CN105506579B - A kind of preparation method of graphene coated silicon carbide nanometer line - Google Patents
A kind of preparation method of graphene coated silicon carbide nanometer line Download PDFInfo
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- CN105506579B CN105506579B CN201510933922.2A CN201510933922A CN105506579B CN 105506579 B CN105506579 B CN 105506579B CN 201510933922 A CN201510933922 A CN 201510933922A CN 105506579 B CN105506579 B CN 105506579B
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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 kind of preparation method of graphene coated silicon carbide nanometer line, technical process is simply easily realized, the depositing temperature of silicon carbide nanometer line is relatively low, reduce preparation cost and simplify preparation technology, the graphene coated silicon carbide nanometer line that linearity is high and diameter is evenly distributed has been obtained by this method, the product strengthens mutually in use, interface cohesion that can be between strengthened silicon carbide nano wire and ceramic matrix as ceramic material;In addition, the graphene on silicon carbide nanometer line surface also has activeness and quietness effect.
Description
Technical field
The present invention relates to a kind of preparation method of graphene coated silicon carbide nanometer line.
Background technology
Carborundum has excellent physical and chemical performance as third generation semi-conducting material:Such as high heat endurance, well
Heat conductivity, high rigidity and high-modulus, it is wide can band, good anti-oxidant and corrosion resistance, these properties cause SiC
Obtained extensively in fields such as Aero-Space, chemical industry, mechanical industry, metallurgical industry, fretting wear, optics, electronics and nuclear energy
General application.And one-dimensional silicon carbide nano material also possesses outstanding in addition to the good characteristic with carborundum block materials
Electricity and mechanical property, therefore, silicon carbide nanometer line can have wide as the preferable activeness and quietness materials'use of composite
Application prospect.
In recent years, scholars prepare various informative silicon carbide nanometer line using different methods in succession, but mostly
The surface of number silicon carbide nanometer line is smooth.And document " G.Y.Zhang, J.Xin, E.G.Wang,
Silicon carbide nanometer line of Appl.Phys.Lett.84 (2004) 2646-2648. " reports with complex surface structures is as enhancing
Toughening material can preferably be embedded in matrix, improve activeness and quietness effect.So far, researchers have been successfully prepared one
The silicon carbide nanometer line of a little labyrinths.For example, document " J.Wei, K.Z.Li, H.J.Li, Q.G.Fu, L.Zhang,
Mater.Chem.Phys.95 (2006) 140-144. " aid in using silica and graphite as raw material, at 1400 DEG C without catalyst
In the case of, the silicon carbide nanometer line of item chain has been prepared by chemical gas-phase reaction method;Document " J.Z.Guo, Y.Zuo,
It is to use chemical vapor deposition in Z.J.Li, W.D.Gao, J.L.Zhang, PhysicaE 39 (2007) 262-266. " reports
Method, pass through Si, SiO2And CH4Biochemical reaction is issued at 1350 DEG C the carborundum with fin shape surface texture is prepared and receive
Rice noodles;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 uses chemical vapour deposition technique, and a kind of carbon of chain structure is prepared in the case of without catalyst
SiClx nano wire.But the most complex process of these preparation methods, surface do not have graphene coated yet, used as reinforcing material
When the shortcomings of adhesion is not high, effect is not strong also be present.
The content of the invention
To solve the deficiencies in the prior art, it is an object of the invention to provide a kind of graphene coated silicon carbide nanometer line
Preparation method.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that:
A kind of preparation method of graphene coated silicon carbide nanometer line, comprises the following steps:
S1, matrix sample is pre-processed:Distillation water washing will be used after porous carbon/carbon compound material sanding and polishing again
Totally, it is placed in baking oven and dries;
S2, the matrix sample of drying immersed in catalyst nickel nitrate solution, be dipped to matrix specimen surface and no longer produce
Bubble, illustrate that the air in the loose structure of carbon/carbon compound material is discharged and has been each filled with nickel nitrate solution, take out matrix examination
Sample is placed in baking oven and dried;
S3, using the carbon/carbon compound material that immersion treatment is crossed as depositing base, binding hangs on vertical gaseous phase deposition stove
In deposition region;
S4, cvd furnace is evacuated to 2kPa, the readings of fidelity sky 30min observation vacuum meters to determine whether gas leakage, then
For logical argon gas to normal pressure, repeating three times is preferably minimized, the oxygen content in cvd furnace;
S5, the furnace temperature of cvd furnace is risen to depositing temperature, persistently lead to argon gas in temperature-rise period into cvd furnace, gas outlet is protected
Hold open mode;To after temperature, carrier gas hydrogen is passed through into the bubbling bottle equipped with methyl trichlorosilane, by reactant gas source methyl trichlorine
Silane is brought into the furnace of cvd furnace, while regulation is passed through the dilution argon gas of burner hearth and dilutes the flow of hydrogen, controls reaction gas
The partial pressure of body, after reactant gas source is into reaction flat-temperature zone reaction 10-120min, dilution hydrogen is closed, when continuing to react one section
Between after turn off carrier gas hydrogen and reactant gas source, while power off cooling, burner hearth is naturally cooled to room temperature, lead to argon in temperature-fall period
Gas shielded.
For a better understanding of the present invention, the reaction mechanism of the present invention is presumed as follows:React early stage, methyl trichlorosilane
Silicon carbide nanometer line has been cracked to form in the case where hydrogen participates in reaction;The later stage is reacted, after closing dilution hydrogen, methyl trichlorine
The preferential graphene in surface-active larger silicon carbide nanometer line Surface Creation of the cracking of silane, so as to which graphene bag be made
The silicon carbide nanometer line covered.
Preferably, aforementioned substrates sample is porous carbon/carbon compound material, density 1.68-1.75g/cm3, size is
20×10×5mm3。
It is highly preferred that in abovementioned steps S1, matrix sample is polished with No. 800 and No. 1000 sand paper successively.
More preferably, the weight/mass percentage composition of nickel nitrate is 5%-50% in foregoing nickel nitrate solution.
It is further preferred that in abovementioned steps S3, the carbon/carbon compound material crossed with carbon fiber binding immersion treatment.
Still further preferably, in abovementioned steps S5, depositing temperature is 1050 DEG C -1300 DEG C, the dilution argon gas, dilution
The flow of hydrogen and carrier gas hydrogen is respectively 200-800sccm, 100-600sccm and 50-200sccm.
Preferably, in abovementioned steps S5, heating rate is 10 DEG C/min.
Further, the purity of foregoing dilution argon gas, dilution hydrogen and carrier gas hydrogen is both greater than 99.99%.
The present invention is advantageous in that:The present invention preparation method technical process simply easily realize, silicon carbide nanometer line
Depositing temperature it is relatively low, reduce and prepare cost and simplify preparation technology, obtained that linearity is high and diameter by this method
The graphene coated silicon carbide nanometer line being evenly distributed, the product as ceramic material enhancing phase in use, carbonization can be strengthened
Interface cohesion between silicon nanowires and ceramic matrix;In addition, the graphene on silicon carbide nanometer line surface also has activeness and quietness
Effect.
Brief description of the drawings
Fig. 1 is the stereoscan photograph figure of the product of embodiments of the invention 1;
Fig. 2 is the XRD of the product of embodiments of the invention 1;
Fig. 3 is the transmission electron microscope photo figure of the product of embodiments of the invention 1, wherein, (a) be product transmission electron microscope photo and
Diffracting spectrum is chosen, (b) is product high-resolution photo, and (c) is the high-resolution enlarged drawing of silicon carbide nanometer line bar portion, and (d) is to receive
The high-resolution photo of nanowire surface graphene;
Fig. 4 is the energy spectrum diagram of the product of embodiments of the invention 1, wherein, (e) is bar portion power spectrum, and (f) is to be wrapped on bar
Product power spectrum;
Fig. 5 is the stereoscan photograph figure of the product of embodiments of the invention 2;
Fig. 6 is the stereoscan photograph figure of the product of embodiments of the invention 3.
Embodiment
Make specific introduce to the present invention below in conjunction with the drawings and specific embodiments.
Embodiment 1
By density about 1.70g/cm3Porous carbon/carbon compound material be processed into 20 × 10 × 5mm3Matrix sample, successively
With using distilled water supersound washing clean after No. 800, No. 1000 sand paper polishings, it is placed in 120 DEG C of baking ovens after drying, is soaked in quality
Percentage is in 10% nickel nitrate solution, until matrix specimen surface no longer produces bubble, takes out after sample in 80 DEG C of baking ovens
Middle drying, as depositing base.
The carbon/carbon compound material after immersion is tied up into rear overhang with a branch of carbon fiber and is hung on the heavy of vertical chemical vapor deposition stove
In product region.Cvd furnace is evacuated to 2kPa, fidelity determines that cvd furnace sealing property is intact for empty 30 minutes, then logical argon gas is to normal
Pressure, this process in triplicate so that the air especially oxygen content in cvd furnace minimizes;Then, with 10 DEG C/min's
Cvd furnace is warming up to 1100 DEG C by speed, leads to argon gas into cvd furnace in temperature-rise period with 400sccm flow, and gas outlet is kept
Open mode, atmospheric pressure state is remained in cvd furnace furnace.To after temperature, load is passed through into the bubbling bottle equipped with methyl trichlorosilane
Gas hydrogen, flow 200sccm, reactant gas source methyl trichlorosilane is brought into furnace, while adjust dilution argon gas and dilution
Hydrogen flowing quantity is respectively 600sccm and 300sccm, and reactant gas source, which enters after reaction flat-temperature zone reacts 60 minutes, closes dilute hydrogen
Gas, carrier gas hydrogen and reactant gas source were closed after 10 minutes, while power off cooling, burner hearth is naturally cooled to room temperature, cooled
During with 200sccm flow lead to argon gas protection.
After above procedure prepares completion taking-up matrix sample, one layer of black product is obtained in matrix specimen surface, i.e.,
For the silicon carbide nanometer line of graphene coated.
Embodiment 2
By density about 1.75g/cm3Porous carbon/carbon compound material be processed into 20 × 10 × 5mm3Matrix sample, successively
With using distilled water supersound washing clean after No. 800, No. 1000 sand paper polishings, it is placed in 120 DEG C of baking ovens after drying, is soaked in quality
Percentage is in 8% nickel nitrate solution, until specimen surface no longer produces bubble, is dried after taking out sample in 80 DEG C of baking ovens
It is dry, as depositing base.
The carbon/carbon compound material after immersion is tied up into rear overhang with a branch of carbon fiber and is hung on vertical chemical vapor deposition stove deposition
In region.Cvd furnace is evacuated to 2kPa, fidelity determines that cvd furnace sealing property is intact for empty 30 minutes, then logical argon gas is to normal
Pressure, this process is in triplicate.Then cvd furnace is warming up to 1100 DEG C with 10 DEG C/min speed, in temperature-rise period with
400sccm flow leads to argon gas into cvd furnace, and gas outlet remains on, and deposits in furnace and remains atmospheric pressure state.Arrive
Wen Hou, carrier gas hydrogen, flow 100sccm, by reactant gas source methyl three are passed through into the bubbling bottle equipped with methyl trichlorosilane
Chlorosilane is brought into furnace, while it is respectively 600sccm and 450sccm to adjust dilution argon gas and dilution hydrogen flowing quantity, reaction gas
Source, which enters after reaction flat-temperature zone reacts 60 minutes, closes dilution hydrogen, and carrier gas hydrogen and reactant gas source were closed after 10 minutes,
Cooling is powered off simultaneously, burner hearth is naturally cooled to room temperature, leading to argon gas in temperature-fall period with 200sccm flow protects.
After above procedure prepares completion taking-up sample, one layer of black product, as graphene are obtained in specimen surface
The silicon carbide nanometer line of cladding.
Embodiment 3
By density about 1.70g/cm3Carbon/carbon compound material be processed into 20 × 10 × 5mm3Matrix sample, successively with 800
Number, it is clean with distilled water supersound washing after the polishing of No. 1000 sand paper, be placed in 120 DEG C of baking ovens after drying, be soaked in quality percentage
Number is in 5% nickel nitrate solution, until matrix specimen surface does not have bubble, dries, makees in 80 DEG C of baking ovens after taking out sample
For depositing base.
The carbon/carbon compound material after immersion is tied up into rear overhang with a branch of carbon fiber and is hung on vertical chemical vapor deposition stove deposition
In region.Cvd furnace is evacuated to 2kPa, fidelity determines that cvd furnace sealing property is intact for empty 30 minutes, then logical argon gas is to normal
Pressure, this process is in triplicate.Then cvd furnace is warming up to 1100 DEG C with 10 DEG C/min speed, in temperature-rise period with
400sccm flow leads to argon gas into cvd furnace, and gas outlet is remained on, and atmospheric pressure state is remained in cvd furnace furnace.
To after temperature, carrier gas hydrogen, flow 50sccm, by reactant gas source methyl three are passed through into the bubbling bottle equipped with methyl trichlorosilane
Chlorosilane is brought into furnace, while it is respectively 450sccm and 400sccm to adjust dilution argon gas and dilution hydrogen flowing quantity, reaction gas
Source, which enters after reaction flat-temperature zone reacts 60 minutes, closes dilution hydrogen, closes carrier gas hydrogen and reactant gas source after 10 minutes, together
When power-off cooling, burner hearth is naturally cooled to room temperature, argon gas protection led to 200sccm flow in temperature-fall period.
After above procedure prepares completion taking-up sample, one layer of black product, as graphene are obtained in specimen surface
The silicon carbide nanometer line of cladding.
Characterization of The Products
Morphology analysis is carried out with reference to Fig. 1 and Fig. 3 to the silicon carbide nanometer line of graphene coated made from embodiment 1 to understand,
Products pure is uniform made from the present embodiment, and diameter is evenly distributed, and wherein nanometer silicon carbide linear diameter is about 30nm, external sheath
Graphene thickness be about several nanometers, length is up to tens microns to hundreds of microns.
Fig. 2 is the XRD of product made from embodiment 1, as seen from the figure:Product is mainly by crystallinity higher graphite and β
Carborundum forms.
Fig. 4 is the energy spectrum diagram of product made from embodiment 1, as seen from the figure:Product bar portion is carborundum, is wrapped in surface
It is graphene.
From above-mentioned Characterization of The Products result, the graphene coated that linearity height and diameter are evenly distributed has been made in the present invention
Silicon carbide nanometer line.
Fig. 5 and Fig. 6 is the SEM figures of embodiment 2 and the product of embodiment 3 respectively, and as seen from the figure, embodiment 2 and 3 also obtains
The graphene coated silicon carbide nanometer line that linearity height and diameter are evenly distributed.
In addition, the present invention graphene coated silicon carbide nanometer line as ceramic material enhancing phase in use, can strengthen
Interface cohesion between silicon carbide nanometer line and ceramic matrix, this is in document " Single-Crystal SiC Nanowires
with a Thin Carbon Coating for Stronger and Tougher Ceramic Composites,Wen
Yang,Hiroshi Araki,Chengchun Tang,Somsri Thaveethavorn,Akira Kohyama,Hiroshi
Suzuki and Tetsuji Noda.Advanced Materials,2005(17):Just ground in detail in 1519-1523 "
Effect of the surface graphite linings to raising silicon carbide nanometer line toughening effect is studied carefully;In addition, the graphene on silicon carbide nanometer line surface
Because its good mechanical property also has preferable activeness and quietness effect.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way for above-described embodiment, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical scheme, all fall within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of graphene coated silicon carbide nanometer line, it is characterised in that comprise the following steps:
S1, matrix sample is pre-processed:It will be done again with distillation water washing after porous carbon/carbon compound material sanding and polishing
Only, it is placed in baking oven and dries;
S2, the matrix sample of drying immersed in nickel nitrate solution, be dipped to matrix specimen surface and no longer produce bubble, take out base
Body sample, which is placed in baking oven, dries;
S3, using the carbon/carbon compound material that immersion treatment is crossed as depositing base, binding hangs on the deposition of vertical gaseous phase deposition stove
In region;
S4, cvd furnace is evacuated to 2kPa, fidelity sky 30min, then logical argon gas repeats three times to normal pressure;
S5, the furnace temperature of cvd furnace is risen to depositing temperature, persistently lead to argon gas in temperature-rise period into cvd furnace, gas outlet keeps beating
Open state;To after temperature, carrier gas hydrogen is passed through into the bubbling bottle equipped with methyl trichlorosilane, by reactant gas source methyl trichlorosilane
Bring into the furnace of cvd furnace, while regulation is passed through the dilution argon gas of burner hearth and dilutes the flow of hydrogen, reactant gas source enters anti-
After answering flat-temperature zone reaction 10-120min, dilution hydrogen is closed, continues to turn off carrier gas hydrogen and reaction gas after reacting a period of time
Source, while cooling is powered off, burner hearth is naturally cooled to room temperature, argon gas protection is led in temperature-fall period;
In the step S5, depositing temperature is 1050 DEG C -1300 DEG C, the stream of the dilution argon gas, dilution hydrogen and carrier gas hydrogen
Amount is respectively 200-800sccm, 100-600sccm and 50-200sccm.
2. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, it is characterised in that described
Matrix sample is porous carbon/carbon compound material, density 1.68-1.75g/cm3, size is 20 × 10 × 5mm3。
3. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, it is characterised in that described
In step S1, matrix sample is polished with No. 800 and No. 1000 sand paper successively.
4. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, it is characterised in that described
The weight/mass percentage composition of nickel nitrate is 5%-50% in nickel nitrate solution.
5. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, it is characterised in that described
In step S3, with the carbon/carbon compound material crossed of carbon fiber binding immersion treatment.
6. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, it is characterised in that described
In step S5, heating rate is 10 DEG C/min.
7. the preparation method of a kind of graphene coated silicon carbide nanometer line according to claim 1, it is characterised in that described
The purity of dilution argon gas, dilution hydrogen and carrier gas hydrogen is both greater than 99.99%.
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