JP2015072365A - フレキシブルカラーフィルター、その製造方法ならびにそれを用いたフレキシブル発光デバイス - Google Patents
フレキシブルカラーフィルター、その製造方法ならびにそれを用いたフレキシブル発光デバイス Download PDFInfo
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- JP2015072365A JP2015072365A JP2013207952A JP2013207952A JP2015072365A JP 2015072365 A JP2015072365 A JP 2015072365A JP 2013207952 A JP2013207952 A JP 2013207952A JP 2013207952 A JP2013207952 A JP 2013207952A JP 2015072365 A JP2015072365 A JP 2015072365A
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- gas barrier
- acid
- barrier layer
- flexible
- color filter
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Abstract
【解決手段】ポリイミド樹脂膜と、前記ポリイミド樹脂膜上のガスバリア層と、前記ガスバリア層上のブラックマトリックスおよび着色画素とを有するフレキシブルカラーフィルターであって、前記ガスバリア層が2層以上の積層体であり、その最上層が酸化ケイ素からなることを特徴とする、フレキシブルカラーフィルター。
【選択図】図1
Description
ポリイミド樹脂膜は、ポリアミック酸等のポリイミド前駆体樹脂の溶液を基板上に塗布した後、乾燥し、加熱することにより作製することができる。ポリアミック酸は、酸無水物とジアミンを反応させることで合成することができる。また、ポリイミド樹脂膜は、溶剤に溶解するポリイミド樹脂を合成してから、そのポリイミド樹脂溶液を基板上に塗布することでも作製することができる。
ポリイミド樹脂膜上のガスバリア層は水蒸気や酸素等の透過を防ぐ役割を果たすものである。特に有機エレクトロルミネッセンス素子(有機EL素子)では、水分による素子の劣化が著しいので、基板にガスバリア性を付与することが必要である。
ブラックマトリックスは、黒色顔料を樹脂に分散した樹脂ブラックマトリックスであることが好ましい。黒色顔料の例としては、カーボンブラック、チタンブラック、酸化チタン、酸化窒化チタン、窒化チタン又は四酸化鉄が挙げられる。特に、カーボンブラック、チタンブラックが好適である。また赤顔料、緑顔料、青顔料を混合して黒色顔料として用いることもできる。
酸無水物、ジアミンおよび溶剤の例としては、前述のポリイミド樹脂で挙げたものを用いることができる。
ブラックマトリックスを形成した後に、着色画素を形成する。着色画素は、赤、緑、青の3色の着色画素からなる。また3色の着色画素に加えて、無色透明または、ごく薄く薄着した第4色の画素を形成することで、表示装置の白色表示の明るさを向上させることもできる。
次に、本発明のCFの製造方法の一例を説明する(図1参照)。透明基板1上にポリイミド樹脂膜2および下層のガスバリア層3、上層のガスバリア層4を上記の方法で作成する。その上に、カーボンブラックまたはチタンブラックからなる黒色顔料を分散したポリアミック酸からなるブラックマトリックス用ペーストをスピンコーター又はダイコーター等の方法でキュア後の膜厚が1μmになるように塗布し、60Pa以下まで減圧乾燥した後に、110〜140℃の熱風オーブン又はホットプレートでセミキュアを行う。
ポリイミド樹脂の透過率は、顕微分光光度計(例えば、MCPD−2000;大塚電子(株)製)を用いて波長380nmから720nmまでの透過率を測定した。測定波長全領域で透過率が80%以上の場合に、透明性は良であると判断した。
CFの色度は顕微分光光度計を用いて各着色画素の透過率スペクトルを測定後、(Y)および色度(x、y)がCIE1931規格に基づいて算出した。
ガスバリア性能は、温度40℃、湿度90%RH、測定面積50cm2の条件で、英国、テクノロックス(Technolox)社製の水蒸気透過率透過率測定装置(機種名:“DELTAPERM”(登録商標))を使用して測定した。サンプル数は水準当たり2検体とし、測定回数は同一サンプルについて各10回とし、その平均値を水蒸気透過率(g/(m2・24h)としてガスバリア性評価の指標とした。
ガラス板から剥離したフレキシブルカラーフィルター8を100mm×140mmにサンプリングし、カラーフィルターを形成した面上の中央部に直径30mmの金属円柱9を固定し、この円柱に沿って、円柱の抱き角0°(サンプルが平面の状態)の状態に置き(図2参照)、円柱への抱き角が180°(円柱で折り返した状態)となる範囲(図3参照)で、100回折り曲げ動作を行った。耐屈曲性は、曲げ動作前後の水蒸気透過率を指標とし、曲げ動作後の水蒸気透過率が曲げ動作前の値に対して2倍以下の場合に良好と判定した。
ガスバリア層の組成は、X線電子分光法(XPS)により組成を測定した。
ガスバリア層の膜厚は、透過型電子顕微鏡により断面膜を観察することにより、膜厚を測定した。
乾燥窒素気流下、200mL4つ口フラスコに3,3’,4,4’−ビフェニルテトラカルボン酸二無水物15.8137g(53.7mmol)、trans−1,4−ジアミノシクロへキサン6.1375g(53.7mmol)、N−メチル−2−ピロリドン100gを入れて65℃で加熱撹拌した。6時間後、冷却してワニスとした。
4,4’−ジアミノフェニルエーテル(0.30モル当量)、パラフェニレンジアミン(0.65モル当量)およびビス(3−アミノプロピル)テトラメチルジシロキサン(0.05モル当量)を、850gのγ−ブチロラクトンおよび850gのN−メチル−2−ピロリドンと共に仕込み、3,3’,4,4’−オキシジフタルカルボン酸二無水物(0.9975モル当量)を添加し、80℃で3時間反応させた。無水マレイン酸(0.02モル当量)を添加し、更に80℃で1時間反応させ、ポリアミック酸樹脂(樹脂の濃度20質量%)溶液を得た。
調製例2のポリアミック酸樹脂溶液(B)250gに、50gのカーボンブラック(MA100;三菱化学(株)製)および200gのN−メチル−2−ピロリドンを混合し、ダイノーミルKDL−Aを用いて、直径0.3mmのジルコニアビーズを使用して、3200rpmで3時間の分散処理を行い、遮光剤分散液1を得た。
調製例2のポリアミック酸樹脂溶液(B)250gに、100gのチタンブラック(窒化チタン試薬、和光純薬工業(株)製、窒化チタン粒子径50nm)および200gのN−メチル−2−ピロリドンを混合しホモミキサー(特殊機化製)で1時間撹拌し、予備分散液1を得た。その後、直径0.40mmのジルコニアビーズを使用して4時間の分散処理を行い、遮光剤分散液2を得た。
着色剤として、50gのPR177(クロモファイン(登録商標)レッド6125EC;大日精化製)および50gのPR254(イルガフォア(登録商標)レッドBK−CF;チバ・スペシャルティケミカルズ(株)製)を混合した。この着色剤中に、100gの高分子分散剤(BYK2000;樹脂濃度40質量%;ビックミージャパン(株)製)、67gのアルカリ可溶性樹脂(サイクロマー(登録商標)ACA250;樹脂濃度45質量%;ダイセル化学製)、83gのプロピレングリコールモノメチルエーテルおよび650gのプロピレングリコールモノメチルエーテルアセテートを混合して、スラリーを作製した。スラリーを入れたビーカーを循環式ビーズミル分散機(ダイノーミルKDL−A;ウイリー・エ・バッコーフェン社製)とチューブでつなぎ、メディアとして直径0.3mmのジルコニアビーズを使用して、3200rpm、4時間の分散処理を行い、着色剤分散液を得た。
着色剤として、65gのPG7(ホスタパーム(登録商標)グリーンGNX;クラリアントジャパン社製)および35gのPY150(E4GNGT;ランクセス(株)製)を混合した。この着色剤に、100gのBYK2000、67gのサイクロマーACA250、83gのプロピレングリコールモノメチルエーテルおよび650gのプロピレングリコールモノメチルエーテルアセテートを混合し、ダイノーミルKDL−Aを用いて、直径0.3mmのジルコニアビーズを使用して、3200rpm、6時間の分散処理を行い、着色剤分散液を得た。
着色剤として、100gのPB15:6(リオノール(登録商標)ブルー7602;東洋インキ社製)を使用し、この着色剤中に100gのBYK2000、67gのサイクロマーACA250、83gのプロピレングリコールモノメチルエーテルおよび650gのプロピレングリコールモノメチルエーテルアセテートを混合して、スラリーを作製した。スラリーを分散機ダイノーミルKDL−Aを用いて、直径0.3mmのジルコニアビーズを使用して、3200rpm、3時間の分散処理を行い、着色剤分散液を得た。
65.05gのトリメリット酸に、280gのガンマブチロラクトンおよび74.95gのγ−アミノプロピルトリエトキシシランを添加し、120℃で2時間加熱した。得られた溶液20gに、7gのビスフェノキシエタノールフルオレンジグリシジルエーテルおよび15gのジエチレングリコールジメチルエーテルを添加し、樹脂組成物を得た。
300×350mmの無アルカリガラス基板上(AN100;旭硝子(株)製)に、調製例1で得られたポリアミック酸樹脂溶液(A)をスリットコーターにより塗布し、チャンバー内壁温度60℃にした減圧乾燥機にて、40Paまで減圧して溶媒を乾燥させた。その後熱風オーブン中140℃で20分加熱処理した。さらに酸素濃度3%の熱風オーブン中300℃で30分加熱処理して、ポリイミド樹脂膜を得た。
下層のガスバリア層を形成する際に酸化亜鉛と二酸化ケイ素と酸化アルミの比率が50/47/3の混合焼結ターゲットを用いたこと以外は実施例1同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて実施例1と同様の評価を行った。結果を表1に示す。
下層のガスバリア層を形成する際に酸化亜鉛と二酸化ケイ素と酸化アルミの比率が80/17/3の混合焼結ターゲットを用いたこと以外は実施例1同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて実施例1と同様の評価を行った。結果を表1に示す。
実施例1と同様にポリイミド樹脂を形成した。その後、酸化亜鉛と二酸化ケイ素と酸化アルミの比率が62/35/3の混合焼結ターゲットを用いて、10%酸素を含むアルゴン雰囲気下でスパッタリングを行い、膜厚150nmのガスバリア層(下層)を得た。このときの圧力は3×10−1Pa、基板温度は150℃で3kWの直流電源を用いてスパッタリングを行った。その後、真空を維持したまま、酸化ケイ素からなるターゲットを用いて、5%酸素を含むアルゴン雰囲気下でスパッタリングを行い、膜厚50nmの酸化ケイ素膜からなるガスバリア層(上層)を得た。このときの圧力は2×10−1Pa、基板温度は150℃で13.56MHzの交流電源を用いてスパッタリングを行い、2層の積層構成のガスバリア層を形成したこと以外は、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて実施例1と同様の評価を行った。結果を表1に示す。
実施例1と同様にポリイミド樹脂を形成した。その後、酸化錫と二酸化ケイ素と酸化アルミの比率が62/35/3の混合焼結ターゲットを用いて、10%酸素を含むアルゴン雰囲気下でスパッタリングを行い、膜厚150nmのガスバリア層(下層)を得た。このときの圧力は3×10−1Pa、基板温度は150℃で3kWの直流電源を用いてスパッタリングを行った。その後、真空を維持したまま、酸化ケイ素からなるターゲットを用いて、アルゴン雰囲気下でスパッタリングを行い、膜厚50nmの酸化ケイ素膜からなるガスバリア層(上層)を得た。このときの圧力は2×10−1Pa、基板温度は150℃で13.56MHzの交流電源を用いてスパッタリングを行い、2層の積層構成のガスバリア層を形成したこと以外は、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて実施例1と同様の評価を行った。結果を表1に示す。
実施例1と同様にポリイミド樹脂を形成した。その後、酸化インジウムと二酸化ケイ素と酸化アルミの比率が62/35/3の混合焼結ターゲットを用いて、10%酸素を含むアルゴン雰囲気下でスパッタリングを行い、膜厚150nmのガスバリア層(下層)を得た。このときの圧力は3×10−1Pa、基板温度は150℃で3kWの直流電源を用いてスパッタリングを行った。その後、真空を維持したまま、酸化ケイ素からなるターゲットを用いて、アルゴン雰囲気下でスパッタリングを行い、膜厚50nmの酸化ケイ素膜からなるガスバリア層(上層)を得た。このときの圧力は2×10-1Pa、基板温度は150℃で13.56MHzの交流電源を用いてスパッタリングを行い、2層の積層構成のガスバリア層を形成したこと以外は、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて実施例1と同様の評価を行った。結果を表1に示す。
実施例1と同様にポリイミド樹脂およびガスバリア層を形成した。その後、調製例4で作製した、黒色遮光剤組成物を用いてブラックマトリックスを形成したこと以外は、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて実施例1と同様の評価を行った。結果を表1に示す。
ガスバリア層を形成しなかったこと以外は、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて上述の方法で各ガスバリア層の組成分析、透明性評価およびガスバリア性評価を行った。結果を表1に示す。ガスバリア性が悪かったため耐屈曲性評価は行わなかった。
実施例1と同様にポリイミド樹脂を形成した。その後、酸化亜鉛と二酸化ケイ素と酸化アルミの比率が62/35/3の混合焼結ターゲットを用いて、10%酸素を含むアルゴン雰囲気下でスパッタリングを行い、膜厚150nmのガスバリア層を得た。このときの圧力は3×10−1Pa、基板温度は150度で3kWの直流電源を用いてスパッタリングを行った。その後、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて上述の方法で各ガスバリア層の組成分析、透明性評価およびガスバリア性評価を行った。結果を表1に示す。ガスバリア性が悪かったため耐屈曲性評価は行わなかった。
実施例1と同様にポリイミド樹脂を形成した。その後、酸化ケイ素からなるターゲットを用いて、アルゴン雰囲気下でスパッタリングを行い、膜厚50nmの酸化ケイ素膜を得た。このときの圧力は2×10−1Pa、基板温度は150℃で13.56MHzの交流電源を用いてスパッタリングを行い酸化ケイ素膜を形成したこと以外は、実施例1と同様にしてフレキシブルCFを作製した。得られたフレキシブルCFについて上述の方法で各ガスバリア層の組成分析、透明性評価およびガスバリア性評価を行った。結果を表1に示す。ガスバリア性が悪かったため耐屈曲性評価は行わなかった。
2 ポリイミド樹脂膜
3 下層のガスバリア層
4 上層のガスバリア層
5 ブラックマトリックス
6R 赤の着色画素
6G 緑の着色画素
6B 青の着色画素
7 平坦化膜
8 フレキシブルカラーフィルター
9 金属円柱
Claims (8)
- ポリイミド樹脂膜と、前記ポリイミド樹脂膜上のガスバリア層と、前記ガスバリア層上のブラックマトリックスおよび着色画素とを有するフレキシブルカラーフィルターであって、前記ガスバリア層が2層以上の積層体であり、その最上層が酸化ケイ素からなることを特徴とする、フレキシブルカラーフィルター。
- 前記ガスバリア層の最上層以外の少なくとも1層が亜鉛、錫およびインジウムからなる群より選ばれる一種以上の酸化物、窒化物または酸窒化物を含む請求項1記載のフレキシブルカラーフィルター。
- 前記ブラックマトリックスが、ポリイミド樹脂に黒色顔料を分散した樹脂ブラックマトリックスである請求項1または2のいずれかに記載のフレキシブルカラーフィルター。
- 前記黒色顔料がカーボンブラックである請求項3記載のフレキシブルカラーフィルター。
- 前記黒色顔料がチタンブラックである請求項3記載のフレキシブルカラーフィルター。
- 枚葉基板上にポリイミド前駆体樹脂溶液またはポリイミド樹脂溶液を塗布した後に減圧乾燥する工程を含む請求項1から5のいずれかに記載のフレキシブルカラーフィルターの製造方法
- 請求項1から5のいずれかに記載のフレキシブルカラーフィルターに発光素子を貼り合わせたフレキシブル発光デバイス。
- 前記発光素子が有機EL素子である請求項7記載のフレキシブル発光デバイス。
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