JP5109657B2 - ポリイミドフィルムの製造方法およびポリイミドフィルム - Google Patents
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Description
この自己支持性フィルムの両面に有機液体を塗布する工程と、
有機液体を塗布した自己支持性フィルムを加熱、イミド化する工程と
を有するポリイミドフィルムの製造方法。
銅メッキ層の厚みが1〜9μmである上記11記載の銅張りポリイミドフィルム。
また、上記の自己支持性フィルムのイミド化率は、特開平9−316199記載のカールフィッシャー水分計を用いる手法で求めることができ、例えば、IR(ATR)で測定し、フィルムとフルキュア品との振動帯ピーク面積の比を利用して、イミド化率を算出することができる。振動帯ピークとしては、イミドカルボニル基の対称伸縮振動帯やベンゼン環骨格伸縮振動帯などを利用できる。
幅が広いフィルムの場合(幅が550〜2000mm程度)、L、C、R(フィルムの左端、中心、右端)から3点サンプリングし、上記と同様にして各測定値を求め、その平均値を求める。
重合槽に所定量のN,N−ジメチルアセトアミドを加え、次いで3,3’,4,4’−ビフェニルテトラカルボン酸二無水物、次いでパラフェニレンジアミンを加え、30℃で10時間重合反応させて、ポリマーの対数粘度(測定温度:30℃、濃度:0.5g/100ml溶媒、溶媒:N,N−ジメチルアセトアミド)が1.60、ポリマー濃度が18質量%であるポリイミド前駆体溶液を得た。このポリイミド前駆体溶液に、ポリイミド前駆体100質量部に対して0.1質量部の割合でモノステアリルリン酸エステルトリエタノールアミン塩および0.5質量部の割合で平均粒径0.08μmのコロイダルシリカを添加し、均一に混合してポリイミド前駆体溶液組成物を得た。このポリイミド前駆体溶液組成物の回転粘度は3000ポイズであった。
参考例1で得られたポリイミド前駆体溶液組成物をTダイ金型のスリットから連続的にキャスティング・乾燥炉の平滑な金属支持体に押出し、支持体上に薄膜を形成した。この薄膜を120〜160℃で10分間加熱後、支持体から剥離して自己支持性フィルムを得た。
溶媒塗布量:11g/m2 カール量:− 6mm、
溶媒塗布量:18g/m2 カール量:− 2mm。
線膨張係数(MD):12.6×10−6cm/cm/℃、
線膨張係数(TD):13.6×10−6cm/cm/℃。
参考例1で得られたポリイミド前駆体溶液組成物をTダイ金型のスリットから連続的にキャスティング・乾燥炉の平滑な金属支持体に押出し、支持体上に薄膜を形成した。この薄膜を120〜160℃で10分間加熱後、支持体から剥離して自己支持性フィルムを得た。
溶媒塗布量:11g/m2 カール量:−16mm、
溶媒塗布量:18g/m2 カール量:−26mm。
線膨張係数(MD):13.2PPM/℃、
線膨張係数(TD):14.0PPM/℃。
参考例1で得られたポリイミド前駆体溶液組成物をTダイ金型のスリットから連続的にキャスティング・乾燥炉の平滑な金属支持体に押出し、支持体上に薄膜を形成した。この薄膜を120〜160℃で10分間加熱後、支持体から剥離して自己支持性フィルムを得た。
自己支持性フィルムのA面、B面上に、シランカップリング剤のN,N−ジメチルアセトアミド溶液を塗布しなかった他は実施例3と同様にしてポリイミドフィルムを製造し、表面粗度を測定した。その結果を表1に示す。
表1中のRms、Ra、Rmaxの単位はnmである。
Claims (12)
- ポリイミド前駆体溶液の自己支持性フィルムを準備する工程と、
この自己支持性フィルムの両面に有機液体を塗布する工程と(ただし、自己支持性フィルムをカップリング剤を含む溶液に浸漬する工程を除く)、
両面に有機液体を塗布した自己支持性フィルムを加熱、イミド化する工程と
を有し、
前記ポリイミド前駆体溶液はポリイミド前駆体の有機溶媒溶液であり、前記有機液体がこのポリイミド前駆体溶液の有機溶媒と同じ有機溶媒を含む、5μm×5μmの測定範囲において、Rmsが両面とも3.0nm以下であり、Raが両面とも2.0nm以下であり、Rmaxが両面とも60nm以下であるポリイミドフィルムを製造する方法。 - 前記ポリイミド前駆体溶液の有機溶媒が、N−メチル−2−ピロリドン、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミドおよびN,N−ジエチルアセトアミドから選ばれる少なくとも1種以上である請求項1に記載のポリイミドフィルムの製造方法。
- ポリイミド前駆体溶液の自己支持性フィルムを準備する工程と、
この自己支持性フィルムの両面に有機液体を塗布する工程と(ただし、自己支持性フィルムをカップリング剤を含む溶液に浸漬する工程を除く)、
両面に有機液体を塗布した自己支持性フィルムを加熱、イミド化する工程と
を有し、
前記有機液体が、N−メチル−2−ピロリドン、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミドおよびN,N−ジエチルアセトアミドから選ばれる少なくとも1種以上を含む、5μm×5μmの測定範囲において、Rmsが両面とも3.0nm以下であり、Raが両面とも2.0nm以下であり、Rmaxが両面とも60nm以下であるポリイミドフィルムを製造する方法。 - 前記有機液体が、ポリイミド前駆体溶液の有機溶媒と同じ有機溶媒、または、溶媒がポリイミド前駆体溶液の有機溶媒と同じ有機溶媒であるカップリング剤の有機溶媒溶液である請求項1〜3のいずれかに記載のポリイミドフィルムの製造方法。
- 自己支持性フィルムの両面に有機液体を塗布する工程が、自己支持性フィルムの片面にカップリング剤の有機溶媒溶液を塗布し、他面にカップリング剤を含まない有機液体を塗布し、カップリング剤を含まない有機液体の塗布量を制御することにより、カールを制御した工程である請求項1〜4のいずれかに記載のポリイミドフィルムの製造方法。
- 自己支持性フィルムの両面に有機液体を塗布する工程が、片面の有機液体の塗布量を制御することにより、カールを制御した工程である請求項1〜4のいずれかに記載のポリイミドフィルムの製造方法。
- 請求項1〜4のいずれかに記載の方法により製造されるポリイミドフィルム。
- 請求項5または6に記載の方法により製造されるポリイミドフィルム。
- フィルムの10cm角の正方形のサンプルについて測定したカールが0〜−30mmの範囲内である請求項8に記載のポリイミドフィルム。
- 厚みが10〜38μmである請求項7〜9のいずれかに記載のポリイミドフィルム。
- 請求項1〜6のいずれかに記載の方法により製造され、自己支持性フィルムの少なくとも片面にカップリング剤の有機溶媒溶液を塗布して製造されたポリイミドフィルムの、製造時にカップリング剤の有機溶媒溶液を塗布した面に、スパッタ下地金属層および銅メッキ層を形成してなる銅張りポリイミドフィルム。
- 下地金属層が厚み1〜30nmのNi/Cr合金層および100〜1000nmのスパッタ銅層からなり、
銅メッキ層の厚みが1〜9μmである請求項11に記載の銅張りポリイミドフィルム。
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JP5164464B2 (ja) * | 2007-07-27 | 2013-03-21 | 株式会社アルバック | 樹脂基板 |
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JP5304490B2 (ja) * | 2009-07-02 | 2013-10-02 | 東洋紡株式会社 | 積層体およびその製造方法 |
JP5267379B2 (ja) * | 2009-08-18 | 2013-08-21 | 住友金属鉱山株式会社 | 金属被覆ポリイミドフィルムとその製造方法 |
JP5609891B2 (ja) * | 2009-12-09 | 2014-10-22 | 宇部興産株式会社 | ポリイミドフィルムの製造方法、およびポリイミドフィルム |
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US20090297837A1 (en) | 2009-12-03 |
KR20070120553A (ko) | 2007-12-24 |
KR100967326B1 (ko) | 2010-07-05 |
US8415024B2 (en) | 2013-04-09 |
CN101184795A (zh) | 2008-05-21 |
CN101184795B (zh) | 2012-03-28 |
WO2006109753A1 (ja) | 2006-10-19 |
JPWO2006109753A1 (ja) | 2008-11-20 |
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