JP2016104913A - 有機薄膜の低圧気相蒸着 - Google Patents
有機薄膜の低圧気相蒸着 Download PDFInfo
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- JP2016104913A JP2016104913A JP2016035497A JP2016035497A JP2016104913A JP 2016104913 A JP2016104913 A JP 2016104913A JP 2016035497 A JP2016035497 A JP 2016035497A JP 2016035497 A JP2016035497 A JP 2016035497A JP 2016104913 A JP2016104913 A JP 2016104913A
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- organic
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- thin film
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/568—Transferring the substrates through a series of coating stations
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45561—Gas plumbing upstream of the reaction chamber
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- H—ELECTRICITY
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Abstract
【課題】基体58上に有機薄膜を形成する方法を提供する。【解決手段】基体58上に有機薄膜を形成する方法であって、その方法は、複数の有機前駆物質(14、48)を気相で与え、前記複数の有機前駆物質(14、48)を大気圧未満で反応させる工程を有する。そのような方法により製造された薄膜及びそのような方法を実施するのに用いられる装置も含む。本方法は、有機発光デバイスの形成及び他のディスプレイ関連技術によく適している。【選択図】図1
Description
[政府の権利]
本発明は、米国空軍OSRによって与えられた契約番号F49620−92−J−05 24(プリンストン大学)に基づく政府の援助でなされた。米国政府は本発明に一定の権利を有する。
本発明は、米国空軍OSRによって与えられた契約番号F49620−92−J−05 24(プリンストン大学)に基づく政府の援助でなされた。米国政府は本発明に一定の権利を有する。
(技術分野)
本発明は、光学的品質の薄膜を製造することに関し、特に非線形光学デバイス及び有機発光デバイスで利用されるそのような薄膜の低圧製造に関する。
本発明は、光学的品質の薄膜を製造することに関し、特に非線形光学デバイス及び有機発光デバイスで利用されるそのような薄膜の低圧製造に関する。
(背景技術)
有機エレクトロルミネッセンスの分野は、急速に成長しつつある技術分野である。ディスプレイへの潜在的な用途に刺激されて、有機発光デバイス(OLED)は、3%を超える外部量子効率を達成し、ビデオ輝度で10,000時間の程度の作動寿命を達成することができる。低分子とポリマーの両方をベースとするOLEDが知られているが、ポリマーベースのデバイスは回転堆積法により簡単で安価に製造できる一般的利点を有する。これに対し、低分子によるデバイスは、通常真空中での熱的蒸発により製造されており、それは通常回転堆積法よりもコストがかかる方法である。OLED構造及び加工方法の例は、公開されたPCT国際公開WO 96/19792(参照により本明細書に援用する)において提供されている。
有機エレクトロルミネッセンスの分野は、急速に成長しつつある技術分野である。ディスプレイへの潜在的な用途に刺激されて、有機発光デバイス(OLED)は、3%を超える外部量子効率を達成し、ビデオ輝度で10,000時間の程度の作動寿命を達成することができる。低分子とポリマーの両方をベースとするOLEDが知られているが、ポリマーベースのデバイスは回転堆積法により簡単で安価に製造できる一般的利点を有する。これに対し、低分子によるデバイスは、通常真空中での熱的蒸発により製造されており、それは通常回転堆積法よりもコストがかかる方法である。OLED構造及び加工方法の例は、公開されたPCT国際公開WO 96/19792(参照により本明細書に援用する)において提供されている。
有機蒸着(organic vapor phase deposition)(OVPD)を使用することにより、ディスプレイ等の多くの潜在的光学的デバイス用途を持つ低分子量の有機層の低コストで大規模な蒸着が進歩してきた。OVPD法はフォレスト(Forrest)等の米国特許第5,554,220号明細書、S.R.フォレストらの「有機蒸着により成長させた有機塩薄膜の強力な二次調波発生及び長距離構造配列」(Intense Second Harmonic Generation and Long-Range Structural Ordering in Thin Films of an Organic Salt Grown by Organic Vapor Phase Deposition)、68 Appl. Phys. Lett., 1326 (1996)、及びP.E.バローズ(Burrows)らの「有機蒸着:大きな光学的非線形性を持つ有機薄膜の新規な成長方法」(Organic Vapor Phase Deposition: a New Method for the Growth of Organic Thin Films with Large Optical Non-linearities)、156 J. of Crystal Growth 91 (1995)(それらは参照により本明細書に援用する)に記載されている。
OVPD法は原料物質を基体(基板)へ運ぶためにキャリヤガスを用い、この場合ガスが凝縮して希望の薄膜を形成する。例えば、OVPD法を用いて、揮発性前駆物質、沃化4’−ジメチルアミノ−N−メチル−4−スチルバゾリウム(DASI)及びメチルp−トルエンスルホネート(メチルトシレート、MT)をキャリヤーガスにより加熱された基体へ運ぶことにより、光学的に非線形の有機(NLO)塩である4’−ジメチルアミノ−N−メチル−4−スチルバゾリウムトシレート(DASI)の膜を蒸着してきた。この方法ではDASIが熱分解して4−ジメチルアミノ−4−スチルバゾール(DAS)を形成し、それが次にMTと反応して基体上にDASTを形成する。
S.R.フォレストら、68 Appl. Phys. Lett., 1326 (1996)
P.E.バローズら、156 J. of Crystal Growth 91 (1995)
著しく異なった蒸気圧を持つ材料を制御して同時蒸着することができるため、OVPDは多成分薄膜の正確な化学量論的成長を行うための唯一の方法であると考えられる。しかし、OVPD法は大気圧で行われ、大気圧又はその近くで成長する膜はしばしば粗く、気相核生成及び拡散律速成長過程により不均一な表面モルフォロジーを有する。
(発明の開示)
本発明は、優れた表面特性を有する有機薄膜を製造するために低圧蒸着法を用いる。一つの態様として、本発明は、基体上に有機薄膜を形成する方法において、以下の工程:複数の有機前駆物質を与え、然も前記有機前駆物質は気相に存在する工程;及び、前記基体の存在下、大気圧未満の圧力(sub-atmospheric pressure)にて、前記複数の有機前駆物質を反応させて前記基体上に薄膜を形成する工程からなる方法にある。別の態様として、本発明は、そのような方法により製造された有機膜を包含する。更に別の態様として、本発明は、大気圧未満、有機前駆物質の反応を促進して基体上に有機膜を形成するように設計された装置を含む。
本発明は、優れた表面特性を有する有機薄膜を製造するために低圧蒸着法を用いる。一つの態様として、本発明は、基体上に有機薄膜を形成する方法において、以下の工程:複数の有機前駆物質を与え、然も前記有機前駆物質は気相に存在する工程;及び、前記基体の存在下、大気圧未満の圧力(sub-atmospheric pressure)にて、前記複数の有機前駆物質を反応させて前記基体上に薄膜を形成する工程からなる方法にある。別の態様として、本発明は、そのような方法により製造された有機膜を包含する。更に別の態様として、本発明は、大気圧未満、有機前駆物質の反応を促進して基体上に有機膜を形成するように設計された装置を含む。
本発明の一つの利点は、膜の各成分の量を正確精密に制御することができる多成分有機薄膜を与えることである。
本発明の別の利点は、滑らかな表面を有する均一な有機薄膜を与えることである。
本発明の更に別な利点は、有機発光材料及び光学的に非線形の有機塩の薄膜を形成するための低圧有機蒸着法及び装置を与えることである。
本発明の更に別な利点は、有機発光材料及び光学的非線形の有機塩の薄膜を形成させる低圧有機分子ビーム蒸着法及び装置を与えることである。
本発明のさらに別な利点は、大きな基体面積にわたって有機材料を均一に蒸着するための方法及び装置を与えることである。
(詳細な説明)
本発明は、大気圧未満の圧力(sub-atmospheric pressure)で基体上に有機薄膜を成長させるための方法及び装置を提供する。本発明の方法は、ここでは低圧有機蒸着(LPOVPD)という。本発明のLPOVPD法は、多成分有機薄膜の蒸着を正確且つ精密に制御することができる。更に、本発明の薄膜は、表面粗さが小さいなどの優れた表面性を特徴とする。
本発明は、大気圧未満の圧力(sub-atmospheric pressure)で基体上に有機薄膜を成長させるための方法及び装置を提供する。本発明の方法は、ここでは低圧有機蒸着(LPOVPD)という。本発明のLPOVPD法は、多成分有機薄膜の蒸着を正確且つ精密に制御することができる。更に、本発明の薄膜は、表面粗さが小さいなどの優れた表面性を特徴とする。
本発明の態様によるLPOVPD反応器10を図1に模式的に示す。反応器10は、反応管12などの反応室、及びその反応室中へ伸びる配管を有する。反応管12は、実験装置では、例えば、10cmの直径及び約45cmの長さなどの適当な大きさを有する円筒である。反応管12は、ガラス又は石英などの好適な材料から作られている。坩堝14などの開口容器には第一有機前駆物質材料が入っており、反応管12の一方の端20に近い管36内に配置されている。あるいは、坩堝14は反応管12上に直接置かれているか、又はその中の棚又は管に配置されている。坩堝14は、実質的に反応管12を取り巻く多領域加熱器/冷却器(マルチゾーンヒーター/クーラー)18により加熱又は冷却される。坩堝14の温度制御により、坩堝14内の第一有機前駆物質材料の熱分解又は蒸発がもたらされる。不活性キャリヤガスの調節された流れ30を、管36を通って反応室中へ送り、それにより第一有機前駆物質の蒸気を反応管12に沿ってその排出端22の方へ流す。不活性キャリヤガスは、窒素、ヘリウム、アルゴン、クリプトン、キセノン、ネオン等の不活性ガスである。水素、アンモニア、メタン等の還元性を持つガスも多くの有機材料に対しては不活性である。これらの還元性ガスを使用することにより、望ましくない過剰の反応原料の燃焼を助けるという付加的利点がしばしば得られる。
不活性ガスは、タンク24から、調節バルブ26を通り、配管28へ入り、少なくとも二つの流路30及び38を通って反応管12中へ送られる。一つの流路30は、直列に接続された圧力調節器32、流量計34、及び高速切り替えバルブ35を有し、そこからキャリヤガスが反応管12の端20中へ送られる。第二流路38は、直列に接続された圧力調節器40、流量計42、及び高速切り替えバルブ39を有し、そこからキャリヤガスがバブラー(bubbler)46中へ流れ、そのバブラーには第二有機前駆物質材料48が入っている。第二有機前駆物質材料48の温度制御をし易くするため、バブラー46は容器52内の浴50内に部分的に浸漬されている。タンク24からの不活性ガスは、第二有機前駆物質48を気泡として通り、配管54を通って第二有機前駆物質48の蒸気を反応管12中へ運ぶ。この工程中、管54は、気化した第二有機前駆物質48がバブラーから反応室へ移動する間に再び凝縮しないように充分高い温度に維持されなければならない。
反応管12中へ入る前駆物質の量は、キャリヤガスの温度及び流速、並びに反応原料の温度などの処理パラメータによって制御される。LPOVPD法は、前駆物質又は反応原料の蒸気圧又は化学的性質とは無関係に、圧力質量流量制御器を用いて、前駆物質又は反応原料の正確な計量をもたらす。本発明の方法は、このようにして、所望する膜の製造に必要な比率で、非常に異なった特性を持つ材料を組合せることを可能にする。
前駆物質の流れは、高速切り替えバルブ35及び39を用いることにより、殆ど瞬間的にオン・オフの切り替えを行うことができる。これらのバルブは前駆物質流を反応器12又はバイパス管(図示せず)中へ向かわせ、任意の時に、異なった前駆物質流が反応器12中へ入り、異なった組成及び特性の膜を蒸着することができる。バルブ39は、バブラー46へ入るキャリヤガスの調節も行う。バルブ35及び39は、このようにして反応器12中へ入る反応原料の流れを迅速に変化させ、成長する膜の性質及び組成を変化させることを可能にする。従って、各文字が異なった分子層又は組成を表すものとして、例えば、ABAB、ABCABC、ABABCAB、及びABCDABCD−型の膜を成長させることができる。
真空ポンプ66及び制御スロットルバルブ68を、反応器10の排気管62の所に取付ける。基体58上に蒸着しなかった有機蒸気の殆どは、ポンプ66より上流に配置されたトラップ64中で凝縮する。トラップ64には、例えば、液体窒素又は中性フルオロカーボンオイルが入っている。スロットルバルブ68は反応器10中の圧力を調節する。適当な圧力ゲージを反応器に取付け(図示せず)、反応器中に希望の圧力を維持するように制御スロットルバルブ68に電気的フィードバックを行う。
真空ポンプ66は、反応管12中に約0.001〜100トールの圧力を与える。受容体層、供与体層、及び単一成分層のいかなる組合せに対しても、実際の圧力は、前駆物質材料を蒸発させるために必要な温度、前駆物質材料の凝縮を防ぐ壁温度、及び反応領域温度勾配に関連して実験的に決定される。圧力の最適選択は、各蒸着される有機層の要件に固有のものである。例えば、トリス−(8−ヒドロキシキノリン)アルミニウム(Alq3)又はN,N’−ジフェニル−N,N−ビス(3−メチルフェニル)−1,1’−ビフェニル−4,4’ジアミン(TPD)等の単一成分層の蒸着のための最適圧力は約0.1〜10トールである。
本発明の薄膜を蒸着する基体は、半導体及び光学デバイスを製造する場合に一般に使用される材料から選択されるのが典型的である。例えば、そのような材料には、ガラス、石英、珪素、砒化ガリウム及び他のIII−V半導体、アルミニウム、金及び他の貴金属及び卑金属、ポリマー膜、二酸化珪素及び窒化珪素、インジウム錫酸化物等が含まれる。高品質の光学的薄膜のためには、蒸着した有機膜に結晶性相互作用をもたらしてエピタキシャル成長を起こす基体を用いるのが好ましい。そのようなエピタキシャル成長を達成するためには、蒸着すべき膜と同様の結晶構造を有する非極性有機物で基体を被覆することがしばしば必要である。
更に、有機薄膜を基体58上に蒸着する場合、基体の温度を制御することがしばしば好ましい。基体温度の独立した制御は、例えば、水、ガス、フレオン、グリセリン、液体窒素等の物質を循環させるための通路(チャネル)を有する温度制御ブロック60を基体58と接触させることにより達成される。基体は、ブロック60上又はその近くに配置した抵抗又は輻射線加熱器を使用することにより加熱することもできる。
図1の反応器20は、付加的前駆物質を反応器20中へ供給するための多重バブラー46Nを含ませるように拡張し得る。同様に、多重キャリヤガス流路30Nを用いて坩堝14Nから更に付加的前駆物質を送る。別法として、坩堝14、14Nは、付加的前駆物質を処理するため反応管12中の棚上又は管中に垂直方向に重ねることもできる。蒸着すべき有機膜に応じて、一つ以上の流路30及び38を単独又は任意の組合せで用いて、必要な前駆物質材料(precursor materials)を供給することができる。
本発明の方法を用いて、極めて多種の有機薄膜を蒸気前駆物質の反応により蒸着することができる。ここで用いる「反応」とは、前駆物質反応物が明確な反応生成物を形成する化学反応を意味するか、又はあるいは、それは前駆物質材料(precursor materials)の組合せ又は混合物を単に意味するか、又は前駆物質材料(precursor materials)が供与体・受容体の関係、又はゲスト・ホストの関係を形成する場合を意味する。例えば、本発明に従い、以下のNLO物質が、その列挙した前駆物質の反応によって薄膜として形成される。
OLEDを製造するのに用いられる発光材料に特に関連した別の例では、前駆物質は、例えば、テトラチスファルバレン(tetrathisferlvalene)(TFF)及び7,7,8,8−テトラシアノキノジメタン(TCNQ)からなる。混合工程は、基体上に蒸着する電荷移動錯体TTF−TCNQを与える結果になる。OLEDに関する別の例では、4−(ジシアノメチレン)−2−メチル−6−(p−ジメチルアミノスチリル)−4H−ピラン(DCM)を大きな流量のキャリヤーガス流中に添加し、一方、Alq3を低流量のキャリヤガス中に添加する。次にこれらの流れを中心反応管中で混合し、それによりホストマトリックス膜中においてゲスト分子を所望の通りに希釈して、単一の発光層を形成する。Alq3ホスト中の他のゲスト分子の例は、5,10,15,20−テトラフェニル−21H,23H−ポルフィン(TPP)、ルブレン(Rubrene)、DCM2、クマリン等である。変形法として、効率的な広いカラー・コンバージョンを達成するため、単一ホスト中に多種ドーパントを添加してもよい。
別の例では、Alq3、ビス−(8−ヒドロキシキノリン)アルミニウムオキシフェニル〔(Alq2)’−OPh〕等の発光層(EL)の表面上に積層した、TPD、α−4,4’−ビス[N−(1−ナフチル)−N−フェニル−アミノ]ビフェニル(α−NPD)、もしくはMTDATA等のホール輸送層(HTL)、又はこれらの層のドープした組合せからなる二層発光デバイスは、順次、HTL及びELを所望の厚さに成長させることにより形成する。次にそれら有機層の上に追加の層を成長させるか、又はトリメチル・インジウム、トリメチル・ガリウム等のような有機金属原料を用いて金属接点(コンタクト,contact)層を成長させる。
図1に関して述べた装置及び方法の外に、本発明は、図2に示すような低圧反応器70及び方法を包含する。反応器70は、一部変更した超高真空室71と、バルブ72に接続されたターボ分子ポンプ等の真空ポンプ(図示せず)を有する。室(チャンバー)71中の典型的なチャンバー基礎圧力は10-8〜10-11トールである。反応器70を用いた有機層蒸着法は、有機分子ビーム蒸着(OMVD)といわれる。LPOVPD及びOMVDの両方共に有機層を蒸着するのに減圧を用いているが、これらの方法の原理的な違いは、後者では分子平均自由行程が室70の大きさに匹敵するか、又はそれより大きいことである。これに対して、LPOVPDの平均自由行程は、ガス反応器の大きさよりもかなり短い。従って、OMVDはインジェクタから基体へと高度に向いた「分子ビーム」の形成を可能にし、成長膜厚さ、純度及びモルフォロジーの正確な速度論的制御を可能にする。
バブラー74が、第一前駆物質材料75を入れるために配備されている。バブラー74は容器76中に入れられ、温度制御浴80中に浸漬されている。高純度不活性キャリヤガス78が第一前駆物質75を気泡として通り、各蒸気を加熱された配管79を通ってインジェクタ82によって真空室71中へ運ぶ。室71中に入ると、前駆物質蒸気は分子ビーム83を形成し、それが基体85に衝突する。基体85は、例えば、冷却剤入口81などの温度を制御するための手段をそなえている。
任意選択により、真空室71には、少なくとも一つのクヌーセン又はK−セル86が備えられていてもよく、その中には第二前駆物質材料88が入っている。K−セル86は、減圧下で蒸発物を流出させるための均一に加熱され且つ制御された炉である。例えば、K−セル86はDASI又は他の前駆物質を分解するまで加熱され、得られたDASを昇華させ、それを分子ビーム89として反応器70中へ注入する。あるいは、K−セル86は、Alq3等の単一成分物質を単に昇華させるだけである。あるいは、K−セル86には、加熱によりガス流中に昇華又は蒸発される分子物質の濃度を希釈するのに用いられるキャリヤガス入口が取付けてある。この希釈方法は、浴80及びクヌーセン・セル86の温度、並びにバブラー74へのキャリヤガス78の流れを制御することによって、DCM−Alq3等のゲスト・ホスト系の正確なドーピング量を達成するのに特に有用である。
有機薄膜を蒸着させるために基体85に物質ビーム83及び89を衝突させ、薄膜の厚さを石英結晶93により監視する。試料ホルダー90は回転して、前駆物質材料の均一な蒸着及び反応を確実にする。前駆物質材料の蒸着は、分子ビーム83及び89を遮断するのに用いられるシャッタ87によって更に制御される。
任意選択で、反応器70は冷却囲い91を有してもよく、それは、再蒸発された前駆物質材料のために、真空室71の圧力を最小値に維持するのに役立つ。また、前駆物質材料が移動して互いに汚染することがないように隔壁92を備えるのも好ましい。
反応器70は、図1に示すLPOVPD反応器の付属品と同じもの、例えば、高速切り替えバルブ、バイパス導管等の多くのものを備えている。反応器70には、多重クヌーセンセル及びバブラーを、基体85の上に複数の前駆物質材料を蒸着するために取付けることができる。反応器70は、試料導入のための「ロード・ロック(load-lock)」を有するのが好ましい。ロード・ロック94は、ドア95及び真空ポンプ96を有し、室71の圧力を落とすことなく、試料の交換をもたらすことができる。
図1の装置は、任意選択により、図3に説明する例によって示すように、大面積基体上に有機層を連続的に蒸着できるように修正してもよい。図3の装置は、導入室146、有機層蒸着室150及び152、接点蒸着室154、及び取出し室156などの複数の真空室を有する。例えば、各蒸着室は図1のLPOVPD反応器10である。基体137はコンベヤベルト148に乗せて、室150、152、154及び156の各々を通って運ぶ。図3に示した態様では、室150、152及び154は、それぞれ、輻射熱源158、160及び162を有し、有機蒸気の凝縮を防ぐ。図3には唯二つの有機層蒸着室150及び152しか示されていないが、所望により、追加の室を設ける。導入室146から有機層蒸着室150及び152へ、また接点蒸着室154から取出し室156へ送られる間に、基体137は空気遮断部(図示せず)を通過して、室150、152及び154の中の真空が損なわれないようにしてある。OLEDに関する例として、室150及び152をそれぞれTPD及びAlq3の蒸着のために用い、室154をMg:Ag接点層を蒸着するために用いる。
図3の例の室150、152、及び154の各々には、図4A及び4Bに詳細に示すように、有機前駆物質材料の蒸着のための反応原料ガス分配器(RGD)108が含まれている。RGD108は、図1及び2の有機前駆物質導入機構の代替物として用いられ、ガスカーテン、120、120’、120’’及び120’’’を与えるのに用いられる。RGD108は、複数の有機前駆物質を蒸着する場合に、前駆物質の反応を行わせることができる基体上に蒸着されるまで、それら前駆物質が分離されていることを確実にする。RGD108には、加熱器122、第二キャリヤガス入口112、及びガスマニホルド132が含まれる。加熱器122は、有機前駆物質材料の早すぎる凝縮を防ぐ。RGD108の上には第一キャリヤガス入口114及び分配器板110が存在する。第一キャリヤガス入口114は、例えば、MT等の一般に低揮発性第一有機前駆物質を通常運ぶガスを供給する。第一キャリヤガスは、例えば、ワイヤ網、ガラスフィルタ材料、又は多孔質ステンレス鋼板である分配器板110を通って反応室へ入る。分配器板110を通って流れるキャリヤガスのカラムは、RGD108により陰になっている。RGD108は、例えばDAS等の一般に低い蒸気圧の第二有機前駆物質の平面状ガスカーテン120をもたらす。第二有機前駆物質を含む第二キャリヤガスは、入口112から入り、ガスマニホルド132の中へ送られる。マニホルド132は、環状空洞126中へ第二キャリヤガスを供給するための並んだ孔134を有する中空管であり、その環状空洞はマニホルド132を取り巻いている。第二キャリヤガスは、それに平面状カーテンの形態を与えるスリット136を通ってRGD108から出る。
例として、カーテン120はTPD蒸気からなり、カーテン120’はAlq3蒸気からなり、カーテン120’’は、伝導性表面を作り出すポリピロール(polypyrole)又は金属有機化合物等の蒸気からなる。所望する場合には、OLEDにより発する光の色の制御又は調節を、室152中の追加のRGDデバイス108を用いてAlq3層の適切なドーピングにより行うことができ、この追加のRGDデバイスはドーパント蒸気のカーテン120’’’を作り出す。
図1、図2、又は図3の装置は、任意選択により、図5に示すような「ロール対ロール」基体搬送装置を用いることにより修正してもよい。図5に示す搬送装置は、大面積可撓性基体上に有機薄膜を蒸着するのに適している。例えば、基体180はポリマーシート又は金属箔からなり、ロール181からロール182へ送られる。基体180への有機前駆物質の蒸着は、基体180がロール181から解かれた時に行われ、従って図1の反応室へ曝されるか、又は図2及び3の分子ビーム又は分子カーテンにそれぞれ曝された時に行われる。ロール181及び182は、速度可変モータ等の適当な手段により駆動される。基体180がロール181からロール182へ送られる速度は、基体180上に形成される有機膜の厚さを決定する。
本発明を、以下の非限定的な例を参照してさらに説明する。
〔例1〕
図1の装置を用い、インジウム錫酸化物(ITO)の透明層で予め被覆したガラス及び可撓性ポリエステル基体を用いて、有機発光材料の層を成長させた。ITOはデバイスのアノードを形成し、ガラス及びポリエステル基体に対し、それぞれ1700Å及び1200Åの厚さをもち、それぞれ10Ω及び60Ωのアノード抵抗を与えた。ガラス基体は超音波浴中の洗剤溶液及び脱イオン水で濯ぎ、次に1,1,1−トリクロロエタン中で煮沸し、アセトンで濯ぎ、最後に2−プロパノールで濯ぐことにより清浄にした。可撓性基体は、有機溶媒に曝すことによる損傷を避けるため、洗剤及び2−プロパノール溶液だけで濯ぐことにより清浄にした。
図1の装置を用い、インジウム錫酸化物(ITO)の透明層で予め被覆したガラス及び可撓性ポリエステル基体を用いて、有機発光材料の層を成長させた。ITOはデバイスのアノードを形成し、ガラス及びポリエステル基体に対し、それぞれ1700Å及び1200Åの厚さをもち、それぞれ10Ω及び60Ωのアノード抵抗を与えた。ガラス基体は超音波浴中の洗剤溶液及び脱イオン水で濯ぎ、次に1,1,1−トリクロロエタン中で煮沸し、アセトンで濯ぎ、最後に2−プロパノールで濯ぐことにより清浄にした。可撓性基体は、有機溶媒に曝すことによる損傷を避けるため、洗剤及び2−プロパノール溶液だけで濯ぐことにより清浄にした。
ガラス基体を反応管12中の、温度が約220℃になる位置に置いた。ITO表面上に蒸着した第一層はTPD、ホール輸送材料であった。特に、TPD蒸気を窒素キャリヤガスにより坩堝14から基体28へ運んだ。TPD成長条件には、200±5℃の原料温度、100sccmの窒素キャリヤガス流量、0.50トールの反応器圧力、及び20分の成長時間が含まれる。100sccmの窒素流量で、装置のレイノルズ数は〜500であり、層流領域内に充分入る操作であることを示していた。TPD層は100〜300Åの厚さに成長させた。
蒸着後、TPD坩堝近くの温度を低下させ、対応する窒素流を遮断した。次にAlq3の電子輸送層を、別の窒素導管を開けて坩堝14NからAlq3蒸気を室12中へ運ぶことにより成長させた。Alq3成長条件には、247±8℃の原料温度、50sccmの窒素流量、0.65トールの圧力、及び10分の成長時間が含まれる。TPD及びAlq3の両方の蒸着中、水冷されたステンレス鋼基体ホルダーを用いて基体を15℃に維持した。TPD層は700〜1100Åの厚さに成長させた。
Alq3 層を蒸着した後、基体を反応器から取り出し、Mg:Ag頂部接点を加熱蒸着により適用した。接点(コンタクト)は、1000Åの厚さの保護Ag層を蒸着させて完成した。
蒸着中、低い圧力を使用することにより、滑らかで均一な表面を有する有機層を与える結果になった。例えば、TPD及びAlq3 層を原子力顕微鏡で測定して、それぞれ6〜8Å及び9〜11ÅのRMS粗さをもっていた。得られたOLEDデバイスは、低電圧でI∝V、高電圧でI∝V9である電流・電圧特性を示した。I対Vのパワー法則依存性(power law dependence of I on V)が変化するターン・オン(turn-on)電圧VTは約6Vであった。
〔例2〕
NLO膜を、図1に示す装置を用いて製造した。シリコーン油浴50によって約80〜100℃に温度を維持した30cm3バブラー46中にMT48を入れた。窒素ガスを用いてMT48に気泡として通し、それによりガラス管54を通してMT蒸気を反応管12中へ、坩堝14を約5cm越えた位置の所から導入した。その坩堝は反応管12の床上に置かれており、DASIが入っていた。反応管12中の圧力を約10-2トールに維持した。DAS蒸気はMT蒸気と反応し、基体ブロック60上に支持された基体58上にDASTの固体膜を形成した。過剰の未反応MT蒸気及び揮発性副反応生成物を排出管62から排出した。そのようにして形成したDAST膜は、例えば、光学的スイッチとして有用である。
NLO膜を、図1に示す装置を用いて製造した。シリコーン油浴50によって約80〜100℃に温度を維持した30cm3バブラー46中にMT48を入れた。窒素ガスを用いてMT48に気泡として通し、それによりガラス管54を通してMT蒸気を反応管12中へ、坩堝14を約5cm越えた位置の所から導入した。その坩堝は反応管12の床上に置かれており、DASIが入っていた。反応管12中の圧力を約10-2トールに維持した。DAS蒸気はMT蒸気と反応し、基体ブロック60上に支持された基体58上にDASTの固体膜を形成した。過剰の未反応MT蒸気及び揮発性副反応生成物を排出管62から排出した。そのようにして形成したDAST膜は、例えば、光学的スイッチとして有用である。
本発明は、低圧蒸着法を用いて、優れた表面特性及び正確精密な組成を有する有機薄膜を製造する。本発明の種々の態様をここに示し記述してきたが、それらは限定することを意味しない。例えば、当業者はこれらの態様に対して或る変更を認めることができるであろうが、それら変更は特許請求の範囲の本質及び範囲に含まれる。
ここに記載した本発明は、次の係属中の出願に関連して用いることができる:「高信頼性、高効率、集積可能な有機発光デバイス及びその製法」(High Reliability, High Efficiency, Integratable Organic Light Emitting Devices and Methods of Producing Same)、シリアル番号08/774,119(1996年12月23日出願);「多色LEDのための新規な材料」(Novel Materials for Multicolor LED's)、シリアル番号08/850,264(1997年5月2日出願);「有機遊離ラジカルに基づく電子輸送及び発光層」(Electron Transporting and Light Emitting Layers Based on Organic Free Radicals)、シリアル番号08/774,120(1996年12月23日出願);「多色表示デバイス」(Multicolor Display Devices)、シリアル番号08/772,333(1996年12月23日出願);「赤色光有機発光デバイス(LED)」(Red-Emitting Organic Light Emitting Devices (LED's))、シリアル番号08/774,087(1996年12月23日出願);「積層有機発光デバイスのための駆動回路」(Driving Circuit For Stacked Organic Light Emitting Devices)、シリアル番号08/792,050(1997年2月3日出願);「高効率有機発光デバイス構造体」(High Efficiency Organic Light Emitting Device Sturctures)、シリアル番号08/772,332(1996年12月23日出願);「真空蒸着した非ポリマー可撓性有機発光デバイス」(Vacuum Deposited, Non-Polymeric Flexible Organic Light Emitting Devices)、シリアル番号08/789,319(1997年1月23日出願);「メサピクセル構造を有するディスプレイ」(Displays Having Mesa Pixel Configuration)、シリアル番号08/794,595(1997年2月3日出願);「積層有機発光デバイス」(Stacked Organic Light Emitting Devices)、シリアル番号08/792,048(1997年2月3日出願);「高コントラスト透明有機発光デバイス表示器」(High Contrast Transparent Organic Light Emitting Device Display)シリアル番号08/821,380(1997年3月20日出願);「ホスト物質として5−ヒドロキシ−キノキサリンの金属錯体を含む有機発光デバイス」(Organic Light Emitting Devices Containing A Metal Complex of 5-Hydroxy-Quinoxaline as A Host Materials)、シリアル番号08/838,099(1997年4月15日出願);「大きな輝度を有する発光デバイス」(Light Emitting Devices Having High Brightness)、シリアル番号08/844,353(1997年4月18日出願);「有機半導体レーザ」(Organic Semiconductor Laser)、シリアル番号60/046,061(1997年5月9日出願);「有機半導体レーザ」(Organic Semiconductor Laser)、シリアル番号08/859,468(1997年5月19日出願);「飽和天然色積層有機発光デバイス」(Saturated Full Color Stacked Organic Light Emitting Devices)、シリアル番号08/858,994(1997年5月20日出願);「ホール注入促進層を有する有機発光デバイス」(An Organic Light Emitting Device Containing a Hole Injection Enhancement Layer)、シリアル番号08/865,491(1997年5月29日出願);「伝導性層のプラズマ処理」(Plasma Treatment of Conductive Layers)、シリアル番号PCT/US97/10252(1997年6月12日出願)
;「有機多色ディスプレイを製造するための薄膜パターン化」(Patterning of Thin Films for the Fabrication of Organic Multi-color Displays)、シリアル番号PCT/US97/10289/(1997年6月12日出願);「二重ヘテロ構造赤外線及び垂直空洞表面発光有機レーザ」(Double Heterostructure Infrared and Vertical Cavity Surface Emitting Organic Lasers)、シリアル番号60/053,176(1997年7月18日出願);「オレッド含有熱安定性不斉電荷キャリヤ材料」(Oleds Containing Thermally Stable Asymmetric Charge Carrier Materials)、シリアル番号08/929,029(1997年9月8日出願);「オレッド積層体を有する発光デバイス及び燐光体周波数逓降変換器」(Light Emitting Device with Stack of Oleds and Phosphor Downconverter)、シリアル番号08/925,403(1997年9月9日出願);「有機発光デバイス中のインジウム錫酸化物層を蒸着するための改良方法」(An Improved Method for Depositing Indium Tin Oxide Layers in Organic Light Emitting Devices)、シリアル番号08/928,800(1997年9月12日出願);「オレッドの発光層中のアズラクトン関連ドーパント」(Azlactone-Related Dopants in the Emissive Layer of an Oled)、シリアル番号08/948,130(1997年10月9日出願);「非金属カソードを用いた高透明性有機発光デバイス」(A Highly Transparent Organic Light Emitting Device Employing A Non-Metallic Cathode)、(1997年11月3日出願)、代理人書類番号
10020/40(暫定出願)、及び「非金属カソードを用いた高透明性有機発光デバイス」(A Highly Transparent Organic Light Emitting Device Employing A Non-Metallic Cathode)、(1997年11月5日出願)、代理人書類番号
10020/44、各係属中の出願は、言及することによって本明細書に組み入れる。本発明は、係属中の米国特許出願シリアル番号08/354,674、08/613,207、08/632,322、及び08/693,359、及び暫定特許出願シリアル番号60/010,013、06/024,001、及び60/025,501(これらの各々は参照によりその全体を本明細書に援用する)の各々の主題に関連して用いることもできる。
;「有機多色ディスプレイを製造するための薄膜パターン化」(Patterning of Thin Films for the Fabrication of Organic Multi-color Displays)、シリアル番号PCT/US97/10289/(1997年6月12日出願);「二重ヘテロ構造赤外線及び垂直空洞表面発光有機レーザ」(Double Heterostructure Infrared and Vertical Cavity Surface Emitting Organic Lasers)、シリアル番号60/053,176(1997年7月18日出願);「オレッド含有熱安定性不斉電荷キャリヤ材料」(Oleds Containing Thermally Stable Asymmetric Charge Carrier Materials)、シリアル番号08/929,029(1997年9月8日出願);「オレッド積層体を有する発光デバイス及び燐光体周波数逓降変換器」(Light Emitting Device with Stack of Oleds and Phosphor Downconverter)、シリアル番号08/925,403(1997年9月9日出願);「有機発光デバイス中のインジウム錫酸化物層を蒸着するための改良方法」(An Improved Method for Depositing Indium Tin Oxide Layers in Organic Light Emitting Devices)、シリアル番号08/928,800(1997年9月12日出願);「オレッドの発光層中のアズラクトン関連ドーパント」(Azlactone-Related Dopants in the Emissive Layer of an Oled)、シリアル番号08/948,130(1997年10月9日出願);「非金属カソードを用いた高透明性有機発光デバイス」(A Highly Transparent Organic Light Emitting Device Employing A Non-Metallic Cathode)、(1997年11月3日出願)、代理人書類番号
10020/40(暫定出願)、及び「非金属カソードを用いた高透明性有機発光デバイス」(A Highly Transparent Organic Light Emitting Device Employing A Non-Metallic Cathode)、(1997年11月5日出願)、代理人書類番号
10020/44、各係属中の出願は、言及することによって本明細書に組み入れる。本発明は、係属中の米国特許出願シリアル番号08/354,674、08/613,207、08/632,322、及び08/693,359、及び暫定特許出願シリアル番号60/010,013、06/024,001、及び60/025,501(これらの各々は参照によりその全体を本明細書に援用する)の各々の主題に関連して用いることもできる。
Claims (43)
- 基体上に有機薄膜を形成する方法であって、
複数の有機前駆物質を供給し、前記有機前駆体が気相中に存在する工程、
前記基体の存在下、大気圧未満の圧力において前記複数の有機前駆物質を反応させて、前記基体上に薄膜を形成させる工程、
を含む方法。 - 前記基体を反応室中に配置する、請求項1記載の方法。
- 前記の複数の有機前駆物質の一つを、前記の反応工程前に反応室中へ輸送する工程をさらに有する、請求項2記載の方法。
- 前記の輸送工程が、不活性ガスを用いて、前記の輸送される有機前駆物質を前記反応室へ運ぶ工程を含む、請求項3記載の方法。
- 不活性ガスを、窒素、アルゴン、ヘリウム、ネオン、クリプトン、及びキセノンからなる群から選択する、請求項4記載の方法。
- 前記の複数の有機前駆物質の少なくとも一つを、MT、DASI、MM、MfM、DASTh、MeOSI、DAS(Et)I、DAS(Et)OH、アセチルトルエンスルホネート、MAf、TTF、TCNQ、DCM、Alq3、TPP、TPD、α−NPD、MTDATA、及び(Alq2)’−OPhからなる群から選択する、請求項1記載の方法。
- 前記の輸送工程前に、前記の輸送される有機前駆物質を気化する工程をさらに有する、請求項3記載の方法。
- 前記の気化工程が、前記の輸送される有機前駆物質をバブラーへ導入する工程を含み;かつ、前記の輸送工程が、前記バブラーに不活性ガスを通して前記の輸送される有機前駆物質を前記反応室中に運ぶ工程を含む、請求項7記載の方法。
- 前記の気化工程が、前記の輸送される有機前駆物質を開口容器中へ入れ、且つ前記開口容器を加熱する工程を含み;さらに、前記の輸送工程が、前記開口容器上に不活性ガスを送り、前記の輸送される有機前駆物質を前記反応室中に運ぶ工程を含む、請求項7記載の方法。
- 前記の気化工程が、 前記反応室中へ伸びているクヌーセン・セルの中へ、前記の輸送される有機前駆物質を導入する工程、次いで 前記クヌーセン・セルを加熱する工程を含む、請求項7記載の方法。
- 前記基体を、回転試料ホルダーに取付ける、請求項1記載の方法。
- 前記の大気圧未満の圧力が約10-11〜102トールの範囲内にある、請求項1記載の方法。
- 請求項1に記載の方法により製造された有機膜。
- 前記膜が発光材料を含む、請求項13記載の有機膜。
- 前記膜が光学的非線形材料を含む請求項13記載の有機膜。
- 基体上に有機薄膜を形成する装置であって、 反応室、 前記反応室を実質的に取り巻く加熱器、 前記反応室中へ伸びる配管、及び 前記反応室へ取付けられた真空ポンプ、を具えた装置。
- 前記反応室が反応管を有する、請求項16記載の装置。
- 前記加熱器が多領域加熱器/冷却器である、請求項16記載の装置。
- 前記配管が、第一端部及び第二端部を有し第二端部が前記反応室中へ伸びる管、並びに前記管の第一端部に接続されたガス源、を有する、請求項16記載の装置。
- 前記管の内部に配置された開口容器をさらに備え、前記開口容器が有機前駆物質材料を保持するためのものである、請求項19記載の装置。
- 前記管が圧力調節器及びバルブを有する、請求項20記載の装置。
- 前記配管が、 第一端部及び第二端部を有する第一管であって、第一管の第二端部が反応室中へ伸びている第一管; 前記第一管の第一端部に接続された、有機前駆物質材料を入れるためのバブラー、;第一端部及び第二端部を有する第二管であって、前記第二管の第二端部が前記バブラーに接続されている第二管;並びに 前記第二管の第一端部に接続されたガス源、を有する、請求項16に記載の装置。
- 前記第二管が圧力調節器及びバルブを有する、請求項22に記載の装置。
- 前記基体と接触している温度制御ブロックをさらに備え、前記温度制御ブロックがその中に流路を有する、請求項16記載の装置。
- 前記反応室に取付けられたトラップをさらに備える、請求項16記載の装置。
- 第一のロールと第二のロールとの間に基体を通すため、前記反応室内に第一ロール及び第二ロールをさらに備えた、請求項16記載の装置。
- 基体上に有機薄膜を形成するための装置であって、 反応室、 前記反応室中へ伸びるクヌーセン・セル、 基体に接続された回転可能な試料ホルダー、及び 前記反応室に取付けられた真空ポンプ、を含む装置。
- 前記反応室中へ伸びる配管をさらに備え、前記配管が、 第一端部及び第二端部を有する第一管であって、第一管の第二端部が前記反応室中へ伸びている第一管、;前記第一管の第一端部に接続された、有機前駆物質材料を入れるためのバブラー;第一端部及び第二端部を有する第二管であって、前記第二管の第二端部が前記バブラーに接続されている第二管;並びに 第二管の第一端部に接続されたガス源、を有する、請求項27記載の装置。
- 前記第一管が加熱されている、請求項27記載の装置。
- 前記反応室中に冷却された囲いをさらに備える、請求項27記載の装置。
- 前記薄膜の厚さを検出するセンサをさらに備える、請求項27記載の装置。
- 前記センサが石英結晶である、請求項31記載の装置。
- 前記反応室へ接続されたロード・ロックをさらに備えた、請求項27記載の装置。
- 前記真空ポンプがターボ分子ポンプである、請求項27記載の装置。
- 前記第一ロールと前記第二ロールとの間に前記基体を通すため、反応室中に第一ロール及び第二ロールをさらに備えた、請求項27記載の装置。
- 基体上に有機薄膜を形成するための装置であって、導入室及び有機層蒸着室を含めた複数の真空室、および、前記複数の真空室を通過するコンベアベルトであって、その上に基体を有するコンベアベルト、を備えた装置。
- 前記有機層蒸着室が反応物ガス分配器を有する、請求項36記載の装置。
- 前記有機層蒸着室が加熱器を有する、請求項36記載の装置。
- 接点の蒸着室をさらに備えた、請求項36記載の装置。
- 基体上に有機薄膜を形成するための装置であって、 反応室、;前記反応室を加熱するための手段、;前記反応室中へ有機前駆物質材料の蒸気を導入するための手段;及び 前記反応室中の圧力を大気圧より低下させるための手段、を備えた装置。
- OLEDを製造するための方法であって、 複数の有機前駆物質を供給し、前記有機前駆物質は気相中に存在する工程、及び前記複数の有機前駆体を大気圧未満の圧力で反応させる工程を有する方法。
- 有機前駆物質が発光材料である、請求項41記載の方法。
- 前記の反応工程が発光物質を形成する結果を与える、請求項41記載の方法。
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1997
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1998
- 1998-11-16 DE DE1998627293 patent/DE69827293T2/de not_active Expired - Lifetime
- 1998-11-16 KR KR1020067004695A patent/KR100606325B1/ko not_active IP Right Cessation
- 1998-11-16 AU AU14124/99A patent/AU1412499A/en not_active Abandoned
- 1998-11-16 KR KR1020007005399A patent/KR100585286B1/ko not_active IP Right Cessation
- 1998-11-16 EP EP19980957997 patent/EP1032722B1/en not_active Expired - Lifetime
- 1998-11-16 JP JP2000521253A patent/JP2001523768A/ja not_active Withdrawn
- 1998-11-16 WO PCT/US1998/024424 patent/WO1999025894A1/en active IP Right Grant
- 1998-11-17 TW TW87118943A patent/TW575699B/zh not_active IP Right Cessation
-
2000
- 2000-12-13 US US09/736,090 patent/US20010002279A1/en not_active Abandoned
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2002
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2003
- 2003-05-02 US US10/427,933 patent/US20040007178A1/en not_active Abandoned
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2007
- 2007-01-19 US US11/655,258 patent/US20070131172A1/en not_active Abandoned
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2009
- 2009-06-09 JP JP2009138382A patent/JP4890592B2/ja not_active Expired - Lifetime
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2010
- 2010-03-08 JP JP2010050397A patent/JP5371837B2/ja not_active Expired - Lifetime
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2013
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Also Published As
Publication number | Publication date |
---|---|
EP1032722A4 (en) | 2001-09-12 |
KR100606325B1 (ko) | 2006-07-31 |
DE69827293D1 (de) | 2004-12-02 |
US20150114296A1 (en) | 2015-04-30 |
TW575699B (en) | 2004-02-11 |
US20010002279A1 (en) | 2001-05-31 |
JP2001523768A (ja) | 2001-11-27 |
US20100104753A1 (en) | 2010-04-29 |
KR20060034312A (ko) | 2006-04-21 |
JP4890592B2 (ja) | 2012-03-07 |
DE69827293T2 (de) | 2006-02-02 |
AU1412499A (en) | 1999-06-07 |
US20040007178A1 (en) | 2004-01-15 |
EP1032722A1 (en) | 2000-09-06 |
JP5371837B2 (ja) | 2013-12-18 |
US20020155230A1 (en) | 2002-10-24 |
EP1032722B1 (en) | 2004-10-27 |
JP2009238756A (ja) | 2009-10-15 |
WO1999025894A1 (en) | 1999-05-27 |
JP2010159497A (ja) | 2010-07-22 |
KR20010024652A (ko) | 2001-03-26 |
US20070131172A1 (en) | 2007-06-14 |
KR100585286B1 (ko) | 2006-05-30 |
US6337102B1 (en) | 2002-01-08 |
JP2013177692A (ja) | 2013-09-09 |
US6558736B2 (en) | 2003-05-06 |
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