JP2018528312A - 導電性ナノ複合体 - Google Patents
導電性ナノ複合体 Download PDFInfo
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- JP2018528312A JP2018528312A JP2018513366A JP2018513366A JP2018528312A JP 2018528312 A JP2018528312 A JP 2018528312A JP 2018513366 A JP2018513366 A JP 2018513366A JP 2018513366 A JP2018513366 A JP 2018513366A JP 2018528312 A JP2018528312 A JP 2018528312A
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- ligand
- conductive
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- polymer
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- 125000001931 aliphatic group Chemical group 0.000 description 2
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- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
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- 238000002329 infrared spectrum Methods 0.000 description 2
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- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 2
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- 238000007641 inkjet printing Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 1
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphonic acid group Chemical group P(O)(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical group N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 239000011970 polystyrene sulfonate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- TVDSBUOJIPERQY-UHFFFAOYSA-N prop-2-yn-1-ol Chemical compound OCC#C TVDSBUOJIPERQY-UHFFFAOYSA-N 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- 125000001273 sulfonato group Chemical class [O-]S(*)(=O)=O 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
- 150000003536 tetrazoles Chemical group 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
a)少なくとも1つの導電性リガンドがナノ構造の表面上に配置された少なくとも1種類の導電性又は半導電性ナノ構造と、
b)少なくとも1つの溶媒と、
を含む、組成物によって解決される。
a)少なくとも1つの第1のリガンドによって安定化された、導電性又は半導電性ナノ構造の分散液の準備と、
b)少なくとも1つの導電性リガンドの添加と、
c)少なくとも1つの導電性リガンドによる第1のリガンドの少なくとも一部の置換と、
を含む方法を行うのが好ましい。
a)表面への本発明による組成物の適用と、
b)少なくとも1つの溶媒の除去と、
を含む、方法も提供する。
エネルギー消費プロセス工程が不要となる。
所与の容量を有するリガンドの除去により、当然ながら粒子の空間要求が所与の容量の分だけ減少する。これにより先に構成された構造が分解される可能性があるか、又は粒子の単分子層が存在する場合、粒子間の直接接触が失われる。
タイプII複合体をウェットコーティングにより一プロセス工程で直接作製することができ、マトリックスポリマーを選択することで、リガンドの除去によりマトリックスポリマーも除去されず、又はその特性が悪影響を受けないことを確実にする必要はない。
20nm〜50nmの直径及び80nm〜150nmの長さのアスペクト比を有する金ナノロッドをYe et al.による方法によって作製した。この目的で、成長溶液(500ml〜2l)をAuCl4(0.5mM)、臭化セチルトリメチルアンモニウム(CTAB 0.4M)、オレイン酸ナトリウム(800mM)、アスコルビン酸(0.16mM)、並びに様々な容量の硝酸銀溶液(4mM)及びHCl(32%)を用いて調製した。異方性結晶成長を特定の容量の球状金核の添加によって誘発した。この核分散液は、NaBH4を用いたCTAB水溶液(0.1M)中5mlのHAuCl4(0.25mM)の還元、及び30分間のインキュベーションにより事前に作製した。反応物を35℃で14時間静置した。次いで、金ナノロッド(AuNR)を遠心分離によって精製し、CTAB溶液(1mM)中で保管した。プロセスは2Lのサイズまでスケールアップすることができた。これは約200mgの金という金ナノロッドの乾燥質量+付加的なリガンドの質量(210mgに対応する)に対応する。作製された金ナノロッドは、断面積(TEMによって測定される)をベースとして10%未満の直径及び長さの偏差を有する。分散液については、pH7で+20mVのゼータ電位が測定された。これは純粋に静電的な安定化という点での平均コロイド安定性を示す。リガンド/金属比は熱重量測定により約5:95(m/m)と決定された。20nmの直径及び100nmの長さ(TEMによって決定される)を有する円筒形と仮定すると、これは1nm2当たり8個のCTAB分子の単分子層に相当する。CTABは水性環境で二重層を形成する傾向がある。金ロッドの単分子層が1nm2当たり4個以下のCTAB分子を有すると仮定する。
項目1に従って作製した、CTABを用いて安定化した金ナノロッド(AuNR@CTAB)を洗浄し、過剰なCTABを除去し、所望の金含量を設定した。この目的で、ポリマーの溶液(水中0.5mg/mlのポリ(2−(3−チエニル)エトキシ−4−ブチルスルホネート(PTEBS) 40kDa〜70kDa))を添加し、AuNR@CTABの分散液(水中0.5mg/mlの金)とともに室温で24時間撹拌した。金ナノロッドを特定の容量の純溶媒中での再分散によって精製し、所望の標的濃度とした。ゼータ電位が+20mVから−45mVへと変化し(pH7)、リガンド交換の成功が示された。リガンド交換の成功は分光法によって確認された。透過型電子顕微鏡写真からリガンドシェルの厚さを約1nmと推定することができ、これは熱重量測定に一致する。いずれの場合にも3つの寸法のうち1つの広がりに関する情報を与える文献データ(Liu et al.(ポリチオフェン骨格におけるモノマーの間隔)、Zhang et al.(この側鎖を有するポリマー鎖を好ましくは互いに対して仮定した間隔)、Colle et al.(共役ポリマー間のp−スタッキング距離(p-stacking distance)))から、使用したポリマーについて1nm3当たり7.2個のモノマーというポリマーのパディング密度(padding density)を算出することができ、加熱時の質量の減少からリガンドシェルの厚さは同様に1nmと決定された。
PEDOT:PSS(ポリ(エチレン−3,4−ジオキシチオフェン):ポリスチレンスルホネート)を用いたリガンド交換を、2.と同様にして行った。分析を用いてリガンドの交換を確認した。得られる分散液は極性溶媒(イソプロパノール、アセトン、メタノール、エタノール)中で少なくとも1週間安定していた。作製されたコーティングは1Ω/sqの伝導性を示し、これはリガンドの除去後のナノ構造の伝導性よりもはるかに良好である。
ポリ(3−ヘキシルチオフェン−2,5−ジイル)(MN 15000〜45000)で修飾された金ナノロッドを作製した。この目的で、リガンドを合成中に添加した。このリガンドは非極性溶媒(クロロホルム、トルエン)中での安定性を促進する。焼結を行わずに作製した層の伝導性を測定した。
金粒子(直径15nm、シトレートを用いて安定化した)上でのリガンド交換を2.と同様にして行った。ゼータ電位は−29.2mVから34.9mVへと変化したが、これは中程度の安定性を示す。
水/メタノール(10:90)中の本発明に従って修飾された金ナノロッドの分散液をガラス基板に適用した。鋳型を用いて直線のラインを作製した。市販の銀塗料を電極に使用した。
Claims (15)
- 導電性又は半導電性層をウェットコーティングによって作製するための組成物であって、
a)少なくとも1つの導電性リガンドがナノ構造の表面上に配置された少なくとも1種類の導電性又は半導電性ナノ構造と、
b)少なくとも1つの溶媒と、
を含む、組成物。 - 前記リガンドが、チオフェンをベースとした導電性ポリマー又はオリゴマーであることを特徴とする、請求項1に記載の組成物。
- 前記ナノ構造が、少なくとも2:1という長さ対直径のアスペクト比を有するナノロッドであることを特徴とする、請求項1又は2に記載の組成物。
- 前記少なくとも1つの導電性リガンドが、前記ナノ構造の表面への配位結合を可能とする少なくとも10個の結合位置を有するポリマー又はオリゴマーを含むことを特徴とする、請求項1〜3のいずれか一項に記載の組成物。
- マトリックスポリマーを含むことを特徴とする、請求項1〜4のいずれか一項に記載の組成物。
- 前記マトリックスポリマーが前記組成物中に溶液として存在することを特徴とする、請求項5に記載の組成物。
- 前記マトリックスポリマーがポリスチレン、ポリアクリレート、ポリビニルアルコール及び/又はポリビニルピロリドンを含むことを特徴とする、請求項5又は6に記載の組成物。
- 前記ナノ構造が金属ナノ構造であることを特徴とする、請求項1〜7のいずれか一項に記載の組成物。
- 前記少なくとも1つの溶媒が、いずれの場合にも120℃未満の沸点を有する溶媒又は該溶媒の溶媒混合物から選択されることを特徴とする、請求項1〜8のいずれか一項に記載の組成物。
- 導電性又は半導電性層を表面上に作製する方法であって、以下の工程:
a)表面への請求項1〜9のいずれか一項に記載の組成物の適用と、
b)少なくとも1つの溶媒の除去と、
を含む、方法。 - 前記表面への適用後に60℃を超える温度での任意のコーティングの処理を含まないことを特徴とする、請求項10に記載の方法。
- 請求項10又は11に記載の方法によって得られる導電性又は半導電性構造。
- 導電性又は半導電性ナノ構造と、少なくとも1つの導電性リガンドと、少なくとも1つのマトリックスポリマーとを含む複合材料。
- ディスプレー、導体トラック、回路、コンデンサ、太陽電池への請求項12に記載の構造又は請求項13に記載の複合材料の使用。
- 請求項1〜9のいずれか一項に記載の組成物を作製する方法であって、以下の工程:
a)少なくとも1つの第1のリガンドによって安定化された、導電性又は半導電性ナノ構造の分散液の準備と、
b)少なくとも1つの導電性リガンドの添加と、
c)前記少なくとも1つの導電性リガンドによる前記第1のリガンドの少なくとも一部の置換と、
を含む、方法。
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