment 3
Density is about 1.70g/cm
3carbon/carbon compound material be processed into 20 × 10 × 5mm
3matrix sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after being placed in 120 DEG C of baking ovens oven dry, being soaked in mass percent is in the nickel nitrate solution of 5%, until matrix specimen surface does not have bubble, dry in 80 DEG C of baking ovens, as depositing base after taking out sample.
With a branch of carbon fiber, the carbon/carbon compound material after immersion is tied up rear overhang to be hung in vertical chemical vapor deposition stove deposition region.Cvd furnace is evacuated to 2kPa, and fidelity sky determines that cvd furnace sealing property is intact for 30 minutes, more logical argon gas is to normal pressure, and this process in triplicate.Then be warming up to 1100 DEG C with the speed of 10 DEG C/min by cvd furnace, with the flow of 400sccm logical argon gas in cvd furnace in temperature-rise period, air outlet stays open state, remains atmospheric pressure state in cvd furnace furnace.After temperature; carrier gas hydrogen is passed in the bubbling bottle that METHYL TRICHLORO SILANE is housed; flow is 50sccm; bring in furnace by reactant gas source METHYL TRICHLORO SILANE, regulate dilution argon gas and dilute hydrogen airshed to be respectively 450sccm and 400sccm simultaneously, reactant gas source enters reaction flat-temperature zone and reacts closedown dilution hydrogen after 60 minutes; carrier gas hydrogen and reactant gas source is closed after 10 minutes; the cooling of power-off simultaneously, make burner hearth naturally cool to room temperature, the flow with 200sccm in temperature-fall period leads to argon shield.
Prepare after taking-up sample through above process, obtained one deck black product at specimen surface, be the silicon carbide nanometer line of graphene coated.
Characterization of The Products
It is known that composition graphs 1 and the silicon carbide nanometer line of Fig. 3 to the graphene coated that embodiment 1 obtains carry out morphology analysis, the products pure that the present embodiment obtains is even, diameter Distribution is even, wherein nanometer silicon carbide linear diameter is about 30nm, the Graphene thickness of external sheath is about a few nanometer, and length reaches tens microns to hundreds of micron.
Fig. 2 is the XRD figure of the obtained product of embodiment 1, as seen from the figure: product is primarily of the higher graphite of degree of crystallinity and beta silicon carbide composition.
Fig. 4 is the energy spectrogram of the product that embodiment 1 obtains, and as seen from the figure: product bar portion is silicon carbide, what be wrapped in surface is Graphene.
From above-mentioned Characterization of The Products result, the present invention has obtained the high and uniform graphene coated silicon carbide nanometer line of diameter Distribution of linearity.
Fig. 5 and Fig. 6 is the SEM figure of embodiment 2 and embodiment 3 product respectively, and as seen from the figure, embodiment 2 and 3 have also been obtained the high and uniform graphene coated silicon carbide nanometer line of diameter Distribution of linearity.
In addition, graphene coated silicon carbide nanometer line of the present invention as stupalith wild phase use time, can interface cohesion between strengthened silicon carbide nano wire and ceramic matrix, this is at document " Single-CrystalSiCNanowireswithaThinCarbonCoatingforStron gerandTougherCeramicComposites, WenYang, HiroshiAraki, ChengchunTang, SomsriThaveethavorn, AkiraKohyama, HiroshiSuzukiandTetsujiNoda.AdvancedMaterials, 2005 (17): 1519-1523 " surperficial graphite linings has just been studied in great detail to the effect improving silicon carbide nanometer line toughening effect, in addition, the Graphene on silicon carbide nanometer line surface also has good activeness and quietness effect due to its good mechanical property.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand, and above-described embodiment does not limit the present invention in any form, the technical scheme that the mode that all employings are equal to replacement or equivalent transformation obtains, and all drops in protection scope of the present invention.
Claims (8)
1. a preparation method for graphene coated silicon carbide nanometer line, is characterized in that, comprises the steps:
S1, pre-treatment is carried out to matrix sample: by clean with distilled water wash again after the carbon/carbon compound material sanding and polishing of porous, be placed in baking oven and dry;
S2, the matrix sample of drying to be immersed in nickel nitrate solution, be dipped to matrix specimen surface and no longer produce bubble, take out matrix sample and be placed in baking oven and dry;
S3, the carbon/carbon compound material immersion treatment crossed are as depositing base, and binding hangs in the deposition region of vertical gaseous phase deposition stove;
S4, cvd furnace is evacuated to 2kPa, the empty 30min of fidelity, more logical argon gas is to normal pressure, repetitive operation three times;
S5, the furnace temperature of cvd furnace is risen to depositing temperature, in cvd furnace, continue logical argon gas in temperature-rise period, air outlet stays open state; After temperature; carrier gas hydrogen is passed in the bubbling bottle that METHYL TRICHLORO SILANE is housed; reactant gas source METHYL TRICHLORO SILANE is brought in the furnace of cvd furnace; regulate the flow of the dilution argon gas passing into burner hearth and dilution hydrogen, reactant gas source closes dilution hydrogen after entering reaction flat-temperature zone reaction 10-120min simultaneously; carrier gas hydrogen and reactant gas source is closed again after continuing reaction for some time; the cooling of power-off simultaneously, makes burner hearth naturally cool to room temperature, logical argon shield in temperature-fall period.
2. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, is characterized in that, described matrix sample is the carbon/carbon compound material of porous, and density is 1.68-1.75g/cm
3, be of a size of 20 × 10 × 5mm
3.
3. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, is characterized in that, in described step S1, polishes successively by No. 800 and No. 1000 sand paper to matrix sample.
4. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, is characterized in that, in described nickel nitrate solution, the mass percentage of nickelous nitrate is 5%-50%.
5. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, is characterized in that, in described step S3, and the carbon/carbon compound material crossed by carbon fiber binding immersion treatment.
6. the preparation method of a kind of graphene coated silicon carbide nanometer line according to any one of claim 1-5, it is characterized in that, in described step S5, depositing temperature is 1050 DEG C-1300 DEG C, and the flow of described dilution argon gas, dilution hydrogen and carrier gas hydrogen is respectively 200-800sccm, 100-600sccm and 50-200sccm.
7. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 6, is characterized in that, in described step S5, temperature rise rate is 10 DEG C/min.
8. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 6, is characterized in that, the purity of described dilution argon gas, dilution hydrogen and carrier gas hydrogen is all greater than 99.99%.
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| CN108947557A (en) * | 2018-09-25 | 2018-12-07 | 航天特种材料及工艺技术研究所 | A kind of carbon/carbon compound material and preparation method thereof |
| CN108947557B (en) * | 2018-09-25 | 2021-05-14 | 航天特种材料及工艺技术研究所 | Carbon/carbon composite material and preparation method thereof |
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