JP2006347878A - Method for manufacturing carbon nanotube - Google Patents

Method for manufacturing carbon nanotube Download PDF

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Publication number
JP2006347878A
JP2006347878A JP2006234173A JP2006234173A JP2006347878A JP 2006347878 A JP2006347878 A JP 2006347878A JP 2006234173 A JP2006234173 A JP 2006234173A JP 2006234173 A JP2006234173 A JP 2006234173A JP 2006347878 A JP2006347878 A JP 2006347878A
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Japan
Prior art keywords
substrate
carbon nanotubes
carbon
step
method
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JP2006234173A
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Japanese (ja)
Inventor
守善 ▲ハン▼
Feng-Yan Fan
Kaili Jiang
Liang Liu
亮 劉
開利 姜
Original Assignee
Kofukin Seimitsu Kogyo (Shenzhen) Yugenkoshi
Qinghua Univ
ツィンファ ユニバーシティ
鴻富錦精密工業(深▲セン▼)有限公司
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Priority to CNB021521093A priority Critical patent/CN1290763C/en
Application filed by Kofukin Seimitsu Kogyo (Shenzhen) Yugenkoshi, Qinghua Univ, ツィンファ ユニバーシティ, 鴻富錦精密工業(深▲セン▼)有限公司 filed Critical Kofukin Seimitsu Kogyo (Shenzhen) Yugenkoshi
Publication of JP2006347878A publication Critical patent/JP2006347878A/en
Application status is Pending legal-status Critical

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/168After-treatment
    • C01B32/174Derivatisation; Solubilisation; Dispersion in solvents
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/127Carbon 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/127Carbon 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
    • D01F9/1271Alkanes or cycloalkanes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/127Carbon 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
    • D01F9/1271Alkanes or cycloalkanes
    • D01F9/1272Methane
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/127Carbon 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
    • D01F9/1273Alkenes, alkynes
    • D01F9/1275Acetylene
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00Structure or properties of carbon nanotubes
    • C01B2202/08Aligned nanotubes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00Structure or properties of carbon nanotubes
    • C01B2202/20Nanotubes characterized by their properties
    • C01B2202/34Length

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing carbon nanotubes in which grown tubes have a uniform and controlled length and do not connect with each other and can easily disperse. <P>SOLUTION: This invention provides a method for manufacturing one kind of carbon nanotube, and the method comprises: (1) a step of providing a substrate; (2) a step of depositing a catalyst onto the substrate; (3) a step of bringing the catalyst into contact with a carbon containing gas for a predetermined period of time at a predetermined temperature, to thereby grow an array of carbon nanotubes having a predetermined length from the substrate in a direction substantially perpendicular to the substrate; and (4) a step of separating the carbon nanotubes from the substrate. This invention provides a method for manufacturing a matrix of carbon nanotubes by the chemical vapor deposition method, in which grown tubes have a uniform and controlled length and do not connect with each other and can easily disperse, as compared to the conventional technology. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a kind of carbon nanotube.

  Carbon nanotubes have excellent physicochemical performance, such as unique metal or semiconductor conductivity, much higher mechanical strength, hydrogen storage capacity, adhesion capacity and stronger microwave storage capacity at the beginning of the 1990s. Attracted attention in the physics, chemistry, materials science academia and advanced technology sector. Carbon nanotubes need to solve problems such as low cost and mass production for industrial realization. Carbon nanotubes have been developed in 1991 and have been extensively studied as a method for producing them. At present, carbon nanotube production methods are mainly arc discharge method, laser evaporation method and chemical vapor deposition method. The products produced by the arc discharge method and the laser evaporation method contain carbon nanotubes and other carbon products, are difficult to purify, have a lower yield, and are difficult to mass produce. Carbon nanotubes produced by chemical vapor deposition using methane as a carbon-containing gas (gas containing carbon) are easy to manufacture, low cost, easy to control production scale, large length, high production rate, etc. Therefore, it has significant research value and is widely used in fields such as field effect displays, electric vacuum devices, nanoelectronics, and high-strength composite materials.

  However, the length of the carbon nanotubes is not controlled by the conventional technology, and the produced carbon nanotubes are easily tied together and difficult to disperse, and are not suitable for industrial implementation such as field effect displays and high-strength composite materials.

  Therefore, there is a need to provide a method for producing carbon nanotubes in which the growth length is uniform and controlled, does not tie, and is easy to disperse.

  An object of the present invention is to provide a method for producing carbon nanotubes in which the growth length is uniform and controlled, and does not tie and is easy to disperse.

  In order to achieve the above object, the present invention provides a method for producing a carbon nanotube, which includes the following steps: (1) providing a substrate; and (2) a catalyst on the substrate. And (3) contacting a catalyst and a carbon-containing gas at a predetermined temperature for a certain period of time to grow carbon nanotubes having a specific length on the substrate, and (4) ) Separating the carbon nanotubes from the substrate.

  In the present invention, after the step (4), the carbon nanotubes are dispersed in a dispersion solution with ultrasonic waves.

  Compared to the prior art, the present invention provides a method for producing a matrix of carbon nanotubes which is uniform and controlled by chemical vapor deposition and is easy to disperse without being tied.

The present invention provides a method for producing a matrix of carbon nanotubes which is uniform and controlled by chemical vapor deposition and is easy to disperse without being tied, and details of the production method are as follows.
(1) Please refer to FIG. Providing a silicon plate or a Brazilian stone plate as the substrate 3 to be used repeatedly,
(2) The catalyst 1 is deposited on one or both surfaces of the above 3 by a thermal deposition method, ion beam evaporation method, splash method or the like to form a catalyst metal film 11 having a thickness of 4 to 10 nm. Or nickel is chosen.
(3) Please refer to FIG. The catalyst film is annealed at 300 to 500 ° C. in an air atmosphere for 8 to 12 hours, and the catalyst film is oxidized to form separated nanoparticles 12.
(4) Please refer to FIG. A plurality of substrates 3 having catalyst particles 12 are simultaneously fed to the reactor 4;
(5) Introducing an inert gas (not shown) and simultaneously heating the reactor 4 to 600-1000 ° C.,
(6) An inert gas and a carbon-containing gas (not shown) are introduced, argon, nitrogen or helium is selected as the inert gas, and acetylene, methane or ethylene is selected as the carbon-containing gas. ,
(7) After reacting for 15 s to 40 min, a carbon nanotube matrix having a certain height grows from the surface of the substrate,
(8) The reactor 4 is cooled to room temperature.
(9) Please refer to FIG. The substrate 3 is taken out, and the carbon nanotubes 5 are swept out by a scraper 6, or blown out by a fine wire or high-pressure gas, and the substrate 3 is directly used for growth or purified and used for the next deposition.

  Further, the carbon nanotubes 5 are dispersed by ultrasonic waves in a dispersion solution such as alcohol or 1,2-ethylidene chloride.

  The carbon nanotubes 5 in the matrix of carbon nanotubes are arranged in parallel and do not tie, thus making it easy to obtain a well dispersed single carbon nanotube. Please refer to FIG. 5 and FIG. 6 together. The carbon nanotubes 5 of the present invention are not tied together, but are dispersed into a single carbon nanotube or a bundle of carbon nanotubes having a small tube diameter by ultrasonic waves.

  Further, by controlling the growth conditions, for example, the reaction time and the reaction temperature are controlled to form a carbon nanotube matrix having a specific height, and the carbon nanotubes 5 therein have a desired precise length. This is shown in FIG. 7, FIG. 8, FIG. 9 and FIG.

  The first embodiment produces a carbon nanotube matrix having a length of 10 μm, the details of which are as follows.

  An iron catalyst film having a thickness of 5 nm is deposited on a porous silicon substrate, the substrate is annealed at 400 ° C. for 10 hours in an air atmosphere, and the substrate is placed in a Brazilian stone reaction dish. The reactor was heated to 690 ° C. in an argon atmosphere, introduced with ethylene, reacted for 15 s, cooled to room temperature, and 10 μm long. Growing a matrix of carbon nanotubes.

  In the second embodiment, a matrix of carbon nanotubes having a length of 100 μm is manufactured, and details thereof are as follows.

  An iron catalyst film having a thickness of 5 nm is deposited on a porous silicon substrate, the substrate is annealed at 400 ° C. for 10 hours in an air atmosphere, the substrate is placed in a Brazilian stone reaction dish, and the reaction dish is placed in a Brazilian stone. The reactor was heated to 690 ° C. in an argon atmosphere, introduced with ethylene, reacted for 5 minutes, cooled to room temperature, and 100 μm long. Growing a matrix of carbon nanotubes.

  The third embodiment produces a carbon nanotube matrix having a length of 500 μm, the details of which are as follows.

  An iron catalyst film having a thickness of 5 nm is deposited on a porous silicon substrate, the substrate is annealed at 400 ° C. for 10 hours in an air atmosphere, and the substrate is placed in a Brazilian stone reaction dish. The reactor was sent to the central reaction chamber of the reactor, heated to 710 ° C. in an argon atmosphere, introduced with ethylene, reacted for 10 min, then cooled to room temperature, and a length of 500 μm. Growing a matrix of carbon nanotubes.

From the experimental results, the carbon nanotube matrix has a density of 0.1 g / cm 3 . Taking a 100 μm high carbon nanotube matrix as an example, a reactor with 30 pieces of a 4 inch (25.4 mm / inch) silicon substrate (with catalyst deposited on one side) simultaneously placed 2.4 g in a reactor. The growth time is about 5 min.

  In general, the present invention is sufficiently prepared as a requirement for a patent and should be registered by law. Moreover, the above is merely a more preferred embodiment in the present application, and does not limit the scope of the present invention. Any modification or change that a person who is familiar with the technology of the present invention can make based on the idea of the present invention shall belong to the claims of the present invention.

It is a schematic diagram which deposits the catalyst of this invention on a board | substrate. It is the schematic diagram which annealed the catalyst of this invention. It is a schematic diagram in which a substrate having a catalyst of the present invention is placed in a reaction furnace, a reaction gas is introduced, and carbon nanotubes are grown. It is a schematic diagram of sweeping from the substrate of the carbon nanotube of the present invention. The matrix of the carbon nanotube of the present invention is a photograph of a transmission electron microscope dispersed ultrasonically in a dispersion solution. The matrix of the carbon nanotube of the present invention is a photograph of a transmission electron microscope dispersed ultrasonically in a dispersion solution, in which the carbon nanotube is dispersed into a single carbon nanotube. It is a SEM photograph of the carbon nanotube of the fixed height of the present invention. It is a SEM photograph of the carbon nanotube of the fixed height of the present invention. It is a SEM photograph of the carbon nanotube of the fixed height of the present invention. It is a SEM photograph of the carbon nanotube of the fixed height of the present invention.

Explanation of symbols

1 Catalyst 3 Substrate 4 Reactor 5 Carbon Nanotube 6 Scraper 11 Catalyst Film 12 Particles

Claims (10)

  1. (1) providing a substrate;
    (2) depositing a catalyst on the substrate;
    (3) contacting the catalyst and the carbon-containing gas at a predetermined temperature for a certain period of time to grow carbon nanotubes of a predetermined length upright on the substrate;
    (4) sweeping with a scraper to separate the carbon nanotubes from the substrate;
    A method for producing a carbon nanotube, comprising:
  2.   The method for producing carbon nanotubes according to claim 1, wherein after the step (4), the carbon nanotubes are dispersed in a dispersion solution with ultrasonic waves.
  3.   The method for producing carbon nanotubes according to claim 1, wherein the catalyst in the step (2) is iron, cobalt, or nickel.
  4.   In the step (2), a catalyst film having a thickness of 4 to 100 nm is formed on the substrate, the catalyst film is annealed at 300 to 500 ° C. for 8 to 12 hours, and the catalyst is oxidized and separated. It forms in particle | grains, The manufacturing method of the carbon nanotube of Claim 1 characterized by the above-mentioned.
  5.   2. The carbon nanotube production method according to claim 1, wherein a predetermined temperature in the step (3) is 600 to 1000 ° C. 3.
  6.   The method for producing carbon nanotubes according to claim 1, wherein the carbon-containing gas in the step (3) is acetylene, methane, or ethylene.
  7.   The method for producing a carbon nanotube according to claim 1, wherein the step (3) introduces an inert gas.
  8.   2. The carbon according to claim 1, wherein the step (3) comprises bringing a matrix of 10 μm long carbon nanotubes upright on the substrate by bringing ethylene and an iron catalyst into contact at 690 ° C. for 15 s. Nanotube matrix manufacturing method.
  9.   2. The carbon according to claim 1, wherein in the step (3), a matrix of 100 μm long carbon nanotubes is grown on the substrate by bringing ethylene and an iron catalyst into contact with each other at 690 ° C. for 5 minutes. Nanotube matrix manufacturing method.
  10. 2. The carbon according to claim 1, wherein in the step (3), a 500 μm long matrix of carbon nanotubes is grown on the substrate by bringing ethylene and an iron catalyst into contact with each other at 710 ° C. for 10 minutes. Nanotube matrix manufacturing method.
JP2006234173A 2002-11-29 2006-08-30 Method for manufacturing carbon nanotube Pending JP2006347878A (en)

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