JP6097985B2 - 積層体、積層体の製造方法、素子用基板の製造方法、及び、素子の製造方法 - Google Patents
積層体、積層体の製造方法、素子用基板の製造方法、及び、素子の製造方法 Download PDFInfo
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- JP6097985B2 JP6097985B2 JP2015523038A JP2015523038A JP6097985B2 JP 6097985 B2 JP6097985 B2 JP 6097985B2 JP 2015523038 A JP2015523038 A JP 2015523038A JP 2015523038 A JP2015523038 A JP 2015523038A JP 6097985 B2 JP6097985 B2 JP 6097985B2
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Description
LsDianhydride,i=Exp[−k3×Coeffi]×Vi y0
LsDiamine,j=Exp[−k4×Coeffj]×Vj y0
K0=2.00、
y0=−1.00、
K1=206.67、
K2=124.78、
K3=3.20、
K4=5.90、
CoeffiとCoeffjは、それぞれポリイミドのモノマーである二無水物iとジアミンjの構造から計算された分子の非球面係数(molecular asphericity)であり、
ViとVjは、それぞれモノマーである二無水物iとジアミンjの構造から計算されたマックグロウン体積(Mcgrown Volume)であり、
前記分子の非球面係数及びマックグロウン体積は、アドリアナ・コード(ADRIANA.Code)のプログラム(Molecular Networks GmbH社)を用いて計算されるものであり、
αFITは、exp(−4.0×|Coeffi−Coeffj|)+0.08<0.90であれば1.0であり、exp(−4.0×|Coeffi−Coeffj|)+0.08≧0.90であれば0.1〜0.95の定数である。
R11〜R14は、各々独立に、炭素数1〜4のアルキル基または炭素数1〜4のハロアルキル基であり、また、aは0〜3の整数、bは0〜2の整数、c及びeは、各々独立に、0〜3の整数、dは0〜4の整数、またfは0〜3の整数である。
また、前記芳香族ジアミン化合物は、下記化学式4aまたは4bの芳香族ジアミン化合物であり得る。
R21〜R23は、各々独立に、炭素数1〜10のアルキル基または炭素数1〜10のハロアルキル基であり、
Xは、各々独立に、−O−、−CR24R25−、−C(=O)−、−C(=O)O−、−C(=O)NH−、−S−、−SO−、−SO2−、−O[CH2CH2O]q−、炭素数6〜18の一環または多環のシクロアルキレン基、炭素数6〜18の一環または多環のアリーレン基、及びこれらの組み合わせからなる群より選択され、このとき、前記R24〜R25は、各々独立に、水素原子、炭素数1〜10のアルキル基、及び炭素数1〜10のハロアルキル基からなる群より選択され、qは1または2の整数であり、l、m、及びnは、各々独立に、0〜4の整数であり、また、pは0または1の整数である。
LsDianhydride,i=Exp[−k3×Coeffi]×Vi y0
LsDiamine,j=Exp[−k4×Coeffj]×Vj y0
K0=2.00、
y0=−1.00、
K1=206.67、
K2=124.78、
K3=3.20、
K4=5.90、
CoeffiとCoeffjは、それぞれポリイミドのモノマーである二無水物iとジアミンjの構造から計算された分子の非球面係数(molecular asphericity)であり、
ViとVjは、それぞれモノマーである二無水物iとジアミンjの構造から計算されたマックグロウン体積(Mcgrown Volume)であり、
前記分子の非球面係数及びマックグロウン体積は、アドリアナ・コード(ADRIANA.Code)のプログラム(Molecular Networks GmbH社)を用いて計算されるものであり、
αFITは、exp(−4.0×|Coeffi−Coeffj|)+0.08<0.90であれば1.0であり、exp(−4.0×|Coeffi−Coeffj|)+0.08≧0.90であれば0.1〜0.95の定数である。
前記数学式において、定数αFITは、exp(−4.0×|Coeffi−Coeffj|)+0.08≧0.90であれば0.1〜0.95の範囲の任意の定数であり得るが、好ましくは0.2〜0.5、最も好ましくは0.33であり得る。
前記アドリアナ・コード(ADRIANA.Code)のプログラムは、ドイツMolecular Networks GmbH社で開発したプログラムであって、分子が有し得る固有の物理的、化学的、電気的特性の計算のために主に使用されるが、分子の構造的情報を入力すると、分子の非球面係数及びマックグロウン体積を計算することができる。
R11〜R14は、各々独立に、炭素数1〜4のアルキル基(例えば、メチル基、エチル基、プロピル基等)または炭素数1〜4のハロアルキル基(例えば、フルオロメチル基、ブロモメチル基、クロロメチル基、トリフルオロメチル基など)であり、また、
aは0〜3の整数、bは0〜2の整数、c及びeは、各々独立に、0〜3の整数、dは0〜4の整数、またfは0〜3の整数であってもよく、前記b、c、d及びeは0の整数であることが好ましい。
R21〜R23は、各々独立に、炭素数1〜10のアルキル基(例えば、メチル基、エチル基、プロピル基など)または炭素数1〜10のハロアルキル基(例えば、フルオロメチル基、ブロモメチル基、クロロメチル基、トリフルオロメチル基など)であり、
Xは、各々独立に、−O−、−CR24R25−、−C(=O)−、−C(=O)O−、−C(=O)NH−、−S−、−SO−、−SO2−、−O[CH2CH2O]q−、炭素数6〜18の一環式または多環式のシクロアルキレン基(例えば、シクロへキシレン基、ノルボルネン基など)、炭素数6〜18の一環式または多環式のアリーレン基(例えば、フェニレン基、ナフタレン基など)、及びこれらの組み合わせからなる群より選択され、このとき、前記R24〜R25は、各々独立に、水素原子、炭素数1〜10のアルキル基(例えば、メチル基、エチル基、プロピル基など)、及び炭素数1〜10のハロアルキル基(例えば、フルオロメチル基、ブロモメチル基、クロロメチル基、トリフルオロメチル基など)からなる群より選択され、qは1または2の整数であり、
l、m、及びnは、各々独立に、0〜4の整数であり、好ましくは0であり、また、
pは0または1の整数であり、好ましくは0である。
一方、前記接着体において、前記第一ポリイミド系樹脂層20上には第二ポリイミド系樹脂層30が位置する。
以下、本発明が属する技術分野で通常の知識を有する者が容易に実施できるように、本発明の実施例について詳しく説明する。しかし、本発明は、様々な異なる形態で具体化でき、ここで説明する実施例に限定されない。
キャリア基板として無アルカリガラスの一面に、BPDA1モルとPDA0.99モルとを重合させて製造したポリアミック酸系樹脂3重量%と、溶媒としてDMAc97重量%を含む第一ポリイミド系樹脂層形成用組成物を乾燥後、厚みが0.1μmとなるように塗布した。結果として製造された第一ポリイミド系樹脂層の形成用の塗膜に対して、120℃の温度における乾燥工程及び250℃の温度における硬化工程(30分間)を連続的に実施して、ポリイミド系樹脂(以下「第1ポリイミド系樹脂」という)を含む第一ポリイミド系樹脂層を形成した。
下記表3に提示されているとおり、第一ポリイミド系樹脂及び第2ポリイミド系樹脂の種類を変化させたことを除いては、前記実施例1と同じ方法で実施して、積層体を製造した。
前記試験積層体において、第一ポリイミド系樹脂層に対して密度(density)、熱膨張係数(CTE)、ガラス転移温度(Tg)、接着力及び剥離強度(Peel strength)をそれぞれ測定した。
試験積層体1−1に対して、第一ポリイミド系樹脂層の形成時の硬化温度を下記表5に示したように多様に変化させて硬化工程を実施することを除いては、上記実施例1と同じ方法で実施して、積層体を製造した。
下記表7に示したとおり、第一及び第二ポリイミド系樹脂層の種類、硬化温度及び第一ポリイミド系樹脂層厚みを多様に変更させることを除いては、上記実施例1と同じ方法で実施して、試験積層体を製造した。
下記表9に示したとおり、第一ポリイミド系樹脂層における硬化温度及び硬化時間を多様に変更させることを除いては、上記実施例1と同じ方法で実施して、試験積層体を製造した。
下記表11に示したとおり、第一及び第二ポリイミド系樹脂層の種類及び硬化条件を多様に変更させることを除いては、前記実施例1と同じ方法で実施して、試験積層体を製造した。
本発明における第一及び第二ポリイミド系樹脂として使用可能なポリイミド系樹脂の物性を評価した。
ディボンディング層の第1ポリイミド系樹脂として、PMDA−PDA、可撓性基板の第2ポリイミド系樹脂としてBPDA−PDAを用いて、実施例1と同じ方法で試験積層体を製造するが、硬化温度を変化させた。接着力及び剥離強度を測定した結果を表15に示した。
ディボンディング層を形成する酸二無水物をBPDAとPMDAとを共に用いて、実施例1と同じ方法で積層体を製造するが、BPDAとPMDAとのモル比を変化させた。可撓性基板を形成する第2のポリイミドは、酸二無水物として、シクロヘキサンテトラカルボン酸二無水物(BPDA_H)を、ジアミン系化合物として、4−アミノ−N−(4−アミノフェニル)ベンズアミド(DABA)と、4,4'−ジアミノジフェニルエーテル(ODA)を9:1のモル比で用いて製造した。接着力及び剥離強度を測定した結果を表17に示した。
ディボンディング層は、試験例8と同じ方法で製造し、可撓性基板を形成するポリイミドは、酸二無水物としてシクロヘキサンテトラカルボン酸二無水物(BPDA−H)を、ジアミン系化合物として4−アミノ−N−(4−アミノフェニル)ベンズアミド(DABA)と、メタ−フェニレンジアミン(mPDA)を9:1のモル比で用いて製造した積層体(9−1)と、酸二無水物として、4,4'−(ヘキサフルオロイソプロピリデン)ジフタル酸二無水物(6FDA)と、ピロメリット酸二無水物(PMDA)を1:1のモル比としてパラフェニレンジアミン(PDA)と反応させて製造した積層体(9−2)を準備した。接着力及び剥離強度の評価結果を表18に示した。
下記表19に提示した組成で積層体を製造して接着力及び剥離強度を評価した。PMDAの含有量が高くなるほど低い剥離強度を示すことを確認した。
20 第一ポリイミド系樹脂層
30 第二ポリイミド系樹脂層
40 素子構造
100 積層体
Claims (22)
- キャリア基板と、
前記キャリア基板の一面または両面に位置する、第一ポリイミド系樹脂層と、
前記第一ポリイミド系樹脂層上に位置し、フレキシブルディスプレイ素子の可撓性基板として用いられる第二ポリイミド系樹脂層と、
を含む積層体であって、
前記キャリア基板は、0.1〜50mmの厚みを有し、
前記第一ポリイミド系樹脂層は、0.05〜5μmの厚みを有し、
前記第一ポリイミド系樹脂層の100〜200℃温度区間での熱膨張係数(CTE)は、前記第二ポリイミド系樹脂層の同一温度区間での熱膨張係数(CTE)と同一または低く、
切断によって前記積層体の積層断面が新たに露出することにより、前記第二ポリイミド系樹脂層に対する第一ポリイミド系樹脂層の接着力が減少することで前記第一ポリイミド系樹脂層を剥離する、
切断剥離用積層体。 - 前記第一ポリイミド系樹脂層と第二ポリイミド系樹脂層の100〜200℃温度区間での熱膨張係数(CTE)はその差が60ppm/℃以下である、
請求項1に記載の切断剥離用積層体。 - 前記第一ポリイミド系樹脂層は、
前記切断によって前記積層体の積層断面が新たに露出する前は、前記第二ポリイミド系樹脂層に対し1N/cm以上の接着力を示し、
前記切断によって前記積層体の積層断面が新たに露出した後は、前記第二ポリイミド系樹脂層に対し0.3N/cm以下の剥離強度(peel strength)を示す、
請求項1又は請求項2に記載の切断剥離用積層体。 - 前記第一ポリイミド系樹脂層は、下記数学式1により計算される類似度値が0.5以下である第一ポリイミド系樹脂を含む、
請求項1から請求項3までの何れか一項に記載の切断剥離用積層体:
LsDianhydride,i=Exp[−k3×Coeffi]×Vi y0
LsDiamine,j=Exp[−k4×Coeffj]×Vj y0
K0=2.00、
y0=−1.00、
K1=206.67、
K2=124.78、
K3=3.20、
K4=5.90、
CoeffiとCoeffjは、それぞれポリイミドのモノマーである二無水物iとジアミンjの構造から計算された分子の非球面係数(molecular asphericity)であり、
ViとVjは、それぞれモノマーである二無水物iとジアミンjの構造から計算されたマックグロウン体積(Mcgrown Volume)であり、
前記分子の非球面係数及びマックグロウン体積は、アドリアナ・コード(ADRIANA.Code)のプログラム(Molecular Networks GmbH社)を用いて計算されるものであり、
αFITは、exp(−4.0×|Coeffi−Coeffj|)+0.08<0.90であれば1.0であり、exp(−4.0×|Coeffi−Coeffj|)+0.08≧0.90であれば0.1〜0.95の定数である。 - 前記第一ポリイミド系樹脂は、ポリアミック酸系樹脂を含む組成物を塗布し、500℃以上の温度でイミド化を行った後、IRスペクトルの1350〜1400cm−1または1550〜1650cm−1で現れるCNバンドの積分強度100%に対して、200℃以上の温度でイミド化を行った後のCNバンドの相対的積分強度の比率をイミド化率としたとき、60%〜99%のイミド化率を有する、
請求項1から請求項4までの何れか一項に記載の切断剥離用積層体。 - 前記第一ポリイミド系樹脂が、200℃以上のガラス転移温度を有する、
請求項1から請求項5までの何れか一項に記載の切断剥離用積層体。 - 前記第一ポリイミド系樹脂層が、100〜200℃の条件で30ppm/℃以下の熱膨張係数及び450℃以上の1%熱分解温度(Td1%)を有する、
請求項1から請求項6までの何れか一項に記載の切断剥離用積層体。 - 前記第二ポリイミド系樹脂層が、イミド化率が50〜99%であり、ガラス転移温度が200℃以上の第二ポリイミド系樹を含む、
請求項1から請求項7までの何れか一項に記載の切断剥離用積層体。 - キャリア基板の一面または両面に、第一ポリイミド系樹脂を含む第一ポリイミド系樹脂層を形成する段階と、
前記第一ポリイミド系樹脂層上に第二ポリイミド系樹脂の前駆体を含む組成物を塗布した後、硬化させて、フレキシブルディスプレイ素子の可撓性基板として用いられる第二ポリイミド系樹脂層を形成する段階と、
を含み、
前記キャリア基板は、0.1〜50mmの厚みを有し、
前記第一ポリイミド系樹脂層は、0.05〜5μmの厚みを有し、
前記第一ポリイミド系樹脂層の100〜200℃温度区間での熱膨張係数(CTE)は、前記第二ポリイミド系樹脂層の同一温度区間での熱膨張係数(CTE)と同一または低く、
切断によって積層体の積層断面が新たに露出することにより、前記第二ポリイミド系樹脂層に対する前記第一ポリイミド系樹脂層の接着力が減少することで前記第一ポリイミド系樹脂層を剥離する、切断剥離用積層体の製造方法。 - 前記第一ポリイミド系樹脂層を形成する段階は、前記キャリア基板の一面または両面に前記第一ポリイミド系樹脂またはその前駆体を含む組成物を塗布した後、硬化させて、前記第一ポリイミド系樹脂を形成する段階を含む、
請求項9に記載の切断剥離用積層体の製造方法。 - 前記第一ポリイミド系樹脂層の形成時の硬化工程は、200℃以上の温度で実施され、
前記第二ポリイミド系樹脂層の形成時の硬化工程は、前記第一ポリイミド系樹脂層の形成時の硬化温度と同一な温度または0〜200℃高い温度で実施される、
請求項10に記載の切断剥離用積層体の製造方法。 - 前記第一または第二ポリイミド系樹脂層の形成段階後、300℃以上の温度で1分〜30分間熱処理する段階をさらに含む、
請求項10又は請求項11に記載の切断剥離用積層体の製造方法。 - 前記第一ポリイミド系樹脂層を形成する段階は、下記化学式1の芳香族テトラカルボン酸二無水物と直線状の構造を有する芳香族ジアミン化合物とを反応させて製造したポリアミック酸を200℃以上の温度で硬化させて、前記第一ポリイミド系樹脂を形成する段階を含む、
請求項9に記載の切断剥離用積層体の製造方法:
R11〜R14は、各々独立に、炭素数1〜4のアルキル基または炭素数1〜4のハロアルキル基であり、また、
aは0〜3の整数、bは0〜2の整数、c及びeは、各々独立に、0〜3の整数、dは0〜4の整数、またfは0〜3の整数である。 - 前記芳香族ジアミン化合物は、下記化学式4aまたは4bの芳香族ジアミン化合物である、
請求項13に記載の切断剥離用積層体の製造方法:
R21〜R23は、各々独立に、炭素数1〜10のアルキル基または炭素数1〜10のハロアルキル基であり、
Xは、各々独立に、−O−、−CR24R25−、−C(=O)−、−C(=O)O−、−C(=O)NH−、−S−、−SO−、−SO2−、−O[CH2CH2O]q−、炭素数6〜18の一環または多環のシクロアルキレン基、炭素数6〜18の一環または多環のアリーレン基、及びこれらの組み合わせからなる群より選択され、このとき、前記R24〜R25は、各々独立に、水素原子、炭素数1〜10のアルキル基、及び炭素数1〜10のハロアルキル基からなる群より選択され、qは1または2の整数であり、
l、m、及びnは、各々独立に、0〜4の整数であり、また、
pは、0または1の整数である。 - キャリア基板の一面または両面に、第一ポリイミド系樹脂を含む第一ポリイミド系樹脂層を形成する段階と、
前記第一ポリイミド系樹脂層上に第二ポリイミド系樹脂またはその前駆体を含む組成物を塗布した後、硬化させて、フレキシブルディスプレイ素子の可撓性基板として用いられる第二ポリイミド系樹脂層が形成された積層体を製造する段階と、
前記積層体を切断した後、前記第二ポリイミド系樹脂層を、前記第一ポリイミド系樹脂層が形成された前記キャリア基板から分離する段階と、
を含み、
前記キャリア基板は、0.1〜50mmの厚みを有し、
前記第一ポリイミド系樹脂層は、0.05〜5μmの厚みを有し、
前記第一ポリイミド系樹脂層の100〜200℃温度区間での熱膨張係数(CTE)は、前記第二ポリイミド系樹脂層の同一温度区間での熱膨張係数(CTE)と同一または低く、
前記積層体は、前記切断によって前記積層体の積層断面が新たに露出することにより、前記第二ポリイミド系樹脂層に対する前記第一ポリイミド系樹脂層の接着力が減少することで前記第一ポリイミド系樹脂層を剥離する切断剥離用積層体である、
素子用基板の製造方法。 - 前記第一ポリイミド系樹脂層を形成する段階は、前記第一ポリイミド系樹脂またはその前駆体を含む組成物を前記キャリア基板上に塗布した後、200℃以上の前記第二ポリイミド系樹脂層の硬化温度並みの温度または当該硬化温度よりも0〜200℃低い温度で硬化させて、前記第一ポリイミド系樹脂を形成する段階を含む、
請求項15に記載の素子用基板の製造方法。 - 前記第一ポリイミド系樹脂層を形成する段階は、下記化学式1の芳香族テトラカルボン酸二無水物と直線状の構造を有する芳香族ジアミン化合物とを反応させて製造したポリアミック酸を200℃以上の温度で硬化させて、前記第一ポリイミド系樹脂を形成する段階を含む、
請求項15又は請求項16に記載の素子用基板の製造方法:
R11〜R14は、各々独立に、炭素数1〜4のアルキル基または炭素数1〜4のハロアルキル基であり、また、
aは0〜3の整数、bは0〜2の整数、c及びeは、各々独立に、0〜3の整数、dは0〜4の整数、またfは0〜3の整数である。 - 前記芳香族ジアミン化合物は、下記化学式4aまたは4bの芳香族ジアミン化合物である、
請求項17に記載の素子用基板の製造方法:
R21〜R23は、各々独立に、炭素数1〜10のアルキル基または炭素数1〜10のハロアルキル基であり、
Xは、各々独立に、−O−、−CR24R25−、−C(=O)−、−C(=O)O−、−C(=O)NH−、−S−、−SO−、−SO2−、−O[CH2CH2O]q−、炭素数6〜18の一環または多環のシクロアルキレン基、炭素数6〜18の一環または多環のアリーレン基、及びこれらの組み合わせからなる群より選択され、このとき、前記R24〜R25は、各々独立に、水素原子、炭素数1〜10のアルキル基、及び炭素数1〜10のハロアルキル基からなる群より選択され、qは1または2の整数であり、
l、m、及びnは、各々独立に、0〜4の整数であり、また、
pは、0または1の整数である。 - キャリア基板の一面または両面に、第一ポリイミド系樹脂を含む第一ポリイミド系樹脂層を形成する段階と、
前記第一ポリイミド系樹脂層上に第二ポリイミド系樹脂またはその前駆体を含む組成物を塗布した後、硬化させて、フレキシブルディスプレイ素子の可撓性基板として用いられる第二ポリイミド系樹脂層が形成された積層体を製造する段階と、
前記積層体の前記第二ポリイミド系樹脂層上に素子構造を形成する段階と、
前記素子構造が形成された積層体を切断した後、前記素子構造が形成された前記第二ポリイミド系樹脂層を、前記積層体のディボンディング層から分離する段階と、
を含み、
前記キャリア基板は、0.1〜50mmの厚みを有し、
前記第一ポリイミド系樹脂層は、0.05〜5μmの厚みを有し、
前記ディボンディング層は、前記キャリア基板及び前記第一ポリイミド系樹脂層を含み、
前記第一ポリイミド系樹脂層の100〜200℃温度区間での熱膨張係数(CTE)が、前記第二ポリイミド系樹脂層の同一温度区間での熱膨張係数(CTE)と同一または低く、
前記積層体は、前記切断によって前記積層体の積層断面が新たに露出することにより、前記第二ポリイミド系樹脂層に対する前記第一ポリイミド系樹脂層の接着力が減少することで前記第一ポリイミド系樹脂層を剥離する切断剥離用積層体である、
素子の製造方法。 - 前記第一ポリイミド系樹脂層を形成する段階は、前記第一ポリイミド系樹脂またはその前駆体を含む組成物を前記キャリア基板上に塗布した後、200℃以上の前記第二ポリイミド系樹脂層の硬化温度並みの温度または当該硬化温度よりも0〜200℃低い温度で硬化させて、前記第一ポリイミド系樹脂を形成する段階を含む、
請求項19に記載の素子の製造方法。 - 前記第一ポリイミド系樹脂層を形成する段階は、下記化学式1の芳香族テトラカルボン酸二無水物と直線状の構造を有する芳香族ジアミン化合物とを反応させて製造したポリアミック酸を200℃以上の温度で硬化させて、前記第一ポリイミド系樹脂を形成する段階を含む、
請求項19又は請求項20に記載の素子の製造方法:
R11〜R14は、各々独立に、炭素数1〜4のアルキル基または炭素数1〜4のハロアルキル基であり、また、
aは0〜3の整数、bは0〜2の整数、c及びeは、各々独立に、0〜3の整数、dは0〜4の整数、またfは0〜3の整数である。 - 前記芳香族ジアミン化合物は、下記化学式4aまたは4bの芳香族ジアミン化合物である、
請求項21に記載の素子の製造方法:
R21〜R23は、各々独立に、炭素数1〜10のアルキル基または炭素数1〜10のハロアルキル基であり、
Xは、各々独立に、−O−、−CR24R25−、−C(=O)−、−C(=O)O−、−C(=O)NH−、−S−、−SO−、−SO2−、−O[CH2CH2O]q−、炭素数6〜18の一環または多環のシクロアルキレン基、炭素数6〜18の一環または多環のアリーレン基、及びこれらの組み合わせからなる群より選択され、このとき、前記R24〜R25は、各々独立に、水素原子、炭素数1〜10のアルキル基、及び炭素数1〜10のハロアルキル基からなる群より選択され、qは1または2の整数であり、
l、m、及びnは、各々独立に、0〜4の整数であり、また、
pは、0または1の整数である。
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KR1020140041571A KR101802558B1 (ko) | 2013-04-09 | 2014-04-07 | 디스플레이 소자의 제조방법 및 이를 이용하여 제조된 디스플레이 소자 |
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