JPH07104527B2 - Electrochromic display element - Google Patents
Electrochromic display elementInfo
- Publication number
- JPH07104527B2 JPH07104527B2 JP60189171A JP18917185A JPH07104527B2 JP H07104527 B2 JPH07104527 B2 JP H07104527B2 JP 60189171 A JP60189171 A JP 60189171A JP 18917185 A JP18917185 A JP 18917185A JP H07104527 B2 JPH07104527 B2 JP H07104527B2
- Authority
- JP
- Japan
- Prior art keywords
- ecd
- layer
- anode
- film
- conductive film
- 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 - Lifetime
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Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、エレクトロクロミツク表示素子に係り、特に
表示安定性に優れたエレクトロクロミツク表示素子に関
するものである。TECHNICAL FIELD The present invention relates to an electrochromic display element, and more particularly to an electrochromic display element having excellent display stability.
（従来技術とその問題点） 従来、エレクトロクロミツク表示素子（Electro Chromi
c device;以下、ECDと略称する。）としては、表示電極
の陽極に酸化インジウム・スズ（ITO）層を用いたECDが
知られている。(Prior art and its problems) Conventional electrochromic display elements (Electro Chromi
c device; hereinafter, abbreviated as ECD. ), An ECD using an indium tin oxide (ITO) layer for the anode of the display electrode is known.
図面は、このようなECDの一例を示すものであつて、こ
の例のECDは、互に対向するガラス板1,1の各々の対向面
に真空蒸着法あるいはスパツタリング法により陽極とし
て陽極用ITO層２、陰極として陰極用ITO層３を設け、さ
らにその陽極用ITO層２の表面の中央部にモノマーを電
解酸化重合した重合体からなるエレクトロクロミツク層
（以下、EC層）４を形成してなるものである。The drawing shows an example of such an ECD, and the ECD of this example is an ITO layer for an anode as an anode by a vacuum deposition method or a sputtering method on each of the facing surfaces of the glass plates 1 and 1 facing each other. 2. A cathode ITO layer 3 is provided as a cathode, and an electrochromic layer (hereinafter referred to as an EC layer) 4 made of a polymer obtained by electrolytically oxidatively polymerizing a monomer is further formed in the center of the surface of the anode ITO layer 2. It will be.
ガラス板1,1間には、スペーサ5,5が配置され、これらス
ペーサ5,5と陰極用ITO層３とEC層４とに囲まれた密閉空
間には、Cl-,Br-,ClO4 -,BF4 -などのアニオンを含む電解
質溶液６が充填されている。Spacers 5 and 5 are arranged between the glass plates 1 and 1, and a closed space surrounded by the spacers 5 and 5, the cathode ITO layer 3 and the EC layer 4 is filled with Cl − , Br − , ClO 4 -, BF 4 - electrolyte solution 6 containing anion such as are filled.
ところが、このECDにあつては、陽極用ITO層２の表面が
極めて平滑であることから、陽極用ITO層２とEC層４と
の結合が十分ではなく、陽極用ITO層２と陰極用ITO層３
との間で電位を繰り返し反転させると、EC層４にしわが
よつたり、剥離部分が生じたりして表示安定性に欠ける
などの問題点があつた。However, in this ECD, since the surface of the anode ITO layer 2 is extremely smooth, the bonding between the anode ITO layer 2 and the EC layer 4 is not sufficient, and the anode ITO layer 2 and the cathode ITO layer 2 are not joined. Layer 3
When the electric potential was repeatedly inverted between and, the EC layer 4 had wrinkles and a peeling portion was generated, resulting in poor display stability.
（発明の目的） 本発明は、上記の事情に鑑みてなされたもので、その目
的とするところは、表示安定性に優れたECDを提供する
ことにある。(Object of the Invention) The present invention has been made in view of the above circumstances, and an object thereof is to provide an ECD excellent in display stability.
（問題点を解決するための手段） 本発明のECDは、陽極が導電性微粉末を高分子重合体に
混合してフィルム状に成型してなる表面が粗な導電性高
分子フイルムであることを特徴とするものである。(Means for Solving Problems) The ECD of the present invention is a conductive polymer film having a rough surface formed by mixing a conductive polymer powder with a polymer and molding the film into a film. It is characterized by.
（実施例） 以下、先の図面を利用して、本発明のECDを詳しく説明
する。(Example) Hereinafter, the ECD of the present invention will be described in detail with reference to the above drawings.
図中符号７は、ECDである。この例のECD7は、図面に示
すように、積層構造体であつて、互に対向するガラス板
1,1のいずれか一方の対向面に陽極として導電性高分子
フイルム（以下、導電性フイルムと略称する。）８を接
合し、他方の対向面に真空蒸着法あるいはスパツタリン
グ法により陰極として陰極用ITO層３を設け、さらに上
記導電性フイルム８の表面の中央部にモノマーを電解酸
化重合してEC層４を形成してなるものである。Reference numeral 7 in the figure is an ECD. As shown in the drawing, the ECD 7 of this example is a laminated structure, and glass plates facing each other.
A conductive polymer film (hereinafter, abbreviated as a conductive film) 8 is bonded as an anode to one of the opposing surfaces of 1, 1 and a cathode is used as a cathode by a vacuum deposition method or a sputtering method on the other opposing surface. The ITO layer 3 is provided, and the EC layer 4 is formed by electrolytically oxidatively polymerizing a monomer on the central portion of the surface of the conductive film 8.
ガラス板1,1間には、スペーサ5,5が配置され、これらス
ペーサ5,5と陽極用ITO層２とEC層４とに囲まれた密閉空
間には、Cl-,Br-,ClO4 -,BF4 -などのアニオンを含む電解
質溶液６が充填されている。Spacers 5 and 5 are arranged between the glass plates 1 and 1, and a closed space surrounded by the spacers 5 and 5, the anode ITO layer 2 and the EC layer 4 is filled with Cl − , Br − , ClO 4 -, BF 4 - electrolyte solution 6 containing anion such as are filled.
導電性フイルム８は、導電性微粉末を高分子重合体に混
練した後、プレス成型法によりフイルム状に成型してな
るものであつて、その表面が若干粗面になつたものであ
る。The electroconductive film 8 is formed by kneading electroconductive fine powder with a high molecular weight polymer and then forming it into a film by a press molding method, and its surface is slightly roughened.
上記導電性微粉末には、電解酸化重合の電解質溶液と反
応しないものが選ばれ、具体的にはTiO2にSnO2をコート
した微粉末が好適に用いられるが、これに限定されるも
のではない。そして、上記高分子重合体の100重量部に
対する導電性微粉末の配合量は、20〜150重量部の範囲
とされ、20重量部未満では得られる導電性フイルム８の
導電性が十分に得られず、また150重量部を越えるもの
では導電性フイルム８の導電性が過剰なものとなり、不
経済である。As the conductive fine powder, one that does not react with the electrolytic solution of electrolytic oxidation polymerization is selected, and specifically, fine powder obtained by coating SnO 2 on TiO 2 is preferably used, but is not limited thereto. Absent. The amount of the conductive fine powder to be added to 100 parts by weight of the high molecular weight polymer is in the range of 20 to 150 parts by weight, and if the amount is less than 20 parts by weight, the conductivity of the obtained conductive film 8 is sufficiently obtained. If the amount exceeds 150 parts by weight, the electroconductivity of the electroconductive film 8 becomes excessive, which is uneconomical.
上記高分子重合体には、電解酸化重合の電解質溶液と相
互作用しないものが選ばれ、具体的にはポリオレフイン
樹脂、ポリアミド樹脂などの合成樹脂が用いられる。A polymer that does not interact with an electrolytic solution for electrolytic oxidation polymerization is selected as the high molecular weight polymer, and specifically, a synthetic resin such as a polyolefin resin or a polyamide resin is used.
また、EC層４の前駆化合物であるモノマーには、その重
合体がEC特性を示す化合物が選ばれ、具体的にはアニオ
ン、チオフエン、ピロールなどが好適に用いられる。従
つて、EC層４を形成する重合体としては、ポリアニリ
ン、ポリチオフエン、ポリピロールなどが挙げられる。Further, as the monomer which is the precursor compound of the EC layer 4, a compound whose polymer exhibits EC characteristics is selected, and specifically, anion, thiophene, pyrrole and the like are preferably used. Therefore, examples of the polymer forming the EC layer 4 include polyaniline, polythiophene, and polypyrrole.
さらに、導電性フイルム８内に分散する材料としては、
導電性微粉末と共に着色剤を使用することも可能であ
る。この着色剤には、導電性微粉末や電解酸化重合の電
解質溶液と反応しないものが選ばれ、具体的にはシアニ
ン系やアゾ系などの顔料が用いられる。Further, as the material dispersed in the conductive film 8,
It is also possible to use a colorant with the conductive fine powder. As the colorant, one that does not react with the conductive fine powder or the electrolytic solution of electrolytic oxidation polymerization is selected, and specifically, a cyanine-based or azo-based pigment is used.
このような構成からなるECDにあつては、導電性フイル
ム８に表面が粗面であるので、この表面に電解酸化重合
によって形成されたEC層４が強く接合し、電位を繰り返
し反転させてもEC層４にしわがよつたり、剥離部分を生
じたりする不都合がないものとなる。In the ECD having such a structure, since the conductive film 8 has a rough surface, the EC layer 4 formed by electrolytic oxidation polymerization strongly adheres to this surface, and even if the potential is repeatedly inverted, There is no inconvenience that the EC layer 4 is wrinkled or peeled off.
また、上記実施例では、導電性フイルム８の表面が若干
粗面になつているが、その表面に微細孔をあけて多孔質
とすることもできる。この表面を多孔質とした導電性フ
イルム８を有するECDにあつては、付随的にEC層４の表
面積もまた大きくなることからEC層４へのイオンの出入
りが効率よく行なわれる様になるので変色に要する時間
が短かくなる。すなわちEC層４のEC特性を向上させたも
のとなる。Further, in the above embodiment, the surface of the conductive film 8 is slightly roughened, but it is also possible to make fine pores on the surface to make it porous. In the case of the ECD having the conductive film 8 having a porous surface, the surface area of the EC layer 4 is also increased incidentally, so that ions can efficiently enter and leave the EC layer 4. The time required for discoloration becomes shorter. That is, the EC characteristics of the EC layer 4 are improved.
次に、本発明のECDを製造する方法について詳述する。
まず、低密度ポリエチレン100重量部にTiO2にSnO2をコ
ートした導電性微粉末を50重量部添加し、160℃のロー
ルで混練後プレス成型して導電性フイルム８を作製す
る。次に、導電性フイルム８をガラス板１に接合して電
極とし、対向電極に白金板を用い、INのH2SO4水溶液に
モノマー（アニリン）を0.5mol/lになるように溶解して
得た溶液中で、0.1mA/cm2の電流密度で３分間電解酸化
重合して導電性フイルム８上にEC層（ポリアニリン薄
膜）４を形成する。別のガラス板１の一面に真空蒸着法
などにより陰極用ITO層３を形成する。これらガラス板
1,1とを互いに対向させて陰極用ITO層３とEC層４とを向
かい合わせ、ガラス板1,1間にスペーサ5,5を配置して密
閉空間を形成して、この空間に電解質溶液（0.1mol/lの
LiCl水溶液）６を充填する。さらに、フイルム表面を多
孔質にするには、化学的処理方法と物理的処理方法とが
ある。まず、化学的な方法としては、熱キシレン中に導
電性フィルム10を数秒間浸漬して表面にエツチングを施
す方法がある。また、物理的な方法としては、導電性フ
イルム10の表面をアルゴンガスプラズマで処理する方法
がある。Next, the method for producing the ECD of the present invention will be described in detail.
First, 100 parts by weight of low-density polyethylene is added with 50 parts by weight of conductive fine powder in which TiO 2 is coated with SnO 2 , and the mixture is kneaded with a roll at 160 ° C. and press-molded to produce a conductive film 8. Next, the conductive film 8 was bonded to the glass plate 1 to form an electrode, a platinum plate was used as the counter electrode, and the monomer (aniline) was dissolved in H 2 SO 4 aqueous solution of IN to 0.5 mol / l. In the obtained solution, the EC layer (polyaniline thin film) 4 is formed on the conductive film 8 by electrolytic oxidation polymerization at a current density of 0.1 mA / cm 2 for 3 minutes. An ITO layer 3 for a cathode is formed on one surface of another glass plate 1 by a vacuum deposition method or the like. These glass plates
Cathode ITO layer 3 and EC layer 4 face each other with 1 and 1 facing each other, spacers 5 and 5 are arranged between glass plates 1 and 1 to form a closed space, and an electrolyte solution is placed in this space. (0.1 mol / l
LiCl aqueous solution) 6. Further, there are a chemical treatment method and a physical treatment method for making the film surface porous. First, as a chemical method, there is a method in which the conductive film 10 is immersed in hot xylene for several seconds to etch the surface. As a physical method, there is a method of treating the surface of the conductive film 10 with argon gas plasma.
（実験例） 以下、実験例を示して本発明の作用効果を明確にする。(Experimental example) Hereinafter, an experimental example is shown and the effect of this invention is clarified.
（実験例１） 低密度ポリエチレン100重量部にTiO2にSnO2をコートし
た導電性微粉末を50重量部添加し、160℃のロールで混
練後、プレス成型して導電性フイルムを作製した。この
導電性フイルムは白色であり、また表面導電率が100Ω
／ロであつた。次に上記導電性フイルムをガラス板に接
合して電極とし、この対向電極に白金板を用い、6NのH2
SO4水溶液にアニリンを0.5ml/lになるように溶解して得
た溶液中で、0.1mA/cm2の電流密度で３分間電解酸化重
合して導電性フイルム上にポリアニリン薄膜を形成し
た。一方、別のガラス板の一面に真空蒸着法により陰極
用ITO層を形成した。これら二枚のガラス板を対向さ
せ、0.1mol/lのLiCl水溶液を電解質溶液としてECDを作
製した。(Experimental Example 1) 100 parts by weight of low-density polyethylene was added with 50 parts by weight of conductive fine powder obtained by coating TiO 2 with SnO 2 , kneading with a roll at 160 ° C., and press molding to produce a conductive film. This conductive film is white and has a surface conductivity of 100Ω.
/ It was hot. Next, the conductive film was bonded to a glass plate to form an electrode, and a platinum plate was used as the counter electrode, and 6N H 2
A polyaniline thin film was formed on the conductive film by electrolytic oxidation polymerization for 3 minutes at a current density of 0.1 mA / cm 2 in a solution obtained by dissolving aniline in a SO 4 aqueous solution to a concentration of 0.5 ml / l. On the other hand, an ITO layer for a cathode was formed on one surface of another glass plate by a vacuum deposition method. These two glass plates were opposed to each other, and an ECD was prepared by using a 0.1 mol / l LiCl aqueous solution as an electrolyte solution.
また、上記のECDの導電性フイルムの代わりに陽極用ITO
層を用い、他は上記のECDと同条件で比較例のECDを作成
した。Also, instead of the conductive film of ECD above, ITO for the anode is used.
The ECD of the comparative example was prepared under the same conditions as the above ECD except that the layers were used.
こられ２個のECDについて変色特性及び変色時間を調べ
た。The discoloration characteristics and discoloration time of these two ECDs were examined.
（イ）変色特性試験：電位を繰り返し反転させてポリア
ニリン薄膜の状態を調べたところ、本発明の条件を満た
すECDでは、50回の電位反転でもポリアニリン薄膜に変
化がなく、剥離も認められなかつた。しかし、比較例の
ECDでは30回の電位反転でポリアニリン薄膜に剥離がみ
られた。(B) Discoloration characteristic test: When the state of the polyaniline thin film was examined by repeatedly reversing the potential, the ECD satisfying the conditions of the present invention showed no change in the polyaniline thin film even after 50 reversals of the potential, and no peeling was observed. . However, in the comparative example
In ECD, peeling was observed in the polyaniline thin film after 30 potential reversals.
（ロ）変色時間試験：対極間電圧を2Vとして、黄紫の
変色に要する時間を測定したところ、本発明の条件を満
たすECDでは、約2.5秒であり、比較例のECDでは６秒で
あつた。(B) Discoloration time test: The time required for discoloration of yellow-purple was measured with the voltage between the electrodes being 2 V, and it was about 2.5 seconds for the ECD satisfying the conditions of the present invention and 6 seconds for the ECD of the comparative example. It was
これらの実験結果からも明らかなように、本発明の条件
を満たすECDは、比較例のECDに比べてポリアニリン薄膜
（EC層）が電位反転の際にも安定である。と共に変色に
要する時間が短かいことがわかる。As is apparent from these experimental results, the ECD satisfying the conditions of the present invention is more stable than the ECD of the comparative example even when the potential of the polyaniline thin film (EC layer) is reversed. Also, it can be seen that the time required for discoloration is short.
（実験例２） 実験例１で作製した導電性フイルムを熱キシレン中に数
秒浸漬してその表面にエツチングを施した。このような
導電性フイルムを用いが実験例１と同様にしてECDを作
製した。(Experimental Example 2) The conductive film produced in Experimental Example 1 was immersed in hot xylene for several seconds to etch the surface thereof. An ECD was produced in the same manner as in Experimental Example 1 using such a conductive film.
このECDの変色特性を調べたところ、50回の電位反転で
ポリアニリン薄膜に変化がなく、また黄紫の変色時間
を調べたところ、対極間電圧2Vで、1.3秒であつた。When the color change characteristics of this ECD were examined, there was no change in the polyaniline thin film after 50 potential reversals, and when the color change time of yellow purple was examined, it was 1.3 seconds at a voltage between the electrodes of 2V.
また、実験例１で作製した導電性フイルムの表面にアル
ゴンプラズマで表面処理を施した。このような導電性フ
イルムを用いて実験例１と同様にしてECDを作製した。The surface of the conductive film prepared in Experimental Example 1 was surface-treated with argon plasma. An ECD was produced in the same manner as in Experimental Example 1 using such a conductive film.
このECDの変色特性を調べたところ、50回の電位反転で
ポリアニリン薄膜に変化がなく、また黄紫の変色時間
を調べたところ対極間電圧2Vで、1,2秒であつた。When the color change characteristics of this ECD were examined, there was no change in the polyaniline thin film after 50 potential reversals, and when the color change time of yellow violet was examined, the voltage between the electrodes was 2 V and it was 1 or 2 seconds.
これらの実験結果からも明らかなように、本発明の条件
を満たし、しかも導電性フイルムに表面処理を施したEC
Dは、ポリアニリン薄膜（EC層）が電位反転の際にも安
定であると共に変色に要する時間をさらに短かくするこ
とがわかる。As is clear from these experimental results, the EC satisfying the conditions of the present invention and having a conductive film surface-treated
It can be seen that D is stable even when the polyaniline thin film (EC layer) is reversed in potential and further shortens the time required for discoloration.
（発明の効果） 以上、説明したように、本発明のエレクトロクロミツク
表示素子は、陽極が導電性微粉末を高分子重合体に混合
してフィルム状に成形した表面が粗な導電性高分子フィ
ルムであるので、陽極とこの陽極上に電解酸化重合して
形成されたエレクトロクロミック層とが強く接合する。
このため、電位反転を繰り返してもエレクトロクロミッ
ク層が剥離したり、しわがよったりすることがなく、優
れた表示安定性を有するものとなる。(Effects of the Invention) As described above, in the electrochromic display element of the present invention, the anode is a conductive polymer having a rough surface formed by mixing conductive fine powder with a polymer to form a film. Since it is a film, the anode and the electrochromic layer formed on the anode by electrolytic oxidation polymerization are strongly bonded.
Therefore, even if the potential inversion is repeated, the electrochromic layer does not peel off or wrinkle, and the display stability is excellent.
図面は、本発明に係るエレクトロクロミツク表示素子の
一例を示す概略断面図である。 ４……エレクトロクロミツク層、６……電解質溶液、７
……エレクトロクロミツク表示素子、10……導電性高分
子フイルム。The drawing is a schematic cross-sectional view showing an example of the electrochromic display element according to the present invention. 4 ... Electrochromic layer, 6 ... Electrolyte solution, 7
…… Electrochromic display element, 10 …… Conductive polymer film.
Claims (1)
重合して形成されたエレクトロクロミック層と、上記陽
極に対向する陰極と、この陰極の対向面と上記エレクト
ロクロミック層との間の空間に充填された電解質溶液と
からなり、上記両電極間に電圧を印加して表示を行うエ
レクトロクロミック表示素子において、 上記陽極が導電性微粉末を高分子重合体に混合してフィ
ルム状に成形してなる表面が粗な導電性高分子フィルム
であることを特徴とするエレクトロクロミック表示素
子。1. An anode, an electrochromic layer formed by electrolytically oxidizing and polymerizing a monomer on the anode, a cathode facing the anode, and a space between the facing surface of the cathode and the electrochromic layer. In an electrochromic display element which is composed of an electrolyte solution filled in, and performs display by applying a voltage between both electrodes, the anode mixes conductive fine powder with a polymer to form a film. An electrochromic display element characterized by being a conductive polymer film having a rough surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60189171A JPH07104527B2 (en) | 1985-08-28 | 1985-08-28 | Electrochromic display element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60189171A JPH07104527B2 (en) | 1985-08-28 | 1985-08-28 | Electrochromic display element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6249333A JPS6249333A (en) | 1987-03-04 |
| JPH07104527B2 true JPH07104527B2 (en) | 1995-11-13 |
Family
ID=16236662
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60189171A Expired - Lifetime JPH07104527B2 (en) | 1985-08-28 | 1985-08-28 | Electrochromic display element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07104527B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5754329A (en) * | 1992-12-22 | 1998-05-19 | Monsanto Company | Electrochromic display laminates |
| US5413739A (en) * | 1992-12-22 | 1995-05-09 | Coleman; James P. | Electrochromic materials and displays |
| EP0871949A2 (en) * | 1995-05-09 | 1998-10-21 | Monsanto Company | Conductive font |
| US5876633A (en) * | 1995-12-26 | 1999-03-02 | Monsanto Company | Electrochromic metal oxides |
| US5891511A (en) * | 1995-12-26 | 1999-04-06 | Monsanto Company | Addition of color to electrochromic displays |
| WO1997023578A1 (en) * | 1995-12-26 | 1997-07-03 | Monsanto Company | Electrochromic tin oxide |
| US5877888A (en) * | 1997-06-10 | 1999-03-02 | Monsanto Company | Single and double sided electrochromic displays |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0652355B2 (en) * | 1985-03-19 | 1994-07-06 | 日立マクセル株式会社 | Electrochromic display element |
-
1985
- 1985-08-28 JP JP60189171A patent/JPH07104527B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6249333A (en) | 1987-03-04 |
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| EXPY | Cancellation because of completion of term |