JPH0465112B2 - - Google Patents
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- Publication number
- JPH0465112B2 JPH0465112B2 JP60178934A JP17893485A JPH0465112B2 JP H0465112 B2 JPH0465112 B2 JP H0465112B2 JP 60178934 A JP60178934 A JP 60178934A JP 17893485 A JP17893485 A JP 17893485A JP H0465112 B2 JPH0465112 B2 JP H0465112B2
- Authority
- JP
- Japan
- Prior art keywords
- weight
- coating composition
- transparent conductive
- conductive coating
- fine powder
- 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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- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Conductive Materials (AREA)
Description
（発明の利用分野）
本発明は、透明導電性被覆組成物に関し、詳し
く述べると、ポリオレフイン、ポリエステル、ア
クリル樹脂、ポリウレタン等の透明樹脂フイルム
の表面に被覆し、透明かつ良好な導電性を有する
フイルムを製造するのに適した透明導電性被覆組
成物を提供するものである。
（従来の技術）
近年、半導体の生産量の増加に伴い、半導体ウ
エハーの運搬容器や保存容器、クリーンルームや
バイオクリーンルームにおける床材、壁材、カー
テン等に導電性塗料を塗布して帯電防止機能を付
与し、静電気による半導体の破壊の防止や、床、
壁、カーテン等クリーンルーム内への塵埃の付着
の防止等が行われている。
これらの目的のため、従来は、カーボン粉末や
金属粉末を合成樹脂フイルムに練り込んだり、又
はこれらの導電性物質を混入して導電性を持たせ
た塗料を塗布して、不導体の帯電を防止すること
が広く行われている。
しかしながら、カーボンブラツクや金属微粉末
を合成樹脂に練り込んで得られるフイルムは、透
明性が悪く包装した後にその内容物を見ることが
できない、容器内の半導体ウエハーの個数を光セ
ンサーでカウントしようとしてもできない、ある
いはクリーンルーム内のカーテン越しに向う側の
様子を見ることができない等の問題があつた。
一方、導電性物質を混入してなる導電性塗料に
おいては、塗膜の色調が灰色または黒色がかるた
め、被塗物の色調を損うことになり好ましくなか
つた。又、この種の塗料の塗布には、グラビアプ
リンターが使用されることが多いが、印刷適性が
劣るという問題もあつた。
このような導電性塗料の問題を解決しようとす
る試みがなされ、例えば、(1)粒系0.2μｍ以下の導
電性微粉末を塗膜主要素たる樹脂との割合で５〜
50重量％含有したことを特徴とする導電性塗料
（特開昭57−85866公報参照）(2)粒径0.4μｍ以下の
平均粒径をもつ導電性微粉末を、塗膜主要素たる
樹脂との割合で５〜90重量％含有したことを特徴
とするが、いずれも、導電性微粉末の粒径及びそ
の配合量を特定の数値で規定し、その組合せによ
り透明性を有し塗膜密着性にも優れる透明導電性
塗料を得るというものである。
しかし、これらの透明導電性塗料の使用では、
透明性がある程度改善されるが、まだ十分とは言
えないもであり、又、必要な導電性を維持するた
めには、多量の導電性微粉末の添加が必要であ
り、該微粉末の分散安定性に問題があつた。
（発明が解決しようとする問題点）
本発明の目的は、前記従来の導電性透明塗料で
は不十分であつた塗膜の透明性を改良し、かつ導
電性を付与するために多量の金属酸化物の微粉末
を配合しても安定であり、またグラビア印刷適性
にも優れる透明導電性被膜組成物を提供すること
にある。
（問題を解決するための手段）
本発明を概説すると、(a)１〜10重量％のビニル
アルコール単位を含有し、かつ塩化ビニル単位が
80重量％以上である塩化ビニル−酢酸ビニル共重
合体ケン化物35〜15重量部、(b)導電性金属酸化物
の微粉末65〜85重量部(c)極性有機溶剤よりなり、
分散状態における金属酸化物の微粉末の粒径が二
次凝集物として0.1〜1.0μｍの範囲にある透明導
電性被覆組成物である。
本発明をより詳細に説明すると(a)成分としてこ
の特定の塩化ビニル−酢酸ビニル共重合体ケン化
物を使用するのは、導電性機能を付与する金属酸
化物の微粉末との親和力が大きく分散性に優れる
ためであり、該金属酸化物の沈降が少なく安定し
た分散体を得るためである。
本発明では前記のように、１〜10重量％のビニ
ルアルコール単位を含有し、かつ塩化ビニル単位
が80重量％以上である塩化ビニル−酢酸ビニル共
重合体ケン化物を使用する。該ケン化物は、酢酸
ビニル単位の完全ケン化物及び部分ケン化物をい
うが、酢酸ビニル単位が存在することが塗膜形成
上望ましい。
これは、分子中にビニルアルコールを含有しな
い場合は、金属酸化物の微粉末の分散性に劣り、
導電性塗膜の透明性の低下や分散体の安定性が劣
るためである。一方、分子中のビニルアルコール
単位が重量％として10％を越えると塗膜の耐薬品
性、耐水性が劣り、又、吸湿性を示しコーテイン
グ剤として好ましくない傾向を示す。これらの変
性塩化ビニル−酢酸ビニル共重合体ケン化物は、
市販品として入手できる。
(b)成分として金属酸化物は、導電性を付与する
際に一般的に使用される酸化錫、酸化アンチモン
及び酸化インジウムから選ばれた少なくとも一種
の微粉末を使用する。該微粉末の粒径は小さいほ
ど塗膜の透明性が優れるため好ましいが(a)成分に
分散させた場合にその粒径が二次凝集物として
0.1〜1.0μｍとなるものが透明性、安定性いずれ
にも優れ好ましい。
この金属酸化物の微粉末の添加量は、前記塩化
ビニル−酢酸ビニル共重合体ケン化物35〜15重量
部に対し、65〜85重量部の割合であり、このよう
な多量の金属酸化物の微粉末の配合量であるにも
かかわらず、該塩化ビニル−酢酸ビニル共重合体
ケン化物を使用することにより、分散安定性に優
れた組成物を得ることが可能になつたのである。
この配合量は、導電性塗膜の表面固有抵抗を
105Ω／□〜107／□の領域に保つために必要であ
り、65重量部より少ないと、表面抵抗が増し十分
な帯電防止機能が発揮されず、一方85重量部より
多くなると透明性が悪くなり、又被覆剤として要
求される塗膜の物理的性質、例えば、密着力、柔
軟性等が劣り好ましくない。
(c)成分として前記塩化ビニル−酢酸ビニル共重
合体ケン化物を溶解する有機溶剤は、酢酸エチ
ル、酢酸ブチル等のエステル系、メチルエチルケ
トン、メチルイソブチルケトン、アセトン、シク
ロヘキサノン等のケトン系、ジオキサン等ののエ
ーテル系、エチレンジクロライド等のハロゲン化
炭化水素等の溶解パラメーターが10〜13である極
性溶剤が使用できる。
本発明の透明導電性被覆組成物は、一例を挙げ
ると次のような方法で調製する。
まず、塩化ビニル−酢酸ビニル共重合体ケン化
物を極性有機溶剤で溶解し、これに金属酸化物の
微粉末を添加し、十分に混合分散することにより
得られる。本発明の被覆組成物は、(a)成分及び(b)
成分を固形分として固形分10〜40重量％の範囲で
使用でき、塗膜及び塗布手段に合わせて適当な固
形分濃度に調製して使用する。
混合手段としては、ボールミル、ダイノミル、
ホモジナイザー、ペイントシエーカー等が使用で
きる。又、本発明の被覆組成物の塗装手段として
は、グラビアプリンター、ロールコーター、ドク
ターナイフコーター、バーコーター、はけ塗り、
スプレー塗装等の方法が使用できる。
（実施例）
以下、本発明をより具体的に説明するために実
施例を示す。
実施例 １
分子中にビニルアルコール単位２重量％を有す
る塩化ビニル−酢酸ビニル共重合体ケン化物（商
品名 MPR−TA 日信化学工業社製）22部、
メチルエチルケトン／シクロヘキサノン＝６：４
（重量部）の混合溶剤300部を仕込み撹拌し溶解さ
せた後、平均粒径0.1μｍの酸化アンチモンドープ
の酸化錫微粉末（商品名Ｔ−１ 三菱金属社製）
78部を徐々に添加し混合した後、これをペイント
シエーカに移し、30分間分散して透明導電性被膜
組成物を調製した。
比較例 １
実施例１と同様の方法において、ヒドロキシ基
を含有しない塩化ビニル−酢酸ビニル（90重量％
〜10重量％）共重合体を使用する以外はすべて同
じ方法で透明導電性被覆組成物を調製した。
実施例２〜３及び比較例２〜３
実施例１の方法において、塩化ビニル−酢酸ビ
ニル共重合体ケン化物と酸化スズ微粉末との配合
割合を第１表に示す割合とする他は、すべて同じ
方法で透明導電性被覆組成物を調製した。
(Field of Application of the Invention) The present invention relates to a transparent conductive coating composition, and more specifically, the present invention relates to a transparent conductive coating composition, which is coated on the surface of a transparent resin film such as polyolefin, polyester, acrylic resin, polyurethane, etc., and which is transparent and has good conductivity. The present invention provides a transparent conductive coating composition suitable for manufacturing. (Conventional technology) In recent years, with the increase in semiconductor production, conductive paint has been applied to containers for transporting and storing semiconductor wafers, as well as flooring, wall materials, curtains, etc. in clean rooms and bio-clean rooms to provide antistatic properties. It can be applied to prevent semiconductors from being destroyed by static electricity, and to protect floors,
Measures are being taken to prevent dust from adhering to walls, curtains, etc. inside the clean room. For these purposes, conventionally, carbon powder or metal powder was kneaded into a synthetic resin film, or conductive paint was applied by mixing these conductive substances to prevent the non-conductor from being charged. Prevention is widely practiced. However, the film obtained by kneading carbon black and fine metal powder into synthetic resin has poor transparency, making it impossible to see the contents after packaging. There were problems such as not being able to do this, or being unable to see what was happening on the other side through the curtains inside the clean room. On the other hand, in the case of a conductive paint containing a conductive substance, the color tone of the coating film becomes gray or blackish, which impairs the color tone of the object to be coated, which is not preferable. Additionally, gravure printers are often used to apply this type of paint, but there is also the problem of poor printability. Attempts have been made to solve this problem of conductive paints.
Conductive paint characterized by containing 50% by weight (see JP-A-57-85866). The particle size of the conductive fine powder and its blending amount are specified by specific values, and the combination provides transparency and adhesion of the coating film. The objective is to obtain a transparent conductive paint with excellent properties. However, with the use of these transparent conductive paints,
Transparency is improved to some extent, but it is still not sufficient, and in order to maintain the necessary conductivity, it is necessary to add a large amount of conductive fine powder, and it is difficult to disperse the fine powder. There was a problem with stability. (Problems to be Solved by the Invention) The purpose of the present invention is to improve the transparency of the coating film, which was insufficient with the conventional conductive transparent paint, and to add a large amount of metal oxidation to impart conductivity. It is an object of the present invention to provide a transparent conductive coating composition which is stable even when a fine powder of a substance is mixed therein, and which has excellent suitability for gravure printing. (Means for Solving the Problems) To summarize the present invention, (a) it contains 1 to 10% by weight of vinyl alcohol units, and contains vinyl chloride units;
35 to 15 parts by weight of a saponified vinyl chloride-vinyl acetate copolymer having an amount of 80% by weight or more, (b) 65 to 85 parts by weight of a fine conductive metal oxide powder, and (c) a polar organic solvent.
This is a transparent conductive coating composition in which the particle size of the metal oxide fine powder in a dispersed state is in the range of 0.1 to 1.0 μm as secondary aggregates. To explain the present invention in more detail, the reason why this specific saponified vinyl chloride-vinyl acetate copolymer is used as component (a) is that it has a high affinity with the fine powder of metal oxide that imparts conductive function and is dispersed. This is for the purpose of obtaining a stable dispersion with less precipitation of the metal oxide. As described above, the present invention uses a saponified vinyl chloride-vinyl acetate copolymer containing 1 to 10% by weight of vinyl alcohol units and 80% by weight or more of vinyl chloride units. The saponified product refers to a completely saponified product or a partially saponified product of vinyl acetate units, and the presence of vinyl acetate units is desirable from the viewpoint of coating film formation. This is because if the molecule does not contain vinyl alcohol, the dispersibility of metal oxide fine powder is poor,
This is because the transparency of the conductive coating film is reduced and the stability of the dispersion is poor. On the other hand, if the vinyl alcohol unit in the molecule exceeds 10% by weight, the coating film will have poor chemical resistance and water resistance, and will tend to be hygroscopic, making it undesirable as a coating agent. These modified vinyl chloride-vinyl acetate copolymer saponified products are
Available as a commercial product. As the metal oxide for component (b), at least one fine powder selected from tin oxide, antimony oxide, and indium oxide, which are commonly used to impart conductivity, is used. The smaller the particle size of the fine powder, the better the transparency of the coating film, so it is preferable, but when it is dispersed in component (a),
Those having a diameter of 0.1 to 1.0 μm are preferable because they are excellent in both transparency and stability. The amount of this metal oxide fine powder added is 65 to 85 parts by weight to 35 to 15 parts by weight of the saponified vinyl chloride-vinyl acetate copolymer. By using the saponified vinyl chloride-vinyl acetate copolymer, it has become possible to obtain a composition with excellent dispersion stability, even though the amount is a fine powder. This amount increases the surface resistivity of the conductive coating.
It is necessary to maintain the resistance within the range of 10 5 Ω/□ to 10 7 /□. If it is less than 65 parts by weight, the surface resistance will increase and sufficient antistatic function will not be exhibited, while if it is more than 85 parts by weight, transparency will decrease. Moreover, the physical properties of the coating film required as a coating material, such as adhesion and flexibility, are unfavorable. The organic solvent for dissolving the vinyl chloride-vinyl acetate copolymer saponified product as component (c) is an ester type such as ethyl acetate or butyl acetate, a ketone type such as methyl ethyl ketone, methyl isobutyl ketone, acetone, or cyclohexanone, or a ketone type such as dioxane. Polar solvents having a solubility parameter of 10 to 13, such as ethers and halogenated hydrocarbons such as ethylene dichloride, can be used. The transparent conductive coating composition of the present invention is prepared by the following method, for example. First, a saponified vinyl chloride-vinyl acetate copolymer is dissolved in a polar organic solvent, a fine powder of a metal oxide is added thereto, and the mixture is thoroughly mixed and dispersed. The coating composition of the present invention comprises (a) component and (b)
The components can be used in a solid content range of 10 to 40% by weight, and are adjusted to an appropriate solid content concentration depending on the coating film and application method. As mixing means, ball mill, dyno mill,
A homogenizer, paint shaker, etc. can be used. In addition, the coating composition of the present invention can be applied using a gravure printer, a roll coater, a doctor knife coater, a bar coater, a brush coating,
Methods such as spray painting can be used. (Examples) Examples will be shown below to more specifically explain the present invention. Example 1 22 parts of saponified vinyl chloride-vinyl acetate copolymer having 2% by weight of vinyl alcohol units in the molecule (trade name: MPR-TA, manufactured by Nissin Chemical Industry Co., Ltd.),
Methyl ethyl ketone/cyclohexanone = 6:4
After charging 300 parts (by weight) of a mixed solvent and stirring to dissolve, fine tin oxide powder doped with antimony oxide (trade name T-1, manufactured by Mitsubishi Metals) with an average particle size of 0.1 μm was prepared.
After gradually adding and mixing 78 parts, this was transferred to a paint shaker and dispersed for 30 minutes to prepare a transparent conductive coating composition. Comparative Example 1 In the same method as in Example 1, vinyl chloride-vinyl acetate (90% by weight) containing no hydroxy group was prepared.
Transparent conductive coating compositions were prepared in all the same manner except that a copolymer (~10% by weight) was used. Examples 2 to 3 and Comparative Examples 2 to 3 In the method of Example 1, except that the blending ratio of saponified vinyl chloride-vinyl acetate copolymer and fine tin oxide powder was as shown in Table 1. A transparent conductive coating composition was prepared in the same manner.
【表】
以上、実施例及び比較例で調製した各透明導電
性被覆組成物を用いて、ポリエチレンテレフタレ
ートフイルム上にグラビアプリンター（175メツ
シユ）により塗布した後、60℃で１分間乾燥を行
い厚さ1.0μｍの導電性塗膜を形成した。
このように作成した各フイルムの表面抵抗、ヘ
ーズを測定した結果をまとめると第２表の通りで
あつた。
なお、各透明導電性被覆組成物の経時安定性及
びグラビア印刷適性の試験結果も記載している。
ただし、
(1) 表面抵抗は、商品名デジタルマルチメーター
（タケダ理研社製）により測定した。
(2) ヘーズとは曇価を表わし、
ヘーズ＝拡散透過率／全光線透過率×100
（拡散透過率＝全光線透過率−平行線透過率）
で算出されるものである）
なおヘーズの値はヘーズメーター（日本電色工
業社製）により測定した。
(3) 経時安定性は、各組成物を50℃の雰囲気下に
20日間静置した後の、液の状態で測定した。
◎……全く変化なし
○……少々沈澱有り
△……沈澱物多い
×……完全に液が分離
(4) 印刷適性は、次のように判定した。
およぎ：フイルムの塗布面にすじ状のムラの有
無を目視で判定。
目視判定でムラが分らない……合格
目視判定でムラが分る……不合格
はいり：グラビアメツシユの目づまりなしに塗
布されるか否かで判定した。
100ｍ目づまりなし……合格
100ｍ以下で目づまり発生……不合格[Table] Each of the transparent conductive coating compositions prepared in Examples and Comparative Examples was applied onto a polyethylene terephthalate film using a gravure printer (175 mesh), and then dried at 60°C for 1 minute to determine the thickness. A conductive coating film of 1.0 μm was formed. Table 2 summarizes the results of measuring the surface resistance and haze of each film thus prepared. In addition, test results of the stability over time and suitability for gravure printing of each transparent conductive coating composition are also described. However, (1) Surface resistance was measured using a digital multimeter (trade name, manufactured by Takeda Riken Co., Ltd.). (2) Haze refers to haze value. Haze = Diffuse transmittance / Total light transmittance x 100 (Diffuse transmittance = Total light transmittance - Parallel light transmittance)
Note that the haze value was measured using a haze meter (manufactured by Nippon Denshoku Kogyo Co., Ltd.). (3) Stability over time was determined by exposing each composition to an atmosphere of 50°C.
Measurements were made in the liquid state after being allowed to stand for 20 days. ◎...No change at all ○...Slight precipitation △...Many sediment ×...Liquid completely separated (4) Printability was determined as follows. Scratch: Visually determine the presence or absence of streak-like unevenness on the coated surface of the film. No unevenness can be seen by visual judgment...Pass No unevenness can be seen by visual judgment...Fail Good: Judgment was made based on whether or not the gravure mesh could be coated without clogging. No clogging for 100m...Pass Clogging occurs within 100m...Fail
【表】
（発明の効果）
前記の説明から明らかなように本発明の被膜組
成物は、不導体のフイルム、シートの表面に優れ
た帯電防止効果を発揮する透明導電性塗膜を形成
できる。又、被覆組成物自身、分散安定性に優
れ、さらに印刷適性にも優れるものである。[Table] (Effects of the Invention) As is clear from the above description, the coating composition of the present invention can form a transparent conductive coating film exhibiting an excellent antistatic effect on the surface of a nonconductive film or sheet. Further, the coating composition itself has excellent dispersion stability and printability.
Claims (1)
有し、かつ塩化ビニル単位が80％以上である塩化
ビニル−酢酸ビニル共重合体ケン化物35〜15重量
部、(b)導電性金属酸化物微粉末65〜85重量部、(c)
極性有機溶剤よりなり、分散状態における導電性
金属酸化物微粉末の粒径が、二次凝集物として
0.1〜1.0μｍの範囲にある透明導電性被覆組成物。 ２ 導電性金属酸化物は、酸化錫（SnO）、酸化
アンチモン（Sb2O3）、酸化インジウム（In2O3）
より選ばれた少なくとも１種よりなる特許請求の
範囲第１項に記載の透明導電性被覆組成物。 ３ 極性有機溶剤は、エステル系、ケトン系、エ
ーテル系、ハロゲン化炭化水素系よりなる群から
選ばれた１種以上である特許請求の範囲第１項ま
たは第２項記載の透明導電性被覆組成物。[Scope of Claims] 1 (a) 35 to 15 parts by weight of a saponified vinyl chloride-vinyl acetate copolymer containing 1 to 10% by weight of vinyl alcohol units and 80% or more of vinyl chloride units, ( b) 65 to 85 parts by weight of conductive metal oxide fine powder, (c)
Made of a polar organic solvent, the particle size of the conductive metal oxide fine powder in the dispersed state is
A transparent conductive coating composition in the range of 0.1 to 1.0 μm. 2 Conductive metal oxides include tin oxide (SnO), antimony oxide (Sb 2 O 3 ), and indium oxide (In 2 O 3 ).
The transparent conductive coating composition according to claim 1, comprising at least one selected from the following. 3. The transparent conductive coating composition according to claim 1 or 2, wherein the polar organic solvent is one or more selected from the group consisting of esters, ketones, ethers, and halogenated hydrocarbons. thing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17893485A JPS6239666A (en) | 1985-08-13 | 1985-08-13 | Electrically conductive transparent coating composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17893485A JPS6239666A (en) | 1985-08-13 | 1985-08-13 | Electrically conductive transparent coating composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6239666A JPS6239666A (en) | 1987-02-20 |
| JPH0465112B2 true JPH0465112B2 (en) | 1992-10-19 |
Family
ID=16057195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17893485A Granted JPS6239666A (en) | 1985-08-13 | 1985-08-13 | Electrically conductive transparent coating composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6239666A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4435376B4 (en) * | 1993-10-05 | 2004-11-11 | Dai Nippon Toryo Co., Ltd. | Composition for forming conductive films |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5481341A (en) * | 1977-12-12 | 1979-06-28 | Shinetsu Polymer Co | Electrically conductive resin composition for release coating |
| JPS54100204A (en) * | 1978-01-24 | 1979-08-07 | Kansai Paint Co Ltd | Radio wave absorbing paint composition |
-
1985
- 1985-08-13 JP JP17893485A patent/JPS6239666A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6239666A (en) | 1987-02-20 |
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