CN1194889C - Process for preparing single wall nano carbon tube - Google Patents
Process for preparing single wall nano carbon tube Download PDFInfo
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- CN1194889C CN1194889C CNB021098050A CN02109805A CN1194889C CN 1194889 C CN1194889 C CN 1194889C CN B021098050 A CNB021098050 A CN B021098050A CN 02109805 A CN02109805 A CN 02109805A CN 1194889 C CN1194889 C CN 1194889C
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- carbon nanotube
- walled carbon
- single walled
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Abstract
The present invention relates to a method for preparing a nanometer carbon tube with a single wall, which has the technical scheme that the mode that the arc discharge is carried out on the cathode and the anode in the pressurized atmosphere, and the anode is a consumptive anode. The present invention is characterized in that the anode is formed by pressing carbon fibers; otherwise, the anode is a circular graphite disk provided with a drilled hole, and carbon fibers are filled in the hole. The present invention has the technical key that carbon fibers are used instead of graphite so as to greatly enhance the purity of the nanometer carbon tube with a single wall and reduce the manufacture cost of the nanometer carbon tube with a single wall.
Description
Technical field;
The present invention relates to the technology of preparing of CNT (carbon nano-tube), provide especially a kind of under pressure atmosphere the method for arc-over mass production Single Walled Carbon Nanotube.
Background technology:
CNT (carbon nano-tube) has caused various countries scholars' extensive concern and very big interest in worldwide since 1991 are found.Theoretical Calculation shows that CNT (carbon nano-tube) has high intensity and Young's modulus, is called as super fiber, can be used for the enhancing body of advanced composite materials; CNT (carbon nano-tube) has unique electronic band structure, is ideal One-dimensional Quantum lead; In addition, CNT (carbon nano-tube) also has potentiality as emtting electrode, absorbing material, hydrogen storage material etc.Exactly because have numerous excellent properties and wide application prospect, CNT (carbon nano-tube) has evoked the very big research enthusiasm of scientists.Preparing highly purified CNT (carbon nano-tube) in a large number is the prerequisite that it is carried out structure observation, performance test and further studies and use, so the preparation of CNT (carbon nano-tube) is most important.In recent years, the preparation of CNT (carbon nano-tube) is in the development and progress always.The synthetic technology of multiple-wall carbon nanotube is comparatively ripe, and can realize oriented growth, and the preparation method of Single Walled Carbon Nanotube mainly contains arc process, laser method and carbon compound catalytic decomposition method etc.Traditional arc process is in the reaction chamber that is filled with the certain pressure rare gas element, between two root graphite electrode rods, produce high temperature by the high frequency or the contact starting the arc, the evaporation Graphite Electrodes, atomic structure of carbon is reset under the effect of catalyzer simultaneously, to obtain Single Walled Carbon Nanotube.Japanese scholar Lijima in 1997 has obtained Single Walled Carbon Nanotube in this way first, but content is very low.1997, C.People such as Journet have obtained result preferably by the method for gaseous tension in transformation catalyst kind and the adjustment reactor.Its experiment condition is reaction atmosphere 660 torr helium; Negative electrode and anode are respectively graphite rods, are of a size of negative electrode φ 16 * 40mm, and anode φ 16 * 100mm is again at the middle deep hole that is drilled with φ a 3.5 * 40mm of anode bar, the mixture of filling catalyzer in the hole (yttrium, nickel) and Graphite Powder 99; Negative electrode and anode are vertically opposite, and its spacing is～3mm that the reaction times is～2 minutes.Obtain product following several form: a is arranged.Generating a large amount of rubber-like cigarettes on reaction chamber wall processs; B.Between negative electrode and wall, form reticulated structure; C.Form the column throw out in cathode end; D.The porous, the lightweight ring that around the column throw out, occur.It is minimum to contain Single Walled Carbon Nanotube during wherein gluey cigarette is processed, and the content of CNT (carbon nano-tube) is the highest in the ring.The present patent application people once disclosed a kind of hydrogen arc discharge means of a large amount of preparation Single Walled Carbon Nanotube, it is lower cost ground manufacture order wall carbon nanotube in large quantities semi-continuously, but still there is graphite carbon in the Single Walled Carbon Nanotube of being produced inevitably, for follow-up use makes troubles.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of Single Walled Carbon Nanotube, it can be semi-continuously, manufacture order wall carbon nanotube in large quantities, and have very high purity.
The invention provides a kind of preparation method of Single Walled Carbon Nanotube, adopt the mode of cathode and anode arc-over under pressure atmosphere, anode is a sacrificial anode, it is characterized in that: described anode is formed by the compacting of charcoal fiber; Perhaps described anode is a graphite disk, and the charcoal fiber is filled in boring on it in hole.
Among the preparation method of Single Walled Carbon Nanotube of the present invention, can contain catalyzer in the anode, one or more in catalyzer chosen from Fe, cobalt, nickel, the yttrium, add-on is 2.5～5.0% atoms.Can also sulfur-bearing or solid sulfate make growth stimulant, add-on is 0.5～1% atom.
Among the preparation method of Single Walled Carbon Nanotube of the present invention, reaction atmosphere is the hydrogen of 50～400 torrs.Can also add argon gas in the nitrogen atmosphere, add-on is no more than 20% volume.
Among the preparation method of Single Walled Carbon Nanotube of the present invention, preferably become 30～80 ° angle between negative electrode and anode.
Among the preparation method of Single Walled Carbon Nanotube of the present invention, described charcoal fiber is diameter multiple-wall carbon nanotube and other nano carbon material in one dimension greater than 50nm.
Key problem in technology of the present invention is to replace graphite with the charcoal fiber, can improve the purity of Single Walled Carbon Nanotube greatly, thereby reduces the manufacturing cost of Single Walled Carbon Nanotube.
Description of drawings:
The Raman spectrum of the Single Walled Carbon Nanotube that the hydrogeneous plasma arc method of Fig. 1 is prepared: (1) is the Single Walled Carbon Nanotube of feedstock production with the multiple-wall carbon nanotube; (2) with the Graphite Powder 99 be the prepared Single Walled Carbon Nanotube of raw material.
Embodiment:
Multiple-wall carbon nanotube is respectively charged into six holes and compacting on the anode graphite disk, charge into 200 torr hydrogen and 50 torr argon gas in the reactor, striking current is the 150A direct current, the distance of two interpolar maintenance～2mm and～30 ° of angles, in the 20 minutes reaction times of accumulative total, obtain 1 gram Single Walled Carbon Nanotube.Raman spectrum is seen accompanying drawing 1.
The powder mix of charcoal fiber, 4% catalyst atom cobalt and 1% atom growth stimulant sulphur is respectively charged into seven holes and compacting on the anode graphite disk, charge into 200 torr hydrogen and 50 torr argon gas in the reactor, striking current is the 150A direct current, the distance of two interpolar maintenance～2mm and～40 ° of angles, in the 23 minutes reaction times of accumulative total, obtain 1.1 gram Single Walled Carbon Nanotube.
Embodiment 3
The charcoal fiber is respectively charged into four holes and compacting on the anode graphite disk, charge into 200 torr hydrogen and 50 torr argon gas in the reactor, striking current is the 150A direct current, the distance of two interpolar maintenance～2mm and～30 ° of angles, in the 15 minutes reaction times of accumulative total, obtain 750 milligrams of Single Walled Carbon Nanotube.
Embodiment 4
The powder mix of nano carbon fiber and 4% catalyst atom iron is respectively charged into six holes and compacting on the anode graphite disk, charge into 200 torr hydrogen and 50 torr argon gas in the reactor, striking current is the 150A direct current, the distance of two interpolar maintenance～2mm and～40 ° of angles, in the 20 minutes reaction times of accumulative total, obtain 1 gram.
Embodiment 5
The powder mix of charcoal fiber and 5% catalyst atom iron is respectively charged into six holes and compacting on the anode graphite disk, charge into 200 torr hydrogen and 50 torr argon gas in the reactor, striking current is the 150A direct current, the distance of two interpolar maintenance～2mm and～40 ° of angles, in the 23 minutes reaction times of accumulative total, obtain 1.1 gram Single Walled Carbon Nanotube.
Claims (8)
1, a kind of preparation method of Single Walled Carbon Nanotube, the mode of employing cathode and anode arc-over under pressure atmosphere, anode is a sacrificial anode, it is characterized in that: described anode is formed by the compacting of charcoal fiber.
2, a kind of preparation method of Single Walled Carbon Nanotube, the mode of employing cathode and anode arc-over under pressure atmosphere, anode is a sacrificial anode, it is characterized in that: described anode is a graphite disk, the charcoal fiber is filled in boring on it in hole.
3, by the preparation method of claim 1 or 2 described Single Walled Carbon Nanotube, it is characterized in that: contain catalyzer in the described anode, one or more in catalyzer chosen from Fe, cobalt, nickel, the yttrium, add-on is 2.5～5.0% atoms.
4, by the preparation method of the described Single Walled Carbon Nanotube of claim 3, it is characterized in that: sulfur-bearing or solid sulfate are made growth stimulant in the described anode, and add-on is 0.5～1% atom.
5, by the preparation method of claim 1 or 2 described Single Walled Carbon Nanotube, it is characterized in that: reaction atmosphere is the hydrogen of 50～400 torrs.
6, by the preparation method of the described Single Walled Carbon Nanotube of claim 5, it is characterized in that: add argon gas in the nitrogen atmosphere, add-on is no more than 20% volume.
7, by the preparation method of claim 1 or 2 described Single Walled Carbon Nanotube, it is characterized in that: become 30～80 ° angle between negative electrode and anode.
8, by the preparation method of claim 1 or 2 described Single Walled Carbon Nanotube, it is characterized in that: described charcoal Fibre diameter is greater than 50nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021098050A CN1194889C (en) | 2002-06-06 | 2002-06-06 | Process for preparing single wall nano carbon tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021098050A CN1194889C (en) | 2002-06-06 | 2002-06-06 | Process for preparing single wall nano carbon tube |
Publications (2)
| Publication Number | Publication Date |
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| CN1463918A CN1463918A (en) | 2003-12-31 |
| CN1194889C true CN1194889C (en) | 2005-03-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021098050A Expired - Fee Related CN1194889C (en) | 2002-06-06 | 2002-06-06 | Process for preparing single wall nano carbon tube |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299980C (en) * | 2004-06-15 | 2007-02-14 | 南开大学 | Arc synthesis of single-wall carbon nanometer tubes |
| CN101234760B (en) * | 2007-01-29 | 2011-04-13 | 旗山材料科技股份有限公司 | Equipment and method for manufacturing nano carbon tube |
| CN101513997B (en) * | 2008-02-20 | 2011-04-20 | 中国科学院金属研究所 | Method for synthesizing nano cable structure of silica-coated single-walled carbon nano tube |
| CN101481788A (en) * | 2008-03-04 | 2009-07-15 | 浙江大学 | Preparation of single wall carbon nano-tube film |
| CN101992104B (en) * | 2010-09-21 | 2012-07-04 | 上海大学 | Method of preparing single-wall carbon nanotube loaded with noble metal nanoparticle |
| CN102530918B (en) * | 2012-01-09 | 2013-08-07 | 中国科学院金属研究所 | Method for preparing single/double walled carbon nano tube structure with small size of tube bundle |
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2002
- 2002-06-06 CN CNB021098050A patent/CN1194889C/en not_active Expired - Fee Related
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