JP2020505486A - ポリアミドイミドフィルムおよびその製造方法 - Google Patents
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Abstract
Description
[ポリアミドイミドフィルム]
次いで、前記ポリアミック酸は、脱水反応によりポリイミドに転換され得、前記ポリイミドはイミド(imide)繰り返し単位を含む。
例えば、前記ポリイミドは、下記化学式3で表される化合物を含み得るが、これに限定されるものではない。
前記化学式3のnは1〜400の整数である。
前記化学式6のxは1〜400の整数である。
前記化学式7のyは1〜400の整数である。
前述のポリアミドイミドフィルムに関する様々な特性が組み合わせわされ得る。
[ポリアミドイミドフィルムの製造方法]
これは所望の粘度を正確に達成できるという点から有利である。
前記第2重合体溶液の粘度が前記範囲であると、押出およびキャスティング工程において効率的にポリアミドイミドフィルムが製造され得る。また、製造されたポリアミドイミドフィルムは、向上されたモジュラスなどの機械的物性を有し得る。
前記中和剤の例として、アルコキシアミン、アルキルアミンまたはアルカノールアミンなどのアミン系中和剤などが挙げられるが、これらに限定されるものではない。
前記中和剤により調節された第2重合体溶液のpHは、約4〜約7であり得る。具体的に、調節された第2重合体溶液のpHは、約4.5〜約7であり得る。
前記押出およびキャスティング工程の際、前述の有機溶媒が使用され得る。
前記乾燥工程は、約60℃〜約150℃の温度で、約5分〜約60分間行える。
また、前記第1減温段階の減温速度が前記第2減温段階の減温速度よりも速いこともあり得る。
例えば、前記第1減温段階中の最大速度が、前記第2減温段階中の最大速度よりも速い。または、前記第1減温段階中の最低速度が、前記第2減温段階中の最低速度よりも速い。
(実施例)
(実施例1〜実施例3)
(比較例1)
(比較例2)
[評価例1:フィルムの厚さ測定]
[評価例2:モジュラス(modulus)測定]
[評価例3:表面硬度測定]
[評価例4:黄色度(YI)測定]
[評価例5:光透過度(TT)およびヘイズ(HZ)測定]
[評価例6:XRDグラフ]
測定されたXRDグラフ結果について、2θ=8°〜32°の区間をベースラインとして指定し、MDI社のJADE9ソフトウェアを利用して、ガウス型(Gaussian type)により2θ=15°付近のピークの面積と2θ=23°付近のピークの面積をそれぞれ算出した。
Claims (20)
- 芳香族ジアミン化合物、芳香族ジアンヒドリド化合物およびジカルボニル化合物を重合して形成されたポリアミドイミド重合体を含み、
XRDグラフにおいて2θ=8°〜32°の区間をベースラインとしたとき、2θ=15°付近のピーク面積を基準に、2θ=23°付近のピーク面積が50%以上である、ポリアミドイミドフィルム。 - 前記XRDグラフにおいて2θ=8°〜32°の区間をベースラインとしたとき、2θ=15°付近のピーク面積を基準に、2θ=23°付近のピーク面積が60%以上である、請求項1に記載のポリアミドイミドフィルム。
- 前記ポリアミドイミドフィルムの厚さ50μmを基準に、モジュラスが5.0GPa以上である、請求項1に記載のポリアミドイミドフィルム。
- 前記ポリアミドイミドフィルムの表面硬度がHB以上である、請求項1に記載のポリアミドイミドフィルム。
- 前記ポリアミドイミドフィルムの厚さ50μmを基準に、黄色度が5以下である、請求項1に記載のポリアミドイミドフィルム。
- 前記ポリアミドイミドフィルムの厚さ50μmを基準に、ヘイズが2%以下である、請求項1に記載のポリアミドイミドフィルム。
- 前記ポリアミドイミドフィルムの厚さ50μmを基準に、550nmで測定した光透過度が85%以上である、請求項1に記載のポリアミドイミドフィルム。
- 前記芳香族ジアンヒドリド化合物は、フッ素含有置換基を有する化合物からなる、請求項1に記載のポリアミドイミドフィルム。
- 前記芳香族ジアミン化合物は、2,2'−ビス(トリフルオロメチル)−4,4'−ジアミノビフェニル(2,2'−Bis(trifluoromethyl)−4,4'−diaminobiphenyl、TFDB)を含み、
前記芳香族ジアンヒドリド化合物は、2,2'−ビス(3,4−ジカルボキシフェニル)ヘキサフルオロプロパンジアンヒドリド(2,2'−Bis(3,4−Dicarboxyphenyl)hexafluoropropane dianhydride、6−FDA)を含む、請求項1に記載のポリアミドイミドフィルム。 - 前記芳香族ジアミン化合物に対する前記芳香族ジアンヒドリド化合物のモル比は10:2〜10:4である、請求項1に記載のポリアミドイミドフィルム。
- 前記ジカルボニル化合物は、互いに異なる少なくとも2種のジカルボニル化合物を含む、請求項1に記載のポリアミドイミドフィルム。
- 前記ジカルボニル化合物は、テレフタロイルクロリド(terephthaloyl chloride、TPC)、1,1'−ビフェニル−4,4'−ジカルボニルジクロリド(1,1'−biphenyl−4,4'−dicarbonyl dichloride、BPDC)またはこれらの組み合わせを含む、請求項1に記載のポリアミドイミドフィルム。
- 芳香族ジアミン化合物、芳香族ジアンヒドリド化合物およびジカルボニル化合物を重合してポリアミドイミド重合体溶液を調製する段階と、
前記重合体溶液をタンクに投入する段階と、
前記タンク内の重合体溶液を押出およびキャスティングした後乾燥させて、ゲルシートを製造する段階と、
前記ゲルシートを熱処理する段階とを含み、
前記重合体溶液の粘度が10万cps〜30万cpsであり、
前記熱処理段階が、80℃〜500℃の温度範囲で2℃/min〜80℃/minの速度で昇温させながら5分〜40分間行われ、前記熱処理段階中の最高温度が300℃〜500℃である、ポリアミドイミドフィルムの製造方法。 - 前記タンクの内部温度が−20℃〜0℃である、請求項13に記載のポリアミドイミドフィルムの製造方法。
- 前記調製された重合体溶液をタンクに投入する段階の後に、
前記タンク内の圧力が0.2bar〜0.4barになるまで、1時間〜2時間真空脱泡する段階をさらに含む、請求項13に記載のポリアミドイミドフィルムの製造方法。 - 前記調製された重合体溶液をタンクに投入する段階の後に、
窒素ガスを使用して1気圧〜2気圧で、前記タンクをパージ(purging)する段階をさらに含む、請求項13に記載のポリアミドイミドフィルムの製造方法。 - 前記乾燥は、60℃〜150℃の温度で、5分〜60分間行われる、請求項13に記載のポリアミドイミドフィルムの製造方法。
- 前記熱処理段階中の最高温度が400℃〜500℃である、請求項13に記載のポリアミドイミドフィルムの製造方法。
- 前記熱処理段階の後に、
前記熱処理されたシートを減温させる段階をさらに含み、
前記減温させる段階は、100℃/minから1000℃/minの速度で減温させる第1減温段階および40℃/minから400℃/minの速度で減温させる第2減温段階を含み、
前記第1減温段階の後に第2減温段階が行われ、
前記第1減温段階の減温速度が前記第2減温段階の減温速度よりも速い、請求項13に記載のポリアミドイミドフィルムの製造方法。 - 前記ポリアミドイミドフィルムがXRDグラフにおいて2θ=8°〜32°である区間をベースラインとしたとき、2θ=15°付近のピーク面積を基準に2θ=23°付近のピーク面積が50%以上である、請求項13に記載のポリアミドイミドフィルムの製造方法。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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KR20170017550 | 2017-02-08 | ||
KR10-2017-0017550 | 2017-02-08 | ||
KR1020170122035A KR101890898B1 (ko) | 2017-02-08 | 2017-09-21 | 폴리아마이드-이미드 필름 및 이의 제조방법 |
KR10-2017-0122035 | 2017-09-21 | ||
PCT/KR2018/001567 WO2018147617A1 (ko) | 2017-02-08 | 2018-02-06 | 폴리아마이드-이미드 필름 및 이의 제조방법 |
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KR102507142B1 (ko) * | 2020-09-29 | 2023-03-07 | 에스케이마이크로웍스 주식회사 | 폴리아마이드계 필름, 이의 제조방법, 및 이를 포함하는 커버 윈도우 및 디스플레이 장치 |
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