JP2000077183A - Manufacture of organic electroluminescent element - Google Patents
Manufacture of organic electroluminescent elementInfo
- Publication number
- JP2000077183A JP2000077183A JP10244601A JP24460198A JP2000077183A JP 2000077183 A JP2000077183 A JP 2000077183A JP 10244601 A JP10244601 A JP 10244601A JP 24460198 A JP24460198 A JP 24460198A JP 2000077183 A JP2000077183 A JP 2000077183A
- Authority
- JP
- Japan
- Prior art keywords
- multilayer structure
- gas
- sealing film
- plasma cvd
- cvd method
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000007789 gas Substances 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 5
- 229910000077 silane Inorganic materials 0.000 claims abstract description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 3
- 238000005401 electroluminescence Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 abstract description 9
- 239000007924 injection Substances 0.000 abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- -1 aluminum chelate complex Chemical class 0.000 abstract description 2
- 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 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910004205 SiNX Inorganic materials 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 125000006617 triphenylamine group Chemical group 0.000 abstract 1
- 239000010408 film Substances 0.000 description 26
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000005525 hole transport Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910007991 Si-N Inorganic materials 0.000 description 2
- 229910006294 Si—N Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical class C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
Landscapes
- Electroluminescent Light Sources (AREA)
Abstract
Description
【０００１】[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（以下、ＥＬと称す）素子の製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing an organic electroluminescence (hereinafter, referred to as EL) device.
【０００２】[0002]
【従来の技術】図１に示すように、有機ＥＬ素子は、ガ
ラス基板１上に陽極２を形成し、その上に有機化合物か
らなる正孔注入層３、正孔輸送層４、発光層５、電子注
入層６を順次積層し、その上に金属材料からなる陰極７
を形成した多層構造体８からなっている。多層構造体８
は大気に曝されると劣化することがあり、発光ムラが生
じる原因となる。特に、陰極７は、電子注入層６に電子
を送るために仕事関数の低い材料、例えば、アルカリ金
属やアルカリ土類金属を基本とした反応性の高い合金系
によって形成されており、劣化しやすい。また、有機化
合物も酸素によって劣化しやすい。そこで、多層構造体
８はガラス基板１の上において封止被膜９で大気から遮
断されている。この封止被膜９にスパッタリング法やプ
ラズマＣＶＤ法の如き薄膜形成法を用いることによっ
て、厚さの薄いコンパクトな有機ＥＬ素子を得ることが
できる。2. Description of the Related Art As shown in FIG. 1, an organic EL device has an anode 2 formed on a glass substrate 1 and a hole injection layer 3, a hole transport layer 4, and a light emitting layer 5 made of an organic compound formed thereon. , An electron injection layer 6 are sequentially laminated, and a cathode 7 made of a metal material is formed thereon.
Is formed of the multilayer structure 8. Multilayer structure 8
May degrade when exposed to the atmosphere, which may cause uneven light emission. In particular, the cathode 7 is formed of a material having a low work function to send electrons to the electron injection layer 6, for example, a highly reactive alloy system based on an alkali metal or an alkaline earth metal, and is easily deteriorated. . Further, organic compounds are also easily deteriorated by oxygen. Therefore, the multilayer structure 8 is shielded from the atmosphere by the sealing film 9 on the glass substrate 1. By using a thin film forming method such as a sputtering method or a plasma CVD method for the sealing film 9, a compact organic EL element having a small thickness can be obtained.
【０００３】プラズマＣＶＤ法によって得られる被膜
は、スパッタリング法によって得られる被膜と比較して
結晶構造が緻密であり、機密性に優れ、多層構造体８を
大気から遮断するための被膜として適している。また、
スパッタリング法や、他のＣＶＤ法と比べて低温での成
膜が可能であり、基板１若しくは多層構造体８が熱によ
って損傷することを回避できる。The film obtained by the plasma CVD method has a denser crystal structure and excellent confidentiality than the film obtained by the sputtering method, and is suitable as a film for shielding the multilayer structure 8 from the atmosphere. . Also,
Film formation can be performed at a lower temperature than a sputtering method or another CVD method, and damage to the substrate 1 or the multilayer structure 8 due to heat can be avoided.
【０００４】[0004]
【発明が解決しようとする課題】プラズマＣＶＤ法によ
って得られる被膜は、その緻密な結晶構造の故に、被膜
の平面方向に高い残留応力が発生する。この残留応力
は、封止被膜９の下の多層構造体８や基板１に作用し
て、これを変形させてしまうことがある。また、皮膜自
体の剥離によって、大気と多層構造体８が接触して素子
が劣化してしまう。そこで本発明は、素子の多層構造体
を長期に亘って気密状態に維持できる封止被膜を有する
有機ＥＬ素子の製造方法の提供を目的とする。The coating obtained by the plasma CVD method has a high residual stress in the plane direction of the coating due to its dense crystal structure. This residual stress may act on the multilayer structure 8 and the substrate 1 under the sealing film 9 to deform the same. In addition, the peeling of the film itself causes the multilayer structure 8 to come into contact with the atmosphere, thereby deteriorating the element. Accordingly, an object of the present invention is to provide a method for manufacturing an organic EL device having a sealing film capable of maintaining a multilayer structure of the device in an airtight state for a long period of time.
【０００５】[0005]
【課題を解決するための手段】本発明による有機ＥＬ素
子の製造方法は、ガラス基板の上に、少なくとも陽極
と、複数の有機化合物層と、陰極と、を順に積層して多
層構造体を形成し、さらに前記多層構造体を気密的に封
止する封止被膜をプラズマＣＶＤ法によって成膜する有
機ＥＬ素子の製造方法であって、前記プラズマＣＶＤ法
による原料ガスが、シランガスと、窒素ガスと、のみか
らなることを特徴とする。According to a method of manufacturing an organic EL device according to the present invention, a multilayer structure is formed by sequentially laminating at least an anode, a plurality of organic compound layers, and a cathode on a glass substrate. And a method of manufacturing an organic EL device in which a sealing film for hermetically sealing the multilayer structure is formed by a plasma CVD method, wherein the source gas by the plasma CVD method is a silane gas, a nitrogen gas, , Only.
【０００６】[0006]
【発明の実施の形態】以下、本発明による有機ＥＬ素子
の製造方法について詳細に説明する。図１に示した従来
例の多層構造体と同様に、透明なガラス基板１上に透光
性のＩＴＯからなる陽極２を図示しない電極パターンを
形成するように蒸着する。その上に、銅フタロシアニン
からなる正孔注入層３、ＴＰＤ（トリフェニルアミン誘
導体）からなる正孔輸送層４、Ａｌｑ3（アルミキレー
ト錯体）からなる発光層５、ＬｉＯ2（二酸化リチウ
ム）からなる電子注入層６を順次、蒸着する。さらに、
この上に蒸着によって、Ａｌからなる陰極７を陽極２の
電極パターンと対向するようにパターニングする。こう
して得られたガラス基板１上の多層構造体８を、大気に
曝すことなく、プラズマＣＶＤのチャンバ内に移送、配
置して、ＳｉＮx（窒化ケイ素）からなる封止被膜９を
その表面に成膜する。このとき、予めガラス基板１の多
層構造体８を形成した面と反対側の表面がマスキングさ
れていることが好ましい。本実施例においては、プラズ
マＣＶＤ法に用いる原料ガスとして、ＳｉＨ4（シラ
ン）ガス及びＮ2（窒素）ガスのみを用い、各々の流量
を10 sccm及び200 sccmとし、RFパワーを10 W、チャン
バ内温度を120℃、チャンバ内圧力を0.9 Torrとした。
得られた膜厚は約2μmであった。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a method for manufacturing an organic EL device according to the present invention will be described in detail. As in the case of the conventional multilayer structure shown in FIG. 1, an anode 2 made of a transparent ITO is deposited on a transparent glass substrate 1 so as to form an electrode pattern (not shown). On top of this, a hole injection layer 3 made of copper phthalocyanine, a hole transport layer 4 made of TPD (triphenylamine derivative), a light emitting layer 5 made of Alq 3 (aluminum chelate complex), and LiO 2 (lithium dioxide). The electron injection layer 6 is sequentially deposited. further,
On this, a cathode 7 made of Al is patterned by vapor deposition so as to face the electrode pattern of the anode 2. The multilayer structure 8 thus obtained on the glass substrate 1 is transferred and arranged in a plasma CVD chamber without exposing it to the atmosphere, and a sealing film 9 made of SiN x (silicon nitride) is formed on the surface thereof. Film. At this time, it is preferable that the surface of the glass substrate 1 opposite to the surface on which the multilayer structure 8 is formed be masked in advance. In this embodiment, only SiH 4 (silane) gas and N 2 (nitrogen) gas are used as source gases used in the plasma CVD method, the flow rates are respectively 10 sccm and 200 sccm, the RF power is 10 W, and the chamber power is 10 W. The internal temperature was 120 ° C. and the pressure in the chamber was 0.9 Torr.
The resulting film thickness was about 2 μm.
【０００７】上記した実施例において得られたＥＬ素子
の封止被膜の被膜平面方向の残留応力を測定したとこ
ろ、成膜直後で0.05dyn/cm2、充分に時間を経過した後
にあっても-0.21dyn/cm2と小さいものであった。ただ
し、正の値を圧縮応力、負の値を引っ張り応力とする。
このＥＬ素子を、それぞれ室温及び高温高湿（60℃、95
％）下に500時間放置した後であっても、封止被膜にク
ラックや剥離を発生せず、ＥＬ素子としての発光動作も
安定していた。The residual stress in the plane direction of the sealing film of the EL element obtained in the above-described embodiment was measured. It was 0.05 dyn / cm 2 immediately after the film formation, even after a sufficient time had passed. It was as small as 0.21 dyn / cm 2 . However, a positive value is a compressive stress, and a negative value is a tensile stress.
The EL element was subjected to room temperature, high temperature and high humidity (60 ° C, 95
%), The sealing film did not crack or peel off even after standing for 500 hours, and the light emitting operation as an EL element was stable.
【０００８】次に、比較例として、原料ガスとして、Ｓ
ｉＨ4ガス及びＮ2ガスにアンモニアを加えた例を検討し
た。つまり成膜条件は、原料ガスとしてのＳｉＨ4ガス
の流量を30 sccm、Ｎ2ガスの流量を140 sccm、ＮＨ3ガ
スの流量を200 sccm、H2ガスの流量を30 sccmとし、RF
パワーを10 W、チャンバ内温度を120℃、チャンバ内圧
力を0.9 Torrとした。得られた膜厚は約2μmであった。
比較例のＥＬ素子の封止被膜の残留応力については、成
膜直後で-0.49dyn/cm2、充分に時間を経過した後にあっ
ては-0.68dyn/cm2であり、実施例と比較して大きな引っ
張りの残留応力を有していた。このＥＬ素子をそれぞれ
室温及び高温高湿（60℃、95％）下で500時間放置した
ところ、室温では変化を示さなかったが、高温高湿下で
は剥離を発生した。剥離を発生したＥＬ素子は、輝度に
ムラを生じて発光動作が不安定になった。Next, as a comparative example, S was used as a raw material gas.
An example in which ammonia was added to iH 4 gas and N 2 gas was examined. That is, the film forming conditions are as follows: the flow rate of the SiH 4 gas as the source gas is 30 sccm, the flow rate of the N 2 gas is 140 sccm, the flow rate of the NH 3 gas is 200 sccm, the flow rate of the H 2 gas is 30 sccm, and the RF
The power was 10 W, the temperature in the chamber was 120 ° C., and the pressure in the chamber was 0.9 Torr. The resulting film thickness was about 2 μm.
Residual stress of the sealing film of the EL device of the comparative example, -0.49dyn / cm 2 immediately after the film formation, in the after a lapse of sufficient time was -0.68dyn / cm 2, compared to Example And had a large tensile residual stress. When this EL element was left for 500 hours at room temperature and high temperature and high humidity (60 ° C., 95%), no change was observed at room temperature, but peeling occurred under high temperature and high humidity. The EL element in which peeling occurred had uneven brightness and the light emitting operation became unstable.
【０００９】FT-IR分析によって、実施例及び比較例に
おける封止被膜の成分を成膜直後及び５００時間経過後
において調べた。比較例では、成膜直後にＮ−Ｈ結合、
Ｓｉ−Ｎ結合、Ｓｉ−Ｈ結合の特性ピークが観察され
て、その存在が確認されたが、５００時間経過後にはＮ
−Ｈ結合の特性ピークが不明瞭となり、Ｎ−Ｈ結合が消
滅していた。実施例では、成膜直後にＳｉ−Ｎ結合、Ｓ
ｉ−Ｈ結合の特性ピークが確認されたが、５００時間経
過後においても特性ピークに変化がなかった。このこと
から、Ｎ−Ｈ結合の経時変化が残留応力を増大させてク
ラックの発生及び被膜の剥離を引き起こすと考えられ
る。The components of the sealing film in Examples and Comparative Examples were examined by FT-IR analysis immediately after film formation and after 500 hours. In the comparative example, N—H bonding was performed immediately after film formation,
Characteristic peaks of Si—N bond and Si—H bond were observed and their existence was confirmed, but after 500 hours, N
The characteristic peak of the -H bond became unclear, and the N-H bond had disappeared. In the embodiment, the Si—N bond, S
Although the characteristic peak of the iH bond was confirmed, the characteristic peak did not change even after 500 hours. From this, it is considered that the temporal change of the NH bond increases the residual stress, causing cracks and peeling of the film.
【００１０】[0010]
【発明の効果】以上の如く、本発明による有機ＥＬ素子
の製造方法によれば、残留応力の少ない安定した封止被
膜を有する有機ＥＬ素子を得ることができる。As described above, according to the method for manufacturing an organic EL device according to the present invention, an organic EL device having a stable sealing film with little residual stress can be obtained.
【図１】 有機ＥＬ素子の断面図である。FIG. 1 is a sectional view of an organic EL device.
１ ガラス基板 ２ 陽極 ３ 正孔注入層 ４ 正孔輸送層 ５ 発光層 ６ 電子注入層 ７ 陰極 ８ 多層構造体 ９ 封止被膜 DESCRIPTION OF SYMBOLS 1 Glass substrate 2 Anode 3 Hole injection layer 4 Hole transport layer 5 Light emitting layer 6 Electron injection layer 7 Cathode 8 Multilayer structure 9 Sealing film
Claims (1)
複数の有機化合物層と、陰極と、を順に積層して多層構
造体を形成し、さらに前記多層構造体を気密的に封止す
る封止被膜をプラズマＣＶＤ法によって成膜する有機エ
レクトロルミネセンス素子の製造方法であって、 前記プラズマＣＶＤ法による原料ガスが、シランガス
と、窒素ガスと、のみからなることを特徴とする有機エ
レクトロルミネセンス素子の製造方法。1. At least an anode on a glass substrate,
An organic electroluminescent device in which a plurality of organic compound layers and a cathode are sequentially laminated to form a multilayer structure, and further, a sealing film for hermetically sealing the multilayer structure is formed by a plasma CVD method. The method for producing an organic electroluminescence device according to claim 1, wherein the source gas by the plasma CVD method comprises only silane gas and nitrogen gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10244601A JP2000077183A (en) | 1998-08-31 | 1998-08-31 | Manufacture of organic electroluminescent element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10244601A JP2000077183A (en) | 1998-08-31 | 1998-08-31 | Manufacture of organic electroluminescent element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000077183A true JP2000077183A (en) | 2000-03-14 |
Family
ID=17121162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10244601A Pending JP2000077183A (en) | 1998-08-31 | 1998-08-31 | Manufacture of organic electroluminescent element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000077183A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004054010A2 (en) * | 2002-12-11 | 2004-06-24 | Applied Materials, Inc. | Low temperature process for passivation applications |
| US7247074B2 (en) * | 2001-12-03 | 2007-07-24 | Denso Corporation | Organic electroluminescent element and process for its manufacture |
| US7994707B2 (en) | 2007-08-28 | 2011-08-09 | Canon Kabushiki Kaisha | Organic el device and method of producing the device |
| CN103904234A (en) * | 2012-12-25 | 2014-07-02 | 海洋王照明科技股份有限公司 | Organic light-emitting device and preparation method |
| JP2020080232A (en) * | 2018-11-12 | 2020-05-28 | キヤノン株式会社 | Semiconductor device, manufacturing method of the same, display device, photoelectric conversion device, electronic device, lighting device, and movable body |
-
1998
- 1998-08-31 JP JP10244601A patent/JP2000077183A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7247074B2 (en) * | 2001-12-03 | 2007-07-24 | Denso Corporation | Organic electroluminescent element and process for its manufacture |
| WO2004054010A2 (en) * | 2002-12-11 | 2004-06-24 | Applied Materials, Inc. | Low temperature process for passivation applications |
| WO2004054010A3 (en) * | 2002-12-11 | 2004-11-18 | Applied Materials Inc | Low temperature process for passivation applications |
| US7086918B2 (en) | 2002-12-11 | 2006-08-08 | Applied Materials, Inc. | Low temperature process for passivation applications |
| US7994707B2 (en) | 2007-08-28 | 2011-08-09 | Canon Kabushiki Kaisha | Organic el device and method of producing the device |
| CN103904234A (en) * | 2012-12-25 | 2014-07-02 | 海洋王照明科技股份有限公司 | Organic light-emitting device and preparation method |
| JP2020080232A (en) * | 2018-11-12 | 2020-05-28 | キヤノン株式会社 | Semiconductor device, manufacturing method of the same, display device, photoelectric conversion device, electronic device, lighting device, and movable body |
| JP7170509B2 (en) | 2018-11-12 | 2022-11-14 | キヤノン株式会社 | Semiconductor device and its manufacturing method, display device, photoelectric conversion device, electronic device, lighting device, and moving body |
| US11765927B2 (en) | 2018-11-12 | 2023-09-19 | Canon Kabushiki Kaisha | Semiconductor device, method of manufacturing the same, display device, photoelectric conversion device, electronic device, illumination device, and mobile object |
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