JPS63221383A - Electrochromic display element - Google Patents
Electrochromic display elementInfo
- Publication number
- JPS63221383A JPS63221383A JP62056257A JP5625787A JPS63221383A JP S63221383 A JPS63221383 A JP S63221383A JP 62056257 A JP62056257 A JP 62056257A JP 5625787 A JP5625787 A JP 5625787A JP S63221383 A JPS63221383 A JP S63221383A
- Authority
- JP
- Japan
- Prior art keywords
- electrode
- display element
- phosphotungstic acid
- polypyrrole
- 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.)
- Pending
Links
- 229920000128 polypyrrole Polymers 0.000 claims description 19
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 16
- 239000002019 doping agent Substances 0.000 claims description 8
- 239000010408 film Substances 0.000 description 13
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- -1 phosphotungstic acid anion Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000003115 supporting electrolyte Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000008317 Condalia obovata Nutrition 0.000 description 1
- 244000147935 Condalia obovata Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 101100184646 Rhodobacter capsulatus modB gene Proteins 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
- 240000009038 Viola odorata Species 0.000 description 1
- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000006386 memory function Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000013598 vector Substances 0.000 description 1
Landscapes
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
- Devices For Indicating Variable Information By Combining Individual Elements (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
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トロクロミック（以下、ＥＣと称す
）表示素子に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to an electrotrochromic (hereinafter referred to as EC) display element.
（従来の技術）
酸化、還元に伴う色変化を利用するＥＣ表示素子は１色
彩が鮮明、視野角が広く、メモリー機能を有し、更に多
色化も可能であるという１種々の特徴を有する。(Prior art) EC display elements that utilize color changes due to oxidation and reduction have various characteristics such as clear colors, wide viewing angles, memory function, and the ability to display multiple colors. .
かようなＥＣ表示素子には還元により青色から黄色へ変
色する導電性ポリピロールが使用できる。For such an EC display element, conductive polypyrrole that changes color from blue to yellow upon reduction can be used.
（発明が解決しようとする問題点）
導電性ｆ ＋７ビロールをＥＣ表示素子として用いる場
合は、製膜が不可避的である。(Problems to be Solved by the Invention) When using conductive f+7 pyrrole as an EC display element, film formation is unavoidable.
導電性ポリピロールの！ＩＩ［は電解酸化重合法を採用
でき、この方法は簡便で好ましいものであるが、このポ
リピロール膜は弱く、膜の構造劣化が早く、耐久性に問
題があった。Conductive polypyrrole! For II[, an electrolytic oxidation polymerization method can be employed, and this method is simple and preferable, but this polypyrrole film is weak, the structure of the film deteriorates quickly, and there are problems with durability.
従って１本発明はＥＣ表示素子の耐久性の改善を主たる
目的とするものである。Therefore, the main object of the present invention is to improve the durability of EC display elements.
（問題点を解決するための手段）
本発明に係るＥＣ表示素子はリンタングステン酸をドー
パントとして有する導電性ポリピロールから成ることを
特徴とするものである。(Means for Solving the Problems) The EC display element according to the present invention is characterized in that it is made of conductive polypyrrole having phosphotungstic acid as a dopant.
かようなＥＣ表示素子は、例えばピロールモノマーとリ
ンタングステン酸アニオンに同一溶液中に溶解しくビロ
ールモノマーと、リンタングステン酸またはその塩を共
存させる）、これを電解酸化重合して、透明導電性電極
とに導電性ポリピロール？薄膜状に形成する方法によっ
て得ることができる。この導電性ポリピロール膜におい
てはポリピロール中に生成した正電荷を中和するためＫ
。Such an EC display element is made by electrolytically oxidizing polymerizing a pyrrole monomer and a phosphotungstic acid anion (by dissolving pyrrole monomer and a phosphotungstic acid anion in the same solution, and coexisting a pyrrole monomer and a phosphotungstic acid or a salt thereof) to form a transparent conductive material. Conductive polypyrrole for electrodes? It can be obtained by a method of forming a thin film. In this conductive polypyrrole film, K is used to neutralize the positive charges generated in the polypyrrole.
.
リンタングステン酸アニオンが咳膜中に取込まれ。The phosphotungstate anion is taken up into the cough membrane.
このリンタングステン酸がポリピロールのドーパントと
して機能する。This phosphotungstic acid functions as a dopant for polypyrrole.
上記の透明導電性電極は何ら制限されるものではないが
１例えば透明導電性材料である酸化スズ。The above-mentioned transparent conductive electrode is not limited in any way, but for example, tin oxide, which is a transparent conductive material.
酸化インジウム、酸化インジウムスズ等ｔ−基材とに蒸
着したものが好適に用いられる。この基材としてはガラ
ス、有機高分子フィルム等透明な基材で蒸着に使えるも
のであれば何でもよい。有機高分子フィルムとしては、
ポリエステルフィルム。Indium oxide, indium tin oxide, etc. deposited on a t-substrate are preferably used. This substrate may be any transparent substrate that can be used for vapor deposition, such as glass or organic polymer film. As an organic polymer film,
Polyester film.
プリイミドフィルム、フッ素樹脂フィルム等を挙げるこ
とができる。またと記透明導電性材料を蒸着以外の方法
５例えばコーティングにより基材上に塗布したものも用
いる事ができる。Examples include priimide film and fluororesin film. It is also possible to use a material in which the transparent conductive material is applied onto a substrate by a method other than vapor deposition, for example, by coating.
ビロールの電解酸化重合の条件も何ら制限されるととＦ
ｉない。電流密度は１０ ＩＪＡ／ｃ＋４〜１０ｍＡ／
ｅ４の範囲が好適に用いられる。ビロール濃度は１通常
、１０ ｍｏＬ／４〜数ｍｏノ／ｊ好ましくは１０−
” ｍｏ４／ｉ！２〜３ｍｏｊ／Ｊの範囲で用いること
ができる。支持電解質としては、ドーパントとすべきリ
ンタングステン酸あるいはその塩類をそのまま用いる。There are no restrictions on the conditions for the electrolytic oxidative polymerization of virol.
I don't. Current density is 10 IJA/c+4~10mA/
A range of e4 is preferably used. The concentration of virol is usually 1, 10 moL/4 to several moL/j, preferably 10-
"mo4/i! can be used in the range of 2 to 3 moj/J. As the supporting electrolyte, phosphotungstic acid or its salts to be used as a dopant can be used as is.
リンタングステン酸以外の支持電解質１例えば過塩素酸
リチウム、ホウフッ化水素酸リチウム等を混在させても
よい。Supporting electrolyte 1 other than phosphotungstic acid, such as lithium perchlorate, lithium borohydrofluoride, etc., may be mixed.
リンタングステン酸あるいはその塩の量は、隘陽両ＩＥ
極間の液間抵抗が、ビロールの電解酸化を妨げるほど高
くならない範囲で自由に設定でき、通常、 １０
ｍｏｌ／ｌ〜数ｍｏｌＪ／ｌであるが、好ましくは１０
−”ｍｏｌ／Ｉ〜３ｍｏｌ／ｌである。溶剤としては。The amount of phosphotungstic acid or its salt is
The liquid resistance between the electrodes can be set freely within a range that does not become so high as to prevent the electrolytic oxidation of virol, and is usually 10.
mol/l to several molJ/l, preferably 10
-"mol/I to 3 mol/l. As a solvent.
ビロールとリンタングステン酸の両方ｙｔｍ解し。YTM analysis of both virol and phosphotungstic acid.
かつ、電解酸化重合時に印加する電圧で酸化されないよ
うなものであれは特に制限されない。例えば、水、プロ
ピレンカーボネート、アセトニトリル、ジメトキシエタ
ン等が好適に用いられる。Moreover, there are no particular limitations as long as the material is not oxidized by the voltage applied during electrolytic oxidative polymerization. For example, water, propylene carbonate, acetonitrile, dimethoxyethane, etc. are preferably used.
このようにして得られたリンタングステン酸をドーパン
トとして有する導電性ポリピロー ル薄膜の電導度は、
１０ Ｓ／ｃｌＬ〜１０Ｓ／ｃＩＬの値を有しており１
通常は１０ Ｓ／ｃｌＬ〜１０Ｓ／ｃＩＩＬの範囲にあ
る。The conductivity of the conductive polypyrrole thin film having phosphotungstic acid as a dopant thus obtained is:
It has a value of 10 S/clL to 10 S/cIL and 1
It is usually in the range of 10 S/clL to 10 S/cIIL.
このように本発明による導電性ポリピロールとリンタン
グステン酸からなるＥＣ表示素子は、例えば上記の如く
電解酸化重合法によシ容易に作製でき、さらに電極上に
生成する導電性−リビロールの量は、電解酸化重合時の
通電量に比例するので、その膜厚を容易に制御できる。As described above, the EC display element made of conductive polypyrrole and phosphotungstic acid according to the present invention can be easily produced, for example, by the electrolytic oxidation polymerization method as described above, and furthermore, the amount of conductive ribirol produced on the electrode is Since it is proportional to the amount of current applied during electrolytic oxidation polymerization, the film thickness can be easily controlled.
本発明による導電性？リビロールフイルムは。Conductivity according to the present invention? Libiroll film.
ドーパントとして、−分子あたり複数個のチャージを有
するリンタングステン酸を保有しているので、その製膜
性が良く、機械的な劣化がしに＜〈。Since it contains phosphotungstic acid, which has multiple charges per molecule, as a dopant, it has good film forming properties and is resistant to mechanical deterioration.
耐久性が優れている。Excellent durability.
本発明による導電性ポリピロールとリンタングステン酸
からなるＥＣ表示素子は、導電性ポリピロールと、リン
タングステン酸が、静電的に強固に複合しているため、
それぞれに特有のＥＣ特性以外に相互作用により、それ
自身では発色しない色を発現する。具体的には、リンタ
ングステン酸は、単独では還元によって青色を示すが、
ポリピロール中では、その発色は、相互作用が強い場合
赤色１弱い場合青紫色となる。The EC display element made of conductive polypyrrole and phosphotungstic acid according to the present invention has a strong electrostatic composite between the conductive polypyrrole and phosphotungstic acid.
In addition to their unique EC characteristics, they interact to produce colors that cannot be produced by themselves. Specifically, phosphotungstic acid shows blue color when reduced alone, but
In polypyrrole, the color is red 1 when the interaction is strong and blue-violet when the interaction is weak.
例えば飽和カロメル電極ｔ−参照電極として＋０．２〜
−〇、２ｖの電位範囲で青色、−０，２〜−〇、６ｖで
赤。For example, as a saturated calomel electrode t-reference electrode +0.2 ~
Blue in the potential range of -〇, 2v, red in the potential range of -0,2 to -〇, 6v.
−〇、４〜−０．６Ｖで黄色を示す。この赤色はポリピ
ロールと、その中にドーパントとして含まれているリン
タングステン酸との相互作用により現れる色である。こ
れまでに、ポリピロールを用いたＥＣ表示素子で赤色が
現れた例は報告されておらず。-○, shows yellow at 4 to -0.6V. This red color appears due to the interaction between polypyrrole and phosphotungstic acid contained therein as a dopant. Up to now, no case has been reported in which a red color appears in an EC display element using polypyrrole.
本発明のリンタングステン酸をドーパントとして有する
導電性ポリピロールによって初めて達成されたものであ
る。This was achieved for the first time using the conductive polypyrrole containing phosphotungstic acid as a dopant according to the present invention.
（実施例） 以下、実施例により本発明を更に詳細に説明する。(Example) Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例１
厚さｌ ｙｔｘのガラス板の片面とに酸化インジウム−
酸化スズから成る薄ＩＩＩを形成した透明導電性電極を
作用極とし、白金からなる電極を対極とし。Example 1 Indium oxide was applied to one side of a glass plate having a thickness of lytx.
A transparent conductive electrode made of thin III made of tin oxide was used as a working electrode, and an electrode made of platinum was used as a counter electrode.
ｄ’ｙ’４を溶解させた水２０ｍを電解液として、参照
電極として用いた飽和カロメル電極（ＳＣＥ）に対して
＋７００ｍＶの定電位電Ｎを８０ｍＣ／−になるまで行
ない透明導電性電極上に導電性ポリピロ−ル膜（厚さ０
．２μ愼）を形成した。Using 20 m of water in which d'y'4 was dissolved as an electrolyte, a constant potential of +700 mV was applied to a saturated calomel electrode (SCE) used as a reference electrode until the voltage reached 80 mC/-, and the electrode was placed on a transparent conductive electrode. Conductive polypyrrole film (thickness 0
．． 2 μm) was formed.
この電極（透明導電性電極Ｊ：ＶＣ導電性ポリピロール
膜を形成したもの） ｆＩ：０．１ｍｏｌ／ｌ ＫＣＩ
水溶液中（ｐＨ＝２）で、対極を白金線、参照電極を５
ＣＥ（飽和カロメル電極）として０．２Ｖから−０，６
Ｖまでの電位を変化させたときの吸収スペクトルを第１
図に示した。このときの電極の色変化は、＋０．２〜−
０．２Ｖテ青−０，２〜−０．４Ｖテ赤、−０．４〜−
０．６Ｖｆ赤紫色’ｅｙｉくした。＋０．２〜−０．２
Ｖ （青廿赤）の範囲での電位走査のサイクルによりて
、 ｓｏｏ。This electrode (transparent conductive electrode J: VC conductive polypyrrole film formed) fI: 0.1 mol/l KCI
In an aqueous solution (pH = 2), the counter electrode is a platinum wire and the reference electrode is 5
CE (saturated calomel electrode) from 0.2V to -0.6
The absorption spectrum when changing the potential up to V is the first
Shown in the figure. The color change of the electrode at this time is +0.2 to -
0.2V Te Blue -0.2~-0.4V Te Red, -0.4~-
0.6Vf reddish purple 'eyi. +0.2~-0.2
By cycles of potential scanning in the range of V (blue-red), soo.
回においても初期の８０％以上の吸光度を保持した。耐
久性を示した。＋０．２〜−〇、４Ｖ（青材赤ぜ青紫）
では、５ｏｏｏ回において初期の５０％以との吸光度を
保持した耐久性を示した。The absorbance was maintained at 80% or more of the initial value even in the second test. It showed durability. +0.2~-〇, 4V (blue wood, red, blue and purple)
In this case, durability was shown in which the absorbance was maintained at 50% or more of the initial value after 500 cycles.
実施例２
実施例１と同様にして調製した電極ｆ ０．１ ｍｏｊ
／１−ＫＣＩ水溶液中（ｐＨ＝７）で対極を白金線、参
Ｍ４電極を５ＣＥ（飽和カロメル電極）として＋〇、２
Ｖから一〇、６Ｖまで、電位を変化させたときの吸収又
ベクトルを第２図に示した。Example 2 Electrode f 0.1 moj prepared in the same manner as Example 1
/1-In a KCI aqueous solution (pH = 7), with a platinum wire as the counter electrode and a 5CE (saturated calomel electrode) as the reference M4 electrode, +〇, 2
Figure 2 shows the absorption and vectors when the potential is changed from V to 10.6V.
このときの電極の色変化は、＋０．２〜−〇、２■で肯
。The color change of the electrode at this time was positive at +0.2 to -〇, 2■.
−０，２〜−０．４Ｖテ赤、−０．４〜−０．６Ｖｆ黄
色を示した。-0.2 to -0.4V showed red and -0.4 to -0.6V showed yellow.
＋０６２〜−０．２Ｖ（青峠赤）の範囲での電位走査の
サイクルによって、５ｏｏｏ回においても初期の７０％
以との吸光度を保持した耐久性を示した。By a cycle of potential scanning in the range of +062 to -0.2V (Aotoge red), 70% of the initial value is reduced even in 5ooo times.
It showed durability while maintaining absorbance.
（発明の効果）
本発明によるＥＣ表示素子は、その製造の簡便さ、多色
性、耐久性から、安価で、大面積の必要な、多色表示素
子を提供できる。(Effects of the Invention) The EC display element according to the present invention can provide a multicolor display element that is inexpensive and requires a large area due to its ease of manufacture, multicolor property, and durability.
第１図および第２図はいずれも本発明に係るＥＣ表示素
子に各種の電圧を印加させた場合の波長と吸光度の関係
を示すスペクトル図である。FIG. 1 and FIG. 2 are both spectral diagrams showing the relationship between wavelength and absorbance when various voltages are applied to the EC display element according to the present invention.
Claims (1)
リピロールから成ることを特徴とするエレクトロクロミ
ック表示素子。An electrochromic display element comprising conductive polypyrrole having phosphotungstic acid as a dopant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62056257A JPS63221383A (en) | 1987-03-11 | 1987-03-11 | Electrochromic display element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62056257A JPS63221383A (en) | 1987-03-11 | 1987-03-11 | Electrochromic display element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63221383A true JPS63221383A (en) | 1988-09-14 |
Family
ID=13022028
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62056257A Pending JPS63221383A (en) | 1987-03-11 | 1987-03-11 | Electrochromic display element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63221383A (en) |
-
1987
- 1987-03-11 JP JP62056257A patent/JPS63221383A/en active Pending
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