WO1999043613A1 - Procede de production d'un nano-tube en carbone - Google Patents

Procede de production d'un nano-tube en carbone Download PDF

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Publication number
WO1999043613A1
WO1999043613A1 PCT/JP1999/000982 JP9900982W WO9943613A1 WO 1999043613 A1 WO1999043613 A1 WO 1999043613A1 JP 9900982 W JP9900982 W JP 9900982W WO 9943613 A1 WO9943613 A1 WO 9943613A1
Authority
WO
WIPO (PCT)
Prior art keywords
carbon
nanotubes
irradiation
carbon nanotubes
laser
Prior art date
Application number
PCT/JP1999/000982
Other languages
English (en)
Japanese (ja)
Inventor
Hisaji Matsui
Chiharu Yamaguchi
Hitoshi Nishino
Ayumu Yasuda
Noboru Kawase
Original Assignee
Osaka Gas Company Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Osaka Gas Company Limited filed Critical Osaka Gas Company Limited
Publication of WO1999043613A1 publication Critical patent/WO1999043613A1/fr

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Classifications

    • 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

Definitions

  • the present invention relates to a method for producing carbon nanotubes or a carbon material containing them.
  • nanotubes have been prepared by using a carbon material such as graphite as a raw material, and using a carbon arc method in the presence of a catalytic metal. It is synthesized by a gas phase method such as a sputtering method, a laser-light irradiation method, or the like.
  • nanotubes have a linear shape, it is advantageous to increase the density of the material, diffuse gas in the material, etc.However, a method for producing such nanotubes with high yield is as follows. unknown.
  • the present invention provides a carbon nanotube having a controlled structure. Its main purpose is to provide technologies that can produce tubes at high yields.
  • the present invention provides the following carbon nanotubes.
  • a method for producing carbon nanotubes characterized in that:
  • carbon nano Form a thin film of tubes or nanotubes.
  • Such force nanotubes can also be formed on substrates, particles and porous bodies.
  • a polymer having a reactive triple bond JP-A-3-44582, JP-A-63-199726, M. Kijima et al, Synthetic Metals, 86 (1997), 2279, etc. It has been disclosed.
  • the nanotubes can be used.
  • these thin films can be obtained.
  • the heating may be performed simultaneously with the irradiation or before or after the irradiation.
  • a laser beam As an irradiation operation for applying reaction energy to raw materials, it is more preferable to use a laser beam as an irradiation source.
  • the nanotubes according to the present invention have a diameter of usually less than 100 nm and can be controlled by selecting the manufacturing conditions.
  • the nanotube according to the present invention is linear, It has a unique shape that there is no entanglement between tubes. Such a shape has not been obtained in a high yield by a known method for producing carbon nanotubes.
  • the obtained carbon nanotubes can be formed on the surface of the precursor as well as being obtained in a linear shape, so that they can be formed in a thin film state on the substrate. You.
  • Electrolytic reduction is performed by a two-electrode method (anode: magnesium, cathode: stainless steel), and a tetrahydrofuran solution (LiCl: 0.8 g, FeCl 2 : 0.48 g, THF: 30 ml) was used.
  • Ten sheets of PTFE film were charged together with a solvent in a flask in which the anode and cathode were installed, and subjected to electrolytic reduction at 0 ° C for 15 hours in an argon atmosphere with stirring.
  • a potential of 25 V was applied between the cathode and the cathode.
  • the PTFE film was washed with THF, dried under vacuum, and stored in an argon atmosphere.
  • a 100-ml internal flask equipped with a three-way cock contains 0.0g of granular Mgl, 2.66 g of anhydrous lithium chloride (LiCl), Iron (FeCl 2 ) l.60 g and PTFE phenol (8ramX 8mra X 50 nm) 20 pieces (total weight (About 0.2 g) and a stirrer chip, heat and reduce the pressure to 1 mm Hg at 50 ° C, dry the raw materials, and introduce dry argon gas into the reactor. To the mixture was added 44 ml of THF previously dried with sodium benzophenokentine, and the mixture was stirred at room temperature with a magnetic stirrer for about 3 hours.
  • LiCl lithium chloride
  • Iron FeCl 2
  • PTFE phenol 8ramX 8mra X 50 nm
  • Electron beam irradiation was performed in the same manner as in Example 1 using a non-electrolytically or chemically reduced PT FE film as in Example 1, and the PT FE was decomposed. / Evaporated and nothing remained. From this, it is clear that irradiation of PTFE directly with an electron beam does not result in the formation of carbon nanotubes.
  • the carbon cluster synthesized in the gas phase was press-molded.
  • This carbon cluster was manufactured by using a carbon arc using a graphite electrode, and had a diameter of 10 nm or less and had a lamellar structure of graphite inside. It was structurally similar to what is called onion-like carbon, and had no fullerene structure.
  • Example 2 or Example 3 using a non-reducing PTFE film In the same manner as in 3, laser light was irradiated under reduced pressure heating. As a result of TEM observation, formation of carbon nanotubes was not recognized in any case without any change.
  • the ion beam was irradiated under reduced pressure and heating in the same manner as in Example 4 using a non-reduced PTFE film.
  • formation of carbon nanotubes was not recognized without any change due to irradiation.
  • Natural graphite from Madagascar was press-molded and irradiated with an ion beam under reduced pressure and heating in the same manner as in Example 4. As a result of TEM observation, formation of carbon nanotubes was not recognized without any change due to irradiation.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Cette invention concerne un procédé de production d'un nano-tube en carbone, lequel procédé consiste à soumettre un matériau carboné et contenant du -C C- et/ou du =C= réactifs à un chauffage et/ou à un rayonnement lumineux, etc.
PCT/JP1999/000982 1998-02-27 1999-03-01 Procede de production d'un nano-tube en carbone WO1999043613A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP10/46757 1998-02-27
JP4675798 1998-02-27

Publications (1)

Publication Number Publication Date
WO1999043613A1 true WO1999043613A1 (fr) 1999-09-02

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP1999/000982 WO1999043613A1 (fr) 1998-02-27 1999-03-01 Procede de production d'un nano-tube en carbone

Country Status (1)

Country Link
WO (1) WO1999043613A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003014018A1 (fr) * 2001-08-06 2003-02-20 Osaka Gas Company Limited Matiere carbonee, matiere d'occlusion de gaz renfermant ladite matiere carbonee et procede de stockage de gaz a l'aide de cette matiere d'occlusion de gaz
GB2384008A (en) * 2001-12-12 2003-07-16 Electrovac Synthesising carbon nano tubes using ion beams
US6960334B1 (en) 1998-12-28 2005-11-01 Osaka Gas Company Limited Amorphous nano-scale carbon tube and production method therefor
US7378075B2 (en) 2002-03-25 2008-05-27 Mitsubishi Gas Chemical Company, Inc. Aligned carbon nanotube films and a process for producing them

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09221309A (ja) * 1996-02-13 1997-08-26 Agency Of Ind Science & Technol カーボンナノチューブを表面に有する炭素質物及びその製造方法
JPH09249405A (ja) * 1996-03-12 1997-09-22 Osaka Gas Co Ltd 炭素材料の製造方法
JPH10167714A (ja) * 1996-12-16 1998-06-23 Osaka Gas Co Ltd 炭素材料の製法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09221309A (ja) * 1996-02-13 1997-08-26 Agency Of Ind Science & Technol カーボンナノチューブを表面に有する炭素質物及びその製造方法
JPH09249405A (ja) * 1996-03-12 1997-09-22 Osaka Gas Co Ltd 炭素材料の製造方法
JPH10167714A (ja) * 1996-12-16 1998-06-23 Osaka Gas Co Ltd 炭素材料の製法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KAWASE N., ET AL.: "IN-SITU OBSERVATION OF FORMATION OF NANOSCALE CARBON TUBULES.", CARBON., ELSEVIER, OXFORD., GB, vol. 36., no. 12., 1 January 1998 (1998-01-01), GB, pages 1864/1865., XP002919083, ISSN: 0008-6223, DOI: 10.1016/S0008-6223(98)90059-8 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6960334B1 (en) 1998-12-28 2005-11-01 Osaka Gas Company Limited Amorphous nano-scale carbon tube and production method therefor
WO2003014018A1 (fr) * 2001-08-06 2003-02-20 Osaka Gas Company Limited Matiere carbonee, matiere d'occlusion de gaz renfermant ladite matiere carbonee et procede de stockage de gaz a l'aide de cette matiere d'occlusion de gaz
GB2384008A (en) * 2001-12-12 2003-07-16 Electrovac Synthesising carbon nano tubes using ion beams
GB2384008B (en) * 2001-12-12 2005-07-20 Electrovac Method of synthesising carbon nano tubes
US7033647B2 (en) 2001-12-12 2006-04-25 Electrovac, Fabrikation Elektrotechnischer Spezialartikel Gesellschaft M.B.H. Method of synthesising carbon nano tubes
US7378075B2 (en) 2002-03-25 2008-05-27 Mitsubishi Gas Chemical Company, Inc. Aligned carbon nanotube films and a process for producing them

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