JP6496812B2 - ポリイミド積層フィルム、ポリイミド積層フィルムの製造方法、熱可塑性ポリイミドの製造方法、およびフレキシブル金属張積層体の製造方法 - Google Patents
ポリイミド積層フィルム、ポリイミド積層フィルムの製造方法、熱可塑性ポリイミドの製造方法、およびフレキシブル金属張積層体の製造方法 Download PDFInfo
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- JP6496812B2 JP6496812B2 JP2017510118A JP2017510118A JP6496812B2 JP 6496812 B2 JP6496812 B2 JP 6496812B2 JP 2017510118 A JP2017510118 A JP 2017510118A JP 2017510118 A JP2017510118 A JP 2017510118A JP 6496812 B2 JP6496812 B2 JP 6496812B2
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- polyimide
- laminated film
- thermoplastic polyimide
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- 229920006259 thermoplastic polyimide Polymers 0.000 title claims description 81
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- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 49
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- XUSNPFGLKGCWGN-UHFFFAOYSA-N 3-[4-(3-aminopropyl)piperazin-1-yl]propan-1-amine Chemical compound NCCCN1CCN(CCCN)CC1 XUSNPFGLKGCWGN-UHFFFAOYSA-N 0.000 claims description 17
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 15
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- 125000006159 dianhydride group Chemical group 0.000 claims 4
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims 4
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Description
本発明のポリイミド積層フィルムは、380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBと、を含む熱可塑性ポリイミド層を含むことを特徴とする。
熱可塑性ポリイミド層を構成する熱可塑性ポリイミドは、380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBと、を共重合させる工程を含む方法によって製造され得る。
本発明に用いられる熱可塑性ポリイミド層の前駆体となる熱可塑性ポリアミド酸を合成することができる原料モノマーは、380℃での貯蔵弾性率が0.15GPa以上であるブロックA、および380℃での貯蔵弾性率が0.10GPa以下であるブロックBを形成し得るものであればよく、通常用いられる芳香族ジアミンおよび芳香族酸二無水物を使用可能である。
本発明における熱可塑性ポリイミドに含まれるブロックAとブロックBとの組成比について、(ブロックAの量:ブロックBの量)が、(30モル%:70モル%)〜(70モル%:30モル%)の範囲であることが好ましい。
熱可塑性ポリアミド酸を製造する際に用いられる溶媒は、熱可塑性ポリアミド酸を溶解する溶媒であればいかなるものも用いることができるが、アミド系溶媒すなわちN,N−ジメチルホルムアミド、N,N−ジメチルアセトアミド、N−メチル−2−ピロリドンなどを好ましく用い得、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミドを特に好ましく用い得る。
本発明における熱可塑性ポリアミド酸の製造方法は、ブロックAとブロックBとを含む熱可塑性ポリイミドであって、380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBとを含む熱可塑性ポリイミド層を形成し得る方法であれば、公知のどうような方法も用いることが可能である。例えば、下記の工程(a)〜(c):
(a)芳香族ジアミンと、芳香族酸二無水物とを、芳香族ジアミンが過剰の状態にて有機極性溶媒中で反応させ、両末端にアミノ基を有するプレポリマーを得る工程、
(b)工程(a)で用いたものとは構造の異なる芳香族ジアミンを、上記有機極性溶媒中に追加添加する工程、
(c)更に、工程(a)で用いたものとは構造の異なる芳香族酸二無水物を、全工程における芳香族ジアミンと芳香族酸二無水物とが実質的に等モルとなるように、上記有機極性溶媒中に添加して重合する工程、
によって、熱可塑性ポリアミド酸を製造することができる。
(a)芳香族ジアミンと、芳香族酸二無水物とを、芳香族酸二無水物が過剰の状態にて有機極性溶媒中で反応させ、両末端に酸無水物基を有するプレポリマーを得る工程、
(b)工程(a)で用いたものとは構造の異なる芳香族酸二無水物を、上記有機極性溶媒中に追加添加する工程、
(c)更に、工程(a)で用いたものとは構造の異なる芳香族ジアミンを、全工程における芳香族ジアミンと芳香族酸二無水物とが実質的に等モルとなるように、上記有機極性溶媒中に添加して重合する工程、
によって、熱可塑性ポリアミド酸を製造することができる。
熱可塑性ポリアミド酸の固形分濃度は特に限定されないが、5重量%〜35重量%の範囲内であれば、十分な機械強度を有する熱可塑性ポリイミドが得られる。
本発明の熱可塑性ポリアミド酸には、フィラー、熱安定剤、酸化防止剤、紫外線吸収剤、帯電防止剤、難燃剤、顔料、染料、脂肪酸エステル、有機滑剤(例えばワックス)等の、各種添加剤を加えることができる。
本発明のポリイミド積層フィルムは、非熱可塑性ポリイミドフィルムの少なくとも片面に本発明の熱可塑性ポリイミド層を有するものであり得る。以下、本発明において用いられる非熱可塑性ポリイミドフィルムの例を説明する。
上記非熱可塑性ポリイミドフィルムの製造方法は、以下の工程:
i)有機溶剤中で芳香族ジアミンと芳香族テトラカルボン酸二無水物とを反応させて非熱可塑性ポリアミド酸溶液を得る工程、
ii)上記非熱可塑性ポリアミド酸溶液を含む製膜ドープをダイスから支持体上に流延して、樹脂膜(樹脂層または液膜ともいうことがある)を形成する工程、
iii)樹脂膜を支持体上で加熱して自己支持性を持ったゲルフィルムとした後、支持体からゲルフィルムを引き剥がす工程、
iv)ゲルフィルムを更に加熱して、残ったアミド酸をイミド化し、かつ乾燥させて非熱可塑性ポリイミドフィルムを得る工程、
を含むことが好ましい。
本発明のポリイミド積層フィルムを製造する方法としては、上記ii)工程において複数の流路を有する共押出しダイを使用して、熱可塑性ポリアミド酸および非熱可塑性ポリアミド酸を含む複層の樹脂膜を同時に形成しても良いし、上記i)において非熱可塑性ポリアミド酸を合成し、その後上記ii)〜iv)工程まで進めて非熱可塑性ポリイミドフィルムを一旦回収した後、その上に塗工などで新たに熱可塑性ポリアミド酸を含む樹脂膜を形成しても良い。イミド化には非常に高い温度が必要となるため、ポリイミド以外の樹脂膜を設ける場合は、熱分解を抑えるために後者の手段を採った方が好ましい。なお、塗工により熱可塑性ポリイミド層を設ける場合は、非熱可塑性ポリイミドフィルム上に熱可塑性ポリアミド酸を塗布し、その後イミド化を行ってもよいし、熱可塑性ポリイミド層を形成することができる熱可塑性ポリイミド溶液を非熱可塑性ポリイミドフィルム上に塗布・乾燥してもよい。
a)上述のようにしてポリイミド積層フィルムを得た後、加熱加圧によりポリイミド積層フィルムに金属箔を貼り合せてフレキシブル金属張積層体を得る手段(熱ラミネート法)、
b)金属箔上に、熱可塑性ポリアミド酸溶液または非熱可塑性ポリアミド酸溶液の少なくともいずれか一方の溶液を含有する多層の有機溶剤溶液をキャストし、加熱により、有機溶剤溶液から溶剤除去、イミド化を行ってフレキシブル金属張積層体を得る手段(キャスト法)、
c)金属箔上に、熱可塑性ポリイミド酸溶液または非熱可塑性ポリイミド酸溶液の少なくともいずれか一方のポリイミドを含有する溶融液をキャストし、当該溶融液を冷却することによりフレキシブル金属張積層体を得る手段(キャスト法)、
が挙げられる。このうち、ポリイミドに溶融性を持たせると、得られるフレキシブル金属張積層体の半田耐熱性や加熱収縮率などが悪化する可能性があるため、a)もしくはb)の手段を用いることが好ましい。ポリイミドが溶剤可溶性のものであるなら、ポリアミド酸を含有する有機溶剤溶液の代わりにポリイミドを含有する有機溶剤溶液を用いても良い。a)ならびにb)の詳細について、以下に説明する。
貯蔵弾性率については、SIIナノテクノロジー社製 DMS6100により空気雰囲気下にて動的粘弾性を測定し、測定温度に対してtanδをプロットしたグラフを作成し、当該グラフから380℃における貯蔵弾性率を読み取った。合成例1〜9の熱可塑性ポリイミド層、合成例1〜4、8、9の熱可塑性ポリイミド層を構成するブロックAおよびブロックB単独の貯蔵弾性率を測定した。ガラス転移温度(Tg(℃))は損失弾性率を貯蔵弾性率で割って得られる損失係数(tanδ)のピークトップの温度とした。
・測定温度範囲;0℃〜440℃
・昇温速度;3℃/分
・歪み振幅;10μm
・測定周波数;5Hz
・最小張力/圧縮力;100mN
・張力/圧縮ゲイン;1.5
・力振幅初期値;100mN
(重量減少率測定)
3cm×7cmにカットしたフィルムを3枚準備し、50℃で30分間加熱した後、初期重量W0を計った。サンプルを80℃に加熱した3%水酸化ナトリウム水溶液に10分間浸漬した。浸漬後、純水で洗浄し、50℃で30分間乾燥させた後に重量W1を計った。下記式を用いて重量減少率を求めた。
重量減少率(%)=(W0−W1)/W0×100
(クラックの有無)
フレキシブル金属箔積層体のデスミア液浸漬時のクラック耐性(具体的には、クラックの有無)を以下の方法により評価した。
クラックが確認されないものを「◎」、クラックが確認されるもののクラックの大きさ(長手方向)が1μm未満のものを「○」、クラックが確認されたものを「×」と評価した。なお、光学顕微鏡を使用して確認されたクラック(割れ、裂け)は、その大きさを問わずクラックとした。光学顕微鏡の倍率はクラックと思われる箇所を判断するために最適な倍率とした。
作製した多層ポリイミドフィルムの両面に、厚さ12μmの電解銅箔(3EC−M3S−HTE(K)、三井金属製)を配置し、ラミネート温度360℃、圧力0.8t、ラインスピード1m/minで熱圧着した。銅箔とポリイミドフィルムとからなるサンプルをJIS C6471の「6.5 引きはがし強さ」に従って解析した。具体的には、1mm幅の金属箔部分を、90度の剥離角度、100mm/分の条件で剥離し、その荷重を測定した。ピール強度が12N/cm以上の場合を「○」、それ未満を「×」と評価した。
(合成例1)
反応系内を20℃に保った状態で、N,N−ジメチルアセトアミド(以下、DMFともいう)167.7kgに、4,4’−ビス(4−アミノフェノキシ)ビフェニル(以下、BAPBともいう)4.87kgを加え、窒素雰囲気下で攪拌しながら、3,3’,4,4’−ビフェニルテトラカルボン酸二無水物(以下、BPDAともいう)3.24kgを徐々に添加した。BPDAが溶解したことを目視確認した後、2,2’−ビス[4−(4−アミノフェノキシ)フェニル]プロパン(以下、BAPPともいう)12.67kgを添加した。続いて、ピロメリット酸二無水物(以下、PMDAともいう)6.88kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:BAPB−BPDA、ブロックB:BAPP−PMDA)。
反応系内を20℃に保った状態で、DMF172.0kgに、4,4’−ジアミノジフェニルエーテル(以下、ODAともいう)6.78kgを加え、窒素雰囲気下で攪拌しながら、BPDA9.19kgを徐々に添加した。BPDAが溶解したことを目視確認した後、BAPP7.48kgを添加した。続いて、PMDA4.15kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:ODA−BPDA、ブロックB:BAPP−PMDA)。
反応系内を20℃に保った状態で、DMF172.0kgに、BAPB5.04kgを加え、窒素雰囲気下で攪拌しながら、BPDA3.35kgを徐々に添加した。BPDAが溶解したことを目視確認した後、BAPP11.23kg、ODA0.91kgを添加した。続いて、PMDA7.11kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:BAPB−BPDA、ブロックB:BAPP−ODA−PMDA)。
反応系内を20℃に保った状態で、DMF172.0kgに、BAPB7.49kg、ODA1.36kgを加え、窒素雰囲気下で攪拌しながら、BPDA7.31kgを徐々に添加した。BPDAが溶解したことを目視確認した後、BAPP7.42kgを添加した。続いて、PMDA4.09kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:BAPB−ODA−BPDA、ブロックB:BAPP−PMDA)。
反応系内を20℃に保った状態で、DMF172.0kgに、BPDA12.43kgを加え、窒素雰囲気下で攪拌しながら、BAPB15.02kgを徐々に添加し30分間攪拌を行った。0.7kgのBAPBを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックB:なし)。
反応系内を20℃に保った状態で、DMF172.0kgに、BAPP18.28kgを加え、窒素雰囲気下で攪拌しながら、PMDA9.38kgを徐々に添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:なし)。
反応系内を20℃に保った状態で、DMF172.0kgに、BAPB4.87kg、BAPP12.67kgを加え、窒素雰囲気下で攪拌し、BAPB、BAPPが溶解したことを確認した。BPDA3.24kg、PMDA6.88kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA、B:なし)。
反応系内を20℃に保った状態で、DMF167.6kgに、BAPB8.85kgを加え、窒素雰囲気下で攪拌しながら、BPDA6.36kgを徐々に添加した。BPDAが溶解したことを目視確認した後、1,3−ビス(4−アミノフェノキシ)ベンゼン (以下、TPE−Rともいう)7.02kgを添加した。続いて、PMDA5.45kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:BAPB−BPDA、ブロックB:TPE−R−PMDA)。
反応系内を20℃に保った状態で、DMF167.4kgに、3,4’−ジアミノジフェニルエーテル(以下、3,4’−ODAともいう)5.03kgを加え、窒素雰囲気下で攪拌しながら、BPDA6.65kgを徐々に添加した。BPDAが溶解したことを目視確認した後、BAPP10.30kgを添加した。続いて、PMDA5.69kgを添加し30分間攪拌を行った。0.7kgのPMDAを固形分濃度7%となるようにDMFに溶解した溶液を調整し、この溶液を粘度上昇に気を付けながら上記反応溶液に徐々に添加し、粘度が300ポイズに達した時点で重合を終了した(ブロックA:3,4’−ODA−BPDA、ブロックB:BAPP−PMDA)。
(合成例10)
反応系内を20℃に保った状態で、DMF170.0kgに、ODA5.50kg、BAPP2.82kgを添加し、窒素雰囲気下で撹拌した。ODA、BAPPが溶解したことを目視確認した後、BTDA4.43kgを添加した。BTDAが溶解したことを目視確認した後、PMDA7.79kgを添加して、溶解したことを確認した後、30分間攪拌を行った。p−PDA3.42kg、ODA0.55kgを添加し、溶解したことを目視確認した後、PMDA7.79kgを徐々に添加し、30分間攪拌を行った。
合成例10で得られたポリイミドフィルムの両面に、合成例1で得られたポリアミック酸溶液を、片面あたりの最終厚みが3.0μmとなるように塗布し、140℃で2分間乾燥した。続いて、350℃で1分間加熱してイミド化を行い、総厚み18.5μmのポリイミド積層フィルムを得た。
合成例1で得られたポリイミドフィルムの代わりに、合成例2で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例3で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例4で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例5で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例6で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例7で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例8で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
合成例1で得られたポリイミドフィルムの代わりに、合成例9で得られたポリイミドフィルムを使用する以外は実施例1と同様の操作を行い、フレキシブル金属箔積層体を作製した。
以下に、合成例1〜4、8、9のブロックA、ブロックBのそれぞれの貯蔵弾性率を測定するためのポリアミド酸の合成例、およびフィルムの製造例を示す。合成例1〜4、8、9のブロックA単独、または、ブロックB単独をそれぞれ等モル量を用いて、ポリアミド酸溶液を得た。当該ポリアミド酸溶液に無水酢酸/イソキノリン/DMF(重量比2.0/0.6/2.8)からなるイミド化促進剤をポリアミド酸溶液に対して重量比50%で添加し、連続的にミキサーで撹拌した。当該混合物をTダイから押出してステンレス製のエンドレスベルト上に流延した。この樹脂膜を130℃×100秒で加熱した後エンドレスベルトから自己支持性のゲル膜を引き剥がした。当該ゲル膜をテンタークリップに固定し、250℃×15秒、300℃×87秒で乾燥・イミド化させ、厚み12.5μmの熱可塑性ポリイミドフィルムを得た。これら熱可塑性ポリイミドフィルムの粘弾性測定結果も表1に示す。
2.不織布
3.金属板
4.クラフト
5.塩化ビニル樹脂フィルム
6.離型フィルム
7.電解銅箔
10.積層材(2、3、4、5、6)
11.フレキシブル金属箔積層体
Claims (7)
- 380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBと、を含む熱可塑性ポリイミド層を含み、
上記ブロックAが、少なくとも、4,4’−ビス(4−アミノフェノキシ)ビフェニル(BAPB)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、3,3’,4,4’−ビフェニルテトラカルボン酸二無水物(BPDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックBが、少なくとも、2,2’−ビス[4−(4−アミノフェノキシ)フェニル]プロパン(BAPP)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、ピロメリット酸二無水物(PMDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックAの含有量が25〜55モル%、ブロックBの含有量が40〜75モル%の範囲であり、
上記熱可塑性ポリイミド層が非熱可塑性ポリイミドフィルムの少なくとも片面に備えられたものであることを特徴とする、ポリイミド積層フィルム。 - 上記ポリイミド積層フィルムは、アルカリ溶液に80℃、10分間浸漬した時に、重量減少率が2重量%未満のものであることを特徴とする、請求項1に記載のポリイミド積層フィルム。
- 上記熱可塑性ポリイミド層は、380℃での貯蔵弾性率が0.05GPa以下のものであることを特徴とする、請求項1または2に記載のポリイミド積層フィルム。
- 380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBと、を共重合させる工程を含み、
上記ブロックAが、少なくとも、4,4’−ビス(4−アミノフェノキシ)ビフェニル(BAPB)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、3,3’,4,4’−ビフェニルテトラカルボン酸二無水物(BPDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックBが、少なくとも、2,2’−ビス[4−(4−アミノフェノキシ)フェニル]プロパン(BAPP)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、ピロメリット酸二無水物(PMDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックAの含有量が25〜55モル%、ブロックBの含有量が40〜75モル%の範囲であることを特徴とする、熱可塑性ポリイミドの製造方法。 - 380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBと、を含む熱可塑性ポリイミド層と、
非熱可塑性ポリイミド層と、を積層する工程を有するポリイミド積層フィルムの製造方法であって、
上記ブロックAが、少なくとも、4,4’−ビス(4−アミノフェノキシ)ビフェニル(BAPB)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、3,3’,4,4’−ビフェニルテトラカルボン酸二無水物(BPDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックBが、少なくとも、2,2’−ビス[4−(4−アミノフェノキシ)フェニル]プロパン(BAPP)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、ピロメリット酸二無水物(PMDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックAの含有量が25〜55モル%、ブロックBの含有量が40〜75モル%の範囲であり、
上記ポリイミド積層フィルムは、上記熱可塑性ポリイミド層が上記非熱可塑性ポリイミド層の少なくとも片面に備えられたものであることを特徴とするポリイミド積層フィルムの製造方法。 - 380℃での貯蔵弾性率が0.15GPa以上であるブロックAと、380℃での貯蔵弾性率が0.10GPa以下であるブロックBと、を含む熱可塑性ポリイミド層を含んでいるポリイミド積層フィルムと、
金属箔と、を積層する工程を有し、
上記ブロックAが、少なくとも、4,4’−ビス(4−アミノフェノキシ)ビフェニル(BAPB)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、3,3’,4,4’−ビフェニルテトラカルボン酸二無水物(BPDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックBが、少なくとも、2,2’−ビス[4−(4−アミノフェノキシ)フェニル]プロパン(BAPP)、4,4’−ジアミノジフェニルエーテル(ODA)から選ばれるジアミンと、ピロメリット酸二無水物(PMDA)である酸二無水物の組合せで得られるブロック成分であり、
上記ブロックAの含有量が25〜55モル%、ブロックBの含有量が40〜75モル%の範囲であり、
上記ポリイミド積層フィルムは、上記熱可塑性ポリイミド層が非熱可塑性ポリイミドフィルムの少なくとも片面に備えられたものであることを特徴とするフレキシブル金属張積層体の製造方法。 - 上記積層する工程は、熱ラミネート法、または、キャスト法によって行われることを特徴とする請求項6に記載のフレキシブル金属張積層体の製造方法。
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JP5931654B2 (ja) * | 2012-09-03 | 2016-06-08 | 日立金属株式会社 | 絶縁電線及びそれを用いたコイル |
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