JP3009581B2 - Conductive paint - Google Patents
Conductive paintInfo
- Publication number
- JP3009581B2 JP3009581B2 JP5353948A JP35394893A JP3009581B2 JP 3009581 B2 JP3009581 B2 JP 3009581B2 JP 5353948 A JP5353948 A JP 5353948A JP 35394893 A JP35394893 A JP 35394893A JP 3009581 B2 JP3009581 B2 JP 3009581B2
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- tin
- paint
- indium
- conductive paint
- 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 - Fee Related
Links
Landscapes
- Liquid Crystal (AREA)
- Paints Or Removers (AREA)
- Conductive Materials (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は塗布法によつて帯電防止
フイルム等の透明導電性被膜、更には液晶デイスプレイ
等の透明電極を形成するのに好適な導電性塗料に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a conductive coating which is suitable for forming a transparent conductive film such as an antistatic film and a transparent electrode such as a liquid crystal display by a coating method.
【０００２】[0002]
【従来の技術】太陽電池や液晶デイスプレイ等の透明電
極或いはエレクトロルミネツセンスデイスプレイやタツ
チパネル等の透明導電膜として広く用いられる錫含有酸
化インジウム（ＩＴＯ）膜は一般にスパツタリング法、
真空蒸着法、塗布法等により形成される。その中でも塗
布法はスパツタリング法や真空蒸着法では困難な大面積
或いは複雑な形状への加工が可能であつたり、パターン
形成が容易でコスト的にも有利である。そのような塗布
法として利用されているのは、有機系のゾル・ゲル法が
一般的であるが、近年の微粒子製造技術の発展に伴い、
微粉末を用いてこれを塗布する方法が成膜温度を低く抑
えられ、基材材質の選択自由度を高め、コストも低減で
きる等から注目されている。2. Description of the Related Art A tin-containing indium oxide (ITO) film widely used as a transparent electrode for a solar cell or a liquid crystal display or a transparent conductive film for an electroluminescence display or a touch panel is generally manufactured by a sputtering method.
It is formed by a vacuum deposition method, a coating method, or the like. Among them, the coating method can be processed into a large area or a complicated shape which is difficult by the sputtering method or the vacuum evaporation method, and the pattern formation is easy and the cost is advantageous. Organic sol-gel method is generally used as such a coating method, but with the recent development of fine particle manufacturing technology,
Attention has been paid to the method of applying the fine powder using the fine powder because the film forming temperature can be kept low, the degree of freedom in selecting the material of the base material can be increased, and the cost can be reduced.
【０００３】単に透明導電性被膜を形成するための導電
性微粉末を用いた導電性塗料ということでは、特公昭６
１−９３４３号、特公昭６３−１３４６３号あるいは特
開平４−３６３３６６号などが提案されているが、これ
らは何れも導電性微粉末としては酸化錫あるいはアンチ
モン等異種元素をドープした酸化錫が用いられているた
め、その導電機能は帯電防止の範囲内に止まり、透明性
からも上記用途には充分と言えないものである。また、
ＩＴＯ微粉末を用いた透明導電性塗料としては例えば特
公平２−５５４６１号に錫化合物またはインジウム化合
物の水溶液を８〜12のpＨ条件下加水分解し、コロイド
粒子を含有するゾルを生成させ、該ゾルを乾燥、焼成し
た後粉砕して得られた導電性微粉末を利用するものが提
案されている。しかしながら、この方法ではゾル液から
コロイド粒子を濾別する際に副生塩の除去が容易でなく
導電性の低下を招き易く、また得られた塗膜も透明性が
必ずしも満足のいくものではなく、ヘーズ値も高い等の
問題点を含むものである。[0003] In the case of a conductive paint using a conductive fine powder simply for forming a transparent conductive film, Japanese Patent Publication No.
Nos. 1-9343, JP-B-63-13463 and JP-A-4-363366 have been proposed. In each case, tin oxide doped with a different element such as tin oxide or antimony is used as the conductive fine powder. Therefore, its conductive function remains within the range of antistatic, and its transparency is not sufficient for the above-mentioned applications. Also,
As a transparent conductive paint using ITO fine powder, for example, Japanese Patent Publication No. 2-55461 discloses a method of hydrolyzing an aqueous solution of a tin compound or an indium compound under a pH condition of 8 to 12 to form a sol containing colloid particles. A method using a conductive fine powder obtained by drying, calcining and then pulverizing a sol has been proposed. However, in this method, when the colloid particles are separated from the sol solution by filtration, the by-product salt is not easily removed, and the conductivity is easily reduced.In addition, the obtained coating film is not necessarily satisfactory in transparency. And the haze value is high.
【０００４】[0004]
【発明が解決しようとする課題】本発明の目的は、上記
した問題点を解消し、透明性及び導電性に優れた錫含有
酸化インジウム（ＩＴＯ）膜を形成し得る透明導電性塗
料を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems and to provide a transparent conductive paint capable of forming a tin-containing indium oxide (ITO) film having excellent transparency and conductivity. It is in.
【０００５】[0005]
【課題を解決するための手段】本発明は錫塩及びインジ
ウム塩の溶液に温度を30℃以下に保持しながらアルカリ
水溶液を反応系のｐＨが最終的に５.０〜９.０となるよ
うに、０.５〜１２時間の添加時間で添加して得られた
酸化錫及び酸化インジウムの水和物を加熱処理して得ら
れた導電性錫含有酸化インジウム微粉末、塗料バインダ
ー及び溶媒を含有することを特徴とする導電性塗料に係
る。According to the present invention, an alkaline aqueous solution is added to a solution of a tin salt and an indium salt while maintaining the temperature at 30 ° C. or lower so that the pH of the reaction system finally becomes 5.0 to 9.0. Contains a conductive tin-containing indium oxide fine powder obtained by heat-treating a hydrate of tin oxide and indium oxide obtained by adding for 0.5 to 12 hours, and a paint binder and a solvent. And a conductive paint.
【０００６】本発明において使用するＩＴＯ微粉末は錫
塩及びインジウム塩の溶液に温度を30℃以下に保持しな
がらアルカリ水溶液を添加して得られた酸化錫及び酸化
インジウムの水和物を加熱処理することにより得られ
る。使用する錫塩及びインジウム塩は水溶性のものであ
れば良く、塩化錫、硫酸錫、硝酸錫、塩化インジウム、
硫酸インジウム、硝酸インジウム等が例示でき、又錫塩
は第１錫塩、第２錫塩何れでもよい。そのような錫塩及
びインジウム塩を水に溶解させ、必要によつてはアルコ
ール、アセトン等の水溶性有機溶媒及び／又は塩酸、硝
酸等の鉱酸を加えた後、温度を30℃以下、好ましくは０
〜20℃に保持しながらアルカリ水溶液を添加する。30℃
を超える場合には他の条件にもよるが概して粒度は粗く
なり、針状形状を有するもの、凝集形態を有するものが
生成するようになる。０℃未満にしても特に効果は上が
らず冷却用の冷媒等のコストが上昇してしまう。また、
この場合の錫とインジウムの割合はＳnＯ2：Ｉn2Ｏ3重
量比にて１：99〜20：80、好ましくは４：96〜15：85で
あり、この範囲より錫は多すぎても、少なすぎても所望
とする導電性が得られない。The fine ITO powder used in the present invention is obtained by subjecting a hydrate of tin oxide and indium oxide obtained by adding an aqueous alkali solution to a solution of a tin salt and an indium salt while maintaining the temperature at 30 ° C. or less, by heat treatment. It is obtained by doing. The tin salt and the indium salt used may be any water-soluble ones, such as tin chloride, tin sulfate, tin nitrate, indium chloride,
Examples include indium sulfate and indium nitrate. The tin salt may be either a stannous salt or a stannic salt. After dissolving such a tin salt and an indium salt in water and adding a water-soluble organic solvent such as alcohol and acetone and / or a mineral acid such as hydrochloric acid and nitric acid as necessary, the temperature is preferably 30 ° C. or lower. Is 0
While maintaining the temperature at 2020 ° C., the aqueous alkali solution is added. 30 ℃
When the value exceeds the above, the particle size generally becomes coarse depending on other conditions, and a product having an acicular shape and a product having an aggregated morphology are formed. Even if the temperature is lower than 0 ° C., the effect is not particularly enhanced, and the cost of the cooling refrigerant or the like increases. Also,
In this case, the ratio of tin to indium is 1:99 to 20:80, preferably 4:96 to 15:85 by weight ratio of SnO 2 : In 2 O 3 . If it is too small, the desired conductivity cannot be obtained.
【０００７】このときの濃度は、反応終了時に（ＳnＯ2
＋Ｉn2Ｏ3）濃度にて２〜50g／lの範囲が適当で、２g／
l未満では収量が少なく不経済であり、50g／lを越える
と粒度が粗くなつてしまう。At this time, the concentration at the end of the reaction (SnO 2
+ In 2 O 3 ) concentration in the range of 2 to 50 g / l is appropriate, and 2 g /
If it is less than 1 liter, the yield is small and uneconomical, and if it exceeds 50 g / l, the particle size becomes coarse.
【０００８】アルカリ水溶液としては、アンモニア水、
水酸化アルカリ、炭酸アルカリ、炭酸アンモニウム等の
水溶液を例示できるが、導電性を阻害する成分を含むア
ルカリ金属塩は適当でなく、アンモニア水及びアンモニ
ウム塩水溶液が好ましい。そして、そのようなアルカリ
水溶液を最終的にpＨが5.0〜9.0となるように添加する
ことにより酸化錫及び酸化インジウムの水和物が生成す
る。pＨが5.0未満では反応が不完全であり、又、pＨが
9.0を越えると逆に一部生成物の解膠が起き、何れもそ
の後の加熱処理工程での焼結を招き粗大粒子が生成して
しまう。As the alkaline aqueous solution, ammonia water,
Aqueous solutions such as alkali hydroxide, alkali carbonate, and ammonium carbonate can be exemplified, but alkali metal salts containing a component that inhibits conductivity are not suitable, and aqueous ammonia and aqueous ammonium salts are preferred. Then, a hydrate of tin oxide and indium oxide is formed by adding such an alkaline aqueous solution so that the pH finally becomes 5.0 to 9.0. If the pH is less than 5.0, the reaction is incomplete.
On the other hand, if it exceeds 9.0, deflocculation of a part of the product occurs, and in any case, sintering is caused in the subsequent heat treatment step, and coarse particles are generated.
【０００９】又、アルカリ水溶液の添加時間は特に限定
するものではないが、30分から12時間程度が好ましく、
30分未満では生成物がゲル状となり濾過洗浄が困難とな
る上、後の加熱処理工程での焼結を招く。12時間以上の
添加時間は生産性が低下する上、粒度も粗くなつてく
る。The addition time of the aqueous alkali solution is not particularly limited, but is preferably about 30 minutes to 12 hours.
If the time is less than 30 minutes, the product will be in a gel state, which will be difficult to filter and wash, and will cause sintering in the subsequent heat treatment step. If the addition time is longer than 12 hours, the productivity decreases and the particle size becomes coarse.
【００１０】以上のような条件により、一次粒子径0.01
5〜0.05μm程度の酸化錫及び酸化インジウムの水和物が
生成する。本発明では、該水和物を必要によつては副生
してくる塩を除去した後に乾燥、更に300〜1200℃、好
ましくは500〜1000℃にて加熱処理することにより目的
とする錫含有酸化インジウム微粉末を得ることができ
る。この場合、必要に応じてＮ2，Ａr等の不活性ガス雰
囲気或いはＨ2，ＮＨ3等の還元雰囲気中にて処理するこ
とにより導電性は更に向上する。得られるＩＴＯ微粉末
は、水和物として生成する段階で従来法がコロイド粒子
であるのに対し、既に0.015〜0.05μｍ程度の一次粒子
としての形骸を有しており、その後の乾燥、加熱処理の
過程で焼結を招くことはなく結晶化されるため、粗大粒
子を含まない均一な粒度を有する微粉末である。Under the above conditions, the primary particle size is 0.01
A hydrate of tin oxide and indium oxide of about 5 to 0.05 μm is formed. In the present invention, the desired tin-containing substance is obtained by removing the salt produced as a by-product if necessary, drying the hydrate, and further heat-treating the hydrate at 300 to 1200 ° C, preferably 500 to 1000 ° C. Indium oxide fine powder can be obtained. In this case, if necessary, the conductivity is further improved by performing the treatment in an inert gas atmosphere such as N 2 or Ar or a reducing atmosphere such as H 2 or NH 3 . The obtained ITO fine powder has a form as a primary particle of about 0.015 to 0.05 μm, whereas the conventional method is a colloidal particle at the stage of being formed as a hydrate, and is subsequently dried and heated. This is a fine powder having a uniform particle size that does not include coarse particles because it is crystallized without causing sintering in the process.
【００１１】本発明で用いる塗料バインダーとしては、
通常の塗料技術により使用できる樹脂であればよく、例
えば、アクリル系、ビニル系、カーボネート系、ポリエ
ステル系、ウレタン系、エポキシ系、ポリプロピレン
系、フエノール系、ポリアミド系、ポリイミド系樹脂等
が挙げられる。又、これら樹脂の混合物あるいは共重合
体でもよい。The paint binder used in the present invention includes:
Any resin can be used as long as it can be used by ordinary coating techniques, and examples thereof include acrylic, vinyl, carbonate, polyester, urethane, epoxy, polypropylene, phenol, polyamide, and polyimide resins. Further, a mixture or a copolymer of these resins may be used.
【００１２】ＩＴＯ微粉末の含有量は、導電性塗料の固
形分中 40〜95重量％となるように混合されることが好
ましい。ＩＴＯ微粉末が40重量％未満では得られる塗膜
の導電性が充分でなく、95重量％を超えると分散が悪く
なり塗膜の透明性及び基材との密着性が損なわれてしま
う。The content of the ITO fine powder is preferably mixed so as to be 40 to 95% by weight based on the solid content of the conductive paint. If the ITO fine powder is less than 40% by weight, the conductivity of the coating film obtained is not sufficient, and if it exceeds 95% by weight, the dispersion is poor and the transparency of the coating film and the adhesion to the substrate are impaired.
【００１３】本発明の導電性塗料はＩＴＯ微粉末と塗料
バインダーとを溶剤中に分散あるいは溶解させることに
より得ることができる。溶剤としては、塗料バインダー
を溶解し得るものであれば使用でき、メタノール、エタ
ノール、ｎ−プロパノール、ｉ−プロパノール、ｎ−ブ
タノール、シクロヘキサノール等のアルコール類、アセ
トン、メチルエチルケトン、シクロヘキサノン等のケト
ン類、メチルセロソルブ、エチルセロソルブ等のエーテ
ル類、酢酸エチル、メチルセロソルブアセテート等のエ
ステル類、ヘキサン、シクロヘキサン、トルエン、キシ
レン等が例示できる。又、水溶性樹脂を用いた場合には
溶剤として水を用いることもできる。これら溶剤の使用
割合は特に限定するものではなく、使用目的に応じ設定
すればよいが、分散、粘度等を考慮し塗料中の固形分が
10〜90重量％となるようにすることが好ましい。The conductive paint of the present invention can be obtained by dispersing or dissolving a fine ITO powder and a paint binder in a solvent. As the solvent, any solvent can be used as long as it can dissolve the paint binder.Methanol, ethanol, n-propanol, i-propanol, n-butanol, alcohols such as cyclohexanol, acetone, methyl ethyl ketone, ketones such as cyclohexanone, Examples thereof include ethers such as methyl cellosolve and ethyl cellosolve, esters such as ethyl acetate and methyl cellosolve acetate, hexane, cyclohexane, toluene and xylene. When a water-soluble resin is used, water can be used as a solvent. The use ratio of these solvents is not particularly limited, and may be set according to the purpose of use.
It is preferable that the content be 10 to 90% by weight.
【００１４】本発明の導電性塗料の調製は上記したＩＴ
Ｏ微粉末、塗料バインダー及び溶剤を通常用いられるボ
ールミル、サンドミル、ペイントシエーカー、３本ロー
ルなどにて混合することにより行われる。又、その際分
散性を向上させる目的でシラン系あるいはチタネート系
等のカツプリング剤や界面活性剤などを添加してもよ
い。The preparation of the conductive paint of the present invention is carried out by using the above-described IT.
This is carried out by mixing O fine powder, a paint binder and a solvent with a commonly used ball mill, sand mill, paint shaker, three rolls or the like. In this case, a silane-based or titanate-based coupling agent or a surfactant may be added for the purpose of improving dispersibility.
【００１５】以上のようにして調製された本発明の導電
性塗料はスプレー法、バーコート法、デイツピング法、
ドクターブレード法などの塗布方法により基材に塗布さ
れ、乾燥あるいは必要によつては加熱処理することによ
つて実用に供される。[0015] The conductive paint of the present invention prepared as described above is prepared by spraying, bar coating, dipping,
It is applied to a substrate by an application method such as a doctor blade method, and is put to practical use by drying or, if necessary, heat treatment.
【００１６】[0016]
【実施例】以下に実施例を挙げて説明するが、本発明は
これに限定されるものではない。The present invention will be described below with reference to examples, but the present invention is not limited to these examples.
【００１７】実施例１ 塩化第２錫（ＳnＣl4・５Ｈ2Ｏ）5.9g及び塩化インジウ
ム（ＩnＣl3）75.9gを水4000mlに溶解し、これに２％ア
ンモニア水を58分かけて添加しpＨを最終的に7.85とす
ることにより酸化錫及び酸化インジウムの水和物を共沈
させた。この間、液温は５℃を維持するようにした。次
いで、該共沈物を洗浄後乾燥、更に900℃にて２時間焼
成することにより、一次粒子径約0.02μmと微細でかつ
粗大粒子を含まない均一粒度を有する錫含有酸化インジ
ウム（ＩＴＯ）微粉末を得た。該ＩＴＯ微粉末 40g、ポ
リエステル樹脂 ８g、（トルエン−ＭＥＫ−酢酸エチ
ル）混合溶剤 50g、及びノニオン系界面活性剤 １gをジ
ルコニアビーズを分散メデイアとするペイントコンデイ
シヨナーにて８時間混合し、透明導電性塗料を調製し
た。EXAMPLE 1 5.9 g of stannic chloride (SnCl 4 .5H 2 O) and 75.9 g of indium chloride (InCl 3 ) were dissolved in 4000 ml of water, and 2% aqueous ammonia was added thereto over 58 minutes to adjust the pH. Was finally set to 7.85 to coprecipitate a hydrate of tin oxide and indium oxide. During this time, the liquid temperature was kept at 5 ° C. Next, the coprecipitate is washed, dried and further calcined at 900 ° C. for 2 hours to obtain a tin-containing indium oxide (ITO) fine particle having a primary particle diameter of about 0.02 μm and a uniform particle size that is fine and does not include coarse particles. A powder was obtained. The ITO fine powder (40 g), polyester resin (8 g), (toluene-MEK-ethyl acetate) mixed solvent (50 g), and nonionic surfactant (1 g) were mixed for 8 hours by a paint conditioner using zirconia beads as a dispersion medium, and then a transparent conductive material was mixed. A water-soluble paint was prepared.
【００１８】実施例２ 実施例１と同様にして得られたＩＴＯ微粉末 40g、ポリ
アミド樹脂 ８g、（トルエン−ｉ−プロパノール）混合
溶剤 50g、及びノニオン系界面活性剤 １gをジルコニア
ビーズを分散メデイアとするペイントコンデイシヨナー
にて８時間混合し、透明導電性塗料を調製した。Example 2 40 g of the fine ITO powder obtained in the same manner as in Example 1, 8 g of a polyamide resin, 50 g of a mixed solvent of (toluene-i-propanol), and 1 g of a nonionic surfactant were mixed with zirconia beads as a dispersion medium. The mixture was mixed for 8 hours with a paint conditioner to prepare a transparent conductive paint.
【００１９】実施例３ 塩化第１錫（ＳnＣl2・２Ｈ2Ｏ）3.9g及び硝酸インジウ
ム〔Ｉn（ＮＯ3）3・３Ｈ2Ｏ〕121.6gを水4000mlに溶解
し、これに２％アンモニア水を73分かけて添加しpＨを
最終的に7.80とすることにより酸化錫及び酸化インジウ
ムの水和物を共沈させた。この間、液温は20℃を維持す
るようにした。次いで該共沈物を洗浄後乾燥、更に900
℃にて２時間焼成し、一次粒子径約0.035μmと微細でか
つ粗大粒子を含まない均一粒度を有するＩＴＯ微粉末を
得た。該ＩＴＯ微粉末 40g、ウレタン樹脂 ８g、（キシ
レ−酢酸ブチル）混合溶剤 50g、及びノニオン系界面活
性剤 １gをジルコニアビーズを分散メデイアとするペイ
ントコンデイシヨナーにて８時間混合し、透明導電性塗
料を調製した。EXAMPLE 3 3.9 g of stannous chloride (SnCl 2 .2H 2 O) and 121.6 g of indium nitrate [In (NO 3 ) 3 .3H 2 O] were dissolved in 4000 ml of water, and 2% aqueous ammonia was added thereto. Was added over 73 minutes to finally adjust the pH to 7.80, thereby co-precipitating a hydrate of tin oxide and indium oxide. During this time, the liquid temperature was maintained at 20 ° C. Next, the coprecipitate was washed, dried, and further 900
C. for 2 hours to obtain an ITO fine powder having a primary particle size of about 0.035 .mu.m and having a fine particle size and a uniform particle size without coarse particles. 40 g of the ITO fine powder, 8 g of urethane resin, 50 g of a mixed solvent of (xylene-butyl acetate), and 1 g of nonionic surfactant were mixed for 8 hours by a paint conditioner using zirconia beads as a dispersion medium, and then a transparent conductive paint Was prepared.
【００２０】実施例４ 塩化第２錫（ＳnＣl4・５Ｈ2Ｏ）5.9g及び塩化インジウ
ム（ＩnＣl3）75.9gを水4000mlに溶解し、これに4.5％
ＮＨ4ＨＣＯ3水溶液を360分かけて添加しpＨを最終的に
5.8とすることにより酸化錫及び酸化インジウムの水和
物を共沈させた。この間、液温は25℃を維持するように
した。次いで該共沈物を洗浄後乾燥、更に700℃にて２
時間焼成し、一次粒子径約0.045μmと微細でかつ粗大粒
子を含まない均一粒度を有するＩＴＯ微粉末を得た。該
ＩＴＯ微粉末を用い、実施例１と同様にして透明導電性
塗料を調製した。Example 4 5.9 g of stannic chloride (SnCl 4 .5H 2 O) and 75.9 g of indium chloride (InCl 3 ) were dissolved in 4000 ml of water, and 4.5%
NH 4 HCO 3 aqueous solution is added over 360 minutes to finally adjust pH.
By setting to 5.8, a hydrate of tin oxide and indium oxide was coprecipitated. During this time, the liquid temperature was kept at 25 ° C. Next, the coprecipitate is washed, dried, and further dried at 700 ° C. for 2 hours.
After baking for an hour, an ITO fine powder having a primary particle diameter of about 0.045 μm and a uniform particle size that is fine and does not include coarse particles was obtained. Using this ITO fine powder, a transparent conductive paint was prepared in the same manner as in Example 1.
【００２１】比較例１ 液温を35℃に維持する以外は実施例１と同様にしてＩＴ
Ｏ微粉末を得た。該微粉末は短軸径0.05〜0.07μm、長
軸径0.30〜0.35μmの針状形状を有していた。該微粉末
を用い、実施例１と同様にして導電性塗料を調製した。Comparative Example 1 The procedure of Example 1 was repeated except that the liquid temperature was maintained at 35 ° C.
O fine powder was obtained. The fine powder had a needle shape with a minor axis diameter of 0.05 to 0.07 μm and a major axis diameter of 0.30 to 0.35 μm. Using the fine powder, a conductive paint was prepared in the same manner as in Example 1.
【００２２】比較例２ pＨを最終的に4.5とする以外は実施例１と同様にしてＩ
ＴＯ微粉末を得た。該微粉末は粗大粒子を多く含むもの
であつた。該微粉末を用い、実施例１と同様にして導電
性塗料を調製した。Comparative Example 2 The procedure of Example 1 was repeated except that the pH was finally adjusted to 4.5.
TO fine powder was obtained. The fine powder contained a large amount of coarse particles. Using the fine powder, a conductive paint was prepared in the same manner as in Example 1.
【００２３】比較例３ pＨを最終的に9.5とする以外は実施例１と同様にしてＩ
ＴＯ微粉末を得た。該微粉末は比較例２と同様粗大粒子
を多く含むものであつた。該微粉末を用い、実施例１と
同様にして導電性塗料を調製した。Comparative Example 3 The procedure of Example 1 was repeated except that the pH was finally adjusted to 9.5.
TO fine powder was obtained. The fine powder contained a large amount of coarse particles as in Comparative Example 2. Using the fine powder, a conductive paint was prepared in the same manner as in Example 1.
【００２４】比較例４ 添加時間を20分とする以外は実施例１と同様にしてＩＴ
Ｏ微粉末を得た。該微粉末は比較例２と同様粗大粒子を
多く含むものであつた。該微粉末を用い、実施例１と同
様にして導電性塗料を調製した。Comparative Example 4 The procedure of Example 1 was repeated except that the addition time was changed to 20 minutes.
O fine powder was obtained. The fine powder contained a large amount of coarse particles as in Comparative Example 2. Using the fine powder, a conductive paint was prepared in the same manner as in Example 1.
【００２５】試験例１ 実施例１〜４及び比較例１〜４で調製した各塗料をポリ
エステルシート上に１milのドクターブレードを用いて
塗布し、常温乾燥して塗膜を得た。各塗膜の表面抵抗値
をロレスタＦＰ（三菱油化製）にて、全光線透過率及び
ヘーズ値をヘーズメーター（日本電色製）にてそれぞれ
測定した結果を表１に示す。Test Example 1 Each coating material prepared in Examples 1 to 4 and Comparative Examples 1 to 4 was applied to a polyester sheet using a 1 mil doctor blade and dried at room temperature to obtain a coating film. Table 1 shows the results obtained by measuring the surface resistance of each coating film with Loresta FP (manufactured by Mitsubishi Yuka) and the total light transmittance and haze value using a haze meter (manufactured by Nippon Denshoku).
【００２６】[0026]
【表１】 [Table 1]
【００２７】[0027]
【発明の効果】本発明の導電性塗料は、粗大粒子を含ま
ない均一な粒度を有するＩＴＯ微粉末を導電性成分とし
ているため、これを用いて形成された塗膜は透明性及び
導電性に優れ、帯電防止被膜、更には透明電極や透明導
電膜として有用である。As described above, the conductive paint of the present invention uses ITO fine powder having a uniform particle size without coarse particles as a conductive component, so that a coating film formed by using the same has transparency and conductivity. It is excellent and is useful as an antistatic coating, furthermore, as a transparent electrode or a transparent conductive film.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ // Ｇ０２Ｆ 1/1343 Ｇ０２Ｆ 1/1343 (72)発明者 金沢 吉十郎 兵庫県神戸市北区道場町生野96番地の１ 富士チタン工業株式会社神戸研究所内 (56)参考文献 特開 平２−120374（ＪＰ，Ａ) 特開 昭62−7627（ＪＰ，Ａ) 特公 平２−55461（ＪＰ，Ｂ２) (58)調査した分野(Int.Cl.7，ＤＢ名) C09D 5/24 C09D 7/12 ────────────────────────────────────────────────── ─── Continued on the front page (51) Int.Cl. 7 Identification symbol FI // G02F 1/1343 G02F 1/1343 (72) Inventor Yoshijuro Kanazawa 96-1, Ikuno, Dojo-cho, Kita-ku, Kobe-shi, Hyogo Fuji (56) References JP-A-2-120374 (JP, A) JP-A-62-2627 (JP, A) JP-B-2-55461 (JP, B2) (58) Field (Int.Cl. 7 , DB name) C09D 5/24 C09D 7/12
Claims (1)
℃以下に保持しながらアルカリ水溶液を反応系のｐＨが
最終的に５.０〜９.０となるように、０.５〜１２時間
の添加時間で添加して得られた酸化錫及び酸化インジウ
ムの水和物を加熱処理して得られた導電性錫含有酸化イ
ンジウム微粉末、塗料バインダー及び溶媒を含有するこ
とを特徴とする導電性塗料。1. The temperature of the tin salt and indium salt solution is adjusted to 30.
While maintaining the temperature below ℃, the pH of the reaction system
0.5 to 12 hours so that the final value is 5.0 to 9.0
A conductive tin-containing indium oxide fine powder obtained by heat-treating a hydrate of tin oxide and indium oxide obtained by adding at a time of addition, a paint binder and a solvent. paint.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5353948A JP3009581B2 (en) | 1993-12-27 | 1993-12-27 | Conductive paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5353948A JP3009581B2 (en) | 1993-12-27 | 1993-12-27 | Conductive paint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07188593A JPH07188593A (en) | 1995-07-25 |
| JP3009581B2 true JP3009581B2 (en) | 2000-02-14 |
Family
ID=18434296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5353948A Expired - Fee Related JP3009581B2 (en) | 1993-12-27 | 1993-12-27 | Conductive paint |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3009581B2 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1169015C (en) | 1996-05-15 | 2004-09-29 | 精工爱普生株式会社 | Thin film device having coating film, liquid crystal panel, and method of manufacturing thin film device |
| DE19757542A1 (en) * | 1997-12-23 | 1999-06-24 | Bayer Ag | Screen printing paste for e.g. liquid crystal display |
| WO2000059040A1 (en) | 1999-03-30 | 2000-10-05 | Seiko Epson Corporation | Method of manufacturing thin-film transistor |
| JP4559581B2 (en) * | 2000-03-22 | 2010-10-06 | 富士チタン工業株式会社 | Tin-containing indium oxide fine particle powder and method for producing the same |
| WO2006093398A1 (en) * | 2005-03-04 | 2006-09-08 | Inktec Co., Ltd. | Conductive inks and manufacturing method thereof |
| JP2007186352A (en) * | 2006-01-11 | 2007-07-26 | Idemitsu Kosan Co Ltd | Method for producing oxide particles |
| JP2008285378A (en) * | 2007-05-18 | 2008-11-27 | Idemitsu Kosan Co Ltd | Conductive metal oxide powder, method for producing the same, and sintered body |
| CN101984371B (en) * | 2010-08-24 | 2012-05-30 | 深圳市中显微电子有限公司 | A method for reducing electric corrosion of liquid crystal display module |
-
1993
- 1993-12-27 JP JP5353948A patent/JP3009581B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07188593A (en) | 1995-07-25 |
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