CN100436312C - Method for preparing carbon nano tube device - Google Patents
Method for preparing carbon nano tube device Download PDFInfo
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- CN100436312C CN100436312C CNB2005101023232A CN200510102323A CN100436312C CN 100436312 C CN100436312 C CN 100436312C CN B2005101023232 A CNB2005101023232 A CN B2005101023232A CN 200510102323 A CN200510102323 A CN 200510102323A CN 100436312 C CN100436312 C CN 100436312C
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Abstract
This invention provides a preparation method for carbon nana-tube devices including: providing a carbon nano-tube wire, dipping it into a volatile organic solvent to be processed on the surface, applying an assistant device to shape the wire to a rudiment of a carbon nano-tube of a preset shape then to be heated to a certain pre-set temperature to keep it at the shape so as to further get a carbon nano-tube device. The manufacturing method includes: processing the nano-tube wire into a shaped apparatus to meet the needs of different shapes in different fields.
Description
[technical field]
The present invention relates to a kind of making method of carbon nano tube device.
[background technology]
Since the Iijima of Japanese NEC Corporation in 1991 finds carbon nanotube, all made significant headway in the oriented growth technology of the synthetic technology of big area carbon nano pipe array, CNT (carbon nano-tube) and the aspects such as modification technique of carbon nanotube.People such as Fan Shoushan are at document Nature, Vol.419,801 (2002), just once pointed out in SpinningContinuous CNT Yarns one literary composition, when extracting a branch of carbon nanotube from super in-line arrangement carbon nano pipe array, carbon nanotube can organize themselves into a long line of successive.Super in-line arrangement carbon nano pipe array role such as same silk cocoon in this process, the carbon nanotube in the array will join end to end owing to the effect of Van der Waals force, thereby can form a successive carbon nano tube line.
Optics, electricity and the mechanical properties of uniqueness because carbon nanotube has many excellences, this kind successive carbon nano tube line presents very application prospects in fields such as field emitting electronic source, illumination and Materials with High Strength.This carbon nano tube line is fixed on the cathode support body of Field Emission Display, can be used as field emitting electronic source; With the polaroid of its formation that is arranged in parallel, can be operated in ultraviolet band.This carbon nano tube line can also be as the filament of incandescent light, and it only needs very little power just can send incandescence.
Yet because different Application Areass, its shape demand to carbon nano tube line also is not quite similar, and extracts the carbon nano tube line of coming with aforesaid method, and its original-shape can not satisfy application demand, so can't directly apply in macroscopical field.
In view of this, be necessary to provide a kind of method for preparing carbon nano tube device, be used for carbon nano tube line is made into the carbon nano tube device with predetermined shape.
[summary of the invention]
To a kind of method for preparing carbon nano tube device be described with embodiment below, it can be made into carbon nano tube line the carbon nano tube device with predetermined shape.
A kind of method for preparing carbon nano tube device may further comprise the steps:
One carbon nano tube line is provided;
Carbon nano tube line is immersed in the volatile organic solvent so that it is carried out surface treatment;
Adopt a supplementary unit, the auxiliary carbon nano tube line of having handled well is shaped, and has the carbon nano tube device blank of predetermined shape so that it forms one;
The carbon nano tube device blank is heat-treated to a preset temperature, make carbon nano tube line maintain this predetermined shape, and then obtain a carbon nano tube device.
With respect to prior art, described method for preparing carbon nano tube device, it has the carbon nano tube device blank of predetermined shape by adopting the auxiliary carbon nano tube line of a supplementary unit to form one, and this carbon nano tube device blank heat-treated to a preset temperature, so that carbon nano tube line maintains this predetermined shape, and then can realize having the making of the carbon nano tube device of predetermined shape.
[description of drawings]
Fig. 1 is that to utilize supplementary unit be the synoptic diagram of a carbon nanotube spring blank with the carbon nanotube assist formation to first embodiment of the invention.
Fig. 2 is that to utilize supplementary unit be the synoptic diagram of a thermal electron emission source blank with the carbon nanotube assist formation to second embodiment of the invention.
[embodiment]
Below in conjunction with accompanying drawing the embodiment of the invention is described in further detail.
The method for preparing carbon nano tube device that the embodiment of the invention provided mainly comprises following five steps:
(1) provides a carbon nano tube line.
At first, adopt the chemical Vapor deposition process growth one to surpass the in-line arrangement carbon nano pipe array.The method that present embodiment provides can disclose No. 02134760.3 referring to the China's Mainland patent application.The growth method of being somebody's turn to do super in-line arrangement carbon nano pipe array mainly comprises step: a smooth substrate (a) is provided, and this substrate can be selected p type or n type silicon base for use; (b) deposition one catalyst layer in this substrate, the material of this catalyst layer can be selected one of iron (Fe), cobalt (Co), nickel (Ni) or its alloy for use; (c) substrate that will deposit catalyst layer is carried out anneal with 300～400 degree celsius temperature in shielding gas, and the time is about 10h; (d) substrate that deposits catalyst layer after the anneal is heated to 500～700 degrees centigrade; feed the mixed gas of carbon source gas and shielding gas; control the flow velocity of this carbon source gas; the temperature head that makes catalyzer and environment is more than 50 ℃; control the velocity ratio of this mixed gas; make the dividing potential drop of carbon source gas be lower than 20%, reacted 530 minutes, carbon nano pipe array will grow from substrate.Wherein, carbon source gas is hydrocarbon polymer, can be acetylene, ethane etc., preferably uses acetylene, and this shielding gas is rare gas element or nitrogen.Carbon nanotube in the super in-line arrangement carbon nano pipe array that is obtained by method for preparing is the pencil dense arrangement, has very high surface density, and have very strong Van der Waals force between the carbon nano-tube bundle, its not only diameter distribute relatively concentrate and also diameter much at one.
Then, adopt a stretching tool to extract a carbon nano tube line from this super in-line arrangement carbon nano pipe array.It can be operated by the following method: (a) the selected one carbon nano-tube bundle fragment that comprises a plurality of carbon nano-tube bundles from super in-line arrangement carbon nano pipe array; (b) use stretching tool, as tweezers, this carbon nano-tube bundle fragment that stretches makes carbon nano tube line form along draw direction.In described drawing process, the carbon nano-tube bundle fragment is in the elongation of the effect lower edge of pulling force direction of pull, and carbon nano-tube bundle fragment two ends will interconnect owing to the effect of Van der Waals force, thereby form a successive carbon nano tube line.
(2) carbon nano tube line is immersed in the volatile organic solvent so that it is carried out surface treatment.Because carbon nano tube line is to be made of the carbon nano-tube bundle that has bigger surface volume ratio in a large number, so its viscosity is bigger, after it is immersed volatile organic solvent and handle, under the capillary effect of volatile organic solvent, the surface volume ratio of carbon nano tube line, diameter all can diminish, and then can eliminate its viscosity, and it will have physical strength and toughness preferably.This step can be carried out with following method: (a) carbon nano tube line that extracts is fully immersed in the volatile organic solvent; (b) again carbon nano tube line is taken out from volatile organic solvent, then it is rolled collection with instruments such as bobbins.Described volatile organic solvent can be selected ethanol, methyl alcohol, acetone, ethylene dichloride or chloroform etc. for use.
(3) adopt a supplementary unit, the auxiliary carbon nano tube line of having handled well is shaped, and has the carbon nano tube device blank of predetermined shape so that it forms one.Can be in this assist formation process by supplementary unit, with the carbon nano tube line of having handled well, look real needs and form one and have the carbon nano tube device blank of predetermined shape.
See also Fig. 1, first embodiment of the invention, a carbon nanotube spring is made in expection, and the carbon nano tube line 10 after volatile organic solvent can being handled twines and be fixed on one and is on the white stone rod 20 of cylindrical shape, and it is one predetermined spiral-shaped that this carbon nano tube line 10 is formed.
See also Fig. 2, among another embodiment, a thermal electron emission source is made in expection, and the carbon nano tube line 10 ' after volatile organic solvent can being handled bends and is fixed on this white stone rod 20 ' along a white stone rod 20 ' that is prism shape, makes this carbon nano tube line 10 ' form a predetermined V-arrangement.
(4) the carbon nano tube device blank is heat-treated to a preset temperature, make carbon nano tube line maintain this predetermined shape, and then obtain a carbon nano tube device.Described preset temperature can be 600～2000 degrees centigrade, and preferred, this preset temperature is 1600～1700 degrees centigrade.This heat treatment process is to described because Van der Waals force.The carbon nano-tube bundle fragment two ends that act on and interconnect can be played a welding effect, and be made it maintain predetermined shape.Described heat treatment process can adopt and pass to heating current or the heat dual mode carries out:
(a), feed a heating current can directly for the carbon nano tube line 10 of assist formation, and keep for some time for passing to the heating current mode.The big I of this heating current is decided according to the diameter of carbon nano tube line 10, and it should guarantee to make the temperature of carbon nano tube line 10 to reach described preset temperature.In passing to the process that heating current heat-treats, if the overlong time that thermal treatment is kept then can cause the increase of carbon nano tube line self-defect and the loss of carbon, so this time of keeping is good to be no more than 4 hours.
(b) for the heat mode, the carbon nano tube line 10 of assist formation can be inserted the hot environment with a preset temperature, in graphite furnace, and to keep for some time, described holding time decided according to the height of temperature.For example under about 2000 degrees centigrade preset temperature, heat-treat, keep and got final product in about 0.5～1 hour, if lengthening is held time, the carbon that graphite furnace itself contains not only can be avoided the loss of carbon in the carbon nano tube line in the heat treatment process, also can remedy the defective of carbon nano tube line self, so can not do particular requirement to this upper limit of holding time.
In addition, above-mentioned heat treated two kinds of methods also can be used in combination, and pass to heating current to it when the carbon nano tube line 10 of assist formation is inserted hot environment, to realize the thermal treatment to carbon nano tube line 10.
First embodiment of the invention adopts the mode that passes to electric current, and the carbon nano tube line 10 that is wrapped on the white stone rod 20 is passed to heating current, makes its temperature be maintained at about 1600 degrees centigrade, and keeps 3～4 hours.After the thermal treatment, white stone rod 20 is removed, can be obtained a carbon nanotube spring.This carbon nanotube spring can keep certain elasticity, can be used for measuring very little quality.
Second embodiment of the invention, the same mode that passes to electric current that adopts, the carbon nano tube line 10 ' that will be fixed on the white stone rod 20 ' passes to heating current, makes its temperature be maintained at about 1600 degrees centigrade, and keeps 3～4 hours.After the thermal treatment, white stone rod 20 ' is removed, can be obtained a V-arrangement carbon nano tube device.This carbon nano tube device can be used as the thermal electron emission source of momentum of electron spectrometer.
The method for preparing carbon nano tube device that the embodiment of the invention provided, it is by adopting a supplementary unit, auxiliary carbon nano tube line forms one and has the carbon nano tube device blank of predetermined shape, and this carbon nano tube device blank heat-treated to a preset temperature, so that carbon nano tube line maintains this predetermined shape, and then can realize having the making of the carbon nano tube device of predetermined shape.
In addition, those skilled in the art also can do other variation in spirit of the present invention, as suitable change heat treatment period and temperature etc., as long as it does not depart from technique effect of the present invention and all can.The variation that these are done according to spirit of the present invention all should be included within the present invention's scope required for protection.
Claims (10)
1. method for preparing carbon nano tube device comprises step:
One carbon nano tube line is provided;
Carbon nano tube line is immersed in the volatile organic solvent so that it is carried out surface treatment;
Adopt a supplementary unit, the auxiliary carbon nano tube line of having handled well is shaped, and has the carbon nano tube device blank of predetermined shape so that it forms one;
The carbon nano tube device blank is heat-treated to a preset temperature, make carbon nano tube line maintain this predetermined shape, and then obtain a carbon nano tube device.
2. method for preparing carbon nano tube device as claimed in claim 1 is characterized in that the making method of described carbon nano tube line may further comprise the steps: adopt the chemical Vapor deposition process growth one to surpass the in-line arrangement carbon nano pipe array;
Adopt a stretching tool to extract a carbon nano tube line from this super in-line arrangement carbon nano pipe array.
3. method for preparing carbon nano tube device as claimed in claim 2 is characterized in that described stretching tool is tweezers.
4. method for preparing carbon nano tube device as claimed in claim 1 is characterized in that described volatile organic solvent is selected from ethanol, methyl alcohol, acetone, ethylene dichloride and chloroform.
5. method for preparing carbon nano tube device as claimed in claim 1 is characterized in that described thermal treatment comprises step: place a vacuum high-temperature environment to heat the carbon nano tube line of assist formation.
6. method for preparing carbon nano tube device as claimed in claim 5 is characterized in that described hot environment is a graphite furnace.
7. method for preparing carbon nano tube device as claimed in claim 1 is characterized in that described thermal treatment comprises step: feed a heating current for the carbon nano tube line of assist formation.
8. method for preparing carbon nano tube device as claimed in claim 7 is characterized in that described heat treatment period no more than 4 hours.
9. as each described method for preparing carbon nano tube device of claim 1 to 8, it is characterized in that described preset temperature is 600～2000 degrees centigrade.
10. method for preparing carbon nano tube device as claimed in claim 9 is characterized in that described preset temperature is 1600～1700 degrees centigrade.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101023232A CN100436312C (en) | 2005-12-06 | 2005-12-06 | Method for preparing carbon nano tube device |
| US11/309,744 US8246874B2 (en) | 2005-12-02 | 2006-09-21 | Method for making carbon nanotube-based device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101023232A CN100436312C (en) | 2005-12-06 | 2005-12-06 | Method for preparing carbon nano tube device |
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| CN1978316A CN1978316A (en) | 2007-06-13 |
| CN100436312C true CN100436312C (en) | 2008-11-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101376497B (en) * | 2007-08-31 | 2011-06-22 | 清华大学 | Carbon nano-tube composite material precast member and preparation thereof |
| CN102372251B (en) | 2010-08-23 | 2014-03-26 | 清华大学 | Carbon nanotube structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483667A (en) * | 2002-09-16 | 2004-03-24 | �廪��ѧ | Carbon nano pipe rpoe and preparation method thereof |
| US6784779B2 (en) * | 2000-07-08 | 2004-08-31 | Lg Electronics, Inc. | Inductor employing carbon nanotube and/or carbon nanofiber |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6784779B2 (en) * | 2000-07-08 | 2004-08-31 | Lg Electronics, Inc. | Inductor employing carbon nanotube and/or carbon nanofiber |
| CN1483667A (en) * | 2002-09-16 | 2004-03-24 | �廪��ѧ | Carbon nano pipe rpoe and preparation method thereof |
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