CN1834287A - Method of preparing carbon-carbon composite material surface silicon carbide nano wire - Google Patents
Method of preparing carbon-carbon composite material surface silicon carbide nano wire Download PDFInfo
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- CN1834287A CN1834287A CN 200510041813 CN200510041813A CN1834287A CN 1834287 A CN1834287 A CN 1834287A CN 200510041813 CN200510041813 CN 200510041813 CN 200510041813 A CN200510041813 A CN 200510041813A CN 1834287 A CN1834287 A CN 1834287A
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Abstract
This invention relates to a method for manufacturing SiC nanowires on the surface of C/C composite, which comprises the steps of: (1) polishing the C/C composite, washing with distilled water, and drying; (2) binding the treated C/C composite with carbon fibers, and suspending in a vertical chemical vapor deposition furnace; (3) evacuating the furnace, pumping Ar into the furnace to normal pressure, and repeating for three times; (4) applying electricity, heating, and pumping H2 for pretreatment; (5) adjusting the flow rates of Ar, H2 and methyl trichlorosilane when the furnace temperature reaches the predetermined deposition temperature, keeping the temperature for deposition, the turning off the power and cooling naturally to obtain a layer of SiC nanowires on the surface of the material. The method has such advantages as simple process, no additive, low deposition pressure and temperature. The morphology and purity of the synthesized SiC nanowires can be effectively controlled by adjusting the deposition factors.
Description
Technical field
The present invention relates to a kind of preparation method of carbon/carbon compound material surface silicon carbide nano wire, is a kind of pattern of carbon/carbon compound material surface silicon carbide nano wire and the control method of purity, is used to prepare high-quality silicon carbide nanometer line.
Background technology:
Silicon carbide has many excellent characteristic, as high strength, high rigidity, low density, fabulous anti-oxidant and resistance to corrosion, low thermal expansivity and high thermal conduction capability.In addition, silicon carbide still is a kind of broadband based semiconductor material, and has high breakdown electric field, high electron saturation velocities and high capability of resistance to radiation.Silicon carbide nanometer line also demonstrates better performance.Nearest result of study shows, the elasticity of silicon carbide nanometer line and intensity be far longer than micro-meter scale silicon carbide whisker and bulk silicon carbide crystal (Wong E.W., Sheehan P.E., Lieber C.M.Science, 1997,277:1971-1975.).The high strength of silicon carbide nanometer line and high rigidity and big length-to-diameter ratio show that it may become the very effective wild phase of ceramic base, metal matrix and polymer matrix composite.On the other hand, the one dimension carbofrax material of nanoscale also can be used to make the nanoelectronic and the opto-electronic device of working under the severe environment such as high frequency, high-power, high temperature resistant and radioprotective.In addition, the field emission characteristic that shown of one dimension silicon carbide nano material also is a kind of characteristic that actual application value is arranged very much.
The synthetic method of silicon carbide monodimension nanometer material-nano wire and The Characteristic Study are inchoate in recent years.Nineteen ninety-five, the human carbon nanotubes such as Dai of department of chemistry of Harvard University are made template, making it is silicon carbide nanometer line (the Dai H.J. that 2-30nm, length reach 20 μ m with having the silicon monoxide of higher vapor pressure or successfully synthesizing diameter first with silicon and Iod R, Wong E.W., Lu Y.Z., Fan S.S., Lieber C.M.Nature, 1995,375:769-772.).The method of several subsequently synthesizing silicon carbide monodimension nanometer materials is developed gradually.These methods are broadly divided into following three types: (1) Gu utilize vapour-liquid-(VLS) growth mechanism synthesizing silicon carbide monodimension nanometer material (Lai H.L., Wong N.B., Zhou X.T., etal.Appl.Phys.Lett.2000,76:294-296).; (2) make reactant with silicon tetrachloride and tetracol phenixin, sodium Metal 99.5 do the catalyzer synthesizing silicon carbide nano wire (Hu J.Q., Lu Q.Y., Tang K.B., etal.J.Phys.Chem.B.2000,104:5251-5254.); (3) control carbon (carbon nanotube or carbon granule) and silicon monoxide reaction synthesizing silicon carbide monodimension nanometer material (Meng G.W., Zhang L.D., Mo C.M., etal.J.Mater.Res.1998,13:2533-2538.).
People have obtained some achievements to the research of silicon carbide nanometer line in recent years, yet, still exist such or such deficiency.For example some method need just can be carried out under very high temperature; Some method building-up process more complicated needs the multistep building-up process; And some method prepares and generates a large amount of silicon-carbide particles in the nanometer silicon carbide line process inevitably, has the more difficult isolating problem of nano wire and particle; In addition, some method need be added metal catalyst in reaction chamber, and after preparation finished, the catalyzer drop was present in the nano wire end, has influenced the mechanical property of silicon carbide nano material widely.Up to the present, yet there are no any about adopting the report of aumospheric pressure cvd method at carbon/carbon compound material surface preparation high quality silicon carbide nanometer line.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of method that adopts the aumospheric pressure cvd method at carbon/carbon compound material surface preparation silicon carbide nanometer line, utilize this method can synthesize a large amount of silicon carbide nanometer lines simply efficiently, and can control the pattern and the purity of nano wire.This method is selected METHYL TRICHLORO SILANE (CH for use
3SiCl
3) and high-purity hydrogen (H
2) as reactant gas source, by adjusting the chemical vapor deposition method parameter, at the disposable silicon carbide nanometer line of preparing in carbon/carbon compound material surface.
Technical scheme
Technical characterictic of the present invention is:
Step 1:, in baking oven, dry with clean behind the carbon/carbon compound material sanding and polishing with distilled water wash;
Step 2: hang in the vertical gaseous phase deposition stove after the carbon/carbon compound material binding that will handle with a branch of carbon fiber;
Step 3: cvd furnace vacuumized vacuum tightness is reached-0.09MPa after 15 minutes, left standstill 10 minutes, logical argon gas is to normal pressure, this process triplicate;
Step 4: energising heats up, when the cvd furnace temperature rises to 800 ℃～1200 ℃, and logical hydrogen pre-treatment sample in burner hearth, hydrogen flowing quantity is 300～600ml/min, the treatment time is 0.5～1h; When furnace temperature reaches predetermined depositing temperature, regulate the flux values of argon gas, hydrogen and METHYL TRICHLORO SILANE, and under this preset temperature, be incubated 1～3 hour, to turn off power supply subsequently and lower the temperature naturally, whole process is led to argon shield.
Described the carbon/carbon compound material sanding and polishing is carried out successively with the sand paper of No. 400, No. 800 and No. 1000 respectively.
At the predetermined depositing temperature described in the step 4 is 1000 ℃～1200 ℃, and the flow of described argon gas, hydrogen and METHYL TRICHLORO SILANE is respectively 300～500ml/min, 150～500ml/min and 50～150ml/min.
When leaving standstill 10 minutes, step 3 need guarantee that system sealing is intact.
Described hydrogen purity is greater than 99.99%.
The content of described METHYL TRICHLORO SILANE is greater than 98%, and passes through H
2The mode of bubbling carries it in the reaction chamber.
Through above-mentioned preparation process, from burner hearth, take out carbon/carbon compound material after opening bell, can see that at material surface one deck product is arranged, be silicon carbide nanometer line.X-Ray diffraction, scanning electron microscope analysis show: the deposition products therefrom is the silicon B-carbide structure, and nanowire surface is comparatively smooth, does not have plethora and bifurcated.Work as CH
3SiCl
3/ H
2Ratio is 1: 10 o'clock, and nanowire diameter is 60～70nm, and length reaches tens microns; Along with CH
3SiCl
3/ H
2The increase of ratio, nanowire diameter increases gradually, and foreign matter content raises, and purity descends.
Beneficial effect
The invention has the beneficial effects as follows: synthesis technique is simple, does not need synthesis technique (preparation carbon nanotube etc.) in advance; Need not add catalyzer; Silicon carbide nanometer line makes under normal pressure, to depositing device require low; In addition, also having outstanding characteristics is exactly that depositing temperature is lower, and can effectively control the pattern and the purity of synthetic silicon carbide nanometer line by adjusting deposition parameter.These advantages make this method have the potentiality of the large-scale commercial production of developing into.
Description of drawings
Fig. 1: silicon carbide nanometer line preparation process synoptic diagram
Fig. 2: work as CH
3SiCl
3/ H
2Ratio is the different amplification stereoscan photograph of 1: 10 o'clock prepared silicon carbide nanometer line
Fig. 3: at the X ray diffracting spectrum of the silicon carbide nanometer line of carbon/carbon compound material surface preparation
Fig. 4: different CH
3SiCl
3/ H
2Stereoscan photograph than the silicon carbide nanometer line for preparing under the condition
Embodiment
Now in conjunction with the accompanying drawings the present invention is further described:
With 500ml CH
3SiCl
3Pour in the bubbler, intend passing through H
2The mode of bubbling is with CH
3SiCl
3Bring reaction chamber into, CH
3SiCl
3Performance index such as table 1.
Table 1 CH
3SiCl
3Performance index
| Composition | Color | Fusing point (℃) | Boiling point (℃) | Burning-point (℃) | Thermal capacitance (kJkg -1·k -1) | Gaseous state thermal capacitance (kJkg -1·k -1) | Latent heat (kJkg -1) |
| CH 3SiCl 3＞98％ | White | -77.5 | 66.1 | 455 | 1.27 | 0.82 | 196.78 |
With density is 1.78g/cm
3Carbon/carbon compound material be cut into the sample of 15 * 5 * 5mm with hacksaw, the sand paper of using No. 400, No. 800 and No. 1000 respectively is clean with distilled water wash behind the sanding and polishing successively, dries in 100 ℃ of baking ovens, as deposition substrate.
Hang in the vertical chemical vapor deposition stove after the carbon/carbon compound material binding with a branch of 3K carbon fiber.Size of burner hearth is Φ 40 * 756mm, and the sample bottom is apart from burner hearth bottom 380～420mm.Vacuumize after 15 minutes cvd furnace vacuum tightness is reached-0.09MPa, left standstill 10 minutes, observe vacuum meter and indicate whether to change, as no change, the illustrative system sealing is intact.Logical argon gas vacuumizes this process triplicate again to normal pressure.Flow logical Ar in cvd furnace with 300ml/min opens the air outlet, remains atmospheric pressure state in the burner hearth.Subsequently furnace temperature is risen to 1100 ℃ from room temperature, heat-up rate is controlled at 8-12 ℃/min, when the cvd furnace temperature rises to 900 ℃, and logical hydrogen pre-treatment sample in burner hearth, hydrogen flowing quantity is 400ml/min, the treatment time is 0.5h.Reach after the predetermined temperature logical dilution H in burner hearth
2, flow is 150～500ml/min, and passes through H
2The mode of bubbling is with reactant gas source CH
3SiCl
3Bring in the reaction chamber, as the H of carrier gas
2Flow is 50～150ml/min.Stop logical H after 2 hours in insulation under 1100 ℃
2And CH
3SiCl
3, and turn off power supply and make burner hearth naturally cool to room temperature, the logical Ar protection of whole process.
From burner hearth, take out carbon/carbon compound material after opening bell, can see that at material surface one deck sedimentation products is arranged.X-Ray diffraction, scanning electron microscope analysis show: the deposition products therefrom is the silicon B-carbide structure, and nanowire surface is comparatively smooth, does not have plethora and bifurcated.Work as CH
3SiCl
3/ H
2Ratio is 1: 10 o'clock, and nanowire diameter is 60～70nm, and length reaches tens microns; Along with CH
3SiCl
3/ H
2The increase of ratio, nanowire diameter increases gradually, and foreign matter content raises, and purity descends.
Fig. 2 is for working as CH
3SiCl
3/ H
2Ratio is the different amplification stereoscan photograph of 1: 10 o'clock prepared silicon carbide nanometer line.As seen the sedimentary nanowire surface of institute is comparatively smooth, does not have plethora and bifurcated, and diameter is 60～70nm, and length reaches tens microns.
Fig. 3 is the X ray diffracting spectrum at the silicon carbide nanometer line of carbon/carbon compound material surface preparation.Adopting the nano wire of chemical Vapor deposition process preparation as can be seen is the silicon B-carbide structure.
Fig. 4 is different CH
3SiCl
3/ H
2Stereoscan photograph than the silicon carbide nanometer line for preparing under the condition.As seen, along with CH
3SiCl
3/ H
2The increase of ratio, nanowire diameter increases gradually, and foreign matter content raises, and purity descends.
Claims (6)
1. the preparation method of a carbon/carbon compound material surface silicon carbide nano wire is characterized in that:
Step 1:, in baking oven, dry with clean behind the carbon/carbon compound material sanding and polishing with distilled water wash;
Step 2: hang in the vertical gaseous phase deposition stove after the carbon/carbon compound material binding that will handle with a branch of carbon fiber;
Step 3: cvd furnace vacuumized vacuum tightness is reached-0.09MPa after 15 minutes, left standstill 10 minutes, logical argon gas is to normal pressure, this process triplicate;
Step 4: energising heats up, when the cvd furnace temperature rises to 800 ℃～1200 ℃, and logical hydrogen pre-treatment sample in burner hearth, hydrogen flowing quantity is 300～600ml/min, the treatment time is 0.5～1h; When furnace temperature reaches predetermined depositing temperature, regulate the flux values of argon gas, hydrogen and METHYL TRICHLORO SILANE, and under this preset temperature, be incubated 1～3 hour, to turn off power supply subsequently and lower the temperature naturally, whole process is led to argon shield.
2. the preparation method of carbon/carbon compound material surface silicon carbide nano wire according to claim 1 is characterized in that: described the carbon/carbon compound material sanding and polishing is carried out successively with the sand paper of No. 400, No. 800 and No. 1000 respectively.
3. the preparation method of carbon/carbon compound material surface silicon carbide nano wire according to claim 1, it is characterized in that: at the predetermined depositing temperature described in the step 4 is 1000 ℃～1200 ℃, and the flow of described argon gas, hydrogen and METHYL TRICHLORO SILANE is respectively 300～500ml/min, 150～500ml/min and 50～150ml/min.
4. the preparation method of carbon/carbon compound material surface silicon carbide nano wire according to claim 1 is characterized in that: need guarantee that when step 3 leaves standstill 10 minutes system sealing is intact.Whether can observe vacuum meter and change, as no change, the illustrative system sealing is intact.
5. the preparation method of carbon/carbon compound material surface silicon carbide nano wire according to claim 3 is characterized in that: described hydrogen purity is greater than 99.99%.
6. the preparation method of carbon/carbon compound material surface silicon carbide nano wire according to claim 3 is characterized in that: the content of described METHYL TRICHLORO SILANE is greater than 98%, and passes through H
2The mode of bubbling carries it in the reaction chamber.
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| US7018947B2 (en) * | 2000-02-24 | 2006-03-28 | Shipley Company, L.L.C. | Low resistivity silicon carbide |
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