JPH0750561B2 - Electrochemiluminescent display device and manufacturing method thereof - Google Patents
Electrochemiluminescent display device and manufacturing method thereofInfo
- Publication number
- JPH0750561B2 JPH0750561B2 JP63108405A JP10840588A JPH0750561B2 JP H0750561 B2 JPH0750561 B2 JP H0750561B2 JP 63108405 A JP63108405 A JP 63108405A JP 10840588 A JP10840588 A JP 10840588A JP H0750561 B2 JPH0750561 B2 JP H0750561B2
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- Prior art keywords
- electrode
- polymer layer
- voltage
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- composition
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Classifications
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- 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
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/135—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising mobile ions
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- Optics & Photonics (AREA)
- Liquid Crystal (AREA)
- Electroluminescent Light Sources (AREA)
Description
【発明の詳細な説明】 ［発明の目的］ （産業上の利用分野） 本発明は、電気的に誘起されて化学発光する組成物を利
用した電気化学発光表示装置及びその製造方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION Object of the Invention (Field of Industrial Application) The present invention relates to an electrochemiluminescent display device using a composition that emits chemiluminescence when electrically induced, and a manufacturing method thereof.
（従来の技術） 電気的に誘起されて化学発光する組成物を用いる電気誘
起化学発光現象は、例えばアセトニトリルのような非水
溶媒にアントラセン、グリセン、ピレン等の発光物質
と、必要に応じて四エチルアンモニウムブロマイド、過
塩素酸四エチレンアンモニウム等の電解質を溶解した溶
液に接する電極に比較的低い交番電圧を印加した場合
に、電極付近が発光する現象であり、この発光は、電極
に印加された交番電圧によって電極付近に生ずる発光物
質のアニオンとカチオンが中和する際に生ずる電気的に
誘起された状態にある発光物質分子が基底状態に戻る際
に光子が放出されて起る。このような現象を用いた表示
装置は例えば特公昭56−2958号公報等で開示されている
ように、一般に、少なくとも一部に透明部を有する容器
に溶液系の電気的に誘起されて化学発光する組成物を封
入し、この電気誘起化学発光組成物に接してセグメント
電極と対向電極とを配設して構成される。(Prior Art) The electro-induced chemiluminescence phenomenon using a composition that is electrically induced and emits chemiluminescence is known as a method in which a non-aqueous solvent such as acetonitrile is mixed with a luminescent substance such as anthracene, glycene, or pyrene, and, if necessary, four When a relatively low alternating voltage is applied to an electrode in contact with a solution in which an electrolyte such as ethylammonium bromide or tetraethyleneammonium perchlorate is dissolved, it is a phenomenon that light is emitted in the vicinity of the electrode, and this light emission is applied to the electrode. Photons are emitted when the luminescent substance molecules in an electrically induced state generated when the anions and cations of the luminescent substance generated near the electrodes are neutralized by the alternating voltage are returned to the ground state. A display device using such a phenomenon, as disclosed in Japanese Patent Publication No. 56-2958, for example, generally has a solution-based electrically induced chemiluminescence in a container having a transparent portion at least in part. The composition is encapsulated, and a segment electrode and a counter electrode are arranged in contact with the electro-induced chemiluminescent composition.
（発明が解決しようとする課題） このような溶液系の電気誘起化学発光組成物を用いた表
示装置の駆動電圧は第９図のグラフの示すように０から
10ボルトの電圧において電圧が高い程発光輝度が高くな
り、通常10ボルト程度の電圧で駆動されている。しか
し、この表示装置を広く利用するためには消費電力を低
減できるようより低い電圧で駆動されることが望まれて
いる。また、溶液系の電気誘起化学発光組成物を用いた
表示装置は電圧を印加することにより電極面に酸化・還
元といった化学反応を起こしその結果発光することか
ら、反応が遅く電極を印加した直後は輝度が低く安定性
及び速応性に劣る問題もあった。(Problems to be Solved by the Invention) As shown in the graph of FIG. 9, the driving voltage of a display device using such a solution-based electro-induced chemiluminescent composition is 0 to
At a voltage of 10 V, the higher the voltage, the higher the brightness of light emission, and the device is usually driven at a voltage of about 10 V. However, in order to widely use this display device, it is desired to be driven at a lower voltage so as to reduce power consumption. In addition, a display device using a solution-based electro-induced chemiluminescent composition causes a chemical reaction such as oxidation / reduction on the electrode surface by applying a voltage and emits light as a result, so the reaction is slow and immediately after applying the electrode. There was also a problem of low brightness and poor stability and quick response.
そこで、本発明は前記問題点に基づいて成されるもので
あり、低電圧で駆動できるとともに、応答性を速め発光
の安定性を増すことのできる電気化学発光表示装置と、
さらに製造が容易な電気化学発光表示装置の製造方法を
提供することを目的とするものである。Therefore, the present invention is made based on the above problems, and an electrochemiluminescent display device capable of being driven at a low voltage and having a quick response and an increased stability of light emission,
Another object of the present invention is to provide a method for manufacturing an electrochemiluminescent display device that is easy to manufacture.
［発明の構成］ （課題を解決するための手段） 本発明の電気化学発光表示装置は、対向配設された金属
電極と透明電極間に、ゲル状の電気的に誘起されて化学
発光する組成物から成り発光層と成る高分子層を設けた
ものである。[Structure of the Invention] (Means for Solving the Problems) The electrochemiluminescent display device of the present invention is a gel-like composition that electrically induces chemiluminescence between a metal electrode and a transparent electrode facing each other. A polymer layer, which is made of a material and serves as a light emitting layer, is provided.
また本発明の電気化学発光表示装置の製造方法は、金属
電極上に電気的に誘起されて化学発光する組成物を含む
水溶性高分子ペーストを製膜して導電性高分子層を形成
し、この高分子層の溶媒を置換した後、混合溶媒を加え
前記高分子層を膨潤させてゲル状に形成し、前記高分子
層上に透明電極を配設したものである。Further, the method for manufacturing an electrochemiluminescent display device of the present invention, a conductive polymer layer is formed by forming a water-soluble polymer paste containing a composition that is chemically induced by being electrically induced on a metal electrode. After replacing the solvent of the polymer layer, a mixed solvent is added to swell the polymer layer to form a gel, and a transparent electrode is arranged on the polymer layer.
（作用） 金属電極と透明電極間に直流電圧を印加することにより
ゲル状の発光層が発光し、この発光は溶液系のものより
も低電圧で行われ、かつ発光の安定性も良好である。(Function) When a DC voltage is applied between the metal electrode and the transparent electrode, the gel-like light emitting layer emits light, and this light emission is performed at a lower voltage than that of the solution type, and the stability of light emission is also good. .
また、電気的に誘起されて化学発光する組成物を含む水
溶性高分子ペーストを製膜して導電性高分子層を形成
し、この高分子層の溶媒を置換した後、混合溶媒を加え
前記高分子層を膨潤させてゲル状に形成するため、前記
組成物を気密空間に封入する必要がなくなり、製造が容
易となる。Further, a water-soluble polymer paste containing a composition that is electrically induced to chemiluminesce is formed into a conductive polymer layer, the solvent of the polymer layer is replaced, and then a mixed solvent is added to the above. Since the polymer layer is swollen to form a gel, it is not necessary to enclose the composition in an airtight space, which facilitates production.
（実施例） 以下、図面の基づいて本発明の一実施例を詳述する。第
１図は断面図、第２図は製造工程のフローチャートを示
しており、先ず、A1（アルミニウム）シート電極（金属
電極）１上に、Ru（ルテニウム）錯体の水溶液とパーフ
ルオリネーテドイオンエクスチェンジパウダー5wt％溶
液（Aldrich）を混合し5mM−Ru(bpy)3 2+／ナフィオン溶
液を調整し、混合溶液を例えばキャスト法により製膜す
ることにより発光層２を形成する。(Example) Hereinafter, one example of the present invention will be described in detail with reference to the drawings. FIG. 1 is a sectional view, and FIG. 2 is a flow chart of the manufacturing process. First, on a A1 (aluminum) sheet electrode (metal electrode) 1, an aqueous solution of Ru (ruthenium) complex and perfluorinated ion exchange. A 5 wt% powder solution (Aldrich) is mixed to prepare a 5 mM-Ru (bpy) 3 2+ / Nafion solution, and the mixed solution is formed into a film by, for example, a casting method to form the light emitting layer 2.
次に、この発光層２を形成したAlシート電極１上に、Li
Cl（塩化リチウム）を溶かした水溶性ナイロン（AQ−ナ
イロン、東レ製）ペースト（水溶性高分子ペースト）を
例えばキャスト法により製膜することにより導電性ナイ
ロン層（導電性高分子層）３を形成する。Next, on the Al sheet electrode 1 on which this light emitting layer 2 is formed, Li
A conductive nylon layer (conductive polymer layer) 3 is formed by casting a water-soluble nylon (AQ-nylon, manufactured by Toray) paste (water-soluble polymer paste) in which Cl (lithium chloride) is dissolved, for example, by a casting method. Form.
次に、このナイロン層３の溶媒を置換するために、これ
を真空乾燥し、テトラ−Ｎ−ブチルアンモニウムパーク
ロレート（TBAP）を含む混合溶媒（炭酸プロピレン：
水:N,N′−ジメチルアセトアミド＝5:3:2）でナイロン
層３を膨潤させてゲル状の固体系にする。Next, in order to replace the solvent of the nylon layer 3, this is dried under vacuum and a mixed solvent containing tetra-N-butylammonium perchlorate (TBAP) (propylene carbonate:
The nylon layer 3 is swollen with water: N, N'-dimethylacetamide = 5: 3: 2) to form a gel-like solid system.
最後に、このゲル状のナイロン層３は粘着力が有るた
め、透明なITO電極（透明電極）４を蒸着したガラス５
をこのナイロン層３に貼合わせて、ナフィオン修飾電極
のECL（Electro Chemical Luminescence）セル６が構成
される。尚、ナイロン層３の伝導度を上げるために、Li
ClとTBAPの二種類の支持電解質を用いているが、この理
由は、LiClのナイロン水溶液への溶解度があまり大きく
なく、LiClのみでは充分な発光が得られないためと、Li
Clが存在しないでTBAPのみの場合にはかなり溶媒に富ん
だ状態にしなければならないためであり、両者を組み合
わせて用いることにより、発光輝度及び安定性が向上す
る。Finally, since this gel-like nylon layer 3 has an adhesive force, a glass 5 on which a transparent ITO electrode (transparent electrode) 4 is vapor-deposited
Is bonded to this nylon layer 3 to form an ECL (Electro Chemical Luminescence) cell 6 of a Nafion modified electrode. In order to increase the conductivity of the nylon layer 3, Li
Two types of supporting electrolytes, Cl and TBAP, are used, because the solubility of LiCl in the nylon aqueous solution is not so large and sufficient light emission cannot be obtained with LiCl alone.
This is because when TBAP alone is used without Cl, the solvent must be in a state rich in solvent, and the combined use of both improves emission brightness and stability.
このように構成される本発明は、Alシート電極１に負、
ITO電極４に正の直流電圧Ｅを印加することにより、ECL
発光が得られる。第３図はその発光スペクトルを示して
いる。尚、印加電圧は3.5ボルトである。ここで実線で
示すECL発光は波線で示す450nmの光で誘起した蛍光スペ
クトルと一致しており、このことからECL発光は電気化
学的に生じた２価のRu錯体の誘起状態からの発光と考え
られる。また、この発光スペクトルは従来の溶液系のEC
Lで得られたスペクトルとも一致するため、本発明は溶
液系と同様な発光過程を有することが確認できる。次に
第４図は駆動電圧と発光強度の関係を示しており、２ボ
ルト程度から発光が始まり、3.5ボルト付近で強度はピ
ークに達し、さらに電圧を上げると逆に強度は下がる。
一方電圧を10ボルトから下げて行くとやはり3.5ボルト
付近で強度がピークに達する。このことから本発明のEC
Lは駆動電圧が3.5ボルト程度であり、従来の溶液系の10
ボルトより低電圧で駆動できる。尚、電圧を10ボルトか
ら下げて行った戻りの場合の方が発光強度が小さいこと
から誘起種生成過程を妨害する反応が起っていると考え
られる。また、第５図はAlシート電極の代わりに白金シ
ート電極を用いた場合の駆動電圧と発光強度との関係を
示しており、この場合、強度のピークは2.5ボルト付近
であり、電極条件により駆動電圧が異なるが、ともに低
電圧で駆動される。According to the present invention having such a configuration, the Al sheet electrode 1 is negative,
By applying a positive DC voltage E to the ITO electrode 4, ECL
Luminescence is obtained. FIG. 3 shows the emission spectrum. The applied voltage is 3.5 volts. Here, the ECL emission indicated by the solid line is in agreement with the fluorescence spectrum induced by the light of 450 nm indicated by the wavy line, suggesting that the ECL emission is the emission from the induced state of the electrochemically generated divalent Ru complex. To be In addition, this emission spectrum shows the EC of the conventional solution system.
Since it also matches the spectrum obtained with L, it can be confirmed that the present invention has a light emission process similar to that of the solution system. Next, FIG. 4 shows the relationship between the driving voltage and the light emission intensity. The light emission starts from about 2 V, reaches the peak at about 3.5 V, and decreases further when the voltage is further increased.
On the other hand, when the voltage is lowered from 10 V, the intensity reaches its peak around 3.5 V. From this, the EC of the present invention
L has a drive voltage of about 3.5 V, which is 10
It can be driven at a voltage lower than volt. Incidentally, it is considered that there is a reaction that interferes with the induced species generation process because the emission intensity is smaller in the case of the return when the voltage is lowered from 10 V. Further, FIG. 5 shows the relationship between the driving voltage and the emission intensity when a platinum sheet electrode is used instead of the Al sheet electrode. In this case, the intensity peak is around 2.5 V, and it depends on the electrode conditions. Although the voltages are different, they are both driven at a low voltage.
第６図は駆動電圧を3.5ボルトにした場合の発光強度の
時間的変化を示しており、電圧を加えた直後に鋭いピー
クが見られ、１分を過ぎると勾配は緩やかになり、６分
程度経過した後は数時間にわたりほとんど変動がなく安
定した発光強度となり従来の溶液系よりも改善されてい
る。Figure 6 shows the change over time in the emission intensity when the drive voltage was set to 3.5 V. A sharp peak was observed immediately after the voltage was applied, and after 1 minute the slope became gentle, about 6 minutes. After the lapse of time, the luminescence intensity is stable with almost no fluctuation for several hours, which is an improvement over the conventional solution system.
第７図は、駆動電圧を周期的に変化させて応答速度を調
べたもので横軸が秒単位の時間変化を示しており、駆動
電圧は周期が0.1Hzである。これによると発光は電圧を
加えた瞬間に始まり、0.6秒経過すると最大強度に達し
ている。また、電圧を０ボルトにしたときの消光も同様
に0.6秒程度を必要となる。このように、応答速度が非
常に良好である。FIG. 7 is a graph in which the response speed is examined by periodically changing the driving voltage, and the horizontal axis shows the time change in seconds, and the driving voltage has a cycle of 0.1 Hz. According to this, the light emission starts at the moment when the voltage is applied and reaches the maximum intensity after 0.6 seconds. Further, quenching when the voltage is set to 0 volt also requires about 0.6 seconds. Thus, the response speed is very good.
第８図は周波数を変化させるときの発光強度を示してお
り、1Hz以下では良好に発光している。従って交流駆動
は難しいが、直流では良好に発光することになる。FIG. 8 shows the light emission intensity when the frequency is changed, and the light is emitted well below 1 Hz. Therefore, AC driving is difficult, but direct current emits light well.
このようにして、本発明による固体系のECLは駆動電圧
を低くすることができるとともに、応答性が速くかつ発
光の安定性も良好である。In this way, the solid-state ECL according to the present invention can have a low driving voltage, a high responsiveness, and a good emission stability.
以上、本発明の一実施例について詳述したが、本発明の
要旨の範囲内で適宜変形できる。例えば、前記実施例で
はRu錯体を含むナフィオン溶液により、先ずAlシート電
極１上に発光層２を形成したが、ナフィオン溶液を用い
ないで、Ru錯体を水溶性ナイロンペーストに含ませて、
導電性ナイロン層３の形成とともに発光層２を形成する
こともできる。また、電気的に誘起されて化学発光する
組成物はRu錯体以外の材料も使用できる。Although one embodiment of the present invention has been described in detail above, it can be appropriately modified within the scope of the present invention. For example, in the above example, the Nafion solution containing the Ru complex was first used to form the light-emitting layer 2 on the Al sheet electrode 1. However, without using the Nafion solution, the Ru complex was contained in the water-soluble nylon paste,
The light emitting layer 2 can be formed together with the formation of the conductive nylon layer 3. In addition, a material other than the Ru complex can be used for the composition that is electrically induced and emits chemiluminescence.
［発明の効果］ 以上詳述したように本発明の電気化学発光表示装置は、
対向配設された金属電極と透明電極間に、ゲル状の電気
的に誘起されて化学発光する組成物から成り発光層と成
る高分子層を設けたことにより、低電圧で駆動できると
ともに、応答性を速め発光の安定性を増すことのできる
電気化学発光表示装置を提供することができる。[Effects of the Invention] As described in detail above, the electrochemiluminescent display device of the present invention is
By providing a polymer layer, which is made of a gel-like composition that is electrically induced and emits chemiluminescence, as a light-emitting layer between the metal electrode and the transparent electrode, which face each other, it can be driven at a low voltage and responds. Thus, it is possible to provide an electrochemiluminescent display device that can accelerate the property and increase the stability of luminescence.
また本発明の電気化学発光表示装置の製造方法は、金属
電極上に電気的に誘起されて化学発光する組成物を含む
水溶性高分子ペーストを製膜して導電性高分子層を形成
し、この高分子層の溶媒を置換した後、混合溶媒を加え
前記高分子層を膨潤させてゲル状に形成し、前記高分子
層上に透明電極を配設したことにより、製造が容易で、
低電圧で駆動できるとともに、応答性を速め発光の安定
性を増すことのできる電気化学発光表示装置の製造方法
を提供することができる。Further, the method for manufacturing an electrochemiluminescent display device of the present invention, a conductive polymer layer is formed by forming a water-soluble polymer paste containing a composition that is chemically induced by being electrically induced on a metal electrode. After replacing the solvent of the polymer layer, a mixed solvent is added to swell the polymer layer to form a gel, and by disposing a transparent electrode on the polymer layer, the production is easy,
It is possible to provide a method of manufacturing an electrochemiluminescent display device that can be driven at a low voltage and can have a high responsiveness and an increased stability of light emission.
第１図は本発明の一実施例を示す断面図、第２図は製造
工程を示すフローチャート、第３図〜第８図は各特性を
示すグラフ、第９図は従来のECLの特性を示すグラフで
ある。 １……Alシート電極（金属電極） ２……発光層 ３……導電性ナイロン層（導電性高分子層） ４……ITO電極（透明電極）FIG. 1 is a sectional view showing an embodiment of the present invention, FIG. 2 is a flow chart showing a manufacturing process, FIGS. 3 to 8 are graphs showing respective characteristics, and FIG. 9 shows characteristics of a conventional ECL. It is a graph. 1 ... Al sheet electrode (metal electrode) 2 ... Emitting layer 3 ... Conductive nylon layer (conductive polymer layer) 4 ... ITO electrode (transparent electrode)
フロントページの続き (72)発明者 横山 明聡 新潟県長岡市東蔵王２丁目２番34号 日本 精機株式会社内 (56)参考文献 特開 昭57−51781（ＪＰ，Ａ) 特開 昭61−55185（ＪＰ，Ａ) 特開 昭59−201392（ＪＰ，Ａ) 特開 昭50−50893（ＪＰ，Ａ) 特公 昭40−16819（ＪＰ，Ｂ１)Front page continuation (72) Inventor Akira Satoshi Yokoyama 2-32 Higashi Zao, Nagaoka City, Niigata Japan Seiki Co., Ltd. (56) References JP-A-57-51781 (JP, A) JP-A-61-55185 (JP, A) JP 59-201392 (JP, A) JP 50-50893 (JP, A) JP 40-16819 (JP, B1)
Claims (2)
ゲル状の電気的に誘起されて化学発光する組成物から成
り発光層と成る高分子層を設けたことを特徴とする電気
化学発光表示装置。1. A metal electrode and a transparent electrode, which are arranged to face each other,
An electrochemiluminescent display device comprising a polymer layer, which is made of a gel-like composition which is electrically induced and emits chemiluminescence, and which serves as a light emitting layer.
する組成物を含む水溶性高分子ペ−ストを製膜して導電
性高分子層を形成し、この高分子層の溶媒を置換した
後、混合溶媒を加え前記高分子層を膨潤させてゲル状に
形成し、前記高分子層上に透明電極を配設したことを特
徴とする電気化学発光表示装置の製造方法。2. A conductive polymer layer is formed by forming a water-soluble polymer paste containing a composition which is electrically induced and chemiluminescent on a metal electrode to form a conductive polymer layer. After the substitution, a mixed solvent is added to swell the polymer layer to form a gel, and a transparent electrode is disposed on the polymer layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63108405A JPH0750561B2 (en) | 1988-04-30 | 1988-04-30 | Electrochemiluminescent display device and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63108405A JPH0750561B2 (en) | 1988-04-30 | 1988-04-30 | Electrochemiluminescent display device and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01277824A JPH01277824A (en) | 1989-11-08 |
| JPH0750561B2 true JPH0750561B2 (en) | 1995-05-31 |
Family
ID=14483921
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63108405A Expired - Lifetime JPH0750561B2 (en) | 1988-04-30 | 1988-04-30 | Electrochemiluminescent display device and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0750561B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070095430A (en) * | 2005-01-21 | 2007-09-28 | 코닌클리즈케 필립스 일렉트로닉스 엔.브이. | Polymer light emitting diode and its formation method |
| KR101757016B1 (en) | 2010-03-11 | 2017-07-11 | 메르크 파텐트 게엠베하 | Radiative fibers |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4356429A (en) * | 1980-07-17 | 1982-10-26 | Eastman Kodak Company | Organic electroluminescent cell |
| JPS59201392A (en) * | 1983-04-28 | 1984-11-14 | アルプス電気株式会社 | Dispersion electroluminescence |
| JPS6155185A (en) * | 1984-08-27 | 1986-03-19 | Canon Inc | El element |
-
1988
- 1988-04-30 JP JP63108405A patent/JPH0750561B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01277824A (en) | 1989-11-08 |
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