JP2015525143A - 積層体、積層体の製造方法、素子用基板、素子用基板の製造方法、素子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、素子用基板の製造方法、素子及び素子の製造方法 Download PDFInfo
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Abstract
Description
また、前記ディボンディング層に加えられる物理的刺激は、前記接着体の積層断面を露出させるものであり得る。
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、
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の常数である。
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。
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の一環式または多環式のシクロアルキレン基、炭素数6〜18の一環式または多環式のアリーレン基、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。
また、本明細書における「接着力」は、物理的刺激の印加前の可撓性基板に対するディボンディング層の接着力を意味し、「剥離強度」は、物理的刺激の印加後の可撓性基板に対するディボンディング層の接着力を意味するものであるが、用語「接着力」と「剥離強度」は混用され得る。
本発明者らの実験の結果、ポリイミド系樹脂の製造のための硬化温度の条件、ポリイミド系樹脂のイミド化率、そしてポリイミド系樹脂層の剥離強度は、下記表2のような関係を満たすことができることが確認された。
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、
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の常数である。
前記式において、定数FITは、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。
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。
また、前記ディボンディング層形成用組成物は、通常、ポリイミド系樹脂層に用いられるバインダ、溶媒、架橋剤、開始剤、分散剤、可塑剤、粘度調節剤、紫外線吸収剤、感光性モノマーまたは増感剤等の添加剤をさらに含むこともできる。
また、前記硬化工程時の硬化時間は特に限定されず、一例として3〜30分間実施できる。
前記後続の熱処理工程は、300℃以上の温度で1分〜30分間実施されることが好ましい。また、前記後続の熱処理工程は、1回実施されてもよく、または2回以上多段階で実施されてもよい。具体的には、200〜250℃における第1の熱処理、300〜350℃における第2の熱処理及び400〜450℃における第3の熱処理を含む3段階で実施できる。
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%を含むディボンディング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ディボンディング層用塗膜に対して、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)を含むディボンディング層を形成した。
下記表3に提示されているとおり、ディボンディング層用第1ポリイミド系樹脂及び可撓性基板のポリマー層用第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、ディボンディング層に対して密度(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。
前記結果において、ディボンディング層における前記化学式1のテトラカルボン酸二無水物と直線状構造のジアミン化合物とを用いて製造されたポリイミドを含む試験積層体1−1〜1−4は、分子内の芳香族環が連結基を介して連結されたものであるテトラカルボン酸二無水物を用いて製造されたポリイミドを含む試験積層体1−5に比べて著しく減少した剥離強度を示した。
試験積層体1−1に対して、ディボンディング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、ディボンディング層及び可撓性基板における第2ポリイミド系樹脂の種類及び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、ディボンディング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10に示したとおり、ディボンディング層における第1ポリイミド系樹脂及び可撓性基板における第2ポリイミド系樹脂の種類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。
本発明におけるディボンディング層及び可撓性基板のポリマー層に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16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。
Claims (26)
- 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し、ポリイミド系樹脂を含むディボンディング層と、
前記ディボンディング層上に位置する可撓性基板と、を含み、
前記ディボンディング層の化学的変化を引き起こさない物理的刺激により前記可撓性基板に対する前記ディボンディング層の接着力が変化する積層体。 - 前記ディボンディング層の可撓性基板に対する接着力は、物理的刺激が加えられる前の接着力A1と、物理的刺激が加えられた後の接着力A2との比A2/A1が0.001〜0.5である請求項1に記載の積層体。
- 前記ディボンディング層が、物理的刺激が加えられた後に、前記可撓性基板に対して0.3N/cm以下の剥離強度(peel strength)を有する請求項1または2に記載の積層体。
- 前記ディボンディング層が、物理的刺激が加えられる前に、前記可撓性基板に対して1N/cm以上の接着力を有する請求項1から3の何れか一項に記載の積層体。
- 前記物理的刺激が、前記積層体の積層断面を露出させる請求項1から4の何れか一項に記載の積層体。
- 前記ポリイミド系樹脂は、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、請求項1から5の何れか一項に記載の積層体:
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。 - 前記ポリイミド系樹脂が、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6の何れか一項に記載の積層体。
- 前記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7の何れか一項に記載の積層体。
- 前記ポリイミド系樹脂が、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製造された請求項1から8の何れか一項に記載の積層体:
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9に記載の積層体:
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。 - 前記ディボンディング層が、ポリイミド系樹脂またはその前駆体を含む組成物をキャリア基板上に塗布した後、200℃以上の温度で硬化させることで製造される請求項1から10の何れか一項に記載の積層体。
- 前記ディボンディング層が、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(Tdl%)を有する請求項1から11の何れか一項に記載の積層体。
- 前記ディボンディング層が、0.05〜5μmの厚みを有する請求項1から12の何れか一項に記載の積層体。
- 前記可撓性基板が、薄膜ガラス層、ポリマー層、及びこれらの2層以上の積層体からなる群より選択される構造体である請求項1から13の何れか一項に記載の積層体。
- 前記ポリマー層が、ポリエーテルスルホン、ポリエチレンナフタレート、ポリエチレンテレフタレート、ポリカーボネート、ポリイミド、ポリエーテルイミド、ポリアミドイミド、ポリエステル、ポリエーテルアミドイミド、ポリエステルアミドイミド、及びポリアリレートからなる群より選択される1種以上の高分子樹脂を含む請求項14に記載の積層体。
- 前記ポリマー層が、イミド化率が50〜99%であり、ガラス転移温度が200℃以上のポリイミド系樹脂を含む請求項14または15に記載の積層体。
- 前記キャリア基板の一面または両面にポリイミド系樹脂を含む前記ディボンディング層を形成する段階と、
前記ディボンディング層上に前記可撓性基板を形成する段階と、を含み、
前記ディボンディング層は、ポリイミド系樹脂またはその前駆体を含む組成物をキャリア基板上に塗布した後、200℃以上の温度で硬化させることで製造される請求項1に記載の積層体の製造方法。 - 前記可撓性基板の形成が、ディボンディング層上にガラス薄膜層を位置させたのち、20〜300℃の温度で熱処理する方法、ポリマーまたはその前駆体を含む組成物を塗布した後、硬化させる方法、及びこれらの組み合わせからなる群より選択されるいずれかの方法により実施される請求項17に記載の積層体の製造方法。
- 前記ディボンディング層の形成段階後、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17または18に記載の積層体の製造方法。
- 請求項17から19の何れか一項に記載の積層体の製造方法によって、キャリア基板、ディボンディング層及び可撓性基板を含む積層体を製造する段階と、
前記積層体に前記ディボンディング層の化学的変化を引き起こさない物理的刺激を加える段階と、
前記積層体の可撓性基板を前記キャリア基板上に形成されたディボンディング層から分離する段階と、を含む素子用基板の製造方法。 - 前記物理的刺激が、前記積層体の積層断面を露出させる請求項20に記載の素子用基板の製造方法。
- 請求項20に記載の素子用基板の製造方法によって製造された素子用基板。
- 請求項17から19の何れか一項に記載の積層体の製造方法によって、キャリア基板、ディボンディング層及び可撓性基板を含む積層体を製造する段階と、
前記積層体の可撓性基板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に前記ディボンディング層の化学的変化を引き起こさない物理的刺激を加えた後、前記素子構造が形成された可撓性基板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、
を含む素子の製造方法。 - 請求項23に記載の素子の製造方法によって製造された素子。
- 前記素子が、太陽電池、有機発光ダイオード照明、半導体素子、及びディスプレイ素子からなる群より選択される請求項24に記載の素子。
- 前記ディスプレイ素子が、フレキシブル有機電界発光素子である請求項25に記載の素子。
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