US20090263310A1 - Method for making carbon nanotubes - Google Patents
Method for making carbon nanotubes Download PDFInfo
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- US20090263310A1 US20090263310A1 US12/384,979 US38497909A US2009263310A1 US 20090263310 A1 US20090263310 A1 US 20090263310A1 US 38497909 A US38497909 A US 38497909A US 2009263310 A1 US2009263310 A1 US 2009263310A1
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- metal substrate
- carbon nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Definitions
- the present disclosure relates to methods for making carbon nanotubes and, particularly, to a method for making carbon nanotubes on a metal substrate.
- Carbon nanotubes are a novel carbonaceous material discovered by Iijima, a researcher of NEC Corporation, in 1991.
- carbon nanotubes have tube-shaped structures with small diameters (less than 100 nanometers) and large aspect ratios (length/diameter). They have excellent electrical properties as well as excellent mechanical properties.
- the electronic conductance of carbon nanotubes is related to their structures. Because the carbon nanotubes can transmit extremely high electrical current and emit electrons easily, at less than 100 volts, they are considered to be promising for use in a variety of electrical devices.
- a number of electronic devices such as field emission devices, traveling-wave tubes or electron guns, employ the carbon nanotubes as electron emitters.
- a substrate for supporting carbon nanotubes should have an ability to endure large amounts of electrical current to pass through. Therefore, it is understood that a substrate made of metal with high conductivity is considered to be a good option for use.
- CVD chemical vapor deposition
- metal catalysts such as transition metal or transition metal complex
- a carbon source gas is thermally decomposed at a predetermined temperature in the presence of the metal catalyst, thereby forming the carbon nanotubes.
- transition metal is used as a catalyst and coated on the metal substrate, it is easy for the transition metal reacting on the metal of the metal substrate to form an alloy. Thus, the transition metal has become an inactive catalyst, and the catalytic reaction for growing carbon nanotubes will be affected. What is needed, therefore, is to provide a method for making carbon nanotubes, which is able to be performed easily on a metal substrate and is suitable to be employed in mass production.
- FIG. 1 is a flowchart of a method for making carbon nanotubes, in accordance with a present embodiment.
- FIG. 2 is a scanning electron microscope (SEM) image of carbon nanotubes formed using the method in accordance with the present embodiment.
- FIG. 3 is a transmission electron microscopy (TEM) image of carbon nanotubes formed using the method in accordance with the present embodiment.
- TEM transmission electron microscopy
- a method for making carbon nanotubes includes the following steps:
- the metal substrate is a copper substrate.
- the metal substrate can vary in shape and thickness according to practical requirements.
- the metal substrate can be a solid rectangular piece.
- a thickness of the metal substrate can be in a range of about 0.5 centimeters (cm) to about 5 centimeters.
- An area of the metal substrate can be in a range of about 4 cm 2 to 100 cm 2 .
- Step 2 polishing a surface of the metal substrate, S 2 , is detailed below.
- the surface of the metal substrate is rubbed along a first direction with an abrasive paper for about 3-5 minutes.
- the abrasive paper is about 600-800 grit.
- powder generated by the sanding during the polishing process is removed by an application of air flow, e.g. blowing.
- the treated surface of the metal substrate is then rubbed along a second direction with an abrasive paper for about 5-8 minutes.
- the abrasive paper employed in such step is about 1000-1300 grit. The powder generated due to sanding in this step is also removed.
- the surface of the metal substrate is rubbed along the first direction with an abrasive paper for about 10-15 minutes.
- the abrasive paper is about 1500-2000 grit.
- powder generated by this is removed.
- An angle ⁇ between the first direction and the second direction is in a range of 0° ⁇ 90°. Particularly, in the present embodiment, the angle ⁇ is about 90°.
- the surface of the metal substrate is substantially flat and smooth by way of the polishing in step 2 that will facilitate the growth of the carbon nanotubes on the metal substrate.
- the notches or fine grooves are formed on a nanometer scale and in a net-like pattern due to repeatedly rubbing steps.
- Step 3 putting the polished metal substrate into a reaction device, S 3 .
- the reaction device is a furnace, e.g. a box furnace or a tube furnace.
- the polished metal substrate is put into a quartz boat, which is subsequently inserted into the center of the tube furnace.
- Step 4 introducing a first protecting gas while heating the environment inside of the reaction device, S 4 .
- the first protecting gas can be nitrogen.
- the environment inside of the reaction device is heated to about 400-800 degrees (C).
- the environment inside of the reaction device is heated to about 700 C.
- a plurality of metal particles e.g. copper particles, forms around the notches or fine grooves formed on the surface of the metal substrate, and can serve as seeds for facilitating the growth of carbon nanotubes.
- diameters of the metal particles range from about 1-10 nanometers (nm).
- the density of the metal particles is closely related to the number of times of rubbing and the angle of the rubbing directions between different rubbing steps. It is understood that the higher density of metal particles is obtained by the greater number of times of rubbing and the smaller angle of rubbing directions between different rubbing steps.
- Step 5 introducing a mixture of a carbon source gas and a second protecting gas, S 5 .
- the carbon source gas can be hydrocarbon, such as acetylene or ethylene while the protecting gas can be inert gas or nitrogen.
- acetylene is chosen as the carbon source gas by virtue of its low decomposition temperature and nitrogen is used as the second protecting gas.
- the first protecting gas and the second protecting gas can be the same gas.
- S 5 once the mixture of carbon source gas and second protecting gas is introduced into the reaction device, the carbon nanotubes are grown in a temperature range from about 400-800 C for about 5-30 minutes. The reaction device is then cooled down and the metal substrate is taken out from the reaction device.
- the carbon nanotubes fabricated by the method, in accordance with the present embodiment are disorderly arranged on the metal substrate.
- One end of each carbon nanotube is connected with the surface of the metal substrate.
- a diameter of each carbon nanotube is in a range from about 5 nm to 20 nm.
- the carbon nanotubes fabricated by the method of the present embodiment can be directly formed on the metal substrate. There is no need to coat a catalyst layer on the metal substrate in advance for growth of the carbon nanotubes. Therefore, the manufacturing procedure is simplified and the manufacturing cost is decreased that is suitable for mass production.
Abstract
Description
- 1. Technical Field
- The present disclosure relates to methods for making carbon nanotubes and, particularly, to a method for making carbon nanotubes on a metal substrate.
- 2. Discussion of Related Art
- Carbon nanotubes (CNTs) are a novel carbonaceous material discovered by Iijima, a researcher of NEC Corporation, in 1991. Typically, carbon nanotubes have tube-shaped structures with small diameters (less than 100 nanometers) and large aspect ratios (length/diameter). They have excellent electrical properties as well as excellent mechanical properties. The electronic conductance of carbon nanotubes is related to their structures. Because the carbon nanotubes can transmit extremely high electrical current and emit electrons easily, at less than 100 volts, they are considered to be promising for use in a variety of electrical devices.
- Generally, a number of electronic devices, such as field emission devices, traveling-wave tubes or electron guns, employ the carbon nanotubes as electron emitters. In order to achieve high power requirements, a substrate for supporting carbon nanotubes should have an ability to endure large amounts of electrical current to pass through. Therefore, it is understood that a substrate made of metal with high conductivity is considered to be a good option for use.
- Currently, a method of chemical vapor deposition (CVD) is mainly adopted for forming the carbon nanotubes on the substrate. CVD is performed by coating metal catalysts, such as transition metal or transition metal complex, on the substrate and directly synthesizing the carbon nanotubes on the substrate. In principle, a carbon source gas is thermally decomposed at a predetermined temperature in the presence of the metal catalyst, thereby forming the carbon nanotubes.
- However, once the transition metal is used as a catalyst and coated on the metal substrate, it is easy for the transition metal reacting on the metal of the metal substrate to form an alloy. Thus, the transition metal has become an inactive catalyst, and the catalytic reaction for growing carbon nanotubes will be affected. What is needed, therefore, is to provide a method for making carbon nanotubes, which is able to be performed easily on a metal substrate and is suitable to be employed in mass production.
- Many aspects of the present method for making carbon nanotubes can be better understood with reference to the following drawings. The components in the drawings are not necessarily to scale, the emphasis instead being placed upon clearly illustrating the principles of the present method for making carbon nanotubes.
-
FIG. 1 is a flowchart of a method for making carbon nanotubes, in accordance with a present embodiment. -
FIG. 2 is a scanning electron microscope (SEM) image of carbon nanotubes formed using the method in accordance with the present embodiment. -
FIG. 3 is a transmission electron microscopy (TEM) image of carbon nanotubes formed using the method in accordance with the present embodiment. - Corresponding reference characters indicate corresponding parts throughout the several views. The exemplifications set out herein illustrate at least one embodiment of the present method for making carbon nanotubes, in at least one form, and such exemplifications are not to be construed as limiting the scope of the disclosure in any manner.
- Reference will now be made to the drawings to describe, in detail, embodiments of the present method for making carbon nanotubes. Referring to
FIG. 1 , a method for making carbon nanotubes, according to a present embodiment, includes the following steps: - Step 1, providing a metal substrate, S1. In the present embodiment, the metal substrate is a copper substrate. The metal substrate can vary in shape and thickness according to practical requirements. For example, the metal substrate can be a solid rectangular piece. A thickness of the metal substrate can be in a range of about 0.5 centimeters (cm) to about 5 centimeters. An area of the metal substrate can be in a range of about 4 cm2 to 100 cm2.
- Step 2, polishing a surface of the metal substrate, S2, is detailed below. In the present embodiment, the surface of the metal substrate is rubbed along a first direction with an abrasive paper for about 3-5 minutes. The abrasive paper is about 600-800 grit. After that, powder generated by the sanding during the polishing process is removed by an application of air flow, e.g. blowing. The treated surface of the metal substrate is then rubbed along a second direction with an abrasive paper for about 5-8 minutes. The abrasive paper employed in such step is about 1000-1300 grit. The powder generated due to sanding in this step is also removed. After rubbing the surface of the metal substrate along the second direction, the surface of the metal substrate is rubbed along the first direction with an abrasive paper for about 10-15 minutes. In this case, the abrasive paper is about 1500-2000 grit. Finally, powder generated by this is removed. An angle α between the first direction and the second direction is in a range of 0°<α≦90°. Particularly, in the present embodiment, the angle α is about 90°.
- As a result, the surface of the metal substrate is substantially flat and smooth by way of the polishing in step 2 that will facilitate the growth of the carbon nanotubes on the metal substrate. However, it is understood that there are micro variations in the form of notches or fine grooves that can be observed on the surface of the metal substrate. Particularly, such the notches or fine grooves are formed on a nanometer scale and in a net-like pattern due to repeatedly rubbing steps.
- Step 3, putting the polished metal substrate into a reaction device, S3. In the present embodiment, the reaction device is a furnace, e.g. a box furnace or a tube furnace. Particularly, the polished metal substrate is put into a quartz boat, which is subsequently inserted into the center of the tube furnace.
- Step 4, introducing a first protecting gas while heating the environment inside of the reaction device, S4. The first protecting gas can be nitrogen. In the present embodiment, the environment inside of the reaction device is heated to about 400-800 degrees (C). For example, the environment inside of the reaction device is heated to about 700 C. In step 4, during the heating process, a plurality of metal particles, e.g. copper particles, forms around the notches or fine grooves formed on the surface of the metal substrate, and can serve as seeds for facilitating the growth of carbon nanotubes. In the present embodiment, diameters of the metal particles range from about 1-10 nanometers (nm). In addition, the density of the metal particles is closely related to the number of times of rubbing and the angle of the rubbing directions between different rubbing steps. It is understood that the higher density of metal particles is obtained by the greater number of times of rubbing and the smaller angle of rubbing directions between different rubbing steps.
-
Step 5, introducing a mixture of a carbon source gas and a second protecting gas, S5. In the present embodiment, the carbon source gas can be hydrocarbon, such as acetylene or ethylene while the protecting gas can be inert gas or nitrogen. Particularly, acetylene is chosen as the carbon source gas by virtue of its low decomposition temperature and nitrogen is used as the second protecting gas. In addition, the first protecting gas and the second protecting gas can be the same gas. Instep 5, S5, once the mixture of carbon source gas and second protecting gas is introduced into the reaction device, the carbon nanotubes are grown in a temperature range from about 400-800 C for about 5-30 minutes. The reaction device is then cooled down and the metal substrate is taken out from the reaction device. - Referring to
FIG. 2 andFIG. 3 , the carbon nanotubes fabricated by the method, in accordance with the present embodiment, are disorderly arranged on the metal substrate. One end of each carbon nanotube is connected with the surface of the metal substrate. In addition, a diameter of each carbon nanotube is in a range from about 5 nm to 20 nm. - In conclusion, the carbon nanotubes fabricated by the method of the present embodiment can be directly formed on the metal substrate. There is no need to coat a catalyst layer on the metal substrate in advance for growth of the carbon nanotubes. Therefore, the manufacturing procedure is simplified and the manufacturing cost is decreased that is suitable for mass production.
- Finally, it is to be understood that the above-described embodiments are intended to illustrate rather than limit the invention. Variations may be made to the embodiments without departing from the spirit of the invention as claimed. The above-described embodiments illustrate the scope of the invention but do not restrict the scope of the invention.
- It is also to be understood that above description and the claims drawn to a method may include some indication in reference to certain steps. However, the indication used is only to be viewed for identification purposes and not as a suggestion as to an order for the steps.
Claims (15)
Applications Claiming Priority (2)
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CN200810066744.8 | 2008-04-18 | ||
CN2008100667448A CN101559939B (en) | 2008-04-18 | 2008-04-18 | Preparation method of carbon nano tube |
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US12/384,979 Abandoned US20090263310A1 (en) | 2008-04-18 | 2009-04-09 | Method for making carbon nanotubes |
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JP (1) | JP5038349B2 (en) |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110189394A1 (en) * | 2008-10-29 | 2011-08-04 | Suguru Noda | Method for forming carbon nanotube |
US20130234025A1 (en) * | 2010-09-17 | 2013-09-12 | Centre National De La Recherche Scientifique (Cnrs) | Electron gun emitting under high voltage, in particular for electron microscopy |
US20150068001A1 (en) * | 2009-12-21 | 2015-03-12 | 4Wind Science And Engineering, Llc | High performance carbon nanotube energy storage device |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5374354B2 (en) * | 2009-12-25 | 2013-12-25 | 日東電工株式会社 | Carbon nanotube composite structure and adhesive member |
CN102324335B (en) * | 2011-06-07 | 2013-10-23 | 天津工业大学 | Method for preparing compound electrical contact material |
CN104637758B (en) * | 2014-12-11 | 2017-08-29 | 温州大学 | The method of direct growth carbon nanotube field emission cathode in nickeliferous metallic substrates |
CN110240145B (en) * | 2019-07-03 | 2021-05-28 | 西安交通大学 | Transition layer-support-free metal-based array carbon nanotube electrode material and preparation method and application thereof |
CN110697686B (en) * | 2019-09-17 | 2021-06-22 | 北京化工大学 | Method for preparing carbon nano tube by heating powder |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US20060234056A1 (en) * | 2005-04-14 | 2006-10-19 | Tsinghua University | Thermal interface material and method for making the same |
US7288321B2 (en) * | 2002-11-21 | 2007-10-30 | Tsinghua University | Carbon nanotube array and method for forming same |
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KR20010074667A (en) * | 1998-06-19 | 2001-08-08 | 추후보정 | Free-standing and aligned carbon nanotubes and synthesis thereof |
JP2001048512A (en) * | 1999-08-04 | 2001-02-20 | Ulvac Japan Ltd | Preparation of perpendicularly oriented carbon nanotube |
CN1174918C (en) * | 2001-09-05 | 2004-11-10 | 武汉大学 | Nanometer carbon pipe preparing process |
JP2005001936A (en) * | 2003-06-11 | 2005-01-06 | Fujikura Ltd | Method of manufacturing carbon nanotube |
JP5049474B2 (en) * | 2005-08-22 | 2012-10-17 | 株式会社アルバック | Method for producing graphite nanofiber |
-
2008
- 2008-04-18 CN CN2008100667448A patent/CN101559939B/en active Active
-
2009
- 2009-04-09 US US12/384,979 patent/US20090263310A1/en not_active Abandoned
- 2009-04-17 JP JP2009101371A patent/JP5038349B2/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7288321B2 (en) * | 2002-11-21 | 2007-10-30 | Tsinghua University | Carbon nanotube array and method for forming same |
US20060234056A1 (en) * | 2005-04-14 | 2006-10-19 | Tsinghua University | Thermal interface material and method for making the same |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20110189394A1 (en) * | 2008-10-29 | 2011-08-04 | Suguru Noda | Method for forming carbon nanotube |
US8435601B2 (en) * | 2008-10-29 | 2013-05-07 | University Of Tokyo | Method for forming carbon nanotube |
US20150068001A1 (en) * | 2009-12-21 | 2015-03-12 | 4Wind Science And Engineering, Llc | High performance carbon nanotube energy storage device |
US20130234025A1 (en) * | 2010-09-17 | 2013-09-12 | Centre National De La Recherche Scientifique (Cnrs) | Electron gun emitting under high voltage, in particular for electron microscopy |
US9048057B2 (en) * | 2010-09-17 | 2015-06-02 | Centre National De La Recherche Scientifique (Cnrs) | Electron gun emitting under high voltage, in particular for electron microscopy |
Also Published As
Publication number | Publication date |
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JP5038349B2 (en) | 2012-10-03 |
CN101559939B (en) | 2011-05-04 |
JP2009256204A (en) | 2009-11-05 |
CN101559939A (en) | 2009-10-21 |
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Owner name: TSINGHUA UNIVERSITY, CHINA Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:DAI, FENG-WEI;YAO, YUAN;CHANG, CHANG-SHEN;AND OTHERS;REEL/FRAME:022589/0604 Effective date: 20090331 Owner name: HON HAI PRECISION INDUSTRY CO., LTD, TAIWAN Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:DAI, FENG-WEI;YAO, YUAN;CHANG, CHANG-SHEN;AND OTHERS;REEL/FRAME:022589/0604 Effective date: 20090331 |
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