JP2020128547A - 樹脂フィルム、積層体、フレキシブルデバイスの前面板、光学部材、ガスバリア材及びタッチセンサー基材 - Google Patents
樹脂フィルム、積層体、フレキシブルデバイスの前面板、光学部材、ガスバリア材及びタッチセンサー基材 Download PDFInfo
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- polyimide
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Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
Description
図1は、樹脂フィルムの一実施形態を示す断面図である。図1に示す樹脂フィルム10は、ポリイミド系高分子を含有し、対向する一対の主面10a及び10bを有する。
本明細書において、「系化合物」とは、当該「系化合物」が付される化合物の誘導体を指す。例えば、「ベンゾフェノン系化合物」とは、母体骨格としてのベンゾフェノンと、ベンゾフェノンに結合している置換基とを有する化合物を指す。
樹脂フィルム10の主面10a及び/又は10bには、後述する機能層との密着性を向上するために、プラズマ処理又はコロナ放電処理のような表面処理が施されていてもよい。
図3は、積層体の一実施形態を示す断面図である。図3に示す積層体30は、樹脂フィルム10と樹脂フィルム10の一方の主面10aに積層された機能層20とを有する積層体である。
樹脂フィルム10の主面10aに、紫外線吸収剤と、紫外線吸収剤が分散される樹脂などの主材とを含む分散液を塗布して塗膜を形成し、その塗膜を乾燥及び硬化させることにより紫外線吸収層を形成する。次いで、その紫外線吸収層に、ハードコート層を形成する樹脂を含む溶液を塗布して塗膜を形成し、その塗膜を乾燥及び硬化させることによりハードコート層を形成してもよい。この方法により、表面に高硬度を発現する機能を有する層と紫外線吸収の機能を有する層とを含む多層の機能層が形成される。
樹脂フィルム10の主面10aに、紫外線吸収剤と、紫外線吸収剤が分散される樹脂などの主材と、ハードコート層を形成する樹脂とを含む分散液を塗布して塗膜を形成し、その塗膜を乾燥及び硬化させて、表面に高硬度を発現する機能及び紫外線吸収の機能を有する単層を形成し、さらに、その単層上に、ハードコート層を形成する樹脂を含む溶液を塗布して塗膜を形成し、その塗膜を乾燥及び硬化させることにより、ハードコート層を形成してもよい。この方法により、表面に高硬度を発現する機能及び紫外線吸収の機能を有する層と表面に高硬度を発現する機能を有する層とを含む多層の機能層が形成される。
図5は、表示装置の一実施形態を示す断面図である。図5に示す表示装置100は、有機EL装置50と、タッチセンサー70と、前面板90とを有する。これらは通常、筐体に収容されている。有機EL装置50とタッチセンサー70との間、及びタッチセンサー70と前面板90との間は、たとえば不図示の光学接着剤(Optical Clear Adhesive、OCA)で接着されている。
窒素置換した重合槽に、式(1)で表される化合物、式(2)で表される化合物、式(3)で表される化合物、触媒及び溶媒(γブチロラクトン及びジメチルアセトアミド)を仕込んだ。仕込み量は、式(1)で表される化合物75.0g、式(2)で表される化合物36.5g、式(3)で表される化合物76.4g、触媒1.5g、γブチロラクトン438.4g、ジメチルアセトアミド313.1gとした。式(2)で表される化合物と式(3)で表される化合物とのモル比は3:7、式(2)で表される化合物及び式(3)で表される化合物の合計と式(1)で表される化合物とのモル比は、1.00:1.02であった。
ポリイミドを、300℃のガラス転移温度を有するポリイミド(三菱ガス化学社製「ネオプリム」、式(PI)の繰り返し構造単位を含むポリイミド系高分子)に変更し、樹脂フィルムを形成するための混合溶液におけるシリカ粒子とポリイミドの質量比を30:70に変更したこと以外は実施例1と同様にして、厚み80μmの樹脂フィルムを得た。得られた樹脂フィルムの黄色度(YI値)は、1.8であった。
ポリイミドを河村産業(株)製「KPI−MX300F(100)、式(PI)の繰り返し構造単位を含むポリイミド系高分子」に変更し、樹脂フィルムを形成するための混合溶液におけるシリカ粒子とポリイミドの質量比を20:80に変更したこと以外は実施例1と同様にして、厚み75μmの樹脂フィルムを得た。得られた樹脂フィルムの黄色度(YI値)は、2.2であった。
300℃のガラス転移温度を有するポリイミド(三菱ガス化学社製「ネオプリム」、式(PI)の繰り返し構造単位を含むポリイミド系高分子)を用い、このポリイミドのみを溶解したγ−ブチロラクトン溶液をガラス基板に塗布した。その他は実施例1と同様にして、80μmの樹脂フィルムを得た。得られた樹脂フィルムの黄色度(YI値)は、1.8であった。
ポリイミドを、390℃のガラス転移温度を有するポリイミド(三菱ガス化学社製「ネオプリム」、式(PI)の繰り返し構造単位を含むポリイミド系高分子)に変更したこと以外は比較例1と同様にして、厚み80μmの樹脂フィルムを得た。得られた樹脂フィルムの黄色度(YI値)は、1.4であった。
樹脂フィルムを形成するための混合溶液に、アミノ基を有するアルコキシシランを加えなかったこと以外は、実施例1と同様にして、厚み80μmの樹脂フィルムを得た。得られた樹脂フィルムの黄色度(YI値)は、2.5であった。
ポリイミドを、300℃のガラス転移温度を有するポリイミド(三菱ガス化学社製「ネオプリム」、式(PI)の繰り返し構造単位を含むポリイミド系高分子)に変更し、樹脂フィルムを形成するための混合溶液におけるシリカ粒子とポリイミドの質量比を40:60に変更し、アミノ基を有するアルコキシシランを混合溶液に加えなかったこと以外は、実施例1と同様にして、厚み80μmの樹脂フィルムを得た。得られた樹脂フィルムの黄色度(YI値)は、2.2であった。
1)弾性率
弾性率の測定装置として、島津製作所製、オートグラフAG−ISを用いた。幅10mm、長さ100mmの短冊状の樹脂フィルムを試験片として準備した。チャック間距離50mm、速度20mm/分の条件で引張試験を行い、樹脂フィルムの引張弾性率を測定した。
測定装置として、TA Instruments製、DSC Q200を用いた。試料量:5mg、温度域:室温〜400℃、昇温速度:10℃/分の条件で、樹脂フィルムの示差操作熱量測定(DSC)を行った。得られたDSC曲線から、ガラス転移温度を求めた。
樹脂フィルムの黄色度(Yellow Index:YI値)を、日本分光社製の紫外可視近赤外分光光度計V−670によって測定した。サンプルがない状態でバックグランド測定を行った後、樹脂フィルムをサンプルホルダーにセットして、300nm〜800nmの光に対する透過率測定を行い、3刺激値(X、Y、Z)を求めた。YI値を、下記の式に基づいて算出した。
YI=100×(1.2769X−1.0592Z)/Y
図6は、屈曲試験の方法を示す概略図である。試験装置として、ユアサシステム機器株式会社製 卓上型耐久試験機「DLDMLH−FS」を使用した。図6の屈曲試験は、面状体無負荷U字伸縮試験とも称される。図6の(a)に示すように、平面形状の1枚の短冊状の樹脂フィルム10(幅10mm×長さ100mm)の両末端を、それぞれ、対向配置された1対のプレート1a及び1bの間、及び、対向配置されたもう1対のプレート2a及び2bの間に挟んだ状態で固定した。プレート1a及びプレート2aを、樹脂フィルム10の同じ面側に配置させた。次いで、図6の(b)に示されるように、プレート1a及び2aを内側にして、これらプレートが向き合うように樹脂フィルムをU字型に折り曲げた。このとき、折り曲げられて向き合う樹脂フィルム10間の距離2Rを3mmに設定した。その後、折り曲げられた樹脂フィルム10を、再び図6の(a)の状態に戻した。これを1サイクルとして、1サイクル/1.2秒の周期で樹脂フィルム10を繰り返し折り曲げた(屈曲した)。屈曲回数(サイクル数)が100000回になるまで試験を継続した。試験終了前に積層体が破断した場合、その時点の屈曲回数を記録した。
ガラス基材上に固定された樹脂フィルムの鉛筆硬度を、JIS K5600−5−4に準拠して測定した。鉛筆硬度の測定における荷重は1kgとした。
樹脂フィルムの一方の主面上に、ハードコート剤(UVHC7800G(商品名)、Momentive社製)を用いて、80℃で3分の加熱、及び500mJ/cm2の照射エネルギーの露光を含む硬化条件で、厚さ5〜6μmのハードコート層を形成させ、樹脂フィルム及びハードコート層(機能層)からなる積層体を作製した。
ガラス基材上に、アクリル系粘着剤を用いて厚さ25μmで弾性率約1MPaの粘着層を形成させた。この粘着層に、上記積層体を、樹脂フィルムが粘着層側になる向きで貼り付けた。この状態で、ハードコート層表面の鉛筆硬度を、JIS K5600−5−4に準拠して測定した。鉛筆硬度の測定における荷重は1kgfとした。
比較例2の樹脂フィルムは、4.0GPa未満であり、30000回未満の屈曲回数で破断した。比較例3の樹脂フィルムは、4.0GPa以上の弾性率を有するものの、1000回未満の屈曲回数で破断した。比較例4の樹脂フィルムは、4.0GPa以上の弾性率を有するものの、20000回未満の屈曲回数で破断した。ガラス基材/樹脂フィルムの積層体における樹脂フィルム表面の鉛筆硬度は、実施例と比較例1、2、3、4とで差異は認められなかった。しかし、粘着層/樹脂フィルム/ハードコート層の積層体におけるハードコート層表面の鉛筆硬度は、実施例の樹脂フィルムの場合のみ、十分に高い値が示された。この結果から、樹脂フィルムが、4GPa以上の引張弾性率、及び100000回を超える屈曲回数の両方を満たすことで、粘着層/樹脂フィルム/ハードコート層の積層体におけるハードコート層表面に十分な硬度を付与できることが確認された。
Claims (11)
- ポリイミド系高分子を含有する樹脂フィルムであって、
樹脂フィルムの引張弾性率が4.0GPa以上であり、
当該樹脂フィルムを向かい合う当該樹脂フィルム間の距離が3mmになるまでU字型に折り曲げて戻すことを繰り返す屈曲試験において、当該樹脂フィルムが破断するまで当該樹脂フィルムを折り曲げる回数が100000回を超え、かつ、黄色度が5以下である、樹脂フィルム。 - 樹脂フィルムの厚みが30〜100μmである請求項1に記載の樹脂フィルム。
- 請求項1又は2に記載の樹脂フィルムと、該樹脂フィルムの少なくとも一方の面側に設けられた機能層と、を備える積層体。
- 樹脂フィルムと機能層との間に設けられたプライマー層を更に備える請求項3に記載の積層体。
- 機能層が、樹脂フィルムの両方の面側に設けられており、
一方の面側の機能層が表面に高硬度を発現する層で、他方の面側の機能層が粘着性の機能を有する層である請求項3又は4に記載の積層体。 - 請求項1又は2に記載の樹脂フィルムを備える光学部材。
- 請求項1又は2に記載の樹脂フィルムを備えるガスバリア材。
- 請求項1又は2に記載の樹脂フィルムを備えるタッチセンサー基材。
- 請求項3〜5のいずれか一項に記載の積層体を備える光学部材。
- 請求項3〜5のいずれか一項に記載の積層体を備えるガスバリア材。
- 請求項3〜5のいずれか一項に記載の積層体を備えるタッチセンサー基材。
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US10399310B2 (en) | 2019-09-03 |
CN107849271A (zh) | 2018-03-27 |
JP6715432B2 (ja) | 2020-07-01 |
KR20170108993A (ko) | 2017-09-27 |
CN107849271B (zh) | 2021-04-23 |
WO2017014287A1 (ja) | 2017-01-26 |
US20180370207A1 (en) | 2018-12-27 |
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