WO2002052903A1 - Procede de production et dispositif utilises avec un element el organique - Google Patents

Procede de production et dispositif utilises avec un element el organique Download PDF

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Publication number
WO2002052903A1
WO2002052903A1 PCT/JP2001/011192 JP0111192W WO02052903A1 WO 2002052903 A1 WO2002052903 A1 WO 2002052903A1 JP 0111192 W JP0111192 W JP 0111192W WO 02052903 A1 WO02052903 A1 WO 02052903A1
Authority
WO
WIPO (PCT)
Prior art keywords
organic
deposited
substrate
thin film
evaporation source
Prior art date
Application number
PCT/JP2001/011192
Other languages
English (en)
Japanese (ja)
Inventor
Kazuo Ishii
Mahito Soeda
Original Assignee
Nippon Steel Chemical Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Steel Chemical Co., Ltd. filed Critical Nippon Steel Chemical Co., Ltd.
Priority to KR1020037007313A priority Critical patent/KR100788152B1/ko
Publication of WO2002052903A1 publication Critical patent/WO2002052903A1/fr

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Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
    • 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
    • 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
    • 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
    • H10K71/10—Deposition of organic active material
    • H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
    • H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/30—Coordination compounds
    • H10K85/321—Metal complexes comprising a group IIIA element, e.g. Tris (8-hydroxyquinoline) gallium [Gaq3]
    • H10K85/324—Metal complexes comprising a group IIIA element, e.g. Tris (8-hydroxyquinoline) gallium [Gaq3] comprising aluminium, e.g. Alq3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/631—Amine compounds having at least two aryl rest on at least one amine-nitrogen atom, e.g. triphenylamine

Definitions

  • the present invention relates to a method for manufacturing an organic EL device by vaporizing an organic EL device material (also referred to as an organic EL material) in order to form an organic thin film for an organic EL device by a vacuum evaporation method.
  • the present invention relates to a method and an apparatus for producing BACKGROUND ART
  • an organic thin film layer such as a hole transport layer, a light emitting layer, and an electron transport layer is formed between an anode made of a transparent conductive film and an anode.
  • Light emission occurs when holes injected from the cathode into the light emitting layer via the hole transport layer and electrons injected from the cathode into the light emitting layer via the electron transport layer are generated. At this time, so-called dark spots are generated due to co-evaporation of some impurities and degraded substances in the material, which causes a problem that a non-colored portion appears in a display device.
  • a shutter is installed on one or both of the evaporation source and the substrate in the evaporation apparatus, and the evaporation amount is stabilized while monitoring the evaporation rate of the organic EL material vaporized from the evaporation source. Then, the shirt is opened and an operation for starting the vapor deposition on the substrate surface is performed. Since this shutter covers the evaporation source and the substrate again when the substrate is replaced or when the organic EL material to be evaporated is changed, the shutter is deposited on the shutter facing the evaporation source by opening and closing the shutter. Material may fall into the evaporation source.
  • a vacuum evaporation apparatus for an organic EL device uses a vessel such as a boat crucible as an evaporation source, and gaseous molecules of the organic EL material vaporized from the evaporation source have an inverted triangular pyramid shape with the evaporation source at the top. As it spreads, it rises and reaches the film-forming substrate, where it is deposited. In any cross section of the inverted triangular pyramid, the concentration of gaseous molecules at the center is the highest, and the concentration decreases as the distance increases in the radial direction. The change in concentration of gaseous molecules in the radial direction increases as the distance from the evaporation source increases, as it approaches the center of the inverted triangular pyramid, and decreases as the distance increases.
  • the film thickness distribution on the substrate is such that the thickness of the central part of the gaseous molecules in the shape of an inverted triangular pyramid is thicker and the thickness of the peripheral part is thinner.
  • the gaseous molecule concentration on the substrate surface is averaged as much as possible, or by depositing only the periphery of the inverted triangular pyramidal gaseous molecular phase on the substrate surface, the film thickness is uniform.
  • efforts are being made to promote in the former case, the gaseous molecules become larger and spread, and a considerable amount of the gaseous molecules precipitate on the inner walls of the apparatus other than the substrate surface.
  • the latter In this case, there is an advantage that the device can be reduced in size, but gaseous molecules in the central portion of the inverted triangular pyramid at the highest concentration do not precipitate on the substrate surface, so that the inner surface of the device other than the substrate surface can be used. The problem of precipitation is even greater.
  • the organic EL material deposited on the surface other than the substrate surface falls into the evaporation source as it is deposited, and may be co-deposited. It is important that the material deposited on these parts is not altered.
  • the organic EL material to be vapor-deposited is an expensive organic compound, and it is desired to recover and reuse the organic EL material. Therefore, in order to collect and recycle the material deposited on the inner wall of the equipment other than the substrate, it is important that the organic EL material is not deteriorated.
  • the material of the part where the gaseous molecules of the organic EL material are deposited such as the vacuum chamber itself, the shutter that is installed in the chamber and the so-called anti-adhesion plate Austenitic stainless steel (sometimes abbreviated as SUS), which is inexpensive, has good workability, and is excellent in anti-dust properties, is often used as the material of components such as objects.
  • SUS anti-adhesion plate Austenitic stainless steel
  • an organic metal complex compound such as 8—hydroxyquinoline aluminum (sometimes abbreviated as A 1 q 3), which is known as a typical organic EL material
  • the SUS plate has It is possible that iron and aluminum in the organometallic complex undergo a metal exchange reaction to form an 8-year-old xyquinoline iron complex. This 8-year-old xyquinoline iron complex also vaporizes.
  • the organic EL material is corrosive or forms an oxidizing atmosphere, Live. Even if the organic EL material does not contain metal elements and is not corrosive, temperature changes occur repeatedly due to the operation and shutdown of the device, resulting in the thermal expansion of the strongly adhered organic EL material and SUS metal plate.
  • an object of the present invention is to prevent deterioration or contamination of an organic EL material.
  • a method of manufacturing an organic EL device capable of producing a good quality organic EL device with good yield, and an apparatus used therefor The purpose is to provide.
  • the method for producing an organic EL device is a method for producing an organic EL thin film, wherein an organic material for an organic EL device is vaporized and deposited on a film forming substrate to form a thin film.
  • an organic EL thin film is deposited by using the inner wall surface of the device on which the liquid is deposited and the components installed inside the device as a material that is inert to the organic material.
  • the organic EL thin film deposition apparatus of the present invention is an organic EL thin film deposition method for vaporizing an organic material for an organic EL element and depositing the organic material on a deposition substrate to form a thin film.
  • a shutter is preferably exemplified as the component. It is also preferable that at least the surface layer of the inner wall surface of the device and the components installed inside the device be made of a material inert to a vaporized organic material.
  • FIG. 1 is a cross-sectional view showing an example of an apparatus for vapor-depositing an organic EL device according to the present invention. It is composed of a chamber 1, an evaporation source 2, an organic EL material 3, a substrate 4, shutters 5 and 6. ing. BEST MODE FOR CARRYING OUT THE INVENTION
  • FIG. 1 is a schematic sectional view showing an example of the device of the present invention.
  • the vacuum deposition apparatus includes a chamber 11 that can be evacuated, an evaporating source 2 such as a crucible disposed in a chamber 1, and holding means (not shown) for holding a substrate 4 at a predetermined position.
  • evaporating source 2 such as a crucible disposed in a chamber 1
  • holding means for holding a substrate 4 at a predetermined position.
  • shutters 5 and 6, which substantially control the timing of deposition, are provided as parts.
  • the shutter 5 is provided near the evaporation source and the shutter 6 is provided near the substrate, it is possible to provide only one of them.
  • the chamber 11 has a structure that can be depressurized by a vacuum pump or the like, and also can take in and out an organic EL material and a substrate to be charged therein. Then, the evaporation source 2 is heated, the pressure inside the chamber 11 is reduced, and the organic EL material 3 charged in the evaporation source is vaporized (evaporated or sublimated) at a constant rate as much as possible. ) To monitor or control the vaporization rate, and release the shutters 5 and 6 when the vaporization rate becomes constant, or control the degree of opening of the shutters 5 and 6 according to the vaporization rate, so that the substrate 4 It controls the rate, amount or thickness of the organic EL material to be attached.
  • the shape of the container of the evaporation source is a crucible, but is not limited to this. Although only one evaporation source 2 is shown, a plurality of evaporation sources may be provided.
  • the shutters 5 and 6 are illustrated in the chamber 11 as components located at the position where the organic EL material adheres, in order to simplify the drawing and facilitate understanding, Often have other components installed.
  • an anti-adhesion plate may be installed that can be attached and detached mainly to reduce the work of cleaning materials deposited on the inner wall of the chamber. This adhesion-preventing plate is formed by bending a thin SUS plate and installing it inside the chamber along the inner wall of the chamber, and is often installed separately for easy attachment and detachment.
  • the organic EL material is a material for forming the light emitting layer
  • an organometallic complex is often used.
  • the complex metal comes in contact with a dissimilar metal at a high temperature, a certain percentage of metal exchange, that is, deterioration occurs. Therefore, materials other than the substrate on which the organometallic complex is deposited must be inert to the organometallic complex. The organometallic complex is altered.
  • the site where the organometallic complex is deposited includes the inner wall of the chamber 11, the shutters 5 and 6 facing the evaporation source, and a so-called anti-adhesion plate.
  • the components such as the chamber 1 and the shutters 5 and 6 may be made of one kind of material such as a metal material, or may be made of two or more layers of materials. It is preferable that at least the material of the surface layer to be precipitated be a material inert to the organic EL material. Instead of using an inert material for the chamber 11, a so-called anti-adhesion plate may be used for the inert material.
  • the inert material as referred to in the present invention means a material which does not cause deterioration, decomposition, contamination or the like of the organic EL material as well as the material itself in contact with the organic EL material. Specifically, it refers to a material that is generated due to contact between the material of the chamber 11 or the like and the organic EL material, but includes a material that is corroded or deteriorated due to its atmosphere. However, it does not mean that the organic EL material simply decomposes by thermal decomposition, but only that which promotes it and actually causes corrosion, alteration and contamination in the atmosphere.
  • Materials preferably used in the present invention include precious metals such as gold, heat-resistant resins such as fluorine resin, polyimide resin and silicon resin, quartz glass, pyrex, hard glass, and the like.
  • Examples include nonmetallic materials such as glasses such as enamel, alumina, silicon nitride, ceramics such as ceramics, and the like. They can be selected as appropriate from the viewpoints of workability and cost.
  • Suitable inert materials include metals, glasses such as enamel, fluororesins, and ceramics. Of these, materials that have no strength or are difficult to mold It is advantageous that the quality or expensive material is made inactive only in the surface layer by means such as thin film deposition and plating.
  • a noble metal which does not cause a metal exchange reaction with the metal or a material having at least the same metal material as the metal on its surface can be used.
  • a material whose surface is aluminum clad can be used.
  • a predetermined amount of the organic EL material 3 to be vapor-deposited is charged into the steam source 2. Further, the substrate 4 on which some layers may be already provided by evaporation or the like is set with the surface to be evaporated facing the evaporation source 2 side. It is advantageous in terms of deposition rate that the substrate 4 is located almost directly above the evaporation source 2, but when the shutter is opened and closed ⁇ ⁇ When the substrate is replaced, there is a risk that the deposits fall into the evaporation source 2 However, if the vapor deposition apparatus of the present invention is used, even in such a case, since there is no alteration or contamination of the deposits, the problem caused thereby can be solved.
  • the temperature of the evaporation source 2 and its surrounding evaporator may be a temperature at which a predetermined vapor pressure of the organic EL material 3 is obtained. Normally, this vapor pressure is about 1 0- 8 Torr several Torr.
  • the shutter covers the evaporation source or substrate because the vaporization rate is not stable. The vaporization rate is monitored by a film thickness sensor, etc., and when the vaporization rate is stabilized, the evaporation source or the shutters 5 and 6 covering the substrate are opened to start vapor deposition on the substrate.
  • Organic EL materials are limited to metal complexes such as A1q3.
  • the present invention is applicable to all organic EL materials used for manufacturing an organic EL device. Examples Hereinafter, specific examples of the present invention will be described based on examples.
  • High-purity 8-hydroxyhydroxylinoleum (Alq3) was deposited on the substrate using the deposition equipment shown in Fig.1.
  • the material of shutters 5 and 6 was SUS304.
  • the collected Alq3 was collected and used as a light emitting layer and an electron transporting layer.
  • a layer was formed on the ITO transparent electrode of the glass substrate on which the ITO film had already been formed.
  • ⁇ , -di- (naphthalene-tolyl)- ⁇ , ⁇ , -diphenyl-benzidine (hereinafter referred to as ⁇ ⁇ ⁇ ) as a hole transport layer, followed by A 1 q 3
  • a multilayer device with an aluminum-lithium cathode was fabricated. The thickness of the organic material was set to 50 nm, the electrode was set to IT ⁇ , and the thickness of the electrode was set to 20 nm for both aluminum and lithium. Observation of this device with a fluorescence microscope immediately after the sealing revealed several dark spots per 1000 ⁇ m square.
  • the molten aluminum plating was applied to the shutter, and the other conditions were the same as in Comparative Example 1. In this case, A 1 q 3 was deposited. No metal-exchanged complex was detected in A1q3 deposited on the shutter 5 facing the evaporation source near the evaporation source after the evaporation was completed.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroluminescent Light Sources (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention concerne un procédé de production d'un élément EL organique ayant de bonnes performances, à savoir l'élément EL organique est difficilement dégénéré lorsque la matière EL organique est déposée par évaporation sous vide sur un substrat ainsi qu'un dispositif mettant en oeuvre ce procédé. On fait appel également à un procédé de dépôt par évaporation sous vide d'un élément EL organique qui utilise un dispositif de dépôt par évaporation sous vide d'un élément EL organique, dans lequel les matières organiques de composants déposées, à savoir une chambre ou un obturateur (5, 6), ajoutées à un substrat formant un film, sont des composants inactifs qui ne dégénèrent pas la matière organique lors d'une opération de dépôt sur un film fin EL organique qui consiste à évaporer la matière EL organique dans une source d'évaporation et à la déposer sur un substrat formant un film (4) afin d'obtenir un film mince.
PCT/JP2001/011192 2000-12-22 2001-12-20 Procede de production et dispositif utilises avec un element el organique WO2002052903A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020037007313A KR100788152B1 (ko) 2000-12-22 2001-12-20 유기 ｅｌ 소자의 제조 방법 및 장치

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2000-390428 2000-12-22
JP2000390428A JP2002190389A (ja) 2000-12-22 2000-12-22 有機ｅｌ素子の製造方法及び装置

Publications (1)

Publication Number Publication Date
WO2002052903A1 true WO2002052903A1 (fr) 2002-07-04

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PCT/JP2001/011192 WO2002052903A1 (fr) 2000-12-22 2001-12-20 Procede de production et dispositif utilises avec un element el organique

Country Status (5)

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JP (1) JP2002190389A (fr)
KR (1) KR100788152B1 (fr)
CN (1) CN100337340C (fr)
TW (1) TW546394B (fr)
WO (1) WO2002052903A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005149924A (ja) * 2003-11-17 2005-06-09 Toray Ind Inc 蒸着装置および蒸着材料の回収・再利用方法並びに有機電界発光装置の製造方法。
WO2012086535A1 (fr) 2010-12-23 2012-06-28 シャープ株式会社 Procédé de récupération de matière filmogène
WO2012090772A1 (fr) * 2010-12-27 2012-07-05 シャープ株式会社 Dispositif de dépôt, outil de coupe et procédé de collecte de matériau de dépôt en phase vapeur
CN103270187A (zh) 2010-12-27 2013-08-28 夏普株式会社 蒸镀装置和回收装置

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08111285A (ja) * 1994-10-07 1996-04-30 Tdk Corp 有機エレクトロルミネセンス素子の製造方法及びその装置
JPH10168559A (ja) * 1996-12-06 1998-06-23 Ulvac Japan Ltd 有機薄膜形成装置及び有機材料の再利用方法
JPH10195641A (ja) * 1997-01-09 1998-07-28 Ulvac Japan Ltd 有機薄膜形成装置
JPH11229123A (ja) * 1998-02-12 1999-08-24 Casio Comput Co Ltd 蒸着装置

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1188516A (zh) * 1996-04-01 1998-07-22 东丽株式会社 带薄膜基板的制造方法和制造装置
JP3899566B2 (ja) * 1996-11-25 2007-03-28 セイコーエプソン株式会社 有機ｅｌ表示装置の製造方法
US6208075B1 (en) * 1998-11-05 2001-03-27 Eastman Kodak Company Conductive fluorocarbon polymer and method of making same
JP3742567B2 (ja) * 2000-06-22 2006-02-08 松下電工株式会社 真空蒸着装置及び真空蒸着方法
JP2002203682A (ja) * 2000-10-26 2002-07-19 Semiconductor Energy Lab Co Ltd 発光装置及びその作製方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08111285A (ja) * 1994-10-07 1996-04-30 Tdk Corp 有機エレクトロルミネセンス素子の製造方法及びその装置
JPH10168559A (ja) * 1996-12-06 1998-06-23 Ulvac Japan Ltd 有機薄膜形成装置及び有機材料の再利用方法
JPH10195641A (ja) * 1997-01-09 1998-07-28 Ulvac Japan Ltd 有機薄膜形成装置
JPH11229123A (ja) * 1998-02-12 1999-08-24 Casio Comput Co Ltd 蒸着装置

Also Published As

Publication number Publication date
CN1483300A (zh) 2004-03-17
KR20030072553A (ko) 2003-09-15
TW546394B (en) 2003-08-11
KR100788152B1 (ko) 2007-12-21
CN100337340C (zh) 2007-09-12
JP2002190389A (ja) 2002-07-05

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