WO2003082738A1 - Procédé permettant de préparer un nanotube de carbone monocouche - Google Patents

Procédé permettant de préparer un nanotube de carbone monocouche Download PDF

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Publication number
WO2003082738A1
WO2003082738A1 PCT/JP2003/003884 JP0303884W WO03082738A1 WO 2003082738 A1 WO2003082738 A1 WO 2003082738A1 JP 0303884 W JP0303884 W JP 0303884W WO 03082738 A1 WO03082738 A1 WO 03082738A1
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Prior art keywords
metal
walled carbon
based catalyst
producing
crystal substrate
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PCT/JP2003/003884
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English (en)
Japanese (ja)
Inventor
Sumio Iijima
Masako Yudasaka
Hiroo Hongoh
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Japan Science And Technology Agency
Nec Corporation
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Priority to US10/509,575 priority Critical patent/US20050106093A1/en
Publication of WO2003082738A1 publication Critical patent/WO2003082738A1/fr

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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
    • 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
    • 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
    • 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
    • C01B2202/36—Diameter

Definitions

  • the invention of this application relates to a method for producing single-walled carbon nanotubes. More specifically, the invention of this application is directed to the production of single-walled carbon nanotubes that can produce single-walled carbon nanotubes by controlling the diameter without requiring a porous material or catalyst fine particles as a catalyst carrier. It is about the method. Background art
  • the chemical vapor reaction (CVD) method As a method for producing high-quality single-walled carbon nanotubes (SWNTs) with high utility value in various industries, the chemical vapor reaction (CVD) method has been attracting attention. This is because this CVD method is capable of mass production of SWNTs, and has the potential to control the gas phase pyrolysis growth of SWNTs by manipulating the type of catalyst and its particle size. This is because it is a method to have.
  • SWNTs can be obtained by heating at J. H. Hafner et al. Report that SWNTs grow by flowing CO gas over nanometer-sized metal particles supported on alumina nanoparticles and heat-treating them.
  • salts of Fe and / or Mo were used as metal-based catalysts and alumina nanoparticles were used as their supports.
  • SWNTs can be produced by using a porous material such as zeolite, silica, or anodized silicon as a carrier for the production of SWNTs by another chemical vapor reaction. .
  • the invention of this application has been made in view of the circumstances described above, and does not require nanoparticles or a porous material as a carrier, and furthermore, manufactures single-walled carbon nanotubes by controlling the diameter. It is an object of the present invention to provide a method for producing a single-walled carbon nanotube that can be used. Disclosure of the invention
  • the invention of this application relates to a metal-based catalyst having a catalytic action in producing graphite, and a single-crystal substrate having a correspondence with the crystal grain size and crystal orientation of the metal-based catalyst.
  • a metal-based catalyst is dispersed in this single-crystal substrate, and a carbon material is supplied in a temperature range of 500 or more to obtain a single-layer carbon.
  • the invention of this application is a method for producing single-walled carbon nanotubes, which comprises using a single-crystal substrate coated with a metal-based catalyst thin film in the above-mentioned invention.
  • the method for producing single-walled carbon nanotubes characterized in that the thickness of the catalyst thin film is 0.1 to 10 nm or less.Fourth, the metal-based catalyst is composed of iron group, platinum group, rare earth metal,
  • a method for producing a single-walled carbon nanotube characterized by being a transition metal or a mixture of two or more of any of these metal compounds.
  • the method for manufacturing a single layer forces one carbon nanotube that wherein a stable material above at 0, the sixth, the single crystal substrate, Safuai ⁇ (a 1 2 0 3), silicon (S i) , to characterized in that either S i ⁇ 2, S i C, M g O
  • a method for producing single-walled carbon nanotubes characterized by using hydroxyapatite instead of a single-crystal substrate
  • a metal-based catalyst A method for producing a single-layer carbon nanotube, characterized in that a single-wall carbon nanotube having a diameter controlled by a combination of a substrate and a single-crystal substrate and a crystal plane thereof is grown by vapor phase pyrolysis.
  • the single-walled carbon nanotubes are characterized in that the combination of the metal-based catalyst and the single-crystal substrate and its crystal plane is any one of A, R, and C planes of Fe and sapphire.
  • the first method is a method for producing a single-walled carbon nanotube, wherein the carbon raw material is a carbon-containing substance that is a gas at 500 or more. Is the carbon Fee, provide methane, ethylene, Fuenatoren, a process for producing single-walled carbon nanotubes, wherein either benzene.
  • Fig. 1 shows the SEM of the deposit grown at 800 on the (a) A-plane, (b) R-plane, and (c) C-plane of sapphire coated with a 2 nm thick Fe thin film. It is the photograph which illustrated the image.
  • Figure 2 shows the SEM of the deposit grown at 800 on the (a) A-plane, (b) R-plane, and (c) C-plane of sapphire coated with a 5 nm thick Fe thin film. It is the photograph which illustrated the image.
  • FIG. 3 is a photograph illustrating a TEM image of a deposit grown on (a) A (2 nm), (b) R (2 nm), and (c) C (5 nm).
  • Fig. 4 shows the Raman scattering spectrum of the single-walled carbon nanotubes manufactured in the example, in the range of (a) to 500 cm- 1 and (b) in the range of 1200 to 180 cm- 1 .
  • the method for producing single-walled carbon nanotubes has a correspondence relationship between a metal-based catalyst having a catalytic action in producing graphite, and the crystal grain size and crystal orientation of the metal-based catalyst.
  • a metal-based catalyst is dispersed in the single-crystal substrate, and a carbon material is supplied in a temperature range of 500 or more, so that single-walled carbon nanotubes are grown by gas phase thermal decomposition. It is characterized by
  • the metal-based catalyst various metals having a catalytic action in the production of graphite, that is, in the gas phase pyrolysis growth of single-walled carbon nanotubes can be used.
  • iron group such as Ni, Fe, Co, etc.
  • platinum group such as Pd, Pt, Rh
  • rare earth metal such as La, Y, or Mo, Mn, etc.
  • the single crystal substrate it is possible to use one made of stable each class of materials in the above process temperature 5 0 0, for example, Safuai ⁇ (A 1 2 0 3), silicon (S i), S i 0 2 , S i C, M g O and the like can be exemplified. These need not be porous structures or nanoparticles as in the past, but may be, for example, planar ones. In the invention of this application, columnar crystals such as hydroxyapatite can be used instead of these single crystal substrates.
  • the metal-based catalyst and the single-crystal substrate have a certain relationship, and are formed by a solid-phase reaction such as precipitation and recrystallization of the metal-based catalyst at a processing temperature of 500 ⁇ or more.
  • a combination with a single crystal substrate that has an effect on the crystal grain size of the recrystallized grains and the correspondence of the crystal orientation between adjacent unrecrystallized grains can be used.
  • the crystal grain size of the metal-based catalyst is controlled in a range of about 0.1 to 10 nm, or Further, it is desirable that the relationship is such that the crystal plane of the metal-based catalyst has an effect of orienting the crystal plane with respect to the single crystal substrate.
  • a combination of such a metal-based catalyst and a single crystal substrate a combination of Fe and sapphire can be exemplified as a preferable combination.
  • the dispersion of the metal-based catalyst on the single-crystal substrate can be realized by uniformly dispersing the fine particles of the metal-based catalyst or by coating the single-crystal substrate with a metal-based catalyst thin film. .
  • the latter method is preferred because it is simple in the actual manufacturing process.
  • Various methods can be used for these dispersion methods. Specifically, for example, a vacuum deposition method, a sputtering method, etc.
  • a wet process such as a lye process, a solution dripping method, a spray coat method, or a spin coat method can be used.
  • the amount of the metal-based catalyst dispersed in the single-crystal substrate is not particularly limited, and may be arbitrary. For example, on a single crystal substrate
  • the temperature of the single crystal substrate in which the metal-based catalyst is dispersed is set to 500 or more, and then a carbon raw material is supplied.
  • the heating of the single crystal substrate to a temperature of 500 or more can be performed in an inert atmosphere.
  • the carbon raw material various carbon-containing substances which are gaseous at a temperature of 500 or more can be used. More specifically, for example, methane (CH 4 ), ethylene (C 2 H 4 ), carbon monoxide (CO), etc. are gaseous at room temperature, and solid or liquid at room temperature, such as phenathrene or benzene. In this case, it is possible to exemplify a material which is a gas at a temperature of 500 or more by heating.
  • single-walled carbon nanotubes can be grown by vapor phase pyrolysis on the surface of the single-crystal substrate.
  • the metal catalyst and the single crystal substrate As a result of conducting a more detailed study focusing on the interaction between the metal catalyst and the single-crystal substrate, the interaction between the metal-based catalyst and the single-crystal substrate It has been found that the crystal plane of the substrate can also be taken into consideration, and furthermore, the diameter of the single-walled carbon nanotube generated by the combination can be controlled to a specific diameter. The ability to control the diameter in the vapor phase pyrolysis growth of single-walled carbon nanotubes has not been known at all, and is realized for the first time by the inventors of the present application.
  • the method for producing single-walled carbon nanotubes is a method of producing single-walled carbon nanotubes whose diameter is controlled by a combination of a metal-based catalyst, a single-crystal substrate and its crystal plane. It is characterized by being thermally decomposed and grown.
  • the combination of Fe and sapphire which is a combination of the above-described preferred metal-based catalyst and single crystal substrate, is further combined with any combination of Fe and sapphire with the A-plane, R-plane, or C-plane.
  • the single-walled carbon nanotubes controlled to have different diameters for each of these combinations can be grown by gas phase pyrolysis.
  • the diameter of the growing single-layer bonano tube is 1.43 nm, 1.30 ⁇ m for A-plane, 1.20 nm, 1.45 nm, 1.24 nm, 1.18 nm for R-plane, 1.49 nm, 1.31 nm, 1.18 nm for C-plane It will be controlled to a specific value.
  • the yield of single-walled carbon nanotubes can be increased by controlling the thickness of the metal-based catalyst thin film for each crystal plane of the single-crystal substrate. More specifically, for example,
  • the yield of single-walled carbon nanotubes is within the above range for the A-plane and R-plane.
  • single-walled carbon nanotubes have various symmetry (chirality).
  • the chirality of the single-walled carbon nanotube can be expressed by the chirality index (m, n), and has a strong correlation with the diameter of the single-walled carbon nanotube. This suggests that the method of the present invention can control not only the diameter of the single-walled carbon nanotube but also the power irritation.
  • the interaction between the metal-based catalyst and the single-crystal substrate material plays an important role in the vapor-phase pyrolysis growth of single-walled carbon nanotubes.
  • a dispersed single crystal substrate single-walled carbon nanotubes can be grown by gas phase pyrolysis.
  • a single-walled carbon nanotube having a controlled diameter can be produced.
  • the yield of single-walled carbon nanotubes can be increased by adjusting the crystal plane of the single-crystal substrate and the thickness of the catalyst thin film.
  • methane (9.999%) as a carbon raw material was introduced at a flow rate of 0.61 / min. The introduction of methane was performed for 5 minutes, and then the argon was introduced again, and the tube furnace was cooled until it reached room temperature.
  • the heat-treated substrate was examined in detail by scanning electron microscope (SEM) observation, Raman spectroscopy, and transmission electron microscope (TEM) observation.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • the sample for SEM observation was covered with a Pd-Pt thin film of about 2 nm in thickness for clearer observation.
  • the Raman spectrum was obtained by measurement using 488 nm light (30 mW) from an Ar laser with a focused spot size of ⁇ 1 m.
  • Samples for TEM observation were prepared by collecting sediments from a sapphire substrate, dispersing them in ethanol, dropping them on TEM grids, and drying.
  • Figures 1 (a), (b), and (c) show the S of the deposit grown at 800 on the A, R, and C planes of sapphire coated with a 2-nm-thick Fe thin film. EM images are shown. It was clearly observed that the amount of tubular sediment deposited on the A-side was greater than that on the R-side. The amount of tubular sediment on the C-plane was found to be the least of the three.
  • Figures 2 (a), (b), and (c) show deposits grown at 800 on the A, R, and C planes of sapphire coated with a 5-nm thick Fe thin film. The SEM image of each was shown. It was confirmed that tubular deposits similar to the above were formed on all three surfaces. These capillaries are either thick and short (20-50 nm in diameter, about 1 mm in length) or thin and long (less than 3 nm in diameter, more than 2 mm in length). I found it.
  • Figure 3 (a) shows a TEM image of the deposit grown on a sapphire surface (hereinafter referred to as A (2 nm)) coated with a 2 nm-thick Fe thin film.
  • a (2 nm) was found to contain SWNT s and a very small amount of amorphous carbon (hereinafter a-C).
  • R (2 nm) was coated with a 2 nm-thick Fe thin film shown in Fig. 3 (b)
  • R (2 nm) Is composed of SWNTs and a—C.
  • Figures 4 (a) and 4 (b) show the Raman scattering spectra of the deposits formed on the A, R, and C planes of sapphire covered with the 2-nm, 3-nm, and 5-nm-thick Fe thin films. .
  • peaks were observed at about 1592 cm- 1 and 1570 cm- 1 and 1 to 4 narrow peaks were observed in the range of 100 to 230 cm- 1 . These peaks are characteristic of SWNTs and indicate the presence of SWNTs in sediments.
  • About 1 5 9 2 cm—1 5 7 0 c m-1 peak corresponds to the tangential mode, 1 0 0 ⁇ 2 3 0 cm one first peak between is equivalent to the Raman breathing mode (RBM) of SWNT s.
  • RBM Raman breathing mode
  • SWNT s formed on the R (2 nm) plane has a strong RBM peak at 167 cm- 1 indicating SWNT Ts with a diameter of 1.4 nm. Although there is a weak peak at 203 cm- 1 indicating that it is a SWNT s of 1.2 nm, these peaks are not so prominent for a sample covered with a thicker Fe thin film. It turns out there is no.
  • the amount of SWNTs generated for the A-plane and R-plane decreases. I understand.
  • the SWNT amount was found to increase as the thickness of the Fe thin film increased from 2 nm to 5 nm.
  • the peak positions and RBM intensities of these SWNTs were different in individual sediments.
  • the width of the RBM peak was as narrow as approximately 7 to 12 cm- 1
  • the number of peaks was 1 to 4
  • the peak position was found to depend on the sapphire surface. More specifically, for example, for the A (2 nm) plane, the R (2 nm) plane, and the C (2 nm) plane, the average of the Raman spectra obtained from 10 locations is averaged, and the RBM peak is calculated.
  • Table 1 shows the diameters of the SWNTs obtained.
  • a silicon wafer provided with a mixture of F e (NO 3) 3 ⁇ ⁇ 20 and alumina nanoparticles (no Mo (acac) 2 ) was prepared as a substrate, and the same heat treatment as in the above example was performed. Was performed, and SWNTs were generated.
  • the Raman spectrum obtained for this SWNTs is also shown in FIG. This Raman spectrum has a broad RBM peak in the range of 120 to 200 cm- 1 and a wide range of SWNT s diameters of 2.0 to 1.2 nm. You.
  • alumina nanoparticles are metal-based catalyst support is the same A 1 2 ⁇ 3 and sapphire, alumina, because nanoparticles has internal various crystal faces and amorphous characteristics from the shape of its However, it was found that SWNTs could be grown, but their diameter could not be controlled, resulting in wide distribution.
  • the present invention relates to a method for producing a single-walled carbon nanotube. More specifically, the invention of this application relates to a method for producing a single-walled carbon nanotube capable of producing a single-walled carbon nanotube by controlling the diameter without using a porous material or catalyst fine particles. Provided.

Abstract

L'invention concerne un procédé permettant de préparer un nanotube de carbone monocouche. Ce procédé consiste à utiliser en combinaison un catalyseur métallique présentant une fonction catalytique dans la formation de graphite, et un substrat monocristallin présentant une certaine correspondance avec le catalyseur métallique du point de vue la taille du grain cristallin, et de l'orientation des cristaux formés par recristallisation à la température de traitement, à disperser le catalyseur métallique sur le substrat monocristallin, à introduire une matière première composée de carbone sur le substrat à une température égale ou supérieure à 500°, afin de former un nanotube de carbone monocouche par décomposition thermique en phase vapeur. Ce procédé permet la préparation d'un nanotube de carbone monocouche présentant un diamètre sélectionné sans nécessiter un support de catalyseur en matériau poreux ou un catalyseur en particules fines. Les combinaisons décrites de catalyseur métallique et de substrat monocristallin comprennent notamment le Fe associé à un substrat de saphir.
PCT/JP2003/003884 2002-03-29 2003-03-27 Procédé permettant de préparer un nanotube de carbone monocouche WO2003082738A1 (fr)

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JP2002097768A JP3537811B2 (ja) 2002-03-29 2002-03-29 単層カーボンナノチューブの製造方法

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