JP2005032618A - Organic el device - Google Patents

Organic el device Download PDF

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JP2005032618A
JP2005032618A JP2003271759A JP2003271759A JP2005032618A JP 2005032618 A JP2005032618 A JP 2005032618A JP 2003271759 A JP2003271759 A JP 2003271759A JP 2003271759 A JP2003271759 A JP 2003271759A JP 2005032618 A JP2005032618 A JP 2005032618A
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hole injection
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injection layer
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upper electrode
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JP4396163B2 (en
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Harumi Suzuki
晴視 鈴木
Junji Kido
淳二 城戸
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Denso Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To suppress damages of a hole injection layer at the time of forming an upper electrode and realize a high hole injection efficiency in the organic EL element having a top emission structure with a transparent upper electrode functioning as an anode. <P>SOLUTION: This is an organic EL element in which a luminous layer 31 composed of an organic EL material, a hole injection layer 40, and the upper electrode 50 functioning as an anode are formed in order on a lower electrode 20 functioning as a cathode. The upper electrode is made of ITO or the like transmitting visible light and the hole injection layer 40 contains an inorganic material made of oxide or the like of transition metal based such as vanadium oxide or the like and has an electron receptiveness. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、有機ＥＬ（エレクトロルミネッセンス）素子に関する。   The present invention relates to an organic EL (electroluminescence) element.

有機ＥＬ素子は、自己発光のため視認性に優れ、かつ、数Ｖ〜数十Ｖの低電圧駆動が可能なため駆動回路を含めた軽量化が可能である。そこで薄膜型ディスプレイ、照明、バックライトとしての活用が期待できる。   The organic EL element is excellent in visibility due to self-emission, and can be driven at a low voltage of several V to several tens V, and thus can be reduced in weight including a driving circuit. Therefore, it can be expected to be used as a thin film display, lighting, and backlight.

このような有機ＥＬ素子は、一般に、基板の上に下部電極、有機ＥＬ材料からなる発光層、上部電極を順次形成してなり、下部電極をＩＴＯ（インジウムチンオキサイド）等の透明導電膜等からなる陽極として機能させ、上部電極を金属膜等からなる陰極として機能させて発光層に電荷を注入し、発光を行うようにしている。そして、この一般的な構成では、発光層の光は下部電極側から取り出される。   Such an organic EL element is generally formed by sequentially forming a lower electrode, a light emitting layer made of an organic EL material, and an upper electrode on a substrate, and the lower electrode is made of a transparent conductive film such as ITO (indium tin oxide). The anode is made to function, and the upper electrode is made to function as a cathode made of a metal film or the like to inject charges into the light emitting layer to emit light. And in this general structure, the light of a light emitting layer is taken out from the lower electrode side.

このような一般的な構成に対して、上部電極をＩＴＯ等からなる透明電極として可視光を透過するものとし、発光層からの光を上部電極側から取り出す構成にしたものがある。このような構成はいわゆるトップエミッション構造といわれている。   In contrast to such a general configuration, there is a configuration in which the upper electrode is a transparent electrode made of ITO or the like and transmits visible light, and the light from the light emitting layer is extracted from the upper electrode side. Such a configuration is called a so-called top emission structure.

このトップエミッション構造を採用する場合、パネル全体が透明であるデバイスを形成することが可能である。また、トップエミッション構造にすることで、アクティブ駆動で問題となる開口率の向上が見込まれ、輝度低下特性の優れたデバイスも形成可能である。   When this top emission structure is adopted, it is possible to form a device in which the entire panel is transparent. Further, the top emission structure is expected to improve the aperture ratio which is a problem in active driving, and a device having excellent luminance reduction characteristics can be formed.

この開口率の向上について具体的に述べると、アクティブ駆動では、各画素毎に下部電極の下側に画素駆動用のＴＦＴ（薄膜トランジスタ）が設けられるが、下部電極側から光の取り出しを行う場合、画素中にＴＦＴが占める領域では光が透過せず、その領域の分、開口率が小さくなる。   Specifically speaking, in the active drive, a pixel driving TFT (thin film transistor) is provided below the lower electrode for each pixel in the active drive. When light is extracted from the lower electrode side, In the area occupied by the TFT in the pixel, light is not transmitted, and the aperture ratio is reduced by that area.

しかし、上部電極側から光の取り出しを行う場合、ＴＦＴの領域に関係なく光を取り出すことができ、開口率低下の問題は回避される。   However, when light is extracted from the upper electrode side, light can be extracted regardless of the TFT region, and the problem of a decrease in aperture ratio is avoided.

従来では、このようなトップエミッション構造の場合、通常、下部電極側を陽極として機能させ、上部透明電極を陰極として機能させる構成としている（例えば、特許文献１参照）。そのために、陰極である透明電極からの電子注入特性をいかに向上させるかがポイントであった。   Conventionally, in the case of such a top emission structure, usually, the lower electrode side is made to function as an anode, and the upper transparent electrode is made to function as a cathode (see, for example, Patent Document 1). Therefore, the point was how to improve the electron injection characteristics from the transparent electrode as the cathode.

上記した一般的な構成では、陰極はＡｌ（アルミニウム）等の金属である。例えばＡｌの仕事関数は３．８ｅＶ程度なので、上記の一般的な構成では、適切な電子注入電極すなわち陰極が実現できている。しかし、ＩＴＯ等の透明電極を陰極とする場合、例えば、ＩＴＯの仕事関数は５ｅＶ程度であるので電子注入性に劣るものとなる。   In the general configuration described above, the cathode is a metal such as Al (aluminum). For example, since the work function of Al is about 3.8 eV, an appropriate electron injection electrode, that is, a cathode can be realized in the above general configuration. However, when a transparent electrode such as ITO is used as the cathode, for example, the work function of ITO is about 5 eV, so that the electron injecting property is inferior.

この問題を回避するために、最近、トップエミッション構造において、下部電極を陰極として機能させ、上部透明電極を陽極として機能させるものが、数は少ないものの提案されている（非特許文献１参照）。   In order to avoid this problem, recently, in the top emission structure, there have been a small number of proposals in which the lower electrode functions as a cathode and the upper transparent electrode functions as an anode (see Non-Patent Document 1).

この非特許文献１のなかで、上部透明電極を陽極として利用する場合の課題として、上部透明電極からのホールの注入が問題となることが明らかにされている。これは、陽極の仕事関数の不整合によってホールの注入が行われにくくなることが原因であるとされている。   In Non-Patent Document 1, it has been clarified that hole injection from the upper transparent electrode becomes a problem as a problem when the upper transparent electrode is used as an anode. This is attributed to the fact that hole injection becomes difficult due to mismatch of the work function of the anode.

具体的には、上記の一般的な構成において、下部透明電極を陽極として用いる場合には、下部透明電極を形成した後、その電極をＵＶ（紫外線）やプラズマを用いた表面処理等によって表面改質（酸化）をすることが可能である。それによって、陽極である下部透明電極の仕事関数を大きくして、ホールの注入障壁を小さくすることが可能である。   Specifically, in the above general configuration, when the lower transparent electrode is used as an anode, after the lower transparent electrode is formed, the electrode is subjected to surface modification by surface treatment using UV (ultraviolet light) or plasma. Quality (oxidation) is possible. As a result, the work function of the lower transparent electrode as the anode can be increased, and the hole injection barrier can be reduced.

しかし、上記非特許文献１に記載のトップエミッション構造のように、上部透明電極を陽極として利用する場合は、有機膜の上に直接、上部透明電極を形成することになる。そのため、上述した表面改質の手法が、陽極である上部透明電極に対して使用できず、上部透明電極のホールの注入障壁が大きいままであり、ホール注入効率が非常に小さくなる。   However, when the upper transparent electrode is used as an anode as in the top emission structure described in Non-Patent Document 1, the upper transparent electrode is formed directly on the organic film. Therefore, the surface modification method described above cannot be used for the upper transparent electrode as the anode, the hole injection barrier of the upper transparent electrode remains large, and the hole injection efficiency becomes very small.

これに対して、さらに、上記非特許文献１では、ペンタセンという非常に導電率の高い有機材料を、ホール注入層として上部透明電極の下地に４０ｎｍ程度形成することで、ホール注入効率が向上することが述べられている。
特表２０００−５０７０２９号公報 Ｔ．Ｄｏｂｂｅｒｔｉｎ、外８名，「Ｉｎｖｅｒｔｅｄ ｔｏｐ−ｅｍｉｔｔｉｎｇ ｏｒｇａｎｉｃ ｌｉｇｈｔ−ｅｍｉｔｔｉｎｇ ｄｉｏｄｅｓ ｕｓｉｎｇ ｓｐｕｔｔｅｒ−ｄｅｐｏｓｉｔｅｄ ａｎｏｄｅｓ」，ＡＰＰＬＩＥＤ ＰＨＹＳＩＣＳ ＬＥＴＴＥＲＳ，（米国），ＶＯＬＵＭＥ２，ＮＵＭＢＥＲ２，ｐ．２８４−２８６ On the other hand, in Non-Patent Document 1, the hole injection efficiency is improved by forming an organic material such as pentacene having a very high conductivity on the base of the upper transparent electrode as the hole injection layer. Is stated.
JP 2000-507029 gazette T.A. Robertin, 8 others, “Inverted top-emitting organic light-emitting diodes using sputter-deposited anodes”, APPLIED PHYSICS LETTERS, (USA), VOLUME2, NUMPER2. 284-286

ところで、上記非特許文献１に記載のトップエミッション構造において、上部透明電極を形成する場合、すなわち上部電極としてＩＴＯ等の透明導電膜を成膜する場合には、通常スパッタ法が用いられる。   By the way, in the top emission structure described in Non-Patent Document 1, when an upper transparent electrode is formed, that is, when a transparent conductive film such as ITO is formed as the upper electrode, a normal sputtering method is used.

しかしながら、この場合、そのスパッタ時に下地の有機膜すなわちホール注入層であるペンタセンが熱やイオンによりダメージを受けて、ホール注入性が低下することが問題となる。   However, in this case, there is a problem that the base organic film, that is, the pentacene which is the hole injection layer is damaged by heat or ions during the sputtering, and the hole injection property is lowered.

本発明は上記問題に鑑み、陰極として機能する下部電極の上に、有機ＥＬ材料からなる発光層、ホール注入層、陽極として機能する上部電極を順次形成してなるトップエミッション構造の有機ＥＬ素子において、上部電極を形成する際のホール注入層のダメージを抑制し、高いホール注入効率の確保を実現することを目的とする。   In view of the above problems, the present invention provides an organic EL element having a top emission structure in which a light emitting layer made of an organic EL material, a hole injection layer, and an upper electrode functioning as an anode are sequentially formed on a lower electrode functioning as a cathode. An object of the present invention is to suppress damage to the hole injection layer when forming the upper electrode and to ensure high hole injection efficiency.

上記目的を達成するため、請求項１に記載の発明では、陰極として機能する下部電極（２０）の上に、有機ＥＬ材料からなる発光層（３１）、ホール注入層（４０）、陽極として機能する上部電極（５０）を順次形成してなる有機ＥＬ素子において、前記上部電極は、可視光を透過するものであり、前記ホール注入層は、無機材料を含むものであって電子受容性を有するものであることを特徴としている。   In order to achieve the above object, according to the first aspect of the present invention, a light emitting layer (31) made of an organic EL material, a hole injection layer (40), and an anode function on the lower electrode (20) functioning as a cathode. In the organic EL device in which the upper electrode (50) is sequentially formed, the upper electrode transmits visible light, and the hole injection layer includes an inorganic material and has an electron accepting property. It is characterized by being.

本発明は、実験的に見出されたものであり、本発明のホール注入層（４０）は、無機材料を含むものであるため、有機膜からなる従来のホール注入層に比べて熱やイオンによるダメージを受けにくい。また、電子受容性を有するのでホール注入層として適切に機能する。   The present invention has been found experimentally, and since the hole injection layer (40) of the present invention contains an inorganic material, it is damaged by heat and ions as compared with a conventional hole injection layer made of an organic film. It is hard to receive. Moreover, since it has an electron accepting property, it functions appropriately as a hole injection layer.

よって、本発明によれば、陽極として機能する透明な上部電極（５０）を有するトップエミッション構造の有機ＥＬ素子において、上部電極（５０）を形成する際のホール注入層（４０）のダメージを抑制し、高いホール注入効率の確保を実現することができる。   Therefore, according to the present invention, in the organic EL device having the top emission structure having the transparent upper electrode (50) functioning as the anode, the damage of the hole injection layer (40) when the upper electrode (50) is formed is suppressed. In addition, high hole injection efficiency can be ensured.

請求項２に記載の発明では、前記ホール注入層（４０）は、２ｎｍ以上２０ｎｍ以下の厚さであることを特徴とする。   The invention according to claim 2 is characterized in that the hole injection layer (40) has a thickness of 2 nm or more and 20 nm or less.

ホール注入層（４０）が薄すぎると、上部電極形成時にダメージが入りやすくホール注入層として機能しにくく、厚すぎると、ホール注入層中のホール移動の抵抗成分が大きくなり、ホール注入効率が低下しやすい。本発明者の検討によれば、ホール注入層（４０）が２ｎｍから２０ｎｍの膜厚であり、好ましくは３ｎｍから１０ｎｍ程度であればよい。   If the hole injection layer (40) is too thin, damage is likely to occur when the upper electrode is formed, and it will be difficult to function as a hole injection layer. If it is too thick, the resistance component of hole movement in the hole injection layer will increase and the hole injection efficiency will decrease. It's easy to do. According to the study of the present inventor, the hole injection layer (40) has a thickness of 2 nm to 20 nm, preferably about 3 nm to 10 nm.

請求項３に記載の発明では、前記ホール注入層（４０）は、前記無機材料として遷移金属系の酸化物を含むものであることを特徴とする。   The invention according to claim 3 is characterized in that the hole injection layer (40) contains a transition metal oxide as the inorganic material.

一般に酸化物は絶縁性であるが、遷移金属系の酸化物は電子受容性を有するため、ホール注入層として適切に機能する。そのため、ホール注入層（４０）に含まれる無機材料として、遷移金属系の酸化物を含むものを採用することができる。   In general, an oxide is insulative, but a transition metal oxide has an electron accepting property, and thus functions appropriately as a hole injection layer. Therefore, as the inorganic material contained in the hole injection layer (40), a material containing a transition metal oxide can be employed.

具体的に、遷移金属系の酸化物としては、請求項４に記載の発明のように、酸化バナジウム、酸化モリブデンおよび酸化ルテニウムから選択されるものを採用することができる。   Specifically, as the transition metal-based oxide, an oxide selected from vanadium oxide, molybdenum oxide, and ruthenium oxide can be adopted as in the invention described in claim 4.

また、請求項５に記載の発明のように、ホール注入層（４０）は、無機物のルイス酸もしくは有機物のルイス酸が添加されたものとしてもよい。それによれば、電子受容性が高まり、ホール注入性のさらなる向上が実現できる。   Further, as in the invention described in claim 5, the hole injection layer (40) may be added with an inorganic Lewis acid or an organic Lewis acid. According to this, the electron acceptability is enhanced, and the hole injection property can be further improved.

具体的に、無機物のルイス酸としては塩化第二鉄等が挙げられ、有機物のルイス酸としてはＤＤＱ（ジシアノージクロロキノン）、ＴＮＦ（トニトロノフルオレノン）、ＴＣＮＱ（テトラシアノキノジメタン）等が挙げられる。   Specific examples of inorganic Lewis acids include ferric chloride, and organic Lewis acids include DDQ (dicyano-dichloroquinone), TNF (tonitronofluorenone), TCNQ (tetracyanoquinodimethane), and the like. Is mentioned.

請求項６に記載の発明では、前記ホール注入層（４０）の直下に位置する下地層として、ホール輸送層（３３）としての銅フタロシアニンからなる膜が形成されていることを特徴とする。   The invention according to claim 6 is characterized in that a film made of copper phthalocyanine as a hole transport layer (33) is formed as an underlayer located immediately below the hole injection layer (40).

ホール注入層（４０）としてはイオン化ポテンシャルが小さい方が、陽極である上部電極（５０）からホール注入層（４０）を介して発光層（３１）へ、ホールが注入されやすい。その点、銅フタロシアニンは比較的イオン化ポテンシャルが小さいので、上部電極（５０）から発光層（３１）へのホールの注入がスムーズになる。   As the hole injection layer (40), when the ionization potential is smaller, holes are more easily injected from the upper electrode (50), which is the anode, into the light emitting layer (31) through the hole injection layer (40). In that respect, since copper phthalocyanine has a relatively low ionization potential, holes are smoothly injected from the upper electrode (50) into the light emitting layer (31).

さらに、銅フタロシアニンは、アモルファスではなく結晶性の膜であるので、有機膜に比べて銅フタロシアニン膜自体が熱に対して安定である。そのため、銅フタロシアニン膜の上に位置し無機材料を含む膜であるホール注入層（４０）が、高温で剥離しにくいものになる。   Furthermore, since copper phthalocyanine is not an amorphous film but a crystalline film, the copper phthalocyanine film itself is more stable against heat than an organic film. Therefore, the hole injection layer (40), which is a film containing an inorganic material and located on the copper phthalocyanine film, is difficult to peel off at a high temperature.

なお、上記各手段の括弧内の符号は、後述する実施形態に記載の具体的手段との対応関係を示す一例である。   In addition, the code | symbol in the bracket | parenthesis of each said means is an example which shows a corresponding relationship with the specific means as described in embodiment mentioned later.

以下、本発明を図に示す実施形態について説明する。なお、以下の各実施形態相互において、同一の部分には図中、同一符号を付してある。   DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments shown in the drawings will be described below. In the following embodiments, the same parts are denoted by the same reference numerals in the drawings.

（第１実施形態）
図１は本発明の第１実施形態に係る有機ＥＬ素子Ｓ１の概略断面構成を示す図である。基板１０は、可視光を透過可能な基板つまり透明基板であり、ガラスや透明樹脂からなる。本例では、基板１０はガラス基板１０である。 (First embodiment)
FIG. 1 is a diagram showing a schematic cross-sectional configuration of an organic EL element S1 according to the first embodiment of the present invention. The substrate 10 is a substrate that can transmit visible light, that is, a transparent substrate, and is made of glass or transparent resin. In this example, the substrate 10 is a glass substrate 10.

ガラス基板１０の上に、陰極として機能する下部電極２０が形成されている。本例では、下部電極２０は、１００ｎｍ程度の厚さの反射電極として銀とマグネシウム（Ａｇ−Ｍｇ）を９：１で共蒸着した層からなる。   A lower electrode 20 that functions as a cathode is formed on the glass substrate 10. In this example, the lower electrode 20 is composed of a layer in which silver and magnesium (Ag—Mg) are co-deposited at a ratio of 9: 1 as a reflective electrode having a thickness of about 100 nm.

下部電極２０の上には、有機ＥＬ材料からなる発光層３１を含む有機層３０、３１、３２、３３が形成されている。これら有機層３０〜３３は一般的な有機ＥＬ素子に用いられるホール輸送性材料、電子輸送性材料、蛍光色素等を採用することができる。   On the lower electrode 20, organic layers 30, 31, 32, and 33 including a light emitting layer 31 made of an organic EL material are formed. These organic layers 30 to 33 can employ hole transport materials, electron transport materials, fluorescent dyes, and the like used in general organic EL elements.

本例では、図１において下部電極２０の直上に位置する電子輸送層３０は、アルミキノリノール（Ａｌｑ３）を２０ｎｍ蒸着した層からなり、その上に位置する発光層３１は、Ａｌｑ３を４０ｎｍ蒸着した層からなる。   In this example, the electron transport layer 30 positioned immediately above the lower electrode 20 in FIG. 1 is a layer in which aluminum quinolinol (Alq3) is deposited by 20 nm, and the light emitting layer 31 positioned thereon is a layer in which Alq3 is deposited by 40 nm. Consists of.

また、その上に位置するホール輸送層３２、３３は２層構成となっており、下から順に、αーナフチル・フェニル・ベンゼン（α−ＮＰＤ）を４０ｎｍ蒸着してなるホール輸送層３２、銅フタロシアニン（ＣｕＰｃ）を１５ｎｍ蒸着してなるホール輸送層３３となっている。   In addition, the hole transport layers 32 and 33 located on the upper layer have a two-layer structure. In order from the bottom, a hole transport layer 32 formed by depositing α-naphthyl phenyl benzene (α-NPD) by 40 nm, copper phthalocyanine. The hole transport layer 33 is formed by vapor-depositing (CuPc) by 15 nm.

ホール輸送層３３の上には、ホール注入層４０が形成されている。本実施形態では、ホール注入層４０は、無機材料を含むものであって電子受容性を有するものである。そして、ホール注入層４０は、２ｎｍ以上２０ｎｍ以下の厚さであることが好ましい。   A hole injection layer 40 is formed on the hole transport layer 33. In the present embodiment, the hole injection layer 40 includes an inorganic material and has an electron accepting property. The hole injection layer 40 preferably has a thickness of 2 nm to 20 nm.

このようなホール注入層４０は、無機材料として遷移金属系の酸化物を含むものにすることができる。具体的に、遷移金属系の酸化物としては、酸化バナジウム、酸化モリブデンおよび酸化ルテニウム等から選択されるものを採用することができる。   Such a hole injection layer 40 can include a transition metal oxide as an inorganic material. Specifically, as the transition metal oxide, an oxide selected from vanadium oxide, molybdenum oxide, ruthenium oxide, and the like can be used.

本例では、ホール注入層４０は、酸化バナジウム（Ｖ2Ｏ5）を５ｎｍ蒸着してなる層としている。そして、ホール注入層４０の上には、陽極として機能する上部電極５０が形成されている。本例では、上部電極５０は厚さ１５０ｎｍのＩＴＯとしている。 In this example, the hole injection layer 40 is a layer formed by depositing 5 nm of vanadium oxide (V 2 O 5 ). An upper electrode 50 that functions as an anode is formed on the hole injection layer 40. In this example, the upper electrode 50 is made of ITO having a thickness of 150 nm.

このような有機ＥＬ素子Ｓ１は、例えば、次のようにして製造される。ガラス基板１０の上に、蒸着法により、厚さ１００ｎｍのＡｇ−Ｍｇからなる下部電極２０を形成し、Ａｌｑ３を２０ｎｍ蒸着し、さらに４０ｎｍ蒸着して電子輸送層３０、発光層３１を形成する。   Such an organic EL element S1 is manufactured as follows, for example. A lower electrode 20 made of Ag-Mg having a thickness of 100 nm is formed on the glass substrate 10 by vapor deposition, and Alq3 is vapor-deposited by 20 nm, and further 40 nm is vapor-deposited to form an electron transport layer 30 and a light-emitting layer 31.

さらに、その上にα−ＮＰＤを４０ｎｍ蒸着し、ＣｕＰｃを１５ｎｍ蒸着してホール輸送層３２、３３を形成し、その上に、酸化バナジウム（Ｖ2Ｏ5）を５ｎｍ蒸着してホール注入層４０を形成する。 Furthermore, α-NPD is vapor-deposited to 40 nm thereon, CuPc is vapor-deposited to 15 nm to form hole transport layers 32 and 33, and vanadium oxide (V 2 O 5 ) is vapor-deposited to 5 nm thereon to form hole injection layer 40. Form.

そして、スパッタ法により厚さ１５０ｎｍのＩＴＯ膜からなる上部電極５０を形成する。ここで、スパッタ条件は、プラズマパワーは５ｎｍ／ｍｉｎ（パワー：５００Ｗ程度）、アルゴンガスも微量の酸素を導入して成膜することができる。こうして、上記した本例の有機ＥＬ素子Ｓ１ができあがる。   Then, an upper electrode 50 made of an ITO film having a thickness of 150 nm is formed by sputtering. Here, the sputtering conditions are such that the plasma power is 5 nm / min (power: about 500 W), and the argon gas can also be formed by introducing a small amount of oxygen. Thus, the above-described organic EL element S1 of this example is completed.

ところで、本実施形態のホール注入層４０は、無機材料を含むものであるため、上記したペンタセンのような有機膜からなる従来のホール注入層に比べて熱やイオンによるダメージを受けにくい。また、電子受容性を有するのでホール注入層として適切に機能する。   By the way, since the hole injection layer 40 of this embodiment contains an inorganic material, it is less susceptible to damage by heat or ions than the conventional hole injection layer made of an organic film such as pentacene. Moreover, since it has an electron accepting property, it functions appropriately as a hole injection layer.

よって、本実施形態によれば、陽極として機能する透明な上部電極５０を有するトップエミッション構造の有機ＥＬ素子Ｓ１において、上部電極５０を形成する際のホール注入層４０のダメージを抑制し、高いホール注入効率の確保を実現することができる。   Therefore, according to this embodiment, in the organic EL element S1 having a top emission structure having the transparent upper electrode 50 functioning as an anode, damage to the hole injection layer 40 when the upper electrode 50 is formed is suppressed, and high holes are formed. It is possible to ensure the injection efficiency.

また、上述したように、ホール注入層４０は、２ｎｍ以上２０ｎｍ以下の厚さであることが好ましいが、これは、ホール注入層４０が薄すぎると、上部電極５０の形成時にダメージが入りやすくホール注入層として機能せず、厚すぎると、ホール注入層４０中のホール移動の抵抗成分が大きくなり、ホール注入効率が低下するためである。   As described above, the hole injection layer 40 preferably has a thickness of 2 nm or more and 20 nm or less. However, if the hole injection layer 40 is too thin, damage is easily caused when the upper electrode 50 is formed. This is because if it does not function as an injection layer and is too thick, a resistance component of hole movement in the hole injection layer 40 increases and hole injection efficiency decreases.

本発明者の検討によれば、ホール注入層４０が２ｎｍから２０ｎｍの膜厚であり、好ましくは３ｎｍから１０ｎｍ程度であればよい。   According to the study of the present inventors, the hole injection layer 40 has a thickness of 2 nm to 20 nm, preferably about 3 nm to 10 nm.

また、上述したように、ホール注入層４０に含まれる無機材料として遷移金属系の酸化物を採用できるが、これは、一般の酸化物が絶縁性であるのに対して、遷移金属系の酸化物は電子受容性を有するため、ホール注入層として適切に機能するためである。   In addition, as described above, a transition metal-based oxide can be employed as the inorganic material included in the hole injection layer 40. This is because a general oxide is insulative, whereas a transition metal-based oxide is used. This is because the material has an electron accepting property and functions appropriately as a hole injection layer.

本実施形態の有機ＥＬ素子Ｓ１の効果について、具体的に述べる。上記したガラス基板１０の上に、Ａｇ−Ｍｇからなる下部電極２０、Ａｌｑ３からなる電子輸送層３０、発光層３１、それぞれα−ＮＰＤ、ＣｕＰｃからなるホール輸送層３２、３３、Ｖ2Ｏ5からなるホール注入層４０、ＩＴＯ膜からなる上部電極５０を順次形成してなる有機ＥＬ素子Ｓ１を形成した。 The effect of the organic EL element S1 of this embodiment will be specifically described. On the glass substrate 10 described above, the lower electrode 20 made of Ag—Mg, the electron transport layer 30 made of Alq 3, the light emitting layer 31, the hole transport layers 32, 33 made of α-NPD and CuPc, respectively, and V 2 O 5 An organic EL element S1 formed by sequentially forming a hole injection layer 40 and an upper electrode 50 made of an ITO film was formed.

この有機ＥＬ素子Ｓ１については、色度座標（０．３２０、 ０．６３）の緑色発光が得られることを確認した。そして、この有機ＥＬ素子Ｓ１の発光特性を調べた結果を図２に示す。図２では、比較例として図１においてホール注入層４０の無い構成とした素子についての発光特性も並記してある。   For this organic EL element S1, it was confirmed that green light emission of chromaticity coordinates (0.320, 0.63) was obtained. And the result of having investigated the light emission characteristic of this organic EL element S1 is shown in FIG. 2, as a comparative example, the light emission characteristics of an element without the hole injection layer 40 in FIG. 1 are also shown.

本実施形態の有機ＥＬ素子Ｓ１によれば、図２に示すように、その発光特性として、６０ｍＡ／ｃｍ2で１０００ｃｄ／ｍ2の高輝度な素子が得られた。また、発光効率は、図２中のグラフ線の傾きから求められるが、本実施形態では、ホール注入層４０の無い比較例の素子と比べて、発光効率は２倍の１．６ｃｄ／Ａに向上した。また、本実施形態では発光面もムラは無く良好であった。 According to the organic EL element S1 of the present embodiment, as shown in FIG. 2, a high-luminance element having a light emission characteristic of 1000 cd / m 2 at 60 mA / cm 2 was obtained. The luminous efficiency can be obtained from the slope of the graph line in FIG. 2, but in this embodiment, the luminous efficiency is 1.6 cd / A, which is twice that of the comparative element without the hole injection layer 40. Improved. Further, in the present embodiment, the light emitting surface is also excellent without unevenness.

さらに、上記した本実施形態の例では、ホール注入層４０の直下に位置する下地層として、ホール輸送層３３としてのＣｕＰｃからなる膜が形成されていることも特徴である。   Furthermore, the above-described example of the present embodiment is characterized in that a film made of CuPc as the hole transport layer 33 is formed as a base layer located immediately below the hole injection layer 40.

ホール注入層４０としてはイオン化ポテンシャル（Ｉｐ）が小さい方が、陽極である上部電極５０からホール注入層４０を介して発光層３１へ、ホールが注入されやすい。その点、ＣｕＰｃは比較的Ｉｐが小さいので、上部電極５０から発光層３１へのホールの注入がスムーズになる。   When the ionization potential (Ip) is smaller as the hole injection layer 40, holes are more easily injected from the upper electrode 50, which is an anode, into the light emitting layer 31 through the hole injection layer 40. In that respect, since CuPc has a relatively small Ip, holes are smoothly injected from the upper electrode 50 into the light emitting layer 31.

ちなみに、上記した本実施形態の例において、ＩＴＯからなる上部電極５０のＩｐは４．７〜４．８ｅＶ、Ｖ2Ｏ5からなるホール注入層４０のＩｐは５．３ｅＶ、ＣｕＰｃからなるホール輸送層３３のＩｐは５．３ｅＶ、α−ＮＰＤからなるホール輸送層３２のＩｐは５．４ｅＶであり、これら各層間のＩｐの変化がスムーズなものとなっている。 Incidentally, in the example of the present embodiment described above, the Ip of the upper electrode 50 made of ITO is 4.7 to 4.8 eV, the Ip of the hole injection layer 40 made of V 2 O 5 is 5.3 eV, and the hole transport made of CuPc. The Ip of the layer 33 is 5.3 eV, the Ip of the hole transport layer 32 made of α-NPD is 5.4 eV, and the change of Ip between these layers is smooth.

さらに、ＣｕＰｃは、アモルファスではなく結晶性の膜であるので、有機膜に比べてＣｕＰｃ膜自体が熱に対して安定である。そのため、ＣｕＰｃ膜３３の上に位置し無機材料を含む膜であるホール注入層４０は、高温で剥離しにくいものになり、安定した膜となる。   Furthermore, since CuPc is not an amorphous film but a crystalline film, the CuPc film itself is more stable against heat than an organic film. Therefore, the hole injection layer 40, which is a film containing an inorganic material and located on the CuPc film 33, is difficult to peel off at a high temperature and becomes a stable film.

（第２実施形態）
図３は、本発明の第２実施形態に係る有機ＥＬ素子Ｓ２の概略断面構成を示す図である。本実施形態は、上記第１実施形態において、電子輸送層３０と発光層３１との間にホールブロック層６０を介在させたことが相違点である。 (Second Embodiment)
FIG. 3 is a diagram showing a schematic cross-sectional configuration of an organic EL element S2 according to the second embodiment of the present invention. The present embodiment is different from the first embodiment in that a hole blocking layer 60 is interposed between the electron transport layer 30 and the light emitting layer 31.

このホールブロック層６０により、発光層３１から電子輸送層３０へのホールの突き抜けを防止するようにしている。   The hole block layer 60 prevents holes from penetrating from the light emitting layer 31 to the electron transport layer 30.

具体的には、基板１０、下部電極２０、有機膜３０、３１、３２、３３、ホール注入層４０、上部電極５０は、上記第１実施形態と同様の材質例とすることができる。   Specifically, the substrate 10, the lower electrode 20, the organic films 30, 31, 32, 33, the hole injection layer 40, and the upper electrode 50 can be made of material examples similar to those in the first embodiment.

そして、ホールブロック層６０としては、蒸着法により形成された厚さ２０ｎｍのＩｐ（イオン化ポテンシャル）＞６．０ｅＶの材料からなる層とすることができる。例えばＢＣＰ（２，９−ジメチル−４，７−ジフェニル−１，１０−フェナントロリン）などが挙げられる。   The hole blocking layer 60 may be a layer made of a material having a thickness of 20 nm and an Ip (ionization potential)> 6.0 eV formed by a vapor deposition method. Examples thereof include BCP (2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline).

このような具体的な構成とした本実施形態の有機ＥＬ素子Ｓ２によれば、その発光効率は、上記図２に示した第１実施形態の有機ＥＬ素子の発光効率に比べて２ｃｄ／Ａに向上した。   According to the organic EL element S2 of this embodiment having such a specific configuration, the luminous efficiency is 2 cd / A compared to the luminous efficiency of the organic EL element of the first embodiment shown in FIG. Improved.

この結果は、ホール注入層４０を形成することで、発光層３１において過剰なホールが存在することを示し、さらに、ホールブロック層６０を挿入することで、下部電極２０である陰極に突き抜けるホールを抑制したことが発光効率の向上に寄与していることを示す。   This result shows that by forming the hole injection layer 40, there are excess holes in the light emitting layer 31, and further, by inserting the hole block layer 60, holes penetrating into the cathode as the lower electrode 20 are formed. It shows that suppressing has contributed to the improvement of luminous efficiency.

そして、このことは、本実施形態および上記第１実施形態のようにホール注入性を改善した場合、反対側の陰極である下部電極２０側からの電子との注入バランスをいかに整えるかが発光効率の向上に重要であるかを示している。   And, this means that when the hole injection property is improved as in the present embodiment and the first embodiment, how to adjust the injection balance with the electrons from the lower electrode 20 side, which is the opposite cathode, is the luminous efficiency. It is important to improve.

（第３実施形態）
また、ホール注入層４０としては、無機物のルイス酸もしくは有機物のルイス酸が添加されたものであってもよい。 (Third embodiment)
Further, the hole injection layer 40 may be one to which an inorganic Lewis acid or an organic Lewis acid is added.

無機物のルイス酸としては塩化第二鉄等が挙げられ、有機物のルイス酸としてはＤＤＱ（ジシアノージクロロキノン）、ＴＮＦ（トニトロノフルオレノン）、ＴＣＮＱ（テトラシアノキノジメタン）等が挙げられる。   Examples of inorganic Lewis acids include ferric chloride, and examples of organic Lewis acids include DDQ (dicyano-dichloroquinone), TNF (tonitronofluorenone), and TCNQ (tetracyanoquinodimethane).

例えば、そのような本実施形態のホール注入層４０としては、ＤＤＱ（ジシアノージクロロキノン）を、酸化バナジウム（Ｖ2Ｏ5）に５％ドープした構造とすることができる。これは、共蒸着により形成することができる。 For example, such a hole injection layer 40 of this embodiment can have a structure in which DDQ (dicyano-dichloroquinone) is doped with 5% of vanadium oxide (V 2 O 5 ). This can be formed by co-evaporation.

このような構成としたホール注入層４０において、上記した各ルイス酸のドープ濃度は、酸化バナジウム等のホール注入・輸送性材料に対して１０倍以内程度がよい。   In the hole injection layer 40 having such a configuration, the doping concentration of each Lewis acid described above is preferably within about 10 times that of a hole injection / transport material such as vanadium oxide.

これは、１０倍を超えると酸化分子すなわち酸化バナジウム等の膜中濃度が極端に少なくなり、上部電極５０の形成時におけるホール注入層４０のダメージ防止の効果が発現しにくくなるためである。   This is because if it exceeds 10 times, the concentration of oxidized molecules, that is, vanadium oxide, in the film becomes extremely small, and the effect of preventing damage to the hole injection layer 40 during the formation of the upper electrode 50 becomes difficult.

なお、上記各実施形態において示した各例の素子構造は、単純化した素子構造であり、下部電極２０や発光層３１等は、他の構造を使ってもよい。   In addition, the element structure of each example shown in each said embodiment is a simplified element structure, and the lower electrode 20, the light emitting layer 31, etc. may use another structure.

例えば、上記例では、発光層３１に蛍光色素をドープしていないが、ドープしてもよい。また、下部電極２０に透明電極を用いれば、非発光時には透明で、発光時に両面から発光を確認する構成とすることも可能である。   For example, in the above example, the light emitting layer 31 is not doped with a fluorescent dye, but may be doped. Further, if a transparent electrode is used for the lower electrode 20, it is possible to adopt a configuration that is transparent when no light is emitted and light emission is confirmed from both sides when light is emitted.

また、ホール注入層４０の形成方法として、その下地の有機膜の分解などを避けるために、ダメージの入りにくい蒸着法を用いたが、成膜法などの工夫により、スパッタなどの他の方法を用いることも可能である。   In addition, as a method for forming the hole injection layer 40, a vapor deposition method that is difficult to cause damage is used in order to avoid decomposition of the underlying organic film. It is also possible to use it.

また、一方で、上部透明電極の構造すなわちトップエミッション構造ではなく、上述した一般的な構造の有機ＥＬ素子ではあるけれども、ホール注入層として、酸化バナジウムを用いたものが、特開平９−６３７７１号公報に提案されている。   On the other hand, although it is not the structure of the upper transparent electrode, that is, the top emission structure, but the organic EL element having the general structure described above, the one using vanadium oxide as the hole injection layer is disclosed in Japanese Patent Application Laid-Open No. 9-63771. Proposed in the gazette.

この場合、トップエミッション構造でないことから、下部電極であるＩＴＯの表面処理後にホール注入層を形成できるため、ホール注入層を３０ｎｍと厚い酸化バナジウム層にすることで高いホール注入効率を得ている。   In this case, since it is not a top emission structure, a hole injection layer can be formed after the surface treatment of ITO which is a lower electrode. Therefore, a high hole injection efficiency is obtained by making the hole injection layer as thick as 30 nm.

つまり、この従来公報における酸化バナジウムを用いた構成は、ＩＴＯの表面処理が可能な一般的な有機ＥＬ素子構造におけるものであり、本発明とは課題が違う。また、電荷注入層としての酸化バナジウム層のメカニズムも違うと考えており、その結果、上記実施形態では、酸化バナジウム層は厚さが２ｎｍ程度と薄くてもホール注入特性を向上させている。   That is, the configuration using vanadium oxide in this conventional publication is in a general organic EL element structure capable of surface treatment of ITO, and is different from the present invention. Further, it is considered that the mechanism of the vanadium oxide layer as the charge injection layer is also different. As a result, in the above embodiment, the hole injection characteristics are improved even if the vanadium oxide layer is as thin as about 2 nm.

本発明の第１実施形態に係る有機ＥＬ素子を示す概略断面図である。It is a schematic sectional drawing which shows the organic EL element which concerns on 1st Embodiment of this invention. 第１実施形態に係る有機ＥＬ素子の発光特性を示す図である。It is a figure which shows the light emission characteristic of the organic EL element which concerns on 1st Embodiment. 本発明の第２実施形態に係る有機ＥＬ素子を示す概略断面図である。It is a schematic sectional drawing which shows the organic EL element which concerns on 2nd Embodiment of this invention.

符号の説明Explanation of symbols

２０…下部電極、３１…発光層、
３３…ホール注入層の直下に位置する下地層としてのホール輸送層、
４０…ホール注入層、５０…上部電極。 20 ... lower electrode, 31 ... light emitting layer,
33 ... a hole transport layer as a base layer located directly under the hole injection layer,
40 ... hole injection layer, 50 ... upper electrode.

Claims (6)

陰極として機能する下部電極（２０）の上に、有機ＥＬ材料からなる発光層（３１）、ホール注入層（４０）、陽極として機能する上部電極（５０）を順次形成してなる有機ＥＬ素子において、
前記上部電極は、可視光を透過するものであり、
前記ホール注入層は、無機材料を含むものであって電子受容性を有するものであることを特徴とする有機ＥＬ素子。 In an organic EL element in which a light emitting layer (31) made of an organic EL material, a hole injection layer (40), and an upper electrode (50) functioning as an anode are sequentially formed on a lower electrode (20) functioning as a cathode. ,
The upper electrode transmits visible light,
The organic EL element, wherein the hole injection layer contains an inorganic material and has an electron accepting property. 前記ホール注入層（４０）は、２ｎｍ以上２０ｎｍ以下の厚さであることを特徴とする請求項１に記載の有機ＥＬ素子。 The organic EL device according to claim 1, wherein the hole injection layer (40) has a thickness of 2 nm or more and 20 nm or less. 前記ホール注入層（４０）は、前記無機材料として遷移金属系の酸化物を含む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ＥＬ素子。 The organic EL element according to claim 1, wherein the hole injection layer includes a transition metal oxide as the inorganic material. 前記遷移金属系の酸化物は、酸化バナジウム、酸化モリブデンおよび酸化ルテニウムから選択されるものであることを特徴とする請求項３に記載の有機ＥＬ素子。 The organic EL device according to claim 3, wherein the transition metal oxide is selected from vanadium oxide, molybdenum oxide, and ruthenium oxide. 前記ホール注入層（４０）は、無機物のルイス酸もしくは有機物のルイス酸が添加されたものであることを特徴とする請求項１ないし４のいずれか一つに記載の有機ＥＬ素子。 5. The organic EL device according to claim 1, wherein the hole injection layer is formed by adding an inorganic Lewis acid or an organic Lewis acid. 6. 前記ホール注入層（４０）の直下に位置する下地層として、ホール輸送層（３３）としての銅フタロシアニンからなる膜が形成されていることを特徴とする請求項１ないし５のいずれか一つに記載の有機ＥＬ素子。
6. A film made of copper phthalocyanine as a hole transport layer (33) is formed as a base layer located immediately below the hole injection layer (40). The organic EL element of description.
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