JP3577115B2 - Organic electroluminescent device - Google Patents
Organic electroluminescent device Download PDFInfo
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- JP3577115B2 JP3577115B2 JP23285094A JP23285094A JP3577115B2 JP 3577115 B2 JP3577115 B2 JP 3577115B2 JP 23285094 A JP23285094 A JP 23285094A JP 23285094 A JP23285094 A JP 23285094A JP 3577115 B2 JP3577115 B2 JP 3577115B2
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- 238000005401 electroluminescence Methods 0.000 claims description 18
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 239000013039 cover film Substances 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 239000010408 film Substances 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910021332 silicide Inorganic materials 0.000 description 5
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- 230000005525 hole transport Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004104 aryloxy group Chemical group 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 238000010549 co-Evaporation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 125000000040 m-tolyl group Chemical group [H]C1=C([H])C(*)=C([H])C(=C1[H])C([H])([H])[H] 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/805—Electrodes
- H10K50/82—Cathodes
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
Landscapes
- Luminescent Compositions (AREA)
- Electroluminescent Light Sources (AREA)
Description
【０００１】
【産業上の利用分野】
本発明は有機エレクトロルミネセンス（ＥＬ）素子に係り、特にその寿命を長くするための保護膜に関する。
【０００２】
【従来の技術】
有機ＥＬ素子は、薄形の新しい発光源として注目されている。従来の有機ＥＬ素子は、図３に示す如く、ガラス基板１０上にＩＴＯからなる透明電極１を形成し、この上に正孔注入輸送層２、発光層３、電子注入輸送層４、陰極５等を形成することにより構成されている。
【０００３】
正孔注入輸送層２としては、例えば下記化１で表されるテトラアリールジアミン誘導体を使用する。
【０００４】
【化１】
〔化１において、Ｒ１ 、Ｒ２ 、Ｒ３ 及びＲ４ はそれぞれアリール基、アルキル基、アルコキシ基、アリールオキシ基、アミノ基又はハロゲン原子を表す。ｒ１ 、ｒ２、ｒ３及びｒ４は、それぞれ０又は１〜５の整数である。Ｒ５ 及びＲ６ は、アルキル基、アルコキシ基、アミノ基又はハロゲン原子を表し、これらは同一でも異なる物であってもよい。ｒ５及びｒ６は、それぞれ０又は１〜４の整数である。〕
発光層３としては、前記化１で示すテトラアリールジアミン誘導体と、後述する電子注入輸送層４で使用されるトリス（８−キノリノラト）アルミニウム等の混合されたものが使用される。
【０００６】
電子注入輸送層４としては、例えばトリス（８−キノリノラト）アルミニウムが使用される。陰極５としては、ＭｇＡｇ（例えば重量比１０：１）を使用する。
【０００７】
【発明が解決しようとする課題】
ところで、前記の如く構成された有機ＥＬ素子は、最初は強く発光しているが、時間が経過するにつれて発光強度が急速に減少するという欠点がある。
【０００８】
本発明者はこの問題を改善すべく研究したところ、これが陰極の構成材料にＭｇが存在するため、非常に酸化し易いことにもとづくことが解明された。従って本発明の目的は、発光強度を長時間持続させるために、陰極が酸化され難いような保護膜を具備した有機ＥＬ素子を提供することである。
【０００９】
【課題を解決するための手段】
前記目的を達成するため、本発明では、図１に示す如く、陰極５をＳｉ層６でコーティングし、このＳｉ層６を更にＳｉＯ２ 等で構成されるカバー膜７でコーティングする。
【００１０】
【作用】
ＭｇＡｇの陰極５をＳｉ層６でコーティングすると陰極５を構成する金属とＳｉとのシリサイドが形成されるので耐酸化性が向上し、有機ＥＬ素子の発光時間を長くできる。しかもその上に更にＳｉＯ２ 等で形成されたカバー膜７をコーティングすることにより耐酸化性が更に向上し、発光時間を一層長くすることができる。
【００１１】
【実施例】
本発明の一実施例を図１及び図２に基づき説明する。図１は本発明の一実施例構成図、図２はその特性図である。
【００１２】
図１において、１は透明電極、２は正孔注入輸送層、３は発光層、４は電子注入輸送層、５は陰極、６はＳｉ層、７はカバー膜、１０はガラス基板である。
透明電極１は陽極となるものであって例えばＩＴＯ等で構成されガラス基板１０上に蒸着又はスパッタリングにより成膜される。
【００１３】
正孔注入輸送層２は、前記化１で表されるテトラアリールジアミン誘導体や、下記化２で表されるＮ，Ｎ′−ジ（３−メチルフェニル）−Ｎ，Ｎ′−ジフェニル−４，４′−ジアミノ−１，１′ビフェニルを蒸着することにより形成される。
【００１４】
【化２】
発光層３は、前記正孔注入輸送層２を構成する例えば化１で表されるテトラアリールジアミン誘導体と、後述する電子注入輸送層４を構成する例えばトリス（８−キノリノラト）アルミニウムとの混合物が使用される。この場合、異なる蒸着源より蒸発させる共蒸着が好ましいがこれに限定されるものではない。勿論蛍光性物質を含ませることもできる。
【００１６】
電子注入輸送層４は、例えばトリス（８−キノリノラト）アルミニウムを蒸着するにより形成される。
陰極５は、仕事関数の小さい材料で構成され、例えばＭｇＡｇで構成されるが、Ｉｎを使用することもできる。陰極５は蒸着又はスパッタリングにより成膜される。
【００１７】
Ｓｉ層６は、陰極５をコーティングして酸化を防止するものであり、Ｓｉをスパッタリングすることで約１０００Åの厚さに成膜される。この条件を下記に示す。
【００１８】
温度 室温
パワー ５０〜５００Ｗ
キャリアガス Ａｒ
圧力 ０．０１ Ｔｏｒｒ
ＤＣ
カバー膜７はＳｉ層６をコーティングして更に陰極５の酸化を防止するものである。このカバー膜７の厚さは例えば２０００Åであり、例えばＳｉＯ２ を用いて下記の条件で成膜される。
【００１９】
温度 室温
Ｐｏｗｅｒ ５０〜５００Ｗ
キャリアガス Ａｒ
圧力 ０．０１ Ｔｏｒｒ
高周波
カバー膜７はＳｉＯ２ に限定されるものではなく、Ｓｉ３ Ｎ４ を用いても同様である。
【００２０】
本発明においては、基板１０に透明電極１、正孔注入輸送層２、発光層３、電子注入輸送層４、陰極５を積層するところまでは図３に示す従来例と同じである。
【００２１】
しかし本発明では、陰極５をＳｉ層６でコーティングし、更にＳｉ層６をＳｉＯ２ 等で形成されたカバー膜７でコーティングする。陰極５をＳｉ層６でコーティングすることによりそのコーティングされた面に陰極５を構成する金属であるＭｇＡｇとシリサイドが形成される。シリサイドは酸化されにくい性質があり、陰極５が酸化しにくいものとなる。しかもこのＳｉ層６の上にＳｉＯ２ 等で形成されたカバー膜７をコーティングするので、これにより一層酸化防止作用が強くなる。
【００２２】
このように、本発明による保護膜でカバーされた有機ＥＬ素子の特性を図２で示す。図２においてＡは、図１で示す如く、本発明による保護膜でカバーされた有機ＥＬ素子の発光時間特性を示し、Ｂは図３で示す従来の構造の有機ＥＬ素子の発光時間特性を示す。図２において横軸は時間（ｈｒ）、縦軸は単位面積当たりの発光光度（カンデラ（ｃｄ）／ｃｍ２ ）を示す。従来の構成の有機ＥＬ素子は１０００ｈｒで発光光度が大きく減衰するのに対し、本発明の保護膜でカバーされた有機ＥＬ素子は１万時間を経由しても１／２の発光光度が保持されている。なお図２はＮ２ 雰囲気中で測定した値である。
【００２３】
また前記実施例では、有機ＥＬ素子として正孔注入輸送層、発光層、電子注入輸送層の３層構成の有機ＥＬ素子例について説明したが本発明はこれに限定されるものではない。例えば正孔輸送層（発光層）＋電子輸送層、正孔輸送層＋電子輸送層（発光層）の如きものに対しても同様に適用できる。
【００２４】
【発明の効果】
請求項１、請求項２、請求項３に記載された本発明によれば、有機ＥＬ素子の陰極に対しシリサイドを形成して耐酸化性を向上することができ、しかもこのシリサイドの上にカバー層を形成して更に耐酸化性を向上する保護膜を提供できるので、有機ＥＬ素子の寿命を非常に長くすることができる。
【図面の簡単な説明】
【図１】本発明の一実施例構成図である。
【図２】本発明の特性図である。
【図３】従来例の有機ＥＬ素子である。
【符号の説明】
１ 透明電極
２ 正孔注入輸送層
３ 発光層
４ 電子注入輸送層
５ 陰極
６ Ｓｉ層
７ カバー層
１０ ガラス基板[0001]
[Industrial applications]
The present invention relates to an organic electroluminescence (EL) device, and more particularly, to a protective film for extending the life of the device.
[0002]
[Prior art]
The organic EL element has been attracting attention as a new thin light emitting source. In a conventional organic EL device, as shown in FIG. 3, a transparent electrode 1 made of ITO is formed on a
[0003]
As the hole injection transport layer 2, for example, a tetraaryldiamine derivative represented by the following formula 1 is used.
[0004]
Embedded image
[In the formula 1, R 1 , R 2 , R 3 and R 4 each represent an aryl group, an alkyl group, an alkoxy group, an aryloxy group, an amino group or a halogen atom. r1 , R2, r3 and r4 are each 0 or an integer of 1 to 5. R 5 and R 6 represent an alkyl group, an alkoxy group, an amino group or a halogen atom, which may be the same or different. r5 and r6 are each 0 or an integer of 1 to 4. ]
As the light-emitting layer 3, a mixture of a tetraaryldiamine derivative represented by Chemical Formula 1 and tris (8-quinolinolato) aluminum used in an electron injection /
[0006]
As the electron
[0007]
[Problems to be solved by the invention]
By the way, the organic EL device configured as described above emits strong light at first, but has a drawback that the light emission intensity rapidly decreases as time passes.
[0008]
The present inventor has studied to improve this problem, and has found that this is based on the fact that Mg is present in the constituent material of the cathode and is very easily oxidized. Accordingly, an object of the present invention is to provide an organic EL device having a protective film in which the cathode is hardly oxidized in order to maintain emission intensity for a long time.
[0009]
[Means for Solving the Problems]
In order to achieve the above object, in the present invention, as shown in FIG. 1, the cathode 5 is coated with a Si layer 6, and the Si layer 6 is further coated with a cover film 7 made of SiO 2 or the like.
[0010]
[Action]
When the MgAg cathode 5 is coated with the Si layer 6, a silicide of the metal constituting the cathode 5 and Si is formed, so that the oxidation resistance is improved and the emission time of the organic EL element can be extended. Moreover, by further coating a cover film 7 made of SiO 2 or the like thereon, the oxidation resistance is further improved, and the light emission time can be further lengthened.
[0011]
【Example】
One embodiment of the present invention will be described with reference to FIGS. FIG. 1 is a configuration diagram of an embodiment of the present invention, and FIG. 2 is a characteristic diagram thereof.
[0012]
In FIG. 1, 1 is a transparent electrode, 2 is a hole injection / transport layer, 3 is a light emitting layer, 4 is an electron injection / transport layer, 5 is a cathode, 6 is a Si layer, 7 is a cover film, and 10 is a glass substrate.
The transparent electrode 1 serves as an anode and is made of, for example, ITO or the like, and is formed on the
[0013]
The hole injecting / transporting layer 2 may be made of a tetraaryldiamine derivative represented by the above formula 1, N, N′-di (3-methylphenyl) -N, N′-diphenyl-4, It is formed by evaporating 4'-diamino-1,1'biphenyl.
[0014]
Embedded image
The light emitting layer 3 is made of a mixture of, for example, a tetraaryldiamine derivative represented by Chemical Formula 1 constituting the hole injection transport layer 2 and tris (8-quinolinolato) aluminum constituting the electron
[0016]
The electron injecting and transporting
The cathode 5 is made of a material having a small work function, for example, MgAg, but In may be used. The cathode 5 is formed by vapor deposition or sputtering.
[0017]
The Si layer 6 is for coating the cathode 5 to prevent oxidation, and is formed to a thickness of about 1000 ° by sputtering Si. The conditions are shown below.
[0018]
Temperature Room temperature power 50-500W
Carrier gas Ar
Pressure 0.01 Torr
DC
The cover film 7 coats the Si layer 6 to further prevent the cathode 5 from being oxidized. The thickness of the cover film 7 is, for example, 2000 °, and is formed using, for example, SiO 2 under the following conditions.
[0019]
Temperature Room temperature Power 50-500W
Carrier gas Ar
Pressure 0.01 Torr
The high-frequency cover film 7 is not limited to SiO 2 , and the same applies even when Si 3 N 4 is used.
[0020]
The present invention is the same as the conventional example shown in FIG. 3 up to the point where the transparent electrode 1, the hole injection / transport layer 2, the light emitting layer 3, the electron injection /
[0021]
However, in the present invention, the cathode 5 is coated with the Si layer 6, and the Si layer 6 is further coated with the cover film 7 formed of SiO 2 or the like. By coating the cathode 5 with the Si layer 6, MgAg which is a metal constituting the cathode 5 and silicide are formed on the coated surface. Silicide has a property of being hardly oxidized, and the cathode 5 is hardly oxidized. Moreover, since the cover film 7 made of SiO 2 or the like is coated on the Si layer 6, the anti-oxidation effect is further enhanced.
[0022]
FIG. 2 shows the characteristics of the organic EL device covered with the protective film according to the present invention. In FIG. 2, A shows the emission time characteristics of the organic EL device covered with the protective film according to the present invention as shown in FIG. 1, and B shows the emission time characteristics of the organic EL device having the conventional structure shown in FIG. . In FIG. 2, the horizontal axis represents time (hr), and the vertical axis represents luminous intensity per unit area (candela (cd) / cm 2 ). While the luminous intensity of the conventional organic EL element is greatly attenuated at 1000 hours, the luminous intensity of the organic EL element covered with the protective film of the present invention is maintained at 1/2 even after 10,000 hours. ing. FIG. 2 shows values measured in an N 2 atmosphere.
[0023]
Further, in the above-described embodiment, an example of an organic EL element having a three-layer structure of a hole injection / transport layer, a light emitting layer, and an electron injection / transport layer has been described, but the present invention is not limited thereto. For example, the present invention can be similarly applied to a material such as a hole transport layer (light emitting layer) + electron transport layer and a hole transport layer + electron transport layer (light emitting layer).
[0024]
【The invention's effect】
According to the first, second, and third aspects of the present invention, the oxidation resistance can be improved by forming silicide on the cathode of the organic EL element, and a cover is formed on the silicide. Since a protective film for improving the oxidation resistance can be provided by forming a layer, the life of the organic EL element can be greatly extended.
[Brief description of the drawings]
FIG. 1 is a configuration diagram of an embodiment of the present invention.
FIG. 2 is a characteristic diagram of the present invention.
FIG. 3 shows a conventional organic EL element.
[Explanation of symbols]
REFERENCE SIGNS LIST 1 transparent electrode 2 hole injection / transport layer 3
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23285094A JP3577115B2 (en) | 1994-09-28 | 1994-09-28 | Organic electroluminescent device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23285094A JP3577115B2 (en) | 1994-09-28 | 1994-09-28 | Organic electroluminescent device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0896962A JPH0896962A (en) | 1996-04-12 |
| JP3577115B2 true JP3577115B2 (en) | 2004-10-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23285094A Expired - Fee Related JP3577115B2 (en) | 1994-09-28 | 1994-09-28 | Organic electroluminescent device |
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| Country | Link |
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| JP (1) | JP3577115B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5608287A (en) * | 1995-02-23 | 1997-03-04 | Eastman Kodak Company | Conductive electron injector for light-emitting diodes |
| US6583557B2 (en) | 2000-04-26 | 2003-06-24 | Canon Kabushiki Kaisha | Organic luminescent element |
| KR20020082038A (en) * | 2001-04-23 | 2002-10-30 | 주식회사 마이크로아이 | Organic electroluminescence element package and method for manufacturing same |
-
1994
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| Publication number | Publication date |
|---|---|
| JPH0896962A (en) | 1996-04-12 |
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