WO2014069153A1 - カーボンナノチューブ複合成形体の製造方法および製造装置 - Google Patents

カーボンナノチューブ複合成形体の製造方法および製造装置 Download PDF

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Publication number
WO2014069153A1
WO2014069153A1 PCT/JP2013/076894 JP2013076894W WO2014069153A1 WO 2014069153 A1 WO2014069153 A1 WO 2014069153A1 JP 2013076894 W JP2013076894 W JP 2013076894W WO 2014069153 A1 WO2014069153 A1 WO 2014069153A1
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Prior art keywords
carbon nanotube
free end
end side
polymer solution
composite molded
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PCT/JP2013/076894
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English (en)
French (fr)
Japanese (ja)
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井上　鉄也
拓行 円山
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日立造船株式会社
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Priority to JP2014544392A priority Critical patent/JP6270731B2/ja
Publication of WO2014069153A1 publication Critical patent/WO2014069153A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Definitions

  • the present invention relates to a method and apparatus for producing a carbon nanotube composite molded body.
  • the method for producing a carbon nanotube composite molded body according to the present invention after a polymer solution in which fine particles having thermal conductivity or conductivity are mixed with a polymer material is applied to the free end side of the carbon nanotube. Since the permeation of the polymer solution is promoted by leveling the free end side of the carbon nanotube with the leveling member, it is possible to manufacture a high-quality carbon nanotube composite molded body containing no bubbles. In addition, according to this manufacturing method, since the free end side of the carbon nanotube can be exposed from the polymer solution by pressing with the pressing member, the carbon nanotube composite molding having high performance such as thermal conductivity and conductivity is achieved. The body can be manufactured. Furthermore, the production apparatus according to the present invention can produce a carbon nanotube composite molded body with good quality and high performance as described above.
  • the carbon nanotube composite molded body according to the present invention mainly includes a plurality of carbon nanotubes 1 and a polymer material 2 contained in the plurality of carbon nanotubes 1.
  • the carbon nanotubes 1 may be single-walled or multi-walled, and are not particularly limited. In this embodiment, multi-walled carbon nanotubes 1 are used.
  • such a carbon nanotube composite molded body is mainly composed of carbon, and therefore, a heat dissipation material utilizing high thermal conductivity, an absorption material for solar energy, an electromagnetic wave absorption material, a conductive material used for a capacitor, or the like. It is known that it can be used for various applications such as materials having multiple composite performances. Since the carbon nanotube 1 according to the present invention has vertical alignment, these performances can be efficiently exhibited. In this example, in order to further improve these performances, the polymer material 2 was mixed with a fine powder 6 having thermal conductivity or conductivity as shown in FIG. A surface film member 9 and a back film member 10 made of a material having any one of thermal conductivity, conductivity, and electromagnetic wave absorption are formed on the front and back surfaces of the plurality of carbon nanotubes 1, respectively.
  • the “vertically oriented carbon nanotube” refers to a brush-like structure formed by a plurality of carbon nanotubes 1 generated upward (perpendicularly) from the substrate 3 in the same direction.
  • carbon nanotube simply refers to a plurality of carbon nanotubes, that is, a carbon nanotube group or a carbon nanotube layer.
  • the polymer material is contained in the carbon nanotube means that the polymer material 2 is filled between the carbon nanotubes 1 in the carbon nanotube group.
  • the formation method of the carbon nanotube 1 may be a known method and is not particularly limited.
  • an arc discharge method in which an arc discharge is generated between a cathode and an anode made of carbon to generate carbon nanotubes, or a carbon lump mixed with catalyst particles is irradiated with a laser beam to evaporate the carbon to form a catalyst.
  • a laser evaporation method for generating carbon nanotubes by reacting with particles is used.
  • it is generated by a chemical vapor deposition method in which carbon nanotubes are generated by catalyst particles obtained by decomposing hydrocarbons at a high temperature and adhering to the substrate. Specifically, as shown in FIGS.
  • the catalyst particles 5 may be appropriately selected from known materials such as iron (Fe), nickel (Ni), platinum (Pt), and cobalt (Co).
  • the polymer material 2 may also be appropriately selected from known materials such as synthetic resins (fluorinated resins, epoxy resins, etc.) and silicon resins.
  • the polymer material 2 is mixed with fine particles 6 having thermal conductivity or conductivity on the free end side of the carbon nanotubes 1 formed on the surface of the substrate 3.
  • a polymer solution 7 in which fine particles 6 having thermal conductivity or conductivity are mixed with the polymer material 2 at a predetermined ratio by a known method is formed on the substrate 3. It is applied to the free end side of the carbon nanotubes 1 formed on the surface.
  • the fine powder 6 having thermal conductivity or conductivity carbon nanopowder is used in this embodiment, and metal nanoparticles are used in addition to this.
  • the application means the polymer solution application means 23b shown in FIG. 4
  • known ones such as a nozzle, a spray nozzle, an industrial brush, and an industrial spatula are used.
  • the polymer solution 7 may be dropped on the free end side of the carbon nanotube 1 and extended with an industrial brush or the like, or the polymer solution 7 may be coated with a nozzle or the like.
  • the surface of the applied polymer solution 7 is leveled by bringing the free end portion of the carbon nanotube 1 into contact with the leveling member 24.
  • the air contained between the carbon nanotubes 1 escapes, and the polymer solution 7 can permeate to the base end side. Accordingly, since the polymer solution 7 is solidified without containing bubbles, a high-quality carbon nanotube composite molded body can be manufactured as a result. In some cases, some free end portions of the carbon nanotubes 1 can be exposed from the polymer solution 7.
  • a roller is used as the leveling member 24.
  • a blade may be used.
  • the material of the roller or blade may be any material having a low affinity with the polymer material 2, and for example, PTFE (PolyTetraFluoroEthylene) or glass is used.
  • the pressing step is performed while heating the carbon nanotubes 1 containing the fine particles 6 and the polymer solution 7 by the heating means (the heating element 25c shown in FIG. 4).
  • the heating means may be any known one, and for example, a heating element such as a heat plate is used. Further, the position of the heating means is not particularly limited, and for example, heating may be performed from the free end side of the carbon nanotube 1 or from the proximal end side.
  • the molded product formed by the pressing step that is, the carbon nanotube 1 containing the fine particle 6 and the polymer material 2 may be referred to as a polymer-containing carbon nanotube layer 8 for convenience.
  • thermosetting resin for example is selected among the above-mentioned polymeric materials 2, if it heats at the temperature and time required for the solidification of the polymeric material 2, Good.
  • the free end side of the carbon nanotube 1 is interposed between the pressing member 25a and the free end side of the carbon nanotube 1 as shown in FIG. 2C.
  • a protective member 25b capable of protecting the damage is provided.
  • the protective member 25b is made of, for example, an endless sheet (endless sheet) made of a metal plate, a net, a porous member, or the like, and the material is not particularly limited.
  • the protective member 25b is a porous member or a net-like material, specifically, a sheet made of carbon fiber or a sheet made of metal fiber, A metal mesh plate, a punched metal plate, or the like is used.
  • a member provided with a vent hole in the portion of the pressing member 25a that contacts the free end portion of the carbon nanotube 1 may be used.
  • the free end portion of the carbon nanotube 1 is exposed from the polymer material 2, the heat absorption and heat dissipation performance, the conductive performance, the electromagnetic wave absorption performance and the like are improved.
  • the molded body can be manufactured. Further, when the base end portion of the carbon nanotube 1 is peeled from the substrate 3, the polymer-containing carbon nanotube layer 8 is exposed from the polymer material 2 on the free end side and the base end side, so that the carbon nanotube composite molding has further improved performance.
  • the body can be manufactured.
  • the vertically aligned carbon nanotubes 1 can be confirmed to be conductive by this method is that the fine particles 6 having thermal conductivity or conductivity exist between the carbon nanotubes, and the carbon nanotubes in the brush-like structure. This is because an electrical path is formed by the fact that they are in contact with each other.
  • the free end side of the carbon nanotube 1 is cut with a laser beam, and the surface side of the polymer-containing carbon nanotube layer 8 is planarized.
  • a laser beam irradiation step may be provided. Should the free end side of the carbon nanotube 1 be covered with the polymer material 2 in the polymer-containing carbon nanotube layer 8, the surface side of the polymer-containing carbon nanotube layer 8 is planarized by laser processing. Thus, the free end portion of the carbon nanotube 1 can be more reliably exposed from the polymer material 2.
  • a surface film-like member forming step for forming the surface film-like member 9 on the free end side of the carbon nanotube 1 is provided after the pressing step. That is, as shown in FIG. 3A, the surface film member 9 is laminated on the polymer-containing carbon nanotube layer 8.
  • the material of the surface film-like member 9 may be appropriately selected depending on the application, and is not particularly limited. Since the surface film-like member 9 according to the present embodiment is used as a heat absorbing and radiating material or an electromagnetic wave absorbing material, a material having any one of thermal conductivity, conductivity and electromagnetic wave absorbing property may be selected. Specifically, as the surface film-like member 9, a conductive material such as Au, Cu, Al or the like is used. Also, a known method such as coating, sputtering, or vapor deposition is used as the forming method.
  • the back face film-like member 10 is formed on the base end side of the carbon nanotube 1.
  • a back membrane member forming step about the method of peeling the base end part of the carbon nanotube 1 from the board
  • the substrate protective film 4 is formed on the surface of the substrate 3, the base end portion of the carbon nanotube 1 is naturally peeled from the substrate protective film 4.
  • the back surface film-shaped member 10 should just be formed by the same or different well-known method, using the surface film-shaped member 9 and the material which has the same performance with the same material or a different material.
  • the front membrane member 9 and the back membrane member 10 are formed on the polymer-containing carbon nanotube layer 8, both ends exposed from the polymer material 2 of the carbon nanotube 1 are directly attached to the surface.
  • the membrane member 9 and the back membrane member 10 can be brought into contact with each other.
  • the carbon nanotube composite molded object which has the structure which makes performances, such as thermal conductivity, electroconductivity, and electromagnetic wave absorptivity of the carbon nanotube 1, exhibit effectively, is formed. be able to.
  • a test piece of a carbon nanotube composite molded body having a thickness of about 100 ⁇ m was produced under the following conditions.
  • a polymer solution 7 was prepared by mixing NMP (N-methylpyrrolidone) with PVDF (Polyvinylidene DiFluoride) at 5 weight percent or 10 weight percent and further mixing acetylene black with 1 weight percent.
  • NMP N-methylpyrrolidone
  • PVDF Polyvinylidene DiFluoride
  • the pressing pressure was 9.80 ⁇ 10 4 to 19.6 ⁇ 10 4 Pa (1-2 kgf / cm 2 )
  • the heating temperature was 110 ° C.
  • the heating time was 2 minutes.
  • aluminum is used as the material of the surface film member 9 and the back film member 10, and the surface film member 9 and the back film member 10 are formed by sputtering. did.
  • the film thickness of the formed front film member 9 and back film member 10 was 50 to 100 nm.
  • thermoelectric element As a result of measuring the thermal conductivity of this test piece, it was 10 W / (m ⁇ K). Also, the characteristics of the thermoelectric element in the case where one end side of a commercially available thermoelectric element is cooled by a fan and the other end side is heated by lamp irradiation, and the test piece is not attached to the other end side. Each was measured. As a result, the output voltage was 60 mV when the test piece was not attached, whereas the output voltage was about 7 times as high as 400 mV when the test piece was attached. Therefore, it was confirmed that this test piece has a highly efficient endothermic property.
  • the value of the thermal conductivity of the test piece of the above-mentioned carbon nanotube composite molded body the significance of 10 W / (m ⁇ K), will be described in comparison with a metal sheet having a high thermal conductivity.
  • a metal sheet When used as a heat dissipation material, a metal sheet is bonded to a heat dissipation object such as a thermoelectric element using an adhesive, and thus heat conduction is performed via the adhesive. Therefore, it can be said that the heat dissipation characteristic of the metal sheet is determined by this adhesive as a result.
  • heat radiation adhesive heat radiation grease having high heat radiation characteristics can be mentioned, and its thermal conductivity is about 3 to 4 W / (m ⁇ K) at maximum.
  • the test piece of the carbon nanotube composite molded body uses the nano-sized fiber shape of the carbon nanotube 1 and uses the heat flow action in the length direction. Specifically, in this test piece, the carbon nanotube 1 is in close contact with fine irregularities (so-called surface roughness) on the surface of the thermoelectric element, and heat transferred from the thermoelectric element is transferred in its length direction.
  • the present invention is an apparatus for manufacturing a carbon nanotube composite molded body in which a polymer material 2 is contained in vertically aligned carbon nanotubes 1 that are moved in a predetermined direction via a substrate 3. That is, it is a roll-to-roll manufacturing apparatus that sequentially performs each manufacturing process while moving the vertically aligned carbon nanotubes 1 in a predetermined direction via the substrate 3. More specifically, in the present embodiment, from the unwinding roll 21 on which the substrate 3 on which the vertically aligned carbon nanotubes 1 are formed is unwound toward the winding roll 22 on which the carbon nanotube composite molded body is wound. Normally, the substrate is moved in the horizontal direction.
  • the manufacturing apparatus is a part of the manufacturing equipment provided in the manufacturing factory, and may be used in combination with another manufacturing apparatus.
  • a polymer solution 7 in which fine particles 6 having thermal conductivity or conductivity are mixed with the polymer material 2 is applied to the carbon nanotubes 1 formed on the surface of the substrate 3 along the movement path of the substrate 3.
  • a polymer solution coating device 23 having a polymer solution coating means 23b, a leveling member 24 for leveling the free end side of the carbon nanotube 1, and a free end side of the carbon nanotube 1 of the polymer solution 7 are pressed in a plane.
  • a carbon nanotube forming apparatus 25 having a pressing member 25a.
  • the leveling member 24 promotes the penetration of the polymer solution 7 applied by the polymer solution coating device 25 into the base end side of the carbon nanotube 1.
  • the leveling member 24 is provided to level the surface of the applied polymer solution 7. More specifically, the leveling member 24 is a glass roller that rotates in the same direction as the unwinding roll 21, and is provided on the free end side of the carbon nanotube 1 and at a height in contact with the free end portion. ing.
  • This leveling member (roller) 24 allows air contained between the carbon nanotubes 1 to escape, and allows the polymer solution 7 to permeate the base end side of the carbon nanotubes 1. In some cases, some free end portions of the carbon nanotubes 1 can be exposed from the polymer solution 7.
  • the leveling member 24 only needs to be provided at a position at least so as to contact the free end portion of the carbon nanotube 1 during operation. Specifically, in this embodiment, the distribution of the height of the carbon nanotubes 1 from the surface of the substrate 3 (the length of the carbon nanotubes) is 100 ⁇ m ⁇ 10%. The lower end portion is provided so as to be positioned 70 ⁇ m away from the surface of the substrate 3.
  • the carbon nanotube forming apparatus 25 includes a pressing member 25a that is disposed on the free end side of the carbon nanotube 1 and presses the free end portion of the carbon nanotube 1 from above.
  • the pressing member 25 a is moved downward from a position away from the free end portion of the carbon nanotube 1 by a predetermined distance to press the free end portion of the carbon nanotube 1.
  • the pressure F is evenly applied to a certain region on the free end side of the carbon nanotube 1, and the free end portion of the carbon nanotube 1 can be exposed from the polymer solution 7.
  • the carbon nanotube forming apparatus 25 is further disposed between the pressing member 25a and the free end side of the carbon nanotube 1 so as to move together with the substrate 3 so that the free end side of the carbon nanotube 1 is located.
  • a protective member 25b for protection is provided.
  • a metal plate formed in an endless sheet, a net-like material, a porous member, or the like is used for the protective member 25b, and the material is not particularly limited.
  • a sheet made of carbon fiber is used as the protective member 25b.
  • the protective member 25b is an endless sheet made of carbon fiber, and is moved at the same direction and at the same speed as the substrate 3 by four rolls rotating in the opposite direction to the unwinding roll 21.
  • the said performance as a carbon nanotube composite molded object can be improved by the polymer solution 7 containing the fine particle 6 which has heat conductivity or electroconductivity. And the said performance as a carbon nanotube composite molded object can further be improved by exposing the free end part of a carbon nanotube by the pressing member 25a. Further, since the above structure can use the movement of the substrate, it can be easily applied to a continuous manufacturing method, and the manufacturing cost can be reduced.
  • the carbon nanotube forming apparatus 25 is provided with a heating means. Specifically, a heating element 25c that is disposed at a position facing the pressing member 25a and that heats the back side of the substrate 3 is provided.
  • a heating element 25c that is disposed at a position facing the pressing member 25a and that heats the back side of the substrate 3 is provided.
  • a heat plate is used, so that a certain area on the back side of the substrate 3 can be heated simultaneously, and the manufacturing efficiency is improved.
  • FIG. 4 if the contact area
  • the surface film-like member forming device 26 for forming the surface film-like member 9 on the free end side of the carbon nanotube 1 is provided behind the carbon nanotube forming device 25 (lower side). It has been.
  • the surface film member forming apparatus 26 includes a material storage tank 26a for storing the material, an application means 26b connected to the material storage tank 26a for applying the material, and a surface to which the applied material is fixed. And a drying heater 26c as the film-like member 9.
  • the surface film member 9 is formed using a conductive material.
  • the conductive material stored in the material storage tank 26a is applied to the polymer-containing carbon nanotube layer 8 by a nozzle used as the application unit 26b, and the drying heater is used.
  • the surface film member 9 is dried by 26c.
  • the film is formed by a coating method, but a known method may be used and is not particularly limited.
  • the surface film member forming apparatus 26 may be provided with a decompression chamber, a vacuum chamber, or the like, and the surface film member 9 may be formed in these chambers.
  • a peeling cutter is used as the peeling means 27.
  • a known method may be used as the peeling unit 27.
  • a laser beam irradiation unit may be used. After the base end portion of the carbon nanotube 1 is peeled from the substrate 3, the substrate 3 is taken up and collected by the substrate take-up roll 28, and the rest other than the substrate 3 is continuously moved in a predetermined direction.
  • the back membrane member forming apparatus 29 is an apparatus having the same material and the same configuration as the front membrane member forming apparatus 26 in this embodiment, and the back membrane film on the base end side of the carbon nanotube 1.
  • a shaped member 10 is formed. That is, the back membrane member forming apparatus 29 includes a material storage tank 29a for storing the material, a nozzle used as an application means 29b connected to the material storage tank 29a and applying the material, and the applied material fixed to the back membrane. And a drying heater 29c as a shape member 10.
  • the surface film-like member 9 may be formed of a material different from that of the surface film-like member 9 and a device having a different configuration.
  • the carbon nanotube composite molded body produced as described above is finally wound on the winding roll 22.
  • both ends exposed from the polymer material 2 of the carbon nanotube 1 are directly attached to the surface film. It is possible to form a carbon nanotube composite molded body having a structure that can be brought into contact with the cylindrical member 9 and the back membrane member 10 and that can effectively exhibit the performance of the carbon nanotubes 1 and that has further improved performance.
  • the continuous manufacturing method and the manufacturing apparatus of the carbon nanotube composite molded body have been described, but the present invention can also be applied to a so-called batch manufacturing method and manufacturing apparatus in which the substrate is not continuously moved.
  • the protective member 25b may not be provided, and when provided, the protective member 25b is not limited to the endless sheet, and may be a flat plate-like member.

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PCT/JP2013/076894 2012-11-05 2013-10-03 カーボンナノチューブ複合成形体の製造方法および製造装置 WO2014069153A1 (ja)

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WO2017154885A1 (ja) * 2016-03-09 2017-09-14 日立造船株式会社 カーボンナノチューブ構造体の起毛方法、カーボンナノチューブ構造体の製造方法およびカーボンナノチューブ構造体
KR101789719B1 (ko) * 2016-04-08 2017-10-25 서울대학교산학협력단 탄소나노튜브 전극 및 그 형성 방법
JP2018067581A (ja) * 2016-10-17 2018-04-26 富士通株式会社 カーボンナノチューブ構造、放熱シート及びカーボンナノチューブ構造の製造方法
WO2018179668A1 (ja) * 2017-03-31 2018-10-04 日立造船株式会社 フィラー・樹脂複合体、フィラー・樹脂複合体の製造方法、フィラー・樹脂複合層、および、フィラー・樹脂複合体の使用方法
WO2019167496A1 (ja) * 2018-03-01 2019-09-06 日立造船株式会社 カーボンナノチューブ複合体の製造方法および多孔質金属材料の製造方法
CN110391340A (zh) * 2018-04-16 2019-10-29 清华大学 聚合物太阳能电池的制备方法
JP2020530432A (ja) * 2017-08-08 2020-10-22 リンテック・オヴ・アメリカ，インコーポレイテッド エッジ面を使用したナノファイバシートの密度の変更

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JP2018067581A (ja) * 2016-10-17 2018-04-26 富士通株式会社 カーボンナノチューブ構造、放熱シート及びカーボンナノチューブ構造の製造方法
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JP2018171809A (ja) * 2017-03-31 2018-11-08 日立造船株式会社 フィラー・樹脂複合体、フィラー・樹脂複合体の製造方法、フィラー・樹脂複合層、および、フィラー・樹脂複合体の使用方法
JP2020530432A (ja) * 2017-08-08 2020-10-22 リンテック・オヴ・アメリカ，インコーポレイテッド エッジ面を使用したナノファイバシートの密度の変更
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