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WO2025234298A1 - Procédé de production d'un faisceau de fibres de nanotubes de carbone - Google Patents

Procédé de production d'un faisceau de fibres de nanotubes de carbone

Info

Publication number
WO2025234298A1
WO2025234298A1 PCT/JP2025/015260 JP2025015260W WO2025234298A1 WO 2025234298 A1 WO2025234298 A1 WO 2025234298A1 JP 2025015260 W JP2025015260 W JP 2025015260W WO 2025234298 A1 WO2025234298 A1 WO 2025234298A1
Authority
WO
WIPO (PCT)
Prior art keywords
carbon nanotube
fiber bundle
fibers
string
nanotube fibers
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2025/015260
Other languages
English (en)
Japanese (ja)
Inventor
フィ テン
森 彩乃 大澤
浩文 韋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Carbon Fly Inc
Original Assignee
Carbon Fly Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Carbon Fly Inc filed Critical Carbon Fly Inc
Publication of WO2025234298A1 publication Critical patent/WO2025234298A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B64—AIRCRAFT; AVIATION; COSMONAUTICS
    • B64G—COSMONAUTICS; VEHICLES OR EQUIPMENT THEREFOR
    • B64G1/00—Cosmonautic vehicles
    • B64G1/22—Parts of, or equipment specially adapted for fitting in or to, cosmonautic vehicles
    • B64G1/52—Protection, safety or emergency devices; Survival aids
    • B64G1/56—Protection against meteoroids or space debris
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B64—AIRCRAFT; AVIATION; COSMONAUTICS
    • B64G—COSMONAUTICS; VEHICLES OR EQUIPMENT THEREFOR
    • B64G1/00—Cosmonautic vehicles
    • B64G1/22—Parts of, or equipment specially adapted for fitting in or to, cosmonautic vehicles
    • B64G1/64—Systems for coupling or separating cosmonautic vehicles or parts thereof, e.g. docking arrangements
    • 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
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/16—Yarns or threads made from mineral substances

Definitions

  • the present invention relates to a method for producing a carbon nanotube fiber bundle.
  • Carbon fiber is a lightweight, high-strength material that is expected to be used in a variety of applications, including aircraft, bicycles, concrete reinforcement, and sports.
  • carbon fiber reinforced plastics which are made up of carbon fiber and a matrix resin, are widely used in the above applications (see, for example, Patent Document 1).
  • carbon nanotubes are known to be particularly lightweight and mechanically strong, and due to their physical shape, are also known to be a material with high electrical and thermal conductivity. Carbon nanotubes are also known as a material with a high aspect ratio.
  • Tether materials are an example of an application that requires a high aspect ratio as well as light weight and mechanical strength. Tether materials are the material used to make tethers that connect a parent satellite and a child satellite connected to the parent satellite. Satellites connected to child satellites by tethers are expected to be used to collect space debris such as used satellites and rocket parts.
  • carbon nanotubes are a material that is light weight, has high mechanical strength, and also exhibits high conductivity. For this reason, there is growing interest in using carbon nanotubes as a tether material.
  • Tethers are generally formed into a mesh-like structure. Furthermore, due to their intended use, tethers are required to be wound around bobbins or the like and be stretchable. Mesh-like tethers are formed, for example, by weaving a tether material formed by twisting together multiple fiber bundles.
  • Tether materials can be formed by twisting together multiple carbon nanotube fiber bundles.
  • carbon nanotube fiber bundles made up of multiple carbon nanotube fibers can sometimes lose the high physical properties of the individual carbon nanotubes.
  • the present invention was made in consideration of the above circumstances, and aims to provide a method for manufacturing carbon nanotube fiber bundles that can produce high-strength carbon nanotube fiber bundles.
  • the present invention provides the following means to solve the above problems.
  • a method for manufacturing a carbon nanotube fiber bundle according to one aspect of the present invention includes a fiber bundle forming step of compressing and pulling the carbon nanotube fibers in a direction intersecting the direction in which the carbon nanotube fibers extend, thereby forming a fiber bundle from the carbon nanotube fibers.
  • the plurality of carbon nanotube fibers may be compressed from the periphery toward the center of the plurality of carbon nanotube fibers.
  • the plurality of carbon nanotube fibers threaded through a string-like member formed in a ring shape may be tightened by the string-like member.
  • the substrate of the string-like member may be carbon nanotubes or jute.
  • the method for producing a carbon nanotube fiber bundle according to any one of [1] to [4] above may further include a drawing step of drawing the plurality of carbon nanotube fibers from the carbon nanotube forest.
  • the method for producing a carbon nanotube fiber bundle according to [5] above may further include a preliminary step of bundling the multiple carbon nanotube fibers drawn from the carbon nanotube forest.
  • the plurality of carbon nanotube fibers may be threaded through a string-like member formed into a ring shape.
  • the preliminary step may include passing the plurality of carbon nanotube fibers through a die.
  • the plurality of carbon nanotube fibers may be pulled together with the wire while being compressed.
  • the present invention provides a method for producing carbon nanotube fiber bundles that can produce high-strength carbon nanotube fiber bundles.
  • FIG. 1 is a perspective view illustrating a method for producing a carbon nanotube fiber bundle according to an embodiment of the present invention.
  • 1 is a cross-sectional view showing an example of pulling out a plurality of carbon nanotube fibers from a carbon nanotube forest in a method for producing a carbon nanotube fiber bundle according to one embodiment of the present invention.
  • FIG. 2 is a plan view of FIG. 1; 1 is a cross-sectional view showing an example of a string-like member constituting a compression section that can be used in a fiber bundle formation step of a method for producing a carbon nanotube fiber bundle according to an embodiment of the present invention.
  • FIG. 5(a) is a schematic diagram showing the structure of a fiber bundle 1Z of carbon nanotubes obtained by a conventional method, and FIG.
  • FIG. 5(b) is a schematic diagram of a carbon nanotube fiber bundle 1 obtained by the above embodiment. 1.
  • FIG. 4 is a perspective view for explaining a method for manufacturing a carbon nanotube fiber bundle according to a modified example of FIG. 1.
  • FIG. 5 is a perspective view for explaining a method for manufacturing a carbon nanotube fiber bundle according to another modified example of FIG. 1.
  • FIG. 5 is a perspective view for explaining a method for manufacturing a carbon nanotube fiber bundle according to another modified example of FIG. 9(a) is a load-deformation curve of Example 1, and FIG. 9(b) is a stress-strain curve of Example 1.
  • 10(a) is the load-deformation curve of Example 2
  • FIG. 10(b) is the stress-strain curve of Example 1.
  • FIG. 11(a) is the load-deformation curve of Example 3, and FIG. 11(b) is the stress-strain curve of Example 1.
  • 12(a) is the load-deformation curve of Example 4, and FIG. 12(b) is the stress-strain curve of Example 1.
  • 13(a) shows the load-deformation curves of Example 1 and Comparative Example 1
  • FIG. 13(b) shows the stress-strain curves of Example 1 and Comparative Example 1.
  • FIG. 14(a) is a load-deformation curve of Example 5
  • FIG. 14(b) is a stress-strain curve of Example 5.
  • a method for manufacturing a carbon nanotube fiber bundle according to one embodiment of the present invention includes a fiber bundle forming process in which a plurality of carbon nanotube fibers are compressed and pulled in a direction intersecting the extension direction of the plurality of carbon nanotube fibers to form a fiber bundle from the plurality of carbon nanotube fibers.
  • a method for manufacturing a carbon nanotube fiber bundle according to one embodiment of the present invention includes, for example, a preparation step of forming a carbon nanotube forest on a substrate such as a wafer, a drawing step of drawing out a plurality of carbon nanotube fibers from the carbon nanotube forest, and a fiber bundle formation step of compressing the plurality of carbon nanotube fibers drawn out in the drawing step and drawing the plurality of carbon nanotube fibers together to form a fiber bundle from the plurality of carbon nanotube fibers.
  • a method for manufacturing a carbon nanotube fiber bundle according to one embodiment of the present invention performs, for example, the drawing step and the fiber bundle formation step in parallel.
  • Figure 1 is a perspective view illustrating a method for manufacturing a carbon nanotube fiber bundle according to one embodiment of the present invention.
  • Figure 1 shows an example in which the drawing process and fiber bundle formation process are performed in parallel, and shows a region R1 where multiple carbon nanotube fibers are drawn out from a carbon nanotube forest F, and a fiber bundle formation region R10 where the multiple carbon nanotube fibers are compressed and drawn to form a carbon nanotube fiber bundle 1.
  • a carbon nanotube forest F is formed on a wafer W (preparation process).
  • the carbon nanotube forest F is composed of a plurality of carbon nanotubes (CNTs).
  • the plurality of carbon nanotubes in the carbon nanotube forest F are also called vertically aligned carbon nanotubes. That is, the plurality of carbon nanotubes are formed in a direction perpendicular to the main surface of the wafer W.
  • the preparation process is carried out, for example, by chemical vapor deposition using a wafer W.
  • a metal catalyst may be formed on the surface of the wafer W used in the preparation process, for example, by sputtering.
  • the carbon nanotube forest F is formed by a dense array of multiple carbon nanotubes, and its density can be adjusted by the amount, density, and type of metal catalyst, the flow rate of the raw material gas used in the chemical vapor deposition process, etc.
  • a plurality of carbon nanotube fibers are pulled out from the carbon nanotube forest F (pulling process).
  • carbon nanotubes located at the ends of the vertically aligned carbon nanotubes that make up the carbon nanotube forest F are pulled out.
  • Figure 2 is a cross-sectional view showing an example of how a plurality of carbon nanotube fibers are pulled out from a carbon nanotube forest in a method for producing a carbon nanotube fiber bundle according to one embodiment of the present invention.
  • Figure 3 is a plan view of Figure 1. For convenience of explanation, the scale of the pulling region R1 is changed in Figure 3.
  • a pull-out member P When pulling out carbon nanotubes from the carbon nanotube forest F, for example, a pull-out member P is used. Tweezers, a drum, or the like can be used as the pull-out member P. By using the pull-out member P to pull out a carbon nanotube located at the end of the carbon nanotube forest F, the van der Waals forces pull out the carbon nanotubes adjacent to the pulled-out carbon nanotube in sequence, forming a carbon nanotube fiber 21 that extends in the direction in which the carbon nanotube located at the end was pulled out.
  • carbon nanotubes are a material that exhibits high van der Waals forces
  • the carbon nanotube fiber 21 is composed of, for example, multiple carbon nanotubes connected to each other by van der Waals forces, for example at their ends, along a predetermined direction.
  • a film is formed in which multiple carbon nanotube fibers 21 are aligned in the in-plane direction.
  • the film composed of multiple carbon nanotube fibers 21 may be referred to as a carbon nanotube film, and is indicated by the reference numeral 20 in Figures 1 to 3.
  • the multiple carbon nanotube fibers 21 that make up the carbon nanotube film 20 are bonded together by van der Waals forces.
  • the width of the longitudinal ends of the carbon nanotube film 20 corresponds, for example, to the width of the drawing member P used in the drawing process. Adjacent carbon nanotube fibers 21 in the width direction, which intersects with the longitudinal direction, are in contact with each other by van der Waals forces, for example.
  • Figure 3 illustrates only some of the carbon nanotube fibers 21 contained in the carbon nanotube film 20 that are spaced apart in the width direction when drawn out of the carbon nanotube forest F. Note that the above-described characteristics of the longitudinal ends of the carbon nanotube film 20 are characteristics of the longitudinal ends of the carbon nanotube film 20 before the fiber bundle forming process is performed. Once the fiber bundle forming process is performed, the carbon nanotube film 20 becomes a narrow fiber bundle.
  • the carbon nanotube film 20 is not limited to a form with a constant width, and may have a width that changes continuously along the longitudinal direction.
  • a pull-out member P having a width smaller than the width of the carbon nanotube forest F is used to form the carbon nanotube film 20 whose width narrows from the carbon nanotube forest F side toward the tip. If the tip of the pull-out member P has a flat shape, the width of the end of the carbon nanotube film 20 corresponds to, for example, the width of the end of the pull-out member P.
  • the carbon nanotube film 20 is formed so that its width (length in the x direction) is greater than its thickness (length in the z direction).
  • the plurality of carbon nanotube fibers 21, for example, the carbon nanotube film 20 are compressed and pulled together in a direction intersecting the extension direction of the plurality of carbon nanotube fibers 21, forming a carbon nanotube fiber bundle.
  • the compression of the plurality of carbon nanotube fibers 21 is performed, for example, by a compression unit 10, as will be described in detail below.
  • At least one compression unit 10 is provided.
  • the compression unit 10 has, for example, a ring structure, and is configured to be able to compress the plurality of carbon nanotube fibers 21 by applying pressure from the periphery toward the center of the plurality of carbon nanotube fibers 21.
  • the carbon nanotube fibers 21 are compressed after their tips are passed through the annular structure of the compression section 10, which has a ring-shaped structure. Compression will be described in detail later.
  • the operation of passing the carbon nanotube fibers 21 through the compression section 10 may be performed while the carbon nanotube fibers 21 are being drawn from the carbon nanotube forest F, i.e., while the carbon nanotube fibers 21 are being drawn, or may be performed while the operation of drawing the carbon nanotube fibers 21 from the carbon nanotube forest F is paused. Because the carbon nanotube fibers 21 are continuous fibers, once their tips are passed through the annular structure of the compression section 10, the carbon nanotube fibers 21 remain in the annular structure until they are terminated.
  • the uncompressed portion may be removed.
  • the removal process is referred to as the "removal process”
  • the carbon nanotube fiber bundle from which the uncompressed region has been removed is called the "carbon nanotube fiber bundle.”
  • ⁇ Fiber bundle forming step> The plurality of carbon nanotube fibers 21 are compressed and pulled together in a direction intersecting the direction in which the plurality of carbon nanotube fibers 21 extend, thereby forming a fiber bundle from the plurality of carbon nanotube fibers 21 (fiber bundle forming step, see FIGS. 1 and 3 ).
  • a fiber bundle made of the plurality of carbon nanotube fibers 21 formed by compressing and pulling the plurality of carbon nanotube fibers 21 is referred to as a carbon nanotube fiber bundle 1.
  • Compression of the plurality of carbon nanotube fibers 21 in the fiber bundle forming step is performed, for example, by a compression unit 10.
  • the compression unit 10 has, for example, a ring-shaped structure that can surround the plurality of carbon nanotube fibers 21 from the outer periphery.
  • the cross-sectional shape of the carbon nanotube fiber bundle 1 may be, for example, circular, elliptical, rectangular with rounded corners, or flat.
  • An example of a flat shape is a ribbon shape.
  • a ribbon shape means a flat, elongated shape, and can also be called a tape or band shape.
  • compressing the plurality of carbon nanotube fibers 21 in a direction intersecting the direction in which the plurality of carbon nanotube fibers 21 extend it is preferable to apply pressure to the plurality of carbon nanotube fibers 21 from the outer periphery toward the center of the plurality of carbon nanotube fibers 21.
  • compressing the plurality of carbon nanotube fibers 21 in a direction intersecting the direction in which the plurality of carbon nanotube fibers 21 extend is not limited to the example of applying pressure in a direction perpendicular to the axial direction of each of the plurality of carbon nanotube fibers 21, and the direction in which pressure is applied may be inclined from the direction perpendicular to the axial direction.
  • the compression section 10 has, for example, a string-like member.
  • Figures 1 and 3 show an example in which the compression section 10 is composed of a string-like member.
  • the multiple carbon nanotube fibers 21 are compressed by being tightened with a ring-shaped string-like member.
  • the ring-shaped string-like member is formed so that a portion of it has a ring structure.
  • the string-like member binds the multiple carbon nanotube fibers 21 and fixes them in a knotted state.
  • the string-like member may be knotted in a manner other than a knotted knot. For example, it may be knotted in a manner such as a wrap knot.
  • the knot formed when the multiple carbon nanotube fibers 21 are processed to have a ring structure is also called a ribbon knot.
  • the ring structure may be configured to bind the multiple carbon nanotube fibers 21, and may be a very small shape that is invisible to the naked eye.
  • the string-like member is preferably fixed in a tensioned state.
  • the string-like member is preferably fixed by the first fixing portion 30a and the second fixing portion 30b.
  • the string-like member is preferably fixed by, for example, being wrapped around, held by, or glued to the first fixing portion 30a and the second fixing portion 30b so that the distance between a predetermined position on one side and a predetermined position on the other side of the ribbon knot is approximately constant.
  • the first fixing portion 30a and the second fixing portion 30b are, for example, rod-shaped members to which the string-like member is fastened.
  • the distance between predetermined positions on one side and the other side of the string-like member in relation to the ribbon knot is fixed, and a predetermined pressure can be applied from the periphery toward the center to tighten the multiple carbon nanotube fibers 21 passing through the ribbon knot.
  • tension may be applied to both ends of the string-like member by any method.
  • the inner diameter of the annular structure of the compressed portion 10 can be adjusted as appropriate depending on the number and inner diameter of the multiple carbon nanotube fibers 21 that make up the carbon nanotube fiber bundle 1.
  • the inner diameter of the annular structure of the compressed portion 10 is, for example, 0.005 to 0.4 mm, may be 0.01 to 0.1 mm, or may be 0.015 to 0.07 mm.
  • the tensile strength of the string-shaped member is, for example, 10 MPa to 10 GPa.
  • the tensile modulus (rigidity) of the string-shaped member is, for example, 100 MPa to 100 GPa.
  • the surface roughness (arithmetic mean roughness Ra) of the string-shaped member is, for example, 1 nm to 500 ⁇ m.
  • the breaking strain of the string-shaped member is, for example, 1 to 500.
  • the annular structure can have a smaller inner diameter. Furthermore, when the surface roughness of the string-shaped member is within the above range, friction with the carbon nanotube fibers can be reduced. Furthermore, when the string-shaped member has the above characteristics, an appropriate amount of pressure can be applied uniformly to the entire outer circumference of multiple carbon nanotube fibers 21 in the fiber bundle forming process.
  • Figure 4 is a cross-sectional view showing an example of a string-like member constituting the compression section 10 that can be used in the fiber bundle formation step of a carbon nanotube fiber bundle manufacturing method according to one embodiment of the present invention.
  • the string-like member constituting the compression section 10 is, for example, composed of a substrate 11, or as shown in Figure 4, is composed of a substrate 11 and a coating layer 12 formed to cover the substrate 11.
  • the string-like member is composed of a substrate 11 and a coating layer 12, it is sufficient that the substrate 11 of the substrate 11 and the coating layer 12 satisfies the above-mentioned tensile modulus and tensile strength described as the characteristics of the string-like member, but it is preferable that both the substrate 11 and the coating layer 12 satisfy the above-mentioned tensile modulus and tensile strength.
  • the string-shaped member that satisfies the above configuration and can be used in this embodiment has a base material 11 made of nylon, polyvinylidene fluoride, polyolefin (e.g., polyethylene, polypropylene), polyacrylonitrile, carbon fiber, carbon nanotubes, jute, etc.
  • the base material is a resin such as nylon, polyvinylidene fluoride, polyolefin (e.g., polyethylene, polypropylene), or polyacrylonitrile, it may be a resin blended with carbon nanotubes.
  • the string-shaped member may be made of a material selected from the group consisting of carbon nanotubes, jute, and polyacrylonitrile. Using the above material for the base material 11 of the string-shaped member is preferable because it allows the string-shaped member to apply high pressure uniformly from the periphery toward the center to tighten the multiple carbon nanotube fibers 21.
  • a configuration in which the string-shaped member as shown in FIG. 4 is provided with a coating layer 12 is effective when the surface roughness of the substrate 11 is high.
  • the coating layer 12 By providing the coating layer 12, the surface roughness can be made smoother. This is thought to reduce friction between the string-shaped member and the multiple carbon nanotube fibers 21 when pulling the multiple carbon nanotube fibers 21 together during the fiber bundle formation process, resulting in a smooth surface for the carbon nanotube fiber bundle that is formed.
  • the coating layer 12 may be composed of, for example, a silicone coating or a water-repellent glass coating.
  • the surface of the string-shaped member is silicone-coated, the flexibility and tensile strength of the string-shaped member are thought to be further improved.
  • a configuration in which the coating layer 12 is not provided on the substrate 11 is a preferred embodiment of the string-shaped member.
  • a string-shaped member made of a substrate 11 that is carbon nanotubes is one preferred embodiment. From the perspective of producing fine carbon nanotube fiber bundles and applying high pressure to the multiple carbon nanotube fibers 21 to produce high-density carbon nanotube fiber bundles, carbon nanotubes without a coating layer are preferred.
  • the string-like member is preferably any one selected from the group consisting of jute, polyacrylonitrile, carbon nanotubes (carbon nanotubes without a coating layer), carbon nanotubes coated with a silicone coating agent, and carbon nanotubes coated with a water-repellent glass coating agent; more preferably any one selected from the group consisting of jute, carbon nanotubes (carbon nanotubes without a coating layer), and carbon nanotubes coated with a silicone coating agent; carbon nanotubes (carbon nanotubes without a coating layer) are particularly preferred.
  • jute, polyacrylonitrile, and carbon nanotubes (without a coating layer) constitute the substrate 11.
  • a plurality of carbon nanotube fibers 21 are compressed and pulled in the extension direction of the plurality of carbon nanotube fibers 21 to form a carbon nanotube fiber bundle 1.
  • the speed at which the carbon nanotube fibers 21 are pulled is arbitrary, but from the perspective of producing a homogeneous carbon nanotube fiber bundle 1, it is preferable that the speed be constant over time.
  • the carbon nanotube fibers 21 are compressed and pulled in a direction intersecting the extension direction of the carbon nanotube fibers 21, so that a force is applied to substantially the entire circumference of the carbon nanotube fibers 21 to form the carbon nanotube fiber bundle 1.
  • the carbon nanotubes that make up the carbon nanotube fibers 21 become straight, and the gaps between those located in the direction intersecting the extension direction become smaller. This increases the van der Waals force between the carbon nanotubes that make up the carbon nanotube fiber bundle 1 to be produced. Therefore, according to this embodiment, a carbon nanotube fiber bundle 1 with high breaking stress and high strength can be manufactured.
  • the carbon nanotube fiber bundle 1 provided by the above embodiment has been confirmed to exhibit higher tensile strength than carbon nanotube fiber bundles produced by drawing multiple carbon nanotube fibers through a metal die. Furthermore, crimping can be suppressed, and the carbon nanotube fiber 21 component in the axial direction of the carbon nanotube fiber bundle 1 can be increased.
  • the width of the multiple carbon nanotube fibers is reduced by the die, it is expected that the distance between the carbon nanotube fibers in the thickness direction will also increase locally. Furthermore, if the inner diameter of the die is too small, it will be impossible to pass multiple carbon nanotube fibers through it. Therefore, it is difficult to increase the proportion of the area on the inner surface of the die that comes into contact with the multiple carbon nanotube fibers by adjusting the inner diameter of the metal die.
  • the method for manufacturing a carbon nanotube fiber bundle of this embodiment it is possible to compress multiple carbon nanotube fibers using a compression section such as a string-like member, such as a carbon nanotube fiber bundle, without using complex equipment or expensive materials, thereby reducing manufacturing costs. Furthermore, forming a ribbon knot that can be used for the compression section 10 does not require the use of complex equipment. In this way, the method for manufacturing a carbon nanotube fiber bundle of this embodiment does not require complex equipment and can save space.
  • the carbon nanotube fiber bundle produced by the carbon nanotube fiber bundle manufacturing method of this embodiment is made up of multiple carbon nanotube fibers compressed in the radial direction, and can be produced with few other components.
  • a method for producing a carbon nanotube fiber bundle 1 by forming a carbon nanotube forest F on a wafer W, passing a plurality of carbon nanotube fibers 21 drawn from the carbon nanotube forest F through a compression unit 10, and compressing and drawing the plurality of carbon nanotube fibers 21 in a direction intersecting the extension direction using the compression unit 10 was exemplified.
  • the present invention is not limited to the above embodiment. In other words, the present invention is not limited to an example in which a preparation step, as in the above embodiment, is followed by a drawing step and a fiber bundle formation step in parallel to continuously produce a carbon nanotube fiber bundle 1.
  • the present invention is not limited to any example in which a fiber bundle formation step is performed on a plurality of carbon nanotube fibers 21.
  • a carbon nanotube film 20 or the like wound on a drum, bobbin, or the like may be compressed and drawn in a direction intersecting the extension direction to form a carbon nanotube fiber bundle.
  • the present invention may be configured to perform the fiber bundle formation step on a plurality of carbon nanotube fibers 21 that have been drawn in advance, in which case steps such as the preparation step and drawing step can be omitted.
  • FIG. 5(a) is a schematic diagram showing the structure of a carbon nanotube fiber bundle 1Z obtained by a conventional method
  • FIG. 5(b) is a schematic diagram of a carbon nanotube fiber bundle 1 obtained by the above embodiment
  • reference numeral 25 represents a short fiber of carbon nanotube.
  • the short fiber 25 is formed by multiple carbon nanotubes bonded together by van der Waals forces.
  • the carbon nanotube fiber 21 is formed by multiple short fibers 25 connected by van der Waals forces.
  • the carbon nanotube fiber bundle 1 is formed by sequentially drawing out a drawn-out carbon nanotube and adjacent carbon nanotubes by van der Waals forces.
  • the carbon nanotube fiber bundle contains a mixture of portions where the short fibers 25 are bonded to each other at close range by van der Waals forces and portions where the short fibers 25 are far apart, forming voids S that are large compared to the diameter of the short fibers 25.
  • the magnitude of the van der Waals force acting between the short fibers 25 depends on the distance between the short fibers 25, with the smaller the distance, the greater the force. Therefore, the van der Waals force acting between the short fibers 25 sandwiching the voids S in FIG. 5(a) is weaker than when the short fibers 25 are bonded together. Accordingly, in the configuration shown in FIG.
  • the strength of the fiber bundle is lower than in the configuration shown in FIG. 5(b) where the short fibers 25 are bonded together and the voids S are suppressed.
  • compressing and pulling multiple carbon nanotube fibers 21 simultaneously bonds the short fibers 25 within the carbon nanotube fibers 21, suppressing the generation of voids S and increasing strength.
  • the method for producing a carbon nanotube fiber bundle of the present invention is not limited to the above example, and may further include other steps. For example, it may be implemented by combining the configurations described in the modified examples described below.
  • Figure 6 is a perspective view illustrating a method for manufacturing a carbon nanotube fiber bundle according to a modified example of Figure 1.
  • Figure 6 differs from Figure 1 in that a preliminary adjustment section 10A is provided upstream of the compression section 10.
  • the method for manufacturing a carbon nanotube fiber bundle according to this embodiment may compress multiple carbon nanotube fibers at multiple locations in a direction intersecting the direction in which the carbon nanotube fibers extend, or may gather multiple carbon nanotube fibers closer to the carbon nanotube forest F and then compress the multiple carbon nanotube fibers 21.
  • the carbon nanotube fiber bundle manufacturing method may further include a preliminary process of bundling multiple carbon nanotube fibers drawn from the carbon nanotube forest.
  • Figure 6 shows a preliminary region R5 where the preliminary process is performed, between the drawing region R1 where the drawing process is performed and the fiber bundle formation region R10 where the fiber bundle formation process is performed.
  • a preliminary adjustment section 10A is provided at one location upstream of the compression section 10 made of a string-like member, but this is not limiting, and preliminary adjustment sections may be provided at two or more locations.
  • the preliminary process can be performed, for example, in parallel with the drawing process and the fiber bundle formation process, and is preferably performed in parallel with the fiber bundle formation process.
  • a first fixing portion 30c and a second fixing portion 30d that fix the preliminary adjustment unit 10A are provided in the preliminary region R5.
  • the preliminary adjustment unit 10A is made of, for example, a string-like member.
  • the preliminary adjustment unit 10A can be made of the same material that can be used as the compression unit 10. That is, the preliminary adjustment unit 10A is made of, for example, a string-like member.
  • the string-like member that makes up the preliminary adjustment unit 10A is formed, for example, to have a ring-like structure. In the preliminary process, for example, multiple carbon nanotube fibers are threaded through a ring-shaped string-like member.
  • a pressure lower than the pressure applied to the multiple carbon nanotube fibers in the fiber bundle formation process is applied to bundle the multiple carbon nanotube fibers.
  • the direction in which pressure is applied to the multiple carbon nanotube fibers in the preliminary process is a direction that intersects the longitudinal direction of the carbon nanotube fibers.
  • the carbon nanotube fiber bundle manufacturing method further includes a preliminary process, which improves the orientation of the multiple carbon nanotube fibers before the fiber bundle formation process, making the finished carbon nanotube fiber bundle denser and stronger.
  • Figure 7 is a perspective view illustrating a method for manufacturing a carbon nanotube fiber bundle according to another variation of Figure 1.
  • multiple carbon nanotube fibers may be passed through the die 40 in a preliminary step.
  • a known die with an internal through-hole can be used as the die 40.
  • the inner diameter of the die 40 can be adjusted depending on the number of carbon nanotube fibers constituting the carbon nanotube fiber bundle 1 and the cross-sectional area of the finished product, but is, for example, 0.025 mm to 0.4 mm, preferably 0.035 mm to 0.2 mm.
  • a sufficiently large inner diameter of the die 40 prevents excessive pressure from being applied locally to the carbon nanotube fibers and prevents the carbon nanotube fibers from failing to pass through.
  • a sufficiently small inner diameter of the die 40 can enhance the orientation of the carbon nanotube fibers before the fiber bundle formation process. While Figure 7 shows an example in which one die 40 and one compression section 10 are provided, the present invention is not limited to this example, and multiple dies 40 and multiple compression sections 10 may be provided.
  • multiple dies 40 and/or compression units 10 are provided, i.e., when the total number of dies 40 and compression units 10 used is three or more, it is preferable to configure them so that the pressure on the multiple carbon nanotube fibers gradually increases along their longitudinal direction, and ultimately produce a carbon nanotube fiber bundle using the compression unit 10.
  • all of the multiple dies 40 are configured so that they are closer to the carbon nanotube forest F than the compression unit 10, and the inner diameter of the dies 40 decreases as they become closer to the compression unit 10.
  • multiple compression units 10 made of string-like members it is preferable that the compression units farther from the carbon nanotube forest F apply stronger compression to the string-like members.
  • the carbon nanotube fibers are bundled in a preliminary process, and their orientation is enhanced before the fiber bundle formation process. Furthermore, pressure can be applied to multiple carbon nanotube fibers in their extension direction at multiple locations, including the locations where the fiber bundle formation process is performed and the locations where the preliminary process is performed. Therefore, by performing the preliminary process and the fiber bundle formation process in parallel, the arrangement of carbon nanotubes in a direction intersecting the longitudinal direction can be adjusted over a wide area in the longitudinal direction of the carbon nanotube fibers in the fiber bundle formation process, making it possible to produce a carbon nanotube fiber bundle with a large contact area between the carbon nanotubes and high orientation. In such a carbon nanotube fiber bundle, a large load can be transmitted to each individual carbon nanotube, achieving high strength.
  • Figure 8 is a perspective view illustrating a method for manufacturing a carbon nanotube fiber bundle according to another variation of Figure 1.
  • the string-like member constituting the compressed section 10 may be configured to bind the wire 15 and multiple carbon nanotube fibers 21.
  • a string-like member clamps the multiple carbon nanotube fibers together with the wire 15, compressing the multiple carbon nanotube fibers from the periphery toward the center.
  • the multiple carbon nanotube fibers 21 may be pulled together while being compressed together with the wire 15.
  • the wire 15 is fixed, for example, at both ends by fixed ends 60a, 60b.
  • a known wire having a linear shape extending in one direction, such as a cylindrical shape, can be used as the wire 15.
  • the string-like member constituting the compression section 10 may be fixed to the first fixing portion 30a, the second fixing portion 30b, etc., while clamping the wire 15 and the multiple carbon nanotube fibers.
  • the upper and/or lower limit values of the numerical ranges described in this specification can be arbitrarily combined to define a preferred range.
  • the upper and lower limit values of the numerical ranges can be arbitrarily combined to define a preferred range
  • the upper limit values of the numerical ranges can be arbitrarily combined to define a preferred range
  • the lower limit values of the numerical ranges can be arbitrarily combined to define a preferred range.
  • the string-like member that constitutes the compression section 10 is shown in a loose state, but it is actually tied in a knot such as a one-sided knot.
  • Example 1 First, as a preparation step, a wafer coated with a catalyst for carbon nanotube growth was prepared, and vertically aligned carbon nanotubes were grown from the catalyst by chemical vapor deposition, creating a vertically aligned carbon nanotube forest oriented perpendicular to the wafer.
  • the carbon nanotube forest formed on the wafer was pinched at the end in one direction and pulled out so that multiple carbon nanotube fibers were arranged in parallel.
  • multiple carbon nanotube fibers were threaded inside the loop of a string-like member with a ring-shaped structure formed by a one-sided knot.
  • the multiple carbon nanotube fibers were tied together with a string-like member acting as a compression section, and both ends were pulled to narrow the inner diameter of the ribbon knot. This compressed and tightened the carbon nanotube fibers from the outer periphery toward the center in a direction intersecting the extension direction of the multiple carbon nanotube fibers, and also pulled the multiple carbon nanotube fibers together, resulting in a carbon nanotube fiber bundle.
  • the ring-shaped structure of the string-like member ribbon knot
  • the ring-shaped structure of the string-like member is thought to have an inner diameter of approximately 0.035 mm when the multiple carbon nanotube fibers are tightened.
  • the string-like members carbon nanotubes coated with a silicone coating agent were used as the string-like members.
  • the base material of the string-like members was a carbon nanotube ribbon made of carbon nanotube fibers.
  • the width of the string-like members was 0.17 mm, and the thickness was 0.06 mm.
  • Example 2 A carbon nanotube fiber bundle was produced in the same manner as in Example 1, except that carbon nanotubes coated with a water-repellent glass coating agent were used as the string-like members. The width and thickness of the string-like members were also the same as in Example 1.
  • Example 3 A carbon nanotube fiber bundle was produced in the same manner as in Example 1, except that the string-like member was made of acrylonitrile (acrylic yarn). The diameter of the string-like member was about 2.5 mm.
  • Example 4 A carbon nanotube fiber bundle was produced in the same manner as in Example 1, except that the string-like member was made of jute (hemp string). The diameter of the string-like member was about 0.6 mm.
  • Example 5 Carbon nanotube fiber bundles were produced in the same manner as in Example 1, except that carbon nanotubes (uncoated carbon nanotubes) were used as the string-like members.
  • the substrate of the string-like members used in Example 5 was a carbon nanotube ribbon with a circular cross section made of carbon nanotube fibers.
  • the diameter of the string-like members was 0.046 mm, and it is believed that the inner diameter of the string-like members was approximately 0.020 mm when the multiple carbon nanotube fibers were tightened.
  • Example 1 A carbon nanotube fiber bundle was produced in the same manner as in Example 1, except that the fiber bundle formation step using a string-like member was not performed, and that a metal die having a through hole with an inner diameter of 0.035 mm was provided at the position where the string-like member was provided in Example 1, and the carbon nanotube fiber bundle was passed through the metal die. That is, in Comparative Example 1, a carbon nanotube fiber bundle was produced by passing a plurality of carbon nanotube fibers drawn from a carbon nanotube forest produced in the same manner as in Example 1 through two metal dies, one having a through hole with an inner diameter of 0.100 mm and the other having a through hole with an inner diameter of 0.035 mm.
  • Example 1 Ten carbon nanotube fiber bundles were produced under the conditions of each of Example 1 and Comparative Example 1, and tensile strength measurements were performed. The tensile strength measurements were performed using a bench-top precision universal testing machine (Shimadzu Corporation, Autograph AGS-X) in accordance with ISO 11566: 1996. The tensile strength measurements were continued until the sample broke.
  • Figure 9(a) is the load-deformation curve for Example 1
  • Figure 9(b) is the stress-strain curve for Example 1.
  • Figure 9 shows the measurement results for all 10 samples produced in Example 1.
  • the horizontal axis in Figure 9(a) represents the displacement [mm], which is the elongation of the carbon nanotube fiber bundle during the test.
  • the vertical axis in Figure 9(a) represents the load [N] applied to the carbon nanotube fiber bundle in the extension direction of the carbon nanotube fiber bundle during the test.
  • the vertical axis in Figure 9(b) represents stress [MPa], which was calculated by dividing the load applied to the carbon nanotube fiber bundle by the cross-sectional area of the carbon nanotube fiber bundle.
  • the horizontal axis in Figure 9(b) represents strain, which was calculated by dividing the elongation of the carbon nanotube fiber bundle during the test by the length of the carbon nanotubes in their initial state.
  • Figure 9(b) also confirms that the carbon nanotube fiber bundle of Example 1 exhibits high tensile strength.
  • Figures 10(a), 11(a), 12(a), and 14(a) are the load-deformation curves for Examples 2, 3, 4, and 5, respectively
  • Figures 10(b), 11(b), 12(b), and 14(b) are the stress-strain curves for Examples 2, 3, 4, and 5, respectively.
  • Each of Figures 10(a) to 12(b) shows the measurement results for all 10 samples under the same conditions.
  • Figures 14(a) and 14(b) shows the measurement results for all five samples under the same conditions.
  • Figure 13(a) shows the load-deformation curves for Example 1 and Comparative Example 1
  • Figure 13(b) shows the stress-strain curves for Example 1 and Comparative Example 1.
  • the samples for Example 1 and Comparative Example 1 contain the same amount of carbon nanotubes drawn from the carbon nanotube forest.
  • the difference in the stress-strain curves shown in Figure 13(b) is thought to be due to the fact that the fiber bundle formation process in Example 1 prevents the outer periphery of the carbon nanotube fiber bundle from being damaged by a die or the like, and improves the adhesion between the multiple carbon nanotube fibers that make up the carbon nanotube fiber bundle, thereby improving tensile strength.
  • the carbon nanotube fiber bundles formed in Examples 1 to 5 and Comparative Example 1 had the highest tensile strength in the following order: Example 5, Example 4, Example 1, Example 3, Example 2, and Comparative Example 1.

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Abstract

Ce procédé de production d'un faisceau de fibres de nanotubes de carbone comprend une étape de formation de faisceau de fibres pour comprimer une pluralité de fibres de nanotubes de carbone et étirer la pluralité de fibres de nanotubes de carbone dans une direction croisant la direction dans laquelle la pluralité de fibres de nanotubes de carbone s'étendent, et former un faisceau de fibres au moyen de la pluralité de fibres de nanotubes de carbone.
PCT/JP2025/015260 2024-05-07 2025-04-18 Procédé de production d'un faisceau de fibres de nanotubes de carbone Pending WO2025234298A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014169521A (ja) * 2013-02-05 2014-09-18 Honda Motor Co Ltd カーボンナノチューブ繊維及びその製造方法
WO2016080526A1 (fr) * 2014-11-21 2016-05-26 リンテック株式会社 Procédé de production de feuille de nanotubes de carbone et feuille de nanotubes de carbone
JP2021050422A (ja) * 2019-09-20 2021-04-01 トクセン工業株式会社 絶縁被覆カーボンナノチューブ線

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014169521A (ja) * 2013-02-05 2014-09-18 Honda Motor Co Ltd カーボンナノチューブ繊維及びその製造方法
WO2016080526A1 (fr) * 2014-11-21 2016-05-26 リンテック株式会社 Procédé de production de feuille de nanotubes de carbone et feuille de nanotubes de carbone
JP2021050422A (ja) * 2019-09-20 2021-04-01 トクセン工業株式会社 絶縁被覆カーボンナノチューブ線

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