JP4910144B2 - Formation and apparatus of organic EL material thin film - Google Patents
Formation and apparatus of organic EL material thin film Download PDFInfo
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本発明は、所定の基材上に有機エレクトロルミネッセンス(以下、有機ＥＬ)材料の薄膜を形成する薄膜形成方法およびその装置に関する。 The present invention relates to a thin film forming method and apparatus for forming a thin film of an organic electroluminescence (hereinafter referred to as organic EL) material on a predetermined substrate.
従来の有機ＥＬ薄膜装置における有機EL層の形成には蒸着法あるいは湿式法がある。蒸着法は、蒸着可能な低分子有機材料を用いる方法で、均一性及び特性が良好なデバイスが実現できる。しかしながら、材料利用率が低い、大面積対応が難しいなどの欠点を有する。
湿式法は、溶液に溶解可能な高分子系有機材料を用いる方法で、簡単形成、大面積化可能、高い材料利用率の長所を持つが、溶液使用に伴う膜不均一、寿命を含めた特性が悪いなどの問題が有る。
There is a vapor deposition method or a wet method for forming an organic EL layer in a conventional organic EL thin film device. The vapor deposition method uses a low-molecular organic material that can be vapor-deposited, and can realize a device having good uniformity and characteristics. However, there are drawbacks such as low material utilization and difficulty in dealing with large areas.
The wet method is a method that uses a high molecular weight organic material that can be dissolved in a solution. It can be easily formed, can have a large area, and has a high material utilization rate. There are problems such as bad.
湿式法の工程は、有機EL溶液塗布工程、および溶媒乾燥工程からなる。有機EL溶液塗布工程にはスピンコート法、バーコート法、ブレードコート法、ロールコート法、スクリーン印刷法、インクジェットプリント法、スプレー法などが提案されている。
特に有機EL層形成は、従来の薄膜形成法以上の膜厚均一性が求められ、膜厚100 nmを形成する際、その不均一性を少なくとも5nm以下に抑えないと、発光むらが生ずる。この点からもより均一な薄膜形成法が求められている。ここで、溶液塗布工程において、基板上に均一に材料を供給することは可能であるが、基板面内の溶媒揮発速度むら、基板表面状態、乾燥雰囲気によって膜厚むらが生ずる。
The wet method process includes an organic EL solution coating process and a solvent drying process. For the organic EL solution coating step, spin coating, bar coating, blade coating, roll coating, screen printing, ink jet printing, spraying, and the like have been proposed.
In particular, the formation of the organic EL layer requires a film thickness uniformity higher than that of the conventional thin film formation method. When the film thickness of 100 nm is formed, if the non-uniformity is not suppressed to at least 5 nm or less, uneven light emission occurs. From this point, a more uniform thin film forming method is demanded. Here, in the solution application step, it is possible to supply the material uniformly onto the substrate, but the film thickness unevenness occurs depending on the solvent volatilization rate unevenness in the substrate surface, the substrate surface state, and the dry atmosphere.
均一な薄膜形成法については、特開2001-351780（特許文献１）で、有機EL溶液塗布工程後に基板回転処理を行うことで平滑層形成が可能と示されている。この工程は塗布工程に加え回転工程を行うプロセス増加が有り、スピンコート法で問題となる溶液流れによる放射状の筋むらが生ずる。また、特開2002-313566（特許文献２）において、前記溶媒を気化した溶媒蒸気中で行うことで溶媒蒸発時間を制御する方法が示されている。この方法では、溶媒蒸気雰囲気の制御を行う密閉環境を作製する必要がある。
面積ディスプレイや面光源用として、有機EL素子が盛んに研究されている。既に、簡便で短時間に大面積形成可能なスプレー法やペイント法が検討されている。しかし、溶液プロセスによる大面積有機材料塗布では、膜厚不均一が大きな問題となっていた。その為、溶液化された有機EL材料をスジむらやフォトルミネセンスむらが無く、均一で極薄膜といわれる100nm±2nmの膜厚を得る有機EL材料薄膜形成方法及び装置を提供が求められていた。 Organic EL devices have been actively researched for area displays and surface light sources. Already, a spray method and a paint method which are simple and can form a large area in a short time have been studied. However, in the application of a large area organic material by a solution process, non-uniform film thickness has been a big problem. Therefore, there has been a need to provide an organic EL material thin film forming method and apparatus for obtaining a film thickness of 100 nm ± 2 nm, which is uniform and called an ultrathin film, without causing unevenness of streaks or photoluminescence in the solution of the organic EL material. .
溶液化された有機ＥＬ材料を塗布する手段、被塗布材料を振動させる手段、被塗布材料を必要塗布量に応じて移動させる手段とを備える装置を使用し、溶液化された有機ＥＬ材料を塗布する工程において、被塗布材料を振動させながら圧着・移動させることで、上記課題を解決できることを見出し、本発明を完成した。 Applying the solutionized organic EL material using an apparatus comprising means for applying the solutionized organic EL material, means for vibrating the material to be applied, and means for moving the material to be applied according to the required application amount In this process, the present inventors have found that the above-mentioned problems can be solved by pressing and moving the material to be coated while vibrating and completed the present invention.
本発明は、溶液化された有機ＥＬ材料を含ませた塗布装置による手段、台の上に固定された被塗布材料を、ピエゾ素子等を用いた振動装置により上下又は左右に振動させる手段、被塗布材料を必要塗布量に応じて塗布装置に対して一定速度で移動させる移動装置、を利用して、溶液化された有機ＥＬ材料を含ませたローラー等の塗布装置に被塗布材料を振動させながら圧着・移動させることで、被塗布材料に均一で、極薄膜の有機ＥＬ材料を塗布する方法である。 The present invention relates to a means by a coating apparatus containing a solutionized organic EL material, a means for vibrating a material to be coated fixed on a table vertically or horizontally by a vibration device using a piezo element, etc. Using a moving device that moves the coating material at a constant speed with respect to the coating device according to the required coating amount, the coating material is vibrated in a coating device such as a roller containing a solutionized organic EL material. This is a method of applying an organic EL material that is uniform and extremely thin to the material to be coated by pressure bonding and moving.
本発明において、溶液化された有機ＥＬ材料を塗布する手段としては、被塗布材料に溶液化された有機ＥＬ材料を塗布することができる手段であれば、特に限定されないが、例えば、ローラー、刷毛、スプレーなどによる塗布が挙げられる。好ましいものは、ローラーによる塗布である。 In the present invention, the means for applying the solutionized organic EL material is not particularly limited as long as it is a means capable of applying the solutionized organic EL material to the material to be applied. For example, a roller, a brush, etc. And application by spraying. Preferable is application by a roller.
本発明において、被塗布材料を振動させる手段としては、被塗布材料自体、または被塗布材料を載せる台を振動させることできる手段であれば、特に限定されないが、例えば、ピエゾ素子を利用した振動が挙げられる。 In the present invention, the means for vibrating the material to be coated is not particularly limited as long as it is a means capable of vibrating the material to be coated itself or a table on which the material to be coated is placed. For example, vibration using a piezo element is generated. Can be mentioned.
本発明において、被塗布材料を振動させる装置の振動数は、振動数は、薄膜の材料等により適宜選択されるが、2KHz〜12kHz、好ましくは3KHz〜10ｋHzである。
また、振動装置の振幅は、薄膜の材料等により適宜選択されるが、1.5〜2.5ミクロン程度、好ましくは２ミクロン程度である。
In the present invention, the frequency of the apparatus for vibrating the material to be coated is appropriately selected depending on the material of the thin film, but is 2 kHz to 12 kHz, preferably 3 kHz to 10 kHz.
The amplitude of the vibration device is appropriately selected depending on the material of the thin film, but is about 1.5 to 2.5 microns, preferably about 2 microns.
本発明において、振動装置での被塗布材料の移動速度は、必要塗布量に応じて、適宜調節されるが、例えば、必要塗布量が、厚さ100nmの場合、固定された回転ローラーに対して10cm/secある。 In the present invention, the moving speed of the material to be coated by the vibration device is appropriately adjusted according to the required coating amount. For example, when the necessary coating amount is 100 nm in thickness, 10cm / sec.
図１は、溶液化された有機ＥＬ材料を塗布する手段としてローラーを使用する場合、図２は、溶液化された有機ＥＬ材料を塗布する手段としてスプレーを使用する場合の模式図である。 FIG. 1 is a schematic diagram in the case where a roller is used as a means for applying the solutionized organic EL material, and FIG. 2 is a schematic view in a case where a spray is used as the means for applying the solutionized organic EL material.
従来技術の問題点を解決することで、面積ディスプレイや面光源用としての大面積有機材料塗布方法及び装置を提供することができ、有機EL材料をスジむらやフォトルミネセンスむらが無い、均一で極薄膜の素子を提供できる。 By solving the problems of the prior art, it is possible to provide a large-area organic material application method and apparatus for area display and surface light source, uniform organic EL materials without uneven stripes or photoluminescence. An ultra-thin element can be provided.
図３は、本発明の一の実施形態に係わる有機EL塗布方法に使用される有機EL材料塗布装置の構成を模式的に示す側面図である。
この有機EL材料塗布装置は、溶液化された有機ＥＬ材料を含ませた回転ローラーを固定し、ピエゾ素子等を用いた振動装置を利用して振動数が3kHz、6kHz及び10kHzとし、振幅が2ミクロン程度にて上下に振動させる台（ステージ）に被塗布材料を載せた被塗布装置、被塗布材料を載せたステージを必要塗布量（厚さ100nm）に応じて固定された回転ローラー
に対して10cm/secで平行移動させて、溶液化された有機ＥＬ材料を含ませたローラーから
被塗布材料に均一に有機ＥＬ材料を塗布させるものである。
以下に、実施例により本発明を具体的に説明するが、本発明はこれら実施例に限定される
ものではない。
FIG. 3 is a side view schematically showing the configuration of an organic EL material coating apparatus used in the organic EL coating method according to one embodiment of the present invention.
This organic EL material application device fixes a rotating roller containing a solution of organic EL material, uses a vibration device using a piezo element, etc., and has a frequency of 3 kHz, 6 kHz and 10 kHz, and an amplitude of 2 A coating device with a material to be coated on a stage (stage) that vibrates up and down around a micron, and a stage with the material to be coated on a rotating roller fixed according to the required coating amount (thickness 100 nm) The organic EL material is uniformly applied to the material to be coated from a roller containing the solution-solved organic EL material by translation at 10 cm / sec.
EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples.
ＩＺＯ基板上に正孔注入層poly(ethylenedioxythiophene)/poly(styrenesulfonate)(ＰＥＤＯＴ)をスピンコートした。次に、正孔輸送性ホストポリマーであるポリ(9-ビニルカルバゾール)［poly(9-vinylcarbazole:PVCz］、電子輸送材料である2,5-ビス(1-ナフチル)-1,3,4-オキサジアゾール［2,5-bis(1-naphtyl)-1,3,4-oxzdiazole；BND］、緑色発光ドーパント材料であるクマリン６[coumarin6；C6]を混合したテトラヒドロフラン(THF)1wt%溶液（PVCz:BND:C6=160:40:1）を作製し、成膜製向上のためテトラリン(tetralin)を15%混入した。インク浸透ローラ下で、基板固定したステージ移動して発光層を成膜した。移動速度は10cm/s、デバイス構造はIZO/PEDOT/PVCｚ＋BND＋C6/LiF(1nm)/Al(70nm)である。最後に、LiF/Al陰極を真空蒸着で成膜した。 A hole injection layer poly (ethylenedioxythiophene) / poly (styrenesulfonate) (PEDOT) was spin-coated on the IZO substrate. Next, hole transporting host polymer poly (9-vinylcarbazole) [poly (9-vinylcarbazole: PVCz]], electron transporting material 2,5-bis (1-naphthyl) -1,3,4- Tetrahydrofuran (THF) 1 wt% solution in which oxadiazole [2,5-bis (1-naphtyl) -1,3,4-oxzdiazole; BND] and green light emitting dopant material coumarin6 [Cumarin6; C6] are mixed ( PVCz: BND: C6 = 160: 40: 1) and mixed with 15% tetralin to improve film formation, moving the stage fixed to the substrate under the ink penetration roller and forming the light emitting layer The moving speed was 10 cm / s, the device structure was IZO / PEDOT / PVCz + BND + C6 / LiF (1 nm) / Al (70 nm) Finally, a LiF / Al cathode was formed by vacuum deposition.
結果は図４(a)にTHF溶媒のみの場合、図４(b)にTHF+tetralin溶液、図４(c)にTHF＋tetralin溶液を使用した薄膜成形法によるフォトルミネセンス（PL）及び電圧印加による発光（EL）写真を示す。発光面積は3cmＸ3cmである。THFのみの場合、膜厚ムラによるリーク電流が大きく、EL発光は得られなかった。テトラリン混入により成膜性は向上し、EL発光は得られたが、膜厚が不均一なため、輝度ムラが発生した。 The results are shown in Fig. 4 (a) with only THF solvent, Fig. 4 (b) with THF + tetralin solution, Fig. 4 (c) with photoluminescence (PL) and voltage application by thin film forming method using THF + tetralin solution. An luminescence (EL) photograph is shown. The light emission area is 3 cm × 3 cm. In the case of THF alone, the leakage current due to film thickness unevenness was large, and EL emission was not obtained. Film formation improved with the incorporation of tetralin, and EL light emission was obtained, but uneven brightness occurred because the film thickness was non-uniform.
その為、薄膜形成法として、溶液化された有機ＥＬ材料を含ませた回転ローラーを固定し、ピエゾ素子等を用いた振動装置を利用して振動数が3kHz、6kHz及び10kHzとし、振幅が２ミクロン程度にて上下に振動させるステージに被塗布材料を載せた被塗布装置、被塗布材料を載せたステージを必要塗布量（厚さ100nm）に応じて固定された回転ローラーに対して10cm/secで平行移動させて、溶液化された有機ＥＬ材料を含ませたローラーから被塗布材料に均一に有機ＥＬ材料を塗布させた所、膜厚均一性向上に成功した。塗布厚さを検証した所、98nm〜102nmの範囲に含まれていた。 Therefore, as a thin film formation method, a rotating roller containing a solution of organic EL material is fixed, and a vibration device using a piezoelectric element or the like is used to set the frequency to 3 kHz, 6 kHz, and 10 kHz, and an amplitude of 2 A coating device with a material to be coated on a stage that vibrates up and down at about a micron, and a stage with the material to be coated on a rotating roller fixed according to the required coating amount (thickness 100 nm) at 10 cm / sec. The film was moved in parallel, and the organic EL material was uniformly applied to the material to be applied from the roller containing the solutionized organic EL material, and the film thickness uniformity was successfully improved. When the coating thickness was verified, it was in the range of 98 nm to 102 nm.
5cm角の大面積で、100nmの極薄膜の有機ELの塗布が確認された。大面積の試料に対して極薄膜で均一な溶液化された有機ＥＬを塗布することが出来、携帯電話のバックライト、デ
ィスプレイ表示等に利用することが可能である。
It was confirmed that the organic EL was applied with a 100nm ultrathin film with a large area of 5cm square. An organic EL in a uniform solution form can be applied to a large-area sample with a very thin film, and can be used for backlights of mobile phones, display displays, and the like.
Claims (10)
The apparatus for forming an organic EL material thin film according to any one of claims 6 to 9, wherein an organic EL material having a thickness of 100 nm is applied to the material to be coated.
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