US20080279752A1 - Method for producing a single-wall carbon nanotube - Google Patents

Method for producing a single-wall carbon nanotube Download PDF

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US20080279752A1
US20080279752A1 US11/808,208 US80820807A US2008279752A1 US 20080279752 A1 US20080279752 A1 US 20080279752A1 US 80820807 A US80820807 A US 80820807A US 2008279752 A1 US2008279752 A1 US 2008279752A1
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carbon nanotube
wall carbon
producing
catalyst
dehydrated alcohol
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Masaki Suzuki
Kouji Ishibashi
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RIKEN Institute of Physical and Chemical Research
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    • 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
    • D01F9/1277—Other organic compounds
    • 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
    • C01B32/162—Preparation characterised by catalysts
    • 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
    • D01F9/133—Apparatus therefor
    • 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
    • C01B2202/02—Single-walled 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
    • 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
    • C01B2202/36—Diameter

Definitions

  • the present invention relates to a method for producing a single-wall carbon nanotube, which is hereinafter also called “SWCNT” in some cases.
  • the arc-discharge is a method in which multiwall carbon nanotubes that are hereinafter also called “MWCNT” in some cases, are produced on an anode by arc-discharging between carbon rods in an atmosphere such as argon at a pressure slightly lower than the atmospheric pressure.
  • MWCNT multiwall carbon nanotubes that are hereinafter also called “MWCNT” in some cases
  • SWCNTs can be formed on an inner side of a container.
  • This arc-discharging method has an advantage that CNTs having a relatively good quality can be produced with fewer defects.
  • this method has the problems that (i) amorphous carbon is simultaneously produced, and (ii) it is costly and (iii) unsuitable for the mass production.
  • the laser ablation is a method in which the CNTs are produced by irradiating a strong pulse beam such as YAG laser upon carbon into which catalyst such as Ni/Co is mixed in a high-temperature atmosphere of 900 to 1300° C.
  • a strong pulse beam such as YAG laser upon carbon into which catalyst such as Ni/Co is mixed in a high-temperature atmosphere of 900 to 1300° C.
  • the CNTs is produced by bringing a carbon compound as a carbon source into contact with fine particles of a catalytic metal at 500 to 1200° C., and both of the MWCNTs and the SWCNTs can be produced.
  • a catalyst is arranged on a substrate, MWCNTs can be obtained, while oriented vertically onto the surface of the substrate.
  • a method for producing the SWCNTs by using the CVD method As the method for producing the SWCNTs by using the CVD method, a method is known from a pamphlet of WO2003/068676, in which a carbon source composed of a compound having oxygen or a mixture of a compound having oxygen and a compound having carbon is contacted with a catalyst at a heating temperature.
  • a method has been sought, which can produce SWCNTs and which can realize high growth rate, growth efficiency, vertical synthesis, etc.
  • the present invention is aimed at solving the above problems, and is to provide a method for producing an SWCNT, which can realize high growth rate, growth efficiency, vertical synthesis, etc.
  • a method for producing a single-wall carbon nanotube comprising contacting an organic dehydrated alcohol with a catalyst in a closed space in vacuum at a temperature of 600 to 900° C.
  • FIG. 1 is a schematic view of a CVD apparatus used in Examples.
  • FIG. 2 is an AFM photograph of SWCNTs obtained in Example 1.
  • FIG. 3 is an enlarged photograph of a part of FIG. 2 .
  • FIG. 4 is an enlarged photograph of a part of FIG. 3 .
  • FIG. 5 is a diagram showing growth distribution proportions of the SWCNTs obtained in Example 1.
  • FIG. 7 shows a result of a Raman spectroscopic analysis (around 100 to 400 cm ⁇ 1 ) of the SWCNT obtained in Example 1.
  • FIG. 8 shows an SEM photograph of SWCNTs obtained in Example 2.
  • FIG. 9 is an enlarged photograph of a part of FIG. 8 .
  • FIG. 10 shows a sectional photograph of SWCNTs obtained in Comparative Example 1.
  • FIG. 11 shows an enlarged photograph of a part of FIG. 10 .
  • FIG. 12 shows a sectional photograph of SWCNTs obtained in Comparative Example 2.
  • FIG. 13 shows an enlarged photograph of a part of FIG. 12 .
  • the method for producing the SWCNTs according to the present invention comprises contacting an organic dehydrated alcohol with a catalyst in a closed space in vacuum at a temperature of 600 to 900° C.
  • the closed space in the present invention is in vacuum when the organic dehydrated alcohol is contacted with the catalyst.
  • the space is in the vacuum state, remaining gases, materials, etc. can easily removed, so that the SWCNTs having a high quality can be obtained.
  • the “vacuum” means a state in which the pressure is reduced and no gas flows, and for example, it means the space obtainable by carrying out a vacuum exhaust of a closed space using a vacuum pump.
  • the degree of the reduced pressure of the vacuum space is preferably at most 1 ⁇ 10 ⁇ 2 Pa, more preferably at most 1 ⁇ 10 ⁇ 4 Pa, and further preferably at most 1 ⁇ 10 ⁇ 5 Pa.
  • a quartz tube can be recited.
  • the vacuum space can be attained by using one or more vacuum pumps, depending upon the degree of the vacuum.
  • the temperature inside the closed space in the present invention is set to a temperature at which the SWCNTs are formed from the organic dehydrated alcohol, and that temperature is preferably 600 to 900° C., and more preferably 700 to 800° C. Such temperature conditions are ordinarily set by raising the temperature in the state that the metal catalyst is introduced into the closed space.
  • the organic dehydrated alcohol is contacted with the metal catalyst.
  • the organic dehydrated alcohol in the present invention includes not only an organic dehydrated alcohol in which water is completely removed, but also an organic dehydrated alcohol containing water in small amount that it is ordinarily regarded as a dehydrated alcohol. For example, those which contain at most 0.005 wt % of water are included in the organic dehydrated alcohol referred to in the present invention.
  • the kind, etc. of the organic dehydrated alcohol used in the present invention are not particularly specified, and two or more kinds of the mixed alcohols suffice.
  • the organic dehydrated alcohol used in the present invention mention may be made of, for example, methanol, ethanol, n-propanol, iso-propanol, n-butanol, iso-butanol, sec-butanol, tert-butanol, n-pentanol, iso-pentanol, n-amyl alcohol, iso-amyl alcohol, n-hexanol, n-heptanol, n-octanol, n-nonylalcohol, n-decanol, etc.
  • the organic dehydrated alcohol including at least one kind selected from methanol, ethanol and iso-propanol as a main component is preferable, and one including ethanol as the main component is more preferable.
  • the main component means a component having the maximum content proportion as calculated by weight, and preferably amounting to at least 99.5 wt %.
  • the pressure at which the organic dehydrated alcohol is contacted with the catalyst is preferably 1 Pa to 100 kPa, and more preferably 100 Pa to 40 kPa, and further preferably 1 kPa to 4 kPa.
  • the organic dehydrated alcohol is contacted with the catalyst.
  • the catalyst used in the present invention is not particularly limited, and one or more kinds of the catalysts may be used together.
  • the metal catalyst is preferable. More specifically, the metal catalyst is at least one kind of Fe, Co, Ni, Mo, Pt, Pd, Rh, Ir, Y, La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er and Lu and their oxides, and Co and Fe are more preferable.
  • Fe/Co, Fe/Mo, Co/Mo, Fe/Ti, Fe/TiO 2 , Fe/Al, Fe/Al 2 O 3 , Co/Ti, Co/TiO 2 , Co/Al, and Co/Al 2 O 3 are preferable.
  • the catalyst used in the present invention is preferably deposited on the substrate.
  • a resist method, a dip coating method or the like can be employed.
  • any one of a negative type electron beam resist (for example, a method described in JAPP 43 (2004) 1356) and a positive type electron beam resist (for example, a method described in J. AM. CHEM. SOC. 127 (2005) 11942) is preferable, and the positive type electron beam resist is more preferable.
  • the catalyst is vapor deposited on a portion of the substrate where the resist is removed. At this time, it is preferable angularly to vapor and deposit the catalyst. This measure is preferably employed, because it can provide a catalyst pattern smaller than an actual pattern.
  • the resist method is preferably for a case where a single CNT is grown on the substrate.
  • a catalyst layer is formed by dipping a substrate into a solution containing a catalyst.
  • the amount of the catalyst can be regulated by adjusting the concentration of the catalyst in the catalyst-containing solution.
  • the dip coating method is preferable in a case where fine catalyst particles are formed on the entire surface of the substrate.
  • the substrate can be appropriately selected depending upon the use, etc. of the SWCNTs produced, and is preferably silicon, SiO 2 , and Al 2 O 3 .
  • the surface of the substrate may be oxidized before the catalyst is deposited. This treatment is preferably employed, because it is likely to suppress the formation of a silicide of the catalyst metal.
  • any carrier may be provided between the substrate and the catalyst.
  • the inside of the closed space is preferably washed before the organic dehydrated alcohol is contacted therewith.
  • the closed space is preferably cleaned by oxygen cleaning, ozone cleaning, plasma cleaning, vacuum thermal cleaning or the like.
  • the oxygen cleaning, the ozone cleaning, and the plasma cleaning are preferable.
  • the pressure of the cleaning gas in the case of the cleaning with oxygen, the ozone cleaning, and the plasma cleaning is preferably 1 to 100 kPa, and more preferably 1 to 3 kPa.
  • the pressure of the cleaning gas in the case of the vacuum thermal cleaning is preferably at most 1 Pa, and more preferably at most 6.6 ⁇ 10 ⁇ 4 Pa.
  • the temperature on cleaning is preferably 500 to 1000° C., and more preferably 800 to 1000° C.
  • the SWCNTs can be produced in the state that the probability that the single-wall carbon nanotube grows from one particle is high (the above probability being also called “growth rate” in some cases in this specification).
  • the growth rate in the producing method of the present invention can be preferably at least 50%, more preferably at least 60%, further preferably at least 80%, and further more preferably 100%.
  • a SWCNT can be grown long. Meanwhile, how long a SWCNT grows is called “growth efficiency” in some case in the present specification.
  • the SWCNT having a length of preferably at least 50 nm, more preferably at least 1000 nm, further preferably at least 3000 nm can be obtained.
  • the diameters of the SWCNTs can be 0.5 to 1.7 mm, and further can be 0.5 to 1.2 nm.
  • the SWCNTs can be synthesized vertically to the substrate.
  • variations in the configurations of the SWCNTs obtained can be reduced.
  • at least 60% (preferably at least 80%) of the SWCNTs can be adjusted to fall in a diameter range of 0.5 to 1.5 nm.
  • the SWCNTs grown according to the method of the present invention can be preferably used as a post-silicon material for field-effect transistors and the like, probes for scanning type probe microscopes, field-emission type electron sources, etc.
  • the SWCNTs can be grown vertically to the carrier in the form of the substrate, they can be expected to be applied to the field-emission type electron source.
  • PMMA Polymethylmethacrylate
  • a silicon substrate of which had been thermally oxidized hereinafter called also “thermally oxidized silicon substrate” in some cases
  • spin coating thereby obtaining a thin film of about 50 nm.
  • rectangular patterns having sizes of 20 to 60 nm were formed by electron beam lithography.
  • Co was deposited, in the average thickness of 0.1 nm, on the resultant by vacuum deposition, and Co patterns were formed by a lift-off technique with acetone.
  • a chemical vapor deposition apparatus constituted by a quartz tube, an electric furnace, a rotary pump and a turbo molecular pump as shown in FIG. 1 was used.
  • Heat treatment was carried out, while an oxygen gas was being flown to clean the interior of the quartz tube and a quartz boat.
  • the quartz tube was vacuum evacuated down to 2 Pa (coarse sucking) by the rotary pump, and then while the oxygen gas was being flown at a flow rate of 0.5 l/min., the tube was heated up to 800° C., and thermally treated at 800° C. for 10 minutes. At that time, the pressure was adjusted by switching a valve to a needle valve so that the inner pressure of the quartz tube might be about 2.7 kPa.
  • the oxygen gas was stopped, the quartz tube was cooled, while the tube was being evacuated to vacuum by the turbo molecular pump.
  • the oxygen gas used was at a G1 grade (99.99995%). Cleaning can be also performed by the oxygen plasma cleaning, the ozone cleaning or the like.
  • a thermally oxidized silicon substrate on which the catalyst metal of Co was formed in a discrete fashion was placed on the quartz boat, the boat was placed in the heating furnace, the interior of the quartz tube was vacuum evacuated down to 6.6 ⁇ 10 ⁇ 4 Pa by using the rotary pump and the turbo molecular pump, and the temperature was raised from room temperature up to 800° C. in about 15 minutes. After the temperature reached the growing temperature, waiting was done for 10 minutes so that the temperature might be stabilized. At that time, the inner pressure of the quartz tube was 6.0 ⁇ 10 ⁇ 5 Pa (the pressure of the closed space at the time of contracting the organic dehydrated alcohol).
  • dehydrated ethanol for organic synthesis (water content: at most 50 ppm, manufactured by Wako Pure Chemical Industries, Ltd.) (pressure at the time of introduction: 6.6 ⁇ 10 ⁇ 5 Pa) was introduced into the quartz tube, and SWCNs were grown in the closed quartz tube at the inner pressure of 1.5 kPa (the pressure at which the organic dehydrated alcohol contacts with the catalyst) for 1 minutes. Thereafter, while the interior of the quartz tube was being evacuated to vacuum using the rotary pump and the turbo molecular pump, the furnace was cooled, and then the substrate was taken outside, thereby obtaining SWCNTs. The pressure inside the quartz tube immediately before taking the sample outside was 9.3 ⁇ 10 ⁇ 5 Pa.
  • FIGS. 2 to 4 A photograph of the SWCNTs obtained was taken by means of an atomic force microscope (AFM). Results are shown in FIGS. 2 to 4 .
  • FIG. 3 is an enlarged photograph of a part of FIG. 2
  • FIG. 4 is an enlarged photograph of a part of FIG. 3 .
  • FIG. 6 and FIG. 7 show results in the Raman spectroscopic analysis (excitation wavelength: 488 nm) of a single SWCNT obtained. It was also confirmed that the ratio (G/D) between the height of a peak near 1590 cm ⁇ 1 and that of a peak near 1350 cm ⁇ 1 was 9.2 in FIG. 6 and that since a peak was observed near 164 cm ⁇ 1 in FIG. 7 , a SWCNT having a high quality was synthesized.
  • Catalyst patterns were formed according to a method described in Chem. Phys. Lett. 403 (2005) 320. Specifically, two kinds of solutions were prepared, which had cobalt acetate tetrahydrate and molybdenum acetate dissolved in an ethanol solutions each in an amount of 0.01 wt %, respectively (cobalt acetate solution and molybdenum acetate solution).
  • a thermally oxidized silicon substrate was dipped in the molybdenum acetate solution, then thermally treated at 400° C. in air for 5 minutes, successively dipped in the cobalt acetate solution, and thereafter thermally treated at 400° C. in air for 5 minutes. Thereby, catalyst patterns in which a catalyst of Co/Mo is deposited on a surface of the substrate at a high density were obtained.
  • SWCNTs were grown in the same manner as in Example 2, except that the organic synthesis ethanol was replaced by a special-grade ethanol (manufactured by Kanto Chemical Co., Ltd.) having 0.4% of water at the maximum.
  • the sectional photograph of the obtained SWCNTs taken by the SEM revealed that they did not grow vertically to the substrate, but hugging the substrate as shown in FIGS. 10 and 11 , while no vertical growth was observed unlike the present invention.
  • SWCNTs were grown in the same manner as in Example 2, except that the interior of the quartz tube was not cleaned. Although the SWCNTs obtained were inferior to those in Example 2, the better SWCNTs were obtained in Example 3 as compared with Comparative Examples 1 and 2.
  • SWCNTs were grown in the same manner as in Example 2, except that instead of the vacuum evacuation of down to 6.6 ⁇ 10 ⁇ 4 Pa, the temperature was raised, while argon gas was filled inside the quartz tube at 0.3 SLM and a pressure of 40 kPa under controlling and that before growing, the interior of the quartz tube was vacuum evacuated to 2 Pa through its one end by the rotary pump.
  • the sectional photograph of the obtained SWCNTs taken by the SEM revealed that they did grow not vertically to the substrate, but hugging the substrate as shown in FIGS. 12 and 13 . Thus, it was recognized that no vertical growth was observed unlike the present invention.
  • Example 2 the interior of the quartz tube was evacuated to vacuum, and the temperature was raised to 800° C., while the pressure was kept at around 2 Pa, and then SWCNTs were grown at 2 Pa.
  • a sectional photograph of the obtained SWCNTs taken by the SEM confirmed that although the SWCNTs obtained were inferior to those in Example 2, the better SWCNTs were obtained in Example 4 as compared with Comparative Examples 1 and 2.
  • the SWCNTs having excellent growth efficiency and growth rate could come to be produced by employing the SWCNT producing method of the present invention. Further, the SWCNTs could come to be grown vertically to the substrate by employing the producing method of the present invention.

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US8591858B2 (en) * 2008-05-01 2013-11-26 Honda Motor Co., Ltd. Effect of hydrocarbon and transport gas feedstock on efficiency and quality of grown single-walled nanotubes
US9174847B2 (en) * 2008-05-01 2015-11-03 Honda Motor Co., Ltd. Synthesis of high quality carbon single-walled nanotubes
JP2010030837A (ja) * 2008-07-29 2010-02-12 Denso Corp Ｃｎｔ合成用基板、ｃｎｔ、及びそれらの製造方法
JP2010208918A (ja) * 2009-03-12 2010-09-24 Hitachi Zosen Corp Ｃｖｄ副生物の除去方法
JP2020029385A (ja) * 2018-08-23 2020-02-27 学校法人 名城大学 単層カーボンナノチューブの製造方法
CN111841561A (zh) * 2020-07-09 2020-10-30 江西铜业技术研究院有限公司 一种生长碳纳米管的高效催化剂及其制备和使用方法

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US20050079118A1 (en) * 2002-02-13 2005-04-14 Shigeo Maruyama Process for producing single-walled carbon nanotube, single-walled carbon nanotube, and composition containing single-walled carbon nanotube
US20060024227A1 (en) * 2003-10-16 2006-02-02 Shigeo Maruyama Array of single-walled carbon nanotubes and process for preparaton thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050079118A1 (en) * 2002-02-13 2005-04-14 Shigeo Maruyama Process for producing single-walled carbon nanotube, single-walled carbon nanotube, and composition containing single-walled carbon nanotube
US20060024227A1 (en) * 2003-10-16 2006-02-02 Shigeo Maruyama Array of single-walled carbon nanotubes and process for preparaton thereof

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