CN1618733A - Preparation method of carbon nano-pipe - Google Patents
Preparation method of carbon nano-pipe Download PDFInfo
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- CN1618733A CN1618733A CNA2003101123354A CN200310112335A CN1618733A CN 1618733 A CN1618733 A CN 1618733A CN A2003101123354 A CNA2003101123354 A CN A2003101123354A CN 200310112335 A CN200310112335 A CN 200310112335A CN 1618733 A CN1618733 A CN 1618733A
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Abstract
A process for preparing the carbon nanotubes includes such steps as providing a smooth basic bottom, depositing magnetic catalyst on the surface of said basic bottom, arranging a magnetic element above said basic bottom, introducing gas-state-carbon source, and reacting while vertically growing carbon nanotubes from said basic bottom.
Description
[technical field]
The present invention relates to a kind of preparation method of carbon nanotube, particularly a kind of preparation method of straight carbon nanotube.
[background technology]
Carbon nanotube is that a kind of diameter of being made up of carbon atom is the pipe of nanometer scale, all is six-ring at carbon nanotube graphite linings central part, endways or turnover five-ring or seven-membered ring are partly then arranged.Carbon nanotube is found first in by the product of Iijima at arc-over in 1991, specifically sees also document Nature, Vol.354, P.56 (1991).The special construction of carbon nanotube determines it to have good comprehensive mechanical property, as high elastic coefficient and low density, and excellent electric property, thermal property and absorption property.Variation along with length, diameter and the spiral way of carbon nanotube, carbon nanotube can present metalline or semiconductor property, wherein, metal mold carbon nanotube itself can be used as a kind of molecule-type plain conductor and plays a significant role in fields such as nanoelectronics, Materials science.
It is several that the present method for preparing carbon nanotube mainly contains arc discharge method, laser evaporation method and chemical Vapor deposition process.The carbon nanotube that arc discharge method and laser evaporation method form has following shortcoming: (1) carbon nanotube output is lower; (2) carbon nanotube is mixed in together with other carbon nano-particle, therefore causes carbon nano pipe purity very low, also needs complicated purification process, increases manufacturing cost; (3) direction of growth of carbon nanotube is uncontrollable, and formed carbon nanotube is unordered chaotic shape, is difficult to industrial as the practical application of molecule-type plain conductor.So the method that forms ordered carbon nanotube array at present mainly is a chemical Vapor deposition process.Chemical vapour deposition is to use the transition metal of nanoscale or its oxide compound or its alloy as catalyzer, and the carbonaceous gas of pyrolysis prepares carbon nano pipe array under relatively low temperature.
See also document " Self～oriented regular arrays of carbon nanotubes and theirfield emission properties ", Science, Vol.283, P.512～514 (1999), the preparation methods that the people provided such as Fan Shoushan are: (1) at first provides at the bottom of the porous silicon-base, and its aperture is approximately 3 nanometers; (2) in substrate, form the catalyst layer that one deck has regular pattern by mask plate deposited by electron beam evaporation method; (3) in air, will deposit the substrate of catalyst layer in 300 ℃ of annealing; (4) substrate is placed in the central reaction chamber of sending into the silica tube Reaktionsofen in the quartz reaction boat, under the protection of argon gas, Reaktionsofen is heated to 700 ℃; (5) feeding flow is the ethylene gas of 1000sccm, reacts 15～60 minutes; (6) with the Reaktionsofen cool to room temperature, ordered carbon nanotube array promptly is formed at the catalyst area of substrate, and perpendicular to substrate.
But, the carbon nanotube that obtains by above-mentioned method for making has defective on microstructure, promptly cause the carbon nanotube bending owing to the thermally labile at its preparation initial stage and the existence of five yuan of carbocyclic rings and seven-element carbon ring, thereby reduce its electroconductibility, it is had difficulties as the molecule-type plain conductor in practical application in industry.So good electroconductibility when guaranteeing carbon nanotube as the molecule-type plain conductor must provide a kind of preparation method of straight carbon nanotube.
[summary of the invention]
For solving carbon nanotube of the prior art has defective on microstructure problem, the object of the present invention is to provide a kind of preparation method of straight carbon nanotube.
For realizing purpose of the present invention, the invention provides a kind of preparation method of straight carbon nanotube, it comprises: a smooth substrate is provided; Magnetic catalyst is deposited on described substrate surface; A distance, top in described substrate is provided with magnetics; Feed carbon source gas and react, carbon nanotube grows from described substrate.
Compared with prior art, the present invention is provided with magnetics in a distance, top of the substrate of carbon nano-tube, the magnetic field that described magnetics is produced in the process of growth of carbon nanotube can guide carbon nanotube along the direction growth perpendicular to described substrate to the effect of magnetic catalyst, prevent carbon nanotube generation crooked and phenomenon such as doping five-ring and seven-membered ring in its six-ring structure, thereby obtain straight carbon nanotube, guarantee conductivity good when carbon nanotube is used as the molecule-type plain conductor.
[description of drawings]
Fig. 1 is the schema that CVD legal system of the present invention is equipped with carbon nanotube.
Fig. 2 is the synoptic diagram before the CVD method carbon nano-tube of the present invention.
Fig. 3 is the synoptic diagram of the carbon nanotube of CVD method acquisition of the present invention.
[embodiment]
See also Fig. 1, the preparation method of carbon nanotube provided by the invention comprises the following steps: step 11, and a smooth substrate is provided; Step 12 is deposited on described substrate surface with magnetic catalyst; Step 13 is provided with magnetics in a distance, top of described substrate; Step 14 feeds carbon source gas and reacts, and carbon nanotube grows from described substrate.
See also Fig. 2 and Fig. 3, the preparation method of carbon nanotube provided by the present invention is elaborated.
One smooth substrate 3 at first is provided.Use P type silicon wafer as substrate in the present embodiment, its diameter is 5.08 centimetres, thick 350 microns, described substrate polishing is promptly obtained smooth substrate 3.Described substrate also can select for use N type silicon wafer, intrinsic silicon wafer or surface that the silicon wafer of one silica layer is arranged.
Secondly, magnetic catalyst 6 is deposited on smooth substrate 3 surfaces.Utilize electron beam vapor deposition method, heat deposition method or sputtering method etc. to be formed on the smooth substrate 3 magneticmetal; The smooth substrate 3 that deposits magneticmetal is positioned in the air,, makes magneticmetal be oxidized to metal oxide particle (figure does not show) in about 10 hours of 300～400 ℃ of thermal treatments; It is reduced into nano-scale magnetic catalyzer 6 with reducing gas; Smooth substrate 3 after will handling again cuts into rectangle.Wherein, magneticmetal can be one of iron (Fe), cobalt (Co), nickel (Ni) or its alloy, selects iron in the present embodiment for use; The deposit thickness of described magneticmetal is that several nanometers arrive the hundreds of nanometer, is preferably 5 nanometers; Reducing gas can be hydrogen or ammonia etc.
Then, in a distance, top of smooth substrate 3 magnetics is set.Will be wherein a slice rectangle smooth substrate 3 pack in the reaction boat 2, reaction boat 2 is sent in the central reaction chamber 1 of quartz tube furnace, opposite face in reaction chamber 1 top, smooth substrate 3 is provided with magnetics, and makes described magnetics and smooth substrate 3 at a distance of a predetermined distance.In the present embodiment, magnetics is one to be wrapped in the spiral coil 5 on the column 7, feeds a scheduled current in spiral coil 5, feeding shielding gas and be heated to a preset temperature to reaction chamber 1 in.Wherein, described shielding gas can be rare gas element or nitrogen, selects argon gas in the present embodiment for use; Described preset temperature when selecting for use metallic iron to be catalyst metal, then generally is heated to 500～700 ℃ because of the difference of magnetic catalyst material is different, is preferably 650 ℃; The action that feeds a scheduled current in spiral coil 5 also can be carried out after feeding shielding gas; Magnetics also can use magnet etc., and other has the element that magnetic can attract magnetic catalyst 6.
At last, feed carbon source gas and react, carbon nanotube 7 grows and perpendicular to smooth substrate 3 from smooth substrate 3.Wherein, carbon source gas is hydrocarbon polymer, comprises acetylene, ethene etc., selects acetylene in the present embodiment for use.
Present embodiment is provided with a spiral coil 5 in a distance, top of smooth substrate 3, control feeds the size of current of spiral coil 5, substrate 3 and the distance of spiral coil 5 and the size and the distribution of magnetic catalyst 6, make the magnetic field force of magnetic catalyst 6 at the spiral coil 5 of energising, under the acting in conjunction of the anchorage force of self gravitation and carbon nanotube 7, guiding carbon nanotube 7 is in the growth of the top of vertical substrate 3 directions and basad 3, because the sucking action of above-mentioned magnetic field force, can overcome carbon nanotube 7 at the thermally labile of early growth period and the buckling phenomenon that causes, and can prevent the generation of microstructural defects phenomenon such as doping five-ring and seven-membered ring in the six-ring of carbon nanotube 7 structure, thereby obtain straight carbon nanotube 7.
Claims (10)
1. the preparation method of a carbon nanotube is characterized in that may further comprise the steps: a smooth substrate is provided; Magnetic catalyst is deposited on described substrate surface; A distance, top in described substrate is provided with magnetics; Feed carbon source gas and react, carbon nanotube grows from described substrate.
2. the preparation method of carbon nanotube as claimed in claim 1 is characterized in that, described smooth substrate is the silicon wafer of silicon wafer or tool silicon oxide layer.
3. the preparation method of carbon nanotube as claimed in claim 1 is characterized in that, described magnetic catalyst comprises iron, cobalt, nickel or its alloy.
4. the preparation method of carbon nanotube as claimed in claim 1 is characterized in that, described magnetics comprises spiral coil or magnet.
5. the preparation method of carbon nanotube as claimed in claim 1 is characterized in that, before feeding the carbon source solid/liquid/gas reactions, also comprise will deposit magnetic catalyst substrate in air in 300～400 ℃ of thermal treatments 10 hours.
6. the preparation method of carbon nanotube as claimed in claim 5 is characterized in that, after described thermal treatment, feed before carbon source gas reacts, also comprises substrate under the atmosphere of shielding gas, preheats 650 ℃.
7. the preparation method of carbon nanotube as claimed in claim 1 is characterized in that, described carbon source gas bag is drawn together ethene or acetylene.
8. the preparation method of carbon nanotube as claimed in claim 6 is characterized in that, described shielding gas comprises argon gas or other rare gas element.
9. the preparation method of carbon nanotube as claimed in claim 1 is characterized in that, polished finish is passed through in described substrate in advance.
10. the preparation method of carbon nanotube as claimed in claim 5 is characterized in that, after depositing the substrate thermal treatment of magnetic catalyst, further comprises it is reduced with reducing gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2003101123354A CN1275851C (en) | 2003-11-22 | 2003-11-22 | Preparation method of carbon nano-pipe |
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| CNB2003101123354A CN1275851C (en) | 2003-11-22 | 2003-11-22 | Preparation method of carbon nano-pipe |
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| CN1618733A true CN1618733A (en) | 2005-05-25 |
| CN1275851C CN1275851C (en) | 2006-09-20 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100515936C (en) * | 2005-10-28 | 2009-07-22 | 鸿富锦精密工业（深圳）有限公司 | Preparation device and method of carbon nano-tube |
| CN105731417A (en) * | 2014-12-11 | 2016-07-06 | 山东大展纳米材料有限公司 | Apparatus and method for purifying carbon nanotubes |
| US9506194B2 (en) | 2012-09-04 | 2016-11-29 | Ocv Intellectual Capital, Llc | Dispersion of carbon enhanced reinforcement fibers in aqueous or non-aqueous media |
| CN106556589A (en) * | 2017-01-12 | 2017-04-05 | 重庆大学 | The preparation method and its substrate of high duplication surface enhanced Raman scattering substrate |
| CN107128901A (en) * | 2017-05-12 | 2017-09-05 | 长春理工大学 | A kind of oriented and ordered preparation method of carbon nano-tube |
| CN107400872A (en) * | 2016-05-20 | 2017-11-28 | 清华大学 | The preparation method of carbon-fiber film |
-
2003
- 2003-11-22 CN CNB2003101123354A patent/CN1275851C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100515936C (en) * | 2005-10-28 | 2009-07-22 | 鸿富锦精密工业（深圳）有限公司 | Preparation device and method of carbon nano-tube |
| US9506194B2 (en) | 2012-09-04 | 2016-11-29 | Ocv Intellectual Capital, Llc | Dispersion of carbon enhanced reinforcement fibers in aqueous or non-aqueous media |
| CN105731417A (en) * | 2014-12-11 | 2016-07-06 | 山东大展纳米材料有限公司 | Apparatus and method for purifying carbon nanotubes |
| CN107400872A (en) * | 2016-05-20 | 2017-11-28 | 清华大学 | The preparation method of carbon-fiber film |
| CN107400872B (en) * | 2016-05-20 | 2019-09-13 | 清华大学 | The preparation method of carbon-fiber film |
| CN106556589A (en) * | 2017-01-12 | 2017-04-05 | 重庆大学 | The preparation method and its substrate of high duplication surface enhanced Raman scattering substrate |
| CN107128901A (en) * | 2017-05-12 | 2017-09-05 | 长春理工大学 | A kind of oriented and ordered preparation method of carbon nano-tube |
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| CN1275851C (en) | 2006-09-20 |
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