KR101110578B1 - Producing method of highly oriented graphene containing coating-products and film - Google Patents

Producing method of highly oriented graphene containing coating-products and film Download PDF

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KR101110578B1
KR101110578B1 KR1020090102067A KR20090102067A KR101110578B1 KR 101110578 B1 KR101110578 B1 KR 101110578B1 KR 1020090102067 A KR1020090102067 A KR 1020090102067A KR 20090102067 A KR20090102067 A KR 20090102067A KR 101110578 B1 KR101110578 B1 KR 101110578B1
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graphene
coating
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coating film
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KR20110045466A (en
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허승헌
최성호
주혜미
지영호
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거림테크 주식회사
한국세라믹기술원
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • 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
    • 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
    • C08J7/04—Coating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/80—Processes for incorporating ingredients

Abstract

본 발명은 2차원적 평면 그라핀이 함유된 코팅물 제조시 간단한 압착 공정을 추가함으로서 그라핀 함유 코팅막 내의 그라핀들이 기판의 표면축과 같은 일방향으로 배열이 되고 동시에 그라핀간 면간 겹침이 크게 향상되는 제조방법에 관한 기술이다.The present invention is to add a simple pressing process in the production of a coating containing two-dimensional planar graphene graphene in the graphene-containing coating film is arranged in one direction, such as the surface axis of the substrate and at the same time the inter-graphene overlap between the surface is greatly improved It is a technique regarding a manufacturing method.

본 발명은 (a) 그라핀 함유 액상물을 마련하는 단계; (b) 상기 그라핀 함유 액상물을 모재에 코팅하여 코팅막을 형성시키는 단계; 및 (c) 상기 코팅막을 압착하는 단계; 를 포함하는 배향(配向) 그라핀 함유 코팅물 제조방법을 제공한다.The present invention comprises the steps of (a) preparing a graphene-containing liquid; (b) coating the graphene-containing liquid on a base material to form a coating film; (C) pressing the coating film; It provides a method for producing an orientation (i) graphene-containing coating comprising a.

그래핀, 그래핀 산화물, 분산, 코팅, 복합체 Graphene, Graphene Oxide, Dispersion, Coatings, Composites

Description

배향 그라핀 함유 코팅물 제조방법 및 배향 그라핀 함유 필름 제조방법{Producing method of highly oriented graphene containing coating-products and film}Production method of highly oriented graphene containing coating-products and film

본 발명은 2차원적 평면 그라핀이 함유된 코팅물 제조시 간단한 압착 공정을 추가함으로서 그라핀 함유 코팅막 내의 그라핀들이 기판의 표면축과 같은 일방향으로 배열이 되고 동시에 그라핀간 면간 겹침이 크게 향상되는 제조방법에 관한 기술이다.The present invention is to add a simple pressing process in the production of a coating containing two-dimensional planar graphene graphene in the graphene-containing coating film is arranged in one direction, such as the surface axis of the substrate and at the same time the inter-graphene overlap between the surface is greatly improved It is a technique regarding a manufacturing method.

그라핀 박막을 제조하는 방법으로는 촉매를 이용하는 CVD(Chemical vapor deposition)법과 액상 분산 기술을 이용한 코팅방법(딥코팅, 프린팅, 스크린프린팅, 스프레이코팅, 그라비아코팅, 스핀코팅, 롤코팅, 롤-투-롤 코팅 등)이 보편적으로 이용되고 있다.As a method for producing a graphene thin film, a chemical vapor deposition (CVD) method using a catalyst and a coating method using a liquid dispersion technique (deep coating, printing, screen printing, spray coating, gravure coating, spin coating, roll coating, roll-to Roll coatings, etc.).

전자는 특정 촉매를 기판 위에 형성시키고 기판을 가열하여 하이드로 카본 전구체가 열적-화학적 작용에 의해 깨지면서 촉매부에서 그라핀 박막이 성장되도록 하는 방법이다. 이러한 CVD법은 단층 혹은 2-3층 그라핀 제조에 매우 중요한 기술이며 차세대 고속 트랜지스터 제조에 핵심 기술로 평가받고 있다. 이러한 CVD법은 고품질 그라핀이 기판과 평행하게 성장되지만 대면적으로 실행시키기는 어려우며, 또한 고가 장비가 요구되는 문제점이 있다.The former is a method of forming a specific catalyst on the substrate and heating the substrate so that the graphene thin film is grown in the catalyst portion while the hydrocarbon precursor is broken by thermal-chemical action. This CVD method is a very important technology for the production of single layer or 2-3 layer graphene and is evaluated as a key technology for the next generation high speed transistor manufacturing. This CVD method has a problem that high-quality graphene is grown in parallel with the substrate but difficult to implement in large areas, and expensive equipment is required.

후자는 합성 혹은 제조된 그라핀을 용매에 넣고 추가로 바인더, 분산제, 계면활성제와 같은 화학 시약 및 폴리머를 첨가한 후 분산하여 코팅시키는 방법이다. 이러한 액상 분산 기술을 이용한 코팅방법은 저가이며 대면적의 그라핀 함유 복합체막 제조가 가능하나 함유된 그라핀들을 기판 방향에 나란히 배열되도록 하고, 그라핀간 면간 겹칩을 유도하기 매우 어려웠다.The latter is a method in which synthetic or manufactured graphene is added to a solvent, additionally, chemical reagents such as binders, dispersants, surfactants, and polymers are added, followed by dispersion and coating. The coating method using the liquid dispersion technique is inexpensive and can produce a large-area graphene-containing composite film, but it is very difficult to arrange the contained graphenes side by side in the direction of the substrate, and to induce the inter-graphene interchips.

그러나, 그라핀들을 기판 방향과 같은 방향으로 배열시키거나 그라핀간 면간 겹침을 유도시키는 기술은 평면 전기전도도 및 방열효과가 매우 우수한 그라핀들을 전기전도성 필름, 코팅막, 박막, 후막, 성형체(섬유, 비닐류, 봉지제) 등으로 활용할 때의 물성 발현 및 물성 조절에 매우 중요하다.However, the technique of arranging the graphenes in the same direction as the substrate direction or inducing the interplanar overlap between the graphenes can provide graphenes having excellent planar conductivity and heat dissipation effect, such as electrically conductive films, coating films, thin films, thick films, and shaped articles (fibers, vinyls). , Encapsulation agent) is very important for physical property expression and physical property control.

본 발명에서는 액상공정(경우에 따라서는 열공정, 열압착공정, 양면 프레싱 공정 등)을 이용하더라도 코팅막내 폴리머 바인더에 함유된 그라핀들의 상당수가 기판의 면에서 일방향으로 배열하도록 유도되고, 동시에 그라핀들간 면간 겹침이 유도되게 하는 간단한 공정 기술을 제공함에 그 목적이 있다.In the present invention, even if a liquid phase process (in some cases, a thermal process, a thermocompression process, a double-side pressing process, etc.) is used, a large number of graphenes contained in the polymer binder in the coating film are induced to align in one direction on the surface of the substrate. Its purpose is to provide a simple process technique that induces interplanar overlap between pins.

[도 1]에서는 [도 1]은 통상적인 그라핀 함유 코팅물 제조방법과 및 본 발명에 따른 배향 그라핀 함유 코팅물 제조방법의 비교도를 도시하였다.In FIG. 1, FIG. 1 shows a comparison between a conventional graphene-containing coating production method and an orientation graphene-containing coating production method according to the present invention.

[도 1]에 도시된 바와 같이 종래의 방법으로 그라핀 함유 액상물로부터 형성되는 그라핀 함유 코팅물은 용매 및 몇몇 화학종들을 제거하기 위하여 건조 또는 열처리와 같은 후처리 공정을 거치게 된다. 이 과정에서 2차원 면 형상을 갖는 그라핀들은 처음 위치한 자리에서 크게 이동되지 않는다. 반면 본 발명에서는 상기 후처리 전에 코팅물을 압착하는 단계를 포함함으로서, 그라핀들이 평면에 나란하게 배열되고 동시에 면간 겹침이 유도된다. 참고로 [도 1]은 그라핀들을 이상적으로 표현한 것인데, 실제의 그라핀들은 열역학적 불안정성 때문에 상당수 구겨지는 형태를 가질 수 있으며, 그러한 경우에도 압착 공정을 통하여 구겨진 형태 그대로 평평해지는 효과를 가질 수 있다.As shown in FIG. 1, the graphene-containing coating formed from the graphene-containing liquid in a conventional manner is subjected to a post-treatment process such as drying or heat treatment to remove the solvent and some chemical species. In this process, graphene having a two-dimensional surface shape does not move significantly at the first position. On the other hand, in the present invention, by including the step of compressing the coating before the post-treatment, the graphenes are arranged side by side in a plane and at the same time the overlap between the faces is induced. For reference, Figure 1 is an ideal representation of the graphene, the actual graphene may have a large number of wrinkles due to thermodynamic instability, even in such a case may have the effect of flattening as it is wrinkled through the compression process.

본 발명 전통적으로 액상 코팅방법을 통하여 제조된 그라핀 함유 박막들의 물성을 간단한 공정을 통하여 물성을 크게 향상 시킬 수 있으며 고가 그라핀을 적게 첨가함에도 기존의 박막 물성을 유지시킬 수 있다. 이렇게 제조된 그라핀 함유 박막, 후막, 필름 등은 정전기차폐제, 전극, 도료, 방열판, 등 산업적으로 크게 활용될 수 있다.The physical properties of the graphene-containing thin films traditionally produced by the liquid coating method can be greatly improved through a simple process, it is possible to maintain the existing thin film properties even if the addition of expensive graphene. The graphene-containing thin film, thick film, film, and the like thus prepared may be widely used industrially, such as an electrostatic shield, an electrode, a paint, a heat sink, and the like.

본 발명은 (a) 그라핀 함유 액상물을 마련하는 단계; (b) 상기 그라핀 함유 액상물을 모재에 코팅하여 코팅막을 형성시키는 단계; 및 (c) 상기 코팅막을 압착하는 단계; 를 포함하는 배향 그라핀 함유 코팅물 제조방법을 제공한다.The present invention comprises the steps of (a) preparing a graphene-containing liquid; (b) coating the graphene-containing liquid on a base material to form a coating film; (C) pressing the coating film; It provides a method for producing an alignment graphene-containing coating comprising a.

상기 (a)단계는 폴리머 바인더에 그라핀을 혼합한 후 열을 가하여 액상으로 전환시키는 과정으로 시행할 수 있으며, 상기 그라핀은 흑연을 가공하여 제조된 것을 적용할 수 있다. 이 때, 상기 흑연을 가공하는 방법으로는 화학적 산화방법을 적용할 수 있다. The step (a) may be carried out by mixing the graphene in the polymer binder and then applying heat to convert the graphene into a liquid phase. The graphene may be prepared by processing graphite. At this time, a chemical oxidation method may be applied as a method of processing the graphite.

상기 (b)단계의 코팅방법으로는 딥코팅, 그라비아코팅, 롤투롤코팅, 스핀코팅, 프린팅, 스크린프린팅, 잉크젯프린팅, 스프레이코팅 중 어느 하나를 적용할 수 있다.The coating method of step (b) may be any one of dip coating, gravure coating, roll-to-roll coating, spin coating, printing, screen printing, inkjet printing, spray coating.

이하에서는 첨부한 도면과 함께 본 발명의 구체적인 실시예를 설명하기로 한다.Hereinafter, with reference to the accompanying drawings will be described a specific embodiment of the present invention.

흑연 원료로부터 그라핀 산화물을 제조하고, 그라핀 산화물들은 화학적 환원법을 통하여 그라핀 분말로 전환할 수 있다. 이러한 그라핀 분말에는 적당한 바인더, 계면활성제 등을 첨가하여 용액상(잉크, 콜로이드, 페이스트 등)에서 분산시킨 액상물로 만든 후 이를 모재에 코팅시킬 수 있다. Graphene oxide is prepared from graphite raw materials, and graphene oxides may be converted into graphene powder through chemical reduction. Such graphene powder may be added to a suitable binder, a surfactant, etc. to make a liquid dispersed in the solution phase (ink, colloid, paste, etc.) and then coated on the base material.

그라핀 분말을 얻는 과정의 구체적인 예는 다음과 같다. 천연흑연 10g과 NaNO3 8g을 350mL H2SO4 용액에 넣고 냉각시키면서 KMnO4(또는 염소산칼륨) 45~50g을 1시간에 걸쳐 천천히 넣어 준다. 그 후 4~7% H2SO4 1L을 1시간에 걸쳐 천천히 넣어주고 H2O2를 넣어준다. 그 후 원심 분리하여 상층액을 버리고 3% H2SO4/0.5%H2O2로 씻어주고 최후로 물로 씻어준다. 이를 반복하면 적갈색의 걸쭉한 그래핀 산화물 용액(약간 젤 상태)이 얻어진다. 이렇게 제조된 그라핀 산화물(3% 수용액) 2g에 증류수 100ml를 넣어서 잘 분산 시킨 후 히드라진 수화물(hydrazine hydrate) 1ml를 넣고 100℃에서 24시간 환원 처리하면 검은색으로 환원된 그라핀 분말들이 침전되며, 이를 거름종이로 걸러 물과 메탄올을 이용하여 세척해 주는 것이 바람직하다.Specific examples of the process of obtaining the graphene powder are as follows. Add 10 g of natural graphite and 8 g of NaNO 3 to 350 mL H 2 SO 4 solution, and slowly add 45-50 g of KMnO 4 (or potassium chlorate) over 1 hour while cooling. After that, slowly add 4 ~ 7% H 2 SO 4 1L over 1 hour and add H 2 O 2 . After centrifugation, the supernatant is discarded, washed with 3% H 2 SO 4 /0.5%H 2 O 2, and finally with water. Repeating this gives a reddish brown thick graphene oxide solution (slightly gelled). After diluting 100ml of distilled water in 2g of the graphene oxide (3% aqueous solution) thus prepared, 1ml of hydrazine hydrate was added thereto, and the blackened graphene powders were precipitated when reduced at 100 ° C for 24 hours. It is preferable to filter the filter paper with water and methanol.

그라핀 분말은 그라핀 함유 액상물로 전환시킨 후 모재에 코팅할 수 있다. 구체적인 예로서, 증류수, 그라핀, CMC(Carboxyl Methyl Cellulose)를 각각 9.6g, 0.2g, 0.2g 씩 혼합한 후 스티어링(stirring)과 초음파 처리를 두 시간 이상씩 해서 균일한 액상물을 제조한다. 이렇게 제조된 그라핀 함유 액상물은 아세톤:에탄올=1:1 용액으로 전처리한 소다석회유리(Sodalime glass)에 스핀코팅(2500RPM)한 후 80℃로 건조 처리하여 그라핀 함유 코팅물을 만들 수 있다. The graphene powder may be converted to a graphene-containing liquid and then coated on the base material. As a specific example, distilled water, graphene, and CMC (Carboxyl Methyl Cellulose) are mixed with 9.6 g, 0.2 g, and 0.2 g, respectively, followed by steering and sonication for at least two hours to prepare a uniform liquid. The graphene-containing liquid prepared in this way may be spin-coated (2500 RPM) in a soda lime glass pretreated with an acetone: ethanol = 1: 1 solution and dried at 80 ° C. to produce a graphene-containing coating. .

[도 2]의 (a)는 스핀 코팅 후 80℃로 건조한 그라핀 함유 코팅막의 사진이며, [도 2]의 (b)는 10g/㎠의 압력을 가한 후, 80℃에서 건조시킨 후의 사진이다. 분명히 육안을 통해서도 압착 공정을 통하여 제조된 그라핀 함유 코팅막이 매우 깨끗함을 알 수 있었다. [도 3]은 [도 2] (b)의 단면 SEM 사진이다.2 is a photograph of a graphene-containing coating film dried at 80 ° C. after spin coating, and FIG. 2 b is a photograph after drying at 80 ° C. after applying a pressure of 10 g / cm 2. . Obviously, the graphene-containing coating film prepared by the compression process was also very clean. Fig. 3 is a cross-sectional SEM photograph of Fig. 2 (b).

좀 더 확대하여 살펴보면, [도 2] (a)의 코팅막에서는 [도 4]의 (a)에서 보이듯 그라핀 분말들이 그대로 관찰된다. 반면, 압착공정을 가한 [도 2] (b)의 코팅막에서는 [도 4]의 (b)에서 보이듯 압착되어 기판과 나란한 형태로 배열되며 그라핀 간 접촉도 상당히 이루어져 있음을 볼 수 있다. Looking at a larger magnification, the graphene powders are observed as shown in (a) of FIG. 4 in the coating film of FIG. On the other hand, in the coating film of FIG. 2 (b) to which the pressing process is applied, as shown in (b) of FIG. 4, the film is compressed and arranged in parallel with the substrate.

한편, 전기저항 측면에서도 [도 2] (b)의 코팅막이 [도 2] (a)의 코팅막에 비해 전기전도도가 약 10~50% 이상 향상되었다. 구체적으로 [도 2] (a)의 코팅막에서는 8.9K Ω/sq, 4(b)는 6.1Ω/sq를 나타내었다.On the other hand, in terms of electrical resistance, the coating film of [FIG. 2] (b) is improved by about 10 to 50% or more compared with the coating film of [FIG. 2] (a). Specifically, in the coating film of FIG. 2 (a), 8.9K Ω / sq and 4 (b) showed 6.1Ω / sq.

또한 에폭시(epoxy)계 수지(resin)와 아크릴 모노머(monomer)를 1:1 혼합한 바인더에 에 약 30~50wt% 의 그라핀을 첨가한 후 열을 가하여 액상으로 만들고 가열된 기판에 딥 코팅을 한 후 압착하여 식힘으로써 그라핀 함유 코팅막을 제조한 경우도 전술한 결과와 비슷한 경향을 보였다.In addition, about 30-50 wt% of graphene is added to a binder mixed with an epoxy resin and an acrylic monomer in a 1: 1 mixture, and then heated to a liquid state, and a dip coating is applied to a heated substrate. After the compression and cooling to produce a graphene-containing coating film also showed a similar tendency to the above results.

그라핀 함유 액상물 제조방법과 코팅막 형성방법으로는 전술한 구체적인 예를 들 수 있으나, 본 발명의 원리는 이에 한정되지는 않는다. 물론, 다른 방법으로 제조된 그라핀 함유 박막들도 비슷한 경향을 보이게 된다.Examples of the graphene-containing liquid material manufacturing method and the method of forming the coating film may include the specific examples described above, but the principles of the present invention are not limited thereto. Of course, graphene-containing thin films prepared by other methods show a similar tendency.

상기 압착(가압)공정은 냉각 또는 가열과 함께 수행할 수 있으며, 단순 압착 공정, 연속 롤링공정, 롤투롤 공정 등 다양한 산업적 프레싱 공정기술들을 적용시킬 수 있다. 위와 같이 가압공정을 가미하여 제조된 배향 그라핀 함유 코팅물에서 코팅막을 벗겨내면 배향 그라핀을 함유한 필름을 얻을 수 있게 된다.The pressing (pressing) process may be performed together with cooling or heating, and various industrial pressing process technologies such as a simple pressing process, a continuous rolling process, and a roll-to-roll process may be applied. When the coating film is peeled off from the alignment graphene-containing coating prepared by applying the pressing process as described above, a film containing the orientation graphene can be obtained.

또한, 본 발명은 폴리머바인더에 그라핀을 혼합한 그라핀-폴리머 혼합물을 양면으로 압착하는 단계를 포함하는 것을 특징으로 하는 배향 그라핀 함유 필름 제조방법을 함께 제공한다. 본 발명의 원리는 일면(일방향) 압착뿐만 아니라, 양면(양방향) 압착에서도 똑같이 적용된다. 상기 그라핀-폴리머 혼합물에는 열을 가하여 액상으로 전환시킨 후 양면으로 압착할 수 있으며, 상기 그라핀은 흑연을 가공하여 제조된 것을 적용할 수 있다. 이 때, 상기 흑연을 가공하는 방법으로 화학적 산화방법을 적용할 수 있음은 전술한 바와 같다. [도 5]는 폴리머바인더에 그라핀을 혼합한 그라핀-폴리머 혼합물을 양면으로 가압하여 제조한 필름의 단면 SEM 사진을 나타낸 것이다. [도 5]에서 보듯이 그라핀 함유 박막의 단면들은 거의 일방향으로 배열되어 있음을 확인할 수 있었다. In another aspect, the present invention provides a method for producing an oriented graphene-containing film comprising the step of compressing the graphene-polymer mixture in which the graphene is mixed into the polymer binder on both sides. The principles of the present invention apply equally to one-side (one-way) compression, as well as to both-side (two-way) compression. The graphene-polymer mixture may be converted to a liquid phase by applying heat, and then compressed to both sides, and the graphene may be prepared by processing graphite. At this time, the chemical oxidation method can be applied to the method of processing the graphite as described above. FIG. 5 shows a cross-sectional SEM photograph of a film prepared by pressing a graphene-polymer mixture mixed with graphene in a polymer binder to both sides. As shown in FIG. 5, the cross-sections of the graphene-containing thin films were almost aligned in one direction.

본 발명은 위에서 언급한 바와 같이 첨부된 도면과 관련하여 설명되었으나, 본 발명의 요지를 벗어남이 없는 범위 내에서 다양한 수정 및 변형이 가능하며, 다양한 분야에서 사용 가능하다. 따라서 본 발명의 청구범위는 이건 발명의 진정한 범위 내에 속하는 수정 및 변형을 포함한다.Although the present invention has been described with reference to the accompanying drawings as mentioned above, various modifications and variations are possible within the scope without departing from the spirit of the present invention, and can be used in various fields. Therefore, the claims of the present invention include modifications and variations that fall within the true scope of the invention.

[도 1]은 통상적인 그라핀 함유 코팅물 제조방법과 및 본 발명에 따른 배향 그라핀 함유 코팅물 제조방법의 비교도이다.1 is a comparison of a conventional graphene-containing coating production method and an orientation graphene-containing coating production method according to the present invention.

[도 2]는 압착공정이 없을 때와 있을 때의 그라핀 함유 코팅물의 디지털 이미지를 비교한 것이다. FIG. 2 compares the digital images of graphene containing coatings with and without a compaction process.

[도 3]은 [도 2] (b)의 단면 SEM 사진이다.Fig. 3 is a cross-sectional SEM photograph of Fig. 2 (b).

[도 4]는 [도 2]의 (a), (b) 각각의 표면 SEM 사진이다.FIG. 4 is a SEM image of the surface of each of (a) and (b) of FIG. 2.

[도 5]는 본 발명에 따라 양면 압착에 의해 얻은 배향 그라핀 함유 필름 단면의 SEM 사진이다.FIG. 5 is a SEM photograph of a cross-section of an orientation graphene-containing film obtained by double-sided compression according to the present invention. FIG.

Claims (10)

(a) 그라핀 함유 액상물을 마련하는 단계;(a) preparing a graphene-containing liquid; (b) 상기 그라핀 함유 액상물을 모재에 코팅하여 코팅막을 형성시키는 단계; 및(b) coating the graphene-containing liquid on a base material to form a coating film; And (c) 상기 코팅막을 압착하는 단계; 를 포함하는 배향(配向) 그라핀 함유 코팅물 제조방법.(c) pressing the coating film; Orientation graphene containing coating manufacturing method comprising a. 제1항에서, In claim 1, 상기 (a)단계는 폴리머 바인더에 그라핀을 혼합한 후 열을 가하여 액상으로 전환시키는 과정으로 시행하는 것을 특징으로 하는 배향 그라핀 함유 코팅물 제조방법.The step (a) is a method for producing an alignment graphene-containing coating, characterized in that to perform a process of converting into a liquid phase by applying heat after mixing the graphene in the polymer binder. 제1항에서, In claim 1, 상기 (a)단계에 적용되는 그라핀은 흑연을 가공하여 제조된 것임을 특징으로 하는 배향 그라핀 함유 코팅물 제조방법.Graphene applied to the step (a) is a method for producing an alignment graphene-containing coating, characterized in that prepared by processing graphite. 제3항에서,4. The method of claim 3, 상기 흑연을 가공하는 방법은 화학적 산화방법인 것을 특징으로 하는 배향 그라핀 함유 코팅물 제조방법.The method of processing the graphite is a method for producing an alignment graphene-containing coating, characterized in that the chemical oxidation method. 제1항에서,In claim 1, 상기 (b)단계의 코팅방법은 딥코팅, 그라비아코팅, 롤투롤코팅, 스핀코팅, 프린팅, 스크린프린팅, 잉크젯프린팅, 스프레이코팅 중 어느 하나임을 특징으로 하는 배향 그라핀 함유 코팅물 제조방법.The coating method of the step (b) is a dip coating, gravure coating, roll-to-roll coating, spin coating, printing, screen printing, inkjet printing, spray coating method characterized in that any one of the coating method. 제1항 내지 제5항 중 어느 한 항의 방법에 의해 제조된 배향 그라핀 함유 코팅물에서 코팅막을 벗겨내어 필름으로 제조하는 배향 그라핀 함유 필름 제조방법.A method for producing an oriented graphene-containing film, wherein the coating film is peeled off from the oriented graphene-containing coating prepared by the method of any one of claims 1 to 5 to prepare a film. 삭제delete 삭제delete 삭제delete 삭제delete
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