CN103754878A - Method for preparing carbon nano tubes on surfaces of silicon carbide particles through in-situ synthesis - Google Patents
Method for preparing carbon nano tubes on surfaces of silicon carbide particles through in-situ synthesis Download PDFInfo
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Abstract
The invention provides a method for growing multi-walled carbon nano tubes on the surface of micron silicon carbide powder in situ. The method comprises the steps of firstly oxidizing, acid-washing and alkali-washing the surface of the silicon carbide powder to remove silicon oxide and other impurities on the surface; secondly wrapping the surface of silicon carbide with a layer of uniformly distributed nano-catalyst particles by adopting the method of chemical codeposition, then putting the powder into a quartz tube furnace, and preparing the carbon nano tubes on the surface of silicon carbide in situ through catalytic cracking by utilizing the method of chemical vapor deposition. By adopting the method, uniform distribution of the carbon nano tubes on the surface of micron silicon carbide can be achieved, the difficulty that the carbon nano tubes are easy to agglomerate is solved, and a basis is provided for preparing high-performance multi-scale composite materials. The method is simple and has high feasibility. The prepared carbon nano tubes are uniformly dispersed on the surface of silicon carbide and are controllable in quantity.
Description
Technical field
The present invention relates to matrix material and preparing technical field thereof, particularly matrix material situ is prepared homodisperse carbon nanotube as the field of wild phase from generation method.
Background technology
Since carbon nanotube in 1991 is found by Iijima, due to its novel structure and distinctive mechanics, electricity and physicochemical property and potential purposes thereof, caused the very big concern of domestic and international chemistry, physics, material, electronics educational circles.Especially the mechanical property of carbon nanotube and excellence thereof: its average Young's modulus reaches 1.8TPa, be about 100 times of steel, flexural strength can reach 14.2GPa, the strain energy of depositing reaches 100keV, demonstrate superpower mechanical property, and its density is low, the density of Single Walled Carbon Nanotube is 1.2～1.3g/cm3 approximately, multi-walled carbon nano-tubes density is only also 1.7g/cm3, is only 1/6 of steel, is almost current specific tenacity and the highest material of specific rigidity.Therefore, if it is made Reinforcements for Metal Matrix Composites and not only can improve intensity, also can further reduce density of material.
But due to the nanoscale effect of carbon nanotube, when as wild phase, easily reunite, in matrix, disperse inequality, do not have the effect of wild phase; Present stage, the methods that adopt were that high-energy ball milling method is that carbon nanotube scatter uniformly in matrix more, but this method is due to the inevitable damage of having shone into carbon nanotube structure of high energy of ball milling, last performance is impacted, and the volume fraction that can make even carbon nanotube disperse is very limited.And searching document is found, in the production method of carbon nanotube, chemical gaseous phase depositing process is simple, and operability is large, but need to carry out separation to the carrier of last Formed nanotube, obtains pure carbon nanotube.
Silicon carbide also has excellent over-all properties due to it, is widely used now, as the wild phase of metal-base composites; And if application silicon carbide is as the carrier of chemical vapor deposition for carbon nanotubes, not only can save the step of carrier separation, and can make silicon carbide and carbon nanotube simultaneously as the wild phase of metallic matrix, strengthening effect may be better.
Existing document and invention retrieval are found in document, also there is no the report of this respect; And Chinese patent (CN102504760A) " preparation method of a kind of silicon carbide and carbon nano tube composite wave-absorbing material ", mainly by pickling process, at silicon carbide, prepare metal-silicon carbide mixture, then evaporate to dryness is directly put into silica tube and is passed into methane, and heating and heat preservation obtains silicon carbide and carbon nano tube composite wave-absorbing material; Chinese patent (CN102962087A) " a kind of carbon nanotube/foam silicon carbon catalytic composite materials and preparation method thereof " is mainly as carrier with foam silicon carbon, Fe-Mg-Al, as composite catalyst, adopts the method for chemical vapor deposition for carbon nanotubes.These two patents have all been prepared carbon nanotube, but in these two patents, main utilization is suction ripple and the catalytic performance of carbon nanotube, and there are many deficiencies: the metal-silicon carbide mixture that (1) adopts pickling process to prepare, metallic particles size and distribution are all inhomogeneous, can not play well catalytic performance; (2) in chemical vapour deposition deposition, do not adopt carrier gas to be easy to produce indefiniteness carbon, the performance of material is shone into impact; (3) adopt Fe-Mg-Al composite catalyst to have bad impact to the last performance of matrix material.
Summary of the invention
The method that the object of this invention is to provide the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ.The method technique even carbon nanotube simple, workable, preparation is controlled.
The present invention is achieved by the following technical solutions: first silicon carbide is oxidized, pickling, alkali cleaning surface treatment, remove surperficial silicon oxide and impurity thereof; Then adopt the method for chemical codeposition to prepare the equally distributed nanocatalyst particle of one deck at silicon carbide, to put into quartz tube furnace containing granules of catalyst silicon carbide again, and utilize the method for chemical vapour deposition to prepare carbon nanotube in silicon carbide situ catalytic.
The present invention includes following steps:
1) surface treatment of silicon-carbide particle: take silicon-carbide particle, be placed in chamber type electric resistance furnace, be heated to 800-1200 ℃, insulation, furnace cooling is to room temperature; Then, silicon carbide is added in the HF aqueous solution, rear by washed with de-ionized water, suction filtration; Join the saturated NaOH aqueous solution again silicon carbide is carried out to roughening treatment, then deionized water suction filtration, cleans.Finally put into loft drier is incubated at 100-200 ℃.
2) preparation of silicon-carbide particle surface catalyst: acetate is dissolved in deionized water and is made into the aqueous solution, stir to clarify, then to the silicon-carbide particle that adds step 1) to process in solution, supersound process; Add NH
3h
2o solution, until required pH value, magnetic agitation, the standing deposition of room temperature, washed with de-ionized water, after suction filtration, 80-150 ℃ dry 10-20 hour, then 300-600 ℃ of calcining in air, makes the oxide particle of nano level catalyzer at catalyst surface.
3) silicon-carbide particle of handling well silicon-carbide particle surface chemistry deposition of carbon nanotubes: by step 2) is layered in quartz boat, is placed in quartz tube furnace; Under argon gas atmosphere protection, be raised to 300-550 ℃, close argon gas, pass into hydrogen 1-5 hour; Then be warmed up to 600-900 ℃, pass into methane and argon gas, insulation reaction 10-120 minute, stops ventilating methane, and cool to room temperature under argon shield obtains silicon carbide and carbon nano tube compound material.
In the present invention, described HF aqueous solution massfraction is 40%.
In the present invention, NH
3h
2o strength of solution is 0.5mol/L.
In the present invention, required pH value is between 6-9.
In the present invention, silicon-carbide particle size used is 10-100 μ m.
In the present invention, the acetate of metal used and the mol ratio of silicon carbide are that 1:10 is between 1:90.Metal used can be nickel or iron or cobalt etc.
In the present invention, described mixed solution room temperature time of repose is between 1-48 hour.
In the present invention, that tells passes into methane and argon gas, the volume ratio of two kinds of gases at 1:3 between 1:10.
The oxide particle of the catalyzer that in the present invention, prepared by silicon carbide is between 1-200nm.
In the method for the invention, first to micron order silicon carbide, with massfraction, be that the 40%HF aqueous solution and saturated sodium hydroxide are processed, can not only remove surperficial impurity, and make silicon carbide alligatoring and activation, increase the adsorptive power of nanoparticle at silicon carbide.Adopt acetate as the raw material of preparing nanoparticle, and the method that adopts chemical codeposition makes nickel acetate react with weakly alkaline solution, at silicon carbide, form the particle of nano level oxyhydroxide, this compares with traditional pickling process, reduce calcining and reduction temperature, saved the energy.Adopt the method for chemical vapour deposition to prepare carbon nanotube, this method simple and feasible, does not need the severe condition such as High Temperature High Pressure in additive method, can realize large-scale production; Select wild phase micron order silicon carbide powder conventional in metal matrix as carrier, the silicon carbide of preparing and carbon nano tube compound material can be directly as the wild phase of matrix material, save will be separated with carrier when carbon nanotube is applied process;
Compared with prior art, beneficial effect of the present invention is:
1, the present invention has realized in-situ growing carbon nano tube, has overcome the nanoscale effect of carbon nanotube, has obtained the composite strengthening phase of uniform loading on micron order silicon-carbide particle.
2, the present invention has saved the purge process of the removal carrier while preparing carbon nanotube, no matter and carrier used and catalyzer finally can in matrix material, play strengthening effect.
3, the technological process simple and feasible that the present invention adopts, has avoided preparing the High Temperature High Pressure needing in carbon nanotube process, can realize large-scale production.
Accompanying drawing explanation
Fig. 1: the process flow sheet of carbon nanotube is prepared in catalytic pyrolysis chemical vapour deposition;
Fig. 2: the granules of catalyst of silicon-carbide particle surface preparation and the scanning electron microscope (SEM) photograph of carbon nanotube;
Fig. 3: the material phase analysis figure of silicon-carbide particle area load carbon nanotube.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.It should be pointed out that following embodiment just further illustrates of the present invention, but protection scope of the present invention is not limited to following examples.
Silicon carbide described in following examples is Powdered α-SiC, has all passed through the process of oxidation, pickling, alkali cleaning before Kaolinite Preparation of Catalyst.The catalyzer of preparation and the detection of carbon nanotube mainly use scanning electronic microscope (SEM) to complete, and the thing of final product has detected mutually X-ray diffractometer and completed.Embodiment implements according to flow process shown in Fig. 1.
The surface treatment flow process of silicon-carbide particle: take silicon-carbide particle, be placed in chamber type electric resistance furnace, be heated to 800-1200 ℃, insulation, furnace cooling is to room temperature; Then, it is in the 40%HF aqueous solution that silicon carbide is added to massfraction, rear by washed with de-ionized water, suction filtration; Join the saturated NaOH aqueous solution again silicon carbide is carried out to roughening treatment, then deionized water suction filtration, cleans.Finally put into loft drier is incubated at 100-200 ℃.
Embodiment 1
By in the beaker of four water acetic acid nickel as for 150ml, add 80ml deionized water, stir to clarify, by surface-treated silicon carbide, by the mol ratio 20:1 with four water acetic acid nickel, join in beaker, put into ultrasonic apparatus ultrasonic cleaning 0.5 hour, take out, be placed on magnetic stirring apparatus, add while stirring the NH of 0.5mol/L
3h
2the O aqueous solution, until pH value is 7, continues magnetic agitation after 1 hour, at room temperature standing 48 hours, then uses deionized water rinsing, suction filtration; Take out the powder in funnel, put into 100 ℃, loft drier, dry 10 hours, then put into the chamber type electric resistance furnace of 450 ℃, under air atmosphere, calcine 2 hours.At catalyst surface, make the oxide particle of nano level catalyzer.
Get the powder of the processing of 500 milligrams; put into quartz boat; be placed in quartz tube furnace; under the argon shield atmosphere of 500ml/min; be warmed up to 500 ℃; close argon gas; the hydrogen reducing 2 hours that passes into 300ml/min, continues to be heated to 700 ℃, passes into argon gas and methane gas that volume ratio is 1:1; react 1 hour; close methane, cool to room temperature under argon shield atmosphere, takes out; weigh the weight of final powder, obtain containing massfraction and be the silicon carbide compound powder of 2% carbon nanotube.
Embodiment 2
By in the beaker of four water acetic acid nickel as for 150ml, add 50ml deionized water, stir to clarify, again by surface-treated silicon carbide, by the mol ratio 10:1 with four water acetic acid nickel, join in beaker, put into ultrasonic apparatus ultrasonic cleaning 0.5 hour, take out, be placed on magnetic stirring apparatus, the NH3H2O aqueous solution 8 that adds while stirring 0.5mol/L, continues to stir after 1 hour at room temperature standing 48 hours, then with deionized water rinsing, to PH, be neutral, suction filtration; Take out the powder in funnel, put into 150 ℃, loft drier, dry 10 hours, then put into the chamber type electric resistance furnace of 500 ℃, under air atmosphere, calcine 2 hours.
Get the powder of the processing of 500 milligrams; put into quartz boat; be placed in quartz tube furnace; under the argon shield atmosphere of 500ml/min; be warmed up to 550 ℃; close argon gas; the hydrogen reducing 1 hour that passes into 300ml/min, continues to be heated to 700 ℃, passes into argon gas and methane gas that volume ratio is 1:2; react 1.5 hours; close methane, cool to room temperature under argon shield atmosphere, takes out; weigh the weight of final powder, obtain containing massfraction and be the silicon carbide compound powder of 5% carbon nanotube.
Embodiment 3
By in the beaker of four water acetic acid nickel as for 150ml, add 50ml deionized water, stir to clarify, by surface-treated silicon carbide, by the mol ratio 20:1 with four water acetic acid nickel, join in beaker again, put into ultrasonic apparatus ultrasonic cleaning 0.5 hour, take out, be placed on magnetic stirring apparatus, add while stirring the ammonia soln of 0.5mol/L, until pH value is 9, continue to stir after 1 hour, at room temperature standing 24 hours, then use deionized water rinsing, suction filtration; Take out the powder in funnel, put into 120 ℃, loft drier, dry 10 hours, then put into the chamber type electric resistance furnace of 500 ℃, under air atmosphere, calcine 2 hours.
Get the powder of the processing of 500 milligrams; put into quartz boat; be placed in quartz tube furnace; under the argon shield atmosphere of 500ml/min; be warmed up to 500 ℃; close argon gas; the hydrogen reducing 2 hours that passes into 300ml/min, continues to be heated to 800 ℃, passes into argon gas and methane gas that volume ratio is 2:1; react 1 hour; close methane, cool to room temperature under argon shield atmosphere, takes out; weigh the weight of final powder, obtain containing massfraction and be the silicon carbide compound powder of 10% carbon nanotube.
By in the beaker of four water acetic acid nickel as for 150ml, add 80ml deionized water, stir to clarify, by surface-treated silicon carbide, by the mol ratio 40:1 with four water acetic acid nickel, join in beaker, put into ultrasonic apparatus ultrasonic cleaning 0.5 hour, take out, be placed on magnetic stirring apparatus, add while stirring the ammonia soln of 0.5mol/L, until pH value is 8, continue to stir after 1 hour, at room temperature standing 48 hours, then use deionized water rinsing, suction filtration; Take out the powder in funnel, put into 100 ℃, loft drier, dry 10 hours, then put into the chamber type electric resistance furnace of 500 ℃, under air atmosphere, calcine 2 hours.
Get the powder of the processing of 500 milligrams; put into quartz boat; be placed in quartz tube furnace; under the argon shield atmosphere of 500ml/min; be warmed up to 500 ℃; close argon gas; the hydrogen reducing 2 hours that passes into 300ml/min, continues to be heated to 800 ℃, passes into argon gas and methane gas that volume ratio is 1:3; react 2 hours; close methane, cool to room temperature under argon shield atmosphere, takes out; weigh the weight of final powder, obtain containing massfraction and be the silicon carbide compound powder of 20% carbon nanotube.
Figure 2 shows that the middle silicon carbide of embodiment 3 is through H
2the stereoscan photograph of the carbon nanotube obtaining after the catalyst n i particle obtaining after reduction and chemical vapour deposition, as we can see from the figure, the granules of catalyst of preparation is evenly distributed, size is tiny, between several nanometers and tens nanometers, illustrate that the catalyzer of preparation can well play katalysis at the preparatory phase of carbon nanotube by this method.From figure, the stereoscan photograph of carbon nanotube can be found out, the carbon nanotube of preparation is even in silicon-carbide particle surface arrangement, substantially there is no the generation of indefiniteness carbon.Fig. 3 is the XRD figure spectrum of last composite powder, learns in final powder, have the Ni simple substance of its katalysis and the existence of carbon nanotube from spectrogram.In the present invention, other embodiment effects are also fine, and therefore, the present invention can prepare the controlled carbon nanotube of one deck amount at carbon powder SiClx surface uniform.
Be more than part preferred embodiment of the present invention, should be understood that, the present invention also has other embodiment, and such as the material mixture ratio in change above-described embodiment and parameter value etc., this is easy to realize to one skilled in the art.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. a method for the spontaneous carbon nanotube of silicon-carbide particle surface in situ, is characterized in that, comprises the following steps:
1) surface treatment of silicon-carbide particle: silicon-carbide particle is placed in to chamber type electric resistance furnace, is heated to 800-1200 ℃, insulation, furnace cooling is to room temperature; Then, silicon carbide is added in the HF aqueous solution, rear by washed with de-ionized water, suction filtration; Join again the saturated NaOH aqueous solution silicon carbide is carried out to roughening treatment, washed with de-ionized water then, suction filtration; Finally put into loft drier is incubated at 100-200 ℃;
2) preparation of silicon-carbide particle surface catalyst: metal acetate salt is dissolved in deionized water and is made into the aqueous solution, stir to clarify, then add the silicon-carbide particle after step 1) is processed, supersound process in solution; Add NH
3h
2o solution, until required pH value, magnetic agitation, the standing deposition of room temperature, cleans, after suction filtration, 80-150 ℃ dry 10-20 hour, then 300-600 ℃ of calcining in air, makes the oxide particle of nano level catalyzer at catalyst surface;
3) silicon-carbide particle of handling well silicon-carbide particle surface chemistry deposition of carbon nanotubes: by step 2) is layered in quartz boat, is placed in quartz tube furnace; Under argon gas atmosphere protection, be raised to 300-550 ℃, close argon gas, pass into hydrogen 1-5 hour; Then be warmed up to 600-900 ℃, pass into methane and argon gas, insulation reaction 10-120 minute, stops ventilating methane atmosphere, and cool to room temperature under argon shield obtains silicon carbide and carbon nano tube compound material.
2. the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ according to claim 1, is characterized in that, in step 1), is placed in chamber type electric resistance furnace, and soaking time is 2 hours; Putting into loft drier soaking time is 10 hours; HF aqueous solution massfraction is 40%.
3. the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ according to claim 1, is characterized in that step 2) in, the mol ratio of metal acetate salt used and silicon carbide is that 1:10 is between 1:90.
4. the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ according to claim 3, is characterized in that step 2) in, metal acetate salt is dissolved in deionized water, and strength of solution is between 0.1mol/L～1mol/L; NH
3h
2o strength of solution is 0.5mol/L.
5. the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ according to claim 4, is characterized in that, described metal acetate salt, and its metal is nickel or iron or cobalt.
6. according to the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ described in claim 1-5 any one, it is characterized in that step 2) in, the supersound process time is 30 minutes; The magnetic agitation time is 1 hour; Required pH value is between 6-9.
7. according to the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ described in claim 1-5 any one, it is characterized in that step 2) in, the standing depositing time of described room temperature is between 1-48 hour.
8. according to the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ described in claim 1-5 any one, it is characterized in that, in step 3), the described volume ratio that passes into methane and argon gas at 1:3 between 1:10.
9. according to the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ described in claim 1-5 any one, it is characterized in that, silicon-carbide particle size used is 10-100 μ m.
10. according to the method for the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ described in claim 1-5 any one, it is characterized in that, the oxide particle of catalyzer prepared by described silicon carbide is between 1-200nm.
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| CN112898101A (en) * | 2021-02-01 | 2021-06-04 | 常州大学 | Preparation method of carbon nano tube doped octogen composite flexible explosive |
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