JP6786644B2 - 銀ナノワイヤを含む組成物のパターニング - Google Patents
銀ナノワイヤを含む組成物のパターニング Download PDFInfo
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- JP6786644B2 JP6786644B2 JP2019030053A JP2019030053A JP6786644B2 JP 6786644 B2 JP6786644 B2 JP 6786644B2 JP 2019030053 A JP2019030053 A JP 2019030053A JP 2019030053 A JP2019030053 A JP 2019030053A JP 6786644 B2 JP6786644 B2 JP 6786644B2
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- Prior art keywords
- conductive layer
- silver nanowires
- etching composition
- composition
- pedot
- Prior art date
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- 238000000059 patterning Methods 0.000 title description 10
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- 239000000758 substrate Substances 0.000 claims description 31
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- 150000002894 organic compounds Chemical class 0.000 claims description 28
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- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical compound OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Description
i)少なくとも銀ナノワイヤおよび溶媒を含む組成物で基板をコーティングするステップと、
ii)前記溶媒を少なくとも部分的に除去し、それによって導電層でコーティングされた基板を得るステップであって、前記導電層は少なくとも前記銀ナノワイヤを含む、ステップと、
iii)前記導電層の選択領域をエッチング組成物と接触させ、それによって前記選択領域における前記導電層の導電率を減少させるステップであって、前記エッチング組成物は、塩素、臭素またはヨウ素を放出できる有機化合物、次亜塩素酸塩を含有する化合物、次亜臭素酸塩を含有する化合物またはこれらの化合物の少なくとも2つの混合物を含む、ステップと
を含む、方法によってなされる。
a)反応混合物を準備するステップであって、前記反応混合物は、
ポリオールと、
銀表面上に吸着される有機化学物質と、
ハロゲン化物を形成する化学物質および/または擬ハロゲン化物を形成する化学物質であって、前記ハロゲン化物を形成する化学物質は、ハロゲン化物であるCl−、Br−および/またはI−のうちの1つの塩であり、前記擬ハロゲン化物を形成する化学物質は、擬ハロゲン化物であるSCN−、CN−、OCN−および/またはCNO−のうちの1つの塩である、ハロゲン化物を形成する化学物質および/または擬ハロゲン化物を形成する化学物質と、
臭素、ヨウ素、バナジウムおよびそれらの混合物からなる群から選択される酸化還元対を形成する化学物質と、
反応混合物の総重量に基づいて好ましくは少なくとも0.5wt%の量の銀塩と
を含む、ステップと、
b)前記反応混合物を、反応の間、少なくとも100℃の温度に加熱するステップと
を含む。
− ポリオールは、好ましくは、エチレングリコール、テトラエチレングリコール、1,2−プロパンジオール、ジプロピレングリコール、1,2−ブタンジオール、1,3−ブタンジオール、1,4−ブタンジオールおよび2,3−ブタンジオールからなる群から選択される。
− 銀表面上に吸着される有機化学物質は、好ましくは、ポリビニルピロリドン(PVP)、ポリビニルアルコール(PVA)およびそれらの様々なグレート(分子量)ならびにそれらのポリマーのコポリマーからなる群から選択される。
R1およびR2は互いに独立して、各々、H、任意に置換されたC1−C18アルキル基または任意に置換されたC1−C18アルコキシ基を示し、R1およびR2は一緒に、任意に置換されたC1−C8アルキレン基(ここで、1つ以上のC原子は、OまたはSから選択される1つ以上の同一または異なるヘテロ原子と置きかえられてもよい)、好ましくはC1−C8ジオキシアルキレン基、任意に置換されたC1−C8オキシチアアルキレン基または任意に置換されたC1−C8ジチアアルキレン基または任意に置換されたC1−C8アルキリデン基(ここで、任意に少なくとも1つのC原子はOまたはSから選択されるヘテロ原子と置きかえられる)を示す。
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るが、好ましくは塩素または臭素を示し、
Yは、N、SおよびPから選択されるが、好ましくはNを示し、
X1およびX2は、同じであっても、異なっていてもよく、各々は、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を示し、1つ以上のさらなる原子が任意にX1およびX2に結合されてもよい)
を含む有機化合物である。X1およびX2に結合するさらなる原子の数はX1およびX2の共有原子価に依存する。
を含むことが最も特に好ましい。これらの有機化合物の中で、ナトリウムジクロロジイソシアヌレート、ナトリウムジブロモジイソシアヌレート、トリブロモイソシアヌル酸およびトリクロロイソシアヌル酸が特に好ましい。
を含むことが好ましい。
を含む。これに関して、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−オキサゾリジノンが、適切な有機化合物の例として挙げられ得る。
iv)エッチング組成物と接触させた導電層を洗浄するステップ
を含んでもよく、洗浄は好ましくは、層構造を溶媒、例えば水中に浸漬することによって行われ、この後に乾燥ステップが行われてもよい。
A)基板の上部の導電層が表面抵抗Rを有する少なくとも1つの領域Aと、
B)基板上の導電層が、Rより少なくとも10倍、好ましくは少なくとも100倍、さらにより好ましくは少なくとも1000倍、さらにより好ましくは少なくとも10,000倍、最も好ましくは少なくとも100,000倍高い表面抵抗を有する少なくとも1つの領域Bと
を含み、色差Δ領域A、領域Bは、多くとも4.5、特に好ましくは多くとも3.0、最も好ましくは多くとも1.5である。色差Δ領域A、領域Bは、以下のように計算される:
表面抵抗の決定
この決定は、例えば、米国特許第6,943,571B1号に記載されているいわゆる4点プローブ測定によって実施した。この値はΩ/スクエアで与える。
コーティングされたPET膜の透過スペクトルの測定を、Perkin Elmer製のLambda 900 2チャネル分光光度計で実施する。この機器は15cm球形光度計を備え、測定は球で実施し、散乱光の干渉が検出されないことを確実にする。したがって、透過率についてここで提示されている値はまた、散乱光も含むか、またはこのために透過率は1−吸収である。
内部透過率はY/Y0×100パーセントに対応する。
銀ナノワイヤ(AgNW)は、例えば、国際公開第2012/022332号に記載されているポリオール合成を使用して合成した。得られた混合物の50gを130mLのアセトンと混合した。混合物を30分間撹拌した。上清溶液を捨て、沈殿物を得る。
透明導電性コーティングのために銀ナノワイヤを有する配合物Clevios pH1000を調製する。2.77gの銀ナノワイヤ(重量測定により2.7%の銀含有量、75mgの銀)を、5.71gの水、7.85gのClevious pH1000(86mgのPEDOT/PSS、Heraeus Precious Metals GmbH & Co.KG、Leverkusen)、0.755gのジメチルスルホキシド(DMSO、ACS試薬、Sigma Aldrich、Munich)および50μLのTriton X100(Sigma Aldrich、Munich)と混合した。配合物は、6μmの湿潤膜厚ドクターブレード(Erichsen K Hand Coater 602)を使用してMelinex 506膜(Putz GmbH+Co.Folien KG.Taunusstein)でコーティングした。コーティングを120℃にて5分間乾燥させた。
実施例2からのコーティングされた膜を約5×10cmの小片に切断した。ストライプの下半分を、異なる水ベースのエッチング溶液中に2分間浸漬し、続いて水浴中で1分間リンスし、120℃で5分間乾燥させた。表面抵抗率を4点プローブ技法による処理の前後に測定した。結果を表1にまとめる。
ジクロロイソシアヌル酸の10%溶液でエッチングされた膜を、2または4日間、85℃および85%湿度にて気候キャビネットに保存し、表面抵抗率を再び測定した。全ての試料について、エッチング部分の表面抵抗率は検出できなかった(>1×108Ω/スクエア)。
Claims (8)
- 層構造を製造する方法であって、
i)少なくとも銀ナノワイヤ、導電性ポリマー、スルホン化ポリマーおよび溶媒を含み、前記導電性ポリマーはポリ(3,4−エチレンジオキシチオフェン)(PEDOT)であり、前記スルホン化ポリマーはポリスチレンスルホン酸(PSS)であり、前記PEDOTおよび前記PSSがPEDOT/PSS複合体の形態で存在する組成物で基板をコーティングするステップと、
ii)前記溶媒を少なくとも部分的に除去し、それによって導電層でコーティングされた基板を得るステップであって、前記導電層は少なくとも前記銀ナノワイヤおよび前記PEDOT/PSS複合体を含む、ステップと、
iii)前記導電層の選択領域をエッチング組成物と接触させ、それによって前記選択領域における前記導電層の導電率を減少させるステップであって、前記エッチング組成物は、塩素をHOClの形態で放出できる有機化合物を含む、ステップと
を含み、
塩素をHOClの形態で放出できる前記有機化合物は、ナトリウムジクロロイソシアヌレートおよびトリクロロイソシアヌル酸を含む群から選択される、方法。 - ステップi)に使用される前記組成物中の前記銀ナノワイヤは、1μm〜200μmの長さ、20nm〜1,300nmの直径および少なくとも5のアスペクト比(長さ/直径)を有する、請求項1に記載の方法。
- ステップi)に使用される前記組成物中の前記銀ナノワイヤは、
a)反応混合物を準備するステップであって、前記反応混合物は、
ポリオールと、
銀表面上に吸着される有機化学物質と、
ハロゲン化物を形成する化学物質および/または擬ハロゲン化物を形成する化学物質であって、前記ハロゲン化物を形成する化学物質は、ハロゲン化物であるCl−、Br−および/またはI−のうちの1つの塩であり、前記擬ハロゲン化物を形成する化学物質は、擬ハロゲン化物であるSCN−、CN−、OCN−および/またはCNO−のうちの1つの塩である、ハロゲン化物を形成する化学物質および/または擬ハロゲン化物を形成する化学物質と、
臭素、ヨウ素、バナジウムおよびそれらの混合物からなる群から選択される酸化還元対を形成する化学物質と、
銀塩と
を含む、ステップと、
b)前記反応混合物を、反応の間、少なくとも100℃の温度に加熱するステップと
を含むステップによって得られる、請求項1または2に記載の方法。 - ステップiii)に使用される前記エッチング組成物は、前記エッチング組成物の総重量に対して0.01〜50wt%の範囲の濃度で、塩素、臭素またはヨウ素を放出できる有機化合物を含む、請求項1〜3のいずれか一項に記載の方法。
- 前記導電層の前記エッチング組成物との接触は、前記導電層を前記エッチング組成物に浸漬することによって、または前記導電層を前記エッチング組成物で印刷することによって実施される、請求項1〜4のいずれか一項に記載の方法。
- 前記方法は、さらなるステップとして、
iv)前記エッチング組成物と接触させた前記導電層を洗浄するステップ
を含む、請求項1〜5のいずれか一項に記載の方法。 - ステップiii)において前記エッチング組成物と接触する前記選択領域の表面抵抗が、ステップii)で提供される前記層の表面抵抗よりも少なくとも10倍高く、
ステップiii)において前記エッチング組成物と接触する前記選択領域と、ステップii)における前記導電層と、の色差ΔEが多くても4.5である、請求項1〜6のいずれか一項に記載の方法。 - 少なくとも銀ナノワイヤとPEDOT/PSS複合体を含む導電層を処理するための、塩素をHOClの形態で放出できる有機化合物の使用であって、
塩素をHOClの形態で放出できる前記有機化合物は、ナトリウムジクロロイソシアヌレートおよびトリクロロイソシアヌル酸を含む群から選択される、使用。
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US10714230B2 (en) | 2017-12-06 | 2020-07-14 | C3Nano Inc. | Thin and uniform silver nanowires, method of synthesis and transparent conductive films formed from the nanowires |
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