JP2013521595A - 表面埋め込み添加物を伴う構造および関連する製造方法 - Google Patents
表面埋め込み添加物を伴う構造および関連する製造方法 Download PDFInfo
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- AQQOUVLRCMEMHI-UHFFFAOYSA-N tributyl(heptyl)azanium Chemical compound CCCCCCC[N+](CCCC)(CCCC)CCCC AQQOUVLRCMEMHI-UHFFFAOYSA-N 0.000 description 1
- FJAPXHMQWAFWMW-UHFFFAOYSA-N tributyl(hexyl)azanium Chemical compound CCCCCC[N+](CCCC)(CCCC)CCCC FJAPXHMQWAFWMW-UHFFFAOYSA-N 0.000 description 1
- VMJGCUPCIRNLPY-UHFFFAOYSA-N tributyl(octyl)azanium Chemical compound CCCCCCCC[N+](CCCC)(CCCC)CCCC VMJGCUPCIRNLPY-UHFFFAOYSA-N 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- DTQVDTLACAAQTR-UHFFFAOYSA-N trifluoroacetic acid Substances OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 1
- 125000004205 trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 description 1
- FLTJDUOFAQWHDF-UHFFFAOYSA-N trimethyl pentane Natural products CCCCC(C)(C)C FLTJDUOFAQWHDF-UHFFFAOYSA-N 0.000 description 1
- ZISSAWUMDACLOM-UHFFFAOYSA-N triptane Chemical compound CC(C)C(C)(C)C ZISSAWUMDACLOM-UHFFFAOYSA-N 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- HWLMPLVKPZILMO-UHFFFAOYSA-N zinc mercury(1+) selenium(2-) Chemical compound [Zn+2].[Se-2].[Hg+] HWLMPLVKPZILMO-UHFFFAOYSA-N 0.000 description 1
- 229940048462 zinc phosphide Drugs 0.000 description 1
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本願は、米国仮出願第61/308,894号(2010年2月27日出願)、米国仮出願第61/311,395号(2010年3月8日出願)、米国仮出願第61/311,396号(2010年3月8日出願)、米国仮出願第61/408,773号(2010年11月1日出願)、米国仮出願第61/409,116号(2010年11月2日出願)の利益を主張する。該出願は、それらの全体が参照により本明細書に引用される。
本発明は、概して、埋め込み添加物を伴う構造に関する。より具体的には、本発明は、電気伝導度等の機能性を付与するように表面埋め込み添加物を伴う構造に関する。
以下の定義は、本発明のいくつかに関して説明される要素のうちのいくつかに該当する。これらの定義は、同様に、本明細書において拡張させられてもよい。
本明細書で説明される表面埋め込み構造は、導電性添加物の組み込みを介して電気伝導度を獲得しようとする他の考えられるアプローチとは異なる。3つの他のアプローチが図1Aから図1Cに図示され、図1Dから図1Hおよび図2Aから図2Gを参照して図示および説明される改良型表面埋め込み構造と対比される。
本明細書で説明される表面埋め込み構造は、ドープした金属酸化物被覆の形態であるTCEを使用する任意のデバイスを含む、種々のデバイスで電極として使用することができる。好適なデバイスの実施例は、太陽電池(例えば、薄膜太陽電池および結晶シリコン太陽電池)、表示デバイス(例えば、フラットパネルディスプレイ、液晶ディスプレイ(「LCD」)、プラズマディスプレイ、有機発光ダイオード(「OLED」)ディスプレイ、電子ペーパー(「eペーパー」)、量子ドットディスプレイ、およびフレキシブルディスプレイ)、固体照明デバイス(例えば、OLED照明デバイス)、タッチスクリーンデバイス(例えば、投影容量性タッチスクリーンデバイス、および抵抗性タッチスクリーンデバイス)、スマートウィンドウ(または他のウィンドウ)、フロントガラス、航空宇宙透明フィルム、電磁干渉遮蔽体、電荷消散遮蔽体、および静電気防止遮蔽体、ならびに他の電子、光学、光電子、量子、光起電、およびプラズモンデバイスを含む。
本明細書では、添加物が、多種多様の母材に耐久的に表面埋め込みされ、母材の中へ添加物をしっかりと潜り込ませる、高度に拡張可能で迅速な低費用の様式で、表面埋め込み構造を形成する製造方法が開示される。
・表面との埋め込み流体の適合性(例えば、ヒルデブランドおよびハンセン溶解度パラメータ、誘電率、分配係数、pKa等の合致または比較)
・蒸発速度、沸点、蒸気圧、埋め込み流体の蒸発のエンタルピー
・表面の中への埋め込み流体の拡散:熱力学および動力学的配慮
・埋め込み流体の粘度
・埋め込み流体の表面張力、吸い上げ、および毛管効果
・共沸、混和性、および他の流体との他の相互作用。
・流体表面露出の持続時間
・温度
・湿度
・塗布方法(例えば、噴霧、印刷、圧延被覆、グラビア被覆、スロットダイ、カップ被覆、ブレード被覆、エアブラッシング、浸漬、浸漬被覆等)
・表面上への添加物の衝突/運動量/速度(例えば、埋め込みの深さおよび程度に影響を及ぼし得る)
・後処理条件(例えば、加熱、蒸発、流体除去、空気乾燥等)。
・表面エネルギー
・粗度および表面積
・前処理(例えば、紫外線オゾン処理、基礎エッチング、清掃、溶媒下塗り等)
・埋め込み前の流体中の添加物の分散/懸濁(例えば、添加物は、物理的撹拌、化学/キャッピング安定化、立体安定化を通して溶液中に分散されたままとなることができる、または本質的に可溶化される)
・望ましくない効果(例えば、かすみ、ひび割れ、白化、母材の不可逆的な破壊、不均等な湿潤、粗度等)の軽減。
以下の実施例は、当業者のための説明を例証および説明するように、本発明のいくつかの実施形態の具体的な側面を説明する。実施例は、本発明のいくつかの実施形態を理解および実践するのに有用である具体的な方法論を提供するにすぎないため、実施例は、本発明を限定するものとして解釈されるべきではない。
1ステップ埋め込みを介した透明伝導性電極の形成
銀ナノワイヤ(直径=90nmおよび長さ=60μm)を5秒間ボルテックスし、5mg/mlの濃度におけるイソプロパノール(50vol.%)および2,2,2−トリフルオロエタノール(50vol.%)(Alfa Aesar 99%+)の溶液中で分散させる。アクリル板から1ミル分離されたブレードを用いて、銀ナノワイヤを含有する溶液を透明アクリル(ポリメタクリル酸メチル、Sign Mart, Inc.)の平板上にカップ被覆し、20℃および23%湿度の下で3インチ/秒の速度にて引き出す。0.5mlのナノワイヤ含有溶液が、1平方メートルのアクリル板の半分を十分に覆った。この処方および手順は、ナノワイヤがアクリル板の表面で部分的に露出され、アクリル板を含む86.6%の透過率Tと、Jenway UV−vis分光光度計およびSP4−Keithley4点プローブシステムによって測定されるような29±6Ω/sq(stdev)のシート抵抗Rとを示すように、効果的に溶媒に埋め込まれた銀ナノワイヤをもたらした。ナノワイヤが埋め込まれたアクリル板は、セロハンテープ付着試験され、透過率、シート抵抗、および他の特性の観察可能な変化を示さず、埋め込まれたナノワイヤの耐久性を実証した。
2ステップ埋め込みを介した透明伝導性電極の形成
銀ナノワイヤ(直径=90nmおよび長さ=60μm)を、2.5mg/mlの濃度におけるイソプロパノール中で分散させ、次いで、20ミルのワイヤ分離距離を伴うメイヤーロッド(Gard Co.)を用いて、透明アクリル(ポリメタクリル酸メチル、Sign Mart, Inc.)の表面上に塗布し、2.5インチ/秒の速度にて引き出す。被覆後、底部に40mlのテトラヒドロフランを含有する直径100mm×20mmの円形断面コンテナ上で表を下にするようにナノワイヤ網を逆転させることによって、結果として生じたナノワイヤ網およびアクリル基板をテトラヒドロフラン(BHTで安定化されたJ.T. Baker 99.5%)に40分間暴露させる。この処方および手順は、アクリル基板を含む74.3%の透過率Tおよび31±2Ω/sq(stdev)のシート抵抗Rを示す、効果的に溶媒に埋め込まれた銀ナノワイヤをもたらした。ナノワイヤが埋め込まれたアクリル基板は、セロハンテープ付着試験され、透過率、シート抵抗、および他の特性の観察可能な変化を示さず、埋め込まれたナノワイヤの耐久性を実証した。
2ステップ埋め込みを介した透明伝導性電極の形成
銀ナノワイヤ(直径=90nmおよび長さ=60μm)を、1mg/mlの濃度におけるメタノール(Sigma Aldrich 99%+)中で分散させ、次いで、20℃および23%湿度の下で、基板から9インチ分離された、20psi入口圧力で動作するIwata LPH400 HVLPスプレーガンを介して、ポリカーボネート基板(Makrolon(登録商標))上に塗布する。メタノールの蒸発速度は、ノズルから極めて細かい霧化円錐パターンを分注する、スプレーガン設定とともに、ノズルから噴出するメタノールが9インチ離れた基板に到達する前に実質的に蒸発する、噴霧をもたらした。メタノールは、ナノワイヤを効果的に懸濁させる働きをし、メタノールおよび霧化空気圧は、基板に向かってナノワイヤを運搬する推進剤の役割を果たす。しかしながら、メタノールは、実質的に蒸発し、基板表面を湿潤せず、それにより、移動、凝集、コーヒーの染みのリング効果、ベルナールセル、および堆積ナノワイヤ網の他の空間的不均一性を引き起こし得る、基板表面の不均等な湿潤を回避または低減する。次いで、底部に40mlのアセトンを含有する直径100mm×20mmの円形断面コンテナ上で表を下にするようにナノワイヤ網を逆転させることによって、基板の中へのナノワイヤ網の溶媒で支援された埋め込みを可能にするように、基板に付着した、結果として生じる乾燥ナノワイヤ網を、アセトン(Sigma Aldrich>99.9%)の蒸気に10分間暴露させる。この処方および手順は、ポリカーボネート基板を含む74.4%の透過率Tおよび23Ω/sq(stdev)のシート抵抗Rを示す、効果的に溶媒に埋め込まれた銀ナノワイヤをもたらした。ナノワイヤが埋め込まれたポリカーボネート基板は、セロハンテープ付着試験され、透過率、シート抵抗、および他の特性の観察可能な変化を示さず、埋め込まれたナノワイヤの耐久性を実証した。
1ステップ埋め込みを介した埋め込み基板の形成
銀シリカの粉末(5μ)を、6.4mg/mlの濃度における酢酸メチル(60vol.%)/酢酸エチル(20vol.%)/シクロロヘキサノン(20vol.%)の溶液中で懸濁し、撹拌し、次いで、20℃および40%湿度の下で、20psi入口圧力で動作し、1.3mm針サイズである、基板から8インチ分離されたIwata LPH101 HVLPスプレーガンを使用して、透明ポリカーボネートの基板上に噴霧する。ナノワイヤ含有溶液が基板に数秒間暴露された後、溶媒系は、周囲室温条件下で揮発し、粒子を軟化したポリカーボネート表面に耐久的に埋め込む。
ガラス上の透明伝導性電極の形成
40mLシンチレーションバイアルに、18.5mLの乾燥200プルーフエタノール(CAS#67−17−5)、0.075mLの脱イオン(「DI」)水中の1M塩酸(18×106Ω)、および0.92mLの付加的なDI水を添加した。この混合物を均質になるまでかき混ぜた。急速にかき混ぜながら、この混合物に5.6mLのテトラエトキシシラン(TEOS、CAS#78−10−4、別名テトラオルトシリケート、Si(OC2H5)4)を添加した。結果として生じる溶液が均質になるまでかき混ぜ続け(約15分)、凝縮を介して部分的に重合するために、溶液を60℃で2日間貯蔵した。
TEOSガラス上の透明伝導性電極の形成
清潔なスポンジを使用した機械的撹拌を介して、ガラス基板を2vol.%Micro90溶液で清掃し、その後に2回のDI水の洗浄槽が続き、DI水を流した。次の段階を待つように、ガラス基板をDI水槽の中で保持した(わずか3時間)。ガラス基板を水槽から除去し、イソプロパノール(IPA、別名2−プロパノール)槽の中へ移行し、その後に流れるIPAを用いて洗浄し(噴出ボトル)、HVLPスプレーガンを使用したエアナイフ乾燥ステップで終了した。TEOS溶液の堆積の直前に、表面調製のためにガラス基板をUVOチャンバ(UVOCS Corp. T10X10)に20分間入れた。
透明伝導性電極の形成
清潔なスポンジを使用した機械的撹拌を介して、ガラス基板を2vol.%Micro90溶液で清掃し、その後に2回のDI水の洗浄槽が続き、DI水を流した。次の段階を待つように、ガラス基板をDI水槽の中で保持した(わずか3時間)。ガラス基板を水槽から除去し、イソプロパノール(IPA、別名2−プロパノール)槽の中へ移行し、その後に流れるIPAを用いて洗浄し(噴出ボトル)、HVLPスプレーガンを使用したエアナイフ乾燥ステップで終了した。TEOS溶液の堆積の直前に、表面調製のためにガラス基板をUVOチャンバ(UVOCS Corp. T10X10)に20分間入れた。
透明伝導性電極の形成および特性化
ポリカーボネートの中の銀ナノワイヤ網の埋め込まれた平面領域を特色とするように、透明伝導性電極を形成した。4点プローブ電気伝導度測定のために、4つの伝導性パッドが堆積され、測定、少なくとも1のサンプルに対して3.2Ω/sqのシート抵抗Rを示した。この抵抗値は、シリコン太陽電池で使用される透明伝導性電極の典型的なシート抵抗値(30〜100Ω/sq)と比べた、かつディスプレイで使用される透明伝導性電極の典型的なシート抵抗値(100〜350Ω/sq)と比べた改良である。UV−vis分光分析を使用して透過率値を判定し、4点プローブ方法を使用してシート抵抗値を判定し、ファンデルパウ方法および2点プローブ方法を使用して照合した。これらの値を用いて、DC対光学伝導度比を導出した。基板に表面埋め込みされたナノワイヤ網は、それらの埋め込まれていない(表面的に堆積された)対応物よりも高いDC対光学伝導度比を示した。ナノワイヤ網は、電気的パーコレーションをほとんど、または全く阻害せず、埋め込み時に損なわれないままである。同時に、ナノワイヤ網の埋め込み性質は、複数のセロハンテープ耐久性応力試験および物理的摩耗にわたって実質的に改変されていないシート抵抗値を伴って、耐久性のある透明伝導性電極をもたらした。
透明伝導性電極の特性化
図11は、ポリカーボネート膜およびアクリルに表面埋め込みされた銀ナノワイヤ網の(一定のDC対光学伝導度比における)透過率および対応するシート抵抗のトレードオフ曲線を図示し、水平線は、所与の表面にわたるシート抵抗の標準偏差を表す。
透明伝導性電極の特性化
図12は、堆積直後および表面埋め込み後のデータを比較する、2ステップ堆積および埋め込み方法を介して製造されたサンプルについて収集された、透明性およびシート抵抗データの表である。表面的に堆積されたナノワイヤを伴うアクリルと表面埋め込みナノワイヤを伴うアクリルとの間の違いを比較するように、アクリル航空機透明フィルムの切り取り試片を作製した。表面的に堆積されたナノワイヤを伴うほとんどの切り取り試片が、単純耐久性応力試験(セロハンテープ方法)の前後に使用された4点プローブツール(Keithley Digital Multimeter)の10MΩ限界を超える、検出不能に高いシート抵抗値を示した一方で、表面埋め込み切り取り試片は、応力試験によって大部分が改変されなかった低いシート抵抗を示した。
透明伝導性電極の特性化
銀ナノワイヤ(平均長さ=7μm、平均直径=70nm)を、表面より下側の深さまで透明ポリカーボネートに埋め込み、80%を上回る透過率値および100Ω/sqまたはそれを下回るシート抵抗値をもたらした。さらなる最適化により、10Ω/sqを下回る(例えば、3Ω/sqほども低い)シート抵抗値を獲得することができる。(例えば、被覆または界面がない場合)モノリシック母材および表面より下側にある埋め込まれた銀ナノワイヤの平面領域を伴う断面を明らかにするために、集束イオンビームを用いた走査型電子顕微鏡像を使用した。
透明伝導性電極の特性化
銀ナノワイヤ(平均長さ=7μm、平均直径=70nm)を、ナノワイヤの直径の100%未満の深さまで透明ポリカーボネートに埋め込み、約90%の透過率値および約100Ω/sqのシート抵抗値をもたらした。さらなる最適化により、10Ω/sqを下回る(例えば、3Ω/sqほども低い)シート抵抗値を獲得することができる。
透明伝導性電極の形成
銀ナノワイヤ(平均長さ=7μm、平均直径=70nm)およびITOナノ粒子(直径<100nm)を、ナノワイヤの直径の100%未満およびナノ粒子の直径の100%未満の深さまで透明ポリカーボネートに埋め込んだ。
Claims (19)
- 埋め込み表面を有する母材と、
前記母材に少なくとも部分的に埋め込まれた添加物と
を備え、
前記添加物は、前記埋め込み表面に隣接する埋め込み領域内に限局され、前記埋め込み領域の厚さは、前記母材の全体厚さよりも小さく、前記添加物は、導電性および半導体のうちの少なくとも1つであり、前記添加物は、ナノサイズの添加物およびミクロンサイズの添加物のうちの少なくとも1つを含む、表面埋め込み構造。 - 前記埋め込み領域の厚さは、前記母材の全体厚さの50%以下の大きさである、請求項1に記載の表面埋め込み構造。
- 前記埋め込み領域の厚さは、前記母材の全体厚さの20%以下の大きさである、請求項2に記載の表面埋め込み構造。
- 前記添加物のうちの少なくとも1つは、nm範囲内の特徴的な寸法を有し、前記埋め込み領域の厚さは、前記特徴的な寸法の5倍以下の大きさである、請求項1に記載の表面埋め込み構造。
- 前記埋め込み領域の厚さは、前記特徴的な寸法の2倍以下である、請求項4に記載の表面埋め込み構造。
- 前記添加物のうちの少なくとも1つは、前記特徴的な寸法の多くて100%の程度まで前記母材に埋め込まれる、請求項4に記載の表面埋め込み構造。
- 前記添加物のうちの少なくとも1つは、前記特徴的な寸法の100%を上回る程度まで前記母材に埋め込まれるが、前記埋め込み表面に隣接して限局される、請求項4に記載の表面埋め込み構造。
- 前記母材は、透明基板に対応し、前記添加物は、前記透明基板に少なくとも部分的に埋め込まれる、請求項1に記載の表面埋め込み構造。
- 前記透明基板は、ポリマーおよびセラミックのうちの少なくとも1つを含む、請求項8に記載の表面埋め込み構造。
- 前記母材は、被覆に対応し、前記添加物は、前記被覆に少なくとも部分的に埋め込まれる、請求項1に記載の表面埋め込み構造。
- 前記被覆は、ポリマーおよびセラミックのうちの少なくとも1つを含む、請求項10に記載の表面埋め込み構造。
- 基板をさらに備え、前記被覆は、前記基板上に配置され、前記埋め込み表面は、前記基板から見て外方に向く、請求項10に記載の表面埋め込み構造。
- 前記被覆は、第1の被覆であり、前記第1の被覆上に配置され、前記添加物に電気的に連結された第2の被覆をさらに備え、前記第2の被覆は、導電性材料を含む、請求項12に記載の表面埋め込み構造。
- 前記導電性材料は、透明である、請求項13に記載の表面埋め込み構造。
- 前記導電性材料は、ドープした金属酸化物および導電性ポリマーのうちの少なくとも1つを含む、請求項14に記載の表面埋め込み構造。
- 前記母材の中の前記添加物の荷重は、電気的パーコレーション閾値を上回る、請求項1に記載の表面埋め込み構造。
- 前記添加物は、ナノチューブ、ナノワイヤ、およびナノ粒子のうちの少なくとも1つを含む、請求項1に記載の表面埋め込み構造。
- 前記表面埋め込み構造は、少なくとも85%の透過率と、100Ω/sq以下であるシート抵抗とを有する、請求項1に記載の表面埋め込み構造。
- 前記シート抵抗は、25Ω/sq以下である、請求項18に記載の表面埋め込み構造。
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US20110281070A1 (en) | 2011-11-17 |
EP2539904A4 (en) | 2018-01-10 |
CN102971805A (zh) | 2013-03-13 |
KR20130010471A (ko) | 2013-01-28 |
WO2011106730A3 (en) | 2011-12-01 |
US20140299359A1 (en) | 2014-10-09 |
US20150137049A1 (en) | 2015-05-21 |
EP2539904A2 (en) | 2013-01-02 |
CA2828468A1 (en) | 2011-09-01 |
AU2011220397A1 (en) | 2012-10-18 |
CN102971805B (zh) | 2016-08-24 |
WO2011106730A2 (en) | 2011-09-01 |
AU2011220397B2 (en) | 2015-09-03 |
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