CN105648418A - Method for preparing SiC nanometer wires and nanometer bands on surfaces of C/C composites - Google Patents
Method for preparing SiC nanometer wires and nanometer bands on surfaces of C/C composites Download PDFInfo
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- CN105648418A CN105648418A CN201610028463.8A CN201610028463A CN105648418A CN 105648418 A CN105648418 A CN 105648418A CN 201610028463 A CN201610028463 A CN 201610028463A CN 105648418 A CN105648418 A CN 105648418A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C23C16/44—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 method of coating
Abstract
The invention discloses a method for preparing SiC nanometer wires and nanometer bands on the surfaces of C/C composites. C/C composites ground, polished and dried are placed in a depositing furnace. After the depositing furnace is electrified under 2kPa low pressure and heated to a preset temperature, air carrying hydrogen is introduced into a bubbling bottle filled with methyl trichlorosilane, and a reaction air source is brought into a hearth to carry out reaction. After deposition is over, the C/C composites are cooled to a room temperature with the furnace, and a large quantity of high-purity SiC nanometer wires and nanometer bands can be obtained. The synthesis technology of the SiC nanometer wires and nanometer bands is simple, and a previous synthesis technology is not required. As depositing temperature is low, energy consumption and preparing cost are reduced. The purity of the prepared SiC nanometer wires and nanometer bands is high, and the controllable growth of the SiC nanometer wires and nanometer bands can be realized through regulating technical parameters. Industrial production is easy to realize, and problems in the prior art, such as complicated SiC nanometer wire and nanometer band preparing technology, high synthesis temperature, high energy consumption, high cost and difficult product control are solved.
Description
Technical field
The invention belongs to chemical material technical field, particularly to the preparation method of a kind of C/C composite material surface SiC nanowire and nano belt.
The preparation method that the present invention relates to a kind of C/C composite material surface SiC nanowire and nano belt, chemical vapor deposition (CVD) method is adopted to synthesize SiC nanowire and nano belt on the C/C matrices of composite material of catalyst-free, the method simply, efficiently, prepare substantial amounts of high-purity alpha-SiC nano wire and nano belt to low energy consumption, can solve the problems such as SiC nanowire and the complicated process of preparation of nano belt in prior art, energy consumption height, purity are low, wayward.
Background technology
From Japanese scholars in 1991 since (Lijima) find CNT, increasing monodimension nanometer material (including: nanotube, nano wire, nanometer rods, nano belt etc.) being found in modern science and technology field and has potential huge applications value, and therefore their technology of preparing receives much concern. Wherein one dimension SiC nano material except have SiC bulk material excellent properties (as high heat stability, good heat conductivity, high rigidity and high-modulus, wide can be with, good antioxidation and corrosion resistance) except, also have outstanding electricity and mechanical property, in Flied emission, nano electron device and advanced composite material field, there is huge using value. The method preparing one dimension SiC nano material is a lot, specifically includes that carbothermic method, chemical gas-phase reaction method, template growth method, organic precursor pyrolysismethod, microwave-hydrothermal method and arc discharge, laser ablation method etc. Although preparation method is different, but having self shortcoming, such as complex process, preparation temperature high energy consumption are big, poor controllability, product purity are low.
Patent name is that " a kind of method (China Patent No.: CN201110359635.7; the applying date: 2011.11.15; publication date: 2012.06.13) preparing SiC nanowire and nano belt " is with carbon dust, silica flour, carborundum powder and alumina powder for raw material, first SiC-Si complex phase ceramic coating is prepared at C/C composite material surface at 200-2200 DEG C of temperature, gas-phase reaction synthesis SiC nanowire and nano belt is there is again through graphite paper parcel, complex technical process, and reaction temperature is high, equipment requirements is high, energy consumption is high, cost is big, is unfavorable for realizing controlled production;Document " Growthandmorphologyofone-dimensionalSiCnanostructureswit houtcatalystassistant.MaterialsChemistryandPhysics.2006,95:140-144 " reports a kind of by C powder, Si powder and SiO2Carbothermic reduction reaction is occurred to prepare SiC nanowire and the method for nanometer pelletron after powder mix homogeneously at 1400 DEG C, although the method has simple and easy to do, the advantage that nano wire yield is higher, but containing substantial amounts of C, Si and SiO in products therefrom2The impurity such as granule, the later stage needs product is purified, thus causing that preparation process is more complicated.
Summary of the invention
Goal of the invention: the preparation method that the invention provides a kind of C/C composite material surface SiC nanowire and nano belt, to solve, technique in prior art is complex, synthesis temperature is high, energy consumption is big, cost is high, the unmanageable problem of product. The method is with methyl trichlorosilane for presoma, adopt low-pressure chemical vapor deposition technology when catalyst-free is assisted and under lower temperature, to synthesize SiC nanowire and nano belt, the method can simply, low energy consumption, low cost and easily controllable prepare substantial amounts of high-purity alpha-SiC nano wire and nano belt.
Technical scheme: to achieve these goals, the present invention by the following technical solutions:
1, the preparation method of a kind of C/C composite material surface SiC nanowire and nano belt, it is characterised in that comprise the following steps:
Step one, by clean with distilled water wash after C/C composite sanding and polishing, then take out after being placed in baking oven to dry standby;
Step 2, with a branch of carbon fiber by processed C/C composite binding after, hang in vertical gaseous phase deposition stove;
Step 3, vertical gaseous phase deposition stove is evacuated to 2kPa, keeps vacuum 30 minutes, it is determined that opening vacuum pump after body of heater is air tight again and continue evacuation, maintenance furnace pressure is 2kPa;
Step 4, energising heat up, temperature-rise period passes into argon shield, after furnace temperature is raised to predetermined depositing temperature, in equipped with the bubbling bottle of methyl trichlorosilane, passes into carrier gas hydrogen, again methyl trichlorosilane is brought in stove, pass into dilution argon, dilution hydrogen simultaneously; And regulate dilution argon, dilute the flow value of hydrogen and carrier gas hydrogen, after depositing 60 minutes��180 minutes under predetermined depositing temperature, close dilution hydrogen, carrier gas hydrogen and methyl trichlorosilane; The cooling of power-off simultaneously, makes to naturally cool in stove room temperature, still keeps furnace pressure 2kPa, and be continually fed into argon shield in temperature-fall period in temperature-fall period.
Further, described C/C composite is density is 1.68��1.75g/cm3, it is of a size of 20 �� 10 �� 5mm3C/C composite.
Further, in described step one, C/C composite sanding and polishing adopt No. 800, No. 1000 sand paper carry out successively.
Further, in described step 3, when vacuum meter is unchanged during maintenance vacuum, then illustrate that body of heater is air tight, seal intact.
Further, in described step 4, described depositing temperature is 1050 DEG C��1300 DEG C.
Further, in described step 4, flow respectively 200��800sccm, 500��1000sccm and the 50��100sccm of dilution argon, dilution hydrogen and carrier gas hydrogen.
Further, in described step 4, the argon flow amount passed in the process of intensification is 100��200sccm, and the argon flow amount passed in the process of cooling is 100sccm.
Further, described hydrogen and purity of argon both are greater than 99.99%.
Further, the purity of described methyl trichlorosilane is more than 98%, and is carried it in vertical gaseous phase deposition stove by the mode of hydrogen bubbling.
Beneficial effect: SiC nanowire of the present invention and nano belt synthesis technique are simple, it is not necessary to pre-synthesis technique; Depositing temperature is relatively low, reduces energy consumption and preparation cost; SiC nanowire and the nano belt purity of preparation are higher; The controllable growth of SiC nanowire and nano belt can be realized by the adjustment of technological parameter, it is easily achieved commercial production, solves in prior art SiC nanowire and nano belt preparation technology is complex, synthesis temperature is high, energy consumption is big, cost is high, the unmanageable problem of product.
Accompanying drawing explanation
Fig. 1 is the low power stereoscan photograph of SiC nanowire prepared by example 2 and nano belt in the present invention;
Fig. 2 is the high power stereoscan photograph of SiC nanowire prepared by example 2 and nano belt in the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
It is 1.70g/cm by density3C/C composite processing become 20 �� 10 �� 5mm3Sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after drying in 120 DEG C of baking ovens, as depositing base.
With a branch of carbon fiber, the C/C composite after drying is tied up rear overhang to be hung in vertical chemical vapor deposition stove deposition region. Cvd furnace is evacuated to 2kPa, after fidelity sky determines that cvd furnace sealing property is intact for 30 minutes, then opens vacuum pump control pressure at 2kPa. Then with the speed of 10 DEG C/min, cvd furnace is warming up to 1050 DEG C, temperature-rise period leads to argon with the flow of 100sccm in cvd furnace. After temperature; to equipped with the bubbling bottle of methyl trichlorosilane passes into carrier gas hydrogen; flow is 50sccm; reactant gas source methyl trichlorosilane is brought in furnace; regulate dilution argon and dilute hydrogen throughput respectively 200sccm and 1000sccm simultaneously; enter after reaction flat-temperature zone reacts 60 minutes and close dilution hydrogen, carrier gas hydrogen and reactant gas source; the cooling of power-off simultaneously; burner hearth is made to naturally cool to room temperature; not closing vacuum pump in this process, furnace pressure still keeps 2kPa and the logical argon shield of flow with 100sccm.
Prepare after taking-up sample through above procedure, obtained a small amount of light green product at specimen surface, be SiC nanowire and nano belt.
Embodiment 2
It is 1.68g/cm by density3C/C composite processing become 20 �� 10 �� 5mm3Sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after drying in 120 DEG C of baking ovens, as depositing base.
With a branch of carbon fiber, the C/C composite after drying is tied up rear overhang to be hung in vertical chemical vapor deposition stove deposition region. Cvd furnace is evacuated to 2kPa, fidelity sky within 30 minutes, determines that cvd furnace sealing property is intact, then open vacuum pump continue evacuation keep furnace pressure be 2kPa. Then with the speed of 10 DEG C/min, cvd furnace is warming up to 1200 DEG C, temperature-rise period leads to argon with the flow of 200sccm in cvd furnace. After temperature; to equipped with the bubbling bottle of methyl trichlorosilane passes into carrier gas hydrogen; flow is 100sccm; reactant gas source methyl trichlorosilane is brought in furnace; regulate dilution argon and dilute hydrogen throughput respectively 500sccm and 800sccm simultaneously; enter after reaction flat-temperature zone reacts 120 minutes and close dilution hydrogen, carrier gas hydrogen and reactant gas source; the cooling of power-off simultaneously; burner hearth is made to naturally cool to room temperature; not closing vacuum pump in this process, furnace pressure still keeps 2kPa and the logical argon shield of flow with 100sccm.
Prepare after taking-up sample through above procedure, obtained a large amount of light green product at specimen surface, be SiC nanowire and nano belt. From Fig. 1 and Fig. 2, covering substantial amounts of high-purity alpha-SiC nano wire and nano belt, gained SiC nanowire even thickness on C/C matrices of composite material, diameter is between 50-100nm, and length is up to hundreds of microns. Gained SiC nano belt width is 100-200 nanometer, and thickness is 5-10nm, and length is up to hundreds of micron.
Embodiment 3
It is 1.75g/cm by density3C/C composite processing become 20 �� 10 �� 5mm3Sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after drying in 120 DEG C of baking ovens, as depositing base.
With a branch of carbon fiber, the C/C composite after drying 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, then opens the lasting evacuation maintenance furnace pressure of vacuum pump at 2kPa. then with the speed of 10 DEG C/min, cvd furnace is warming up to 1300 DEG C, temperature-rise period leads to argon with the flow of 200sccm in cvd furnace, after temperature, to equipped with the bubbling bottle of methyl trichlorosilane passes into carrier gas hydrogen, flow is 80sccm, reactant gas source methyl trichlorosilane is brought in furnace, regulate dilution argon and dilute hydrogen throughput respectively 500sccm and 1000sccm simultaneously, enter after reaction flat-temperature zone reacts 180 minutes and close dilution hydrogen, carrier gas hydrogen and reactant gas source, the cooling of power-off simultaneously, burner hearth is made to naturally cool to room temperature, this process is not closed vacuum pump, furnace pressure still keeps 2kPa and the logical argon shield of flow with 100sccm.
Prepare after taking-up sample through above procedure, obtained a small amount of light green product at specimen surface, be SiC nanowire and nano belt.
Embodiment 4
It is 1.75g/cm by density3C/C composite processing become 20 �� 10 �� 5mm3Sample, successively with clean with distilled water supersound washing after No. 800, No. 1000 sand paperings, after drying in 120 DEG C of baking ovens, as depositing base.
With a branch of carbon fiber, the C/C composite after drying 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, then opens the lasting evacuation maintenance furnace pressure of vacuum pump at 2kPa. then with the speed of 10 DEG C/min, cvd furnace is warming up to 1300 DEG C, temperature-rise period leads to argon with the flow of 150sccm in cvd furnace, after temperature, to equipped with the bubbling bottle of methyl trichlorosilane passes into carrier gas hydrogen, flow is 80sccm, reactant gas source methyl trichlorosilane is brought in furnace, regulate dilution argon and dilute hydrogen throughput respectively 800sccm and 500sccm simultaneously, enter after reaction flat-temperature zone reacts 180 minutes and close dilution hydrogen, carrier gas hydrogen and reactant gas source, the cooling of power-off simultaneously, burner hearth is made to naturally cool to room temperature, this process is not closed vacuum pump, furnace pressure still keeps 2kPa and the logical argon shield of flow with 100sccm.
Prepare after taking-up sample through above procedure, obtained a small amount of light green product at specimen surface, be SiC nanowire and nano belt.
The above is only the preferred embodiment of the present invention; it is noted that, for those skilled in the art; under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. the preparation method of a C/C composite material surface SiC nanowire and nano belt, it is characterised in that comprise the following steps:
Step one, by clean with distilled water wash after C/C composite sanding and polishing, then take out after being placed in baking oven to dry standby;
Step 2, with a branch of carbon fiber by processed C/C composite binding after, hang in vertical gaseous phase deposition stove;
Step 3, vertical gaseous phase deposition stove is evacuated to 2kPa, keeps vacuum 30 minutes, it is determined that opening vacuum pump after body of heater is air tight again and continue evacuation, maintenance furnace pressure is 2kPa;
Step 4, energising heat up, temperature-rise period passes into argon shield, after furnace temperature is raised to predetermined depositing temperature, in equipped with the bubbling bottle of methyl trichlorosilane, passes into carrier gas hydrogen, again methyl trichlorosilane is brought in stove, pass into dilution argon, dilution hydrogen simultaneously; And regulate dilution argon, dilute the flow value of hydrogen and carrier gas hydrogen, after depositing 60 minutes��180 minutes under predetermined depositing temperature, close dilution hydrogen, carrier gas hydrogen and methyl trichlorosilane; The cooling of power-off simultaneously, makes to naturally cool in stove room temperature, still keeps furnace pressure 2kPa, and be continually fed into argon shield in temperature-fall period in temperature-fall period.
2. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterised in that: described C/C composite is density is 1.68��1.75g/cm3, it is of a size of 20 �� 10 �� 5mm3C/C composite.
3. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterised in that: in described step one, C/C composite sanding and polishing adopt No. 800, No. 1000 sand paper carry out successively.
4. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterised in that: in described step 3, when vacuum meter is unchanged during maintenance vacuum, then illustrate that body of heater is air tight, seal intact.
5. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterised in that: in described step 4, described depositing temperature is 1050 DEG C��1300 DEG C.
6. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterized in that: in described step 4, flow respectively 200��800sccm, 500��1000sccm and the 50��100sccm of dilution argon, dilution hydrogen and carrier gas hydrogen.
7. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterized in that: in described step 4, the argon flow amount passed in the process heated up is 100��200sccm, and the argon flow amount passed in the process of cooling is 100sccm.
8. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterised in that: described hydrogen and purity of argon both are greater than 99.99%.
9. the preparation method of C/C composite material surface SiC nanowire according to claim 1 and nano belt, it is characterised in that: the purity of described methyl trichlorosilane is more than 98%, and is carried it in vertical gaseous phase deposition stove by the mode of hydrogen bubbling.
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| CN201610028463.8A CN105648418A (en) | 2016-01-18 | 2016-01-18 | Method for preparing SiC nanometer wires and nanometer bands on surfaces of C/C composites |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834287A (en) * | 2005-03-18 | 2006-09-20 | 西北工业大学 | Method of preparing carbon-carbon composite material surface silicon carbide nano wire |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834287A (en) * | 2005-03-18 | 2006-09-20 | 西北工业大学 | Method of preparing carbon-carbon composite material surface silicon carbide nano wire |
Non-Patent Citations (2)
| Title |
|---|
| 李军等: "C/C复合材料表面原位生长SiCw的工艺", 《中国有色金属学报》 * |
| 葛毅成等: "C/C复合材料表面无催化剂CVD制备SiC纳米线的结构表征（英文）", 《TRANSACTIONS OF NONFERROUS METALS SOCIETY OF CHINA》 * |
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