JPWO2013002026A1 - ガスバリア性フィルム、ガスバリア性フィルムの製造方法、および電子デバイス - Google Patents
ガスバリア性フィルム、ガスバリア性フィルムの製造方法、および電子デバイス Download PDFInfo
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- JPWO2013002026A1 JPWO2013002026A1 JP2013522575A JP2013522575A JPWO2013002026A1 JP WO2013002026 A1 JPWO2013002026 A1 JP WO2013002026A1 JP 2013522575 A JP2013522575 A JP 2013522575A JP 2013522575 A JP2013522575 A JP 2013522575A JP WO2013002026 A1 JPWO2013002026 A1 JP WO2013002026A1
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- 239000013076 target substance Substances 0.000 description 1
- 125000004213 tert-butoxy group Chemical group [H]C([H])([H])C(O*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 125000001981 tert-butyldimethylsilyl group Chemical group [H]C([H])([H])[Si]([H])(C([H])([H])[H])[*]C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000000037 tert-butyldiphenylsilyl group Chemical group [H]C1=C([H])C([H])=C([H])C([H])=C1[Si]([H])([*]C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- IFLREYGFSNHWGE-UHFFFAOYSA-N tetracene Chemical compound C1=CC=CC2=CC3=CC4=CC=CC=C4C=C3C=C21 IFLREYGFSNHWGE-UHFFFAOYSA-N 0.000 description 1
- 125000001935 tetracenyl group Chemical group C1(=CC=CC2=CC3=CC4=CC=CC=C4C=C3C=C12)* 0.000 description 1
- VELSFHQDWXAPNK-UHFFFAOYSA-N tetracontacyclo[25.6.5.516,28.44,32.35,11.321,34.28,10.212,15.222,35.229,31.113,20.124,38.02,6.014,19.017,25.018,23.030,37.033,36.547,54.446,53.448,58.126,51.150,52.03,45.07,42.09,61.039,40.041,43.044,63.049,76.055,78.056,62.057,68.059,64.060,67.065,69.066,71.070,73.072,75.074,77]octaheptaconta-1,3(45),4(48),5(61),6,8,10,12,14,16,18,20,22,24(39),25,27(38),28,30,32,34(42),35(40),36,41(43),44(63),46,49(76),50(77),51,53,55(78),56(62),57,59,64,66,68,70(73),71,74-nonatriacontaene Chemical compound c12c3c4c5c6c1c1c7c8c2c2c3c3c9c4c4c5c5c%10c%11c%12c%13c%14c%15c%12c%12c%16c%17c%18c%19c%20c%21c%17c%17c%22c%21c%21c%23c%20c%20c%19c%19c%24c%18c%16c%15c%15c%24c%16c(c7c%15c%14c1c6c5%13)c8c1c2c2c3c3c(c%21c5c%22c(c%11c%12%17)c%10c4c5c93)c%23c2c%20c1c%19%16 VELSFHQDWXAPNK-UHFFFAOYSA-N 0.000 description 1
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- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
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- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
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- YZVRVDPMGYFCGL-UHFFFAOYSA-N triacetyloxysilyl acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)OC(C)=O YZVRVDPMGYFCGL-UHFFFAOYSA-N 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- 125000000025 triisopropylsilyl group Chemical group C(C)(C)[Si](C(C)C)(C(C)C)* 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- CDGIKLPUDRGJQN-UHFFFAOYSA-N trimethyl(octoxy)silane Chemical compound CCCCCCCCO[Si](C)(C)C CDGIKLPUDRGJQN-UHFFFAOYSA-N 0.000 description 1
- KXFSUVJPEQYUGN-UHFFFAOYSA-N trimethyl(phenyl)silane Chemical compound C[Si](C)(C)C1=CC=CC=C1 KXFSUVJPEQYUGN-UHFFFAOYSA-N 0.000 description 1
- VFFKJOXNCSJSAQ-UHFFFAOYSA-N trimethylsilyl benzoate Chemical compound C[Si](C)(C)OC(=O)C1=CC=CC=C1 VFFKJOXNCSJSAQ-UHFFFAOYSA-N 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000003960 triphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C3=CC=CC=C3C12)* 0.000 description 1
- PKRKCDBTXBGLKV-UHFFFAOYSA-N tris(ethenyl)-methylsilane Chemical compound C=C[Si](C)(C=C)C=C PKRKCDBTXBGLKV-UHFFFAOYSA-N 0.000 description 1
- FUJPAQRDHMJPBB-UHFFFAOYSA-N tris(ethenyl)-phenylsilane Chemical compound C=C[Si](C=C)(C=C)C1=CC=CC=C1 FUJPAQRDHMJPBB-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
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- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0203—Containers; Encapsulations, e.g. encapsulation of photodiodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
- B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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Abstract
Description
(A)ガスバリア層の組成をSiOwNxで表したときに、w≧0.8、x≧0.3、2w+3x≦4である。
(B)ガスバリア層の組成をSiOyNzで表したときに、0<y≦0.55、z≧0.55、2y+3z≦4である。
(A)ガスバリア層の組成をSiOwNxで表したときに、w≧0.8、x≧0.3、2w+3x≦4である。
(B)ガスバリア層の組成をSiOyNzで表したときに、0<y≦0.55、z≧0.55、2y+3z≦4である。
本発明のガスバリア性フィルムは、基材の少なくとも一方の面側に、SiとOとNとを含有する酸化窒化珪素からなるガスバリア層を有し、ガスバリア層が、厚さ方向に少なくとも2種の組成範囲を有する領域に分かれており、基材に近い側に上記(A)の組成範囲を有するSiOwNx領域が連続して20nm以上存在し、基材から遠い側に上記(B)の組成範囲を有するSiOyNz領域が連続して50nm以上存在することを特徴とする。上記以外のガスバリア層を厚さ方向の任意の位置に形成してガスバリア性を更に向上させることもできる。また、基材の両面に、上記のガスバリア層を形成させた構成であっても良い。
本発明に用いられる基材は、長尺な支持体であって、後述のガスバリア性(単に「バリア性」ともいう)を有するガスバリア層(単に「バリア層」ともいう)を保持することができるもので、下記のような材料で形成されるが、特にこれらに限定されるものではない。
本発明のガスバリア性フィルムにおいては、各機能を有する各種の中間層を設けることができる。
本発明に係る基材の塗膜(ガスバリア層)を形成する側の表面には、ガスバリア層との密着性の向上を目的として、アンカーコート層を形成してもよい。
本発明のガスバリア性フィルムにおいては、基材とガスバリア層との間に、平滑層を有してもよい。本発明に用いられる平滑層は突起等が存在する透明樹脂フィルム支持体の粗面を平坦化し、あるいは、透明樹脂フィルム支持体に存在する突起により透明無機化合物層に生じた凹凸やピンホールを埋めて平坦化するために設けられる。このような平滑層は、基本的には感光性材料、または、熱硬化性材料を硬化させて作製される。
本発明のガスバリア性フィルムは、上記平滑層を設けた面とは反対側の基材面にブリードアウト防止層を有してもよい。
本発明では、少なくともSiとOとNとを含有するガスバリア層(以下、単にガスバリア層またはバリア層とする)が2層以上存在する。ガスバリア層が2層以上存在すると、ガスバリア性が大きく向上する点で有利である。
本発明に係るガスバリア層は、ポリシラザンを含む溶液を塗布して形成した層(ポリシラザンを含有する層)に真空紫外線照射を施して形成されることが好ましい。
本発明において、好ましい改質(ポリシラザンの酸化窒化珪素への転化)方法は、真空紫外線照射による処理である。本発明に係るガスバリア層は、ポリシラザンを含む溶液を塗布して形成した層に、真空紫外線を照射することにより形成されることが好ましい。真空紫外線照射による処理は、ポリシラザン内の原子間結合力より大きい100〜200nmの光エネルギーを用い、好ましくは100〜180nmの波長の光(VUV)のエネルギーを用い、原子の結合を光量子プロセスと呼ばれる光子のみの作用により、直接切断しながら脱水素によるSi−N結合の形成や、活性酸素やオゾンによる酸化反応を進行させることで、比較的低温で、酸化窒化珪素膜の形成を行うことができる。この工程で、ポリシラザンの少なくとも一部が酸化窒化珪素へと改質され、層の厚さ方向の部分的領域として、前述のSiOwNxの組成で示されるガスバリア層や、SiOyNzの組成で示されるガスバリア層が形成される。ここで、水素と炭素が存在する場合でもこの組成式では示されないが、良好なガスバリア性を得るためには、ガスバリア層中には、炭素原子は実質的に存在しないことが好ましく、ガスバリア層の安定性を高めるためには、水素原子は少ない方が好ましい。
パーヒドロポリシラザン中のSi−H結合やN−H結合は真空紫外線照射による励起等で比較的容易に切断され、不活性雰囲気下ではSi−Nとして再結合すると考えられる(Siの未結合手が形成される場合もある)。すなわち、酸化することなくSiNy組成として硬化する。この場合はポリマー主鎖の切断は生じない。Si−H結合やN−H結合の切断は触媒の存在や、加熱によって促進される。切断されたHはH2として膜外に放出される。
パーヒドロポリシラザン中のSi−N結合は水により加水分解され、ポリマー主鎖が切断されてSi−OHを形成する。二つのSi−OHが脱水縮合してSi−O−Si結合を形成して硬化する。これは大気中でも生じる反応であるが、不活性雰囲気下での真空紫外線照射中では、照射の熱によって基材からアウトガスとして生じる水蒸気が主な水分源となると考えられる。水分が過剰となると脱水縮合しきれないSi−OHが残存し、SiO2.1〜SiO2.5の組成で示されるガスバリア性の低い硬化膜となる。
真空紫外線照射中、雰囲気下に適当量の酸素が存在すると、酸化力の非常に強い一重項酸素が形成される。パーヒドロポリシラザン中のHやNはOと置き換わってSi−O−Si結合を形成して硬化する。ポリマー主鎖の切断により結合の組み換えを生じる場合もあると考えられる。
真空紫外線のエネルギーはパーヒドロポリシラザン中のSi−Nの結合エネルギーよりも高いため、Si−N結合は切断され、周囲に酸素源(酸素、オゾン、水等)が存在すると酸化されてSi−O−Si結合(場合によってはSi−O−N結合)を生じると考えられる。ポリマー主鎖の切断により結合の組み換えを生じる場合もあると考えられる。
・装置:アルバックファイ製QUANTERASXM
・X線源:単色化Al−Kα
・測定領域:Si2p、C1s、N1s、O1s
・スパッタイオン:Ar(2keV)
・デプスプロファイル:1分間スパッタ後、測定を繰り返す
・定量:バックグラウンドをShirley法で求め、得られたピーク面積から相対感度係数法を用いて定量した。データ処理は、アルバックファイ社製のMultiPakを用いた。
本発明においては、SiとOとNとを含有する酸化窒化珪素からなるガスバリア層が、厚さ方向に少なくとも2種の組成範囲を有する領域に分かれており、ガスバリア層のいずれかに下記(A)の組成範囲を有するSiOwNx領域が連続して20nm以上の厚さで存在する。そして、(B)の組成範囲を有するSiOyNz領域よりも基材側に存在する。(A)ガスバリア層の組成をSiOwNxで表したときに、w≧0.8、x≧0.3、2w+3x≦4である。ここで、上記関係から、wの上限は、1.55であり、xの上限は、0.8である。
本発明においては、SiとOとNとを含有する酸化窒化珪素からなるガスバリア層が、厚さ方向に少なくとも2種の組成範囲を有する領域に分かれており、(A)の組成範囲を有するSiOwNx領域に比べて基材から遠い側に、下記(B)の組成範囲を有するSiOyNz領域が連続して50nm以上の厚さで存在する。(B)ガスバリア層の組成をSiOyNzで表したときに、0<y≦0.55、z≧0.55、2y+3z≦4である。
e+Xe→Xe*
Xe*+2Xe→Xe2 *+Xe
Xe2 *→Xe+Xe+hν(172nm)
となり、励起されたエキシマ分子であるXe2 *が基底状態に遷移するときに172nmのエキシマ光を発光する。
紫外線照射時の反応には、酸素が必要であるが、真空紫外線は、酸素による吸収があるため紫外線照射工程での効率を低下しやすいため、真空紫外線の照射は、できるだけ酸素濃度の低い状態で、行うことが好ましい。
本発明に係るガスバリア層上には、オーバーコート層を設けてもよい。
オーバーコート層に用いられる有機物としては、有機モノマー、オリゴマー、ポリマー等の有機樹脂を好ましく用いることができる。これらの有機樹脂は重合性基や架橋性基を有することが好ましく、これらの有機樹脂を含有し、必要に応じて重合開始剤や架橋剤等を含有する有機樹脂組成物塗布液から塗布形成した層に、光照射処理や熱処理を加えて硬化させることが好ましい。ここで「架橋性基」とは、光照射処理や熱処理で起こる化学反応によりバインダーポリマーを架橋することができる基のことである。このような機能を有する基であれば特にその化学構造は限定されないが、例えば、付加重合し得る官能基としてエチレン性不飽和基、エポキシ基/オキセタニル基等の環状エーテル基が挙げられる。また光照射によりラジカルになり得る官能基であってもよく、そのような架橋性基としては、例えば、チオール基、ハロゲン原子、オニウム塩構造等が挙げられる。中でも、エチレン性不飽和基が好ましく、特開2007−17948号公報の段落0130〜0139に記載された官能基が含まれる。
本発明のガスバリア性フィルムは、主に電子デバイス等のパッケージ、又は有機EL素子や太陽電池、液晶等のプラスチック基板といったディスプレイ材料に用いられるガスバリア性フィルム及びガスバリア性フィルムを用いた各種デバイス用樹脂基材、及び各種デバイス素子に適用することができる。
本発明に係る有機光電変換素子は、本発明のガスバリア性フィルムを具備するが、有機光電変換素子に用いる際には、ガスバリア性フィルムは透明であることが好ましく、このガスバリア性フィルムを基材(支持体ともいう。)として用い、この面側から太陽光の受光を行うように構成できる。
有機光電変換素子及び太陽電池の好ましい態様を説明する。なお、以下、本発明に係る有機光電変換素子の好ましい態様について詳細に説明するが、当該太陽電池は当該有機光電変換素子をその構成として有するものであり、太陽電池の好ましい構成も同様に記載することができる。
(ii)陽極/正孔輸送層/発電層/陰極
(iii)陽極/正孔輸送層/発電層/電子輸送層/陰極
(iv)陽極/正孔輸送層/p型半導体層/発電層/n型半導体層/電子輸送層/陰極
(v)陽極/正孔輸送層/第1発電層/電子輸送層/中間電極/正孔輸送層/第2発電層/電子輸送層/陰極。
有機光電変換素子の発電層(「光電変換層」ともいう)の形成に用いられる材料について説明する。
有機光電変換素子の発電層(バルクへテロジャンクション層)として好ましく用いられるp型半導体材料としては、種々の縮合多環芳香族低分子化合物や共役系ポリマー・オリゴマーが挙げられる。
バルクへテロジャンクション層に用いられるn型半導体材料としては特に限定されないが、例えば、フラーレン、オクタアザポルフィリン等、p型半導体の水素原子をフッ素原子に置換したパーフルオロ体(パーフルオロペンタセンやパーフルオロフタロシアニン等)、ナフタレンテトラカルボン酸無水物、ナフタレンテトラカルボン酸ジイミド、ペリレンテトラカルボン酸無水物、ペリレンテトラカルボン酸ジイミド等の芳香族カルボン酸無水物や、そのイミド化物を骨格として含む高分子化合物等を挙げることができる。
本発明に係る有機光電変換素子は、バルクへテロジャンクション層と陽極との中間には正孔輸送層を、バルクへテロジャンクション層で発生した電荷をより効率的に取り出すことが可能となるため、これらの層を有していることが好ましい。
本発明に係る有機光電変換素子は、バルクへテロジャンクション層と陰極との中間には電子輸送層を作製することで、バルクへテロジャンクション層で発生した電荷をより効率的に取り出すことが可能となるため、これらの層を有していることが好ましい。
エネルギー変換効率の向上や、素子寿命の向上を目的に、各種中間層を素子内に有する構成としてもよい。中間層の例としては、正孔ブロック層、電子ブロック層、正孔注入層、電子注入層、励起子ブロック層、UV吸収層、光反射層、波長変換層等を挙げることができる。
透明電極は、陰極、陽極は特に限定せず、素子構成により選択することができるが、好ましくは透明電極を陽極として用いることである。例えば、陽極として用いる場合、好ましくは380〜800nmの光を透過する電極である。
対電極は導電材単独層であってもよいが、導電性を有する材料に加えて、これらを保持する樹脂を併用してもよい。対電極の導電材としては、仕事関数の小さい(4eV以下)金属、合金、電気伝導性化合物及びこれらの混合物を電極物質とするものが用いられる。
また、前記有機光電変換素子の層構成の(v)のようなタンデム構成の場合に必要となる中間電極の材料としては、透明性と導電性を併せ持つ化合物を用いた層であることが好ましく、前記透明電極で用いたような材料(ITO、AZO、FTO、酸化チタン等の透明金属酸化物、Ag、Al、Au等の非常に薄い金属層又はナノ粒子・ナノワイヤーを含有する層、PEDOT:PSS、ポリアニリン等の導電性高分子材料等)を用いることができる。
導電性繊維としては、金属でコーティングした有機繊維や無機繊維、導電性金属酸化物繊維、金属ナノワイヤー、炭素繊維、カーボンナノチューブ等を用いることができるが、金属ナノワイヤーが好ましい。
有機光電変換素子は、太陽光のより効率的な受光を目的として、各種の光学機能層を有していてもよい。光学機能層としては、例えば、反射防止層、マイクロレンズアレイ等の集光層、陰極で反射した光を散乱させて再度発電層に入射させることができるような光拡散層等を設けてもよい。
電子受容体と電子供与体とが混合されたバルクヘテロジャンクション層、及び輸送層・電極の作製方法としては、蒸着法、塗布法(キャスト法、スピンコート法を含む)等を例示することができる。このうち、バルクへテロジャンクション層の作製方法としては、蒸着法、塗布法(キャスト法、スピンコート法を含む)等を例示することができる。
電極、発電層、正孔輸送層、電子輸送層等をパターニングする方法やプロセスには特に制限はなく、公知の手法を適宜適用することができる。
《基材の作製》
〔基材(ア)の作製〕
熱可塑性樹脂基材(支持体)として、両面に易接着加工された厚さ125μmのポリエステルフィルム(帝人デュポンフィルム株式会社製、極低熱収PET Q83)を用い、下記に示すように、片面にブリードアウト防止層を、反対面に平滑層を形成したものを基材(ア)とした。
上記熱可塑性樹脂基材の一方の面側に、JSR株式会社製のUV硬化型有機/無機ハイブリッドハードコート材 OPSTAR Z7535を、乾燥後の膜厚が4.0μmになる条件で塗布した後、硬化条件として、照射エネルギー量1.0J/cm2で、空気雰囲気下、高圧水銀ランプを使用し、乾燥条件80℃で、3分間の硬化処理を行い、ブリードアウト防止層を形成した。
次いで、上記熱可塑性樹脂基材のブリードアウト防止層を形成した面とは反対側の面側に、JSR株式会社製のUV硬化型有機/無機ハイブリッドハードコート材 OPSTAR Z7501を、乾燥後の膜厚が4.0μmになる条件で塗布した後、80℃で、3分間乾燥した後、空気雰囲気下、高圧水銀ランプを使用し、硬化条件として、照射エネルギー量1.0J/cm2で照射、硬化して、平滑層1を形成した。
耐熱性基材として、両面に易接着加工が施された200μm厚みの透明ポリイミド系フィルム(三菱瓦斯化学株式会社製、ネオプリムL)を用い、下記に示すように、基材の両面に平滑層を形成したものを、基材(イ)とした。
〈平滑層2の塗布液の作製〉
トリメチロールプロパントリグリシジルエーテル(エポライト100MF 共栄社化学社製)を8.0g、エチレングリコールジグリシジルエーテル(エポライト40E 共栄社化学社製)を5.0g、オキセタニル基を有するシルセスキオキサン:OX−SQ−H(東亞合成社製)を12.0g、3−グリシドキシプロピルトリメトキシシランを32.5g、Al(III)アセチルアセトネートを2.2g、メタノールシリカゾル(日産化学社製、固形分濃度30質量%)を134.0g、BYK333(ビックケミー・ジャパン社製、シリコン系界面活性剤)を0.1g、ブチルセロソルブを125.0g、0.1モル/Lの塩酸水溶液を15.0g混合し、充分に攪拌した。これを室温でさらに静置脱気して、平滑層塗布液を得た。
上記耐熱性基材の一方の面側に、定法によりコロナ放電処理を施した後、上記平滑層塗布液を、乾燥後の膜厚が4.0μmとなる条件で塗布した後、80℃で3分間乾燥した。更に、120℃で10分間の加熱処理を施して、平滑層2を形成した。
上記耐熱性基材の平滑層2を形成した面とは反対側の面に、上記平滑層2の形成方法と同様にして、平滑層3を形成した。
上記基材(イ)の作製において、耐熱性基材である両面に易接着加工が施された200μm厚みの透明ポリイミド系フィルム(三菱瓦斯化学株式会社製、ネオプリムL)に代えて、耐熱性基材として、有機無機ハイブリッド構造を有するシルセスキオキサンを基本骨格としたフィルムである、100μm厚の新日鐵化学社製のシルプラスH100を用いた以外は同様にして、基材(ウ)を作製した。なお、基材(ウ)の平滑層2及び平滑層3の表面粗さを同様にして測定した結果、Rzは約20nmであった。
表1に示す基材種、層構成、真空紫外線照射処理条件により、複数層からなるガスバリア層を塗設した後に形成し、ガスバリア性フィルム1〜11を作製した。なお、表中の層構成は、基材に近い方のガスバリア層を第1層として記した。
(ポリシラザン層の形成)
対象とする基材、あるいは、下層となるガスバリア層上に、下記ポリシラザン化合物を含有する塗布液を、スピンコーターを用いて、乾燥後の膜厚がそれぞれ設定膜厚となる条件で塗布した。乾燥条件は、100℃で2分とした。
無触媒のパーヒドロポリシラザンを20質量%含むジブチルエーテル溶液(AZエレクトロニックマテリアルズ(株)製アクアミカ NN120−20)と、アミン触媒としてN,N,N’,N’−テトラメチル−1,6−ジアミノヘキサンを固形分で5質量%含有
するパーヒドロポリシラザンの20質量%ジブチルエーテル溶液(AZエレクトロニックマテリアルズ(株)製アクアミカ NAX120−20)を混合して用い、アミン触媒を固形分として1質量%(パーヒドロポリシラザンに対して)になるように調整した後、さらに必要があればジブチルエーテルで希釈することにより、総固形分量が2質量%〜20質量%のジブチルエーテル溶液として、ポリシラザン化合物含有塗布液を調製した。これらをポリシラザン層の設定膜厚に応じて適宜用いた。
上記の様にしてポリシラザン層塗膜を形成した後、下記の方法に従って、真空紫外線照射処理を施して、各ガスバリア層を形成した。それぞれの層に施した各処理条件の詳細は表1に示した。表中、酸素濃度は、ガスバリア層を形成した後、真空紫外線照射工程で真空紫外線を照射する際の酸素濃度を表している。この濃度や試料ステージ温度、積算照射エネルギーを制御すること、および、薄層のポリシラザン層を多層積層することでガスバリア層の組成を変化させた。
図1は真空紫外線照射装置の断面模式図である。真空紫外線照射は、この装置を用いて行った。
〔ガスバリア性フィルム12の作製〕
真空プラズマCVD装置を用いて、基材(ア)の平滑層表面上へ第1層のガスバリア層の形成を行った。この時、使用した高周波電源は、27.12MHzの高周波電源で、電極間距離は20mmとした。原料ガスとして、シランガスを流量として7.5sccm、アンモニアガスを流量として50sccm、水素ガスを流量として200sccmの条件で真空チャンバー内へ導入し、次いで、成膜開始時にフィルム基板温度を100℃とし、成膜時のガス圧を30Paに設定して窒化珪素を主成分とするガスバリア層を100nmの膜厚で形成し、ガスバリア性フィルム12を得た。
上記のガスバリア性フィルム12において、原料ガスとして、シランガスを流量として7.5sccm、アンモニアガスを流量として100sccm、亜酸化窒素ガスを流量として50sccmの条件で真空チャンバー内へ導入し、次いで、成膜開始時にフィルム基板温度を100℃とし、成膜時のガス圧を100Paに設定して酸化窒化珪素を主成分とするガスバリア層を200nmの膜厚で形成した以外は同様にして、ガスバリア性フィルム13を得た。
上記作製したガスバリア性フィルム1〜13について、ガスバリア層の厚さ方向の組成分布を、XPS分析を用いた方法で測定して求めた。その際、前述のような厚さ方向の補正を行った。
・装置:アルバックファイ製QUANTERASXM
・X線源:単色化Al−Kα
・測定領域:Si2p、C1s、N1s、O1s
・スパッタイオン:Ar(2keV)
・デプスプロファイル:1分間スパッタ後、測定を繰り返す
※SiO2換算のエッチングレートで厚さ約5nmに相当
・定量:バックグラウンドをShirley法で求め、得られたピーク面積から相対感度係数法を用いて定量した。データ処理は、アルバックファイ社製のMultiPakを用いた。
※SiOwNx領域が複数ある場合は、その最大厚さを有する領域の厚さとした。
※SiOyNz領域が複数ある場合は、その最大厚さを有する領域の厚さとした。
(水蒸気バリア性評価試料の作製装置)
蒸着装置:日本電子(株)製真空蒸着装置JEE−400
恒温恒湿度オーブン:ヤマト科学株式会社製、Yamato Humidic ChamberIG47M
(原材料)
水分と反応して腐食する金属:カルシウム(粒状)
水蒸気不透過性の金属:アルミニウム(φ3〜5mm、粒状)
(水蒸気バリア性評価試料の作製)
真空蒸着装置(日本電子(株)製真空蒸着装置 JEE−400)を用い、作製したガスバリア性フィルムのガスバリア層表面に、マスクを通して12mm×12mmのサイズで金属カルシウムを蒸着させた。この際、蒸着膜厚は、80nmとなるようにした。
△:金属カルシウムが腐食した面積が1.0%以上、5.0%未満である
×:金属カルシウムが腐食した面積が、5.0%以上である
《評価2:フレキシブル性の評価》
各ガスバリア性フィルムについて、20mmΦ相当の往復曲げを100回繰り返した。この際、ガスバリア性フィルムのガスバリア層表面には部材が接触しないように保持した。次いで、上記評価1の水蒸気バリア性の評価と同様にして、水蒸気バリア性評価を行った。
各ガスバリア性フィルムについて、目視により透明性の評価を行った。着色が認められないレベルを○、やや着色が認められるレベルを△、明らかに着色しているレベルを×とした。
上記作製したガスバリア性フィルム10、11について、220℃で10分間の大気雰囲気下で加熱処理を施した。この際、ガスバリア性フィルムのガスバリア層表面には部材が接触しないように保持した。加熱処理後、室温の大気中に取り出し、そのまま室温まで冷却した。次いで、上記評価1の水蒸気バリア性の評価と同様にして、水蒸気バリア性評価を行った。結果は加熱処理しない場合と同様で良好であった。このように、本発明のガスバリア性フィルムは、耐熱性に優れ、かつ、非常に高いバリア性を有することが分かる。
《有機薄膜電子デバイスの作製》
実施例1で作製したガスバリア性フィルム1〜13を封止フィルムとして用いて、有機薄膜電子デバイスである有機EL素子1〜13をそれぞれ作製した。
(第1電極層の形成)
各ガスバリア性フィルムのガスバリア層上に、厚さ150nmのITO(インジウムチンオキシド)をスパッタ法により成膜し、フォトリソグラフィー法によりパターニングを行い、第1電極層を形成した。なお、パターンは発光面積が50mm平方になるようなパターンとした。
第1電極層が形成された各ガスバリア性フィルムの第1電極層の上に、以下に示す正孔輸送層形成用塗布液を押出し塗布機で塗布した後、乾燥し正孔輸送層を形成した。正孔輸送層形成用塗布液は乾燥後の厚みが50nmになるように塗布した。
塗布工程は大気中、25℃相対湿度50%の環境で行った。
ポリエチレンジオキシチオフェン・ポリスチレンスルホネート(PEDOT/PSS、Bayer社製 Baytron P AI 4083)を純水で65%、メタノール5%で希釈した溶液を正孔輸送層形成用塗布液として準備した。
正孔輸送層形成用塗布液を塗布した後、成膜面に向け高さ100mm、吐出風速1m/s、幅手の風速分布5%、温度100℃で溶媒を除去した後、引き続き、加熱処理装置を用い温度150℃で裏面伝熱方式の熱処理を行い、正孔輸送層を形成した。
引き続き、正孔輸送層まで形成した各ガスバリア性フィルムの正孔輸送層上に、以下に示す白色発光層形成用塗布液を押出し塗布機で塗布した後、乾燥し発光層を形成した。白色発光層形成用塗布液は乾燥後の厚みが40nmになるように塗布した。
ホスト材のH−Aを1.0gと、ドーパント材D−Aを100mg、ドーパント材D−Bを0.2mg、ドーパント材D−Cを0.2mg、100gのトルエンに溶解し白色発光層形成用塗布液として準備した。なお、上記ホスト材のH−A、ドーパント材D−A、ドーパント材D−B及びドーパント材D−Cは、それぞれ、下記構造を有する。
塗布工程を窒素ガス濃度99%以上の雰囲気で、塗布温度を25℃とし、塗布速度1m/minで行った。
白色発光層形成用塗布液を塗布した後、成膜面に向け高さ100mm、吐出風速1m/s、幅手の風速分布5%、温度60℃で溶媒を除去した後、引き続き、温度130℃で加熱処理を行い、発光層を形成した。
引き続き、発光層まで形成したのち、以下に示す電子輸送層形成用塗布液を押出し塗布機で塗布した後、乾燥し電子輸送層を形成した。電子輸送層形成用塗布液は乾燥後の厚みが30nmになるように塗布した。
塗布工程は窒素ガス濃度99%以上の雰囲気で、電子輸送層形成用塗布液の塗布温度を25℃とし、塗布速度1m/minで行った。
電子輸送層はE−Aを2,2,3,3−テトラフルオロ−1−プロパノール中に溶解し0.5質量%溶液とし電子輸送層形成用塗布液とした。
電子輸送層形成用塗布液を塗布した後、成膜面に向け高さ100mm、吐出風速1m/s、幅手の風速分布5%、温度60℃で溶媒を除去した後、引き続き、加熱処理部で、温度200℃で加熱処理を行い、電子輸送層を形成した。
引き続き、形成された電子輸送層上に電子注入層を形成した。まず、基板を減圧チャンバーに投入し、5×10-4Paまで減圧した。あらかじめ、真空チャンバーにタンタル製蒸着ボートに用意しておいたフッ化セシウムを加熱し、厚さ3nmの電子注入層を形成した。
引き続き、形成された電子注入層の上に5×10-4Paの真空下にて第2電極形成材料としてアルミニウムを使用し、取り出し電極を有するように蒸着法にて、発光面積が50mm平方になるようにマスクパターン成膜し、厚さ100nmの第2電極を積層した。
第2電極まで形成した各ガスバリア性フィルムを、再び窒素雰囲気に移動し、規定の大きさに、紫外線レーザーを用いて裁断し、有機EL素子を作製した。
作製した有機EL素子に、ソニーケミカル&インフォメーションデバイス株式会社製の異方性導電フィルムDP3232S9を用いて、フレキシブルプリント基板(ベースフィルム:ポリイミド12.5μm、圧延銅箔18μm、カバーレイ:ポリイミド12.5μm、表面処理NiAuメッキ)を接続した。
電極リード(フレキシブルプリント基板)を接続した有機EL素子を、市販のロールラミネート装置を用いて封止部材を接着し、有機EL素子1〜13を製作した。
ジシアンジアミド(DICY)
エポキシアダクト系硬化促進剤
しかる後、封止基板を、取り出し電極および電極リードの接合部を覆うようにして密着・配置して、圧着ロールを用いて圧着条件、圧着ロール温度120℃、圧力0.5MPa、装置速度0.3m/minで密着封止した。
上記作製した有機EL素子1〜13について、下記の方法に従って、耐久性の評価を行った。
(加速劣化処理)
上記作製した各有機EL素子を、60℃、90%RHの環境下で400時間の加速劣化処理を施した後、加速劣化処理を施していない有機EL素子と共に、下記の黒点に関する評価を行い、耐久性を評価した。
加速劣化処理を施した有機EL素子及び加速劣化処理を施していない有機EL素子に対し、それぞれ1mA/cm2の電流を印加し、24時間連続発光させた後、100倍のマイクロスコープ(株式会社モリテックス製MS−804、レンズMP−ZE25−200)でパネルの一部分を拡大し、撮影を行った。撮影画像を2mm四方に切り抜き、黒点の発生面積比率を求め、下式に従って素子劣化耐性率を算出し、下記の基準に従って耐久性を評価した。評価ランクが、◎、○であれば、実用上好ましい特性であると判定した。
◎:素子劣化耐性率が、90%以上である
○:素子劣化耐性率が、60%以上、90%未満である
△:素子劣化耐性率が、20%以上、60%未満である
×:素子劣化耐性率が、20%未満である
以上により得られた結果を、表3に示す。
本出願は、2011年6月27日に出願された日本特許出願番号2011−141490号に基づいており、その開示内容は、参照され、全体として、組み入れられている。
Claims (6)
- 基材上に、少なくともSiとOとNとを含有するガスバリア層が2層以上積層されたガスバリア性フィルムにおいて、ガスバリア層全体において厚さ方向の組成分布が基材に近い方から順に、下記(A)の組成範囲を満たす厚さ方向に連続した20nm以上の領域と、下記(B)の組成範囲を満たす厚さ方向に連続した50nm以上の領域とを有するガスバリア性フィルム。
(A)ガスバリア層の組成をSiOwNxで表したときに、w≧0.8、x≧0.3、2w+3x≦4である。
(B)ガスバリア層の組成をSiOyNzで表したときに、0<y≦0.55、z≧0.55、2y+3z≦4である。 - (A)の組成範囲を満たす厚さ方向に連続した領域が、40nm以上100nm以下である、請求項1に記載のガスバリア性フィルム。
- (B)の組成範囲を満たす厚さ方向に連続した領域が、100nm以上1.0μm以下である、請求項1または2に記載のガスバリア性フィルム。
- 前記ガスバリア層が、ポリシラザンを含有する層に真空紫外線照射を施して形成された層である、請求項1〜3のいずれか一項に記載のガスバリア性フィルム。
- 請求項1〜4のいずれか一項に記載のガスバリア性フィルムを用いる電子デバイス。
- 請求項1〜4のいずれか一項に記載のガスバリア性フィルムの製造方法において、前記ガスバリア層を、ポリシラザンを含む溶液を塗布して形成した層に真空紫外線照射を施して形成することを有するガスバリア性フィルムの製造方法。
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2012
- 2012-06-13 US US14/125,166 patent/US20140106151A1/en not_active Abandoned
- 2012-06-13 EP EP12805138.0A patent/EP2724854A4/en not_active Withdrawn
- 2012-06-13 CN CN201280031320.2A patent/CN103796827B/zh active Active
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WO2005099311A1 (ja) * | 2004-04-05 | 2005-10-20 | Idemitsu Kosan Co., Ltd. | 有機エレクトロルミネッセンス表示装置 |
JP2009255040A (ja) * | 2008-03-25 | 2009-11-05 | Kyodo Printing Co Ltd | フレキシブルガスバリアフィルムおよびその製造方法 |
WO2011027619A1 (ja) * | 2009-09-02 | 2011-03-10 | コニカミノルタホールディングス株式会社 | バリアフィルム及びその製造方法 |
JP2011173057A (ja) * | 2010-02-24 | 2011-09-08 | Konica Minolta Holdings Inc | ガスバリアフィルム、ガスバリアフィルムの製造方法、ガスバリアフィルムを有する有機光電変換素子及び該素子を有する太陽電池 |
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EP2724854A1 (en) | 2014-04-30 |
KR101452680B1 (ko) | 2014-10-22 |
KR20140016995A (ko) | 2014-02-10 |
CN103796827A (zh) | 2014-05-14 |
JP5888329B2 (ja) | 2016-03-22 |
WO2013002026A1 (ja) | 2013-01-03 |
CN103796827B (zh) | 2015-06-10 |
US20140106151A1 (en) | 2014-04-17 |
EP2724854A4 (en) | 2015-03-25 |
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