WO2013062182A1 - Procédé de fabrication d'un film composite de graphène par utilisation d'irradiation par micro-ondes et lumière pulsée intense (ipl) - Google Patents

Procédé de fabrication d'un film composite de graphène par utilisation d'irradiation par micro-ondes et lumière pulsée intense (ipl) Download PDF

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Publication number
WO2013062182A1
WO2013062182A1 PCT/KR2012/000464 KR2012000464W WO2013062182A1 WO 2013062182 A1 WO2013062182 A1 WO 2013062182A1 KR 2012000464 W KR2012000464 W KR 2012000464W WO 2013062182 A1 WO2013062182 A1 WO 2013062182A1
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WIPO (PCT)
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substrate
graphene
composite film
layer
irradiation
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PCT/KR2012/000464
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English (en)
Korean (ko)
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유명재
양우석
이우성
김형근
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전자부품연구원
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Publication of WO2013062182A1 publication Critical patent/WO2013062182A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/28—Treatment by wave energy or particle radiation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • C08J7/16—Chemical modification with polymerisable compounds
    • C08J7/18—Chemical modification with polymerisable compounds using wave energy or particle radiation

Definitions

  • the present invention relates to a graphene composite film manufacturing method, and more particularly to a graphene composite film manufacturing method using microwave and IPL (high sensitivity light source) irradiation.
  • Graphene (Graphene), which is in the spotlight recently, is flexible, has a very high electrical conductivity, and is transparent. Therefore, studies are being actively conducted to use it as a transparent and curved electrode or as an electron transport material such as an electron transport layer in an electronic device.
  • a graphene is grown by supplying a reaction source including a carbon source on the metal catalyst and performing heat treatment at atmospheric pressure, which has a problem that a high temperature of 1000 or more is required.
  • a reaction source including a carbon source on the metal catalyst
  • heat treatment at atmospheric pressure
  • Embodiments of the present invention to form a graphene layer by microwave and / or IPL (high sensitivity light source) irradiation, to provide a graphene composite film manufacturing method capable of forming a graphene layer at a high speed at a relatively low temperature.
  • IPL high sensitivity light source
  • IPL Intensed Pulse Light
  • the substrate is a non-catalyst substrate, a metal substrate or a substrate on which a metal base layer is formed
  • the non-catalytic substrate is a polyethylene terephthalate (PET) substrate, a polyethersulfone (PES) substrate, a polyimide substrate, a boron nitride substrate, Si A substrate, a Si / Si02 substrate, a Si3N4 substrate, a sapphire substrate, a quartz substrate, and a glass substrate.
  • the metal substrate or the metal substrate layer may be formed of silicon, Ni, Co, Fe, Pt, At least one metal selected from the group consisting of Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V, Zr, brass, bronze, cupronickel, stainless steel and Ge or It can be made of an alloy.
  • the polymer layer including the carbon source may be at least one selected from polymethacrylate, polystyrene, acrylonitrile butadiene styrene (ABS), self-assembled monolayer (SAM), and polyimide.
  • the second step may heat the polymer layer to 1000 to 1500 through at least one heat source of the microwave irradiation and IPL (Intensed Pulse Light) irradiation.
  • IPL Intensed Pulse Light
  • the graphene composite film manufacturing method may further include a third step of coating the metal catalyst particles on the first graphene layer after the second step.
  • the metal catalyst particles are silicon, Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V, Zr, brass, One or more metals or alloys selected from the group consisting of bronze, cupronickel, stainless steel and Ge.
  • the graphene composite film manufacturing method after the third step, by laminating a second graphene layer on the first graphene layer, at least of microwave irradiation and IPL (Intensed Pulse Light) irradiation
  • the method may further include a fourth step of locally melting the metal catalyst particles through at least one heat source to bond the second graphene layer to an upper portion of the first graphene layer.
  • a graphene composite film manufactured by the graphene composite film manufacturing method according to an aspect of the present invention may be provided.
  • Embodiments of the present invention by heating the polymer layer containing a carbon source through microwave and / or IPL (high sensitivity light source) irradiation, it is possible to form a graphene layer at a low speed at a high speed.
  • IPL high sensitivity light source
  • FIG. 1 is a first process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • FIG. 2 is a second process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • FIG. 3 is a third process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • FIG. 4 is a fourth process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • FIG. 5 is a fifth process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • FIG. 1 is a first process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • a polymer layer 120 including a carbon source is coated on the substrate 110.
  • the substrate 110 may have transparency, flexibility, stretchability, or a combination thereof.
  • the substrate 110 may be a catalyst-free substrate.
  • the catalyst-free substrate may be a polyethyleneterephthalate (PET) substrate, a polyethersulfone (PES) substrate, a polyimide substrate, a boron nitride substrate, a Si substrate, or a Si / Si0 2. It may be at least one selected from a substrate, a Si 3 N 4 substrate, a sapphire substrate, a quartz substrate, and a glass substrate.
  • the substrate 110 may be a metal substrate or may further include a metal substrate layer (not shown) formed between the substrate 110 and the polymer layer 120.
  • the metal substrate layer may be formed on the substrate 110 using a conventional deposition or coating method.
  • the metal in the metal substrate or the metal substrate layer is, for example, silicon, Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, At least one metal or alloy selected from the group consisting of W, U, V, Zr, brass, bronze, cupronickel, stainless steel and Ge. 1 to 5 show that the substrate 110 is shown only in the case of a non-catalyst substrate.
  • the shape of the substrate 110 is not limited.
  • the substrate 110 may have the form of a sheet, rod or wire.
  • the following description will be made with respect to the case where the substrate 110 is formed in a sheet shape.
  • the polymer layer 120 (hereinafter, referred to as a polymer layer) including a carbon source may serve as a seed layer for graphene synthesis.
  • the polymer layer 120 may be, for example, at least one selected from polymethacrylate, polystyrene, acrylonitrile butadiene styrene (ABS), self-assembled monolayer (SAM), and polyimide.
  • Examples of the carbon source may be carbon monoxide, carbon dioxide, methane, ethane, ethylene, ethanol, acetylene, propane, butane, butadiene, pentane, pentene, cyclopentadiene, hexane, cyclohexane, benzene, toluene and the like.
  • the method of forming the polymer layer 120 is not limited.
  • the polymer layer 120 may use a conventional coating method or a coating method such as spin coating, dip coating, and spray coating on the substrate 110 (first step above).
  • FIG. 2 is a second process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • the polymer layer 120 is heated through at least one heat source of microwave irradiation and IPL (Intensed Pulsed Light) irradiation in which the polymer layer 120 is coated on the substrate 110.
  • the first graphene layer 130 is formed.
  • the polymer layer 120 may be heated to 300 to 1000 through the heat source. Therefore, it is possible to form a graphene layer at a temperature relatively lower than the conventional graphene synthesis temperature.
  • microwave refers to electromagnetic radiation having a wavelength between 1 and 0.1 m generated by Klystron and Magnetron in an electromagnetic wave having a wavelength between radio waves and infrared rays.
  • the microwave heating method has the advantage of heating the inside of the material at the same time by selectively heating only the material absorbing the frequency to vibrate the molecules according to the frequency.
  • IPL Intensed Pulsed Light, short white wavelength
  • the IPL irradiation has the advantage of changing pulses at high speed and heating without damaging the substrate.
  • the microwave irradiation and / or IPL irradiation may be performed using a microwave irradiation device and an IPL irradiation device that are commonly used.
  • a photoreactive polymer for example, polyvinyl alcohol (PVP)
  • PVP polyvinyl alcohol
  • the graphene layer may be directly synthesized at the same time by removing the surface oxide layer by rapidly heating at a relatively low temperature.
  • the first graphene layer 130 formed through microwave irradiation and / or IPL irradiation is a graphene layer in which a plurality of carbon atoms are covalently connected to each other to form polycyclic aromatic molecules to form a layer or sheet.
  • the covalently linked carbon atoms form a 6-membered ring as shown in FIG. 1 as a basic repeating unit, but is not limited thereto. That is, the carbon atoms may be formed of a 5-membered ring, a 7-membered ring, or the like.
  • the first graphene layer 130 may be formed of a single layer, but is not limited thereto and may be formed of a plurality of layers.
  • the first graphene layer 130 may be formed of 50 layers.
  • the first graphene layer 130 may be formed in a large area, and for example, the first graphene layer 130 may be formed to have a length in the transverse or longitudinal direction of about 1 mm or more to 1000 m (above the second step).
  • FIG. 3 is a third process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • the graphene composite film manufacturing method according to an embodiment of the present invention may further include coating the metal catalyst particles 140 on the first graphene layer 130.
  • the metal catalyst particles 140 may serve as a medium for bonding the first graphene layer 130 and the second graphene layer 150 to be described later.
  • the metal in the metal catalyst particles 140 is not limited to a specific kind, for example, silicon, Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta And at least one metal or alloy selected from the group consisting of Ti, W, U, V, Zr, brass, bronze, cupronickel, stainless steel and Ge.
  • the method of coating the metal catalyst particles 140 on the first graphene layer 130 is not limited.
  • FIG. 4 is a fourth process chart of the graphene composite film manufacturing method according to an embodiment of the present invention
  • Figure 5 is a fifth process chart of the graphene composite film manufacturing method according to an embodiment of the present invention.
  • the second graphene layer 150 is laminated on the first graphene layer 130, microwave irradiation and / or IPL.
  • the method may further include locally melting the metal catalyst particles 140 through irradiation to bond the second graphene layer 150 to an upper portion of the first graphene layer 130.
  • the second graphene layer 150 is the same as or similar to the first graphene layer 130 and may be manufactured by the same or similar method as the first graphene layer 130. The duplicate description will be omitted.
  • the second graphene layer 150 may be manufactured by a method different from the first graphene layer 130. For example, it is possible to manufacture the second graphene layer 150 by directly growing graphene on a metal catalyst and then removing the metal catalyst.
  • the microwave irradiation and the IPL irradiation may selectively and locally melt the metal catalyst particles 140 coated on the first graphene layer 130, and thus, the first graphene layer 130 and the second graphene without remaining contaminants.
  • the graphene layer 150 may be bonded.
  • a graphene composite film manufactured according to the graphene composite film manufacturing method according to the above embodiments may be provided.
  • the graphene composite film may be used in the manufacture of electrodes (especially transparent electrodes) of various electronic and electronic devices such as next-generation field effect transistors or diodes requiring flexibility and / or stretchability, or in photovoltaics, touch sensors, and related flexible electronic technologies. It is possible to be used as graphene transparent electrode for miracle applications.
  • embodiments of the present invention can form a graphene layer at a low speed at a low speed by heating a polymer layer including a carbon source through microwave and / or IPL (high sensitivity light source) irradiation.
  • a polymer layer including a carbon source through microwave and / or IPL (high sensitivity light source) irradiation.
  • IPL high sensitivity light source

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

L'invention propose un procédé de fabrication d'un film composite de graphène. Le procédé de fabrication d'un film composite de graphène conformément à un mode de réalisation de la présente invention comprend : une première étape consistant à appliquer une couche de polymère contenant une source de carbone sur une surface supérieure d'un substrat ; et une seconde étape consistant à chauffer la couche de polymère par utilisation d'au moins une source de chaleur d'irradiation par micro-ondes et d'irradiation par lumière pulsée intense (IPL) pour former une première couche de graphène.
PCT/KR2012/000464 2011-10-26 2012-01-19 Procédé de fabrication d'un film composite de graphène par utilisation d'irradiation par micro-ondes et lumière pulsée intense (ipl) WO2013062182A1 (fr)

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KR10-2011-0110007 2011-10-26
KR1020110110007A KR101236138B1 (ko) 2011-10-26 2011-10-26 마이크로파 및 ｉｐｌ조사를 이용한 그래핀 복합필름 제조방법

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Cited By (1)

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CN106832363A (zh) * 2016-12-31 2017-06-13 南京新月材料科技有限公司 石墨烯改性聚酰亚胺基复合薄膜的制备方法及柔性电路板

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KR101918299B1 (ko) * 2011-11-09 2018-11-13 주식회사 삼천리 표면에 그래핀이 형성된 금속선 또는 판재의 제조방법
KR101512412B1 (ko) 2013-03-06 2015-04-15 성균관대학교산학협력단 투명 전극 및 이의 제조 방법
KR101600395B1 (ko) * 2014-04-01 2016-03-07 성균관대학교산학협력단 투명 전극 및 이의 제조 방법
CN104211977B (zh) * 2014-09-10 2017-01-25 浙江碳谷上希材料科技有限公司 一种基于石墨烯复合膜的制备方法
US10626231B2 (en) 2016-12-28 2020-04-21 King Fahd University Of Petroleum And Minerals Microwave irradiated poly(vinyl alcohol) and graphene nanocomposite
KR102131057B1 (ko) * 2018-10-04 2020-07-07 한국기계연구원 면광원을 이용한 그래핀 필름 제조방법
KR102606035B1 (ko) * 2019-08-28 2023-11-24 부산대학교 산학협력단 레이저를 이용한 센서제조방법 및 이 방법에 의하여 제조된 센서
KR20230031641A (ko) 2021-08-27 2023-03-07 부산대학교 산학협력단 나노패턴 고분자 필름의 표면 경도 및 인성 제어 방법
CN115108550B (zh) * 2022-07-18 2023-02-28 哈尔滨工业大学 一种减少石墨膜面内缺陷的改性处理方法

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CN106832363A (zh) * 2016-12-31 2017-06-13 南京新月材料科技有限公司 石墨烯改性聚酰亚胺基复合薄膜的制备方法及柔性电路板

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