JP6763115B2 - 超薄膜ブラックポリイミドフィルム及びその製造方法(ultra thin black polyimide film and method for preparing the same) - Google Patents
超薄膜ブラックポリイミドフィルム及びその製造方法(ultra thin black polyimide film and method for preparing the same) Download PDFInfo
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- C09D179/00—Coating compositions based on 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 C09D161/00 - C09D177/00
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Description
超薄膜ブラックポリイミドフィルムの製造(厚さ7.5μm)
ポリアミック酸溶液重合工程であって、300L反応器に窒素雰囲気下で溶媒としてN,N’-ジメチルホルムアミド(DMF)を733.5g投入した。温度を25℃にして、ジアミンとして4,4'-ジアミノフェニレンエーテル(ODA)63.25g及び1,4-フェニレンジアミン(PPD)11.39gを入れた。30分ほど攪拌し単量体が溶解されたことを確認してからピロメリット酸二無水物(PMDA)を91.86g投入した。投入が終わると温度を維持しながら1時間攪拌してポリアミック酸溶液を重合した。
超薄膜ブラックポリイミドフィルムの製造(厚さ7.5μm)
下記表1に記載された第1カーボンブラック及び第2カーボンブラックの平均粒径及び含量を使用したことを除いては、実施例1と同一の方法で厚さ7.5μmの超薄膜ブラックポリイミドフィルムを製造した。
超薄膜ブラックポリイミドフィルムの製造(厚さ5μm)
下記表2に記載された第1カーボンブラック及び第2カーボンブラックの平均粒径及び含量を用い、SUS plateにドクターブレードを使用して50μmにキャストすることを除いては、実施例1と同一の方法で厚さ5μmの超薄膜ブラックポリイミドフィルムを製造した。
超薄膜ブラックポリイミドフィルムの製造(厚さ7.5μm)
下記表3に記載されたPPDの含量を使用したことを除いては、実施例1と同一の方法で厚さ7.5μmの超薄膜ブラックポリイミドフィルムを製造した。
超薄型ブラックポリイミドフィルムの製造(厚さ5μm)
下記表4に記載されたPPDの含量を用い、SUS plateにドクターブレードを使用して50μmにキャストすることを除いては、実施例1と同一の方法で厚さ5μmの超薄膜ブラックポリイミドフィルムを製造した。
(実験例1)
光沢の評価
光沢度測定装備(モデル名:E406L、製造社:Elcometer)で60°の角度でASTMD523の方法で測定した。
透過率の評価
透過率測定機器(モデル名:ColorQuesetXE、製造社:HunterLab)を用いて可視光領域においてASTMD1003の方法で透過度を測定した。
寸法安定性の評価-熱膨張係数(CTE)
熱分析器(モデル名:Q400、製造社:TA)を用いて0.05Nの圧力下で10℃/分の速度で400℃まで昇温させた後、さらに10℃/分の速度で40℃まで冷却させた。その後、10℃/分の速度で400℃まで昇温させながら、昇温区間中の100〜200℃区間の傾きを測定した。
Claims (9)
- 二無水物とジアミン類から得られたポリアミック酸をイミド化して得られるポリイミドフィルムであって、
平均粒径1〜5μmの第1カーボンブラック及び平均粒径0.1〜0.99μmの第2カーボンブラックを前記フィルム総重量に対してそれぞれ3〜10重量%及び1〜5重量%含み、
前記ジアミン類が1,4-フェニレンジアミン、オキシジアニリン、4,4'-メチレンジアニリン(MDA)、及び1,3-ビス(4-アミノフェノキシ)ベンゼン(TPE-R)からなる群から選択された1種以上であり、
前記1,4-フェニレンジアミンが総ジアミン類に対して20〜30モル%で含まれ、
可視光線領域における光透過度が10%以下であり、光沢度が10〜40%であり、
フィルムの厚さが8μm以下である超薄膜ブラックポリイミドフィルム。 - 第1項において、
前記二無水物がピロメリット酸二無水物(PMDA)、ビフェニルテトラカルボン酸二無水物(BPDA)、及びオキシジフタル酸無水物(ODPA)からなる群から選択された1種以上である超薄膜ブラックポリイミドフィルム。 - 第1項において、
前記フィルムの厚さが5〜8μmである超薄膜ブラックポリイミドフィルム。 - 第1項において、
前記超薄膜ブラックポリイミドフィルムが10〜20ppm/℃の熱膨張係数(CTE)を有する超薄膜ブラックポリイミドフィルム。 - (1)二無水物とジアミン類からポリアミック酸溶液を重合する段階;
(2)ミリング機器を用いて平均粒径1〜5μmの第1カーボンブラック、及び平均粒径0.1〜0.99μmの第2カーボンブラックをそれぞれ製造する段階;
(3)前記ポリアミック酸溶液に第1カーボンブラック及び第2カーボンブラックを混合して分散させた後、支持体に製膜する段階;
(4)熱処理してイミド化する段階;及び
(5)冷却処理してフィルム化する段階を含み、
前記ジアミン類が1,4-フェニレンジアミン、オキシジアニリン、4,4'-メチレンジアニリン(MDA)、及び1,3-ビス(4-アミノフェノキシ)ベンゼン(TPE-R)からなる群から選択された1種以上であり、
前記1,4-フェニレンジアミンが総ジアミン類に対して20〜30モル%で含まれ、
フィルムが8μm以下の厚さを有する、超薄膜ブラックポリイミドフィルムの製造方法。 - 第5項において、
前記フィルムが前記第1カーボンブラック及び第2カーボンブラックを前記フィルム総重量に対して3〜10重量%及び1〜5重量%で含む超薄型ブラックポリイミドフィルムの製造方法。 - 第5項において、
前記段階(3)において、前記第1カーボンブラック及び第2カーボンブラックは極性溶媒に分散させた溶液の形態で混合される超薄膜ブラックポリイミドフィルムの製造方法。 - 第7項において、
前記極性溶媒は、N,N’-ジメチルホルムアミド、N,N’-ジメチルアセトアミド、及びN-メチル-ピロリドンからなる群から選択された1種以上である超薄膜ブラックポリイミドフィルムの製造方法。 - 第5項において、
前記フィルムが可視光線領域において10%以下の光透過度、10〜40%の光沢度及び10〜20ppm/℃の熱膨張係数(CTE)を有する、超薄膜ブラックポリイミドフィルムの製造方法。
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KR20230171297A (ko) * | 2022-06-13 | 2023-12-20 | 피아이첨단소재 주식회사 | 블랙 폴리이미드 필름 및 그의 제조방법 |
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US3024092A (en) * | 1957-06-03 | 1962-03-06 | Exxon Research Engineering Co | Modified carbon black and methods of preparing and using same |
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US8574720B2 (en) * | 2009-08-03 | 2013-11-05 | E.I. Du Pont De Nemours & Company | Matte finish polyimide films and methods relating thereto |
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US20130273254A1 (en) * | 2012-04-13 | 2013-10-17 | Mortech Corporation | Polymide film and method for manufacturing the same |
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US20180346720A1 (en) | 2018-12-06 |
CN108976447A (zh) | 2018-12-11 |
US10519312B2 (en) | 2019-12-31 |
KR101908684B1 (ko) | 2018-10-16 |
TW201900748A (zh) | 2019-01-01 |
CN108976447B (zh) | 2021-07-06 |
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