JP6177235B2 - 積層体の製造プロセスおよびそのプロセスで得られる積層体 - Google Patents
積層体の製造プロセスおよびそのプロセスで得られる積層体 Download PDFInfo
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- JP6177235B2 JP6177235B2 JP2014517520A JP2014517520A JP6177235B2 JP 6177235 B2 JP6177235 B2 JP 6177235B2 JP 2014517520 A JP2014517520 A JP 2014517520A JP 2014517520 A JP2014517520 A JP 2014517520A JP 6177235 B2 JP6177235 B2 JP 6177235B2
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Description
i)基板(3)および基板(3)に塗布され、導電性ポリマーP1を含む導電層を含む積層体S1(2)の提供;
ii)導電層の少なくとも1つの被覆領域Ddおよび少なくとも1つの非被覆領域Duを得るための、導電層の、ポリマーP2を含む、被覆相由来の被覆層Dでの部分的な被覆;
iii)少なくとも1つの被覆領域における導電層の電気伝導率と比較して、少なくとも1つの非被覆領域Duのうちの少なくとも一部における導電層の電気伝導率の削減;
iv)アルカリ水溶液処理による被覆層Dの少なくとも部分的な除去。
R7およびR8は、それぞれ互いに独立に、H、任意に置換されたC1〜C18のアルキルラジカルまたは任意に置換されたC1〜C18のアルコキシラジカルを表し、R7およびR8は共に、1以上のC原子がOまたはSから選ばれる1以上の同一のまたは異なるヘテロ原子で置換されうるC1〜C8のアルキレンラジカル、好ましくはC1〜C8のジオキシアルキレンラジカル、任意に置換されたC1〜C8のオキシチアアルキレンラジカルまたは任意に置換されたC1〜C8のジチアアルキレンラジカルを表し、または任意に少なくとも1つのC原子がOまたはSから選択されるヘテロ原子により置換されている任意に置換されたC1〜C8のアルキリデンラジカルを表す。
ia)基板の提供;
ib)基板の表面の少なくとも一部への導電性ポリマーP1および溶媒を含む組成物Z2の塗布;
ic)導電層を得るための上記溶媒の少なくとも部分的な除去
のプロセス段階を含むプロセスにより得られうる。
iia)ポリマーP2を含む被覆相の導電層の一部への塗布;
iib)被覆層Dを得るための溶媒の少なくとも部分的な除去。
iiia)少なくとも1つの非被覆領域Buのうちの少なくとも一部を、塩素、臭素またはヨウ素を放出しうる有機化合物を含む組成物Z1と接触させる工程。
Halは、塩素、臭素またはヨウ素からなる群から選択されるハロゲンであり、好ましくは塩素または臭素を表し、
Yは、N、SおよびPから選択され、好ましくはNであり、
X1およびX2は、同一または異なり、それぞれ、ハロゲン(好ましくは塩素または臭素)、炭素原子または硫黄原子であり、1以上のさらなる原子が任意にX1およびX2に結合されうる。X1およびX2に結合されているさらなる元素の数は、X1およびX2の共役原子価によって決まる。
iiib)組成物Z1に接触させられている導電層の洗浄
ここで、洗浄工程は、溶媒中、例えば水中に積層体を浸すことにより行われ、続いて乾燥されうる。
v)pH7未満、好ましくはpH1〜6、好ましくはpH1〜5、好ましくはpH1〜4を有する酸性溶液との積層体S2の処理。
A)基板の後に続く層が表面抵抗Rを有する少なくとも1つのエリアA;
B)基板の後に続く層がRより10倍、特に好ましくは100倍、さらにより好ましくは1,000倍、さらにより好ましくは10,000倍、最も好ましくは100,000倍大きい表面抵抗を有する少なくとも1つのエリアB;を有し
色分離ΔEエリアA,エリアBは最大4.5、特に好ましくは最大3.0、最も好ましくは最大1.5である。
A)基板の後に続く層が表面抵抗Rを有する少なくとも1つのエリアA;
B)基板の後に続く層がRより10倍、特に好ましくは100倍、さらにより好ましくは1,000倍、さらにより好ましくは10,000倍、最も好ましくは100,000倍大きい表面抵抗を有する少なくとも1つのエリアB;であり、
色分離ΔEエリアA,エリアBは最大4.5、特に好ましくは最大3.0、最も好ましくは最大1.5であるものを含む。
SB/SA≧0.5、特に好ましくは≧0.75、最も好ましくは≧0.90。
特段の記載がない限り、試験方法および実施例は標準条件下で行われる。特段の記載がない限り、%範囲は、wt%範囲である。
表面抵抗の決定のため、2.5cm長さのAg電極を、抵抗測定が各エリアAおよびBにおいて可能であるようにシャドーマスクを介して蒸着する。表面抵抗を電位計(Keithly614)を用いて決定する。その決定は、例えば米国特許第6,943,571(B1)号明細書に記載されている、いわゆる「4点プローブ」測定方法を用いて行った。
被覆したPETフィルムの透過スペクトルの測定手順はASTM308−94aに従っている。このため、Perkin Elmer(パーキンエルマー)製の2チャンネルフォト分光器Lambda900型を用いる。その装置は15cmの光度計球(photometer sphere)を備える。そのフォト分光計の好ましい機能は、製造業者の提言と取扱説明書にしたがっての検出器の波長の校正と線形性の基本的な確認により確かめられる。
積層体を、85℃かつ85%の相対的大気湿度で保存する。明度L、およびbを、前もっておよび後で測定する。
(溶液/形態の調製)
(ポリマーP1)
Clevios(クレビオス)(登録商標)FE−T(Heraeus Clevios GmbH(ヘレウス・クレビオス・ゲーエムベーハー)から入手できるPEDOT/PSS分散剤)を組成物Z2として用いる。
20gのBelland(ベランド)ポリマー88140(Belland AG(ベランドアーゲー)から入手できるアクリル酸ブチル/メタクリル酸/スチレン共重合体)を、室温で(およそ22℃)、ガラスの透明な溶液が得られるまで撹拌しながら、80gの溶媒混合物(体積比1:4のメチルエチルケトン−エタノール)に溶解させた。
25wt%の強度のアンモニア水溶液を、この溶液のpHが10〜12になるまで水で希釈する。
およそ1wt%の強度の水溶液を調整する。
10gのジクロロジイソシアヌル酸ナトリウム二水和物を、室温(およそ22℃)で、撹拌しながら、90gの水に溶解させる。この原液を、ジクロロジイソシアヌル酸ナトリウム二水和物の含有量がそれぞれ10wt%および5wt%となるように、水で希釈した。
Clevios(登録商標)FE−T分散剤から作製された導電性のPEDOT/PSS層を、バーコーターを用いてDuPont Teijin製のポリエステルフィルム(Melinex(メリネックス)505型)に被覆する。乾燥前の膜厚は4〜12μmである。乾燥を130℃で5分間行う。12μmの厚さの乾燥フィルムにおける表面抵抗は、およそ200ohm/sqである。
5wt%のジクロロヂジソシアヌル酸ナトリウム二水和物溶液を用いた以外は、実施例1と同じ手順で行った。
ジクロロジイソシアヌル酸ナトリウム二水和物溶液の代わりに、15wt%の硝酸セリウム水溶液を用いる以外は上記のとおりの同じプロセスを行う。気候試験前および気候試験後のエッチングした領域とエッチングしていない領域のそれぞれのL、aおよびbの値は、本発明に係る積層体と比較して異なる色を示す(表1)。
色の位置をL*a*b*座標系で決定した。「エッチングされていない」は、ジクロロジイソシアヌル酸ナトリウム二水和物溶液または硝酸セリウム溶液で処理されていない特定の領域を意味する(被覆領域Ddに相当する)。「エッチングされている」は、ジクロロジイソシアヌル酸ナトリウム二水和物溶液または硝酸セリウム溶液で処理されている特定の領域を意味する(非被覆領域Duに相当する)。
PEDOT/PSS層の形態にある導電層4を、バーコーターを用いてDuPont Teijin製のポリエステルフィルム(Melinex(メリネックス)505型)からなる基板3にClevios(登録商標)FE−T分散剤を被覆した。乾燥前の膜厚は4〜12μmだった。乾燥を130℃で5分間行った。12μmの厚さの乾燥フィルムにおける表面抵抗は、およそ180ohm/sqだった。
DuPontのポリエステルフィルム(Melinex505型)より架橋度の高い形態で被覆されているPETフィルムAを基板として用いる以外は、実施例3と同じ手順で行った。
Clexios(登録商標)FET(Heraeus Precious Metals GmbH & Co.KG(ドイツ)から購入できる)より架橋度の高い形態で被覆されているPETフィルムAを基板として用いる以外は、実施例3と同じ手順で行った。
Claims (19)
- 以下のプロセス段階を含む、積層体S2(1)の製造プロセス:
i)基板(3)および基板(3)に塗布されかつ導電性ポリマーP1を含む導電層(4)を含む積層体S1(2)の提供;
ii)導電層の少なくとも1つの被覆領域Dd(6)および少なくとも1つの非被覆領域Du(7)を得るための、導電層(4)の部分の、ポリマーP2を含む、被覆相由来の被覆層D(5)での部分的な被覆であって、ここでポリマーP2は、少なくとも1つのモノマーα1および少なくとも1つのコモノマーα3の共重合体であるか、または少なくとも1つのモノマーα1、少なくとも1つのモノマーα2および少なくとも1つのコモノマーα3の共重合体であり、モノマーα1は、カルボン酸基またはそれらの塩を含むモノマーであり、モノマーα2はカルボン酸の直鎖状もしくは分枝状のC 1 〜C 20 のアルコールエステルであり、コモノマーα3は少なくとも1つのエチレン性不飽和基で置換されたアリール基であり、
被覆層D(5)が、以下のプロセス段階を含むプロセスにより得られる:
iia)ポリマーP2と任意に溶媒を含む被覆相の前記導電層(4)の一部へのパターンとしての塗布であって、前記被覆領域Dd(6)及び前記非被覆領域Du(7)はパターンとなる:
iib)任意に、前記被覆層D(5)を得るための前記溶媒の少なくとも部分的な除去;
iii)少なくとも1つの被覆領域Dd(6)における導電層(4)の電気伝導率と比較して、少なくとも1つの非被覆領域Du(7)のうちの少なくとも一部における導電層(4)の電気伝導率の削減であって、少なくとも1つの非被覆領域D u (7)のうちの少なくとも一部を、塩素、臭素またはヨウ素を放出しうる有機化合物を含む組成物Z1と接触させる工程を少なくとも包含する;
iv)アルカリ水溶液処理による被覆層D(5)の少なくとも部分的な除去。 - 前記被覆層が、被覆層に基づき、20wt%未満のフォトラッカーを含む、請求項1に記載の製造プロセス。
- 積層体(1,2)のうちの少なくとも一部が、プロセス段階ii)〜iv)の1以上の前、後または間に加熱される、請求項1または2に記載の製造プロセス。
- プロセス段階iv)において、被覆層D(5)の除去が、被覆層D(5)のうちの少なくとも一部をpH>7の溶液と接触させることで実施され、色分離ΔEエリアA,気候試験前,エリアA,気候試験後およびΔEエリアB,気候試験前,エリアB,気候試験後における差異(|ΔΕエリアA,気候試験前,エリアA,気候試験後−ΔEエリアB,気候試験前,エリアB,気候試験後|)は、最大3.0である、請求項1〜3のいずれか1項に記載の製造プロセス。
- プロセス段階iv)において、被覆層D(5)の除去が、被覆層D(5)のうちの少なくとも一部をpH8〜14である溶液と接触させることで実施される、請求項1〜4のいずれか1項に記載の製造プロセス
- 前記ポリマーP2が、少なくとも1つのモノマーα1、少なくとも1つのモノマーα2および少なくとも1つのコモノマーα3の共重合体である、請求項1〜5のいずれか1項に記載の製造プロセス。
- 前記ポリマーP2が、メタクリル酸、アクリル酸ブチルおよびスチレンの繰り返し単位の共重合体である、請求項1〜6のいずれか1項に記載の製造プロセス。
- 前記被覆相が、ポリマーP2および溶媒を含む溶液または分散剤である、請求項1〜7のいずれか1項に記載の製造プロセス。
- 前記溶媒が水、アルコール、ケトン、エステルまたはこれらの2以上の混合物からなる群から選択される、請求項8に記載の製造プロセス。
- プロセス段階ii)において、被覆層D(5)が印刷プロセスを用いて塗布される、請求項1〜9のいずれか1項に記載の製造プロセス。
- プロセス段階iii)において、少なくとも1つの非被覆領域Du(7)のうちの少なくとも一部における導電層(4)の電気伝導率が、少なくとも1つの被覆領域Dd(6)における導電層(4)の電気伝導率と比較して、少なくとも10倍で減少される、請求項1〜10のいずれか1項に記載の製造プロセス。
- 前記iii)の工程における前記導電層(4)の電気伝導率の減少が、前記導電層(4)を前記組成物Z1中への浸漬によりまたは、前記導電層(4)を前記組成物Z1で印刷することにより行われる、請求項1〜11のいずれか1項に記載の製造プロセス。
- 最大4.5の色分離ΔE前,後が、導電層を組成物Z1と接触させることで生じる、請求項12に記載の製造プロセス。
- 前記導電層を前記組成物Z1と接触させることが、前記組成物Z1に接触させられる領域における前記導電層の厚さが最大50%で減少される条件下で行われる、請求項12または13に記載の製造プロセス。
- 前記導電層が導電性ポリマーに加えてポリアニオンを含む、請求項1〜14のいずれか1項に記載の製造プロセス。
- 前記導電層が、ポリ(3,4−エチレンジオキシチオフェン)とポリスチレンスルホン酸とのコンプレックスを含む、請求項1〜15のいずれか1項に記載の製造プロセス。
- 前記積層体S1(2)が、以下のプロセス段階を含むプロセスにより得られうる、請求項1〜16のいずれか1項に記載の製造プロセス:
ia)基板(3)の提供;
ib)基板(3)の表面の少なくとも一部へ導電性ポリマーP1および溶媒を含む組成物Z2の塗布;
ic)導電層(4)を得るための前記溶媒の少なくとも部分的な除去。 - 前記組成物Z2が、ポリ(3,4−エチレンジオキシチオフェン)およびポリスチレンスルホン酸のコンプレックスを含む溶液または分散剤である、請求項17に記載の製造プロセス。
- さらに、以下のプロセス段階を含む、請求項1〜18のいずれか1項に記載の製造プロセス:
v)pH<7である溶液を用いた前記積層体S2(1)の処理。
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