JP2005347204A - Organic el element and its manufacturing method - Google Patents
Organic el element and its manufacturing method Download PDFInfo
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- 239000000758 substrate Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 13
- 239000005394 sealing glass Substances 0.000 claims abstract description 13
- 239000011241 protective layer Substances 0.000 claims abstract description 5
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- 229920005989 resin Polymers 0.000 claims description 11
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- 238000001179 sorption measurement Methods 0.000 claims description 5
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
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- 239000004952 Polyamide Substances 0.000 description 1
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- 229910021536 Zeolite Inorganic materials 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
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- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
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- 239000000440 bentonite Substances 0.000 description 1
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
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- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
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- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
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- 150000001925 cycloalkenes Chemical class 0.000 description 1
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- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
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Images
Abstract
Description
本発明は発光を素子の陽極側で取り出すことの出来る有機電界発光素子及びその製造方法に関するものであり、詳しくは有機発光層に電界をかけて発光するタイプの薄型ディスプレイの封止方法に関するものである。 The present invention relates to an organic electroluminescent device capable of extracting light emission on the anode side of the device and a method for manufacturing the same, and more particularly to a sealing method for a thin type display that emits light by applying an electric field to an organic light emitting layer. is there.
現在開発中の有機ＥＬ素子の構成は、ガラス基板上に有機発光層が二つの電極の間に挟まれたサンドイッチ構造であるが、前記有機発光層の光を外に取り出せるようにするために、電極の片方は透明のものが使われており、一般的には陽極にITO(Indium Tin Oxide)透明電極が使われている。更に前記有機発光層の外周面は封止材により封止され、外部駆動回路により電圧を印加することにより発光する。 The structure of the organic EL element currently under development is a sandwich structure in which an organic light emitting layer is sandwiched between two electrodes on a glass substrate, but in order to be able to take out the light of the organic light emitting layer, One of the electrodes is transparent, and generally an ITO (Indium Tin Oxide) transparent electrode is used for the anode. Furthermore, the outer peripheral surface of the organic light emitting layer is sealed with a sealing material, and emits light when a voltage is applied by an external drive circuit.
以上の原理により発光する有機ＥＬ素子は、視認性とフレキシブル性に優れ且つ発色性が多様であることから、車載用カーコンポや携帯電話等のディスプレイや表示素子に利用されている。 Organic EL elements that emit light based on the above principle are used for displays and display elements such as in-vehicle car components and mobile phones because they are excellent in visibility and flexibility and have various coloring properties.
ところで、これらの特性を有するディスプレイではあるが、一方で有機ＥＬ素子は一般的に水分に極めて弱いという問題がよく知られている。一例としては有機ＥＬ素子中に有機発光層を形成した後にガラス基板を封止する際の環境雰囲気中に含まれる水分や封止層欠陥部を透過してくる水分が進入することにより、ダークスポットと称する非発光領域が発生、発光が維持出来なくなるといった寿命の課題が生じている。 By the way, although it is a display which has these characteristics, on the other hand, the problem that an organic EL element is generally very weak to moisture is known well. As an example, the dark spot is caused by the moisture contained in the environmental atmosphere when the glass substrate is sealed after the organic light emitting layer is formed in the organic EL element or the moisture that permeates through the defective portion of the sealing layer. The non-light-emitting area | region called this generate | occur | produces and the subject of the lifetime that the light emission cannot be maintained has arisen.
従来、請求項１〜１１に対し、有機ＥＬ素子の製品寿命に対する課題を解決するために、積層フィルムが基材として用いられることが知られている。この積層フィルムは、ポリエチレンテレフタレートなどの熱可塑性フィルムの片面あるいは両面に蒸着法により酸化珪素などの無機膜が形成されてなるガスバリア性を有するフィルムをラミネート法により積層した構成となっている。（特許文献１）
しかしながら、上記特許文献１に記載されているラミネート法でフィルムを積層する場合、通常紫外線硬化接着剤や室温硬化型接着剤などの接着剤を両面に塗布してフィルムを貼り合わせて製造するため、元々前記接着剤中に含有する水分や硬化後に未反応モノマーなどの発生するガスによって、有機ＥＬ発光素子に対して悪影響を与えてしまう課題がある。
However, in the case of laminating a film by the laminating method described in the above-mentioned
例えば室温硬化エポキシ系接着剤をガスバリア性フィルム同士のラミネートに用いると、接着剤中に元来含有する水分や低分子モノマーが硬化時及び硬化後に発生し、有機ＥＬ素子内部に発生ガスが閉じこめられ残留し、有機ＥＬ素子の発光効率が低下するといった問題がある。 For example, when a room temperature curing epoxy adhesive is used for laminating gas barrier films, moisture and low molecular weight monomers originally contained in the adhesive are generated during and after curing, and the generated gas is trapped inside the organic EL element. There exists a problem that it remains and the luminous efficiency of an organic EL element falls.
また、前記積層フィルムの接着層に接着剤を塗布の際に発生するボイドなどの空隙が存在することが原因で、水分が進入しやすくなり、ダークスポットと称する非発光部が生じ、有機ＥＬ素子の劣化を促進するなどの問題があった。 In addition, due to the presence of voids such as voids generated when an adhesive is applied to the adhesive layer of the laminated film, moisture easily enters and a non-light emitting portion called a dark spot is generated, resulting in an organic EL element. There were problems such as promoting the deterioration of
上記の寿命に関する課題を解決するために、ガラス基板上に有機ＥＬ発光層、保護層、充填材及び封止ガラスから形成された有機ＥＬ積層構造体において、前記保護層と前記充填材、及び前記封止ガラスの少なくとも一方の接合について、直接接触して配置することを提案する。 In order to solve the above-mentioned problem relating to the lifetime, in the organic EL laminated structure formed from an organic EL light emitting layer, a protective layer, a filler and a sealing glass on a glass substrate, the protective layer, the filler, and the It is proposed that at least one joint of the sealing glass be placed in direct contact.
また、前記接合する方法が表面活性処理による直接接合法であることを提案する。 It is also proposed that the bonding method is a direct bonding method by surface activation treatment.
また、前記表面活性処理法が常圧プラズマ法であることを提案する。 It is also proposed that the surface activation treatment method is an atmospheric pressure plasma method.
また、前記保護膜がシリコン窒化酸化物であることを提案する。 Further, it is proposed that the protective film is silicon nitride oxide.
また、前記充填材が透明樹脂フィルムであることを提案する。 It is also proposed that the filler is a transparent resin film.
また、前記充填材がガラス基板上に形成したフォトレジスト膜であることを提案する。 It is also proposed that the filler is a photoresist film formed on a glass substrate.
また、前記充填材中に水分吸着作用を有するフィラーが内添されていることを提案する。 Further, it is proposed that a filler having a moisture adsorption action is internally added to the filler.
また、前記透明樹脂がシクロオレフィンポリマーであることを提案する。 It is also proposed that the transparent resin is a cycloolefin polymer.
また、前記水分吸着作用を有するフィラーが多孔質フィラーであることを提案する。 Further, it is proposed that the filler having the moisture adsorption action is a porous filler.
有機ＥＬ素子の封止において、接着剤を用いないで接合する本発明は、次の点で従来技術と比較して優位性がある。 In sealing an organic EL element, the present invention that joins without using an adhesive is superior to the prior art in the following points.
（１）接着剤中に含有する水分の影響がない。 (1) There is no influence of moisture contained in the adhesive.
（２）貼りあわせ時に発生する空隙による界面からの水分の侵入がなくなる。 (2) Moisture intrusion from the interface due to voids generated during bonding is eliminated.
これらのことから、ダークスポットの少ない安定性のある有機ＥＬ発光素子を形成することが出来た。 From these facts, it was possible to form a stable organic EL light emitting device with few dark spots.
本発明に係る有機ＥＬ積層構造体において、接着剤レスで充填材を接合することにより、これまで大きな課題であった元々接着剤中に含有していた水分の影響や貼りあわせ時のボイドによる欠陥の影響は無くなったため、信頼性の高い有機ＥＬ素子を安価に提供することが可能となる。 In the organic EL laminated structure according to the present invention, by bonding the filler without using an adhesive, the influence of moisture originally contained in the adhesive, which has been a major problem, and defects due to voids at the time of bonding. Therefore, it is possible to provide a highly reliable organic EL element at low cost.
本発明の代表図を図１に示す。符号１のガラス基板上に蒸着装置などの成膜装置により透明電極と有機発光層と電極からなる符号３の有機ＥＬ素子を形成した後、スパッタリング法やＣＶＤ法により符号４の保護膜としてシリコン窒化酸化物などが成膜される。
A typical view of the present invention is shown in FIG. After forming an organic EL element of
次に図２に示すように符号２の封着ガラス基板と符号５の充填材の表面を符号６の常圧プラズマ装置を用い、窒素ガス中で表面活性化処理を行い、前記封止ガラス、充填材及び保護膜を接着剤レスで接合する。接合後、電極を外部回路に接続することにより本発明の有機ＥＬ素子が発光する。
Next, as shown in FIG. 2, the surface of the
ここで本発明の詳細について、充填材５の部分を拡大した図を示す。（図３）ここで図３の符号７はフィラーを示し、符号８は有機材料を示す。
Here, for details of the present invention, an enlarged view of the
符号７のフィラーは、水分吸着作用を持つフィラーであり、具体的には、シリカ（合成シリカ含む）、カオリン、デラミカオリン、水酸化アルミニウム、チタンホワイト、重質炭酸カルシウム、軽質炭酸カルシウム、硫酸カルシウム、硫酸バリウム、二酸化チタン、焼成カオリン、タルク、酸化亜鉛、炭酸亜鉛、硫化亜鉛、アルミナ、微粒子状アルミナ、ケイソウ土、焼成ケイソウ土、珪酸アルミニウム、珪酸カルシウム、珪酸マグネシウム、酸化マグネシウム、炭酸マグネシウム、アルミノ珪酸塩、コロイダルシリカ、活性白土、ベントナイト、ゼオライト、セリサイト、リトポン等の鉱物質顔料、多孔質顔料や有機顔料等の微粒子、多孔質微粒子、及び中空微粒子等が挙げられる。 The filler of the code | symbol 7 is a filler with a water | moisture-content adsorption | suction effect | action, Specifically, a silica (a synthetic silica is included), a kaolin, a delaminated kaolin, aluminum hydroxide, titanium white, heavy calcium carbonate, light calcium carbonate, calcium sulfate , Barium sulfate, titanium dioxide, calcined kaolin, talc, zinc oxide, zinc carbonate, zinc sulfide, alumina, particulate alumina, diatomaceous earth, calcined diatomaceous earth, aluminum silicate, calcium silicate, magnesium silicate, magnesium oxide, magnesium carbonate, alumino Examples thereof include mineral pigments such as silicate, colloidal silica, activated clay, bentonite, zeolite, sericite, and lithopone, fine particles such as porous pigments and organic pigments, porous fine particles, and hollow fine particles.
また、符号８の有機材料としては、エポキシ樹脂、環状ポリオレフィン系樹脂、ポリ塩化ビニル系樹脂、ポリ（メタ）アクリル系樹脂、ポリエチレンテレフタレート系樹脂、各種ナイロンのポリアミド樹、ポリイミド樹脂、ポリアミドイミド樹脂、ポリアリールフタレート樹脂、シリコーン樹脂、ポリスルホン系樹脂、ポリフェニレンスルフィド系樹脂、ポリエーテルスルホン系樹脂、ポリウレタン系樹脂、アセタール系樹脂、及上記列挙の前駆体を共重合してなる共重合体が挙げられる。
Moreover, as an organic material of the code |
ここで一例として、前記有機材料としてはシクロオレフィンポリマーのフィルム（ゼオノアフィルム／日本ゼオン製）を用い、前記フィルム中に吸湿作用を併せ持つフィラーとして、ここでは合成シリカ（商品名：マイクロイド／東洋化学工業製）を１０ｗｔ％添加した材料を充填材として用いた。 As an example, a cycloolefin polymer film (ZEONOR FILM / manufactured by Nippon Zeon Co., Ltd.) is used as the organic material, and synthetic silica (trade name: Microid / Toyo Chemical Co., Ltd.) is used as a filler having a hygroscopic action in the film. A material to which 10 wt% of Kogyo) was added was used as a filler.
ここで上記保護膜と封止ガラスとを充填材を介して常圧プラズマ接合により接合させる工程は、グローブボックス（不図示）中の水分濃度を１０ｐｐｍ以下に制御して行うことにより、組み立て直後にこれまで大きな課題であったダークスポットの発生を押さえ込むことが可能となった。また、長期信頼性においても６０℃／９０％ＲＨの雰囲気条件で１０００時間の連続耐久試験を行ったが、輝度劣化等の発光特性の低下は確認されず、ダークスポット等の発生もなく、安定した有機ＥＬ素子とその製造方法を得ることが出来た。 Here, the step of bonding the protective film and the sealing glass by atmospheric pressure plasma bonding through a filler is performed by controlling the moisture concentration in the glove box (not shown) to 10 ppm or less, immediately after assembly. It has become possible to suppress the occurrence of dark spots, which has been a major issue. Also, for long-term reliability, a continuous durability test of 1000 hours was performed under an atmospheric condition of 60 ° C./90% RH, but no deterioration in light emission characteristics such as luminance deterioration was confirmed, and there was no occurrence of dark spots or the like. An organic EL device and a method for producing the same were obtained.
（第１の実施例）
本発明の代表図を図１に示す。ここで符号１はガラス基板であり、符号３は蒸着装置などの成膜装置により透明電極と有機発光層と電極からなる有機ＥＬ素子を示す。ここで、該有機ＥＬ素子の詳細な作製方法について以下に述べる。
(First embodiment)
A typical view of the present invention is shown in FIG.
［Ｃｒ電極形成］
ガラス基板１上に、ＣｒターゲットをＤＣスパッタし陽極Ａとして100nmの厚さにＣｒ膜を成膜した。この際成膜マスクを用いて、３ｍｍのストライプとした。Ａｒガスを用いて、0.2Ｐａの圧力、３００Ｗの投入Ｐｗ条件で行った。
[Cr electrode formation]
On the
［大気開放］
次に基板をスパッタ装置より取り出してアセトン、イソプロピルアルコール（ＩＰＡ）で順次超音波洗浄し、次いでＩＰＡで煮沸洗浄後乾燥した。さらに、ＵＶ／オゾン洗浄により有機物質を分解除去した。
[Atmospheric release]
Next, the substrate was taken out of the sputtering apparatus, ultrasonically cleaned with acetone and isopropyl alcohol (IPA) in sequence, then boiled and washed with IPA, and then dried. Furthermore, organic substances were decomposed and removed by UV / ozone cleaning.
［前処理］
有機ＥＬ蒸着装置へ移し真空排気し、前処理室で基板付近に設けたリング状電極に５０ＷのＲＦ電力を投入し酸素プラズマ洗浄処理を行った。酸素圧力は0.6Ｐａ、処理時間は40秒であった。
[Preprocessing]
The sample was transferred to an organic EL vapor deposition apparatus and evacuated, and 50 W RF power was applied to a ring electrode provided near the substrate in the pretreatment chamber to perform an oxygen plasma cleaning process. The oxygen pressure was 0.6 Pa and the treatment time was 40 seconds.
［正孔輸送層形成］
基板を前処理室より成膜室へ移動し、成膜室を、１×10Ｅ（-4）Ｐａまで排気した後、正孔輸送性を有するαＮＰＤを抵抗加熱蒸着法により成膜速度０.２〜０.３nm/secの条件で成膜、膜厚３５ｎｍ正孔輸送層を形成した。なお、正孔輸送層、発光層、および電子注入層は、同一の蒸着マスクを用いることにより所定の部分に蒸着した。所定の部分とは基板上で、Ｃｒが露出している部分である。（画素電極）
［発光層形成］
続いて正孔輸送層の上にアルキレート錯体であるＡｌｑ３を抵抗加熱蒸着法により正孔輸送層と同様の成膜条件で膜厚１５nm成膜、発光層を形成した。
[Hole transport layer formation]
The substrate was moved from the pretreatment chamber to the film formation chamber, and the film formation chamber was evacuated to 1 × 10E (−4) Pa. Then, αNPD having hole transportability was formed at a film formation rate of 0.2 by resistance heating vapor deposition. A film was formed under a condition of ˜0.3 nm / sec, and a 35 nm-thick hole transport layer was formed. Note that the hole transport layer, the light emitting layer, and the electron injection layer were deposited on predetermined portions by using the same deposition mask. The predetermined portion is a portion where Cr is exposed on the substrate. (Pixel electrode)
[Light emitting layer formation]
Subsequently, Alq 3 as an alkylate complex was formed on the hole transport layer by a resistance heating vapor deposition method under the same film formation conditions as the hole transport layer to form a 15 nm-thick film and a light emitting layer.
［電子注入電極層形成］
次に、発光層の上に抵抗加熱共蒸着法によりＡｌｑ３と炭酸セシウム（Ｃｓ２ＣＯ３）を膜厚比９：１の割合で混合されるよう、各々の蒸着速度を調整して成膜、膜厚３５nm電子注入層を形成した。詳しくは、それぞれの蒸着ボートにセットした材料を抵抗加熱方式で蒸発させ、有機層は〜５Ａ/Ｓ、共蒸着層もそれぞれのボート電流値を調整することで、あわせて〜5Ａ/Ｓの蒸着速度で膜形成を行った。
[Electron injection electrode layer formation]
Next, each deposition rate is adjusted to form a film so that Alq 3 and cesium carbonate (Cs 2 CO 3 ) are mixed on the light emitting layer by a resistance heating co-evaporation method at a film thickness ratio of 9: 1. An electron injection layer having a thickness of 35 nm was formed. Specifically, the material set in each vapor deposition boat is evaporated by resistance heating method, the organic layer is ~ 5A / S, and the co-deposition layer is also adjusted for each boat current value. Film formation was performed at a speed.
［陰極（透明導電膜）形成］
次に別の成膜室に基板を移し、電子注入層の上にＩＴＯターゲットを用いてDCマグネトロンスパッタリング法により、膜厚が130nmになるようマスク成膜によりＣｒ画素電極を覆って、Ｃｒストライプに交差するように、陰極Ｋを形成した。
[Cathode (transparent conductive film) formation]
Next, the substrate is moved to another film formation chamber, and the Cr pixel electrode is covered with a Cr film by using a magnetron sputtering method with an ITO target on the electron injection layer so that the film thickness becomes 130 nm. A cathode K was formed so as to intersect.
成膜中においては、成膜時間の経過につれてH2Oガス供給量を減少させることにより陰極Ｋの膜厚方向にHの濃度勾配を形成した。Hの濃度勾配は、電子注入電極層界面近傍においてHを5×1021〜1×1022atom/ccとし、膜厚方向に向かって連続的に濃度を低下させ、陰極Ｋの膜厚中心付近（電子注入電極層界面より65nm）でHの含有量が1020atom/cc台とした。なお、前述のようにＩＴＯターゲット裏面には強磁場タイプのマグネットが配置されており、低電圧スパッタリングが可能となっている。 During film formation, an H concentration gradient was formed in the film thickness direction of the cathode K by decreasing the H 2 O gas supply amount as the film formation time elapses. The concentration gradient of H is 5 × 10 21 to 1 × 10 22 atom / cc in the vicinity of the electron injection electrode layer interface, and the concentration is decreased continuously in the film thickness direction, near the film thickness center of the cathode K. The H content was on the order of 10 20 atoms / cc (65 nm from the electron injection electrode layer interface). As described above, a strong magnetic field type magnet is disposed on the back surface of the ITO target, and low voltage sputtering is possible.
成膜条件としては、基板加熱なしの室温成膜で成膜圧力を1.0Ｐａ、Ａｒ、H2OおよびO2ガスを用いそれぞれの流量は500、1.5、5.0scccmとし、ターゲットに印加する投入パワーはＩＴＯ：500Ｗで成膜を行った。透過率は85％（at.450nm）、比抵抗値は8.0Ｅ−4Ωcmであった。 Deposition conditions include room temperature film formation without substrate heating, film formation pressure of 1.0 Pa, Ar, H 2 O and O 2 gases, flow rates of 500, 1.5, 5.0 scccm, and input power applied to the target. Formed a film with ITO: 500W. The transmittance was 85% (at 450 nm), and the specific resistance value was 8.0E −4 Ωcm.
以上のようにして、符号１のガラス基板上に、陽極、正孔輸送層、発光層、電子注入電極層及び陰極を設け、有機ＥＬ発光素子を形成した。
As described above, the anode, the hole transport layer, the light emitting layer, the electron injection electrode layer, and the cathode were provided on the glass substrate denoted by
［保護膜の形成］
前述のガラス基板１上に形成した有機ＥＬ発光素子の表面上にスパッタリング法によりシリコン窒化酸化物を成膜、保護膜とした。
[Formation of protective film]
A silicon nitride oxide film was formed on the surface of the organic EL light emitting element formed on the
［充填工程］
次にシリコン窒化酸化物で保護した有機ＥＬ発光素子に空気中の水蒸気が浸入しないような充填材料でバリア性を付与させるため、封止工程に移る。
[Filling process]
Next, in order to impart barrier properties to the organic EL light-emitting element protected with silicon nitride oxide with a filling material that prevents water vapor from entering, the process proceeds to a sealing step.
用いる充填材としては、シクロオレフィンポリマーのフィルム（商品名：ゼオノアフィルム／日本ゼオン製）を用い、前記前記フィルム中に吸湿作用を併せ持つフィラーとして、ここでは合成シリカ（商品名：マイクロイド／東洋化学工業製）を１０ｗｔ％添加した材料を充填材として用いた。 As a filler to be used, a cycloolefin polymer film (trade name: ZEONOR FILM / manufactured by ZEON CORPORATION) is used. As a filler having a hygroscopic action in the film, synthetic silica (trade name: Microid / Toyo Chemical Co., Ltd.) is used here. A material to which 10 wt% of Kogyo) was added was used as a filler.
ここで上記保護膜と封止ガラスとを充填材を介して常圧プラズマ接合により接合させる工程は、グローブボックス（不図示）中の水分濃度を１０ｐｐｍ以下に制御した環境雰囲気中で行い、組み立て直後に、これまで大きな課題であったダークスポットの発生を押さえ込むことが可能となった。また、長期信頼性においても６０℃／９０％ＲＨの雰囲気条件で１０００時間の連続耐久試験を行ったが、輝度劣化等の発光特性の低下は確認されず、ダークスポット等の発生もなく、安定した有機ＥＬ素子とその製造方法を得ることが出来た。 Here, the step of bonding the protective film and the sealing glass by atmospheric pressure plasma bonding via a filler is performed in an environmental atmosphere in which the moisture concentration in the glove box (not shown) is controlled to 10 ppm or less, immediately after assembly. In addition, it has become possible to suppress the occurrence of dark spots, which has been a major issue. Also, for long-term reliability, a continuous durability test of 1000 hours was performed under an atmospheric condition of 60 ° C./90% RH, but no deterioration in light emission characteristics such as luminance deterioration was confirmed, and there was no occurrence of dark spots or the like. An organic EL device and a method for producing the same were obtained.
［素子評価］
長期信頼性においても表１に示すように、６０℃／９０％ＲＨの雰囲気条件で１０００時間の連続耐久試験を行ったが、封止材料中に内添したフィラーの作用により、外部からの余分な水分の浸入がないため、輝度劣化等の発光特性の低下はほとんど確認されず、ダークスポット等の発生もなく、安定した有機ＥＬ素子とその製造方法を得ることが出来た。
[Element evaluation]
In long-term reliability, as shown in Table 1, a continuous durability test was conducted for 1000 hours under an atmospheric condition of 60 ° C./90% RH. Since there was no permeation of moisture, there was almost no decrease in light emission characteristics such as luminance deterioration, and there was no occurrence of dark spots and the like, and a stable organic EL device and a method for producing the same could be obtained.
（第１の比較例）
第１の比較例は第１の実施例に対して、保護膜と充填材、及び封止ガラスの接合について、エポキシ系接着剤を用いた場合について示す。
(First comparative example)
The 1st comparative example shows the case where an epoxy system adhesive is used about joining of a protective film, a filler, and sealing glass to the 1st example.
ここで充填材として用いるシクロオレフィン系フィルム（商品名：ゼオノアフィルム／日本ゼオン製）の両面を不図示のスピンコーターにより塗布する。塗布後、封着ガラス２に貼り付け、次に保護膜側に貼り付ける。貼り付けた後、紫外線照射装置（ＥＸ２５０ HOYA-SHOTT製）により硬化させた。尚、その時の紫外線照射強度は１００ｍＷ／ｃｍ２で光量は３，０００ｍＪ／ｃｍ２である。
Here, both surfaces of a cycloolefin-based film (trade name: ZEONOR film / manufactured by Nippon Zeon) used as a filler are applied by a spin coater (not shown). After application, it is attached to the sealing
以上述べた封着工程は、グローブボックス（不図示）中の水分濃度を１０ｐｐｍ以下に制御して封着した。 In the sealing step described above, sealing was performed by controlling the water concentration in the glove box (not shown) to 10 ppm or less.
［素子評価］
組み立てた有機ＥＬ素子について、６０℃／９０％ＲＨの雰囲気条件で１０００時間の連続耐久試験を行ったが、余分な水分が封止材及び封止界面から浸入し、表１に示すように輝度劣化が進み、安定性に乏しい有機ＥＬ素子となった。
[Element evaluation]
The assembled organic EL device was subjected to a continuous durability test for 1000 hours under an atmospheric condition of 60 ° C./90% RH. Excess water entered from the sealing material and the sealing interface, and the luminance was as shown in Table 1. Deterioration progressed and it became an organic EL element with poor stability.
１ ガラス基板
２ 封着ガラス
３ 有機ＥＬ素子
４ 保護膜
５ 充填材
６ 常圧プラズマ表面処理装置
７ フィラー
８ 有機材料
DESCRIPTION OF
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| JP2004168319A JP2005347204A (en) | 2004-06-07 | 2004-06-07 | Organic el element and its manufacturing method |
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| JP2004168319A JP2005347204A (en) | 2004-06-07 | 2004-06-07 | Organic el element and its manufacturing method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007207521A (en) * | 2006-01-31 | 2007-08-16 | Tdk Corp | El panel |
| JP2011526052A (en) * | 2008-06-02 | 2011-09-29 | スリーエム イノベイティブ プロパティズ カンパニー | Adhesive encapsulating composition and electronic device made thereof |
| WO2013187500A1 (en) * | 2012-06-15 | 2013-12-19 | ランテクニカルサービス株式会社 | Electronic element sealing method and substrate junction |
| JP2015043422A (en) * | 2007-12-14 | 2015-03-05 | コミサリア ア レネルジー アトミック エ オ ゼネルジー アルテルナティブＣｏｍｍｉｓｓａｒｉａｔ Ａｌ’Ｅｎｅｒｇｉｅ Ａｔｏｍｉｑｕｅ Ｅｔ Ａｕｘ Ｅｎｅｒｇｉｅｓａｌｔｅｒｎａｔｉｖｅｓ | Device comprising organic component and package layer with moisture-reactive material |
| JP2017107756A (en) * | 2015-12-10 | 2017-06-15 | エルジー ディスプレイ カンパニー リミテッド | Flexible organic el display device, and method of manufacturing the same |
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2004
- 2004-06-07 JP JP2004168319A patent/JP2005347204A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007207521A (en) * | 2006-01-31 | 2007-08-16 | Tdk Corp | El panel |
| JP2015043422A (en) * | 2007-12-14 | 2015-03-05 | コミサリア ア レネルジー アトミック エ オ ゼネルジー アルテルナティブＣｏｍｍｉｓｓａｒｉａｔ Ａｌ’Ｅｎｅｒｇｉｅ Ａｔｏｍｉｑｕｅ Ｅｔ Ａｕｘ Ｅｎｅｒｇｉｅｓａｌｔｅｒｎａｔｉｖｅｓ | Device comprising organic component and package layer with moisture-reactive material |
| JP2011526052A (en) * | 2008-06-02 | 2011-09-29 | スリーエム イノベイティブ プロパティズ カンパニー | Adhesive encapsulating composition and electronic device made thereof |
| WO2013187500A1 (en) * | 2012-06-15 | 2013-12-19 | ランテクニカルサービス株式会社 | Electronic element sealing method and substrate junction |
| CN104412706A (en) * | 2012-06-15 | 2015-03-11 | 须贺唯知 | Electronic element sealing method and substrate junction |
| KR20150032252A (en) * | 2012-06-15 | 2015-03-25 | 랜 테크니컬 서비스 가부시키가이샤 | Electronic element sealing method and substrate junction |
| JP5704619B2 (en) * | 2012-06-15 | 2015-04-22 | 須賀 唯知 | Electronic device sealing method and substrate assembly |
| US9331305B2 (en) | 2012-06-15 | 2016-05-03 | Lan Technical Service Co., Ltd. | Electronic element sealing method and bonded substrate |
| KR102082954B1 (en) * | 2012-06-15 | 2020-02-28 | 랜 테크니컬 서비스 가부시키가이샤 | Electronic element sealing method and substrate junction |
| JP2017107756A (en) * | 2015-12-10 | 2017-06-15 | エルジー ディスプレイ カンパニー リミテッド | Flexible organic el display device, and method of manufacturing the same |
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