JP6110319B2 - ナノ構造化物品 - Google Patents
ナノ構造化物品 Download PDFInfo
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- JP6110319B2 JP6110319B2 JP2013558042A JP2013558042A JP6110319B2 JP 6110319 B2 JP6110319 B2 JP 6110319B2 JP 2013558042 A JP2013558042 A JP 2013558042A JP 2013558042 A JP2013558042 A JP 2013558042A JP 6110319 B2 JP6110319 B2 JP 6110319B2
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- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000010702 perfluoropolyether Substances 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229920006126 semicrystalline polymer Polymers 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 238000000807 solvent casting Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- UWSYCPWEBZRZNJ-UHFFFAOYSA-N trimethoxy(2,4,4-trimethylpentyl)silane Chemical compound CO[Si](OC)(OC)CC(C)CC(C)(C)C UWSYCPWEBZRZNJ-UHFFFAOYSA-N 0.000 description 1
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 238000000489 vacuum metal deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
Images
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- G—PHYSICS
- G02—OPTICS
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- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/006—Anti-reflective coatings
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- C—CHEMISTRY; METALLURGY
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- G02B1/11—Anti-reflection coatings
- G02B1/118—Anti-reflection coatings having sub-optical wavelength surface structures designed to provide an enhanced transmittance, e.g. moth-eye structures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
- Y10T428/24364—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.] with transparent or protective coating
Description
本出願は2011年3月14日出願の米国特許仮出願第61/452430号の利益を主張するものであり、その開示の全容をここに援用するものである。
様々な電源が可能であるが、RF電力が好ましい。これは、適切に構成された通電された電極上に自己バイアスを形成するのに、周波数は十分高いが、得られるプラズマに定在波を作るには十分高くないためである。RF電力は、高出力(幅の広いウェブ又は基材、急速なウェブ速度)に対して測定可能である。RF電力が使用されるとき、電極上の負バイアスは、負自己バイアスであり、すなわち電極上に負バイアスを誘発するために使用される、別個の電源は必要ない。RF電力が好ましいため、本記載の残りはそのタイプについてのみ焦点を当てる。
第1主表面及び概して反対側の第2主表面を有する基材と、反対側の第1及び第2主表面を有する機能層とを提供することであって、機能層の第1主表面は基材の第1主表面上に配置される、ことと、
マトリックス材料及びマトリックス材料中のナノスケール分散相を含む、コーティング可能な組成物を、機能層の第1主表面上にコーティングすることと、
必要に応じてコーティングを乾燥させ(及び必要に応じて乾燥させたコーティングを硬化させ)、マトリックス及びマトリックス中のナノスケール分散相を含む物品を提供することと、
物品の第2主表面を反応性イオンエッチングに暴露することと、を含む方法により製造することができ、イオンエッチングは、
減圧容器中で円筒形の電極上に物品を配置すること、
既定の圧力にて(例:1ミリトール〜20ミリトール(0.13Pa〜2.67Pa)の範囲で)エッチングガスを減圧容器に導入すること、
円筒形の電極と対電極の間にプラズマ(例:酸素プラズマ)を生成すること、
円筒形の電極を回転させて、基材を移動させること、及び
コーティングを異方性エッチングして、ランダムナノ構造化異方性表面を提供することを含む。
第1主表面及び概して反対側の第2主表面を有する基材を提供することと、
マトリックス材料及び第1マトリックス材料中のナノスケール分散相を含む、コーティング可能な組成物を、基材の第1主表面上にコーティングすることと、
必要に応じてコーティングを乾燥させて(及び必要に応じて乾燥させたコーティングを硬化させて)、マトリックス及びマトリックス中のナノスケール分散相を含む物品を提供することと、
物品の主表面を反応性イオンエッチングに暴露することとを含む方法により製造することができ、イオンエッチングは、
減圧容器中で円筒形の電極上に物品を配置すること、
既定の圧力にて(例:1ミリトール〜20ミリトール(0.13Pa〜2.67Pa)の範囲で)エッチングガスを減圧容器に導入すること、
円筒形の電極と対電極の間にプラズマ(例:酸素プラズマ)を生成すること、
円筒形の電極を回転させて、基材を移動させること、及び
コーティングを異方性エッチングして、第1ランダムナノ構造化異方性表面を提供すること、及び
ランダムナノ構造化異方性表面上に機能層を配置することを含む。
1.第1主表面、及び概して反対側の第2主表面を有する基材と、第1主表面上の第1層とを含む物品であって、この第1層は第1ランダムナノ構造化表面を有し、この第1層は0.5マイクロメートルまで(一部の実施形態では0.4マイクロメートル、0.3マイクロメートル、0.25マイクロメートル、0.2マイクロメートル、0.1マイクロメートル、0.15マイクロメートル、又は更には0.075マイクロメートルまで)の平均厚さを有する。
以下の実施例において、手順1に対する参照は以下の操作を表す。処理されるポリマーフィルムは、図1に表される円筒形RIE装置内に配置された。より詳細には、ドラム電極の幅は42.5インチ(106.3cm)であり、かつターボ分子ポンプによりポンピングを実施した。当業者は、このことが、プラズマ加工において従来的に行なわれるよりも遥かに低い操作圧で、本装置が動作したことを意味するものと認識する。
手順2は、高分子フィルムのシートサンプルがドラム電極の縁部周囲に貼られたことを除き、手順1の説明と同じである。ドラムは一定速度で回転させられ、その後、特定の実施例において記載されるように、異なる時間の長さでプラズマ処理が行われた。
この手順の結果により、プラズマ処理された薄膜表面の平均反射率%(%R)の測定値が得られた。薄膜の1つのサンプルは、サンプルの裏側に黒いビニルテープ(Yamato International Corporation(Woodhaven,MI)から商標名「200−38」として得られる)を適用することによって調整された。この黒いテープは、ブラックテープとサンプルの間に捕捉された気泡が、確実にないようにするために、ローラーを用いて適用された。同じ黒いビニルテープを、似通った方法で透明のガラススライドに適用した。この透明のガラススライドの両面の反射率は、対照サンプルに単独で黒色ビニルテープのパーセント反射率を確率させるよう予め設定されていた。光学的に透明な接着剤を含む複合物品を測定するために、この手順が使用されたとき、複合物品が透明のガラススライドに最初に予め積層され、その後、黒いテープでガラス表面上に更に積層された。
平均%透過率及びヘイズの測定は、分光光度計(モデル9970;BYK Gardnerから商品名「BYK GARDNER TCS PLUS SPECTROPHOTOMETER」)を使用して測定された。
50wt%のシリカナノ粒子を含むトリメチロールプロパントリアクリレート(TMPTA)組成物(Hanse Chemie USA(Hilton Head Island,SC)から商品名「NANOCRYL C150」で入手)を、トリメチロールプロパントリアクリレート(Sartomer(Exton,PA)から商品名「SR351H」で入手)で希釈し、20wt%のシリカナノ粒子コーティング溶液を作製した。20wt%のシリカナノ粒子コーティング濃縮物を70/30のメチルエチルケトン(MEK)/メトキシルプロパノールを用いて更に希釈することで固形分2.5wt%のコーティング溶液を作製した。光開始剤(BASF Specialty Chemicals(Tarrytown,NY)から商品名「IRGACURE 184」で入手)を、以下の表1の配合に従って溶液に添加した。
干渉縞のない実施例1及び2からのサンプルは、手順1に従って反応性イオンエッチング(RIE)によって処理された。RIE後のサンプルは干渉縞がない。RIE後の平均反射率対処理時間は以下の表3に示す。
実施例7及び8は、固体コーティング含有量中のシリカナノ粒子が30wt%であったことを除き、実施例1の説明どおりに調製された。コーティング配合物の構成成分を以下の表4に示す。
干渉縞のない実施例7及び8からのサンプルは、手順1に従って反応性イオンエッチング(RIE)によって処理された。RIE後のサンプルは干渉縞がない。RIE後の平均反射率対処理時間は、以下の表6に示す(手順3を使用して測定した)。
400グラムのコロイド状5nmシリカ粒子(Nalco Chemical Co.(Naperville,IL)から、商品名「NALCO 2325」として得られる)が、1クオート(0.95リットル)ジャーに充填された。阻害剤濃度5重量%にて、水に、450グラムの1−メトキシ−2−プロパノール、27.82グラムの3−(メタクリロイルオキシ)プロピルトリメトキシシラン、及び0.23グラムのヒンダードアミン窒素酸化物阻害剤(Ciba Specialty Chemical,Inc.(Tarrytown,NY)から商品名「PROSTAB 5128」で入手)を一緒に混合し、撹拌しながら広口瓶に加えた。ジャーは密閉されて、80℃まで16時間にわたり加熱され、表面改質シリカ分散体を形成した。溶媒を回転蒸発によって混合物から除去し、44.3wt.%の固溶体を形成した。溶液は、10wt.%の5nm SiO2コーティングを形成するためにトリメチロールプロパントリアクリレート(「SR 351H」)と混合され、イソプロピルアルコール(IPA)と更に希釈され、以下の表7に示される組成物を有する2.5wt.%固体のコーティング溶液を形成した。
実施例11〜13のサンプルは、手順2に従って反応性イオンエッチング(RIE)によって処理された。RIE後のサンプルは干渉縞がない。RIE後の光学特性対処理時間を、以下の表9に示す(手順3及び4によって測定された)。
[1]
第1主表面、及び概して反対側の第2主表面を有する基材と、前記第1主表面上の第1層とを含む物品であって、前記第1層は第1ランダムナノ構造化表面を有し、前記第1層は0.5マイクロメートルまでの平均厚さを有する、物品。
[2]
前記第1層がマトリックス及びナノスケール分散相を含む、項目1に記載の物品。
[3]
前記マトリックスが高分子マトリックスである、項目2に記載の物品。
[4]
前記第1層が0.15マイクロメートルまでの平均厚さを有する、項目1〜3のいずれか一項に記載の物品。
[5]
前記第1ランダムナノ構造化表面が異方性である、項目1〜4のいずれか一項に記載の物品。
[6]
前記第1ランダムナノ構造化異方性表面が、1%未満の反射率(%)を有する、項目5に記載の物品。
[7]
前記基材の前記第1主表面と前記第1層の間に配置された機能層を更に含み、前記機能層が、透明な導電層又はガスバリア層のうちの少なくとも1つである、項目1〜6のいずれか一項に記載の物品。
[8]
前記第1ランダムナノ構造化表面上に配置された機能層を更に含み、前記機能層が、透明な導電層又はガスバリア層のうちの少なくとも1つである、項目1〜6のいずれか一項に記載の物品。
[9]
前記基材の前記第2主表面上に第2層を更に含み、前記第2層がランダムナノ構造化表面を有し、前記第2層が0.5マイクロメートルまでの平均厚さを有する、項目1〜8のいずれか一項に記載の物品。
[10]
前記基材の前記第2主表面と前記第2層の間に配置された機能層を更に含み、前記機能層が透明な導電層又はガスバリア層のうちの少なくとも1つである、項目9に記載の物品。
[11]
前記第2ランダムナノ構造化表面上に配置された機能層を更に含み、前記機能層が透明な導電層又はガスバリア層のうちの少なくとも1つである、項目9に記載の物品。
Claims (6)
- 第1主表面、及び概して反対側の第2主表面を有する基材と、前記第1主表面上の第1層とを含む物品であって、前記第1層は第1ランダム異方性ナノ構造化表面を有し、前記第1ランダム異方性ナノ構造化表面は、幅に対する高さの比率が2以上であるナノ形体を有し、前記ナノ形体は、前記第1主表面に垂直であり、前記第1層は0.5マイクロメートルまでの平均厚さを有する、物品。
- 前記第1層がマトリックス及びナノスケール分散相を含む、請求項1に記載の物品。
- 前記マトリックスが高分子マトリックスである、請求項2に記載の物品。
- 前記ナノ形体の幅に対する高さの比率が5以上である、請求項1〜3のいずれか一項に記載の物品。
- 前記基材の前記第1主表面と前記第1層の間に配置された機能層を更に含み、前記機能層が、透明な導電層又はガスバリア層のうちの少なくとも1つである、請求項1〜4のいずれか一項に記載の物品。
- 前記第1ランダム異方性ナノ構造化表面上に配置された機能層を更に含み、前記機能層が、透明な導電層又はガスバリア層のうちの少なくとも1つである、請求項1〜4のいずれか一項に記載の物品。
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EP (1) | EP2686389B1 (ja) |
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JP2014509967A (ja) | 2014-04-24 |
CN103443211A (zh) | 2013-12-11 |
BR112013023128A2 (pt) | 2019-09-24 |
KR20140013028A (ko) | 2014-02-04 |
EP2686389B1 (en) | 2016-08-10 |
US9435924B2 (en) | 2016-09-06 |
KR101943671B1 (ko) | 2019-01-29 |
US20130344290A1 (en) | 2013-12-26 |
CN106865493A (zh) | 2017-06-20 |
CN106865493B (zh) | 2019-06-07 |
EP2686389A1 (en) | 2014-01-22 |
CN103443211B (zh) | 2016-12-14 |
WO2012125324A1 (en) | 2012-09-20 |
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