US20070009420A1 - Fullerene shell tube and process for producing the same - Google Patents

Fullerene shell tube and process for producing the same Download PDF

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Publication number
US20070009420A1
US20070009420A1 US10/574,506 US57450606A US2007009420A1 US 20070009420 A1 US20070009420 A1 US 20070009420A1 US 57450606 A US57450606 A US 57450606A US 2007009420 A1 US2007009420 A1 US 2007009420A1
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US
United States
Prior art keywords
fullerene
shell tube
tube
producing
fullerene shell
Prior art date
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Abandoned
Application number
US10/574,506
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English (en)
Inventor
Kun'ichi Miyazawa
Toshiyuki Mori
Chikashi Nishimura
Tadatomo Suga
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National Institute for Materials Science
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National Institute for Materials Science
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Publication date
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Assigned to NATIONAL INSTITUTE FOR MATERIALS SCIENCE reassignment NATIONAL INSTITUTE FOR MATERIALS SCIENCE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MIYAZAWA, KUN'ICHI, MORI, TOSHIYUKI, NISHIMURA, CHIKASHI, SUGA, TADATOMO
Publication of US20070009420A1 publication Critical patent/US20070009420A1/en
Abandoned legal-status Critical Current

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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
    • 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
    • C01B32/152—Fullerenes
    • C01B32/156—After-treatment

Definitions

  • the invention of this application relates to a fullerene shell tube which can be used in wide applications such as field emission devices, gas filters, hydrogen storage materials and catalyst supports in various industries such as energy, chemical industries, electronics and semiconductors, and a process for producing the same.
  • fullerene Although the presence of a fullerene was experimentally proved by researchers abroad in 1985 , its structural model had been already known in Japan in 1970. Thus, Japan has always led the world in studies of fullerenes. As a typical fullerene, C 60 has been known. Various fullerenes such as C 70 , C 76 , C 78 , C 82 , C 84 , C 240 , C 540 and C 720 other than C 60 have been known. The technology in the field of fullerenes has been progressed very quickly, and new fullerene compounds have been introduced one after another.
  • Non-Patent Document 1 a process in which a shell structure comprising amorphous carbon derived from fullerene is formed by heat-treating crystals of typical fullerene C 60 in vacuum (non-Patent Document 1), a process in which fullerene whiskers (carbon filaments) are produced by a liquid-liquid interfacial precipitation method, and the like have been proposed by the inventors of this application (for example, Patent Document 1 and non-Patent Documents 2 and 3).
  • This carbon nanotube has a structure in which a graphite sheet is cylindrically rolled up. Unlike such a structure of the carbon nanotube, a structure of a fullerene shell tube derived from a fullerene whisker (FW) or a fullerene nanowhisker (FNW) having a three-dimensional periodical structure in which symmetry of fullerene needle crystals or the like is defined by a space group has been imagined. It has been so far known that a fullerene shell is formed by heat-treating crystals of a fullerene, but a tubular fullerene shell (hereinafter referred to as a fullerene shell tube) or a process for producing the same has been to date utterly unknown.
  • a fullerene shell tube tubular fullerene shell
  • Patent Document 1 JP-A 2003-1600
  • non-Patent Document 1 H. Sakuma, M. Tachibana, H. Sugiura, K. Kojima, S. Ito, T. Sekiguchi, Y. Achiba, J. Mater, Res., 12(1997)1545.
  • non-Patent Document 2 K. Miyazawa, Y. Kuwasaki, A. Obayashi and M. Kuwabara, “C60 nanowhiskers formed by the liquid-liquid interfacial precipitation method”, J. Mater, Res., 17[1](2002)83.
  • non-Patent Document 3 Kunichi Miyazawa “C70 Nanowhiskers Fabricated by Forming Liquid/Liquid Interfaces in the Systems of Toluene Solution of C70 and Isopropyl Alcohol”, J. Am. Ceram. Soc., 85[5] (2002) 1297.
  • the fullerene shell tube can be used in applications such as hydrogen storage materials, catalyst supports, new semiconductors, field emission materials and fuel cell electrode materials.
  • applications such as hydrogen storage materials, catalyst supports, new semiconductors, field emission materials and fuel cell electrode materials.
  • the fact is that a process for producing a fullerene shell tube and various possibilities of this fullerene shell tube structure have been unknown.
  • the invention of this application aims to provide a fullerene shell tube expected as a new functional material and a process for producing the same.
  • the invention first provides a process for producing a fullerene shell tube, which comprises heat-treating a fullerene whisker or fiber at a temperature of from 500 to 1,000° C.
  • the fullerene is C 60 fullerene, a higher-order fullerene having the carbon number of 70 or more, a metal-containing fullerene or fullerene derivatives.
  • the invention of this application third provides a fullerene shell tube in which a diameter is in the range of from 10 nm to 100 ⁇ m, and a length is 100 nm or more.
  • the tube wall comprises crystalline carbon or amorphous carbon.
  • FIG. 1 is a transmission electron microscope (TEM) photograph of a fullerene shell tube produced by heating a fullerene nanowhisker in vacuum at 600° C. for 30 minutes.
  • TEM transmission electron microscope
  • FIG. 2 is a transmission electron microscope (TEM) photograph of a fullerene shell tube produced by heating a fullerene nanowhisker in vacuum at 700° C. for 30 minutes.
  • TEM transmission electron microscope
  • FIG. 3 is a transmission electron microscope (TEM) photograph of a fullerene shell tube produced by heating a fullerene nanowhisker in vacuum at 600° C. for 30 minutes.
  • TEM transmission electron microscope
  • FIG. 4 is a transmission electron microscope (TEM) photograph of a fullerene shell tube with a filling tissue thereinside which tube is produced by heating a fullerene nanowhisker in vacuum at 600° C. for 30 minutes.
  • TEM transmission electron microscope
  • the fullerene shell tube is produced by heat-treating various fullerene whiskers or fibers at the temperature of from 500 to 1,000° C.
  • the fullerene includes not only typical C 60 whiskers or fibers, but also whiskers or fibers of higher-order fullerenes having the carbon number of 70 or more, metal-containing fullerenes and further various fullerene derivatives which have been so far known.
  • the heating at the temperature of from 500° C. to 1,000° C. is conducted in vacuum or in a gas atmosphere.
  • a degree of vacuum is a pressure of 1 Pa or less
  • the gas atmosphere is an oxygen partial pressure of 10 ⁇ 1 Pa or less, and the like.
  • An inert gas such as argon may be present.
  • Example The invention is thus illustrated more specifically below by referring to Example. Of course, the invention is not limited by the following Example.
  • liquid-liquid interfacial precipitation method 30 ml of isopropyl alcohol is first gently added to 30 ml of toluene saturated with fullerene (C 60 ) having a purity of 99.5%.
  • the solution is kept at room temperature (from 15° C. to 21° C.) for approximately 50 hours to produce a fullerene nanowhisker.
  • the resulting fullerene nanowhisker is retained in vacuum at 600° C., and heat-treated for 30 minutes to produce a fullerene shell tube having a wall of amorphous carbon.
  • FIG. 1 is a transmission electron microscope (TEM) photograph of the resulting fullerene shell tube.
  • the fullerene shell tube made of the fullerene nanowhisker has a nanometer-order diameter, and it is confirmed, as shown by the arrow, that a polygonal wall structure is present by reflecting the crystal habit surface of the original fullerene nanowhisker.
  • the crystal habit here referred to indicates characteristics of the size and the form of the crystal.
  • FIG. 2 is a transmission electron microscope (TEM) photograph of a fullerene shell tube wall produced by heating a fullerene nanowhisker in vacuum at 700° C. for 30 minutes. From the transmission electron microscope photograph, it is confirmed that the fullerene shell tube wall comprises amorphous carbon and has a thickness of approximately 30 nm.
  • TEM transmission electron microscope
  • FIG. 3 is a transmission electron microscope (TEM) of the fullerene shell tube wall.
  • a fullerene shell tube useful as a functional material in wide applications such as field emission devices, gas filters, hydrogen storage materials and catalyst supports in energy, catalyst and semiconductor industries.
  • a fullerene shell tube having a specific size is provided.
  • the foregoing effect is obtained, and further a shape of a carbon wall constituting the fullerene shell tube is specified.
  • the foregoing effect is obtained, and further a structure of an end of the fullerene shell tube wall is specified.
  • a state of the inside of the fullerene shell tube is specified.
  • the fullerene shell tube obtained in the invention of this application is useful as a new functional material in wide applications such as field emission devices, gas filters, hydrogen storage materials and catalyst supports in various industries such as energy, chemical industries, electronics and semiconductors.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Catalysts (AREA)
US10/574,506 2003-10-03 2004-10-01 Fullerene shell tube and process for producing the same Abandoned US20070009420A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2003346117A JP3845731B2 (ja) 2003-10-03 2003-10-03 フラーレンシェルチューブとその製造方法
JP2003-346117 2003-10-03
PCT/JP2004/014878 WO2005033008A1 (ja) 2003-10-03 2004-10-01 フラーレンシェルチューブとその製造方法

Publications (1)

Publication Number Publication Date
US20070009420A1 true US20070009420A1 (en) 2007-01-11

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US10/574,506 Abandoned US20070009420A1 (en) 2003-10-03 2004-10-01 Fullerene shell tube and process for producing the same

Country Status (4)

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US (1) US20070009420A1 (ja)
EP (1) EP1681264A4 (ja)
JP (1) JP3845731B2 (ja)
WO (1) WO2005033008A1 (ja)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060090689A1 (en) * 2003-01-10 2006-05-04 Tetsuro Yoshii Fullerene crystal and method for producing same
US20150140474A1 (en) * 2007-07-06 2015-05-21 M. Technique Co., Ltd. Method for producing metal-supported carbon, method for producing crystals consisting of fullerene molecules and fullerene nanowhisker/nanofiber nanotubes, and apparatus for producing the same

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5093436B2 (ja) * 2006-02-17 2012-12-12 独立行政法人物質・材料研究機構 物質担持フラーレンチューブとその製造方法
JP5205672B2 (ja) * 2007-08-29 2013-06-05 独立行政法人物質・材料研究機構 フラーレン細線付き基盤とその製造方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020192143A1 (en) * 2001-04-18 2002-12-19 Miyazawa Kun-Ichi Fine carbon wires and methods for producing the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020192143A1 (en) * 2001-04-18 2002-12-19 Miyazawa Kun-Ichi Fine carbon wires and methods for producing the same

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060090689A1 (en) * 2003-01-10 2006-05-04 Tetsuro Yoshii Fullerene crystal and method for producing same
US7351284B2 (en) * 2003-01-10 2008-04-01 Nippon Sheet Glass Company, Limited Fullerene crystal and method for producing same
US20150140474A1 (en) * 2007-07-06 2015-05-21 M. Technique Co., Ltd. Method for producing metal-supported carbon, method for producing crystals consisting of fullerene molecules and fullerene nanowhisker/nanofiber nanotubes, and apparatus for producing the same
US9917308B2 (en) * 2007-07-06 2018-03-13 M. Technique Co., Ltd. Method for producing crystals comprising fullerene molecules and fullerene nanowhisker/nanofiber nanotubes

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Publication number Publication date
EP1681264A4 (en) 2009-09-09
EP1681264A1 (en) 2006-07-19
JP2005112643A (ja) 2005-04-28
WO2005033008A1 (ja) 2005-04-14
JP3845731B2 (ja) 2006-11-15

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