JP5371837B2 - 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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- JP5371837B2 JP5371837B2 JP2010050397A JP2010050397A JP5371837B2 JP 5371837 B2 JP5371837 B2 JP 5371837B2 JP 2010050397 A JP2010050397 A JP 2010050397A JP 2010050397 A JP2010050397 A JP 2010050397A JP 5371837 B2 JP5371837 B2 JP 5371837B2
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- organic
- carrier gas
- precursor material
- substrate
- light emitting
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic 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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- 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
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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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- 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
- 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
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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Description
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、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。
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。
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、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。
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。
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。
;「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 (7)
- 第一キャリヤーガス流を供給し;
前記第一キャリヤーガス流中へ第一有機前駆物質材料を気化して入れ;
前記第一キャリヤーガス流を、装置に通して送り;
前記装置の壁温度を、前記気化した第一有機前駆物質材料の凝縮を起こさないようにするのに充分な高い温度に維持し;
前記第一キャリヤーガス流を1.333×10−3〜1.333×102ミリバール(0.001トール〜100トール)の圧力で反応室中の基体上に通し;そして
前記基体上に前記第一有機前駆物質材料を蒸着して前記基体上に前記第一有機前駆物質材料を含む有機フィルムを形成する際に、
更に、第二有機前駆物質材料を含む第二キャリヤーガス流を供給し;そして
前記第二キャリヤーガス流と第一キャリヤーガス流とを一緒にする;
ことを含み、ここで、蒸着が、基体上に第一有機前駆物質材料と共に第二有機前駆物質材料を蒸着することを含み、それにより前記有機フィルムが、前記第一有機前駆物質材料及び第二有機前駆物質材料を含み、;且つ、
前記第一キャリアーガス及び第二キャリアーガスのそれぞれの温度及び流速を制御することによって、前記有機フィルムが、所望のフィルムの作製に必要な正確な割合で前記第一有機前駆物質と前記第二有機前駆物質の両方を含む、有機フィルムの製造方法。 - 少なくとも一種類のキャリヤーガスの圧力が、1.333×10−1〜13.33ミリバール(0.1トール〜10トール)である、請求項1に記載の製造方法。
- キャリヤーガスが、不活性ガスを含む、請求項1又は2に記載の製造方法。
- 不活性ガスが、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される、請求項3に記載の製造方法。
- 有機発光デバイス中へ前記のフィルムを組込むことを含む、請求項1〜4のいずれか1項に記載の有機フィルムの製造方法。
- 前記有機フィルムの一つが発光層であるか;又は
前記有機フィルムの一つがホール輸送層であるか;又は
前記有機フィルムの一つが発光層で、前記有機フィルムの一つがホール輸送層である;
請求項1〜5のいずれか1項に記載の製造方法。 - 前記ホール輸送層が、N,N’−ジフェニル−N,N’−ビス(3−メチルフェニル)−1,1’−ビスフェニル−4,4’−ジアミンを含むか;又は
前記発光層が、トリス−(8−キノリン)アルミニウムを含み、そして前記ホール輸送層が、N,N’−ジフェニル−N,N’−ビス(3−メチルフェニル)−1,1’−ビスフェニル−4,4’−ジアミンを含むか;又は
それらの組合せである、請求項6に記載の製造方法。
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2000
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2002
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2007
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JP2016104913A (ja) | 2016-06-09 |
US6337102B1 (en) | 2002-01-08 |
JP2001523768A (ja) | 2001-11-27 |
US20010002279A1 (en) | 2001-05-31 |
TW575699B (en) | 2004-02-11 |
US20020155230A1 (en) | 2002-10-24 |
EP1032722B1 (en) | 2004-10-27 |
US20040007178A1 (en) | 2004-01-15 |
EP1032722A4 (en) | 2001-09-12 |
DE69827293T2 (de) | 2006-02-02 |
AU1412499A (en) | 1999-06-07 |
EP1032722A1 (en) | 2000-09-06 |
US20070131172A1 (en) | 2007-06-14 |
KR100585286B1 (ko) | 2006-05-30 |
US6558736B2 (en) | 2003-05-06 |
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US20150114296A1 (en) | 2015-04-30 |
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US20100104753A1 (en) | 2010-04-29 |
KR100606325B1 (ko) | 2006-07-31 |
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