CN100374369C - Method of treating carbon nano tube using electric arc discharging - Google Patents
Method of treating carbon nano tube using electric arc discharging Download PDFInfo
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- CN100374369C CN100374369C CNB2006100147800A CN200610014780A CN100374369C CN 100374369 C CN100374369 C CN 100374369C CN B2006100147800 A CNB2006100147800 A CN B2006100147800A CN 200610014780 A CN200610014780 A CN 200610014780A CN 100374369 C CN100374369 C CN 100374369C
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Abstract
The present invention discloses a method for treating carbon nano tube by utilizing electric arc discharge, belonging to the field of carbon nano tube purification and directional arrangement technology. Said method includes the following steps: directly applying voltage and current to carbon nano tube, making electric spark treatment, removing metal or oxide catalyst attached to the surface of carbon nano tube and stripping deposited amorphous carbon layer, at the same time cutting and directionally arranging carbon nano tube.
Description
Technical field
The present invention relates to a kind of method, belong to the technology of carbon nanotube purifying and ordered arrangement with arc-over processing carbon nanotube.
Background technology
Because carbon nanotube has the potential superstrength, high tenacity, high conduction, high heat conduction, semi-conductor, air-sensitive, temperature-sensitive, numerous good unusual structures and physics-chem characteristics such as electromechanical reaction, and application prospects make the preparation of carbon nanotube and purifying seem extremely important.Synthetic main three kinds of methods of carbon nanotube: arc discharge method, laser evaporation method and catalystic pyrolysis, the carbon nanotube of different methods preparation all can contain identical impurity such as amorphous carbon, and main employing is that catalystic pyrolysis prepares carbon nanotube at present.Impurities is mainly metal and decolorizing carbon and graphite-like fragment in the carbon nanotube of catalystic pyrolysis preparation.The wide application prospect of carbon nanotube needs the carbon nanotube of high-purity carbon nanotube, particularly high-purity single wall, but still lacks a kind of ideal purification technique up to now.At present general by the acid oxidase method, carbon nanotube that will be impure immerses in the strong acid solution and dissolves away metallic impurity, by process separated products such as filtration, cleaning, centrifugal, dryings to reach the purpose of purifying carbon nano-tube.Yet by the destruction that the pickling oxidative pathway can cause carbon nanotube structure, this is because the heat of amorphous carbon and carbon nanotube is close with oxidation structure stability, in the time of by the oxidation amorphous carbon, is difficult to the not oxidized or structure deteriorate of controlling carbon nanotube.In addition, the macroscopic carbon nanotube fiber handled it is aligned, it also is the problem that realizes the required solution of its numerous application that cutting waits.
Summary of the invention
The object of the present invention is to provide a kind of method with arc-over processing carbon nanotube, this method can effectively be removed the amorphous particle of carbon nanotube, and it is aligned, and its process is simple.
For achieving the above object, the present invention is realized by following technical proposals: to the carbon nano-tube fibre bundle, handle the method for this carbon nanotube with arc-over.It is characterized in that comprising following concrete steps:
In air or under inert atmosphere protection, the two ends of carbon nano-tube bundle are directly applied 10~100 volts direct current or voltage of alternating current; make it to produce electrical spark in moment; remove the adhesion metal or the oxide catalyst of carbon nano tube surface and peel off sedimentary amorphous carbon layer, and realize the cutting with its two ends of aligning of carbon nanotube.
The carbon nanotube that ins all sorts of ways at present and prepare, all containing small granules of catalyst and amorphous carbon is deposited on the carbon tube wall, granules of catalyst all is nano-grade size and combines closely on the carbon tube wall with Fan Dehuali that sedimentary decolorizing carbon then is to cover the carbon tube-surface with chemical bond.Be difficult to remove fully with general method.On carbon nanotube, apply an instantaneous voltage, can produce two kinds of purifying mechanism: the one, can make the carbon pipe produce local high electric current and high calorie, the particle of nano-scale produces migration and is gathered into bigger microscopic particles, thereby is of value to its removal; The 2nd, have the resistance higher owing to cover the amorphous carbon on surface than carbon nanotube, and their different thermal expansivity, thereby producing a large amount of heat, peels away on the amorphous carbon surface layer with carbon nanotube.If handle in air, amorphous carbon will be peeled off from carbon nano tube surface.Thereby can well carry out purifying to carbon nanotube.
When the two ends at carbon nano-tube bundle apply a high transient voltage, make its discharge, local produces a large amount of heat and is burnt in the contact, thereby realizes the cutting to carbon nano-tube fibre bundle two ends.
Apply voltage in a flash to carbon nanotube, produce two kinds and arrange mechanism: the one, make carbon nanotube produce momentary current, thereby produce magnetic effect, give the process of a rearrangement of carbon nanotube, it is aligned; The 2nd, owing to be point of contact with the ring-type between the carbon nanotube, this point of contact is in high resistance state, produces high calorie and it is twined assemble catalyst sites and peel off under the voltage effect, thereby also can make the carbon nanotube marshalling.
The invention has the advantages that: can remove carbon nano tube surface fully and be deposited on the amorphous carbon and the metallic impurity of upper layer, thereby reach the purpose of purifying carbon nano-tube with physical adsorption or with the chemical bond combination; And the two ends of energy cutting carbon nanotubes, align neat.The carbon nanotube that the present invention also makes applicable to additive method carries out purifying and aligns and cut.
Description of drawings
Accompanying drawing 1: with the metallic iron is the undressed carbon nano-tube fibre bundle of catalyzer gas phase synthetic SEM photo.
The SEM photo that the carbon nano-tube bundle of accompanying drawing 2: Fig. 1 is handled through spark discharge.
Accompanying drawing 3: with the metallic iron is the natural end SEM photo of the undressed carbon nano-tube fibre bundle of catalyzer gas phase synthetic.
The carbon nanotube of accompanying drawing 4: Fig. 3 is through the fiber end SEM photo of discharge process cutting.
Accompanying drawing 5: with the metallic iron is carbon nanotube TEM photo before catalyzer gas phase synthetic is handled.The light color that presents among this figure shows in carbon nano tube surface and is depositing amorphous carbon layer.
Accompanying drawing 6: Fig. 5 handles the TEM photo of carbon nanotube through electrical spark.
Accompanying drawing 7: with the metallic iron is the pattern photo of catalyzer gas phase synthetic through the carbon nano-tube fibre bundle of electrical spark processing.
Embodiment
Embodiment one: will adopt (long 10 millimeters in metallic iron catalyzer gas phase synthetic carbon nanofiber bundle sample, thick 500 microns) insert in three mouthfuls of glass beakers, the negative pole of the direct supply side mouth by glass beaker is entered in the glass beaker a end in contact with the carbon nano-tube fibre bundle, the sealing of oral area plug, positive source enters in the beaker by another inlet, the sealing of oral area plug is evacuated to 10 by top opening to beaker
-3Torr charges into an atmospheric high-purity argon gas then, airtight top inlet mouth.Voltage of supply is transferred to 24 volts, the of short duration contact of the other end in the beaker outside with the fiber in anode electrode and the beaker, 0.1 millisecond of time, can see the point of contact place in the beaker outside has electrical spark to emit.The sample of discharge process by scanning electron microscope and transmission electron microscope observing, can be seen that amorphous carbon and the iron catalyst impurity on the carbon pipe is eliminated in the fibrous bundle, form the particle of tens nanometers, the carbon pipe in the fibrous bundle is purified, and it is regular that phase transformation is got in the arrangement between the carbon pipe.As shown in Figure 2.
Embodiment two: will adopt laser evaporation synthetic Single Walled Carbon Nanotube fibrous bundle, thick 1 millimeter, long 2 centimetre of one end is connected in the negative pole of direct supply, voltage is transferred 24 volts, another electrode is put the other end that touches fibrous bundle fast, leave, can be observed electrical spark at the place, contact and emitted.Whole process is carried out in air.Carbon nano-tube fibre sampling to discharge process is put on the transmission electron microscope copper mesh and observes, and the end of visible fiber point spark discharge is cut.As shown in Figure 4.
Embodiment three: will adopt arc-over synthetic non-crystal carbon nano tube floss, volume 5mm * 5mm * 5mm, an end be connected in the utmost point of direct supply, voltage is transferred 24 volts, another electrode is put the opposite side that touches the non-crystal carbon nano tube floss fast, can be observed electrical spark at the place, contact and emitted.Whole process is carried out in air.Carbon nanotube floss sampling to discharge process is put on scanning electron microscope and the transmission electron microscope copper mesh and observes, and the amorphous layer on visible original non-crystal carbon nano tube surface is stripped from, and forms the carbon nanotube bundles of cleaning surfaces.Amorphous layer originally is transformed into the particle that diameter is 20nm.As shown in Figure 6.
Embodiment four: will adopt metallic iron catalyzer gas phase synthetic carbon nano-tube fibre bundle, thick 1 millimeter, long 2 centimetre of one end is connected in the negative pole of direct supply, adopt AC power, voltage transfers to 50 volts, another is extremely fast put the other end that touches fibrous bundle, leave, can be observed electrical spark at the place, contact and emitted.Whole process is carried out in air.Carbon nano-tube fibre sampling to discharge process is put on the transmission electron microscope copper mesh and observes, and finds that carbon pipe oriented becomes neat in the fiber, and carbon tube-surface amorphous carbon is removed.
Claims (1)
1. method of handling carbon nanotube with arc-over; this method is at the carbon nano-tube fibre bundle; it is characterized in that comprising following concrete steps: in air or under inert atmosphere protection, the two ends of carbon nano-tube bundle are directly applied 10~100 volts direct current or voltage of alternating current; make it to produce electrical spark in moment; remove the adhesion metal or the oxide catalyst of carbon nano tube surface and peel off sedimentary amorphous carbon layer, and realize the cutting with its two ends of aligning of carbon nanotube.
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CNB2006100147800A CN100374369C (en) | 2006-07-17 | 2006-07-17 | Method of treating carbon nano tube using electric arc discharging |
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CNB2006100147800A CN100374369C (en) | 2006-07-17 | 2006-07-17 | Method of treating carbon nano tube using electric arc discharging |
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CN1903710A CN1903710A (en) | 2007-01-31 |
CN100374369C true CN100374369C (en) | 2008-03-12 |
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Families Citing this family (5)
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CN101746745A (en) * | 2008-12-04 | 2010-06-23 | 索尼株式会社 | Method for preparing and purifying carbon nano tubes, carbon nano tubes and carbon nano tube elements |
US10273599B2 (en) | 2015-07-24 | 2019-04-30 | Lg Chem, Ltd. | Apparatus for manufacturing carbon nanotube fiber |
CN105080409A (en) * | 2015-08-30 | 2015-11-25 | 青岛科技大学 | Dispersing method of carbon nanotube |
CN105080684A (en) * | 2015-09-10 | 2015-11-25 | 青岛科技大学 | Carbon nanotube dispersion device |
CN106120296B (en) * | 2016-06-21 | 2018-09-11 | 郑州大学 | A kind of carbon nano-tube fibre purification process |
Citations (4)
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JP2002308610A (en) * | 2001-04-06 | 2002-10-23 | Sony Corp | Method for purifying carbon nanotube |
CN1549280A (en) * | 2003-05-14 | 2004-11-24 | 中国科学院物理研究所 | Method for raising electrical property of nano-materials |
CN1554578A (en) * | 2003-12-19 | 2004-12-15 | 哈尔滨工业大学 | Method for preparing nano carbon tube needle tip |
EP1612187A1 (en) * | 2004-06-30 | 2006-01-04 | E.I. du Pont de Nemours and Company | Carbon nanotube microfibers |
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Patent Citations (4)
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JP2002308610A (en) * | 2001-04-06 | 2002-10-23 | Sony Corp | Method for purifying carbon nanotube |
CN1549280A (en) * | 2003-05-14 | 2004-11-24 | 中国科学院物理研究所 | Method for raising electrical property of nano-materials |
CN1554578A (en) * | 2003-12-19 | 2004-12-15 | 哈尔滨工业大学 | Method for preparing nano carbon tube needle tip |
EP1612187A1 (en) * | 2004-06-30 | 2006-01-04 | E.I. du Pont de Nemours and Company | Carbon nanotube microfibers |
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