JP7421867B2 - 導電積層体の製造方法 - Google Patents
導電積層体の製造方法 Download PDFInfo
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- JP7421867B2 JP7421867B2 JP2019057628A JP2019057628A JP7421867B2 JP 7421867 B2 JP7421867 B2 JP 7421867B2 JP 2019057628 A JP2019057628 A JP 2019057628A JP 2019057628 A JP2019057628 A JP 2019057628A JP 7421867 B2 JP7421867 B2 JP 7421867B2
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Landscapes
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Description
したがって、上記の方法が適用できない場合においても、硬化樹脂層上に導電層を形成した導電積層体を得る方法が求められていた。
樹脂フィルムは、例えば、ポリエステルフィルム、ポリカーボネートフィルム、ポリイミドフィルム、トリアセチルセルロースフィルム、ポリオレフィンフィルム、ポリアクリレートフィルム、ポリスチレンフィルム、ポリ塩化ビニルフィルム、ポリビニルアルコールフィルム、ナイロンフィルム等が挙げられる。特に、各種の用途へ展開するために、耐熱性や機械特性により優れることが好ましく、ポリエステルフィルム、ポリカーボネートフィルム、ポリイミドフィルムが好適に用いられ、さらに透明性や成形性、汎用性を考慮するとポリエステルフィルムがより好適に用いられる。
ポリエステルフィルムは、無延伸フィルム(シート)であっても延伸フィルムであってもよい。中でも、一軸方向又は二軸方向に延伸された延伸フィルムであるのが好ましい。その中でも、力学特性のバランスや平面性に優れる点で、二軸延伸フィルムであるのが好ましい。
ホモポリエステルからなる場合、芳香族ジカルボン酸と脂肪族グリコールとを重縮合させて得られるものが好ましい。芳香族ジカルボン酸としては、テレフタル酸、2,6-ナフタレンジカルボン酸などが挙げられ、脂肪族グリコールとしては、エチレングリコール、ジエチレングリコール、1,4-シクロヘキサンジメタノール等が挙げられる。代表的なポリエステルとしては、ポリエチレンテレフタレート等が例示される。
一方、共重合ポリエステルのジカルボン酸成分としては、イソフタル酸、フタル酸、テレフタル酸、2,6-ナフタレンジカルボン酸、アジピン酸、セバシン酸、オキシカルボン酸等の一種または二種以上が挙げられ、グリコール成分として、エチレングリコール、ジエチレングリコール、プロピレングリコール、ブタンジオール、4-シクロヘキサンジメタノール、ネオペンチルグリコール等の一種または二種以上が挙げられる。
また、チタン化合物を重合触媒としたポリエステルを用いる場合、溶融押出する工程での劣化抑制の目的で、チタン化合物の活性を下げるためにリン化合物を使用することが好ましい。リン化合物としては、ポリエステルの生産性や熱安定性を考慮すると正リン酸が好ましい。リン元素含有量は、溶融押出するポリエステル量に対して、好ましくは1~300ppm、より好ましくは3~200ppm、さらに好ましくは5~100ppmの範囲である。リン化合物の含有量が多すぎる場合は、ゲル化や異物の原因となる可能性があり、また、含有量が少なすぎる場合は、チタン化合物の活性を十分に下げることができず、黄色味のあるフィルムとなる場合がある。
これら一連の粒子は、必要に応じて2種類以上を併用してもよい。
例えば、二軸延伸ポリエステルフィルムを製造する場合、まずポリエステル原料を、押出機を用いてダイから溶融押し出しし、溶融シートを冷却ロールで冷却固化して未延伸シートを得る。この場合、シートの平面性を向上させるためシートと回転冷却ドラムとの密着性を高めることが好ましく、静電印加密着法や液体塗布密着法が好ましく採用される。次に得られた未延伸シートを一方向にロールまたはテンター方式の延伸機により延伸する。延伸温度は、好ましくは70~120℃、より好ましくは80~110℃であり、延伸倍率は好ましくは2.5~7倍、より好ましくは3.0~6倍である。次いで、一段目の延伸方向と直交する方向に、好ましくは70~170℃で、延伸倍率は好ましくは2.5~7倍、より好ましくは3.0~6倍で延伸する。引き続き180~270℃の温度で緊張下または30%以内の弛緩下で熱処理を行い、二軸配向フィルムを得る方法が挙げられる。上記の延伸においては、一方向の延伸を2段階以上で行う方法を採用することもできる。その場合、最終的に二方向の延伸倍率がそれぞれ上記範囲となるように行うのが好ましい。
それゆえ、導電層をコーティングにより設けた後に施される熱処理が他の方法では達成されない高温とすることができるために、導電層の造膜性が向上し、強固な導電層を形成することができる。特に架橋剤を反応させるには非常に有効である。
導電性能又は帯電防止性能を有する有機高分子化合物として、例えば、導電性有機高分子、4級アンモニウム塩化合物、ポリエーテル化合物、スルホン酸化合物類、ベタイン化合物等が挙げられる。
それら中でも特に高い導電性を示し、湿度依存性が少なく、かつ様々な用途展開が期待できるという点において、導電性有機高分子であることが好ましい。
かかるウレタン樹脂は、塗布後の乾燥工程において中和剤が外れたカルボキシル基を、他の架橋剤による架橋反応点として用いることが出来る。これにより、コーティング前の液の状態での安定性に優れる上、得られる導電層の耐久性、耐溶剤性、耐水性、耐ブロッキング性等をさらに改善することが可能となる。
ポリグリセリンとはグリセリンが2以上重合した化合物であり、重合度は2~20の範囲が好ましい。グリセリンを用いた場合、透明性が若干劣る場合がある。
本発明における基材フィルムを構成するフィルムにはあらかじめ、コロナ処理、プラズマ処理等の表面処理を施してもよい。
本発明において、硬化樹脂層とは、導電層上に硬化性化合物を塗布し、硬化させて形成される層のことであり、導電層との密着性に優れ、基材フィルムから導電層と共に剥離が可能な層である。
硬化樹脂層としては、湿気硬化(水分硬化)樹脂層、熱硬化樹脂層、活性エネルギー線硬化樹脂層が挙げられるが、生産性の観点から、活性エネルギー線硬化樹脂層が好ましい。
また、硬化樹脂層としては、例えば、ハードコート層、プリズム層、マイクロレンズ層、光拡散層、インキ層等、各種の機能を付与するために硬化性組成物を硬化させて形成された層が挙げられる。
これら硬化樹脂層の中でも、本発明においては、硬化樹脂層を導電層と共に剥離しやすい(硬化樹脂層への導電層の転写がしやすい)という観点において、ハードコート層であることが好ましい。
本発明において、ハードコート層とは、導電層上に形成することで積層フィルムのハードコート層側表面の耐摩耗性、表面硬度が向上する(硬度が高くなる)層をいう。
また、硬化樹脂層は表面平滑な層に限られず、表面に凹凸を有する硬化樹脂層であってもよい。本発明によれば、表面に凹凸を有する硬化樹脂層であっても簡便に導電層を形成することができる。
被着体は特に限定されず、フィルム、シート、板状、および各種形状のものがその用途に応じて使用でき、その材質も樹脂、紙、金属、無機物等に限定されない。
導電積層体が、例えば、各種ディスプレイやタッチパネル等の光学用途に用いられる場合には、被着体は、透明性を有する樹脂材料からなる樹脂フィルムが好ましい。
透明性を有する樹脂材料からなる樹脂フィルムとしては、基材フィルムとして上述した各種フィルムが挙げられ、中でもポリエステルフィルム、ポリカーボネートフィルム、ポリイミドフィルムが好適に用いられる。
導電積層体の構成は、具体的には、導電層/硬化樹脂層、導電層/硬化樹脂層/粘着層、導電層/硬化樹脂層/接着層、導電層/硬化樹脂層/被着体、導電層/硬化樹脂層/粘着層/被着体、導電層/硬化樹脂層/接着層/被着体が挙げられるが、特にこれらに限定されず、例えば、粘着層又は接着層と被着体との間に易接着層(プライマー層)が設けられていてもよいし、導電層上に他の層を設けてもよい。
他の層としては、保護層、ハードコート層、粘着層等が挙げられる。
ポリエステルに非相溶な成分を除去したポリエステル1gを精秤し、フェノール/テトラクロロエタン=50/50(重量比)の混合溶媒100mlを加えて溶解させ、30℃で測定した。
株式会社島津製作所製、遠心沈降式粒度分布測定装置 SA-CP3型を使用して測定した等価球形分布における積算(重量基準)50%の値を平均粒径とした。
導電層の表面をRuO4で染色し、エポキシ樹脂中に包埋した。その後、超薄切片法により作成した切片をRuO4で染色し、導電層断面を透過型電子顕微鏡(株式会社日立ハイテクノロジーズ製 H-7650、加速電圧100kV)を用いて測定した。
株式会社三菱ケミカルアナリテック製、低抵抗率計:ロレスタGP MCP-T600に四探針型ESPプローブ(探針間隔:5mm、探針先形状:直径2mmの円筒、探針押し圧:240g/本、RCF値は4.235一定とした)を使用し、23℃、50%RHの測定雰囲気でサンプルを30分間調湿後、中央付近の表面抵抗率を測定した。
9Vマンガン乾電池と橙色高輝度LED電球と短路保護に510Ωの抵抗を直列に入れ、基材フィルムから硬化樹脂層と共に剥離した導電層上に30mm以上離してプラスとマイナスの指針を置いたときに電球が点灯する場合をA、点灯しない場合をBとした。
<ポリエステル(A)>
重合触媒として酢酸マグネシウム・四水和物およびテトラブチルチタネートを用いて得られる、極限粘度が0.63dl/gのポリエチレンテレフタレートホモポリマー。
重合触媒として酢酸マグネシウム・四水和物、正リン酸および二酸化ゲルマニウムを用いて得られる、極限粘度が0.64dl/gのポリエチレンテレフタレートホモポリマー。
平均粒子径2μmのシリカ粒子を0.3重量%含有する、ポリエチレンテレフタレートホモポリマー。
(化合物例)
・導電性材料:(I)
ポリ(3,4-エチレンジオキシチオフェン)をポリスチレンスルホン酸と複合させた導電性有機高分子化合物。
下記組成で共重合したポリエステル樹脂の水分散体。
モノマー組成:(酸成分)2,6-ナフタレンジカルボン酸/5-ソジウムスルホイソフタル酸//(ジオール成分)エチレングリコール/ジエチレングリコール=92/8//80/20(mol%)
・イソシアネート系化合物:(IIIB)
ヘキサメチレンジイソシアネート1000部を60℃で攪拌し、触媒としてテトラメチルアンモニウム・カプリエート0.1部を加えた。4時間後、リン酸0.2部を添加して反応を停止させ、イソシアヌレート型ポリイソシアネート組成物を得た。得られたイソシアヌレート型ポリイソシアネート組成物100部、数平均分子量400のメトキシポリエチレングリコール42.3部、プロピレングリコールモノメチルエーテルアセテート29.5部を仕込み、80℃で7時間保持した。その後反応液温度を60℃に保持し、イソブタノイル酢酸メチル35.8部、マロン酸ジエチル32.2部、ナトリウムメトキシドの28%メタノール溶液0.88部を添加し、4時間保持した。n-ブタノール58.9部を添加し、反応液温度80℃で2時間保持し、その後、2-エチルヘキシルアシッドホスフェート0.86部を添加して得られる活性メチレンによるブロックポリイソシアネート。
ポリエステル(A)、(B)、(C)をそれぞれ91質量%、3質量%、6質量%の割合で混合した原料を最外層(表層)の原料とし、ポリエステル(A)、(B)をそれぞれ97質量%、3質量%の割合で混合した原料を中間層の原料として、2台の押出機に各々を供給し、各々285℃で溶融した後、40℃に設定した冷却ロール上に、2種3層(表層/中間層/表層=1:8:1の吐出量)の層構成で共押出し冷却固化させて未延伸シートを得た。
次いで、ロール周速差を利用してフィルム温度85℃で縦方向に3.5倍延伸した後、この縦延伸フィルムの片面に、下記表1に示す塗布液1を塗布し、テンターに導き、95℃で15秒間乾燥させた後、横方向に120℃で4.0倍延伸し、230℃で15秒間熱処理を行った後、横方向に2%弛緩し、膜厚(乾燥後)が0.3μmの導電層を有する厚さ50μmのポリエステルフィルムを得た。
表1に示す塗布液組成に変更する以外は実施例1と同様にして製造し、導電積層体を得た。下記表2に示すとおり、導電層の導電性能は良好であった。
導電層を形成しない以外は実施例1と同様にしてポリエステルフィルムを作成した。当該ポリエステルフィルム上に、上述の導電性材料(I)を10質量部、ジメチルスルフィドを0.5質量部、側鎖にポリエチレンオキサイドを有するアセチレン構造を有する界面活性剤を0.3質量部混合した塗布液4を乾燥後の膜厚が0.2μmになるように塗布し、100℃で1分間乾燥させ、表面抵抗値が300Ωの導電層を得た。その後、実施例1と同様にして導電積層体を得た。
導電積層体の導電層には割れが見られたが表面抵抗値が400Ωと導電性能は良好であり、電気特性もAと良好であった。
Claims (16)
- 基材フィルムの片面に導電層および硬化樹脂層をこの順に形成し、当該硬化樹脂層を導電層と共に基材フィルムから剥離することにより、硬化樹脂層上に導電層を形成することを特徴とする導電積層体の製造方法において、
前記導電層は、導電性有機材料及びナフタレン構造を有するポリエステル樹脂を含有し、
前記導電層が架橋剤を用いて形成され、
前記架橋剤として、メラミン化合物及びイソシアネート系化合物を含有する、導電積層体の製造方法。 - 前記導電層を基材フィルム表面に直接形成する請求項1に記載の導電積層体の製造方法。
- 前記導電性有機材料は、ポリ(3,4-エチレンジオキシチオフェン)をポリスチレンスルホン酸と複合させた導電性有機高分子である請求項1または2に記載の導電積層体の製造方法。
- 前記ナフタレン構造を有するポリエステル樹脂は、2,6-ナフタレンジカルボン酸構造を有するポリエステル樹脂である請求項1~3のいずれか一項に記載の導電積層体の製造方法。
- 前記ナフタレン構造を有するポリエステル樹脂は、ポリエステル樹脂中のジカルボン酸成分100モル%に対してナフタレンジカルボン酸を10モル%以上含むものである請求項1~4のいずれか一項に記載の導電積層体の製造方法。
- 前記導電層中にポリオール化合物を含有する請求項1~5のいずれか一項に記載の導電積層体の製造方法。
- 前記ポリオール化合物として、糖アルコールを含有する請求項6に記載の導電積層体の製造方法。
- 前記硬化樹脂層は、ジペンタエリスリトールヘキサ(メタ)アクリレートを含有する請求項1~7のいずれか一項に記載の導電積層体の製造方法。
- 前記基材フィルムがポリエステルフィルムである請求項1~8のいずれか一項に記載の導電積層体の製造方法。
- 前記導電層の膜厚を0.001~10μmの範囲とする請求項1~9のいずれか一項に記載の導電積層体の製造方法。
- 前記導電層および硬化樹脂層のうち、前記硬化樹脂層のみが活性エネルギー線により硬化させて形成される請求項1~10のいずれか一項に記載の導電積層体の製造方法。
- 前記基材フィルムの片面に前記導電層を設けた後、前記硬化樹脂層を形成する迄の間に、当該導電層を前記基材フィルムと共に少なくとも一方向に延伸する請求項1~11のいずれか一項に記載の導電積層体の製造方法。
- 前記導電層を形成するための塗布液を基材フィルムの片面に塗布した後、前記硬化樹脂層を形成する迄の間に、前記基材フィルム及び前記塗布液に対して180~270℃の熱処理を行うことにより前記導電層を形成する請求項1~12のいずれか一項に記載の導電積層体の製造方法。
- 粘着層を前記硬化樹脂層上に積層した後、当該粘着層および硬化樹脂層を導電層と共に基材フィルムから剥離する請求項1~13のいずれか一項に記載の導電積層体の製造方法。
- 前記基材フィルムの片面に前記導電層を形成し、前記硬化樹脂層を形成する前の段階での、前記導電層の表面抵抗値が1×1012Ω以下である請求項1~14のいずれか一項に記載の導電積層体の製造方法。
- 前記導電積層体における前記導電層の表面抵抗値が1×1012Ω以下である請求項1~15のいずれか一項に記載の導電積層体の製造方法。
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JP2017200995A (ja) | 2016-04-28 | 2017-11-09 | 昭和電工株式会社 | 導電膜の製造方法 |
JP2017212057A (ja) | 2016-05-24 | 2017-11-30 | 大日本印刷株式会社 | 導電性基材、導電膜転写フィルム、及び表示装置 |
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JP2017200995A (ja) | 2016-04-28 | 2017-11-09 | 昭和電工株式会社 | 導電膜の製造方法 |
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