WO2007099975A1 - Ensemble de nanotubes de carbone, fibre de nanotubes de carbone et procede de production de fibre de nanotubes de carbone - Google Patents

Ensemble de nanotubes de carbone, fibre de nanotubes de carbone et procede de production de fibre de nanotubes de carbone Download PDF

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Publication number
WO2007099975A1
WO2007099975A1 PCT/JP2007/053693 JP2007053693W WO2007099975A1 WO 2007099975 A1 WO2007099975 A1 WO 2007099975A1 JP 2007053693 W JP2007053693 W JP 2007053693W WO 2007099975 A1 WO2007099975 A1 WO 2007099975A1
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Prior art keywords
carbon nanotube
carbon
aggregate
carbon nanotubes
ratio
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PCT/JP2007/053693
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English (en)
Japanese (ja)
Inventor
Nobuyuki Taniguchi
Kouji Kita
Masaki Nishimura
Tomoyuki Akai
Osamu Suekane
Atsuko Nagataki
Makoto Horiguchi
Hironobu Hori
Yoshikazu Nakayama
Original Assignee
Toyo Boseki Kabushiki Kaisha
Osaka Prefectural Government
Osaka University
The Kansai Electric Power Co., Inc.
Osaka Industrial Promotion Organization
Public University Corporation Osaka Prefecture University
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Application filed by Toyo Boseki Kabushiki Kaisha, Osaka Prefectural Government, Osaka University, The Kansai Electric Power Co., Inc., Osaka Industrial Promotion Organization, Public University Corporation Osaka Prefecture University filed Critical Toyo Boseki Kabushiki Kaisha
Priority to JP2008502808A priority Critical patent/JP4968854B2/ja
Publication of WO2007099975A1 publication Critical patent/WO2007099975A1/fr

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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
    • 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
    • C01B32/168—After-treatment

Definitions

  • Carbon nanotube aggregate, carbon nanotube fiber, and carbon nanotube fiber manufacturing method Carbon nanotube aggregate, carbon nanotube fiber, and carbon nanotube fiber manufacturing method
  • the present invention relates to a carbon nanotube aggregate, a carbon nanotube fiber, and a method for producing a carbon nanotube fiber.
  • Carbon nanotubes are excellent in electrical characteristics, mechanical characteristics, and the like, and are expected to be used and applied in various industries including field emission displays.
  • Non-patent Documents 1 and 2 fibers composed of carbon nanotubes and carbon nanotube sheets using the same have been proposed.
  • Non-Patent Document 1 carbon nanotube aggregates (also called “carbon nanotube forest”) grown on a substrate with high density and high orientation by chemical vapor deposition are used. A method for forming nanotube fibers is disclosed.
  • Non-Patent Document 2 proposes a method of forming a carbon nanotube sheet from an aggregate of carbon nanotubes grown in a high density and high orientation on a substrate by a chemical vapor deposition method.
  • Non-Patent Document 1 Zhang et al., Science, 306, 1358-1361, 2004
  • Non-Patent Document 2 Zhang et al., Science, 309, 1215-1219, 2005
  • an object of the present invention is to provide a carbon nanotube aggregate from which a long carbon nanotube fiber can be pulled out with high probability, a carbon nanotube fiber obtained from the aggregate, and the like.
  • the present inventors have intensively studied to solve the above problems. As a result, contrary to the method that has been actively performed in recent years, it is an aggregate of carbon nanotubes that is not highly crystallized and in which a large amount of amorphous carbon is laminated, and has a specific structure. As a result, it was found that long carbon nanotube fibers can be pulled out with an excellent probability by using the aggregate of carbon nanotubes, and the present invention (Embodiment 1) was completed. In addition, even if a large amount of amorphous carbon is not laminated, it has been subjected to a predetermined treatment, and even by using a carbon nanotube aggregate having a specific structure, it is long with an excellent probability. The inventors have found that carbon nanotube fibers can be pulled out, and have completed the present invention (Embodiment 2). That is, the present invention relates to the following.
  • Item 1 A carbon nanochu having a plurality of carbon nanotubes formed on a substrate (1) Amorphous carbon is laminated on the surface of the carbon nanotube at a coverage of 55 to 100%, and (2) the average thickness of the amorphous carbon is 0.3 to 5 nm. (3) The order parameter of the aggregate of carbon nanotubes is 0.85 to 1.0, (4) The bulk density of the aggregate of carbon nanotubes is 1 to:! OOOmgZcm 3 and (5) (6) In the Raman spectrum of the carbon nanotube aggregate, the G band that appears near 1590c ⁇ 1 and the lSSOcnT 1 vicinity An aggregate of carbon nanotubes, characterized in that the area ratio (G / D ratio) to the appearing D band is 0.45 to 0.75.
  • Item 2 A carbon nanotube fiber obtained by drawing a plurality of carbon nanotube aggregates according to Item 1 from the substrate in a continuous manner.
  • Item 3 The carbon nanotube fiber according to Item 2, which is formed by twisting.
  • Item 4 The carbon nanotube fiber according to Item 2 or 3, further comprising a binder.
  • Item 5 A carbon nanotube cross-layered product comprising the carbon nanotube fibers according to any one of Items 2 to 4.
  • Item 6 The carbon nanotube cross-layered product according to Item 5, further comprising a binder.
  • Item 7 A carbon nanotube aggregate in which a plurality of carbon nanotubes are formed on a substrate, wherein ( a ) a polarization treatment is applied, and (b) the order parameter of the carbon nanotube aggregate. Is from 0.85 to 1.0, and (c) the density of the carbon nanotube aggregate is:! To 1000 mg / cm 3 , and (d) the number of oxygen / carbon atoms in the carbon nanotube aggregate. (E) The area ratio between the G band that appears near ⁇ ⁇ 1 and the D band that appears near lSSOcnT 1 (G / D) The carbon nanotube assembly is characterized in that the ratio is 0.45-0.60.
  • Item 8 The aggregate of carbon nanotubes according to Item 7, wherein the polarization treatment is an oxidation treatment.
  • Item 9 The aggregate of carbon nanotubes according to Item 8, wherein the oxidation treatment is a plasma treatment.
  • Item 10 A method for producing a long carbon nanotube fiber, wherein a plurality of the carbon nanotube assemblies are bowed from an end surface of the carbon nanotube assembly according to any one of Items 1 and 7-9. I pull out the long carbon nanotube fiber continuously A method for producing a carbon nanotube fiber comprising a forming step.
  • the carbon nanotube aggregate that is Embodiment 1 of the present invention is a carbon nanotube aggregate in which a plurality of carbon nanotubes are formed on a substrate,
  • Amorphous carbon is laminated on the surface of the carbon nanotube with a coverage of 55-100%
  • the average thickness of the amorphous carbon is 0.3-5 nm
  • the oxygen-to-carbon atom ratio of the carbon nanotube aggregate is 0.002 to 0.350
  • a known or commercially available substrate can be used without limitation.
  • a plastic substrate; a glass substrate; a silicon substrate; a metal substrate containing a metal such as iron or copper or an alloy thereof can be used.
  • a silicon dioxide film may be laminated on the surface of these substrates.
  • a plurality of carbon nanotubes stand on a substrate in high density and high orientation.
  • the carbon nanotubes formed on the substrate have amorphous carbon (amorphous component) laminated on the surface with an average coverage of 55 to 100%, and the average thickness of the laminated amorphous carbon. Is 0.3 to 5 nm. Because of these characteristics, the surface of the carbon nanotube of the present invention has minute irregularities that become the hooking force part, and when pulled out (carbon nanotube During the manufacture of the fiber, it is possible to increase the force similar to the frictional force between adjacent carbon nanotubes. As a result, it exhibits excellent pull-out properties, and long carbon nanotube fibers can be easily obtained.
  • the coverage is preferably 57 to 90%. As a result, it is possible to exert an excellent pull-out characteristic while suppressing a decrease in physical properties (high conductivity, high strength, etc.) inherent to the carbon nanotube.
  • the average thickness of the amorphous carbon is preferably 0.7 to 2 nm. The coverage and average thickness of the amorphous carbon can be confirmed by observing an image (magnification: about 6 million times) obtained by a transmission electron microscope (TEM).
  • the carbon nanotube preferably has a plurality of bent portions. Preferably, there are about 20 or more per carbon nanotube, more preferably about 50 to about 1000 per one. As a result, the bent portion becomes a catching portion, and the force similar to the frictional force between the adjacent carbon nanotubes is increased, so that the drawing characteristics of the carbon nanotube aggregate can be further improved.
  • the bent portion may be present at any portion with respect to the long axis direction of the carbon nanotube.
  • the carbon nanotube may be present at any of the root part (the vicinity of the substrate), the tip part (the part farthest from the substrate), and the intermediate part between the root part and the tip part.
  • the presence or absence and the number of bent portions of the carbon nanotube can be confirmed by observing an image (magnification: about 40,000 to 120,000 times) obtained by a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • the average diameter of the carbon nanotubes is not limited and is usually from lnm to about! OOnm, preferably about 5 to 50nm.
  • the average length is not limited and is preferably ⁇ ⁇ ⁇ or more. It may be a single-walled carbon nanotube or a multi-walled carbon nanotube.
  • the carbon nanotubes may contain elements other than carbon and oxygen, and may have a functional group such as a carboxyl group, a hydroxyl group, a carbonyl group, and an ether group.
  • the aggregate of carbon nanotubes of Embodiment 1 is such that the carbon nanotubes are formed in a highly oriented and high density on the substrate, and the carbon nanotube aggregates
  • the order parameter is 0 ⁇ 85 to: 1.0, the bulk density of the carbon nanotube aggregate is 1 to 1000 mg / cm 3 , and the oxygen / carbon atomic ratio of the carbon nanotube aggregate (ie, O / C ratio) is 0 - 002 to 0.350, the area ratio of the Raman spectrum of the carbon nanotube aggregate, the G band and 1350Cm- D band appearing in the vicinity of 1 appearing in the vicinity 1590cm- 1 (GZD ratio) It is 0.45-0.75.
  • carbon nanotubes are formed on a substrate in a highly oriented state.
  • High orientation means that carbon nanotubes stand adjacent to each other and are perpendicular to the substrate plane.
  • the order parameter ( ⁇ P) represented by the following formula (1) is in the range of 0.85 to 1.0 (preferably 0.90 to 0.99).
  • ⁇ j represents the angle formed by the molecular axis of an arbitrary carbon nanotube formed on the substrate and the substrate.
  • ⁇ Cos 2 (90- ⁇ j)> is defined on the substrate. (The average value of all the carbon nanotubes formed is shown.)
  • carbon nanotubes are formed on a substrate at a high density. That is, the bulk density of the carbon nanotubes on the substrate:! ⁇ 1 OOOmg / cm 3 , preferably 10 to 500 mg / cm 3, more preferably 10 to: a 100 mg / cm 3. If the bulk density is lower than this range, the interaction between the adjacent carbon nanotube molecules is weakened, and the drawing characteristics may be deteriorated. If the bulk density is larger than this range and a large amount of carbon nanotubes are pulled out at the same time when being pulled out, there is a possibility that long fibers having a uniform thickness cannot be obtained.
  • the aggregate of carbon nanotubes of Embodiment 1 has an oxygen Z-carbon atom number ratio (OZC ratio) of 0.002 to 0.350. Preferably ⁇ , 0.002 to 0.27.
  • OZC ratio oxygen Z-carbon atom number ratio
  • the O / C ratio is obtained by obtaining the peak area of carbon atoms having a binding energy of 282 to 298 eV and the peak area of oxygen atoms having 526 to 540 eV in a spectrum obtained by photoelectron spectroscopy (ESCA). These values can be calculated by taking into consideration the peak areas and sensitivity correction values for each element.
  • the aggregate of carbon nanotubes of Embodiment 1 has an area ratio (G / D ratio) between the G band appearing near 1590 cm- 1 and the D band appearing near lSSOcnT 1 in the Raman spectrum of 0 • 45 to 0.75. It is in the range.
  • the upper limit of G / Di is 0.75 to ⁇ , preferably 0.75 to 0.60, and more preferably 0.56.
  • the G / D ratio exceeds 0.75, the catching will be insufficient and the drawing characteristics may deteriorate. On the other hand, if the G / D ratio is less than 0.45, the strength of the drawn carbon nanotube fibers may be reduced, and long carbon nanotube fibers may not be obtained.
  • absorption peak area of G-band and D-band of the present invention Ramansu Bae Kutonore 800 to 2000 cm _ 1 wavenumber region Niore Te, a line connecting the both ends of the spectrum in a straight line as a base line, 1350 cm _ 1 D band absorption peak appearing in the vicinity of the absorption peak appearing in the vicinity of 1590 cm _ 1 as G band, which is determined by performing a waveform separation by these two absorption peaks curve fitting using Lorentz function It is.
  • Figure 1 shows an example of the spectrum obtained by Raman spectroscopy.
  • the absorption peak area of the D band is indicated by the hatched portion
  • the absorption peak area of the G band is indicated by the vertical line portion.
  • the area of the G band and D band can be calculated using commercially available software (for example, origin Ver6 manufactured by Microcal Software. Inc.).
  • the G / D ratio is obtained by dividing the absorption peak area of the G band (vertical line) by the absorption peak area of the D band (shaded area).
  • the method for producing the aggregate of carbon nanotubes of Embodiment 1 is not particularly limited. For example, it can be produced by adjusting the O / C ratio, the G / D ratio, and the like within the above ranges. More specifically, by performing chemical vapor deposition using a hydrocarbon gas such as acetylene, a desired carbon nanotube aggregate can be suitably produced on the substrate.
  • a hydrocarbon gas such as acetylene
  • the substrate examples include those described above.
  • the iron is obtained by evaporating or sputtering iron on a silicon substrate coated with a silicon dioxide film by vapor deposition or thermal oxidation. It is a film laminated silicon substrate.
  • the iron film takes in carbon and makes fine particles on the substrate surface with a suitable particle size and density, so that the aggregate of carbon nanotubes formed in a high-density and highly-oriented state is formed. It can be manufactured more reliably.
  • the temperature is not limited, but is preferably 600 to 1000. About C, more preferably about 650 to 750 ° C.
  • the pressure is not limited, it is usually carried out under atmospheric pressure (preferably about 0.8 to about 1.2 atm).
  • the gas to be introduced is not limited as long as it has carbon atoms, but hydrocarbons such as acetylene can be preferably used.
  • a rare gas such as helium may be used in combination as a carrier gas.
  • the rate of increase in the concentration of the acetylene gas supplied onto the substrate at the initial stage of the carbon nanotube synthesis reaction it is particularly preferable to control the rate of increase in the concentration of the acetylene gas supplied onto the substrate at the initial stage of the carbon nanotube synthesis reaction.
  • the substrate material such as iron takes in carbon and is easily formed into fine particles on the substrate surface with an optimum particle size and density
  • the aggregate of carbon nanotubes of the present invention can be suitably manufactured.
  • the rising speed may be a force that can be appropriately set according to the manufacturing conditions, for example, about 0.01 to 0.45 vol%, preferably about 0.05 to 0. 20 vol%.
  • reaction time it is possible to control the coverage, average thickness, and the like of amorphous carbon laminated on the surface layer of carbon nanotubes.
  • the reaction time can be appropriately set depending on the production conditions, but it may be, for example, about 3 seconds to 2 hours, preferably about 15 seconds to 30 minutes.
  • the carbon nanotube aggregate of Embodiment 2 is a carbon nanotube aggregate in which a plurality of carbon nanotubes are formed on a substrate,
  • Examples of the substrate are the same as those described above in Embodiment 1. Each measurement method and the like are all the same as in the first embodiment.
  • the carbon nanotube aggregate of Embodiment 2 is subjected to a polarization treatment.
  • Polarization treatment refers to treatment for introducing a functional group such as a carboxyl group, a hydroxyl group, a carbonyl group, or an ether group into a carbon nanotube. A specific example of the polarization process will be described later. Since Embodiment 2 is subjected to this polarization treatment and has a specific structure, it exhibits excellent drawing characteristics when producing carbon nanotube fibers, and a long carbon nanotube fiber can be obtained.
  • the average diameter of the carbon nanotubes constituting the aggregate of Embodiment 2 is not limited, and is usually about lnm to about OOnm, preferably about 5 to 50nm.
  • the average length is not limited and is preferably 1 ⁇ or more. It may be a single-walled carbon nanotube or a multi-walled carbon nanotube. Further, it may contain other elements other than carbon and oxygen.
  • the carbon nanotube may have a functional group such as a carboxyl group, a hydroxyl group, a carbonyl group, or an ether group. Further, for the same reason as in the first embodiment, it is preferable to have a plurality of bent portions. Preferably, there are about 20 or more carbon nanotubes, more preferably about 50 to about 1000 carbon nanotubes.
  • the aggregate of carbon nanotubes of Embodiment 2 is such that the carbon nanotubes are formed in a highly oriented and high density state on the substrate, and the order parameter of the aggregate of carbon nanotubes is 0.85 to: 1. 0 (preferably 0.90 to 0.99) and the bulk density of the carbon nanotube aggregate is:! To lOOOOmgZcm 3 (preferably 10 to 500 mgZcm 3 , more preferably 10 to 100 mg / cm 3 ). is there. If the bulk density is smaller than this range, the interaction between the adjacent force-bonn nanotube molecules becomes weak, and the pulling-out property may be deteriorated.
  • the aggregate of carbon nanotubes of Embodiment 2 has an oxygen / carbon atomic number ratio (ie, O / Ci) force SO. 05 to 0.35. It is preferably ⁇ , 0.09 to 0.27.
  • the aggregate of carbon nanotubes of Embodiment 2 has an area ratio G / D ratio of 0.45 to 0.60 between the G band appearing near 1590 cm-1 in the Raman spectrum and the D band appearing near l S SOcnT 1 . (Preferably 0.47-0.60).
  • G / D the soot in this range, the defects introduced on the surface of the carbon nanotube and the force derived from the amorphous component are attracted by the minute irregularities on the surface of the single-bonn nanotube, and the adjacent carbon nanotube A force similar to the friction force between them can be increased. For this reason, it is possible to easily obtain a long carbon nanotube fiber exhibiting excellent drawing characteristics.
  • the method for producing the carbon nanotube aggregate of Embodiment 2 is not limited as long as the polarization treatment is performed.
  • the polarization treatment is not particularly limited as long as polarity can be imparted to the carbon nanotube, but oxidation treatment is preferable.
  • oxidation treatment include plasma treatment, acid treatment, electrolytic oxidation treatment, and dry oxidation treatment.
  • the atmosphere is not limited. Examples include oxygen, argon, nitrogen, hydrogen, ammonia, methane, and ethylene. More preferred are oxygen, argon and the like. These gases may be used alone or in combination of two or more.
  • the pressure is not limited, specifically, it is preferable to carry out under reduced pressure, and it is preferably carried out at about 0.01 to about ⁇ ⁇ rr (especially 0 ⁇ ! To lTorr).
  • the processing time of the plasma treatment may be appropriately determined according to the apparatus used, the OZC ratio before the plasma treatment, the GZD ratio, the amorphous carbon coverage, etc., for example:! To 60 minutes, preferably 5 to 20 minutes. If the processing time is extremely shortened, the effect of the processing will be reduced. On the other hand, if the treatment time is extremely long, damage to the carbon nanotubes becomes excessive, and the high strength, high conductivity, etc. of the carbon nanotubes are significantly impaired, which is preferable.
  • the output in plasma processing is as follows: equipment used, OZC ratio before plasma processing, G / D ratio, What is necessary is just to determine suitably according to the coverage of an amorphous carbon, etc., for example, 10-: 1000 w, What is necessary is just to be 100-500 w.
  • An extremely small output is not preferable because the effect of the processing is reduced.
  • the output is extremely increased, damage to the carbon nanotubes becomes excessively large, and the high strength, high conductivity, etc. of the carbon nanotubes are significantly impaired.
  • the acid treatment method is not particularly limited.
  • a known method such as treatment with a nitric acid / sulfuric acid mixture can be applied.
  • the anion species serving as the radical generation source is not limited.
  • nitrate ions can be used as the radical generation source.
  • the amount of electricity to be energized during the electrolytic oxidation treatment may be appropriately selected according to the O / C ratio, G / D ratio, amorphous carbon coverage, etc. before the electrolytic oxidation treatment. If the amount of electricity is extremely small, the effect of treatment becomes small, which is not preferable. On the other hand, an extremely large amount of electricity is not preferable because damage to the carbon nanotubes increases, and the high strength and high conductivity of the carbon nanotubes are impaired.
  • the dry oxidation treatment method is not particularly limited, and for example, a known method such as ozone-promoted oxidation treatment can be applied.
  • the aggregate of carbon nanotubes before the polarization treatment can be produced, for example, in the same manner as the aggregate of embodiment 1.
  • the carbon nanotube fiber of the present invention includes a long fiber formed by being drawn from the carbon nanotube assembly of Embodiment 1 or Embodiment 2, and carbon. It is a bundle of multiple nanotubes, and has a continuous structure.
  • the carbon nanotube fiber may be twisted or untwisted. From the viewpoint of higher strength and easy handling, twisted fibers (carbon nanotube twisted yarn) are preferred.
  • the fiber length may be appropriately determined according to the use of the final product without limitation, and the fiber length is preferably 25 cm or more, more preferably 30 cm or more.
  • the fiber diameter is not limited and may be appropriately determined according to the use of the final product.
  • the carbon nanotube fiber may contain a binder. Thereby, the strength of the carbon nanotube fiber can be further increased, and the handling becomes easy.
  • the binder is not limited as long as it binds the carbon nanotubes, and a known binder can be used. For example, polybulu alcohol etc. are mentioned.
  • the binding method is not limited, for example, after forming carbon nanotube fibers, a method of immersing the carbon nanotube fibers in a binder, a method of applying or spraying the binder on the carbon nanotube fibers, and the like.
  • the amount of binder adhering to the binder is limited and may be appropriately determined according to the type of binder to be used, the use of the final product, and the like.
  • the carbon nanotube two-dimensional structure of the present invention is formed by two-dimensionally arranging the above-described carbon nanotube fibers of the present invention.
  • the two-dimensional structure of carbon nanotubes only needs to be formed in a planar shape, and may be in any form such as a woven shape, a film shape, and a plate shape.
  • a carbon nanotube sheet in which a plurality of carbon nanotube fibers of the present invention are adjacent in parallel is preferred.
  • the two-dimensional structure of carbon nanotubes may contain a binder or the like.
  • the binder is not limited as long as it binds carbon nanotube fibers, and the above-mentioned known binders can be used.
  • the two-dimensional structure of carbon nanotubes is obtained by linearly pulling out carbon nanotubes, which may be carbon nanotubes drawn from a carbon nanotube aggregate in a planar shape.
  • carbon nanotubes which may be carbon nanotubes drawn from a carbon nanotube aggregate in a planar shape.
  • a plurality of (or knitted) carbon nanotube fibers may be obtained.
  • the carbon nanotube two-dimensional structure of the present invention is formed in combination with a known fiber other than the carbon nanotube fiber of the present invention, as long as the carbon nanotube fiber of the present invention is included in part. Motole.
  • the carbon nanochu laminate of the present invention is formed by laminating the carbon nanotube two-dimensional structure of the present invention.
  • two or more carbon nanotube sheets in which a plurality of carbon nanotube fibers are adjacent to each other in parallel are laminated
  • the angle formed by adjacent single-walled carbon nanotube fibers may be a right angle or an oblique angle.
  • the average thickness of the laminate is not limited and can be selected from a wide range according to the use of the final product.
  • the carbon nanotube fiber production method of the present invention is the carbon nanotube from the end face (side surface) of the carbon nanotube aggregate formed in a high density and high orientation on the substrate according to the present invention (Embodiment 1 or Embodiment 2). It is characterized by comprising a step of continuously forming long carbon nanotube fibers by pulling out a part of the aggregate.
  • a force similar to a frictional force acts between the extracted carbon nanotubes and the carbon nanotubes (on the substrate) in the aggregate adjacent to the carbon nanotubes. it is conceivable that.
  • the carbon nanotubes in the aggregate are further pulled out following the drawn carbon nanotubes, and this process proceeds continuously one after the other, so that a long carbon nanotube fiber or a two-dimensional structure of carbon nanotubes is obtained.
  • the body is formed.
  • a carbon nanotube two-dimensional structure can be manufactured.
  • a carbon nanotube two-dimensional structure can also be produced by arranging or weaving a plurality of carbon nanotube fibers.
  • the method of pulling out is not limited.
  • a known method can be used as a method for producing a carbon nanotube two-dimensional structure or a carbon nanotube laminate from a carbon nanotube fiber.
  • a known weaving method such as plain weave or twill weave may be employed.
  • a binder or the like may be applied and dried during production of the carbon nanotube fiber, the carbon nanotube two-dimensional structure, or the carbon nanotube laminate. Moreover, you may employ
  • a long carbon nanotube fiber or the like can be produced with high probability.
  • the carbon nanotube fibers and the like of the present invention have high strength and high conductivity derived from carbon nanotubes, various fiber products such as bulletproof and protective clothing; It can be used for a wide variety of applications such as product parts.
  • the Raman spectrum was measured using a micro Raman spectrophotometer.
  • the measurement conditions were as follows.
  • Irradiation beam diameter ⁇ ⁇ ⁇ ⁇ ⁇ ⁇
  • the O / C ratio was measured by photoelectron spectroscopy (ESCA) using an X-ray photoelectron spectrometer.
  • the measurement conditions were as follows.
  • the degree of vacuum in the chamber one: 1 X 10- 7 Pa ⁇ l X 10- 8 Pa
  • the Cls peak area was obtained by drawing a straight baseline in the range of binding energy 282 to 298 eV, and the oxygen (Ols) peak area was in the range of 526-540 eV. Obtained by drawing the ground.
  • the intensity of the two endpoints when drawing the background was obtained by numerically averaging the intensity of 10 points near each endpoint.
  • the O / C ratio was calculated by dividing the ratio of the Cls peak area to the Ols peak area determined above by the device-specific sensitivity correction value.
  • the inherent sensitivity correction value of “ESCA — 58 01MC” manufactured by ULVAC-FUY) used in the present invention was 2.40.
  • This substrate was placed in a thermal CVD apparatus, and a carbon nanotube aggregate was formed in a substrate shape by performing a thermal CVD method.
  • Gas supplied into the thermal CVD is acetylene gas and A mixed gas of helium gas (acetylene gas 5 ⁇ 77 vt%) was used.
  • the thermal CVD conditions were as follows: temperature: 700 ° C, pressure: atmospheric pressure, acetylene gas concentration increase rate in the initial stage: 0.10 vol% / second, reaction time: 10 minutes.
  • the coverage of amorphous carbon was 57%, and the average thickness of amorphous carbon was 1. lnm.
  • the carbon nanotube aggregate of Example 1 has a G / D ratio of 0.66, an oxygen Z carbon atom number ratio ( ⁇ / C ratio) of 0.008, a bulk density of 40 mg / cm 3 , and an order parameter (OP) of 0. 94.
  • the average length of the carbon nanotube was 190 ⁇ m.
  • Fig. 2 shows a scanning electron microscope (SEM) photograph of the cross section of the carbon nanotube aggregate obtained.
  • a carbon nanotube assembly of Example 2 was produced in the same manner as Example 1 except that the reaction time was 30 minutes.
  • the amorphous carbon coverage rate S100%, and the average thickness of the amorphous carbon was 1.7 nm.
  • the carbon nanotubes of Example 2 had a G / D ratio of 0.60, a ⁇ / C ratio of 0.002, a bulk density of 20 mg / cm 3 , and an OP of 0.92.
  • the average length of the carbon nanotubes was 220 / im.
  • a carbon nanotube of Comparative Example 1 was produced in the same manner as in Example 1 except that the reaction time was 5 minutes and the rate of increase in the acetylene gas concentration at the initial stage was 0.25 vol% / sec.
  • the coverage rate of amorphous carbon was 7%, and the average thickness of amorphous carbon was 0.2 nm.
  • the aggregate of carbon nanotubes had a GZD ratio of 0.69, an OZC ratio of 0.01, a bulk density of 60 mgZcm 3 , and an OP of 0.95.
  • the average length of the carbon nanotubes was 160 ⁇ m.
  • a carbon nanotube aggregate of Comparative Example 2 was produced in the same manner as in Example 1 except that the reaction time was 2 minutes and the rate of increase in the acetylene gas concentration at the initial stage was 0.35 vol% / second.
  • the coverage rate of amorphous carbon was 3 ⁇ 4%, and the average thickness of amorphous carbon was 0 ⁇ lnm.
  • the aggregate of carbon nanotubes had a G / D ratio of 1.60, an O / C ratio of 0.00, a bulk density of 15 mg / cm 3 , and an OP of 0.75.
  • the average length of the carbon nanotubes was 160 ⁇ m.
  • the carbon nanotube assembly of Example 3 was subjected to plasma treatment on the aggregate of carbon nanotubes produced in Comparative Example 1 using a low-temperature plasma surface treatment apparatus (produced by Hirano Kotone Co., Ltd., low-temperature plasma surface treatment apparatus). Aggregates were produced.
  • This plasma treatment was started at room temperature while a carbon nanotube aggregate substrate was placed on a parallel plate electrode having a diameter of 30 cm, and cooling water (room temperature) was passed through the electrode.
  • the irradiation power was 300 W
  • the oxygen gas flow rate was 45.9 ccm
  • the pressure inside the chamber was 0.221 Torr
  • the treatment time was 10 minutes.
  • the amorphous carbon coverage ratio was 7%, and the average thickness of the amorphous carbon was 0.7 nm.
  • the G / D ratio of the aggregate of carbon nanotubes of Example 3 was 0.56, the ⁇ / C ratio was 0.14, the bulk density was 60 mg / cm 3 , and OP was 0.91.
  • a carbon nanotube aggregate of Example 4 was manufactured in the same manner as in Example 3 except that the conditions of the plasma treatment were irradiation power: 500 W and treatment time: 5 minutes.
  • the aggregate of carbon nanotubes of Example 4 had a G / D ratio of 0.55, an O / C ratio of 0.10, a bulk density of 60 mg / cm ", and an OP of 0.95.
  • a carbon nanotube aggregate of Example 5 was manufactured in the same manner as in Example 3 except that the conditions of the plasma treatment were irradiation power: 500 W and treatment time: 20 minutes.
  • the aggregate of carbon nanotubes of Example 5 had a GZD ratio of 0.53, an O / C ratio of 0.27, a bulk density of 60 mg / cm 3 , and ⁇ P of 0.92.
  • Plasma treatment is performed on the aggregate of carbon nanotubes manufactured in Example 2 using a low-temperature plasma surface treatment apparatus (manufactured by Hirano Kotone Co., Ltd., low-temperature plasma surface treatment apparatus).
  • a low-temperature plasma surface treatment apparatus manufactured by Hirano Kotone Co., Ltd., low-temperature plasma surface treatment apparatus.
  • This plasma treatment was started at room temperature while a carbon nanotube assembly substrate was placed on a parallel plate electrode having a diameter of 30 cm, and cooling water (room temperature) was passed through the electrode.
  • the irradiation power was 500 W
  • the argon gas flow rate was 45.9 ccm
  • the pressure inside the chamber was 0.221 Torr
  • the treatment time was 10 minutes.
  • the aggregate of carbon nanotubes of Example 6 had a GZD ratio of 0.50, an O / C ratio of 0.09, a bulk density of 20 mg / cm 3 , and ⁇ P of 0.91.
  • a carbon nanotube aggregate of Example 7 was produced in the same manner as in Example 3 except that the conditions of the plasma treatment were irradiation power: 100 W and treatment time: 50 minutes.
  • the aggregate of carbon nanotubes of Example 7 had a GZD ratio of 0.57, an O / C ratio of 0.20, a bulk density of 55 mg / cm 3 , and ⁇ P of 0.88.
  • a carbon nanotube aggregate of Comparative Example 3 was produced in the same manner as in Example 3 except that the conditions of the plasma treatment were irradiation power: 500 W and treatment time: 40 minutes.
  • the carbon nanotube aggregate of Comparative Example 3 had a G / D ratio of 0.45, an O / C ratio of 0.40, a bulk density of 58 mg / cm 3 , and an OP of 0.75.
  • a carbon nanotube aggregate of Comparative Example 4 was produced in the same manner as in Example 3 except that the conditions of the plasma treatment were irradiation power: 500 W and treatment time: 35 minutes.
  • the carbon nanotube aggregate of Comparative Example 4 had a G / D ratio of 0.55, an O / C ratio of 0.45, a bulk density of 57 mg / cm 3 , and an OP of 0.70.
  • the tip of X-type tweezers (manufactured by FONTAX, product model number “4X_S”) is pierced by 0.5 to lmm to pinch multiple carbon nanotubes, and then pinch carbon nanotubes into XYZ Carbon nanotube fiber (carbon nanotube twisted yarn) by pulling it while twisting at a spinning speed of lcm / min after fixing to a stage twisting machine (manufactured by Daiei Science Equipment Mfg., Product model number “M_ 1”) was manufactured. This measurement was performed 10 times, and the length of the longest drawn yarn was taken as the maximum twisted yarn length. This is shown in Table 1.
  • the length of 25 cm which is a length that sufficiently squeezes one round, was used as the standard for the twisted yarn length. That is, the case where the maximum twist length was 25 cm or more was evaluated as “ ⁇ ”, and the case where it was less than 25 cm was evaluated as “X”.
  • FIG. 3 A SEM photograph of the carbon nanotube twisted yarn obtained using the carbon nanotube aggregate of Example 3 is shown in FIG. 3, and a SEM photograph of the carbon nanotube twisted yarn obtained using the carbon nanotube aggregate of Example 4 is shown in FIG. Figure 4 shows.
  • Example 10 The end of the carbon nanotube assembly produced in Example 5 was pinched with a tip of X-type tweezers 0.5 to 1 mm to pinch a plurality of carbon nanotubes, and then the pinned carbon nanotubes were twisted on the XYZ stage.
  • a carbon nanotube twisted yarn was produced by fixing to (made by Daiei Scientific Instruments Mfg., Product model number “M — 1”) and pulling it while twisting at a spinning speed of 1 cmZ.
  • the obtained carbon nanotube twisted yarn was cut to a length of 6 cm and made into polybulal alcohol 0.01 wt% aqueous solution (manufacturer name “Nacalai Testa”, product name “Polybutalol (Code 28310-35)”). After soaking for 30 minutes, the binder-containing carbon nanotube twisted yarn of Example 10 was produced by air drying.
  • Example 8 The carbon nanotube sheet produced in Example 8 was dipped in an aqueous solution of 0.01% by weight polybutyl alcohol for 45 minutes and then air-dried to produce the binder-containing carbon nanotube sheet of Example 11.
  • Figure 1 shows the spectrum obtained by Raman spectroscopy.
  • FIG. 2 shows an SEM photograph of the carbon nanotube assembly of Example 1.
  • FIG. 3 shows an SEM photograph of the carbon nanotube tube of Example 3.
  • FIG. 4 shows an SEM photograph of the carbon nanotube tube of Example 4.
  • FIG. 5 shows a SEM photograph of the carbon nanotube sheet of Example 8.
  • FIG. 6 shows an optical micrograph of the carbon nanotube cross-layered product of Example 9.

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Abstract

La présente invention concerne un ensemble de nanotubes de carbone ayant une multitudes de nanotubes de carbone formés sur un substrat, caractérisé en ce que (1) un carbone amorphe est superposé sur la surface de chacun des nanotubes de carbone avec un rapport de revêtement allant de 55 à 100 % ; (2) le carbone amorphe a une épaisseur moyenne allant de 0,3 à 5 nm ; (3) l'ensemble de nanotubes de carbone a un paramètre d'ordre allant de 0,85 à 1,0 ; (4) l'ensemble de nanotubes de carbone a une densité apparente allant de 1 à 1000 mg/cm3 ; (5) l'ensemble de nanotubes de carbone a un rapport atomique oxygène/carbone allant de 0,002 à 0,350 ; et (6) dans le spectre de Raman de l'ensemble de nanotubes de carbone, le rapport de l'aire de la bande G apparaissant à proximité de 1590 cm-1 sur la bande D apparaissant à proximité de 1350 cm-1 (rapport G/D) est dans la gamme de 0,45 à 0,75.
PCT/JP2007/053693 2006-02-28 2007-02-27 Ensemble de nanotubes de carbone, fibre de nanotubes de carbone et procede de production de fibre de nanotubes de carbone WO2007099975A1 (fr)

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JP7434810B2 (ja) 2019-11-05 2024-02-21 Ｔｏｐｐａｎホールディングス株式会社 ペリクル膜及びペリクル

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