JP2014508371A - 有機エッチング液で処理することによる層構造の製造方法およびそれにより得られる層構造 - Google Patents
有機エッチング液で処理することによる層構造の製造方法およびそれにより得られる層構造 Download PDFInfo
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- JP2014508371A JP2014508371A JP2013537045A JP2013537045A JP2014508371A JP 2014508371 A JP2014508371 A JP 2014508371A JP 2013537045 A JP2013537045 A JP 2013537045A JP 2013537045 A JP2013537045 A JP 2013537045A JP 2014508371 A JP2014508371 A JP 2014508371A
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- DHNRXBZYEKSXIM-UHFFFAOYSA-N chloromethylisothiazolinone Chemical compound CN1SC(Cl)=CC1=O DHNRXBZYEKSXIM-UHFFFAOYSA-N 0.000 description 1
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
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- PFZLGKHSYILJTH-UHFFFAOYSA-N thieno[2,3-c]thiophene Chemical compound S1C=C2SC=CC2=C1 PFZLGKHSYILJTH-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
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Abstract
【選択図】図1
Description
i)基板および、当該基板上にある電気伝導性のポリマーを含む電気伝導性の層を含む層構造を準備する工程、
ii)その電気伝導性の層の表面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することができる有機化合物を含む組成物Z1と接触させる工程。
ia)基板を準備する工程;
ib)当該基板の表面のうちの少なくとも一部に、電気伝導性のポリマーおよび溶媒を含む組成物Z2の塗布する工程;
ic)少なくとも部分的に溶媒を除去して、電気伝導性の層を得る工程。
iii)組成物Z1に接触させられる電気伝導性の層を洗浄する工程、
ここで、洗浄は、好ましくは本発明の層構造を溶媒(例えば、水)に浸漬し、続けてその層構造を乾燥し得ることにより行う。
A)基板上にある層が表面抵抗Rを有する少なくとも1つの領域であり;
B)基板上にある層が、約10倍、特に好ましくは約100倍、さらにより好ましくは約1000倍、さらにより好ましくは約10,000倍および最も好ましくは約100,000倍、Rより大きい表面抵抗を有する少なくとも1つの領域であり;
ここで、色差ΔEareaA,areaBは、最大4.5、特に好ましくは最大3.0および最も好ましくは最大1.5である。当該色差ΔEareaA,areaBは、以下のとおりに計算される:
表面抵抗の決定
表面抵抗を決定するため、長さ2.5cmのAg電極を、領域AおよびBの両方で抵抗測定が可能となる方法でシャドーマスクを使用して蒸着している。この表面抵抗を電位計(Keithley 614)を使用して決定している。例えば米国特許第6,943,571号に記載されている、いわゆる4点プローブ法の手法を行い決定した。
被覆されたPETフィルムの透過率のスペクトルを、ASTM 308−94aに従って行い測定している。Lambda 900 2チャネル分光光度計(Perkin Elmer製)を、この目的のために使用している。その機器を、15cm光度計の球と一致させている。この分光光度計の補正関数を、取扱説明書に従って、波長の較正および検出器の線形性を定期的にチェックして確保し、記録している。
ジクロロジイソシアヌル酸ナトリウムを含む洗浄剤溶液を用いた、PEDOT/PSSで被覆されたPETフィルムストリップのエッチング:
大きさが約2×10cmのストリップをPEDOT/PSS製剤で被覆されたPETフィルムから切り取る。加えて、“Dr.Weigert neodisher LaboClean A8”洗浄剤の飽和溶液(pH=10.0)を水中で作製する。上記ストリップの下半分をこの溶液に浸す。この浸した下半分および浸していない上半分の表面抵抗を、1、2および3分間後に測定する。
ジクロロジイソシアヌル酸ナトリウム溶液(pH=6)を用いた、PEDOT/PSSで被覆されたPETフィルムストリップのエッチング:
大きさが約2×10cmのストリップをPEDOT/PSS製剤で被覆されたPETフィルムから切り取る。加えて、ジクロロジイソシアヌル酸ナトリウム5%および10%水溶液を調製する。ストリップの下半分を、この水溶液に浸す。浸された下半分の表面抵抗および浸されていない上半分の表面抵抗を測定する。
ジクロロジイソシアヌル酸ナトリウム溶液(pH=10)を用いた、PEDOT/PSSで被覆されたPETフィルムストリップのエッチング:
大きさが約2×10cmのストリップをPEDOT/PSS製剤で被覆されたPETフィルムから切り取る。加えて、ジクロロジイソシアヌル酸ナトリウム5%および10%水溶液を調製し、水酸化ナトリウムを用いてpH=10に調整する。ストリップの下半分を、この水溶液に浸す。浸された下半分の表面抵抗および浸されていない上半分の表面抵抗を測定する。浸された下半分の表面抵抗および浸されていない上半分の表面抵抗を測定する。
エッチングされたPEDOT/PSS層の明度の測定:
L*a*b*座標系での色座標は、このエッチングされ、もはや導電性のない一片に基づいて決定され:
印刷されたPEDOT/PSSアンテナレイアウトのエッチング:
PEDOT/PSS製剤でプリントされたアンテナレイアウトの下半分(図3中のレイアウトa)参照)を実施例1で得られる溶液に浸す。浸された半分は、わずかに、ほとんど認知できないくらい色を薄くし、一方で、電気伝導率は、完全に破壊されている(図3中のレイアウトc)参照)。それに反して、上記アンテナレイアウトを硝酸セリウム溶液に浸す場合、PEDOT/PSS層は、広範囲にわたって脱色される(図3中のレイアウトb)参照)。
Claims (36)
- 層構造を製造するための方法であって:
i)基板および、前記基板に塗布された電気伝導性のポリマーを含む電気伝導性の層を含む層構造を準備する工程、
ii)前記電気伝導性の層の表面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することができる有機化合物を含む組成物Z1と接触させる工程、
のプロセス工程を含む方法。 - 前記組成物Z1が、少なくともpH4である水溶液または水性分散液である、請求項1に記載の方法。
- 前記電気伝導性の層が、前記電気伝導性のポリマーに加えてポリアニオンを含む、請求項1または2に記載の方法。
- 前記電気伝導性の層が、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からなる錯体を含む、請求項3に記載の方法。
- 前記電気伝導性の層が、以下のプロセス工程を含む方法によって得られる、請求項1から請求項4のいずれか1項に記載の方法:
ia)前記基板を準備する工程;
ib)前記基板の表面のうちの少なくとも一部に、前記電気伝導性のポリマーおよび溶媒を含む組成物Z2を塗布する工程;
ic)少なくとも部分的に溶媒を除去して、電気伝導性の層を得る工程。 - 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錯体を含む分散液である、請求項5に記載の方法。
- 前記有機化合物が、Halが塩素原子または臭素原子を示し、かつYが窒素を示す、少なくとも2つの構成要素(I)を含み、前記少なくとも2つの構成要素(I)が、任意に、互いに異なっている、請求項7に記載の方法。
- 前記有機化合物が、ジクロロジイソシアヌル酸ナトリウム、ジブロモジイソシアヌル酸ナトリウム、トリブロモイソシアヌル酸またはトリクロロイソシアヌル酸である、請求項9に記載の方法。
- 前記有機化合物が、1−ブロモ−3−クロロ−5,5−ジメチルヒダントイン、1−クロロ−3−ブロモ−5,5−ジメチルヒダントイン、1,3−ジクロロ−5,5−ジメチルヒダントインまたは1,3−ジブロモ−5,5−ジメチルヒダントインである、請求項11に記載の方法。
- 前記有機化合物が、ただ1つの構成要素(I)(YがNを示す)を含む、請求項1〜7のいずれか1項に記載の方法。
- 前記有機化合物が、N−クロロスクシンイミドまたはN−ブロモスクシンイミドである、請求項13に記載の方法。
- 前記有機化合物が、3−ブロモ−5−クロロメチル−2−オキサゾリジノン、3−クロロ−5−クロロメチル−2−オキサゾリジノン、3−ブロモ−5−ブロモメチル−2−オキサゾリジノンおよび3−クロロ−5−ブロモメチル−2−オキサゾリジノンからなる群から選択される、請求項15に記載の方法。
- 前記有機化合物が、ハラゾン、N,N−ジクロロスルホンアミド、N−クロロ−N−アルキルスルホンアミドまたはN−ブロモ−N−アルキルスルホンアミドであり、前記アルキル基がC1−C4アルキル基である、請求項13に記載の方法。
- 前記組成物Z1がpH4〜12である水溶液または水性分散液である、請求項1から請求項17のいずれか1項に記載の方法。
- 前記組成物Z1がpH6〜8である水溶液または水性分散液である、請求項18に記載の方法。
- 前記組成物Z1が、前記組成物Z1の総重量に対して、0.1〜50重量%の範囲の濃度で前記有機化合物を含む、請求項1から請求項19のいずれか1項に記載の方法。
- 前記組成物Z1が、前記組成物Z1の総重量に対して、1〜20重量%の範囲の濃度で前記有機化合物を含む、請求項1から請求項20のいずれか1項に記載の方法。
- 前記プロセス工程ii)で使用される組成物Z1が、請求項7〜17のいずれか1項に記載の有機化合物に加えて、安定剤としての成分シアヌル酸をさらに含む、請求項1から請求項21のいずれか1項に記載の方法。
- プロセス工程ii)で、前記電気伝導性の層を前記組成物Z1と接触させる工程が、前記組成物Z1に前記電気伝導性の層を浸漬することにより、または前記組成物Z1に前記電気伝導性の層を印刷することにより行われる、請求項1から請求項22のいずれか1項に記載の方法。
- 前記方法が、さらなるプロセス工程を含む、請求項1から請求項23のいずれか1項に記載の方法:
iii)前記組成物Z1に接触させられる電気伝導性の層を洗浄する工程。 - 前記電気伝導性の層を前記組成物Z1と接触させる工程が、色差ΔEbefore,afterが最大4.5であるような条件で行われる、請求項1から請求項24のいずれか1項に記載の方法。
- 前記電気伝導性の層を前記組成物Z1と接触させる工程が、前記組成物Z1に接触させられる領域で前記電気伝導性の層の厚さが最大50%に減少される、請求項1から請求項25のいずれか1項に記載の方法。
- 請求項1〜26のいずれか1項に記載の方法により得られうる層構造。
- 基板(2)および基板上にある電気伝導性のポリマーを含む層を含む層構造(1)であって、前記層構造が、
A)前記基板(2)上にある層が表面抵抗Rを有する少なくとも1つの領域A(3);
B)前記基板(2)上にある層が、約10倍、Rより大きい表面抵抗を有する少なくとも1つの領域B(4);
を含み、色差ΔEareaA,areaBが最大4.5である、層構造。 - 前記領域A(3)およびB(4)の透過率の差異(│TA−TB│)が領域Aの透過率(TA)の値の最大5%である、請求項28または29に記載の層構造。
- 前記領域A(3)およびB(4)が幾何学的図形を有する、請求項28〜30のいずれか1項に記載の層構造(1)。
- 前記領域A(3)およびB(4)が回路設計を一緒に形成する、請求項31に記載の層構造(1)。
- 前記領域A(3)およびB(4)がそれぞれ少なくとも0.00004mm2の表面積を有する、請求項28〜32のいずれか1項に記載の層構造(1)。
- 電子部品、タッチパネル、タッチスクリーンまたは帯電防止コーティングを製造するために請求項27〜33のいずれか1項に記載の層構造(1)の使用。
- 請求項27〜33のいずれか1項に記載の層構造(1)を含む電子部品、タッチパネル、タッチスクリーン。
- 電気伝導性のポリマーを含む電気伝導性の層を処理するための、塩素、臭素またはヨウ素を放出することができる有機化合物の使用。
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