JP3509693B2 - Manufacturing method of organic EL device - Google Patents
Manufacturing method of organic EL deviceInfo
- Publication number
- JP3509693B2 JP3509693B2 JP2000103991A JP2000103991A JP3509693B2 JP 3509693 B2 JP3509693 B2 JP 3509693B2 JP 2000103991 A JP2000103991 A JP 2000103991A JP 2000103991 A JP2000103991 A JP 2000103991A JP 3509693 B2 JP3509693 B2 JP 3509693B2
- Authority
- JP
- Japan
- Prior art keywords
- organic
- gas
- film
- manufacturing
- supporting gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 238000001771 vacuum deposition Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 description 40
- 239000010410 layer Substances 0.000 description 15
- 238000007789 sealing Methods 0.000 description 11
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 8
- 229910001882 dioxygen Inorganic materials 0.000 description 8
- 239000012298 atmosphere Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000005525 hole transport Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- APVPOHHVBBYQAV-UHFFFAOYSA-N n-(4-aminophenyl)sulfonyloctadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NS(=O)(=O)C1=CC=C(N)C=C1 APVPOHHVBBYQAV-UHFFFAOYSA-N 0.000 description 1
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 1
- 229910000127 oxygen difluoride Inorganic materials 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
- H10K2102/301—Details of OLEDs
- H10K2102/341—Short-circuit prevention
Landscapes
- Electroluminescent Light Sources (AREA)
Description
【発明の詳細な説明】
【０００１】
【発明の属する技術分野】本発明は、有機エレクトロル
ミネセンス（ＥＬ）の製造方法に関し、詳しくは、短絡
の発生を防止して信頼性を向上させた有機ＥＬ素子の製
造方法に関する。
【０００２】
【従来の技術】定電流駆動される有機ＥＬ素子では、陽
極と陰極とが短絡すると、特定の画素が発光しなくなっ
たり、短絡箇所が存在することにより素子の発光輝度が
低下したり、さらには電流のほとんどすべてが短絡部位
を流れることによって素子全体が発光しなくなったりす
る。
【０００３】
【発明が解決しようとする課題】このような短絡の発生
を防止するため、特開平１１−４０３４６号公報には、
有機ＥＬ素子を封止する気密ケース内に支燃性ガスを封
入し、この支燃性ガスにより短絡部位を酸化して絶縁化
する有機エレクトロルミネセンス表示素子が開示されて
いる。しかしこの素子によると、気密ケース内の余分な
支燃性ガスによって素子自体の劣化が促進されるおそれ
がある。
【０００４】本発明の目的は、短絡の発生を防止して素
子の信頼性を向上させ、かつ素子の劣化に及ぼす影響を
抑えた有機ＥＬ素子の製造方法を提供することにある。
【０００５】
【課題を解決するための手段】本発明の製造方法は、透
明基板上に、陽極、有機ＥＬ膜および陰極が形成された
有機ＥＬ素子で、上記有機ＥＬ膜内には上記陽極と上記
陰極との短絡を防止するための支燃性ガスが含有されて
いる有機ＥＬ素子を製造する方法であって、支燃性ガス
分圧０．５×１０−４Ｐａ〜１０×１０−４Ｐａで真空
蒸着を行うことにより上記有機ＥＬ膜を形成することを
特徴とする。
【０００６】以下、本発明につき詳細に説明する。上記
「透明基板」としては、有機ＥＬ積層体の発光による文
字、図形等の視認が損なわれない程度の透明性を有する
材質からなるものを使用することができる。また、有機
ＥＬ素子の表層としての形状を保持し得るだけの強度を
併せ有し、かつ表面が容易に傷付かない程度の硬さを有
するものが好ましい。そのような基板としては、ガラス
の他、ポリエチレンテレフタレート、ポリエーテルスル
ホン、ポリカーボネート等からなるものを使用すること
もできる。この透明基板は無色透明であってもよいし、
適宜の色調に着色された着色透明のものであってもよ
い。
【０００７】この透明基板上に、陽極、有機ＥＬ膜およ
び陰極を積層して有機ＥＬ積層膜が構成される。通常は
透明基板上に陽極を形成し、その上に有機ＥＬ膜および
陰極をこの順で積層する。両極の間に配置される「有機
ＥＬ膜」は、少なくとも発光層を備え、この発光層に加
えて正孔輸送層および／または電子輸送層を有してもよ
く、さらに正孔注入層および／または電子注入層を有し
てもよい。陽極および陰極および有機ＥＬ膜を構成する
材料としては、それぞれ種々の公知材料を用いることが
できる。これらの各層を形成する方法は、真空蒸着法、
スピンコート法、キャスト法、スパッタリング法、ＬＢ
法等の方法から適宜選択すればよい。
【０００８】上記「支燃性ガス」とは、気体酸化剤であ
って、自燃性がなく、他の物質の燃焼を助ける物質をい
う。この支燃性ガスとしては、酸素ガス、一酸化二窒素
ガス、オゾンガス、塩素ガス、一酸化窒素ガス、フッ素
ガス、三フッ化窒素ガス、二フッ化酸素ガス、三酸化フ
ッ化塩素ガス等が挙げられ、これらのうち一種のみを使
用してもよく二種以上を併用してもよい。本発明におい
ては酸素ガスを用いることが特に好ましい。
【０００９】本発明の製造方法により得られる有機ＥＬ
素子は、有機ＥＬ膜内にこの支燃性ガスを含有するもの
である。この支燃性ガスは、有機ＥＬ膜を構成する材料
に吸着されたり、有機ＥＬ膜の隙間に閉じ込められたり
して膜中に保持されている。支燃性ガスの含有量は、有
機ＥＬ膜全体の体積を１００体積％として、そのうち支
燃性ガスを０．０５〜２体積％の割合で含むものであ
り、好ましくは０．１〜１体積％とすることができる。
支燃性ガスの含有割合が少なすぎると、短絡防止の効果
が十分に発揮されない場合がある。一方、支燃性ガスの
含有割合が多すぎると、ダークスポットが発生しやすく
なり、また有機ＥＬ膜の密度が低下して素子の駆動電圧
が上昇する傾向にあるため好ましくない。なお、この支
燃性ガスは、有機ＥＬ膜を構成する上記各層の全部に含
まれてもよく、一部の層のみに含まれていてもよい。
【００１０】支燃性ガスを含有する有機ＥＬ膜を製造す
るには、支燃性ガスの存在する雰囲気下で成膜する方
法、支燃性ガスを溶解させた溶液等から有機ＥＬ膜を成
膜する方法等によればよい。このうち、支燃性ガスの存
在する雰囲気下で真空蒸着を行うことにより有機ＥＬ膜
を製造する方法が好ましく用いられる。この場合、真空
蒸着に用いる真空槽内における支燃性ガス分圧としては
０．５×１０-4Ｐａ〜１０×１０-4Ｐａの範囲が好まし
く、より好ましくは０．８×１０-4Ｐａ〜５×１０-4Ｐ
ａ、さらに好ましくは１×１０-4Ｐａ〜３×１０-4Ｐａ
である。支燃性ガス分圧が０．５×１０-4Ｐａ未満では
短絡防止の効果が十分に発揮されない場合があり、１０
×１０-4Ｐａを超えるとダークスポットが発生しやすく
なる。
【００１１】本発明の製造方法により得られる有機ＥＬ
素子は、通常は上記透明基板に接着剤等により固定され
て上記有機ＥＬ積層膜を気密に封止する封止部材を備え
る。この封止空間に充填する封止ガスとしては窒素、ア
ルゴン等の不活性ガスを使用し、支燃性ガスを実質的に
含まない（封止ガス全体に対する支燃性ガスの割合が多
くとも０．０１体積％以下）封止ガスを充填することが
好ましい。封止空間に封止部材を充填するには、封止ガ
ス雰囲気下で封止部材を透明基板に固定する等の方法に
よればよい。
【００１２】本発明の製造方法により得られる有機ＥＬ
素子は、例えば電流密度１０ｍＡ／ｃｍ２で連続駆動し
た場合において、短絡して全体が発光しなくなるまでの
時間が２００時間以上（より好ましい条件では２５０時
間以上、さらに好ましい条件では３００時間以上）のも
のとすることができる。また、温度１００℃にて５００
時間保存した後に素子を駆動した場合において、駆動初
期の非発光部（ダークエリア）の割合が面積比で１０％
以下（より好ましい条件では８％以下、さらに好ましい
条件では５％以下）のものとすることができる。なお、
用途にもよるが、通常はこの条件で保存した後に非発光
部の割合が１０％程度であれば実用上は問題とならな
い。
【００１３】
【発明の実施の形態】以下、実験例により本発明を更に
具体的に説明する。
（実験例１）下記工程（１）〜（６）により有機ＥＬ素
子を製造した。
（１）ソーダ石灰ガラスからなる透明基板上にＩＴＯか
らなる陽極を形成した。
（２）真空蒸着に用いる真空槽内を、真空度が０．３×
１０-4Ｐａ以下になるまで真空排気した。
（３）マスフローコントローラにより流量を制御しなが
ら真空槽内に酸素ガスを導入し、真空槽内の酸素ガス分
圧が２×１０-4Ｐａとなるように流量を調整した。この
とき、真空槽内の気体組成は実質的に酸素ガス１００体
積％であった。
（４）この雰囲気下で、陽極の形成された透明基板上
に、正孔注入層としての銅フタロシアニン３０ｎｍ、正
孔輸送層としてのＮ，Ｎ’−ビス（４−ジフェニルアミ
ノ−４−バイフェニル）−Ｎ，Ｎ’−ジフェニルベンジ
ジン（トリフェニルアミンの４量体）３０ｎｍ、発光層
および電子輸送層としてのアルミキノリウム錯体６０ｎ
ｍを順次成膜した。
（５）酸素導入を止め、槽内の真空度を１×１０-4Ｐａ
以下とした後に、電子注入層としてのＬｉＦ０．５ｎｍ
および陰極としてのアルミニウム１５０ｎｍを成膜し
た。
（６）その後、大気に曝すことなく素子を窒素ガスで封
止した。この封止は、窒素ガス雰囲気中においてＳＵＳ
製の封止部材を、エポキシ系の紫外線硬化型接着剤を用
いて透明基板に接着することにより行った。
【００１４】（実験例２、３）上記工程（２）〜（４）
における酸素ガス分圧を、実験例２では１×１０-4Ｐ
ａ、実験例３では３×１０-4Ｐａとし、その他の点につ
いては実験例１と同様にして有機ＥＬ素子を製造した。
【００１５】（実験例４）上記工程（２）〜（４）にお
いて酸素ガスを導入せず、真空度を０．３×１０ -4Ｐａ
（酸素ガス分圧０．０６×１０-4Ｐａ）とし、その他の
点については実験例１と同様にして有機ＥＬ素子を製造
した。
【００１６】（性能評価）実験例１〜４により得られた
有機ＥＬ素子につき、下記の性能評価を行った。その結
果を表１に示す。
ショート発生時間：電流密度１０ｍＡ／ｃｍ2で有機
ＥＬ素子を連続駆動し、短絡が発生して素子全体が発光
しなくなるまでの時間を測定した。
非発光部の割合：有機ＥＬ素子を１００℃にて５００
時間保存した後に素子を駆動し、駆動初期における非発
光部（ダークエリア）の面積比を測定した。
【００１７】
【表１】
【００１８】表１から判るように、酸素ガス分圧１×１
０-4Ｐａ〜３×１０-4Ｐａの真空蒸着により有機ＥＬ膜
を形成した実験例１〜３の有機ＥＬ素子は、いずれも３
００時間以上の連続駆動によっても短絡が起こらなかっ
た。また、１００℃の高温で５００時間保存した後の非
発光部の面積は全体に対して５％以下であり、実用上は
問題のないレベルであった。一方、真空蒸着時の酸素ガ
ス分圧が０．０６×１０-4Ｐａである実験例４の有機Ｅ
Ｌ素子は、駆動開始から１２０時間後に短絡して全体が
発光しなくなった。
【００１９】
【発明の効果】有機ＥＬ素子の電極間には、電極製造時
に生じた微細な突起、電極や有機ＥＬ膜の膜厚のバラツ
キ、製造時に混入した異物等による低抵抗部分（他の部
分に比べて電流の流れやすい箇所）が存在することがあ
り、この低抵抗部分が短絡を引き起こしやすい。有機Ｅ
Ｌ膜中に支燃性ガスを含有させた本発明の有機ＥＬ素子
によると、このような低抵抗部分は電流集中のため他の
部分よりも高温となることを利用して、この低抵抗部分
に支燃性ガスを反応させ、低抵抗部分の電極および／ま
たは有機ＥＬ膜の材料を酸化して絶縁体とすることによ
り、素子の短絡を防止することができる。これにより、
有機ＥＬ素子の信頼性が向上する。
【００２０】本発明の製造方法により得られる有機ＥＬ
素子は、封止空間ではなく有機ＥＬ層内に支燃性ガスを
含有するので、この支燃性ガスが低抵抗部分に効率よく
供給され、少量の支燃性ガスによって十分な短絡防止効
果を発揮することができる。このため、過剰の支燃性ガ
スによる素子の劣化は最小限に抑えられる。本発明の製
造方法によると、真空蒸着時の支燃性ガス濃度をコント
ロールするという簡単な方法により、短絡防止に適当な
量の支燃性ガスを含有する有機ＥＬ膜を備えた上記有機
ＥＬ素子を得ることができる。DETAILED DESCRIPTION OF THE INVENTION
[0001]
TECHNICAL FIELD The present invention relates to an organic electroluminescent device.
For details on the manufacturing method of luminescence (EL),
Of organic EL devices with improved reliability by preventing
Construction method.
[0002]
2. Description of the Related Art In an organic EL device driven by a constant current, a positive
Certain pixels do not emit light when the pole and cathode are shorted
Or the presence of a short-circuited part,
Drop or even almost all of the current
The entire device stops emitting light
You.
[0003]
The occurrence of such a short circuit
In order to prevent this, JP-A-11-40346 discloses that
Oxidizing gas is sealed in an airtight case that seals the organic EL element.
And oxidize the short-circuited area with this supporting gas to make it insulated.
Organic electroluminescent display device is disclosed
I have. However, according to this element, extra
Deterioration of element itself may be accelerated by supporting gas
There is.
An object of the present invention is to prevent occurrence of a short circuit and
To improve the reliability of the element
An object of the present invention is to provide a method for manufacturing an organic EL element in which the organic EL element is suppressed.
[0005]
According to the present invention, there is provided a manufacturing method comprising:
An anode, an organic EL film, and a cathode were formed on a light substrate.
In the organic EL device, the anode and the anode are provided in the organic EL film.
Contains combustible gas to prevent short circuit with cathode
A method for manufacturing an organic EL device, comprising:
Partial pressure 0.5 × 10-4Pa-10 × 10-4Va at Pa
Forming the organic EL film by performing vapor deposition;
Features.
Hereinafter, the present invention will be described in detail. the above
The term “transparent substrate” refers to a statement based on light emission of the organic EL laminate.
Transparency that does not impair the visibility of characters and figures
A material made of a material can be used. Also organic
Strength that can maintain the shape as the surface layer of the EL element
It also has a hardness that does not damage the surface easily.
Are preferred. Such substrates include glass
In addition, polyethylene terephthalate, polyether sulf
Phone, polycarbonate, etc.
You can also. This transparent substrate may be colorless and transparent,
It may be colored and transparent with an appropriate color.
No.
On this transparent substrate, an anode, an organic EL film and
And the cathode are laminated to form an organic EL laminated film. Normally
An anode is formed on a transparent substrate, and an organic EL film and
The cathodes are stacked in this order. "Organic" located between the two poles
The “EL film” includes at least a light emitting layer, and is added to the light emitting layer.
May have a hole transport layer and / or an electron transport layer.
And further has a hole injection layer and / or an electron injection layer.
You may. Construct anode and cathode and organic EL film
Various known materials can be used for each material.
it can. The method of forming each of these layers is a vacuum evaporation method,
Spin coating, casting, sputtering, LB
The method may be appropriately selected from methods such as a method.
[0008] The above-mentioned "combustible gas" is a gas oxidizing agent.
Are substances that are not self-combustible and help burn other substances.
U. The supporting gas includes oxygen gas and nitrous oxide.
Gas, ozone gas, chlorine gas, nitric oxide gas, fluorine
Gas, nitrogen trifluoride gas, oxygen difluoride gas,
Chloride gas, etc., of which only one type is used.
Or two or more of them may be used in combination. In the present invention
It is particularly preferable to use oxygen gas.
[0009] The present inventionObtained by manufacturing methodOrganic EL
The element contains this combustion supporting gas in the organic EL film
It is. This supporting gas is a material constituting the organic EL film.
Or is trapped in the gap of the organic EL film
And is held in the membrane. The content of supporting gas is
Assuming that the volume of the entire EL film is 100% by volume,
Containing flammable gas at a rate of 0.05 to 2% by volume
And preferably 0.1 to 1% by volume.
If the content of the supporting gas is too low, the effect of preventing short circuit
May not be fully exhibited. On the other hand,
If the content is too high, dark spots are likely to occur.
And the density of the organic EL film is reduced, and the driving voltage of the device is reduced.
Is unfavorable because it tends to increase. This support
The flammable gas is contained in all of the above layers constituting the organic EL film.
It may be rare or may be included in only some of the layers.
[0010] An organic EL film containing a supporting gas is manufactured.
To form a film in an atmosphere where a supporting gas exists.
Organic EL film is formed from a solution in which a supporting gas is dissolved, etc.
A method for forming a film may be used. Of these, the presence of supporting gas
Organic EL film by performing vacuum deposition in an existing atmosphere
Is preferably used. In this case, vacuum
The partial pressure of the supporting gas in the vacuum chamber used for vapor deposition
0.5 × 10-FourPa-10 × 10-FourPa range is preferred
And more preferably 0.8 × 10-FourPa-5 × 10-FourP
a, more preferably 1 × 10-FourPa ~ 3 × 10-FourPa
It is. The supporting gas partial pressure is 0.5 × 10-FourBelow Pa
In some cases, the effect of short circuit prevention may not be sufficiently exhibited.
× 10-FourIf it exceeds Pa, dark spots are likely to occur
Become.
[0011] The present inventionObtained by manufacturing methodOrganic EL
The element is usually fixed to the transparent substrate with an adhesive or the like.
A sealing member for hermetically sealing the organic EL laminated film
You. Nitrogen and air are used as the sealing gas to fill the sealing space.
Uses inert gas such as rugon to substantially reduce the supporting gas.
Not included (a large proportion of the supporting gas to the entire sealing gas
At least 0.01% by volume) Filling with sealing gas
preferable. To fill the sealing space with the sealing member,
Such as fixing the sealing member to a transparent substrate in a gas atmosphere
I'll do it.
The present inventionObtained by manufacturing methodOrganic EL
The element has a current density of, for example, 10 mA / cm.2Drive continuously
In the event that the
200 hours or more (250 hours under more preferable conditions)
For more than 300 hours under more preferable conditions)
And can be. In addition, 500
When the device is driven after storing for a
Of non-light emitting part (dark area) in the period is 10% by area ratio
Or less (8% or less under more preferred conditions, even more preferred
(5% or less under the condition). In addition,
Depending on the application, it usually emits no light after storage under these conditions
If the ratio of parts is about 10%, there is no practical problem.
No.
[0013]
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be further described by experimental examples.
This will be specifically described.
(Experimental example 1) Organic EL devices were prepared by the following steps (1) to (6).
The child was manufactured.
(1) ITO on a transparent substrate made of soda-lime glass
A positive anode was formed.
(2) The inside of the vacuum chamber used for vacuum deposition has a degree of vacuum of 0.3 ×
10-FourEvacuation was performed until the pressure became Pa or less.
(3) While controlling the flow rate with the mass flow controller
Oxygen gas is introduced into the vacuum chamber from the
Pressure is 2 × 10-FourThe flow rate was adjusted to Pa. this
When the gas composition in the vacuum chamber is substantially 100 oxygen gas
%.
(4) Under this atmosphere, on a transparent substrate on which an anode is formed
First, copper phthalocyanine as a hole injection layer having a thickness of 30 nm was used.
N, N'-bis (4-diphenylamido as a hole transport layer
No-4-biphenyl) -N, N'-diphenylbenzyl
Gin (triphenylamine tetramer) 30 nm, light emitting layer
And aluminum quinolium complex 60n as electron transport layer
m were sequentially formed.
(5) Oxygen introduction is stopped, and the degree of vacuum in the tank is reduced to 1 × 10-FourPa
After the following, LiF 0.5 nm as an electron injection layer
And a 150 nm aluminum film as the cathode
Was.
(6) After that, the element is sealed with nitrogen gas without being exposed to the atmosphere.
Stopped. This sealing is performed in a nitrogen gas atmosphere under SUS.
Sealing member made of epoxy-based UV-curable adhesive
And bonded to a transparent substrate.
(Experimental Examples 2, 3) The above steps (2) to (4)
The oxygen gas partial pressure at-FourP
a, 3 × 10 in Experimental Example 3-FourPa and other points
Then, an organic EL device was manufactured in the same manner as in Experimental Example 1.
(Experimental Example 4) In the above steps (2) to (4),
Without introducing oxygen gas, and reducing the degree of vacuum to 0.3 × 10 -FourPa
(Oxygen gas partial pressure 0.06 × 10-FourPa) and other
An organic EL device was manufactured in the same manner as in Experimental Example 1 with regard to the points.
did.
(Performance Evaluation) Obtained by Experimental Examples 1-4
The following performance evaluation was performed on the organic EL device. The result
The results are shown in Table 1.
Short-circuit occurrence time: current density 10 mA / cmTwoOrganic
Continuous driving of the EL element, short circuit occurs and the entire element emits light
The time until no longer occurs was measured.
Ratio of non-light-emitting portion: 500 at 100 ° C. for organic EL element
After the device has been stored for a period of time, the device is
The area ratio of the light part (dark area) was measured.
[0017]
[Table 1]
As can be seen from Table 1, the oxygen gas partial pressure 1 × 1
0-FourPa ~ 3 × 10-FourOrganic EL film by vacuum deposition of Pa
The organic EL devices of Experimental Examples 1 to 3 in which
No short circuit even with continuous driving for more than 00 hours
Was. In addition, after storage for 500 hours at a high temperature of 100 ° C.,
The area of the light emitting part is 5% or less of the whole,
There was no problem. On the other hand, oxygen
The partial pressure is 0.06 × 10-FourOrganic E of Experimental Example 4 with Pa
The L element is short-circuited 120 hours after the start of driving, and
It no longer emits light.
[0019]
According to the present invention, an electrode is provided between the electrodes of the organic EL element when the electrodes are manufactured.
Variations in the thickness of electrodes, organic EL films, and fine protrusions
G, low resistance parts (other parts)
Parts where current flows more easily than minutes).
In addition, the low resistance portion easily causes a short circuit. Organic E
Organic EL device of the present invention containing a flammable gas in the L film
According to these low resistance parts, other
Utilizing the fact that it becomes hotter than the part, this low resistance part
Reacts a supporting gas with the electrode and / or
Or by oxidizing the material of the organic EL film into an insulator.
Thus, short circuit of the element can be prevented. This allows
The reliability of the organic EL element is improved.
The present inventionObtained by manufacturing methodOrganic EL
The device uses a supporting gas in the organic EL layer instead of the sealed space.
Contains, this combustible gas efficiently
Sufficient short-circuit prevention effect provided by a small amount of supporting gas
Fruit can be demonstrated. As a result, excessive
Deterioration of the element due to heat is minimized. Of the present invention
According to the manufacturing method, the concentration of the supporting gas during vacuum deposition is controlled.
Easy to roll, suitable for short circuit prevention
With an organic EL film containing an amount of flammable gasthe aboveOrganic
An EL element can be obtained.
フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) H05B 33/14 H05B 33/10 H05B 33/26 Continuation of the front page (58) Field surveyed (Int.Cl. 7 , DB name) H05B 33/14 H05B 33/10 H05B 33/26
Claims (1)
陰極が形成された有機ＥＬ素子で、上記有機ＥＬ膜内に
は上記陽極と上記陰極との短絡を防止するための支燃性
ガスが含有されている有機ＥＬ素子の製造方法であっ
て、 支燃性ガス分圧０．５×１０ −４ Ｐａ〜１０×１０ −４
Ｐａで真空蒸着を行うことにより上記有機ＥＬ膜を形成
することを特徴とする有機ＥＬ素子の製造方法 。(57) Claims 1. An organic EL device having an anode, an organic EL film, and a cathode formed on a transparent substrate, wherein the anode and the cathode are short-circuited in the organic EL film. A method for manufacturing an organic EL device containing a flammable gas for preventing
And the partial pressure of the supporting gas 0.5 × 10 −4 Pa to 10 × 10 −4
The above organic EL film is formed by performing vacuum deposition with Pa
A method for manufacturing an organic EL device, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000103991A JP3509693B2 (en) | 2000-04-05 | 2000-04-05 | Manufacturing method of organic EL device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000103991A JP3509693B2 (en) | 2000-04-05 | 2000-04-05 | Manufacturing method of organic EL device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001291582A JP2001291582A (en) | 2001-10-19 |
| JP3509693B2 true JP3509693B2 (en) | 2004-03-22 |
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ID=18617611
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|---|---|---|---|
| JP2000103991A Expired - Fee Related JP3509693B2 (en) | 2000-04-05 | 2000-04-05 | Manufacturing method of organic EL device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004054325A1 (en) * | 2002-12-12 | 2004-06-24 | Semiconductor Energy Laboratory Co., Ltd. | Light-emitting device, manufacturing apparatus, film-forming method, and cleaning method |
| JP4538304B2 (en) * | 2004-12-02 | 2010-09-08 | パイオニア株式会社 | Organic electroluminescence display panel and manufacturing method thereof |
| JP5270385B2 (en) * | 2009-01-19 | 2013-08-21 | 日本特殊陶業株式会社 | Solid electrolyte fuel cell |
| JP2011081966A (en) * | 2009-10-05 | 2011-04-21 | Toshiba Mobile Display Co Ltd | Organic el device and method of manufacturing the same |
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|---|---|
| JP2001291582A (en) | 2001-10-19 |
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