WO2013011741A1 - Organic electroluminescence panel and method of manufacturing same - Google Patents

Organic electroluminescence panel and method of manufacturing same Download PDF

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Publication number
WO2013011741A1
WO2013011741A1 PCT/JP2012/063547 JP2012063547W WO2013011741A1 WO 2013011741 A1 WO2013011741 A1 WO 2013011741A1 JP 2012063547 W JP2012063547 W JP 2012063547W WO 2013011741 A1 WO2013011741 A1 WO 2013011741A1
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layer
organic
sheet
electrode
adhesive layer
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PCT/JP2012/063547
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French (fr)
Japanese (ja)
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功太郎 菊地
真人 奥山
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コニカミノルタホールディングス株式会社
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    • 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
    • H05B33/02—Details
    • H05B33/04—Sealing arrangements, e.g. against humidity
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/80—Constructional details
    • H10K59/87—Passivation; Containers; Encapsulations
    • H10K59/874—Passivation; Containers; Encapsulations including getter material or desiccant

Definitions

  • the present invention relates to an organic electroluminescence panel, and more particularly to an organic electroluminescence panel sealed with a barrier film and a method for producing the same.
  • a barrier film in which aluminum is laminated on the surface of a plastic substrate or film is used to prevent alteration of articles that require blocking of various gases such as water vapor and oxygen, for example, food, industrial supplies, and pharmaceuticals. Widely used in packaging applications.
  • organic electronic device substrate for liquid crystal display elements, photoelectric conversion elements (solar cells), organic electroluminescence (hereinafter abbreviated as organic EL) elements, and the like.
  • the surface of these electronic devices is covered with a curable resin adhesive layer, or the surface of the barrier film is covered with an adhesive, and the barrier film is surface-bonded to the surface of the organic EL element and sealed by thermocompression bonding.
  • Technology to stop is proposed.
  • a getter material that absorbs oxygen and moisture is formed on the organic EL element, an adhesive layer is formed on the other sealing member, and they are bonded together to form an adhesive for the organic EL element.
  • a getter material that absorbs oxygen and moisture is formed on the organic EL element, an adhesive layer is formed on the other sealing member, and they are bonded together to form an adhesive for the organic EL element.
  • An organic EL panel in which a sealing member is formed on a second electrode of an organic EL element having a first electrode, an organic EL layer, and a second electrode on a flexible substrate, and a method for manufacturing the same,
  • An object of the present invention is to provide an organic EL panel having excellent performance easily by a simple manufacturing process.
  • an organic electroluminescent panel which has a 1st electrode, an organic electroluminescent layer, a 2nd electrode, and a sealing member in this order on a flexible base material, this sealing member adheres in an order from the 2nd electrode side.
  • An organic electroluminescence panel comprising: an agent layer; a sheet-like hygroscopic layer having a hygroscopic layer formed on a support; an adhesive layer; and a barrier film.
  • the sheet-like hygroscopic agent layer is a sheet-like material which is previously formed on a support by containing a hygroscopic agent in a binder.
  • a sheet-like hygroscopic layer having a pressure-sensitive adhesive layer on one side and a hygroscopic layer formed on the other side is bonded so that the pressure-sensitive adhesive layer is in contact with the second electrode.
  • a sheet-like adhesive layer comprising a sheet-like adhesive layer formed on a releasable support and peeled off from the releasable support and bonded to the barrier film. Are bonded so as to be in contact with the sheet-like hygroscopic agent layer to form a sealing member, and a method for producing an organic electroluminescence panel.
  • a hygroscopic agent is disposed on the second electrode.
  • an adhesive layer is provided on one surface of the sheet-like hygroscopic layer formed between two supports in advance, and the adhesive layer is bonded so as to contact the second electrode,
  • a barrier film having an adhesive layer in which an adhesive layer formed in advance on a support is peeled off from the releasable support and bonded to the barrier film, and the adhesive layer absorbs moisture.
  • an adhesive material layer is provided between the second electrode of the organic EL element and the sheet-like moisture absorbent layer, and further on the sheet-like moisture absorbent layer.
  • the element that the first electrode, the electroluminescence layer, and the second electrode have in this order on the flexible substrate is defined as an organic EL element, and the organic EL element is sealed with a sealing member.
  • the stopped panel is defined as an organic EL panel.
  • FIG. 1 is a cross-sectional view showing a preferred example of the layer structure of the organic EL panel of the present invention.
  • an organic EL panel 100 has an organic EL element in which a first electrode 12 is formed on a flexible substrate 11, an organic EL layer 13 is formed thereon, and a second electrode 14 is formed thereon.
  • the sealing member 50 is bonded onto the second electrode.
  • the sealing member 50 includes, in order from the second electrode side, a pressure-sensitive adhesive layer 21, a sheet-like moisture absorbent layer 20, an adhesive layer 30, and a barrier film 40.
  • the sheet-like moisture absorbent layer 20 is a support. 22, a hygroscopic agent layer 23, and a support 23.
  • the support body 23 may be used or not used depending on necessity, and the support body 23 used is the most preferable embodiment of the present invention.
  • FIG. 2 schematically shows a method for forming these laminated structures. Formed by laminating a pressure-sensitive adhesive layer 21 and a sheet-like hygroscopic layer 20 on the organic EL element 10 and further laminating a barrier film 40 having a sheet-like adhesive layer 30 on one surface from above. can do.
  • FIG. 3 shows an example of the manufacturing method of the organic EL panel of the present invention, which uses a flexible base material that continuously runs.
  • FIG. 3A shows a sheet-like hygroscopic layer 20 having a pressure-sensitive adhesive layer 21 and a sheet-like adhesive layer on a continuously running organic EL element in which a plurality of organic EL elements are formed on a flexible substrate.
  • 3 and FIG. 3 (b) are diagrams showing a production method for laminating 30 and the barrier film 40, and FIG. It is a figure which shows the manufacturing method which transfers and bonds the barrier film 40 in which the sheet-like adhesive layer 30 was formed. In either case, after being transferred by a vacuum laminator or a pressure bonding machine, the adhesive layer is cured, and an organic EL panel is formed through a cutting step 60.
  • the flexible substrate referred to in the present invention refers to a flexible substrate, and it is preferable that the light transmittance is usually 80% or more from various resin films, and the oxygen transmittance and humidity transmittance are low.
  • thin glass having a thickness of about 200 ⁇ m or less can also be used as the flexible substrate, and is included in the concept of flexible substrate here.
  • the organic EL element in the present invention is formed by sequentially laminating at least a first electrode (transparent electrode), an organic EL layer, and a second electrode on the flexible substrate.
  • a sealing member comprising an adhesive layer, a sheet-like hygroscopic layer, an adhesive layer, and a barrier film is provided on the second electrode of the organic EL element, although the barrier film basically prevents moisture from entering from the outside, even if moisture enters the barrier film, it is absorbed by the hygroscopic layer and does not reach the organic EL element. .
  • the pressure-sensitive adhesive layer, sheet-like hygroscopic agent layer, adhesive layer and barrier film constituting the sealing member of the present invention will be described sequentially.
  • the sheet-like hygroscopic layer used in the present invention is one in which a hygroscopic layer containing a binder resin component and a hygroscopic component is formed on a support.
  • the binder resin component it is necessary that the moisture-absorbing agent component does not inhibit the moisture adsorption action, and a material having high gas permeability is preferably used.
  • a material having high gas permeability is preferably used.
  • polymer materials such as polyolefin-based, polyacrylic-based, polyacrylonitrile-based, polyamide-based, polyester-based, epoxy-based, polycarbonate-based, and fluorine-based materials can be exemplified.
  • the hygroscopic component is preferably a compound having a moisture adsorption function, and particularly a compound that chemically adsorbs moisture and maintains a solid state even after adsorption.
  • a compound having a moisture adsorption function and particularly a compound that chemically adsorbs moisture and maintains a solid state even after adsorption.
  • metal oxides, metal inorganic acid salts and organic acid salts, and the like can be mentioned.
  • the alkaline earth metal oxide include calcium oxide (CaO), barium oxide (BaO), and magnesium oxide (MgO).
  • sulfate examples include lithium sulfate (Li 2 SO 4 ), sodium sulfate (Na 2 SO 4 ), potassium sulfate (CaSO 4 ), magnesium sulfate (MgSO 4 ), cobalt sulfate (CoSO 4 ), and gallium sulfate (Ga). 2 (SO 4 ) 3 ), titanium sulfate (Ti (SO 4 ) 2 ), nickel sulfate (NiSO 4 ), and the like.
  • hygroscopic silica powder, molecular sieve powder, and the like can also be used.
  • the sheet-like hygroscopic layer As a method for forming the sheet-like hygroscopic layer, 5 to 40% by mass of the binder resin component and 95 to 60% by mass of the hygroscopic component are uniformly mixed, and melted or cast on a support using a solvent.
  • the sheet-like hygroscopic agent layer can be formed by coating and drying.
  • the sheet-like hygroscopic layer of the present invention is more preferably a sandwich type in which the hygroscopic layer is sandwiched between two supports.
  • the sheet-like hygroscopic layer may contain other additives as necessary.
  • the film thickness is preferably 10 to 300 ⁇ m.
  • the elastic modulus is preferably in the range of 10 to 100 MPa in the range of the lamination temperature of 80 to 200 ° C.
  • Adhesive layer In this invention, it has the adhesive layer between the support body which a sheet-like moisture absorbent layer has, and the 2nd electrode of an organic EL element, It is characterized by the above-mentioned.
  • the pressure-sensitive adhesive layer referred to in the present invention is a material that does not require the help of heat or a solvent and can be applied to other subjects with extremely low pressure such as finger pressure, and is made of a material such as rubber, acrylic or silicone. You can choose.
  • a pressure-sensitive adhesive having a storage elastic modulus at 25 ° C. in the range of 1.0 ⁇ 10 4 to 1.0 ⁇ 10 9 Pa in at least a part of the pressure-sensitive adhesive layer is preferably used.
  • a curable pressure-sensitive adhesive that forms a high molecular weight body or a crosslinked structure by various chemical reactions after being applied and bonded may be used.
  • urethane adhesives examples include, for example, urethane adhesives, epoxy adhesives, aqueous polymer-isocyanate adhesives, curable adhesives such as thermosetting acrylic adhesives, moisture-curing urethane adhesives, polyether methacrylate types
  • curable adhesives such as thermosetting acrylic adhesives, moisture-curing urethane adhesives, polyether methacrylate types
  • anaerobic pressure-sensitive adhesives such as ester-based methacrylate type and oxidized polyether methacrylate, cyanoacrylate-based instantaneous pressure-sensitive adhesives, and acrylate-peroxide-based two-component instantaneous pressure-sensitive adhesives.
  • the above-mentioned pressure-sensitive adhesive may be a one-component type or a type in which two or more components are mixed before use.
  • Adhesive layer Next, the adhesive layer used in the present invention will be described.
  • the adhesive layer of the present invention it is preferable to use an adhesive resin coated on a releasable support and formed into a sheet shape.
  • the adhesive layer is formed in a sheet shape previously formed on an organic EL element. Transfer onto the hygroscopic layer or transfer onto the barrier film in advance, peel off the releasable support, and bond the barrier film having the adhesive layer onto the sheet-like hygroscopic layer Is preferred.
  • thermosetting adhesive resin an ultraviolet curable adhesive resin, or the like can be used.
  • thermosetting adhesive resin for example, phenol resin, silicone resin, allyl ester, acrylic resin, epoxy resin, polyimide, or urethane resin can be used.
  • the ultraviolet curable adhesive resin for example, a silicone resin, an acrylic resin, an epoxy resin, a polyimide, or a urethane resin can be used.
  • curable adhesive resins can be obtained as commercial products.
  • Barrier film Although it will not specifically limit as a gas barrier film used for this invention if it has a barriering laminated body on a base film, The thing similar to the flexible base material of an organic EL element can be used. Thin glass having a thickness of about 200 ⁇ m or less may be used, and a humidity transmittance of 10 ⁇ 5 g / m 2 / day or less is preferable.
  • Organic EL element forming step First electrode 12 is formed on flexible substrate 11 directly or via another layer, organic EL layer 13 including a light emitting layer is formed on first electrode 12, and an organic layer is formed. By forming the second electrode 14 on 13, the organic EL element 10 is formed.
  • the organic EL element 10 may be formed of a plurality of organic EL elements on a continuous flexible substrate 11 or may be formed on a single wafer.
  • the conductive material of the first electrode 12 is formed on the substrate 11 that has been subjected to surface processing and cleaning by a film formation method such as sputtering or vapor deposition, and, for example, one pixel is formed by a photolithography process.
  • a film formation method such as sputtering or vapor deposition
  • one pixel is formed by a photolithography process.
  • Four units of 20 ⁇ 16.5 mm are formed in a four-column shape (a total area of 41 ⁇ 34 mm for four pixels), and one unit of the first electrode 12 is formed.
  • the organic EL layer 13 is sequentially stacked on the pixel area of the partitioned first electrode 12.
  • the organic EL layer 13 is formed, for example, by sequentially depositing a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, and the like by vacuum deposition. . After that, the second electrode 14 is formed on the organic EL layer 13 in the same manner as the first electrode 12 in a quadrant.
  • the sheet-like hygroscopic layer 20 has a hygroscopic agent layer 23 formed on a support 22 in advance, and a support 24 on which a sandwich structure is formed.
  • a pressure-sensitive adhesive layer 21 is formed on one support, and a sheet-like hygroscopic layer 20 formed so as to cover the entire organic EL element portion is used so that the pressure-sensitive adhesive layer 21 is in contact with the second electrode 14. It is arranged on the organic EL element 10.
  • Adhesive layer forming step the adhesive layer 30 is a sheet-like adhesive layer formed in such a width that the adhesive layer 30 is previously formed on the releasable support 31 and covers the flexible substrate of the organic EL element. 30 and is placed in contact with the hygroscopic layer.
  • Bonding step sealing the flexible substrate 11 with the sheet-like moisture absorbent layer 20, the sheet-like adhesive layer 30 and the barrier film 40 having the pressure-sensitive adhesive layer 21 on the organic EL element so as to cover at least the entire organic EL element portion.
  • the barrier film 40 of the stopper member 50 is bonded via the adhesive layer 30.
  • the flexible substrate 11 and the sealing member 50 are pressure-bonded with a predetermined pressure, and heated as necessary to cure the adhesive.
  • the sealing structure can be easily formed by the method of the present invention as described above. That is, by adopting a structure in which the surface of the organic EL element and the sheet-like hygroscopic layer are bonded via an adhesive layer, there are few failures immediately after form, and the light emitting function of the organic EL element can be maintained even during storage over time. It was possible to maintain it well, and an organic EL panel having a reduced thickness and high strength could be obtained.
  • the organic EL element used in the present invention uses a 200 ⁇ m glass substrate as a support, and a substrate on which an ITO (indium tin oxide) film is deposited as a first electrode, and is patterned by a lithography method. A known organic EL layer and a second electrode were formed thereon to form an organic EL element.
  • ITO indium tin oxide
  • the organic EL element obtained as described above is a four-part light emission pattern having a light emission pattern of 20 ⁇ 16.5 mm ⁇ 4 pixels (a total area of 41 ⁇ 34 mm for four pixels).
  • Procedure b Next, the following adhesive A was applied on the aluminum surface of the barrier film prepared in Procedure a.
  • Procedure d The adhesive layer surface of the barrier film prepared by applying the adhesive in Procedure b and the PET surface of the hygroscopic sheet were placed together.
  • Procedure e The organic EL device, the hygroscopic sheet, and the barrier film prepared in Procedure d are pressure-bonded at 100 ° C. for 60 seconds at a pressing force of 0.1 MPa in a reduced pressure environment of 1 ⁇ 10 ⁇ 2 Pa using a vacuum laminator. Further, as a curing treatment, heating was performed at 100 ° C. for 30 minutes, and the organic EL panel no. 1 was produced.
  • sealing configuration 4 The procedures b and d of the sealing configuration 3 are the same as those of the sealing configuration 2, and the organic EL panel No. 4 was produced.
  • the adhesive used is shown below.
  • Adhesive A Thermosetting adhesive (Struct Bond E-413, manufactured by Mitsui Chemicals, Inc.)
  • Adhesive B UV curable adhesive (ThreeBond 3124C, manufactured by Three Bond Co., Ltd.) ⁇ Evaluation of organic EL panel >> About each produced organic EL panel, the generation
  • the organic EL panel was stored in an environmental condition of 60 ° C. and 90% RH. The panel was turned on immediately after the organic EL panel was fabricated and after 300 hours had elapsed after storage, and the number of dark spots (spot-like non-light-emitting portions) and the subsequent generation ratio were observed by area. For lighting the panel, a DC voltage of 5 V was applied to one pixel of the organic EL element using a constant voltage power source. Evaluation was performed by the number or occurrence rate (area ratio) of 4 pixels (41 ⁇ 34 mm). The obtained results are shown in Table 1.
  • the sample of the present invention has a small number of dark spots generated immediately after formation, and has a low dark spot generation rate even after storage, and maintains excellent performance.

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  • Manufacturing & Machinery (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

Provided is an organic electroluminescence panel having superior performance with ease by a simple manufacturing process. An organic electroluminescence panel comprises, upon a flexible substrate, in this order: a first electrode; an organic electroluminescence layer; a second electrode; and a sealing member. The sealing member has, stacked in order from the second electrode side, an adhesive layer, a sheet-shaped moisture absorption agent layer in which an absorption layer is formed upon a support body, a bonding agent layer, and a barrier film.

Description

有機エレクトロルミネッセンスパネル及びその製造方法Organic electroluminescence panel and manufacturing method thereof
　本発明は有機エレクトロルミネッセンスパネルに関し、特にバリアフィルムにより封止された有機エレクトロルミネッセンスパネル及びその製造方法に関する。 The present invention relates to an organic electroluminescence panel, and more particularly to an organic electroluminescence panel sealed with a barrier film and a method for producing the same.
　従来から、プラスチック基板やフィルムの表面にアルミニウムをラミネートしたバリア性フィルムは、水蒸気や酸素等の各種ガスの遮断を必要とする物品、例えば、食品、工業用品および医薬品等の変質を防止するための包装用途に広く用いられている。 Conventionally, a barrier film in which aluminum is laminated on the surface of a plastic substrate or film is used to prevent alteration of articles that require blocking of various gases such as water vapor and oxygen, for example, food, industrial supplies, and pharmaceuticals. Widely used in packaging applications.
　また、包装用途以外にも液晶表示素子、光電変換素子（太陽電池）、有機エレクトロルミネッセンス（以下有機ＥＬと略す。）素子等の有機電子デバイス基板として使用されている。 In addition to packaging applications, it is used as an organic electronic device substrate for liquid crystal display elements, photoelectric conversion elements (solar cells), organic electroluminescence (hereinafter abbreviated as organic EL) elements, and the like.
　これらの有機電子デバイスは水分や酸素によって著しくその機能が低下するという問題がある。そこで、これらの有機電子デバイスを水分、酸素等の外気から遮断し、封止する技術が提案されている。 These organic electronic devices have a problem that their functions are remarkably lowered by moisture and oxygen. In view of this, a technique has been proposed in which these organic electronic devices are sealed off from the outside air such as moisture and oxygen.
　例えば、これらの電子デバイスの表面を硬化性樹脂接着剤層で覆う技術、或いはバリア性フィルムの表面を接着剤で覆い、該バリアフィルムを有機ＥＬ素子の表面に面接着し熱圧着することにより封止する技術が提案されている。 For example, the surface of these electronic devices is covered with a curable resin adhesive layer, or the surface of the barrier film is covered with an adhesive, and the barrier film is surface-bonded to the surface of the organic EL element and sealed by thermocompression bonding. Technology to stop is proposed.
　しかしながら、これらの技術には下記の様な課題があった。 However, these technologies have the following problems.
　即ち、
　（ｉ）バリアフィルムの防湿性だけでは有機ＥＬの長寿命化は困難である
　（ii）封止時に混入した異物を圧迫することで有機ＥＬ層へダメージを与えてしまう
　（iii）封止熱によって接着剤から悪影響成分が有機ＥＬ層へ浸透しダークスポット（ＤＳ）となる
　更なる高度な防湿技術として、有機ＥＬ素子とバリアフィルムとの間に吸湿剤粉末をバインダー樹脂に分散させた吸湿シートを配置し、該吸湿シートと有機ＥＬ素子とを面接着する技術が開示されている（例えば、特許文献１参照。）。 That is,
(I) It is difficult to extend the life of the organic EL only by the moisture resistance of the barrier film. (Ii) The organic EL layer is damaged by pressing the foreign matter mixed at the time of sealing. Adverse components from the adhesive penetrate into the organic EL layer and become dark spots (DS) As a further advanced moisture-proof technology, a moisture-absorbing sheet in which moisture-absorbing powder is dispersed in a binder resin between the organic EL element and the barrier film is used. A technique for arranging and adhering the moisture absorbing sheet and the organic EL element to each other is disclosed (for example, see Patent Document 1).
　更に、バインダー樹脂と吸湿剤成分に加え、柔軟性を有する粒子状樹脂を含有するシート状吸湿剤層を有機ＥＬ素子表面に用いる技術が開示されている（例えば、特許文献２参照。）。 Furthermore, a technique of using a sheet-like hygroscopic layer containing a flexible particulate resin in addition to the binder resin and the hygroscopic component on the surface of the organic EL element is disclosed (for example, see Patent Document 2).
　また、酸素や水分を吸収するゲッター材（吸湿剤）を有機ＥＬ素子上に形成し、もう一方の封止部材に接着剤層を形成し、それらを貼り合わせることにより有機ＥＬ素子には接着剤が直接接しない様にする方法が開示されている（特許文献３参照。）。 Also, a getter material (hygroscopic agent) that absorbs oxygen and moisture is formed on the organic EL element, an adhesive layer is formed on the other sealing member, and they are bonded together to form an adhesive for the organic EL element. Has been disclosed (see Patent Document 3).
　このような新たな吸湿剤層を用いた防湿技術が開示されてきているが、まだまだ十分なレベルまで至っていず、例えば、バリアフィルムと吸湿剤層は接着されていないため界面が弱く、外力に対して脆弱であったり、またシート状吸湿剤が直接有機ＥＬ素子に接触し、その上からバリアフィルムを面圧着させるため、圧着時に吸湿剤粉末が第２の電極や有機層を破壊してしまい、ダークスポットの原因となっていた。これらを改良する技術として、更に柔軟性を持つ粒子状樹脂を含有させることにより、圧力を緩和しリーク電流の発生を抑制する技術（特許文献２）が開示されているが、未だ不十分であった。 Although a moisture-proof technique using such a new moisture absorbent layer has been disclosed, it has not yet reached a sufficient level.For example, the barrier film and the moisture absorbent layer are not bonded, so the interface is weak and external force is not applied. The sheet-like hygroscopic agent is in direct contact with the organic EL element and the barrier film is pressed onto the surface of the barrier film, so that the hygroscopic powder destroys the second electrode and the organic layer during the pressure bonding. Was the cause of dark spots. As a technique for improving these, there is disclosed a technique (Patent Document 2) that reduces the pressure and suppresses the generation of leak current by containing a more flexible particulate resin, but it is still insufficient. It was.
特開平２－１９７０７１号公報Japanese Laid-Open Patent Publication No. 2-97071 特開２００９－２６６４８号公報JP 2009-26648 A 特開２０１１－２８８９６号公報JP 2011-28896 A
　フレキシブル基材上に、第１の電極、有機ＥＬ層、第２の電極を有する有機ＥＬ素子の第２の電極上に封止部材が形成された有機ＥＬパネルおよびその製造方法であって、簡単な製造プロセスにより、容易に、優れた性能を有する有機ＥＬパネルを提供することを目的とするものである。 An organic EL panel in which a sealing member is formed on a second electrode of an organic EL element having a first electrode, an organic EL layer, and a second electrode on a flexible substrate, and a method for manufacturing the same, An object of the present invention is to provide an organic EL panel having excellent performance easily by a simple manufacturing process.
　上記課題は、下記の本発明の構成により、解決することができた。 The above problem could be solved by the following configuration of the present invention.
　１．フレキシブル基材上に、第１の電極、有機エレクトロルミネッセンス層、第２の電極、封止部材をこの順で有する有機エレクトロルミネッセンスパネルにおいて、該封止部材が、第２の電極側から順に、粘着剤層、支持体上に吸湿剤層が形成されたシート状吸湿剤層、接着剤層およびバリアフィルムが積層されてなることを特徴とする有機エレクトロルミネッセンスパネル。 1. In the organic electroluminescent panel which has a 1st electrode, an organic electroluminescent layer, a 2nd electrode, and a sealing member in this order on a flexible base material, this sealing member adheres in an order from the 2nd electrode side. An organic electroluminescence panel comprising: an agent layer; a sheet-like hygroscopic layer having a hygroscopic layer formed on a support; an adhesive layer; and a barrier film.
　２．前記シート状吸湿剤層が、吸湿剤をバインダー中に含有させてあらかじめ支持体上に形成しシート状にしたものであることを特徴とする前記１に記載の有機エレクトロルミネッセンスパネル。 2. 2. The organic electroluminescence panel according to 1 above, wherein the sheet-like hygroscopic agent layer is a sheet-like material which is previously formed on a support by containing a hygroscopic agent in a binder.
　３．前記シート状吸湿剤層が、吸湿剤をバインダー中に含有させて、あらかじめ２枚の支持体に挟んで形成しシート状にしたものであることを特徴とする前記１または２に記載の有機エレクトロルミネッセンスパネル。 3. 3. The organic electrophoretic material according to 1 or 2 above, wherein the sheet-like hygroscopic agent layer is formed by previously containing a hygroscopic agent in a binder and sandwiching it between two supports. Luminescence panel.
　４．前記接着剤層が、接着剤をあらかじめ離形性支持体上に形成しシート状にしたものであることを特徴とする前記１～３の何れか１項に記載の有機エレクトロルミネッセンスパネル。 4. 4. The organic electroluminescence panel according to any one of 1 to 3, wherein the adhesive layer is a sheet formed by previously forming an adhesive on a releasable support.
　５．前記接着剤層が、熱硬化性樹脂であることを特徴とする前記１～４の何れか１項に記載の有機エレクトロルミネッセンスパネル。 5. 5. The organic electroluminescence panel according to any one of 1 to 4, wherein the adhesive layer is a thermosetting resin.
　６．フレキシブル基材上に、第１の電極、エレクトロルミネッセンス層、第２の電極、封止部材をこの順で有する有機エレクトロルミネッセンスパネルの製造方法であって、該第２の電極上に、支持体の一方の面に粘着剤層を有し、他方の面に吸湿剤層が形成されたシート状吸湿剤層を、粘着剤層が第２の電極と接するように貼り合わせ、次いで、接着剤をあらかじめ離形性支持体上に形成してシート状にしたシート状接着剤層を離形性支持体から剥がしてバリアフィルムと貼り合わせたシート状接着剤層を有するバリアフィルムを、シート状接着剤層がシート状吸湿剤層に接するように貼り合わせて、封止部材を形成したことを特徴とする有機エレクトロルミネッセンスパネルの製造方法。 6. A method for producing an organic electroluminescence panel having a first electrode, an electroluminescence layer, a second electrode, and a sealing member in this order on a flexible substrate, wherein the support is formed on the second electrode. A sheet-like hygroscopic layer having a pressure-sensitive adhesive layer on one side and a hygroscopic layer formed on the other side is bonded so that the pressure-sensitive adhesive layer is in contact with the second electrode. A sheet-like adhesive layer comprising a sheet-like adhesive layer formed on a releasable support and peeled off from the releasable support and bonded to the barrier film. Are bonded so as to be in contact with the sheet-like hygroscopic agent layer to form a sealing member, and a method for producing an organic electroluminescence panel.
　７．フレキシブル基材上に、第１の電極、エレクトロルミネッセンス層、第２の電極、封止部材をこの順で有する有機エレクトロルミネッセンスパネルの製造方法であって、該第２の電極上に、吸湿剤をバインダー中に含有させて、あらかじめ２枚の支持体に挟んで形成したシート状吸湿剤層の一方の面に粘着剤層を設け、粘着剤層が第２の電極と接するように貼り合わせ、次いで、接着剤をあらかじめ支持体上に形成してシート状にした接着剤層を離形性支持体からはがしてバリアフィルムと貼り合わせた接着剤層を有するバリアフィルムを、接着剤層がシート状吸湿剤層に接するように貼り合わせて、封止部材を形成したことを特徴とする有機エレクトロルミネッセンスパネルの製造方法。 7. A method for producing an organic electroluminescence panel having a first electrode, an electroluminescence layer, a second electrode, and a sealing member in this order on a flexible substrate, wherein a hygroscopic agent is disposed on the second electrode. In the binder, an adhesive layer is provided on one surface of the sheet-like hygroscopic layer formed between two supports in advance, and the adhesive layer is bonded so as to contact the second electrode, A barrier film having an adhesive layer in which an adhesive layer formed in advance on a support is peeled off from the releasable support and bonded to the barrier film, and the adhesive layer absorbs moisture. A method for producing an organic electroluminescence panel, wherein a sealing member is formed by bonding so as to be in contact with an agent layer.
　支持体上に吸湿剤層を有するシート状吸湿剤層を用い、有機Ｅｌ素子の第２の電極とシート状吸湿剤層との間に粘着材層を設け、更にシート状吸湿剤層の上に接着剤層およびバリアフィルムを積層することにより、簡便なプロセスにより、故障が無く、耐久性に優れた有機エレクトロルミネッセンスパネルを提供することができた。 Using a sheet-like moisture absorbent layer having a moisture absorbent layer on the support, an adhesive material layer is provided between the second electrode of the organic EL element and the sheet-like moisture absorbent layer, and further on the sheet-like moisture absorbent layer. By laminating the adhesive layer and the barrier film, it was possible to provide an organic electroluminescence panel having no failure and excellent durability by a simple process.
本発明の有機ＥＬパネルの層構成の好ましい一例を示す断面図である。It is sectional drawing which shows a preferable example of the laminated constitution of the organic electroluminescent panel of this invention. 本発明の有機ＥＬパネルの製造方法を模式的に示した図である。It is the figure which showed typically the manufacturing method of the organic electroluminescent panel of this invention. 本発明の連続走行するフレキシブル基材を用いた有機ＥＬパネルの製造方法の例を示す図である。It is a figure which shows the example of the manufacturing method of the organic electroluminescent panel using the flexible base material which runs continuously of this invention.
　本発明においては、フレキシブル基材上に、第１の電極、エレクトロルミネッセンス層、第２の電極がこの順で有する素子を有機ＥＬ素子と定義し、前記有機ＥＬ素子の上を封止部材で封止されたパネルを有機ＥＬパネルと定義する。 In the present invention, the element that the first electrode, the electroluminescence layer, and the second electrode have in this order on the flexible substrate is defined as an organic EL element, and the organic EL element is sealed with a sealing member. The stopped panel is defined as an organic EL panel.
　以下、本発明を図をもって説明する。 Hereinafter, the present invention will be described with reference to the drawings.
　図１は、本発明の有機ＥＬパネルの層構成の好ましい一例を示す断面図である。 FIG. 1 is a cross-sectional view showing a preferred example of the layer structure of the organic EL panel of the present invention.
　図１中、有機ＥＬパネル１００は、フレキシブル基板１１上に、第１の電極１２、その上に有機ＥＬ層１３、更にその上には第２の電極１４が形成された有機ＥＬ素子を有し、第２の電極上には、封止部材５０が貼合されている。封止部材５０は、第２の電極側から順に、粘着剤層２１、シート状吸湿剤層２０及び接着剤層３０及びバリアフィルム４０から構成されており、シート状吸湿剤層２０は、支持体２２、吸湿剤層２３、支持体２３を有している。なお、支持体２３は必要により用いても、用いなくても良く、支持体２３は用いたものが本発明の最も好ましい態様である。 In FIG. 1, an organic EL panel 100 has an organic EL element in which a first electrode 12 is formed on a flexible substrate 11, an organic EL layer 13 is formed thereon, and a second electrode 14 is formed thereon. The sealing member 50 is bonded onto the second electrode. The sealing member 50 includes, in order from the second electrode side, a pressure-sensitive adhesive layer 21, a sheet-like moisture absorbent layer 20, an adhesive layer 30, and a barrier film 40. The sheet-like moisture absorbent layer 20 is a support. 22, a hygroscopic agent layer 23, and a support 23. In addition, the support body 23 may be used or not used depending on necessity, and the support body 23 used is the most preferable embodiment of the present invention.
　これらの積層構造を形成する方法を模式的に示したのが、図２である。有機ＥＬ素子１０上に、粘着剤層２１、シート状吸湿剤層２０を積層し、更にその上から、一方の面にシート状接着剤層３０を有するバリアフィルム４０を貼合することにより、形成することができる。 FIG. 2 schematically shows a method for forming these laminated structures. Formed by laminating a pressure-sensitive adhesive layer 21 and a sheet-like hygroscopic layer 20 on the organic EL element 10 and further laminating a barrier film 40 having a sheet-like adhesive layer 30 on one surface from above. can do.
　また、本発明の有機ＥＬパネルの製造方法であって、連続走行するフレキシブル基材を用いた製造方法の例を図３に示した。 Further, FIG. 3 shows an example of the manufacturing method of the organic EL panel of the present invention, which uses a flexible base material that continuously runs.
　図３（ａ）は、フレキシブル基板上に複数の有機ＥＬ素子が形成された、連続走行する有機ＥＬ素子上に、順次、粘着剤層２１を有するシート状吸湿剤層２０、シート状接着剤層３０及びバリアフィルム４０を貼合する製造方法を示す図であり、図３（ｂ）は、予め形成されたシート状接着剤層３０から離形性支持体３１を剥離し、バリアフィルム４０上に転着し、シート状接着剤層３０が形成されたバリアフィルム４０を貼合する製造方法を示す図である。何れも真空ラミネーター或いは圧着機により転合された後、接着剤層を硬化し、断裁工程６０を経て、有機ＥＬパネルが形成される。 FIG. 3A shows a sheet-like hygroscopic layer 20 having a pressure-sensitive adhesive layer 21 and a sheet-like adhesive layer on a continuously running organic EL element in which a plurality of organic EL elements are formed on a flexible substrate. 3 and FIG. 3 (b) are diagrams showing a production method for laminating 30 and the barrier film 40, and FIG. It is a figure which shows the manufacturing method which transfers and bonds the barrier film 40 in which the sheet-like adhesive layer 30 was formed. In either case, after being transferred by a vacuum laminator or a pressure bonding machine, the adhesive layer is cured, and an organic EL panel is formed through a cutting step 60.
　以下、本発明に用いられる各材料について説明する。 Hereinafter, each material used in the present invention will be described.
　〔フレキシブル基材〕
　本発明で言うフレキシブル基材とは可撓性基材を指し、通常は種々の樹脂フィルムから、光透過率が８０％以上のもので有ることが好ましく、酸素透過率、湿度透過率が低いもので有れば特に限定されないが、これらに加えて、厚みが２００μｍ程度以下の薄板ガラスも可撓性基材として使用可能であり、ここで言うフレキシブル基材の概念に含めるものである。 [Flexible substrate]
The flexible substrate referred to in the present invention refers to a flexible substrate, and it is preferable that the light transmittance is usually 80% or more from various resin films, and the oxygen transmittance and humidity transmittance are low. In addition to these, thin glass having a thickness of about 200 μm or less can also be used as the flexible substrate, and is included in the concept of flexible substrate here.
　本発明における有機ＥＬ素子は、前記フレキシブル基材上に少なくとも第１の電極（透明電極）、有機ＥＬ層、第２の電極を順次積層して形成される。 The organic EL element in the present invention is formed by sequentially laminating at least a first electrode (transparent electrode), an organic EL layer, and a second electrode on the flexible substrate.
　本発明の有機ＥＬパネルは、前記有機ＥＬ素子の第２の電極上に、粘着剤層、シート状吸湿剤層、接着剤層、バリアフィルムからなる封止部材が設けられており、最も外側のバリアフィルムによって外部からの湿度の浸入を基本的に防止するが、例えバリアフィルム内に湿気が浸入したとしても、それを吸湿剤層で吸収し、有機ＥＬ素子まで到達させない構造としたものである。 In the organic EL panel of the present invention, a sealing member comprising an adhesive layer, a sheet-like hygroscopic layer, an adhesive layer, and a barrier film is provided on the second electrode of the organic EL element, Although the barrier film basically prevents moisture from entering from the outside, even if moisture enters the barrier film, it is absorbed by the hygroscopic layer and does not reach the organic EL element. .
　本発明の封止部材を構成する粘着剤層、シート状吸湿剤層、接着剤層およびバリアフィルムについて順次説明する。 The pressure-sensitive adhesive layer, sheet-like hygroscopic agent layer, adhesive layer and barrier film constituting the sealing member of the present invention will be described sequentially.
　〔シート状吸湿剤層〕
　本発明に用いられるシート状吸湿剤層とは、支持体上にバインダー樹脂成分と吸湿剤成分とを含有する吸湿剤層が形成されたものである。 [Sheet hygroscopic layer]
The sheet-like hygroscopic layer used in the present invention is one in which a hygroscopic layer containing a binder resin component and a hygroscopic component is formed on a support.
　バインダー樹脂成分としては、吸湿剤成分が水分吸着作用を阻害しないものであることが必要であり、好ましくは気体透過性の高い材料を用いる。例示すると、ポリオレフィン系、ポリアクリル系、ポリアクリロニトリル系、ポリアミド系、ポリエステル系、エポキシ系、ポリカーボネーオ系、フッ素系等の高分子材料を挙げることが出来る。 As the binder resin component, it is necessary that the moisture-absorbing agent component does not inhibit the moisture adsorption action, and a material having high gas permeability is preferably used. For example, polymer materials such as polyolefin-based, polyacrylic-based, polyacrylonitrile-based, polyamide-based, polyester-based, epoxy-based, polycarbonate-based, and fluorine-based materials can be exemplified.
　吸湿剤成分としては、水分吸着機能を有し、特に、化学的に水分を吸着すると共に吸着した後でも固体状態を維持する化合物であることが好ましい。例えば、金属酸化物、金属の無機酸塩・有機酸塩等が挙げられるが、本発明の実施形態としては、特に、アルカリ土類金属酸化物及び硫酸塩の少なくとも１種を用いることが好ましい。アルカリ土類金属酸化物としては、例えば、酸化カルシウム（ＣａＯ）、酸化バリウム（ＢａＯ）、酸化マグネシウム（ＭｇＯ）等を挙げることができる。硫酸塩としては、例えば、硫酸リチウム（Ｌｉ２ＳＯ４）、硫酸ナトリウム（Ｎａ２ＳＯ４）、硫酸カリウム（ＣａＳＯ４）、硫酸マグネシウム（ＭｇＳＯ４）、硫酸コバルト（ＣｏＳＯ４）、硫酸ガリウム（Ｇａ２（ＳＯ４）３）、硫酸チタン（Ｔｉ（ＳＯ４）２）、硫酸ニッケル（ＮｉＳＯ４）等を挙げることができる。その他にも、吸湿性を有するシリカ粉末、モレキュラーシーブ粉末等も用いることができる。 The hygroscopic component is preferably a compound having a moisture adsorption function, and particularly a compound that chemically adsorbs moisture and maintains a solid state even after adsorption. For example, metal oxides, metal inorganic acid salts and organic acid salts, and the like can be mentioned. As an embodiment of the present invention, it is particularly preferable to use at least one of alkaline earth metal oxides and sulfates. Examples of the alkaline earth metal oxide include calcium oxide (CaO), barium oxide (BaO), and magnesium oxide (MgO). Examples of the sulfate include lithium sulfate (Li 2 SO 4 ), sodium sulfate (Na 2 SO 4 ), potassium sulfate (CaSO 4 ), magnesium sulfate (MgSO 4 ), cobalt sulfate (CoSO 4 ), and gallium sulfate (Ga). 2 (SO 4 ) 3 ), titanium sulfate (Ti (SO 4 ) 2 ), nickel sulfate (NiSO 4 ), and the like. In addition, hygroscopic silica powder, molecular sieve powder, and the like can also be used.
　シート状吸湿剤層の形成方法としては、前記バインダー樹脂成分５～４０質量％と吸湿剤成分を９５～６０質量％を均一に混合し、溶融或いは溶媒を用いて、支持体上に溶融流延或いは塗布乾燥することによりシート状吸湿剤層を形成することができる。 As a method for forming the sheet-like hygroscopic layer, 5 to 40% by mass of the binder resin component and 95 to 60% by mass of the hygroscopic component are uniformly mixed, and melted or cast on a support using a solvent. Alternatively, the sheet-like hygroscopic agent layer can be formed by coating and drying.
　また、本発明のシート状吸湿剤層は、吸湿剤層を２枚の支持体で挟み込んだサンドイッチ形式のものであることが更に好ましい態様である。 Further, the sheet-like hygroscopic layer of the present invention is more preferably a sandwich type in which the hygroscopic layer is sandwiched between two supports.
　また、シート状吸湿剤層には、必要に応じて他の添加剤を含有していても良い。 The sheet-like hygroscopic layer may contain other additives as necessary.
　本発明のシート状吸湿剤層に用いられる支持体は、その後の製造工程において、ラミネート等により有機ＥＬ素子上に圧着成型されることから、膜厚としては、１０～３００μｍであることが好ましく、また、弾性率はラミネート温度８０～２００℃の範囲で、１０～１００ＭＰａの範囲であることが好ましい。 Since the support used for the sheet-like hygroscopic layer of the present invention is pressure-molded on the organic EL element by laminating or the like in the subsequent production process, the film thickness is preferably 10 to 300 μm. The elastic modulus is preferably in the range of 10 to 100 MPa in the range of the lamination temperature of 80 to 200 ° C.
　〔粘着剤層〕
　本発明においては、シート状吸湿剤層が有する支持体と有機ＥＬ素子の第２の電極との間に粘着剤層を有することを特徴とする。 (Adhesive layer)
In this invention, it has the adhesive layer between the support body which a sheet-like moisture absorbent layer has, and the 2nd electrode of an organic EL element, It is characterized by the above-mentioned.
　本発明で言う粘着剤層とは、熱や溶剤の助けを必要とせず、指圧などのごく低い圧力で他の被写体に被着できる材料であり、ゴム系、アクリル系、シリコーン系などの材料から選択できる。粘着剤としては、粘着層の少なくとも一部分において２５℃での貯蔵弾性率が１．０×１０４～１．０×１０９Ｐａの範囲である粘着剤が用いられていることが好ましく、粘着剤を塗布し、貼り合わせた後に種々の化学反応により高分子量体又は架橋構造を形成する硬化型粘着剤であってもよい。 The pressure-sensitive adhesive layer referred to in the present invention is a material that does not require the help of heat or a solvent and can be applied to other subjects with extremely low pressure such as finger pressure, and is made of a material such as rubber, acrylic or silicone. You can choose. As the pressure-sensitive adhesive, a pressure-sensitive adhesive having a storage elastic modulus at 25 ° C. in the range of 1.0 × 10 4 to 1.0 × 10 9 Pa in at least a part of the pressure-sensitive adhesive layer is preferably used. A curable pressure-sensitive adhesive that forms a high molecular weight body or a crosslinked structure by various chemical reactions after being applied and bonded may be used.
　具体例としては、例えば、ウレタン系粘着剤、エポキシ系粘着剤、水性高分子－イソシアネート系粘着剤、熱硬化型アクリル粘着剤等の硬化型粘着剤、湿気硬化ウレタン粘着剤、ポリエーテルメタクリレート型、エステル系メタクリレート型、酸化型ポリエーテルメタクリレート等の嫌気性粘着剤、シアノアクリレート系の瞬間粘着剤、アクリレートとペルオキシド系の２液型瞬間粘着剤等が挙げられる。 Specific examples include, for example, urethane adhesives, epoxy adhesives, aqueous polymer-isocyanate adhesives, curable adhesives such as thermosetting acrylic adhesives, moisture-curing urethane adhesives, polyether methacrylate types, Examples include anaerobic pressure-sensitive adhesives such as ester-based methacrylate type and oxidized polyether methacrylate, cyanoacrylate-based instantaneous pressure-sensitive adhesives, and acrylate-peroxide-based two-component instantaneous pressure-sensitive adhesives.
　上記粘着剤としては一液型であっても良いし、使用前に二液以上を混合して使用する型であっても良い。 The above-mentioned pressure-sensitive adhesive may be a one-component type or a type in which two or more components are mixed before use.
　〔接着剤層〕
　次に本発明に用いられる接着剤層について説明する。 [Adhesive layer]
Next, the adhesive layer used in the present invention will be described.
　本発明の接着剤層としては、離形性支持体上に接着樹脂を塗布し、シート状に形成したものを用いることが好ましく、接着剤層を、予め有機ＥＬ素子の上に形成したシート状吸湿剤層の上に転写するか、或いは、予めバリアフィルム上に転写して、離形性支持体を剥離し、接着材層を有するバリアフィルムをシート状吸湿剤層の上に貼合することが好ましい。 As the adhesive layer of the present invention, it is preferable to use an adhesive resin coated on a releasable support and formed into a sheet shape. The adhesive layer is formed in a sheet shape previously formed on an organic EL element. Transfer onto the hygroscopic layer or transfer onto the barrier film in advance, peel off the releasable support, and bond the barrier film having the adhesive layer onto the sheet-like hygroscopic layer Is preferred.
　接着剤層を形性する接着樹脂としては、熱硬化性接着樹脂或いは紫外線硬化型接着樹脂等を用いることができる。 As the adhesive resin that forms the adhesive layer, a thermosetting adhesive resin, an ultraviolet curable adhesive resin, or the like can be used.
　熱硬化性接着樹脂として、例えば、フェノール樹脂、シリコーン樹脂、アリルエステル、アクリル樹脂、エポキシ樹脂、ポリイミド、又はウレタン樹脂などを用いることができる。 As the thermosetting adhesive resin, for example, phenol resin, silicone resin, allyl ester, acrylic resin, epoxy resin, polyimide, or urethane resin can be used.
　紫外線硬化性接着樹脂として、例えば、シリコーン樹脂、アクリル系樹脂、エポキシ系樹脂、ポリイミド、又はウレタン系樹脂などを用いることができる。 As the ultraviolet curable adhesive resin, for example, a silicone resin, an acrylic resin, an epoxy resin, a polyimide, or a urethane resin can be used.
　これらの硬化性接着樹脂は市販品として入手することができる。 These curable adhesive resins can be obtained as commercial products.
　本発明においては、有機ＥＬ素子に貼り合わせるまではシート状接着剤の接着剤表面には更に保護フィルムをかぶせておくことが好適である。 In the present invention, it is preferable to further cover the adhesive surface of the sheet-like adhesive with a protective film until it is bonded to the organic EL element.
　〔バリアフィルム〕
　本発明に用いられるガスバリアフィルムとしては、基材フィルムの上にバリア性積層体を有するものであれば特に限定されないが、有機ＥＬ素子のフレキシブル基材と同様の物を用いることができる。厚みが２００μｍ程度以下の薄板ガラス等であっても良く、湿度透過率として、１０-５ｇ／ｍ2／ｄａｙ以下のものが好ましい。 [Barrier film]
Although it will not specifically limit as a gas barrier film used for this invention if it has a barriering laminated body on a base film, The thing similar to the flexible base material of an organic EL element can be used. Thin glass having a thickness of about 200 μm or less may be used, and a humidity transmittance of 10 −5 g / m 2 / day or less is preferable.
　［パネル製造方法］
　有機ＥＬ素子形成工程；フレキシブル基板１１上に直接または他の層を介して第１の電極１２を形成し、第１の電極１２の上に発光層を含む有機ＥＬ層１３を形成し、有機層１３上に第２の電極１４を形成することで、有機ＥＬ素子１０が形成される。 [Panel manufacturing method]
Organic EL element forming step: First electrode 12 is formed on flexible substrate 11 directly or via another layer, organic EL layer 13 including a light emitting layer is formed on first electrode 12, and an organic layer is formed. By forming the second electrode 14 on 13, the organic EL element 10 is formed.
　有機ＥＬ素子１０は、連続するフレキシブル基板１１上に複数の有機ＥＬ素子が連続的に形成されても良く、また、枚葉に形成されていても良い。 The organic EL element 10 may be formed of a plurality of organic EL elements on a continuous flexible substrate 11 or may be formed on a single wafer.
　具体的には、表面加工及び洗浄が施された基板１１に対して、スパッタリング、蒸着等の成膜方法で第１の電極１２の導電材料を成膜し、フォトリソ工程によって、例えば、１画素が２０×１６．５ｍｍを４個田形状に形成した（４画素分合計で４１×３４ｍｍの面積となる）４分割パターニングして１単位の第１の電極１２を形成する。そして、区画された第１の電極１２の画素領域上に有機ＥＬ層１３を順次積層させる。有機ＥＬ層１３は、第１の電極１２を陽極とする場合には、例えば、正孔注入層、正孔輸送層、発光層、電子輸送層、電子注入層等を順に真空蒸着によって成膜する。その後、有機ＥＬ層１３上に第２の電極１４を第１の電極１２と同様に４分割状に成膜する。 Specifically, the conductive material of the first electrode 12 is formed on the substrate 11 that has been subjected to surface processing and cleaning by a film formation method such as sputtering or vapor deposition, and, for example, one pixel is formed by a photolithography process. Four units of 20 × 16.5 mm are formed in a four-column shape (a total area of 41 × 34 mm for four pixels), and one unit of the first electrode 12 is formed. Then, the organic EL layer 13 is sequentially stacked on the pixel area of the partitioned first electrode 12. When the first electrode 12 is used as the anode, the organic EL layer 13 is formed, for example, by sequentially depositing a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, and the like by vacuum deposition. . After that, the second electrode 14 is formed on the organic EL layer 13 in the same manner as the first electrode 12 in a quadrant.
　シート状吸湿剤層形成工程；シート状吸湿剤層２０は、支持体２２上に予め吸湿剤層２３を形成し、更にその上に支持体２４でサンドイッチ構造とした。一方の支持体上に粘着剤層２１を形成し、有機ＥＬ素子部全体を覆う巾に形成されたシート状吸湿剤層２０を用い、該粘着剤層２１が第２の電極１４と接するように有機ＥＬ素子１０上に配備する。 Sheet-like hygroscopic layer forming step: The sheet-like hygroscopic layer 20 has a hygroscopic agent layer 23 formed on a support 22 in advance, and a support 24 on which a sandwich structure is formed. A pressure-sensitive adhesive layer 21 is formed on one support, and a sheet-like hygroscopic layer 20 formed so as to cover the entire organic EL element portion is used so that the pressure-sensitive adhesive layer 21 is in contact with the second electrode 14. It is arranged on the organic EL element 10.
　接着剤層形成工程；接着剤層３０は、離形性支持体３１上に予め接着剤層３０を形成し、有機ＥＬ素子のフレキシブル基材を覆うような巾に形成されたシート状接着剤層３０を用い、吸湿剤層と接するように配備する。 Adhesive layer forming step; the adhesive layer 30 is a sheet-like adhesive layer formed in such a width that the adhesive layer 30 is previously formed on the releasable support 31 and covers the flexible substrate of the organic EL element. 30 and is placed in contact with the hygroscopic layer.
　貼り合わせ工程；有機ＥＬ素子上に粘着剤層２１を有するシート状吸湿剤層２０、シート状接着剤層３０及びバリアフィルム４０を、少なくとも有機ＥＬ素子部全体を覆うようにしてフレキシブル基板１１と封止部材５０のバリアフィルム４０とを接着剤層３０を介して貼合する。フレキシブル基板１１と封止部材５０とは所定の圧力で圧着し、必要に応じて加熱を行って接着剤を硬化させる。 Bonding step; sealing the flexible substrate 11 with the sheet-like moisture absorbent layer 20, the sheet-like adhesive layer 30 and the barrier film 40 having the pressure-sensitive adhesive layer 21 on the organic EL element so as to cover at least the entire organic EL element portion. The barrier film 40 of the stopper member 50 is bonded via the adhesive layer 30. The flexible substrate 11 and the sealing member 50 are pressure-bonded with a predetermined pressure, and heated as necessary to cure the adhesive.
　以上説明したような本発明の方法により、封止構造を容易に形成することが可能となった。即ち、有機ＥＬ素子の表面とシート状吸湿剤層を粘着剤層を介して貼合する構造を採用したことにより、形性直後の故障が少なく、経時保存時においても有機ＥＬ素子の発光機能を良好に維持することが可能となり、薄型化かつ高い強度を有する有機ＥＬパネルを得ることができた。 The sealing structure can be easily formed by the method of the present invention as described above. That is, by adopting a structure in which the surface of the organic EL element and the sheet-like hygroscopic layer are bonded via an adhesive layer, there are few failures immediately after form, and the light emitting function of the organic EL element can be maintained even during storage over time. It was possible to maintain it well, and an organic EL panel having a reduced thickness and high strength could be obtained.
　〈有機ＥＬ素子の作製〉
　本発明に用いられる有機ＥＬ素子は、支持体として２００μｍのガラス基板を用い、その上に第１の電極としてＩＴＯ（インジウム酸化スズ）膜が蒸着された基板を用い、リソグラフィー法によりパターンニングし、その上に公知の有機ＥＬ層及び第２の電極を形成して有機ＥＬ素子を形成した。 <Production of organic EL element>
The organic EL element used in the present invention uses a 200 μm glass substrate as a support, and a substrate on which an ITO (indium tin oxide) film is deposited as a first electrode, and is patterned by a lithography method. A known organic EL layer and a second electrode were formed thereon to form an organic EL element.
　以上のようにして得られた有機ＥＬ素子は、発光パターンが２０×１６．５ｍｍ×４画素の４分割発光パターンである（４画素分合計で４１×３４ｍｍの面積となる）。 The organic EL element obtained as described above is a four-part light emission pattern having a light emission pattern of 20 × 16.5 mm × 4 pixels (a total area of 41 × 34 mm for four pixels).
　《封止作業》
　（封止構成１）
　手順ａ　基材として、膜厚５０μｍを有するポリエチレンテレフタレートフィルム上に、アルミ箔３０μｍのバリア膜をラミネートしたバリアフィルムを作製した。 <Sealing work>
(Sealing configuration 1)
Procedure a A barrier film was produced by laminating a barrier film of aluminum foil 30 μm on a polyethylene terephthalate film having a film thickness of 50 μm as a substrate.
　手順ｂ　次に手順ａで作製したバリアフィルムのアルミ面上に下記接着剤Ａを塗布した。 Procedure b Next, the following adhesive A was applied on the aluminum surface of the barrier film prepared in Procedure a.
　手順ｃ　次に粘着剤層付き吸湿剤シート（ドライキープ０１　佐々木化学薬品株式会社製、層構成：粘着剤層／ＰＥＴ／吸湿剤層／ＰＥＴ）の粘着剤層側を上記で作製した有機ＥＬ素子の第２の電極上に貼り付けた。 Procedure c Next, the organic EL device in which the pressure-sensitive adhesive layer side of the moisture-absorbent sheet with the pressure-sensitive adhesive layer (Dry Keep 01, manufactured by Sasaki Chemical Co., Ltd., layer configuration: pressure-sensitive adhesive layer / PET / humidifier layer / PET) was prepared as described above. Affixed on the second electrode.
　手順ｄ　手順ｂで接着剤を塗布して作製したバリアフィルムの接着剤層面と吸湿剤シートのＰＥＴ面を合わせて配置した。 Procedure d The adhesive layer surface of the barrier film prepared by applying the adhesive in Procedure b and the PET surface of the hygroscopic sheet were placed together.
　手順ｅ　手順ｄで準備された、有機ＥＬ素子、吸湿剤シート、バリアフィルムに対して、１×１０－２Ｐａの減圧環境下で真空ラミネーターを用い押圧力０．１ＭＰａで１００℃６０秒間圧着し、さらに硬化処理として１００℃３０分間加熱を施し、密着封止して有機ＥＬパネルＮｏ．１を作製した。 Procedure e The organic EL device, the hygroscopic sheet, and the barrier film prepared in Procedure d are pressure-bonded at 100 ° C. for 60 seconds at a pressing force of 0.1 MPa in a reduced pressure environment of 1 × 10 −2 Pa using a vacuum laminator. Further, as a curing treatment, heating was performed at 100 ° C. for 30 minutes, and the organic EL panel no. 1 was produced.
　（封止構成２）
　封止構成１の手順ｂにおいて接着剤Ａを下記接着剤Ｂに換え、手順ｅの硬化処理を１００℃３０分加熱の代わりに、素子基板上にフォトマスクを配置し、有機層領域は遮光した状態で、主波長３６５ｎｍの紫外線照射し、有機ＥＬパネルＮｏ．２を作製した。 (Sealing configuration 2)
In the procedure b of the sealing configuration 1, the adhesive A is changed to the following adhesive B, a photomask is arranged on the element substrate instead of heating at 100 ° C. for 30 minutes in the curing process of the procedure e, and the organic layer region is shielded from light. In the state, the organic EL panel No. 2 was produced.
　（封止構成３）
　封止構成１の手順ｃにおいて、シート状吸湿剤層の代わりに塗布型乾燥剤（Ｏｌｅｄｒｙ　双葉電子工業株式会社製）を有機ＥＬ素子上へ塗布して、有機ＥＬパネルＮｏ．３を作製した。 (Sealing configuration 3)
In the procedure c of the sealing configuration 1, in place of the sheet-like hygroscopic agent layer, a coating type desiccant (Oldry Futaba Electronics Co., Ltd.) was applied onto the organic EL element, and the organic EL panel No. 3 was produced.
　（封止構成４）
　封止構成３の手順ｂ、ｄを封止構成２と同様にして、有機ＥＬパネルＮｏ．４を作製した。 (Sealing configuration 4)
The procedures b and d of the sealing configuration 3 are the same as those of the sealing configuration 2, and the organic EL panel No. 4 was produced.
　（封止構成５）
　封止構成１において、シート状吸湿剤層を用いないで、有機ＥＬパネルＮｏ．５を作製した。 (Sealing configuration 5)
In the sealing configuration 1, without using the sheet-like hygroscopic agent layer, the organic EL panel No. 5 was produced.
　（封止構成６）
　封止構成２において、シート状吸湿剤層を用いないで、有機ＥＬパネルＮｏ．６を作製した。 (Sealing configuration 6)
In the sealing configuration 2, without using the sheet-like hygroscopic agent layer, the organic EL panel No. 6 was produced.
　尚、用いた接着剤を以下に示す。 The adhesive used is shown below.
　接着剤Ａ：熱硬化型接着剤（ストラクトボンドＥ－４１３　三井化学株式会社製）
　接着剤Ｂ：紫外線硬化型接着剤（ＴｈｒｅｅＢｏｎｄ３１２４Ｃ　株式会社スリーボンド社製）
　《有機ＥＬパネルの評価》
　作製した各有機ＥＬパネルについて、ダークスポット（スポット状の非発光部）の発生割合を下記試験法で試験し、下記評価ランクに従って評価した。 Adhesive A: Thermosetting adhesive (Struct Bond E-413, manufactured by Mitsui Chemicals, Inc.)
Adhesive B: UV curable adhesive (ThreeBond 3124C, manufactured by Three Bond Co., Ltd.)
<< Evaluation of organic EL panel >>
About each produced organic EL panel, the generation | occurrence | production ratio of the dark spot (spot-shaped non-light-emission part) was tested with the following test method, and it evaluated according to the following evaluation rank.
　（ダークスポット試験法）
　有機ＥＬパネルを６０℃９０％ＲＨの環境条件に保存した。有機ＥＬパネル作製直後と保存後３００時間経過後にパネルを点灯し、それぞれのダークスポット（スポット状の非発光部）の数及びその後の発生割合を面積で観察した。なお、パネルの点灯は定電圧電源を用いて有機ＥＬ素子の１画素に直流５Ｖを印加した。評価は４画素分（４１×３４ｍｍ）における個数若しくは発生率（面積比）で評価した。得られた結果を表１に示す。 (Dark spot test method)
The organic EL panel was stored in an environmental condition of 60 ° C. and 90% RH. The panel was turned on immediately after the organic EL panel was fabricated and after 300 hours had elapsed after storage, and the number of dark spots (spot-like non-light-emitting portions) and the subsequent generation ratio were observed by area. For lighting the panel, a DC voltage of 5 V was applied to one pixel of the organic EL element using a constant voltage power source. Evaluation was performed by the number or occurrence rate (area ratio) of 4 pixels (41 × 34 mm). The obtained results are shown in Table 1.
　〔封止直後の評価〕
　○：ダークスポット個数０～１０個
　△：ダークスポット個数１１～５０個
　×：ダークスポット個数５１～１００個
　〔６０℃９０％ＲＨ－３００時間経過後の評価〕
　◎：ダークスポット発生率０％（ダークスポットの発生が全く無い）
　○：ダークスポット発生率１％以上５％未満
　△：ダークスポット発生率５％以上１０％未満
　×：ダークスポット発生率１０％以上 [Evaluation immediately after sealing]
○: Number of dark spots 0 to 10 Δ: Number of dark spots 11 to 50 ×: Number of dark spots 51 to 100 [Evaluation after 60 ° C. 90% RH-300 hours]
A: Dark spot occurrence rate 0% (no dark spots are generated)
○: Dark spot occurrence rate of 1% or more and less than 5% Δ: Dark spot occurrence rate of 5% or more and less than 10% ×: Dark spot occurrence rate of 10% or more
Figure JPOXMLDOC01-appb-T000001
  
Figure JPOXMLDOC01-appb-T000001
  
　表１の結果から分かるように、本発明の試料は形成直後のダークスポットの発生数が少なく、保存経過後においても、ダークスポット発生率も少なく、優れた性能を維持していることが分かる。 As can be seen from the results of Table 1, it can be seen that the sample of the present invention has a small number of dark spots generated immediately after formation, and has a low dark spot generation rate even after storage, and maintains excellent performance.
　１０　有機ＥＬ素子
　１１　フレキシブル基板
　１２　第１の電極
　１３　有機ＥＬ層
　１４　第２の電極
　２０　シート状吸湿剤層
　２１　粘着層
　２２　支持体
　２３　吸湿剤層
　２４　支持体
　３０　接着剤層
　４０　バリアフィルム
　４５　搬送ローラ
　５０　封止部材
　１００　有機ＥＬパネル
  DESCRIPTION OF SYMBOLS 10 Organic EL element 11 Flexible substrate 12 1st electrode 13 Organic EL layer 14 2nd electrode 20 Sheet-like hygroscopic agent layer 21 Adhesive layer 22 Support body 23 Hygroscopic agent layer 24 Support body 30 Adhesive layer 40 Barrier film 45 Conveyance roller 50 Sealing member 100 Organic EL panel

Claims (7)

  1. フレキシブル基材上に、第１の電極、有機エレクトロルミネッセンス層、第２の電極、封止部材をこの順で有する有機エレクトロルミネッセンスパネルにおいて、該封止部材が、第２の電極側から順に、粘着剤層、支持体上に吸湿剤層が形成されたシート状吸湿剤層、接着剤層およびバリアフィルムが積層されてなることを特徴とする有機エレクトロルミネッセンスパネル。 In the organic electroluminescent panel which has a 1st electrode, an organic electroluminescent layer, a 2nd electrode, and a sealing member in this order on a flexible base material, this sealing member adheres in an order from the 2nd electrode side. An organic electroluminescence panel comprising: an agent layer; a sheet-like hygroscopic layer having a hygroscopic layer formed on a support; an adhesive layer; and a barrier film.
  2. 前記シート状吸湿剤層が、吸湿剤をバインダー中に含有させてあらかじめ支持体上に形成しシート状にしたものであることを特徴とする請求項１に記載の有機エレクトロルミネッセンスパネル。 2. The organic electroluminescence panel according to claim 1, wherein the sheet-like hygroscopic layer is a sheet formed by previously containing a hygroscopic agent in a binder and formed on a support.
  3. 前記シート状吸湿剤層が、吸湿剤をバインダー中に含有させて、あらかじめ２枚の支持体に挟んで形成しシート状にしたものであることを特徴とする請求項１または２に記載の有機エレクトロルミネッセンスパネル。 The organic sheet according to claim 1 or 2, wherein the sheet-like hygroscopic layer is formed by previously containing a hygroscopic agent in a binder and sandwiched between two supports. Electroluminescence panel.
  4. 前記接着剤層が、接着剤をあらかじめ離形性支持体上に形成しシート状にしたものであることを特徴とする請求項１～３の何れか１項に記載の有機エレクトロルミネッセンスパネル。 The organic electroluminescence panel according to any one of claims 1 to 3, wherein the adhesive layer is formed by previously forming an adhesive on a releasable support and forming a sheet.
  5. 前記接着剤層が、熱硬化性樹脂であることを特徴とする請求項１～４の何れか１項に記載の有機エレクトロルミネッセンスパネル。 The organic electroluminescence panel according to any one of claims 1 to 4, wherein the adhesive layer is a thermosetting resin.
  6. フレキシブル基材上に、第１の電極、エレクトロルミネッセンス層、第２の電極、封止部材をこの順で有する有機エレクトロルミネッセンスパネルの製造方法であって、該第２の電極上に、支持体の一方の面に粘着剤層を有し、他方の面に吸湿剤層が形成されたシート状吸湿剤層を、粘着剤層が第２の電極と接するように貼り合わせ、次いで、接着剤をあらかじめ離形性支持体上に形成してシート状にしたシート状接着剤層を離形性支持体から剥がしてバリアフィルムと貼り合わせたシート状接着剤層を有するバリアフィルムを、シート状接着剤層がシート状吸湿剤層に接するように貼り合わせて、封止部材を形成したことを特徴とする有機エレクトロルミネッセンスパネルの製造方法。 A method for producing an organic electroluminescence panel having a first electrode, an electroluminescence layer, a second electrode, and a sealing member in this order on a flexible substrate, wherein the support is formed on the second electrode. A sheet-like hygroscopic layer having a pressure-sensitive adhesive layer on one side and a hygroscopic layer formed on the other side is bonded so that the pressure-sensitive adhesive layer is in contact with the second electrode. A sheet-like adhesive layer comprising a sheet-like adhesive layer formed on a releasable support and peeled off from the releasable support and bonded to the barrier film. Are bonded so as to be in contact with the sheet-like hygroscopic agent layer to form a sealing member, and a method for producing an organic electroluminescence panel.
  7. フレキシブル基材上に、第１の電極、エレクトロルミネッセンス層、第２の電極、封止部材をこの順で有する有機エレクトロルミネッセンスパネルの製造方法であって、該第２の電極上に、吸湿剤をバインダー中に含有させて、あらかじめ２枚の支持体に挟んで形成したシート状吸湿剤層の一方の面に粘着剤層を設け、粘着剤層が第２の電極と接するように貼り合わせ、次いで、接着剤をあらかじめ支持体上に形成してシート状にした接着剤層を離形性支持体からはがしてバリアフィルムと貼り合わせた接着剤層を有するバリアフィルムを、接着剤層がシート状吸湿剤層に接するように貼り合わせて、封止部材を形成したことを特徴とする有機エレクトロルミネッセンスパネルの製造方法。
          A method for producing an organic electroluminescence panel having a first electrode, an electroluminescence layer, a second electrode, and a sealing member in this order on a flexible substrate, wherein a hygroscopic agent is disposed on the second electrode. In the binder, an adhesive layer is provided on one surface of the sheet-like hygroscopic layer formed between two supports in advance, and the adhesive layer is bonded so as to contact the second electrode, A barrier film having an adhesive layer in which an adhesive layer formed in advance on a support is peeled off from the releasable support and bonded to the barrier film, and the adhesive layer absorbs moisture. A method for producing an organic electroluminescence panel, wherein a sealing member is formed by bonding so as to be in contact with an agent layer.
PCT/JP2012/063547 2011-07-15 2012-05-25 Organic electroluminescence panel and method of manufacturing same WO2013011741A1 (en)

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