KR102008203B1 - Silicon coating method of polyimide film - Google Patents

Silicon coating method of polyimide film Download PDF

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KR102008203B1
KR102008203B1 KR1020170118332A KR20170118332A KR102008203B1 KR 102008203 B1 KR102008203 B1 KR 102008203B1 KR 1020170118332 A KR1020170118332 A KR 1020170118332A KR 20170118332 A KR20170118332 A KR 20170118332A KR 102008203 B1 KR102008203 B1 KR 102008203B1
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film
silicon
impregnated
low temperature
polyimide film
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KR1020170118332A
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Korean (ko)
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KR20190030832A (en
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김유신
설경식
김정환
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(주)티디엘
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Priority to KR1020170118332A priority Critical patent/KR102008203B1/en
Priority to PCT/KR2017/010657 priority patent/WO2019054544A1/en
Priority to CN201780096848.0A priority patent/CN111356537A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00Processes for applying liquids or other fluent materials
    • B05D1/18Processes for applying liquids or other fluent materials performed by dipping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/02Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
    • B05D3/0254After-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B05D3/0406Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B05D3/0406Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
    • B05D3/0426Cooling with air
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2252/00Sheets
    • B05D2252/04Sheets of definite length in a continuous process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2518/00Other type of polymers
    • B05D2518/10Silicon-containing polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers

Abstract

본 발명은 차량용 내비게이션 등의 사용 가능한 폴리이미드 필름의 실리콘 코팅방법에 관한 것으로, 공급롤로부터 폴리이미드 필름을 풀어 공급하는 필름공급단계; 공급된 필름을 실리콘 액이 저장된 함침조를 통과시켜 실리콘을 함침시키는 함침단계; 실리콘이 함침된 함침 필름을 저온처리하는 제1저온처리단계; 저온처리 후 함침 필름을 고온처리하는 고온처리단계: 고온처리 후 함침 필름을 저온처리하는 제2저온처리단계; 저온처리된 실리콘 함침 필름을 권취롤에 권취하는 필름권취단계를 포함하는 것을 특징으로 한다.The present invention relates to a silicone coating method of a polyimide film that can be used, such as vehicle navigation, comprising: a film supplying step of releasing and supplying a polyimide film from a supply roll; An impregnation step of impregnating silicon by passing the supplied film through an impregnation tank in which a silicon liquid is stored; A first cryogenic treatment step of low temperature treating the impregnated film impregnated with silicon; A high temperature treatment step of high temperature treatment of the impregnated film after the low temperature treatment: a second low temperature treatment step of low temperature treatment of the impregnated film after the high temperature treatment; It characterized in that it comprises a film winding step of winding the cold-treated silicon impregnated film on the take-up roll.

Description

폴리이미드 필름의 실리콘 코팅방법{SILICON COATING METHOD OF POLYIMIDE FILM}Silicone coating method of polyimide film {SILICON COATING METHOD OF POLYIMIDE FILM}

본 발명은 폴리이미드 필름의 실리콘 코팅방법에 관한 것으로, 보다 상세하게는 폴리이미드 필름에 실리콘을 코팅하는 과정에서 불완전 응고되는 것을 방지하고, 탄성도 및 입자결속력이 강화될 수 있는 폴리이미드 필름의 실리콘 코팅방법에 관한 것이다.The present invention relates to a silicone coating method of a polyimide film, and more particularly, to prevent incomplete solidification in the process of coating the silicone on the polyimide film, the silicone of the polyimide film which can enhance the elasticity and particle binding strength It relates to a coating method.

일반적으로 폴리이미드(PI) 필름은 폴리이미드 수지를 필름화한 것으로, 폴리이미드 수지는 방향족 디안하이드라이드와 방향족 디아민 또는 방향족 디이소시아네이트를 용액중합하여 폴리아믹산 유도체를 제조한 후, 고온에서 폐환 탈수시켜 이미드 화하여 제조되는 고내열 수지를 일컫는다.In general, a polyimide (PI) film is a film of a polyimide resin, and a polyimide resin is a solution polymerization of an aromatic dianhydride and an aromatic diamine or an aromatic diisocyanate to prepare a polyamic acid derivative, and then ring-dehydration at high temperature. Refers to a high heat resistant resin produced by imidization.

폴리이미드 수지는 불용, 불융의 초고내열성 수지로서 내열산화성, 내열특성, 내방사선성, 저온특성, 내약품성 등에 우수한 특성을 가지고 있어, 자동차 재료, 항공소재, 우주선 소재 등의 내열 첨단소재 및 절연코팅제, 절연막, 반도체, TFT-LCD의 전극 보호막 등 전자재료에 광범위한 분야에 사용되고, 최근에는 광섬유나 액정 배향막 같은 표시재료 및 필름 내에 도전성 필러를 함유하거나 표면에 코팅하여 투명전극필름 등에도 이용되고 있다.Polyimide resin is an insoluble and insoluble ultra high heat resistant resin, and has excellent characteristics such as heat oxidation resistance, heat resistance, radiation resistance, low temperature property, chemical resistance, and so on. It is used in a wide range of fields for electronic materials such as insulating films, semiconductors, electrode protective films of TFT-LCDs, and recently, it has been used in transparent electrode films and the like by containing conductive fillers in the display materials and films such as optical fibers and liquid crystal alignment films or by coating the surfaces thereof.

이와 같이 폴리이미드 수지는 다양한 분야에서 사용되고 있으나, 기능성의 향상을 위해 폴리이미드에 실리콘 코팅을 하기도 한다. As described above, the polyimide resin is used in various fields, but in order to improve the functionality, a polyimide resin is also coated with silicone.

그러나 실리콘 코팅을 위해 단순히 실리콘 액에 폴리이미드 필름을 함침시켜 코팅을 하는 경우 불완전 응고가 발생하는 문제가 있었다.However, there was a problem that incomplete coagulation occurs when the coating by simply impregnating the polyimide film in the silicone liquid for the silicon coating.

대한민국등록특허 제10-1049927호 : 실리콘 코팅된 플라스틱 본딩시트 및 그 제조방법Republic of Korea Patent No. 10-1049927: Silicone coated plastic bonding sheet and its manufacturing method 대한민국등록특허 제10-0651386호 : 폴리이미드 커버레이의 이형처리방법 및 상기 이형처리된폴리이미드 커버레이를 이용한 경연성 다층인쇄회로기판의 제조방법Republic of Korea Patent No. 10-0651386: Release method of polyimide coverlay and manufacturing method of a flexible multilayer printed circuit board using the release-treated polyimide coverlay

본 발명은 상기와 같은 문제점을 해결하기 위한 것으로, 폴리이미드 필름에 실리콘 코팅을 용이하고 견고하게 할 수 있는 폴리이미드 필름의 실리콘 코팅방법을 제공하는데 그 목적이 있다.The present invention is to solve the above problems, and an object of the present invention is to provide a silicone coating method of a polyimide film that can easily and firmly silicone coating on a polyimide film.

본 발명에 따른 폴리이미드 필름의 실리콘 코팅방법은 공급롤로부터 폴리이미드 필름을 풀어 공급하는 필름공급단계와, 공급된 필름을 실리콘 액이 저장된 함침조를 통과시켜 실리콘을 함침시키는 함침단계와, 실리콘이 함침된 함침 필름을 저온처리하는 제1저온처리단계와, 저온처리 후 함침 필름을 고온처리하는 고온처리단계와, 고온처리 후 함침 필름을 저온처리하는 제2저온처리단계와, 저온처리된 실리콘 함침 필름을 권취롤에 권취하는 필름권취단계를 포함한다.The silicon coating method of the polyimide film according to the present invention includes a film supply step of releasing and supplying a polyimide film from a supply roll, an impregnation step of impregnating silicon by passing the supplied film through an impregnation tank in which a silicon liquid is stored, and A first low temperature treatment step of low temperature treatment of the impregnated impregnated film, a high temperature treatment step of high temperature treatment of the impregnated film after low temperature treatment, a second low temperature treatment step of low temperature treatment of the impregnated film after high temperature treatment, and a low temperature treated silicon impregnation And a film winding step of winding the film on a winding roll.

상기 실리콘 액을 함침할 때 함침온도가 20℃ 이하인 것이 바람직하다.When impregnating the said silicone liquid, it is preferable that an impregnation temperature is 20 degrees C or less.

상기 함침조에 저장된 실리콘액을 냉각시켜 온도계의 측정값이 20℃에 도달한 다음 20분 이상 에이징한 후 상기 폴리이미드 필름을 상기 함침조에 통과시키는 것이 바람직하다.It is preferable to cool the silicon liquid stored in the impregnation tank to reach a temperature of 20 ° C. and then age the film for 20 minutes or more, and then pass the polyimide film through the impregnation tank.

상기 필름권취단계에서 실리콘 함침 필름이 권취롤에 권취되는 동안 실리콘 함침 필름을 급냉 처리할 수 있으며, 상기 실리콘 함침 필름의 급냉 처리는 제트스프레이에 의해 이루어지는 것이 바람직하다.In the film winding step, the silicon impregnated film may be quenched while the silicon impregnated film is wound on the take-up roll, and the quenching treatment of the silicon impregnated film is preferably performed by jet spray.

본 발명의 폴리이미드 필름의 실리콘 코팅방법에 따라 제조된 폴리이미드 필름은 실리콘의 코팅 과정에서 실리콘의 불완전 응고가 방지되며, 탄성도 및 입자결속력이 강해지는 이점이 있다.The polyimide film prepared according to the silicon coating method of the polyimide film of the present invention has the advantage that the incomplete solidification of the silicon is prevented in the coating process of the silicon, the elasticity and the particle binding strength is stronger.

도 1은 본 발명에 따른 폴리이미드 필름의 구조를 모식적으로 도시한 예시도이다.
도 2는 본 발명의 폴리이미드 필름의 실리콘 코팅방법에 따른 제조과정을 도시한 개념도이다.
도 3은 본 발명의 폴리이미드 필름의 실리콘 코팅방법에 따른 제조단계를 도시한 순서도이다.
1 is an exemplary view schematically showing the structure of a polyimide film according to the present invention.
Figure 2 is a conceptual diagram showing a manufacturing process according to the silicon coating method of the polyimide film of the present invention.
Figure 3 is a flow chart showing the manufacturing step according to the silicone coating method of the polyimide film of the present invention.

이하, 첨부한 도면을 참조하여 본 발명의 실시예에 따른 폴리이미드 필름의 실리콘 코팅방법에 대해 상세히 설명한다. 본 발명은 다양한 변경을 가할 수 있고 여러 가지 형태를 가질 수 있는 바, 특정 실시 예들을 도면에 예시하고 본문에 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 개시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술 범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. 이 과정에서 도면에 도시된 선들의 두께나 구성요소의 크기 등은 설명의 명료성과 편의상 과장되게 도시되어 있을 수 있다.Hereinafter, with reference to the accompanying drawings will be described in detail a silicon coating method of a polyimide film according to an embodiment of the present invention. As the inventive concept allows for various changes and numerous embodiments, particular embodiments will be illustrated in the drawings and described in detail in the text. However, this is not intended to limit the present invention to a specific disclosed form, it should be understood to include all modifications, equivalents, and substitutes included in the spirit and scope of the present invention. In this process, the thickness of the lines or the size of the components shown in the drawings may be exaggerated for clarity and convenience of description.

제1, 제2 등의 용어는 다양한 구성요소들을 설명하는데 사용될 수 있지만, 상기 구성요소들은 상기 용어들에 의해 한정되어서는 안 된다. 상기 용어들은 하나의 구성요소를 다른 구성요소로부터 구별하는 목적으로만 사용된다. 예를 들어, 본 발명의 권리 범위를 벗어나지 않으면서 제1 구성요소는 제2 구성요소로 명명될 수 있고, 유사하게 제2 구성요소도 제1 구성요소로 명명될 수 있다. Terms such as first and second may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as the second component, and similarly, the second component may also be referred to as the first component.

본 출원에서 사용한 용어는 단지 특정한 실시 예를 설명하기 위해 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다. 본 출원에서, "포함하다" 또는 "가지다" 등의 용어는 명세서 상에 기재된 특징, 숫자, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting of the invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this application, the terms "comprise" or "have" are intended to indicate that there is a feature, number, step, action, component, part, or combination thereof described on the specification, and one or more other features. It is to be understood that the present invention does not exclude the possibility of the presence or the addition of numbers, steps, operations, components, parts, or combinations thereof.

다르게 정의되지 않는 한, 기술적이거나 과학적인 용어를 포함해서 여기서 사용되는 모든 용어들은 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에 의해 일반적으로 이해되는 것과 동일한 의미를 가지고 있다. 일반적으로 사용되는 사전에 정의되어 있는 것과 같은 용어들은 관련 기술의 문맥 상 가지는 의미와 일치하는 의미를 가지는 것으로 해석되어야 하며, 본 출원에서 명백하게 정의하지 않는 한, 이상적이거나 과도하게 형식적인 의미로 해석되지 않는다.
Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art. Terms such as those defined in the commonly used dictionaries should be construed as having meanings consistent with the meanings in the context of the related art and shall not be construed in ideal or excessively formal meanings unless expressly defined in this application. Do not.

도 1에는 본 발명의 폴리이미드 필름의 실리콘 코팅방법에 의해 제작된 실리콘이 함침된 폴리이미드 필름이 도시되어 있다.Figure 1 shows a polyimide film impregnated with silicon produced by the silicone coating method of the polyimide film of the present invention.

도시된 것처럼 폴리이미드 필름(1)에 실리콘(2)이 함침되어 코팅되어 있으며, 일측에 이형막(3)이 형성된다.As shown, the polyimide film 1 is coated with silicon 2 impregnated thereon, and a release film 3 is formed on one side.

도 2 및 도 3을 참조하면, 본 발명의 폴리이미드 필름의 실리콘 코팅방법은 필름공급단계, 함침단계, 저온처리단계, 고온처리단계, 저온처리단계, 필름권취단계를 포함한다.2 and 3, the silicon coating method of the polyimide film of the present invention includes a film supply step, impregnation step, low temperature treatment step, high temperature treatment step, low temperature treatment step, film winding step.

폴리이미드 필름(1)은 폴리아믹산 용액을 지지체에 캐스팅하여 이미드화 함으로써 필름을 얻는 방법을 통해 제조될 수 있다. 이 때 적용되는 이미드화법으로는 열이미드화법, 화학이미드화법, 또는 열이미드화법과 화학이미드화법을 병용하여 적용할 수 있다. The polyimide film 1 may be produced by casting a polyamic acid solution onto a support to imide to obtain a film. The imidation method applied at this time can be applied in combination with a thermal imidation method, a chemical imidation method, or a thermal imidation method and a chemical imidation method.

화학이미드화법은 폴리아믹산 용액에 아세트산무수물 등의 산무수물로 대표되는 탈수제와 이소퀴놀린, β-피콜린, 피리딘 등의 3급 아민류 등으로 대표되는 이미드화 촉매를 투입하는 방법이다. 열이미드화법 또는 열이미드화법과 화학이미드화법을 병용하는 경우 폴리아믹산 용액의 가열 조건은 폴리아믹산 용액의 종류, 제조되는 폴리이미드 필름(1)의 두께 등에 의하여 변동될 수 있다.The chemical imidization method is a method of injecting an imidization catalyst represented by a dehydrating agent represented by an acid anhydride such as acetic anhydride and tertiary amines such as isoquinoline, β-picolin and pyridine into a polyamic acid solution. In the case of using the thermal imidization method or the thermal imidization method together with the chemical imidization method, the heating conditions of the polyamic acid solution may vary depending on the kind of the polyamic acid solution, the thickness of the polyimide film 1 to be produced, and the like.

열이미드화법과 화학이미드화법을 병용하는 경우의 폴리이미드 필름(1)의 제조 예를 보다 구체적으로 설명하면, 폴리아믹산 용액에 탈수제 및 이미드화 촉매를 투입하여 지지체상에 캐스팅한 후 80~200℃, 바람직하게는 100~180℃에서 가열하여 탈수제 및 이미드화 촉매를 활성화함으로써 부분적으로 경화 및 건조한 후 겔 상태의 폴리아믹산 필름을 지지체로부터 박리하여 얻고, 상기 겔 상태의 필름을 200~400℃에서 5~400초간 가열함으로써 폴리이미드 필름(1)을 얻을 수 있다.When explaining the manufacturing example of the polyimide film (1) in the case of using a thermal imidation method and a chemical imidation method together more concretely, 80 to-after casting a dehydrating agent and an imidation catalyst in a polyamic-acid solution, and casting on a support body After heating at 200 ° C, preferably 100-180 ° C to activate the dehydrating agent and the imidization catalyst, the polyamic acid film in the gel state is obtained by peeling from the support, and the film in the gel state is 200-400 ° C. The polyimide film 1 can be obtained by heating for 5 to 400 seconds at.

이렇게 얻어진 폴리이미드 필름(1)은 공급롤(10)에 권취되어 실리콘 코팅을 위해 재료를 공급하는 수단으로 사용될 수 있다.The polyimide film 1 thus obtained may be wound on a feed roll 10 and used as a means for supplying a material for silicon coating.

필름공급단계(S100)에서는 공급롤(10)에 권취되어 있는 폴리이미드 필름(1)을 공급롤(10)로부터 풀어 후속공정이 이루어질 수 있도록 일정속도로 공급한다.In the film supply step (S100), the polyimide film 1 wound on the supply roll 10 is released from the supply roll 10 and supplied at a constant speed so that a subsequent process can be performed.

함침단계(S200)는 공급롤(10)에서 풀려나온 폴리이미드 필름(1)에 실리콘을 코팅하기 위해 함침시키는 단계이다. The impregnation step (S200) is a step of impregnating the polyimide film 1 released from the supply roll 10 to coat silicon.

도시된 것처럼 폴리이미드 필름(1)이 공급롤(10)에서 풀려나온 후 실리콘 액이 담긴 함침조(20)를 통과하게 함으로써 함침조(20)의 통과 과정에서 실리콘의 함침이 이루어진다.As shown, the polyimide film 1 is released from the supply roll 10 and then passed through the impregnation tank 20 containing the silicon liquid, so that impregnation of silicon is performed in the passage of the impregnation tank 20.

폴리이미드 필름(1)이 함침조(20)의 실리콘액에 잠겨서 이동할 수 있도록 복수개의 가이드롤러를 이용해 폴리이미드 필름(1)의 진행경로를 가이드할 수 있으며, 폴리이미드 필름(1)은 함침조(20)의 실리콘액에 잠겼다가 나와서 후속공정을 진행하도록 이동하게 된다.A plurality of guide rollers may guide the traveling path of the polyimide film 1 so that the polyimide film 1 is immersed in the silicone liquid of the impregnation tank 20, and the polyimide film 1 is impregnated. It is immersed in the silicone liquid of (20) and then moved to proceed with the subsequent process.

상기 함침조(20)에서 실리콘 액에 함침되는 시간은 공급롤(10)에서 필름이 공급되는 속도와 함침된 상태로 필름이 이동하는 이동거리로 조절할 수 있다. The time impregnated in the silicon liquid in the impregnation tank 20 may be adjusted to the moving distance that the film moves in the state impregnated with the speed of supplying the film from the supply roll 10.

아울러 상기 폴리이미드 필름(1)을 함침조(20)에 함침시킬 때 함침온도는 20℃ 이하가 되는 것이 바람직하다. 이는 함침조(20)의 온도가 20℃ 이상으로 상승되어 유지될 경우 실리콘 코팅액에 포함된 촉매가교제(Catalyst)에 의하여 함침조 안에서 실리콘의 응고가 먼저 진행될 수 있기 때문이다. 이로인해 코팅 처리단계에서 양호한 표면상태를 구현하기 힘들어지며, 따라서 함침조(20) 외부에 일반적인 냉각장치를 이용해 20℃ 이하로 온도를 유지해야 한다.In addition, when the polyimide film 1 is impregnated in the impregnation tank 20, the impregnation temperature is preferably 20 ° C or less. This is because when the temperature of the impregnation tank 20 is maintained at 20 ° C. or higher, solidification of silicon in the impregnation tank may proceed first by a catalyst cross-linking agent included in the silicon coating solution. This makes it difficult to achieve a good surface state in the coating step, and therefore it is necessary to maintain the temperature below 20 ℃ using a common cooling device outside the impregnation tank (20).

그리고 냉각장치를 이용해 함침조(20)에 저장된 실리콘액을 냉각시킬 때, 온도계를 통해 측정된 실리콘액의 온도가 20℃에 도달한 후 20분 이상 에이징한 다음 폴리이미드 필름(1)의 함침을 진행한다.When the silicon liquid stored in the impregnation tank 20 is cooled by using a cooling device, the temperature of the silicon liquid measured by the thermometer reaches 20 ° C., and then aged for 20 minutes or more, and then impregnation of the polyimide film 1 is performed. Proceed.

실리콘액이 20℃로 최초로 측정된 상태에서도 함침조(20)에 저장된 전체 실리콘액의 온도가 20℃에 도달하지 못했을 수 있다. 따라서 대류현상으로 실리콘액이 전체적으로 20℃ 이하로 냉각되기 까지 기다리기 위해 약 20분 이상 에이징한다.Even when the silicon liquid is initially measured at 20 ° C., the temperature of the entire silicon liquid stored in the impregnation tank 20 may not reach 20 ° C. FIG. Therefore, due to convection, the silicone liquid is aged for about 20 minutes or more to wait until it is cooled below 20 ° C.

폴리이미드 필름(1)이 함침조(20)를 통과한 후에는 저온처리기(30, 제1저온처리기), 고온처리기(40) 및 저온처리기(30, 제2저온처리기)에서 각각 저온처리, 고온처리 및 저온처리 단계를 거친다.After the polyimide film 1 passes through the impregnation tank 20, the low temperature treatment and the high temperature treatment are performed in the low temperature processor 30 (the first low temperature processor), the high temperature processor 40 and the low temperature processor 30 (the second low temperature processor), respectively. Treatment and cold treatment steps.

저온처리단계(S300)는 폴리이미드 필름(1)에 함침된 실리콘의 안정화 및 평활도를 위한 것이다. Low temperature treatment step (S300) is for the stabilization and smoothness of the silicon impregnated in the polyimide film (1).

저온처리단계(제1저온처리단계)에서는 함침조(20)를 통과하여 실리콘이 함침된 폴리이미드 필름(1)은 4 내지 6M/min의 속도로 저온처리기(30)를 통과하며 저온코팅처리가 진행된다. 이때 저온처리기(30)의 온도는 90℃ 내지 110℃ 전후로 유지된다. In the low temperature treatment step (first low temperature treatment step), the polyimide film 1 impregnated with silicon through the impregnation tank 20 passes through the low temperature processor 30 at a rate of 4 to 6 M / min, and a low temperature coating process is performed. Proceed. At this time, the temperature of the low temperature processor 30 is maintained at about 90 ℃ to 110 ℃.

고온처리단계(S400)에서는 저온처리기(30)를 통과한 폴리이미드 필름(1)을 4 내지 6min 의 속도로 고온처리기(40)를 통과시켜 실시하는데, 이 때, 고온처리기의 온도는 170℃ 내지 180℃ 전후로 유지되는 것이 바람직하다.In the high temperature treatment step (S400), the polyimide film 1 that has passed through the low temperature processor 30 is passed through the high temperature processor 40 at a rate of 4 to 6 min. At this time, the temperature of the high temperature processor is 170 to It is preferable to maintain around 180 degreeC.

저온처리단계 및 고온처리단계의 진행 시 지정된 속도 및 온도 유지조건이 상기 조건과 다를 경우 실리콘의 불완전 응고가 나타나게 되므로 강도가 저하되거나 버블(bubble) 발생 등과 같이 제품의 표면 및 물질적 성질에 비정상적인 영향을 줄 수 있다.If the specified speed and temperature maintenance conditions differ from the above conditions during the low temperature treatment and high temperature treatment, incomplete solidification of the silicon may occur. Therefore, abnormal effects on the surface and material properties of the product, such as reduced strength or bubble, may occur. Can give

저온처리단계(S500)(제2저온처리단계)에서 폴리이미드 필름(1)은 4 내지 6M/min의 속도로 저온처리기(30)를 통과하여 저온코팅처리가 진행된다. 이때 저온처리기(30)의 온도는 90℃ 내지 110℃ 전후로 유지된다.In the low temperature treatment step S500 (second low temperature treatment step), the polyimide film 1 passes through the low temperature processor 30 at a rate of 4 to 6 M / min, and is subjected to a low temperature coating process. At this time, the temperature of the low temperature processor 30 is maintained at about 90 ℃ to 110 ℃.

후술할 것과 같이 폴리이미드 필름(1)은 권취롤(50)에서 급냉처리 되는데, 이러한 급냉처리 시 발생되는 습기가 실리콘 내부 입자를 분리시켜 갈라짐 현상이 발생할 수 있다, 이에 따라 본 발명에서는 고온에서 바로 급냉처리가 진행되는 것이 아니라 재차 저온처리 단계를 거치도록 하여 습기를 억제한다.As will be described later, the polyimide film 1 is quenched in the take-up roll 50, and the moisture generated during the quenching process may separate the silicon internal particles and cause a cracking phenomenon. The quenching process is not carried out, but again to the low temperature treatment step to suppress the moisture.

또한 이와 같이, 고온에서 응고된 실리콘 입자에 저온처리를 다시 진행함에 따라 실릴푸마레이트와 실릴말레이미드의 화학물과 폴리이미드 필름 간의 결속력이 증진되어 우수한 물성을 가지는 것이 가능하며, 그 내구성이 향상될 수 있다.In this way, as the low temperature treatment is further performed on the silicon particles solidified at a high temperature, the binding force between the chemicals of the silyl fumarate and the silyl maleimide and the polyimide film can be enhanced to have excellent physical properties, and the durability thereof can be improved. Can be.

이렇게 실리콘이 함침된 폴리이미드 필름(1)은 저온처리와 고온처리를 거친 뒤에 재차 저온처리를 거쳐 권취롤(50)에 권취된다.After the silicon-impregnated polyimide film 1 is subjected to a low temperature treatment and a high temperature treatment, the polyimide film 1 is wound on the winding roll 50 again through a low temperature treatment.

그리고 권취롤(50)에 권취되는 과정에서 급냉처리를 실시하는데, 급냉처리를 위해 권취롤(50)의 인근에 제트스프레이(60)를 설치하고, 상기 제트스프레이(60)를 통해 권취되는 필름을 급냉시킨다.And the quenching process is carried out in the process of being wound on the take-up roll 50, the jet spray 60 is installed in the vicinity of the take-up roll 50 for the quenching process, and the film wound through the jet spray (60) Quench.

상기 제트스프레이(60)는 적정 분사거리의 70 내지 80% 정도의 거리에서 냉각제를 분사하도록 설치되는 것이 바람직하다.The jet spray 60 is preferably installed to inject the coolant at a distance of about 70 to 80% of the proper injection distance.

즉, 예를 들어 설치된 제트스프레이의 적정 분사거리가 20cm라면, 본 작업을 위해 해당 제트스프레이를 권취롤에 감기는 폴리이미드 필름으로부터 약 14 ~ 16cm 이격된 위치에서 냉각제를 분사하도록 설치하는 것이 바람직하다.That is, for example, if the proper jet distance of the installed jet spray is 20 cm, it is preferable to install the jet spray at a position about 14 to 16 cm away from the polyimide film winding the jet spray on the take-up roll for this operation. .

아울러 권취롤(50)에 감김이 진행됨에 따라 폴리이미드 필름(1)의 표면이 제트스프레이(60)와 가까워지게 되므로 상기 제트스프레이(60)를 상기 권취롤(50)의 중심으로부터 방사상의 방향을 따라 이동 가능하게 설치되는 이동부재에 장착하여 제트스프레이(60)를 이동 가능하게 지지하는 것이 바람직하다.In addition, as the winding roll 50 proceeds, the surface of the polyimide film 1 comes closer to the jet spray 60, so that the jet spray 60 has a radial direction from the center of the winding roll 50. It is preferable that the jet spray 60 is movably supported by being mounted on the movable member which is installed to be movable.

이렇게 권취롤(50)에 감기는 필름을 급냉처리함으로써 필름의 탄성도 및 입자결속력이 강화된다.By thus quenching the film wound on the winding roll 50, the elasticity and the particle binding force of the film are strengthened.

이상에서 설명한 본 발명에 따른 폴리이미드 필름(1)의 실리콘 코팅 방법에 따르면 실리콘을 함침시킨 후 저온처리 및 고온처리를 거친 후 재차 저온처리를 거치고, 권취되는 과정에서 급냉시킴으로써 실리콘의 불완전 응고가 방지되고 탄성도 및 입자결속력이 강화된 필름을 제조할 수 있다.According to the silicone coating method of the polyimide film 1 according to the present invention described above, after impregnating the silicon and then undergoing a low temperature treatment and a high temperature treatment, the silicon coating method is subjected to a low temperature treatment again and quenched in the winding process to prevent incomplete solidification of the silicon. And a film having enhanced elasticity and particle binding force.

제시된 실시예들에 대한 설명은 임의의 본 발명의 기술분야에서 통상의 지식을 가진 자가 본 발명을 이용하거나 또는 실시할 수 있도록 제공된다. 이러한 실시예들에 대한 다양한 변형들은 본 발명의 기술 분야에서 통상의 지식을 가진자에게 명백할 것이며, 여기에 정의된 일반적인 원리들은 본 발명의 범위를 벗어남이 없이 다른 실시예들에 적용될 수 있다. 그리하여, 본 발명은 여기에 제시된 실시예들로 한정되는 것이 아니라, 여기에 제시된 원리들 및 신규한 특징들과 일관되는 최광의의 범위에서 해석되어야 할 것이다.The description of the presented embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the scope of the invention. Thus, the present invention should not be limited to the embodiments set forth herein but should be construed in the broadest scope consistent with the principles and novel features set forth herein.

1: 폴리이미드 필름
2: 실리콘 코팅
3: 이형막
10: 공급롤
20: 함침조
30: 저온처리기
40: 고온처리기
50: 권취롤
60: 제트스프레이
1: polyimide film
2: silicone coating
3: release film
10: feed roll
20: impregnation tank
30: low temperature processor
40: high temperature processor
50: winding roll
60: jet spray

Claims (5)

공급롤로부터 폴리이미드 필름을 풀어 공급하는 필름공급단계;
공급된 필름을 실리콘 액이 저장된 함침조를 통과시켜 실리콘을 함침시키는 함침단계;
실리콘이 함침된 함침 필름을 저온처리하는 제1저온처리단계;
저온처리 후 함침 필름을 고온처리하는 고온처리단계:
고온처리 후 함침 필름을 저온처리하는 제2저온처리단계;
저온처리된 실리콘 함침 필름을 권취롤에 권취하는 필름권취단계를 포함하고,
상기 필름권취단계에서 실리콘 함침 필름이 권취롤에 권취되는 동안 실리콘 함침 필름을 급냉 처리하되, 상기 실리콘 함침 필름의 급냉 처리는 권취되는 실리콘 함침 필름으로 냉각제를 분사하는 제트스프레이에 의해 이루어지며, 상기 제트스프레이는 상기 권취롤의 중심으로부터 방사상의 방향을 따라 이동 가능하게 설치되는 것을 특징으로 하는 폴리이미드 필름의 실리콘 코팅방법.
A film supplying step of releasing and supplying a polyimide film from a supply roll;
An impregnation step of impregnating silicon by passing the supplied film through an impregnation tank in which a silicon liquid is stored;
A first cryogenic treatment step of low temperature treating the impregnated film impregnated with silicon;
High temperature treatment step of high temperature treatment of impregnated film after low temperature treatment:
A second low temperature treatment step of low temperature treatment of the impregnated film after the high temperature treatment;
It comprises a film winding step of winding the low temperature treated silicon impregnated film on the take-up roll,
In the film winding step, the silicon impregnated film is quenched while the silicon impregnated film is wound on the take-up roll, and the quenching treatment of the silicon impregnated film is made by a jet spray for spraying a coolant onto the silicon impregnated film to be wound, and the jet Spray is a silicone coating method of the polyimide film, characterized in that installed so as to move in a radial direction from the center of the winding roll.
제1항에 있어서,
상기 실리콘 액을 함침할 때 실리콘 액의 온도가 20℃ 이하인 것을 특징으로 하는 폴리이미드 필름의 실리콘 코팅방법.
The method of claim 1,
The silicon coating method of the polyimide film, characterized in that the temperature of the silicone liquid is 20 ℃ or less when the silicone liquid is impregnated.
제2항에 있어서,
상기 함침조에 저장된 실리콘액을 냉각시켜 온도계의 측정값이 20℃에 도달한 다음 20분 이상 에이징한 후 상기 폴리이미드 필름을 상기 함침조에 통과시키는 것을 특징으로 하는 폴리이미드 필름의 실리콘 코팅방법.
The method of claim 2,
Cooling the silicone liquid stored in the impregnating tank to reach the 20 ℃ ℃ measured value of the thermometer and then the polyimide film of the polyimide film, characterized in that passed through the impregnating tank after aging for 20 minutes or more.
삭제delete 삭제delete
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