JPH0519691B2 - - Google Patents
Info
- Publication number
- JPH0519691B2 JPH0519691B2 JP59029375A JP2937584A JPH0519691B2 JP H0519691 B2 JPH0519691 B2 JP H0519691B2 JP 59029375 A JP59029375 A JP 59029375A JP 2937584 A JP2937584 A JP 2937584A JP H0519691 B2 JPH0519691 B2 JP H0519691B2
- Authority
- JP
- Japan
- Prior art keywords
- counter electrode
- carbon
- electrode
- display
- display device
- 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
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000003575 carbonaceous material Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000005486 organic electrolyte Substances 0.000 claims 2
- 239000007772 electrode material Substances 0.000 claims 1
- 206010063836 Atrioventricular septal defect Diseases 0.000 description 13
- 238000001211 electron capture detection Methods 0.000 description 13
- 230000007334 memory performance Effects 0.000 description 13
- 125000004151 quinonyl group Chemical group 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 239000012769 display material Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910001930 tungsten oxide Inorganic materials 0.000 description 4
- 239000006231 channel black Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/155—Electrodes
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
- G02F1/1524—Transition metal compounds
Description
産業上の利用分野
本発明は、エレクトロクロミツク表示装置（以
下ECDと略す）の対極の製造方法に関する。
従来例の構成とその問題点
ECDはエレクトロクロミツク表示材料を表示
極とし、これに対向して設けられた対極との間に
電解質が存在し、表示極と対極との間に電圧を印
加することによつて、表示極が電気化学的に還元
または酸化反応を起こし、表示極が発色または消
色する現象を利用した表示装置である。
従来、この種の表示装置では、表示材料に酸化
タングステンや酸化モリブデン等の遷移金属酸化
物や、ビオロゲン等の有機エレクトロクロミツク
材料を使用し、また対極としては一般に電気化学
的に可逆酸化還元を行なう活物質と導電材料であ
るカーボンとを混合して成形したものが用いられ
ていた。
ところが従来のECDは、表示のメモリー性能
が悪いという欠点を有し、ECDの商品価値を低
下させていた。ここで「メモリー性能」とは、
ECDの表示極に−1V，１秒の電圧を印加して着
色状態となし、室温で24時間後に表示極に残存す
る電気量の、着色電気量に対する比をいう。
発明の目的
本発明は上述のような欠点を改善し、メモリー
性能に優れたECDの対極の製造方法を提供する
ことを目的とすものである。
発明の構成
上記目的を達成するために本発明は、対極のカ
ーボン材料と、硫酸水溶液、塩酸水溶液、硝酸水
溶液のうちの少なくとも一つで洗浄処理すること
としたものである。
このような簡単な処理なメモリー性能が向上す
る原因は明確ではないが、発明者らはカーボン表
面の官能基滴定の結果から、おおよそ次のように
推定している。カーボンの表面には酸化作用ある
いは還元作用を有する様々な官能基が存在してい
るとされている。酸化作用の官能基の代表はキノ
ン基であり、還元作用の官能基の代表はハイドロ
キノン基である。本発明の洗浄処理を行なうと、
キノン基の減少が確認できた。つまり、未洗浄処
理のカーボンを使用した場合には、キノン基を保
持したカーボン微粉末が対極から電解液中に溶出
し、表示極に到達して還元状態（着色状態）にあ
る表示極を酸化させる（消色反応に相当する）た
め、メモリー性能が低下することになる。一方、
洗浄処理したカーボンを使用した場合には、表示
板に対する上述のような悪影響が減少し、メモリ
ー性能が向上したものと思われる。
実施例の説明
図は本発明方法により製造したECDの一実施
例の断面図である。図において、１はガラス基
板、２は酸化インジウム、酸化スズなどの薄膜透
明電極、３は薄膜透明電極２上に設けられた表示
極で、酸化タングステンを3000オングストローム
蒸着して構成されている。４は背面ガラス基板、
５はアルミナ反射板、６は対極、７は電解液
（0.3MLiBF4を含む炭酸プロピレン溶液）、８は
集電体である。表示極３以外の薄膜透明電極２上
には、SiO2等の絶縁膜９が設けられている。
次に対極を構成するカーボン材料として、黒
鉛、チヤンネルブラツクの２種を用い、10-4Ｍ，
0.01M，1Mの３種の濃度の異なる硫酸水溶液で
洗浄処理した。
すなわち、カーボン50gを硫酸水溶液2000c.c.に
分散させ、15時間攪拌し、攪拌後、多量の純水で
洗浄して硫酸を除去し、さらに105℃10時間乾燥
した。次に、それぞれのカーボンとフツソ樹脂を
１：１の重量比で混合し、この混合粉末をステン
レスネツトの集電体に加圧成形して作つた対極を
用いてECDを作製した。
表１は洗浄処理によるカーボンのキノン基の量
と、作製したECDのメモリー性能との関係を調
べた結果である。
INDUSTRIAL APPLICATION FIELD The present invention relates to a method for manufacturing a counter electrode of an electrochromic display device (hereinafter abbreviated as ECD). Conventional structure and problems ECD uses an electrochromic display material as a display electrode, an electrolyte exists between it and a counter electrode, and a voltage is applied between the display electrode and the counter electrode. This is a display device that utilizes a phenomenon in which the display electrode electrochemically causes a reduction or oxidation reaction, causing the display electrode to develop or discolor. Conventionally, this type of display device uses a transition metal oxide such as tungsten oxide or molybdenum oxide or an organic electrochromic material such as viologen as a display material, and generally uses electrochemical reversible redox as a counter electrode. A molded mixture of an active material and carbon as a conductive material was used. However, conventional ECDs have the disadvantage of poor display memory performance, reducing the commercial value of ECDs. What is "memory performance" here?
A voltage of -1V for 1 second is applied to the display electrode of an ECD to make it colored, and it is the ratio of the amount of electricity remaining in the display electrode to the amount of colored electricity after 24 hours at room temperature. OBJECTS OF THE INVENTION It is an object of the present invention to provide a method for manufacturing a counter electrode of an ECD that improves the above-mentioned drawbacks and has excellent memory performance. Structure of the Invention In order to achieve the above object, the present invention is to perform a cleaning treatment on a counter electrode carbon material with at least one of an aqueous sulfuric acid solution, an aqueous hydrochloric acid solution, and an aqueous nitric acid solution. Although the reason for the improvement in memory performance due to such a simple process is not clear, the inventors estimate the following from the results of functional group titration on the carbon surface. It is said that various functional groups having oxidizing or reducing effects exist on the surface of carbon. A representative functional group for oxidizing action is a quinone group, and a representative functional group for reducing action is a hydroquinone group. When the cleaning treatment of the present invention is performed,
A decrease in quinone groups was confirmed. In other words, when unwashed carbon is used, fine carbon powder holding quinone groups is eluted from the counter electrode into the electrolyte, reaches the display electrode, and oxidizes the display electrode, which is in a reduced state (colored state). (equivalent to a decoloring reaction), resulting in a decline in memory performance. on the other hand,
It is believed that when cleaned carbon was used, the above-mentioned adverse effects on the display board were reduced and memory performance was improved. DESCRIPTION OF EMBODIMENTS The figure is a sectional view of an embodiment of an ECD manufactured by the method of the present invention. In the figure, 1 is a glass substrate, 2 is a thin film transparent electrode made of indium oxide, tin oxide, etc., and 3 is a display electrode provided on the thin film transparent electrode 2, which is constructed by vapor-depositing tungsten oxide to a thickness of 3000 angstroms. 4 is the back glass substrate,
5 is an alumina reflector, 6 is a counter electrode, 7 is an electrolytic solution (a propylene carbonate solution containing 0.3 MLiBF 4 ), and 8 is a current collector. An insulating film 9 made of SiO 2 or the like is provided on the thin film transparent electrode 2 other than the display electrode 3 . Next, two types of carbon materials, graphite and channel black, were used as the counter electrode, and 10 -4 M,
Cleaning treatment was performed with sulfuric acid aqueous solutions of three different concentrations: 0.01M and 1M. That is, 50 g of carbon was dispersed in 2000 c.c. of sulfuric acid aqueous solution, stirred for 15 hours, washed with a large amount of pure water to remove sulfuric acid, and further dried at 105° C. for 10 hours. Next, each carbon and fluorine resin were mixed at a weight ratio of 1:1, and the mixed powder was pressure-molded onto a stainless steel net current collector, and a counter electrode was used to fabricate an ECD. Table 1 shows the results of investigating the relationship between the amount of quinone groups in carbon after cleaning treatment and the memory performance of the fabricated ECD.
【表】
表１より明らかなように、未洗浄のカーボンを
使用した場合は、メモリー性能が０〜２％にすぎ
ないが、硫酸水溶液で洗浄した場合には、キノン
基量の減少とともに、25％以上のメモリー性能を
得ることができた。
表２は塩酸水溶液または硝酸水溶液で洗浄処理
した場合の結果を示したものであり、硫酸以外の
酸の水溶液を使用した場合でも同様に、メモリー
性能の向上が確認された。尚、ここで使用したチ
ヤンネルブラツクは表１のものとは異なるもので
ある。[Table] As is clear from Table 1, when unwashed carbon is used, the memory performance is only 0-2%, but when washed with sulfuric acid aqueous solution, the amount of quinone groups decreases, and the memory performance decreases by 25%. % or more memory performance was achieved. Table 2 shows the results of cleaning treatment with an aqueous hydrochloric acid solution or an aqueous nitric acid solution, and it was confirmed that memory performance was similarly improved even when an aqueous solution of an acid other than sulfuric acid was used. Note that the channel black used here is different from that in Table 1.
【表】
次に、比表面積が異なる４種の黒鉛と、チヤン
ネルブラツクとを、いずれも1Mの硫酸水溶液で
洗浄処理し、これらのカーボンで作製した対極を
用いたECDを、60℃の恒温槽に保存した場合の
着色電気量の変化度合いを測定した結果を表３に
示す。[Table] Next, four types of graphite with different specific surface areas and channel black were washed with a 1M sulfuric acid aqueous solution, and an ECD using a counter electrode made of these carbons was placed in a constant temperature bath at 60℃. Table 3 shows the results of measuring the degree of change in the amount of colored electricity when stored in .
【表】
表３より明らかなように、比表面積が100m2／
ｇ以上の黒鉛を用いることにより、着色電気量の
保持とメモリー性能の向上が達成されることが判
明した。
発明の効果
以上説明したように、本発明によれば、優れた
メモリー性能を有する商品価値の高いECDを提
供することができる。
尚、本発明は表示材料が酸化タングステンであ
る場合に限定されるものではなく、他の表示体、
たとえば酸化モリブデン単独、酸化タングステン
と酸化モリブデンの混合体等の遷移金属酸化物
や、ビオロゲン等の有機エレクトロクロミツク材
料を使用したECDにも適用されることは言うま
でもない。また、電解液も炭酸プロピレンである
場合に限定されるものではなく、ガンマブチロラ
クトン等を使用したECDにも適用されることは
言うまでもない。[Table] As is clear from Table 3, the specific surface area is 100m 2 /
It has been found that by using graphite with a weight of 1.5 g or more, the amount of coloring electricity can be maintained and the memory performance can be improved. Effects of the Invention As explained above, according to the present invention, it is possible to provide an ECD with excellent memory performance and high commercial value. Note that the present invention is not limited to cases in which the display material is tungsten oxide, and may be applied to other display materials,
It goes without saying that it is also applicable to ECDs using transition metal oxides such as molybdenum oxide alone, a mixture of tungsten oxide and molybdenum oxide, and organic electrochromic materials such as viologen. Further, the electrolytic solution is not limited to propylene carbonate, and it goes without saying that it is also applicable to ECD using gamma-butyrolactone or the like.
図は本願発明方法を実施するエレクトロクロミ
ツク表示装置の断面図である。
１……ガラス基板、２……薄膜透明電極、３…
…表示極、４……背面ガラス基板、５……アルミ
ナ反射板、６……対極、７……電解液、８……集
電体、９……絶縁膜。
The figure is a sectional view of an electrochromic display device implementing the method of the present invention. 1...Glass substrate, 2...Thin film transparent electrode, 3...
... Display electrode, 4 ... Back glass substrate, 5 ... Alumina reflecting plate, 6 ... Counter electrode, 7 ... Electrolyte, 8 ... Current collector, 9 ... Insulating film.
Claims (1)
られた表示極と、カーボンからなる対極とを備え
たエレクトロクロミツク表示装置において、対極
のカーボン材料を、硫酸水溶液、塩酸水溶液、硝
酸水溶液のうちの少なくとも一つで洗浄処理する
ことを特徴とするエレクトロクロミツク表示装置
の対極の製造方法。 ２ カーボンからなる対極の材料が、比表面積が
100m2／ｇ以上の黒鉛であることを特徴とする特
許請求の範囲第１項記載のエレクトロクロミツク
表示装置の対極の製造方法。[Claims] 1. In an electrochromic display device comprising an organic electrolyte, a display electrode provided in contact with the organic electrolyte, and a counter electrode made of carbon, the carbon material of the counter electrode is prepared by using a sulfuric acid aqueous solution, 1. A method for manufacturing a counter electrode of an electrochromic display device, comprising cleaning with at least one of an aqueous hydrochloric acid solution and an aqueous nitric acid solution. 2 The counter electrode material made of carbon has a specific surface area of
A method for producing a counter electrode for an electrochromic display device according to claim 1, wherein the counter electrode is made of graphite with a density of 100 m 2 /g or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59029375A JPS60173524A (en) | 1984-02-18 | 1984-02-18 | Electrochromic display device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59029375A JPS60173524A (en) | 1984-02-18 | 1984-02-18 | Electrochromic display device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60173524A JPS60173524A (en) | 1985-09-06 |
| JPH0519691B2 true JPH0519691B2 (en) | 1993-03-17 |
Family
ID=12274396
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59029375A Granted JPS60173524A (en) | 1984-02-18 | 1984-02-18 | Electrochromic display device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60173524A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6697185B2 (en) | 1999-08-19 | 2004-02-24 | Gentex Corporation | Color-stabilized electrochromic devices |
| US6433914B1 (en) * | 1999-08-19 | 2002-08-13 | Gentex Corporation | Color-stabilized electrochromic devices |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS584119A (en) * | 1981-07-01 | 1983-01-11 | Matsushita Electric Ind Co Ltd | Electrochromic display device |
| JPS58125020A (en) * | 1982-01-21 | 1983-07-25 | Seiko Instr & Electronics Ltd | Electrochemical cell |
-
1984
- 1984-02-18 JP JP59029375A patent/JPS60173524A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS584119A (en) * | 1981-07-01 | 1983-01-11 | Matsushita Electric Ind Co Ltd | Electrochromic display device |
| JPS58125020A (en) * | 1982-01-21 | 1983-07-25 | Seiko Instr & Electronics Ltd | Electrochemical cell |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60173524A (en) | 1985-09-06 |
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