CN101234760B - Equipment and method for manufacturing nano carbon tube - Google Patents
Equipment and method for manufacturing nano carbon tube Download PDFInfo
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- CN101234760B CN101234760B CN2007100061819A CN200710006181A CN101234760B CN 101234760 B CN101234760 B CN 101234760B CN 2007100061819 A CN2007100061819 A CN 2007100061819A CN 200710006181 A CN200710006181 A CN 200710006181A CN 101234760 B CN101234760 B CN 101234760B
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Abstract
The invention relates to a manufacturing equipment of a carbon nano-tube and a manufacturing method thereof. The manufacturing equipment comprises a carbon material, a base and a heating device. The base which corresponds to the carbon material is provided with a carbon layer and a catalyst; the catalyst is arranged on the carbon layer and towards the carbon material. The heating device is used for heating the carbon material and the heating lasts for an operation period, so that carbon ion in the carbon material can be dissociated out, and the carbon nano-tube can be formed on random specified catalyst of the base. At the same time, the carbon nano-tube of array distribution is formed on the substrate by the equipment of the carbon material.
Description
Technical field
The invention relates to making equipment of a kind of CNT (carbon nano-tube) and preparation method thereof; Particularly relevant a kind of directly making equipment of growth CNT (carbon nano-tube) and preparation method thereof under atmospheric environment.
Background technology
CNT (carbon nano-tube) is a kind of type material of just finding at the nineties initial stage, particularly, is a kind of cylindrical carbon material with nano-grade size, and its hardness is greater than diamond or steel, and has good heat conductivity, electroconductibility and stable chemical property.
Because outstanding and unique electronics and the mechanical characteristics of CNT (carbon nano-tube), therefore, it is in Materials science, chemistry, physics and other interdisciplinary fields, all have widely and use, for example, can be applicable to probe, nanoelectronic element, photoelectronics element, strengthening material of Field Emission Display, field-effect transistor(FET), hydrogen storage device, electron microscope etc., become one of critical material of development in science and technology of future.
The method of making CNT (carbon nano-tube) at present is quite a lot of, and have its relative merits respectively, the more common arc discharge method that the physical principle utilized is arranged (Arc Discharge), laser evaporation method (Laser Vaporization), or various chemical Vapor deposition processs (Chemicai Vapor Deposition, CVD), comprise thermo-cracking chemical Vapor deposition process (Thermal CVD), plasma chemical vapor deposition (Plasma Enhanced CVD) etc., wherein, common chemical method is to feed acetylene (C in reaction chamber
2H
2), under the environment of 350 degree～700 degree Celsius, deposit.
In above-mentioned three kinds of methods, be used so that arc discharge method is the most normal again, the ultimate principle of arc discharge method mainly is to utilize two graphite rods that are connected to power supply, arc-over as negative electrode and anode, in inert gas environment, discharges respectively, owing to can produce the high temperature more than 3000 ℃, the vertical part carbon of graphite anode rod can dissociate out, and then be deposited on the negative electrode graphite rod surface that is coated with catalyst, thus, just can be on cathode surface the formation of deposits CNT (carbon nano-tube).
Yet, utilize arc discharge method to make CNT (carbon nano-tube) and still have following shortcoming:
(1) the present technology that forms CNT (carbon nano-tube) with arc discharge method, must under special inert environments (being generally helium or argon gas), carry out, be subject to the special inert environments that to set up in advance, make the growth position and the area of CNT (carbon nano-tube) be restricted, and can increase its manufacturing cost;
(2) because the service temperature of arc discharge method is higher, the about high temperature more than 3000 ℃ of its local generation, therefore, with carbon is the CNT (carbon nano-tube) structure of material, be easy to generate combustion reactions after growing to certain altitude, so the height of the CNT (carbon nano-tube) of being grown is restricted, whole yield also significantly reduces;
(3) because CNT (carbon nano-tube) is to grow up in large area on the surface of negative electrode graphite rod, and uncontrollable its growth position.Therefore, when reality is used, need to collect earlier grown up CNT (carbon nano-tube) on the negative electrode graphite rod of part, afterwards again with its transfer coating to subject matter; Perhaps,, but must select to form in large area earlier, more unwanted part be struck off subsequently even can directly apply on the subject matter with having technology now.Thus, must increase degree of difficulty in the application;
(4) because the easy oxidation scission of CNT (carbon nano-tube), be difficult to the generation of inhibited oxidation reaction in the arc-over operation, so the CNT (carbon nano-tube) of being produced in this way, also be restricted its work-ing life.
In view of this, provide directly making equipment of growth CNT (carbon nano-tube) and preparation method thereof under atmospheric environment, an industry problem demanding prompt solution for this reason.
Summary of the invention
Main purpose of the present invention provides making equipment of a kind of CNT (carbon nano-tube) and preparation method thereof.The making method of disclosed CNT (carbon nano-tube) is to cooperate catalytic with simple arc discharging device, utilize the carbon material and have the substrate of carbon-containing bed and catalyst respectively as anode and negative electrode, the two has small spacing, again with the discharge mode of specific long fabric width (duration), and enough time generation chemical reactions are arranged and under the catalysis of catalyst, make CNT (carbon nano-tube) can be formed on the surface of substrate (negative electrode).
Another object of the present invention is and can directly forms CNT (carbon nano-tube) under atmospheric environment.General carbon material is heated under atmospheric environment, preferential easily generation oxidation, be unfavorable for the production CNT (carbon nano-tube), yet the present invention will be controlled at below several microseconds discharge time, make plasma body and the effect of carbon material after, just stop discharge behind the moment growth carbon pipe, so, before CNT (carbon nano-tube) also has little time oxidizing reaction takes place, promptly generate CNT (carbon nano-tube).
Another purpose of the present invention is to control flexibly the generation position of CNT (carbon nano-tube).Because CNT (carbon nano-tube) can be formed on the substrate corresponding to anode carbon material part, by adjusting the anodic position, be the growth position of may command CNT (carbon nano-tube), even directly the specific region on subject matter become to grow required CNT (carbon nano-tube), to increase its range of application.
For reaching above-mentioned purpose, the making method of CNT (carbon nano-tube) of the present invention comprises the following step: at first, provide a carbon material and a substrate relative with the carbon material, wherein have a carbon-containing bed and catalyst in the substrate, this catalyst is to be positioned at carbon-containing bed go up and towards the carbon material; Afterwards, carry out a heating steps, and continue an operating period, make the carbon ion on the carbon material dissociate out, on the catalyst of substrate, generate CNT (carbon nano-tube) subsequently for the carbon material.
The present invention also discloses a kind of making equipment of CNT (carbon nano-tube), and it comprises: a carbon material, a substrate and a heating unit.This substrate is with respect to the carbon material, and it has a carbon-containing bed and catalyst, and this catalyst is to be positioned at carbon-containing bed go up and towards the carbon material.Heating unit is in order to heating carbon material, and continues an operating period, makes the carbon ion on the carbon material dissociate out, generates CNT (carbon nano-tube) subsequently on the catalyst of substrate.
For above-mentioned purpose of the present invention, technical characterictic and advantage can be become apparent, hereinafter will be elaborated with the preferred embodiment conjunction with figs..
Description of drawings
Fig. 1 is the synoptic diagram of CNT (carbon nano-tube) making equipment of the present invention and circuit framework thereof;
Fig. 2 is in the CNT (carbon nano-tube) making equipment, the schematic perspective view of carbon material and substrate;
Fig. 3 A is for being linearly aligned needle electrode; And
Fig. 3 B is the needle electrode that the matrix pattern is arranged.
Embodiment
Fig. 1 is the synoptic diagram that CNT (carbon nano-tube) making equipment of the present invention cooperates circuit framework, and Fig. 2 is the schematic perspective view of CNT (carbon nano-tube) making equipment.In this embodiment, the present invention adopts arc discharge method, desires directly to produce in atmospheric environment required CNT (carbon nano-tube).Please also refer to Fig. 1 and Fig. 2, the making equipment 100 of CNT (carbon nano-tube) of the present invention is to be arranged in the general atmosphere environment, and it mainly comprises a carbon material 110, a substrate 120 and a pulse heating device.In this embodiment, heating unit is to be example explaining with power supply 130, yet the user also can adopt other heating units, and to heat this carbon material 110, the present invention does not impose any restrictions for the pattern of heating unit.
Furthermore, the anode of this power supply 130 and negative electrode are connected to respectively in carbon material 110 and the substrate 120, when applying an operating voltage and an actuating current in carbon material 110 and substrate 120, produce a stable electric arc between carbon material 110 and the substrate 120, and continue an operating period, so, can make the carbon ion on carbon material 110 dissociate out, be deposited on the catalyst 124 on substrate 120 surfaces, to generate CNT (carbon nano-tube) 200 corresponding to carbon material 110 parts.In one embodiment of this invention, operating voltage is relevant with the thickness of electrode, and when electrode is thin more, operating voltage just can be more little, and operating voltage is between 30 volts～180 volts, and actuating current is between 1 ampere～5 amperes.
Specifically, the situation of oxidation takes place in the CNT (carbon nano-tube) 200 that produces for preventing under atmospheric environment, the present invention utilizes control loop 140 that a pulsed signal is provided, control transistor 150 is according to the specific time sequence switch, so that operating period (discharge time) is controlled between 0.1 microsecond to 500 microsecond, thus, plasma body and carbon material 110 are done in order to moment growth CNT (carbon nano-tube) 200, because the reaction times is short, can effectively suppress when CNT (carbon nano-tube) 200 generates the situation of oxidation to take place, or make it have little time to take place oxidizing reaction.In this embodiment, be to adopt transistor, yet the user also can adopt other switching elements to control discharge time, has in this technical field and knows that usually the knowledgeable can other alternative be controlled as switching element, the present invention does not limit this.
Because the position that CNT (carbon nano-tube) 200 is grown up is the position corresponding to carbon material 110, therefore, the user can adjust the position of carbon material 110, and directly becomes to grow required CNT (carbon nano-tube) 200 on a specific region of substrate 120 (subject matter).If need to form CNT (carbon nano-tube) more in large area, can utilize and a plurality ofly as shown in Fig. 3 A, be linearly aligned carbon material 110, or the carbon material 110 that is the arrangement of matrix pattern shown in Fig. 3 B, in substrate 120 (subject matter), to become to grow to be linear array or to be the CNT (carbon nano-tube) that the matrix pattern is arranged.The present invention does not impose any restrictions for the number and the arrangement mode thereof of carbon material 110.
In addition, with regard to different substrate 120, the present invention also can have various application examples, for example with measuring probe as this substrate 120.Clearer and more definite, after the arc-over operation, CNT (carbon nano-tube) can be formed at the place, tip of measuring probe, because CNT (carbon nano-tube) has high strength, has a characteristic of amount of deflection simultaneously, when it is applied to probe, can promote the scope of application of measuring probe, easily give birth to the destructive shortcoming when improving probe tip and contacting, and then increase the service life with determinand.
Make the CNT (carbon nano-tube) with arc discharge method except above-mentioned, type of heating of the present invention also can adopt the heater means of a pulse heat source, laser evaporation method (laser vaporization) for example, it is to utilize superlaser to replace arc-over, produces required CNT (carbon nano-tube).Specifically, this type of heating is to utilize a laser heating device heating this carbon material 110, and continues an of short duration operating period, makes the carbon ion on the carbon material 110 dissociate out, and generates CNT (carbon nano-tube) subsequently in substrate 120.In another embodiment of the present invention, also can adopt other pulse heat sources, infrared rays for example is to heat this carbon material 110.Must explanation be, no matter use which kind of heater means, operating period is to be controlled between 0.1 microsecond to 500 microsecond equally, promptly stops behind the instantaneously heating carbon material 110, to suppress the situation of CNT (carbon nano-tube) generation oxidation.
In sum, making equipment of CNT (carbon nano-tube) of the present invention and preparation method thereof, be that a carbon material and a substrate relative with it are provided under atmospheric environment, and utilize the electric arc that is produced or directly utilize laser to heat this carbon material, and continue one period extremely of short duration operating time, moment makes the carbon ion on the carbon material dissociate out, to form CNT (carbon nano-tube) corresponding to carbon material part in substrate.The making of existing CNT (carbon nano-tube) needs to carry out under particular surroundings, yet the present invention can directly can form CNT (carbon nano-tube) under atmospheric environment, can reduce its cost of manufacture, and its growth scope is difficult for being subject to the size of reaction chamber.
In addition, general carbon material is heated under atmospheric environment, will be easy to produce oxidation behavior, and can't produce CNT (carbon nano-tube), yet the present invention is controlled at operating period between 0.1 microsecond to 500 microsecond, to suppress the situation of CNT (carbon nano-tube) generation oxidation.Moreover because the position of the CNT (carbon nano-tube) that is generated is the position corresponding to the carbon material, therefore, the user can adjust the position of carbon material, and directly becomes to grow required CNT (carbon nano-tube) on a specific region of subject matter, the flexibility ratio when using to increase it.
The above embodiments only are used for exemplifying enforcement aspect of the present invention, and explain technical characterictic of the present invention, are not to be used for limiting protection category of the present invention.Any be familiar with this operator can unlabored change or the arrangement of the isotropism scope that all belongs to the present invention and advocated, the scope of the present invention should be as the criterion with the application's claim scope.
Claims (26)
1. method of making CNT (carbon nano-tube) under atmospheric environment comprises the following step:
One carbon material and a substrate relative with this carbon material are provided, wherein have a carbon-containing bed and catalyst in this substrate, this catalyst is to be positioned at this carbon-containing bed goes up and towards this carbon material; And
Carry out a pulse heating step for this carbon material, continue an operating period at every turn, this operating period is between 0.1 microsecond to 500 microsecond, makes the carbon ion on this carbon material dissociate out whereby, and produces CNT (carbon nano-tube) subsequently on the catalyst of this substrate.
2. making method as claimed in claim 1 is characterized in that this pulse heating step is for providing an electric arc.
3. making method as claimed in claim 2 is characterized in that also comprising and provides a power supply, this power supply to connect this carbon material and this substrate, and making this carbon material is an anode, and this substrate is a negative electrode.
4. making method as claimed in claim 3 is characterized in that this power supply applies an operating voltage and an actuating current in this anode and this negative electrode, to produce this electric arc between this anode and this negative electrode.
5. making method as claimed in claim 4 it is characterized in that this operating voltage is between 30 volts to 180 volts, and this actuating current is between 1 ampere to 5 amperes.
6. making method as claimed in claim 3 is characterized in that this anode is a needle electrode.
7. making method as claimed in claim 6 is characterized in that this needle electrode is graphite or carbon fiber.
8. making method as claimed in claim 6 is characterized in that the top of this needle electrode and the distance between this catalyst are between 1 micron to 10 microns.
9. making method as claimed in claim 6, the diameter that it is characterized in that an end of this needle electrode is less than 1 millimeter.
10. making method as claimed in claim 9 is characterized in that this carbon material is a graphite rod, and this graphite rod has 3 centimetres the diameter and the cone angle of 60 degree, to form this needle electrode.
11. making method as claimed in claim 1 is characterized in that this catalyst comprises the material that is selected from following group: iron, cobalt, nickel, lanthanum, yttrium and combination thereof.
12. making method as claimed in claim 1 is characterized in that this pulse heating step is for providing a pulse heat source at this carbon material.
13. making method as claimed in claim 12 is characterized in that this pulse heat source is laser or infrared rays.
14. making method as claimed in claim 1 is characterized in that this substrate is made up of a probe, forms this CNT (carbon nano-tube) with the top in this probe.
15. an equipment of making CNT (carbon nano-tube) under atmospheric environment comprises:
One carbon material;
One substrate is with respect to this carbon material, wherein has a carbon-containing bed and catalyst in this substrate, and this catalyst is to be positioned at this carbon-containing bed goes up and towards this carbon material; And
One pulse heating device in order to heat this carbon material, continues an operating period at every turn, and this operating period is between 0.1 microsecond to 500 microsecond, makes the carbon ion on this carbon material dissociate out whereby, and produces CNT (carbon nano-tube) subsequently on the catalyst of this substrate.
16. making equipment as claimed in claim 15, it is characterized in that this pulse heating device is a power supply, in order to apply an operating voltage and an actuating current in this carbon material and this substrate, making this carbon material is an anode, and this substrate is a negative electrode, and continue an operating period, make to produce an electric arc between this carbon material and this substrate, on this catalyst of this substrate, to produce CNT (carbon nano-tube).
17. making equipment as claimed in claim 16 it is characterized in that this operating voltage is between 30 volts to 180 volts, and this actuating current is between 1 ampere to 5 amperes.
18. making equipment as claimed in claim 16 is characterized in that this anode is a needle electrode.
19. making equipment as claimed in claim 18 is characterized in that this needle electrode is graphite or carbon fiber.
20. making equipment as claimed in claim 18 is characterized in that the top of this needle electrode and the distance between this catalyst are between 1 micron to 10 microns.
21. making equipment as claimed in claim 18, the diameter that it is characterized in that an end of this needle electrode is less than 1 millimeter.
22. making equipment as claimed in claim 21 is characterized in that this carbon material is a graphite rod, this graphite rod has 3 centimetres the diameter and the cone angle of 60 degree, to form this needle electrode.
23. making equipment as claimed in claim 15 is characterized in that this catalyst comprises the material that is selected from following group: iron, cobalt, nickel, lanthanum, yttrium and combination thereof.
24. making equipment as claimed in claim 15 is characterized in that this pulse heating device is to produce a pulse heat source.
25. making equipment as claimed in claim 24 is characterized in that this pulse heat source is laser or infrared rays.
26. making equipment as claimed in claim 15 is characterized in that this substrate is made up of a probe, forms this CNT (carbon nano-tube) with the top in this probe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100061819A CN101234760B (en) | 2007-01-29 | 2007-01-29 | Equipment and method for manufacturing nano carbon tube |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100061819A CN101234760B (en) | 2007-01-29 | 2007-01-29 | Equipment and method for manufacturing nano carbon tube |
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| Publication Number | Publication Date |
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| CN101234760A CN101234760A (en) | 2008-08-06 |
| CN101234760B true CN101234760B (en) | 2011-04-13 |
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| CN2007100061819A Expired - Fee Related CN101234760B (en) | 2007-01-29 | 2007-01-29 | Equipment and method for manufacturing nano carbon tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102874749B (en) * | 2012-09-12 | 2014-03-19 | 中国科学技术大学 | Method for manufacturing nano pipes |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235121A (en) * | 1999-06-04 | 1999-11-17 | 北京大学 | Method for preparing mono-layer nano-pipe |
| CN1463918A (en) * | 2002-06-06 | 2003-12-31 | 中国科学院金属研究所 | Process for preparing single wall nano carbon tube |
| CN1823006A (en) * | 2003-07-15 | 2006-08-23 | 索尼株式会社 | Carbon nanotube and production method therefor and carbon nanotube producing device |
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2007
- 2007-01-29 CN CN2007100061819A patent/CN101234760B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235121A (en) * | 1999-06-04 | 1999-11-17 | 北京大学 | Method for preparing mono-layer nano-pipe |
| CN1463918A (en) * | 2002-06-06 | 2003-12-31 | 中国科学院金属研究所 | Process for preparing single wall nano carbon tube |
| CN1823006A (en) * | 2003-07-15 | 2006-08-23 | 索尼株式会社 | Carbon nanotube and production method therefor and carbon nanotube producing device |
Non-Patent Citations (2)
| Title |
|---|
| 郭连权等.碳纳米管的制备及形貌研究.沈阳工业大学学报26 3.2004,26(3),353-356. |
| 郭连权等.碳纳米管的制备及形貌研究.沈阳工业大学学报26 3.2004,26(3),353-356. * |
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