US20040105807A1 - Method for manufacturing carbon nanotubes - Google Patents
Method for manufacturing carbon nanotubes Download PDFInfo
- Publication number
- US20040105807A1 US20040105807A1 US10/410,069 US41006903A US2004105807A1 US 20040105807 A1 US20040105807 A1 US 20040105807A1 US 41006903 A US41006903 A US 41006903A US 2004105807 A1 US2004105807 A1 US 2004105807A1
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- substrate
- carbon nanotubes
- catalyst material
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- array
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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
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1271—Alkanes or cycloalkanes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1271—Alkanes or cycloalkanes
- D01F9/1272—Methane
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1273—Alkenes, alkynes
- D01F9/1275—Acetylene
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/08—Aligned nanotubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/34—Length
Definitions
- the present invention relates to a method for manufacturing carbon nanotubes, and more particularly to a method for manufacturing carbon nanotubes having a predetermined same length.
- Carbon nanotubes have shown many unique electrical and mechanical properties. Their potential applications include use in field emitters, gas storage and separation, nanoprobes, chemical sensors and high strength composites.
- the carbon nanotubes made by arc discharge and laser ablation are often accompanied by a large volume (up to 50%) of contaminants and are tangled with each other. It is very difficult to separate the carbon nanotubes.
- those production techniques are capital-intensive and are likely limited to research quantities.
- the carbon nanotubes made using a chemical vapor deposition technique are in good yield—occasionally over 90%—and have few contaminants.
- Carbon nanotubes having a predetermined same length and being parallel to each other are generally desired in field emission devices, in composite reinforced material and in electrovacuum device. However, not all methods can directly produce carbon nanotubes having a predetermined same length and being parallel to each other.
- an object of the present invention is to provide a method for manufacturing carbon nanotubes that have a predetermined same length and that are aligned parallel to each other.
- the present invention provides a method for manufacturing carbon nanotubes.
- the method comprises the follows steps:
- FIG. 1 is a schematic view of depositing a catalyst material onto a substrate in accordance with the present invention
- FIG. 2 is a schematic view of an annealed catalyst material on a substrate in accordance with the present invention
- FIG. 3 is a schematic view of growing an array of carbon nanotube on a plurality of substrates in accordance with the present invention
- FIG. 4 is a schematic view of removing the carbon nanotubes from one of the substrates of FIG. 3 in accordance with the present invention
- FIG. 5 is a transmission electron microscope image of an array of carbon nanotubes in accordance with the present invention after treatment by ultrasonitication in a dispersant;
- FIG. 6 is a transmission electron microscope image of the array of carbon nanotubes in accordance with the present invention after treatment by ultrasonication in a dispersant, wherein the carbon nanotubes of the array are separated;
- FIGS. 7, 8, 9 and 10 are respectively arrays of carbon nanotube having different lengths in accordance with the present invention.
- the present invention provides a method for manufacturing carbon nanotubes that have a predetermined same length and that are aligned parallel to each other.
- the method comprises steps as follows:
- the predetermined length of the carbon nanotubes 5 can be obtained by controlling reaction conditions such as a time of reaction and a temperature of reaction.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Textile Engineering (AREA)
- Organic Chemistry (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
- 1. Field of the Invention
- The present invention relates to a method for manufacturing carbon nanotubes, and more particularly to a method for manufacturing carbon nanotubes having a predetermined same length.
- 2. Description of Related Art
- Carbon nanotubes have shown many unique electrical and mechanical properties. Their potential applications include use in field emitters, gas storage and separation, nanoprobes, chemical sensors and high strength composites. Currently there are three principal techniques to manufacture high quality carbon nanotubes, namely arc discharge, laser ablation and chemical vapor deposition. The carbon nanotubes made by arc discharge and laser ablation are often accompanied by a large volume (up to 50%) of contaminants and are tangled with each other. It is very difficult to separate the carbon nanotubes. Furthermore, those production techniques are capital-intensive and are likely limited to research quantities. The carbon nanotubes made using a chemical vapor deposition technique are in good yield—occasionally over 90%—and have few contaminants.
- Carbon nanotubes having a predetermined same length and being parallel to each other are generally desired in field emission devices, in composite reinforced material and in electrovacuum device. However, not all methods can directly produce carbon nanotubes having a predetermined same length and being parallel to each other.
- Therefore, a method for manufacturing carbon nanotubes having a predetermined same length and being parallel to each other is desired.
- Accordingly, an object of the present invention is to provide a method for manufacturing carbon nanotubes that have a predetermined same length and that are aligned parallel to each other.
- In order to achieve the object set forth above, the present invention provides a method for manufacturing carbon nanotubes. The method comprises the follows steps:
- (1) depositing a catalyst material onto a substrate;
- (2) exposing the catalyst material to a carbon containing gas for a predetermined period of time at a predetermined temperature such that an array of carbon nanotubes having a predetermined length grows from the substrate in a direction substantially perpendicular to the substrate; and
- (3) removing the carbon nanotubes from the substrate.
- Other objects, advantages and novel features of the present invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings, in which:
- FIG. 1 is a schematic view of depositing a catalyst material onto a substrate in accordance with the present invention;
- FIG. 2 is a schematic view of an annealed catalyst material on a substrate in accordance with the present invention;
- FIG. 3 is a schematic view of growing an array of carbon nanotube on a plurality of substrates in accordance with the present invention;
- FIG. 4 is a schematic view of removing the carbon nanotubes from one of the substrates of FIG. 3 in accordance with the present invention;
- FIG. 5 is a transmission electron microscope image of an array of carbon nanotubes in accordance with the present invention after treatment by ultrasonitication in a dispersant;
- FIG. 6 is a transmission electron microscope image of the array of carbon nanotubes in accordance with the present invention after treatment by ultrasonication in a dispersant, wherein the carbon nanotubes of the array are separated; and
- FIGS. 7, 8,9 and 10 are respectively arrays of carbon nanotube having different lengths in accordance with the present invention.
- The present invention provides a method for manufacturing carbon nanotubes that have a predetermined same length and that are aligned parallel to each other. The method comprises steps as follows:
- (1) referring to FIG. 1, providing a
substrate 3 comprising a wafer silicon or silica; - (2) depositing a catalyst material1 onto a surface of the
substrate 3 by electron beam evaporation, sputtering or coating, such that acatalyst material film 11 between 4-10 nm thick is formed on the surface of thesubstrate 3, the catalyst material 1 being selected from the group consisting of iron, nickel and cobalt; - (3) referring to FIG. 2, annealing the
catalyst material film 11 in air at 300-500 degrees Centigrade for between 8-12 hours, such that thecatalyst material film 11 is changed into separate nanoparticles 12; - (4) referring to FIG. 3, putting a plurality of the
substrates 3 with nanoparticles 12 in afurnace 4; - (5) heating the
furnace 4 to between 600-1000 degrees Centigrade in flowing protecting gas (not labeled), the protecting gas being selected from the group consisting of argon, nitrogen and helium; - (6) introducing a flow of carbon containing gas into the
furnace 4 for between 15 seconds and 40 minutes, the carbon containing gas being selected from the group consisting of acetylene, methane and ethylene; - (7) growing an array of carbon nanotubes5 (see FIG. 4) having a predetermined length from the surface of each
substrate 3; - (8) cooling the
furnace 4 to room temperature, and taking thesubstrates 3 out from thefurnace 4; - (9) referring to FIG. 4, removing the
carbon nanotubes 5 from the array of eachsubstrate 3 by using ablade 6; and - (10) dispersing the
carbon nanotubes 5 via ultrasonication in a dispersant, the dispersant being ethanol or 1-2 dichloroethane. - Referring to FIGS. 5 and 6, since the
carbon nanotubes 5 of the array are substantially parallel to each other, a multiplicity ofseparate carbon nanotubes 5 can be easily obtained after ultrasonication in the dispersant. - Referring to FIGS. 7, 8,9, and 10, the predetermined length of the
carbon nanotubes 5 can be obtained by controlling reaction conditions such as a time of reaction and a temperature of reaction. - growing a carbon nanotube array of 10 microns height on each of a plurality of silicon wafers. An iron film of 5 nm thickness is deposited on a porous surface of each silicon wafer. The porous surfaces of the silicon wafers are obtained by electrochemical etching of P-doped N+-type silicon wafers. The silicon wafers are then annealed in air at 400 degrees Centigrade for 10 hours. This annealing step oxidizes the iron film to create a largely iron oxide nanoparticles. The silicon wafers are then placed in a cylindrical quartz boat sealed at one end, and the quartz boat is put into the center of a 2-inch quartz tube reactor housed in a tube furnace. The furnace is heated to 690 degrees Centigrade in flowing argon. Ethylene is then introduced into the furnace for 15 seconds, after which the furnace is cooled to room temperature.
- growing a carbon nanotube array of 100 microns height on each of a plurality of silicon wafers. An iron film of 5 nm thickness is deposited on a porous surface of each silicon wafer, similar to that described above in relation to Example 1. The substrates are then annealed in air at 400 degrees Centigrade for 10 hours. The substrates are placed in a cylindrical quartz boat sealed at one end, and the quartz boat is put into the center of a 2-inch quartz tube reactor housed in a tube furnace. The furnace is heated to 690 degrees Centigrade in flowing argon. Ethylene is then introduced into the furnace for 5 minutes, after which the furnace is cooled to room temperature.
- growing a carbon nanotube array of 500 microns height on each of a plurality of silicon wafers. An iron film of 5 nm thickness is deposited on a porous surface of each silicon wafer, similar to that described above in relation to Example 1. The substrates are then annealed in air at 400 degrees Centigrade for 10 hours. The substrates are placed in a cylindrical quartz boat sealed at one end, and the quartz boat is put into the center of a 2-inch quartz tube reactor housed in a tube furnace. The furnace is heated to 710 degrees Centigrade in flowing argon. Ethylene is then introduced into the furnace for 10 minutes, after which the furnace is cooled to room temperature.
- It is understood that the invention may be embodied in other forms without departing from the spirit thereof. Thus, the present examples and embodiments are to be considered in all respects as illustrative and not restrictive, and the invention is not to be limited to the details given herein.
Claims (14)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN02152109.3 | 2002-11-29 | ||
CNB021521093A CN1290763C (en) | 2002-11-29 | 2002-11-29 | Process for preparing nano-carbon tubes |
Publications (1)
Publication Number | Publication Date |
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US20040105807A1 true US20040105807A1 (en) | 2004-06-03 |
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ID=32331914
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US10/410,069 Abandoned US20040105807A1 (en) | 2002-11-29 | 2003-04-08 | Method for manufacturing carbon nanotubes |
Country Status (3)
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US (1) | US20040105807A1 (en) |
JP (2) | JP2004182581A (en) |
CN (1) | CN1290763C (en) |
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US20060263524A1 (en) * | 2005-03-31 | 2006-11-23 | Tsinghua University | Method for making carbon nanotube array |
US20060263274A1 (en) * | 2005-03-25 | 2006-11-23 | Tsinghua University | Apparatus for making carbon nanotube array |
US20060269668A1 (en) * | 2005-03-16 | 2006-11-30 | Tsinghua University | Method for making carbon nanotube array |
US20070103048A1 (en) * | 2005-11-04 | 2007-05-10 | Tsinghua University | Method for fabricating carbon nanotube-based field emission device |
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CN1290763C (en) | 2006-12-20 |
CN1504407A (en) | 2004-06-16 |
JP2004182581A (en) | 2004-07-02 |
JP2006347878A (en) | 2006-12-28 |
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