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WO2013002564A2 - Composition anti-décollement, stratifié à base de graphène en contenant et procédé de préparation associé - Google Patents

Composition anti-décollement, stratifié à base de graphène en contenant et procédé de préparation associé Download PDF

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Publication number
WO2013002564A2
WO2013002564A2 PCT/KR2012/005102 KR2012005102W WO2013002564A2 WO 2013002564 A2 WO2013002564 A2 WO 2013002564A2 KR 2012005102 W KR2012005102 W KR 2012005102W WO 2013002564 A2 WO2013002564 A2 WO 2013002564A2
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graphene
group
layer
alkyl group
release
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Korean (ko)
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WO2013002564A3 (fr
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최정옥
정준호
권오관
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LMS Co Ltd
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LMS Co Ltd
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    • 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
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material

Definitions

  • the present invention relates to a release preventing composition having excellent adhesion to graphene, a graphene laminate including the composition, and a method of manufacturing the same.
  • Graphene is a term made by combining the suffix -ene, which means a molecule having a double bond of graphite, which means graphite, and a two-dimensional allotrope of carbon, which has hexagonal lattice. do.
  • the infinite plane of graphene shows an energy region where electrons are empty at the point where the valence and conduction bands meet. Looking at the properties of the graph in more detail as follows.
  • the thickness of the graphene layer is about 0.34 nm, which corresponds to one carbon atom, and has a very useful property different from existing materials.
  • carrier mobility in monolayer graphene is up to 200,000 cm 2 / Vs, which is 100 times higher than silicon at room temperature, far beyond the 70,000 cm 2 / Vs of InSb.
  • the electrical resistance at room temperature is also 2/3 smaller than that of copper, and has a current density of 100 to 200 million A / cm 2 to withstand about 100 times the current density of copper. Due to such excellent physical properties, the graphene layer has a very high application potential as an electronic device material, and is applicable to transistors, lasers, touch panels, organic light emitting devices, solar cells, or electrodes of secondary batteries.
  • chemical vapor deposition is a method of preparing a metal catalyst coating film such as copper or a metal catalyst foil in a vacuum furnace and heat-processing at about 1000 ° C. while cooling a carbon source such as methane into a gas phase.
  • This chemical vapor deposition method can produce several layers of uniform graphene thin film in a single layer, and a thin film graphene layer of several nanometers to several hundred nanometers thick and hundreds of nanometers to several micron thick depending on the deposition time. have.
  • the graphene layer formed on the metal catalyst is opaque and thus has poor applicability in itself.
  • a separate transfer technique for transferring only the graphene layer from which the metal catalyst has been removed to the target substrate is required.
  • a polymer is coated and etched on the graphene layer formed on the metal catalyst layer to transfer the graphene layer to the polymer support, which is then placed on the desired target substrate. Thereafter, a method of melting and transferring the polymer support is known.
  • various problems such as crushing, overlapping, or tearing of the graphene layer are generated due to shrinkage of the organic solvent used in the transfer process or the polymer generated during the drying process.
  • the etching process may cause defects such as release, crushing, overlapping, or tearing of the graphene layer by the etching solution.
  • the present invention provides an anti-release composition having excellent adhesion to the graphene layer, a graphene laminate including the composition, and a method of manufacturing the same.
  • the graphene laminate according to the present invention includes a substrate, a release preventing layer and a graphene layer formed on the substrate.
  • the present invention provides an anti-release composition having excellent adhesion to the graphene layer, and provides a method of manufacturing a graphene laminate using the composition.
  • the present invention provides a release preventing composition excellent in adhesion to the graphene layer, the graphene laminate including the composition is low in sheet resistance, excellent in durability can be utilized in various forms of electronic devices.
  • FIG. 1 is a schematic view showing a laminated structure for the graphene laminate according to an embodiment of the present invention
  • FIG. 2 and 3 is a schematic diagram showing a manufacturing process of the graphene laminate according to an embodiment of the present invention, respectively;
  • FIG. 4 is a cross-sectional view showing a laminated structure including a graphene layer according to an embodiment of the present invention
  • Figure 6 is a graph comparing the degree of hydrophobicity by measuring the contact angle of water droplets for the release preventing layer of the present invention
  • FIG. 10 is a photograph of observing the result of transferring the graphene layer on the substrate using an anti-release composition according to an embodiment of the present invention with an optical microscope.
  • the graphene laminate of the present invention includes a substrate, a release preventing layer and a graphene layer formed on the substrate.
  • the anti-release layer of the present invention may include a hydrophobic polymer material.
  • the release preventing layer including the hydrophobic polymer material has an advantage of excellent adhesion with the hydrophobic graphene.
  • the release preventing layer may have a contact angle of 60 ° or more. More specifically, the release preventing layer may have a droplet contact angle of 60 ° to 110 ° range.
  • the droplet contact angle refers to an angle formed when the droplet reaches the thermodynamic equilibrium on the release preventing layer, and the high contact angle indicates low wettability, that is, hydrophobicity.
  • the water droplet contact angle for the release preventing layer according to the present invention exhibits a high contact angle of 60 ° or more, which means that the release preventing layer according to the present invention has excellent adhesion to the hydrophobic graphene.
  • the hydrophobic polymer material may be a hydrocarbon derivative, it may be a structure containing a hydrophobic portion and a polar portion at the same time.
  • the hydrophobic moiety may comprise one or more of C1 to C50 alkyl groups, C4 to C60 cycloalkyl groups, and C6 to C60 aromatic hydrocarbon groups.
  • the polar moiety includes an alcohol group (-OH), a carboxylic acid group (-COOH), a sulfonic acid group (-SO 3 H), an amine group (-NH 2 or -NH-), a carbonyl group (-CO-), It may be a hydrocarbon derivative including at least one of a cyano group (-CN) and a halogen group.
  • the hydrophobic polymer material according to the present invention is not particularly limited, and for example, acrylic, epoxy, silicone, ethylene vinyl acetate, polyvinyl chloride, polyurethane, phenol, polyester, polyether, poly It may include one or more of sulfide-based, polyimide-based and polyamide-based.
  • the release preventing layer according to the present invention has excellent adhesion properties with the graphene layer and the substrate.
  • the release preventing layer may be an acrylic copolymer exhibiting adhesive performance by room temperature or heating.
  • the anti-release layer may effectively bond the graphene layer and the anti-release layer by applying pressure at the same time as normal temperature or heating by facing the graphene layer formed on the metal catalyst layer such as copper foil and the anti-release layer due to the excellent adhesion to the graphene layer. have.
  • Such excellent adhesion properties can increase the transfer efficiency of graphene, and can improve the stability of the graphene layer against external environmental factors.
  • adhesion means maintaining an intimate contact relationship by intermolecular attraction of different materials at the interface between the graphene and the release preventing layer, and adhesion means attraction between atoms, molecules or ions in the release preventing layer. do. Therefore, in order for the release preventing layer to have excellent adhesive properties, it is necessary to simultaneously have excellent adhesion characteristics between the substrate and the graphene layer as well as excellent intermolecular adhesion properties of the material constituting the release preventing layer. In particular, in order to improve the transfer efficiency of the graphene layer to be achieved in the present invention and physical or chemical stability of the transferred graphene layer, excellent adhesion between the graphene layer and the substrate is required.
  • the release preventing layer according to the present invention may have a structure in which a large amount of hydrophobic groups are introduced into a branch chain of an acrylic polymer. This is generally intended to have excellent adhesive properties with the graphene layer showing hydrophobic properties.
  • the hydrophobic group may include, for example, a hydrocarbon derivative composed of a single bond such as an alkyl group and a cycloalkyl group.
  • the hydrophobic group may include an aromatic hydrocarbon derivative including a phenyl group or an aryl group having a large amount of pi electrons. In the case of the aromatic hydrocarbon derivative, it is possible to improve the adhesion with graphene having a large amount of pi electrons.
  • the release preventing layer may include one or more repeating structures of the following Chemical Formulas 1 and 2.
  • R 1 is a C5 to C30 alkyl group
  • R 2 is a C5 to C20 alkyl group; Or a C6 to C30 aryl group having a substituted or unsubstituted C1 to C20 alkyl group,
  • X 1 and X 2 are each independently hydrogen or a C1 to C5 alkyl group
  • n is an integer of 0-10.
  • the release preventing layer according to the present invention may have a structure in which a polar group is introduced to a branch portion of the acrylic polymer to improve adhesion.
  • the release preventing layer may further include a repeating structure of Formula 3 below.
  • R 3 is an alcohol group; Halogen group; Or a C1 to C10 alkyl group containing at least one of an alcohol group, a carboxyl group, a sulfonic acid group, an amine group, a carbonyl group, a cyano group and a halogen group at the terminal,
  • X 3 is hydrogen or an alkyl group of C1 to C5.
  • the release preventing layer according to the present invention can control the adhesion characteristics according to the temperature of the release preventing material by controlling the glass transition temperature, which is an important factor for imparting the adhesive properties.
  • the functional group which gives rigidity like a methyl group can be introduce
  • the release preventing layer may include a repeating structure of Formula 4 below.
  • R 4 is an alkyl group containing a C1 to C10 linear or branched chain
  • X 4 is hydrogen or a C1 to C5 alkyl group.
  • the number of repetitions of the structure shown in Chemical Formulas 1 to 4 is not particularly limited. This is because the repeating structures of Formulas 1 to 4 form one layer while forming a matrix structure.
  • the number of repetitions of the structures of Chemical Formulas 1 to 4 may be independently 1 to 1,000,000, but is not limited thereto.
  • the prepared anti-release layer may have a glass transition temperature in the range of minus 10 °C to image 80 °C.
  • the composition of the release preventing layer is a repeating structure of 60 to 95 mole percent of the repeating structure of Formula 1 and / or 2 having a functional group for improving the adhesion with graphene, the repeating formula of the formula 3 having the adhesion improving function of the adhesive It may include 2 to 20 mol% of the structural fraction, and 3 to 20 mol% of the repeating structural formula (4) having a flexible or rigidity imparting functional group.
  • the sheet resistance of the graphene layer may be 5k ⁇ / sq or less.
  • the sheet resistance of the graphene layer may be in the range of 10 ⁇ / sq to 2.8k ⁇ / sq.
  • the release preventing layer according to the present invention is characterized by a very low sheet resistance. Due to such excellent electrical properties, the graphene laminate of the present invention can be applied to electrodes of various electronic devices.
  • FIG. 1 is a schematic diagram showing a laminated structure of a graphene-coated substrate according to an embodiment of the present invention. Referring to FIG. 1, it can be seen that the substrate 10, the release preventing layer 20 and the graphene layer 30 on the substrate 10 are sequentially stacked.
  • the present invention also provides an anti-release composition comprising a repeating structure of at least one of the following Chemical Formulas 1 and 2.
  • R 1 is an alkyl group of C5 to C30
  • R 2 is an alkyl group of C5 to C20; Or a C6 to C30 aryl group having a substituted or unsubstituted C1 to C20 alkyl group,
  • X 1 and X 2 are each independently hydrogen or an alkyl group of C1 to C5,
  • n is an integer of 0-10.
  • the release preventing composition may further include a structure of Formula 3 below.
  • R 3 is an alcohol group; Halogen group; Or a C1 to C10 alkyl group containing at least one of an alcohol group, a carboxyl group, a sulfonic acid group, an amine group, a carbonyl group, a cyano group and a halogen group at the terminal,
  • X 3 is hydrogen or a C1 to C5 alkyl group.
  • the release control composition may further include a structure of formula (4).
  • R 4 is an alkyl group containing a C1 to C10 linear or branched chain
  • X 4 is hydrogen or a C1 to C5 alkyl group.
  • the anti-release composition according to the invention may comprise a repeating structure of the formula 5 to 8.
  • x, y and z are each independently an integer of 0 or 1 or more, and the range is not particularly limited because the above repeating structures form a matrix structure in the composition.
  • x is each independently an integer of 1 to 1,000,000
  • y and z may each independently be an integer of 0 to 100,000.
  • x, y and z mean molar ratios of the respective chemical formulas.
  • x, y and z may be in a ratio of 60 to 95: 2 to 20: 3 to 20.
  • Anti-release composition according to the invention may have a glass transition temperature of minus 10 °C to image 80 °C range. If the glass transition temperature is below 10 ° C., the mechanical properties of the release preventing layer may be inferior, and the graphene layer transferred to the release preventing layer may be easily damaged. Also, if the glass transition temperature exceeds 80 ° C., the release preventing layer and the graphene may be damaged. The interfacial contact between them is difficult and the adhesion may be degraded.
  • the release barrier layer having the glass transition temperature range may improve thermal and mechanical stability when undergoing an additional curing process after the graphene transfer process.
  • Anti-release composition according to the invention may include one or more of the repeating structure of the formula (1) to 4 described above.
  • the composition ratio of each repeating structure is not particularly limited.
  • the release preventing composition the release preventing composition
  • Formula 4 may include 3 to 20 mol%.
  • the anti-release composition according to the present invention may exhibit excellent adhesion between the graphene layer and the substrate.
  • the composition is a release preventing composition for graphene lamination.
  • the present invention provides a manufacturing method for transferring the graphene layer using the release control composition. Through this manufacturing method it is possible to manufacture a graphene laminate.
  • the manufacturing method For example, the manufacturing method, the manufacturing method, the manufacturing method, and
  • the polymer used in the release preventing composition used in step (a) is not particularly limited, and both curable polymers and non-curable polymers may be used.
  • the lamination step (b) when the release preventing composition is made of a curable polymer may be subjected to a separate curing process.
  • the method may include attaching a graphene layer formed on the metal catalyst layer and a substrate coated with a release preventing composition and irradiating heat or UV.
  • a dry or wet transfer method may be used depending on a method of removing a metal catalyst layer.
  • a roll-to-roll method may be used.
  • the dry transfer method has the advantage that the graphene formed in the metal catalyst layer can be directly transferred onto the target substrate without including a solution process using a solvent or water.
  • the present invention does not exclude a wet process.
  • the metal catalyst layer can be removed using an etching solution.
  • the roll-to-roll system can be used, for example.
  • the graphene layer formed on the metal catalyst layer and the release preventing composition applied on the substrate are laminated to contact each other, and then the metal catalyst layer and the graphene layer are separated by a roll-to-roll method.
  • the metal catalyst layer can be removed using, for example, an etchant.
  • the metal catalyst layer may be removed using an etching solution.
  • the metal catalyst layer is not particularly limited, and for example, a copper or nickel thin film may be used.
  • the etching solution is not particularly limited as long as the metal catalyst layer can be removed, and for example, acid, hydrofluoric acid (HF), buffered oxide etch (BOE), ferric chloride (FeCl 3 ) solution, and ferric nitrate (Fe). (NO 3 ) 3 ) with one or more of the solutions.
  • the graphene layer in the present invention may be a structure formed on both sides of the metal catalyst layer, after attaching a substrate coated with a release preventing composition, respectively, on the outer surface of the graphene layer formed on both sides of the metal catalyst layer, the process of removing the metal catalyst layer It may include.
  • This has the advantage of significantly increasing the manufacturing efficiency in that two graphene laminates can be formed through one manufacturing process. Even in this case, a separate curing process may be performed depending on the type of polymer used. For example, after laminating the substrate coated with the anti-release composition on each of the outer surface of the graphene layer formed on both sides of the metal catalyst layer, it may include a step of irradiating heat or UV.
  • the anti-release composition including the hydrophobic polymer material may include a repeating structure of any one or more of Chemical Formulas 1 to 4 described above.
  • the substrate is polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polycarbonate (PC), polyethersulfone (PES), polycyclic olefin (PCO), polyacrylate (PA), polyether ether ketone ( PEEK) and polyimide (PI).
  • PET polyethylene terephthalate
  • PEN polyethylene naphthalate
  • PC polycarbonate
  • PES polyethersulfone
  • PCO polycyclic olefin
  • PA polyacrylate
  • PEEK polyether ether ketone
  • PI polyimide
  • FIGS. 2 and 3 schematically show a method of manufacturing a graphene laminate according to an embodiment of the present invention, respectively.
  • the release preventing layer 20 is formed by applying a release preventing composition to one surface of the PET substrate 10. Then, the metal catalyst layer 40 on which the graphene layer 30 is formed is laminated. In this case, the release prevention layer 20 and the graphene layer 30 to be in direct contact, it may be in close contact using a roller or the like to increase the adhesion. Although it may vary depending on the composition of the composition constituting the anti-release layer, when the anti-release composition is photocurable, it may include a step of curing through UV irradiation. Then, the metal catalyst layer 40 is removed. Removal of the metal catalyst layer 40 may be performed through a roll-to-roll process.
  • the graphene layer 30 remains on the PET substrate 10 even if the metal catalyst layer is separated by the adhesive force of the release preventing layer 20.
  • the metal catalyst layer 40 can be removed using an etchant.
  • the kind of etching liquid which can be used is not specifically limited. After the metal catalyst layer 40 is removed, a laminated structure consisting of the PET substrate 10, the release preventing layer 20, and the graphene 30 remains.
  • 3 shows a process chart of the graphene transfer method according to another embodiment.
  • 3 discloses a method in which both graphene layers 31 and 32 formed on both surfaces of the metal catalyst layer 40 can be utilized.
  • Two PET substrates 11 and 12 having the release preventing layers 21 and 22 are laminated on the upper and lower graphene layers 31 and 32 of the metal catalyst layer 40, respectively. If necessary, the process of irradiating heat or UV may be further processed. Then, when the metal catalyst layer is removed using a roll-to-roll or etching solution, two laminated structures consisting of the PET substrate 10, the release preventing layers 21 and 22 and the graphene layers 31 and 32 are obtained.
  • This method compared with the conventional graphene transfer method can improve the process efficiency twice, and can minimize the amount of graphene lost in the transfer process.
  • the present invention also provides an intermediate structure of the graphene laminate formed during the transfer process.
  • the intermediate structure is a state before the metal catalyst layer is removed.
  • the graphene laminate may include a structure in which a substrate, a release preventing layer, a graphene layer, a metal catalyst layer, a graphene layer, a release preventing layer, and a substrate are sequentially stacked.
  • 4 shows an example of a graphene laminate.
  • the laminate has a symmetrical structure based on the copper foil 40 which is a metal catalyst layer.
  • the PET substrate 11, the release preventing layer 21, and the graphene layer 31 are sequentially stacked, and the metal catalyst layer 40 is formed on the graphene layer 31.
  • the graphene layer 32, the release preventing layer 22, and the PET substrate 10 are sequentially formed on the metal catalyst layer 40.
  • the present invention provides a graphene device comprising the graphene laminate described above.
  • the graphene device may be utilized in various forms without particular limitation, and for example, may be used in an electronic device in the form of a transparent electrode or a conductive thin film.
  • the graphene device may be applied to a field effect transistor, a laser device, a touch panel using a transparent conductive film, a transparent electrode of an organic light emitting device or a solar cell, an electrode material of a lithium ion secondary battery, and the like.
  • LA lauryl acrylate
  • SA stearyl acrylate
  • NA naphthyl acrylate
  • ENPA ethoxylated nonyl-phenol acrylate
  • acrylic acid AA
  • n-butylacrylate n-butylacrylate, BA
  • the solution was prepared in a composition according to Table 1 above.
  • the prepared solution was coated on a PET film (thickness 75 ⁇ m) by the spin coating method.
  • the solution-coated PET substrate was dried at 70 ° C. for 1 hour to prepare a PET film coated with a release prevention layer having a thickness of about 1 ⁇ m.
  • Copper foil (thickness 25 ⁇ m, purity 99.8%), a metal catalyst having a size of 5 cm ⁇ 5 cm, was charged to a quartz tube for graphene fabrication.
  • the graphene layer formed on the copper foil was transferred onto a PET substrate to which the anti-release composition was applied. Specifically, the surface where the graphene layer was formed on the copper foil and the surface on which the anti-release composition was applied to the PET substrate were faced to each other, and the PET substrate and the copper foil were laminated by applying appropriate heat and pressure. Then, the copper foil was removed with a 1M FeCl 3 aqueous solution to prepare a PET substrate having a graphene layer.
  • a release preventing composition showing hydrophilicity was prepared. Specifically, polyethylene oxide acrylate (PEOA), acrylic acid (AA) and n-butylacrylate (n-butylacrylate, BA) were used as monomers in the mixing ratios shown in [Table 1]. The remaining manufacturing process was carried out under the same conditions as in Example.
  • PEOA polyethylene oxide acrylate
  • AA acrylic acid
  • n-butylacrylate n-butylacrylate
  • the sheet resistance of the graphene laminates prepared in Examples and Comparative Examples was measured by a 4-point probe. Specifically, nine points in arbitrary sections of the graphene laminate were respectively measured. The measurement results are shown in FIG. 5.
  • the graphene laminate coated with the release preventing layer having the hydrophobic or pi-electron functional group of the embodiment it may be confirmed that the graphene laminate coated with the hydrophilic release preventing layer has a very low sheet resistance.
  • the electrical properties of the transferred graphene laminate are lower than that of the transfer layer to the substrate to which the release preventing layer having hydrophobic or pi-electron functional groups is transferred. You can see the fall.
  • the anti-release composition according to Examples 1 to 10 was found to have a water droplet contact angle of 60 ° or more, but was measured to be about 30 ° in the comparative example. Through this, it can be seen that the anti-release composition according to the present invention has a relatively strong hydrophobic tendency.
  • the transmittance of light having a wavelength of 550 nm was measured for the graphene laminates prepared in Examples and Comparative Examples. The measurement results are shown in FIG. 7.
  • the sheet resistance of the graphene laminate prepared in Examples and Comparative Examples was measured according to the bending test. The greater the increase in sheet resistance, the lower the electrical stability of the transferred graphene layer. The measurement results are shown in FIG. 8.
  • the sheet resistance increased rapidly from 6.4 k ⁇ / sq, which is an initial sheet resistance value, to 13.8 k ⁇ / sq.
  • the graphene laminate coated with a hydrophobic release preventing layer or a release preventing layer containing a large number of pi electrons was found to have almost no sheet resistance change.
  • the graphene layer transferred on the PET substrate by Example 3 was observed with an optical microscope.
  • the observation result is shown in FIG. Referring to FIG. 10, the slightly darkened portion in the photograph shows a portion where the graphene layer is transferred onto the PET substrate, and the bright portion shows a PET substrate in which the graphene layer is not transferred.
  • the graph shows that the graphene layer was efficiently transferred onto the PET substrate.

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Abstract

La présente invention concerne une composition anti-décollement adhérant très fortement au graphène, un stratifié à base de graphène en contenant et un procédé de préparation associé, le stratifié à base de graphène ainsi préparé présentant une faible résistance de couche et une remarquable durabilité et pouvant ainsi être utilisé dans divers dispositifs.
PCT/KR2012/005102 2011-06-29 2012-06-28 Composition anti-décollement, stratifié à base de graphène en contenant et procédé de préparation associé Ceased WO2013002564A2 (fr)

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KR101454463B1 (ko) * 2009-09-21 2014-10-23 삼성테크윈 주식회사 그래핀의 제조 방법
ES2717903T3 (es) * 2009-10-16 2019-06-26 Graphene Square Inc Procedimiento de transferencia de rollo a rollo de grafeno, rollo de grafeno producido por el procedimiento, y equipo de transferencia de rollo a rollo para grafeno
KR101603766B1 (ko) * 2009-11-13 2016-03-15 삼성전자주식회사 그라펜 적층체 및 그의 제조방법
KR20110064164A (ko) * 2009-12-07 2011-06-15 서울대학교산학협력단 화학 기상 증착법을 이용한 그래핀 제조방법

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