JP4161086B2 - Transparent conductive film forming coating liquid and transparent conductive film forming method - Google Patents
Transparent conductive film forming coating liquid and transparent conductive film forming method Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は液晶表示素子やタッチパネル等の各種エレクトロニクス素子に好適に用いられる透明導電膜形成用塗布液および透明導電膜の形成方法に関するものである。
【０００２】
【従来の技術】
従来より、透明導電膜は液晶表示素子、タッチパネル、電磁波シールド材、赤外線反射膜等に広く使用されている。
透明導電膜としては錫をドープした酸化インジウム膜（ＩＴＯ）、アンチモンをドープした酸化スズ膜（ＡＴＯ）等があり、これらは蒸着法やスパッタ法、焼成法（塗布熱分解法とも言う）等により形成されていた。
【０００３】
【発明が解決しようとする課題】
透明導電膜の形成方法の中で蒸着法及びスパッタ法は、気相中で目的物質を基板に堆積させて膜を成長させるものであり、真空容器を使用するため装置が大がかりで高価なうえ、生産性が悪く、又、大面積の成膜が困難なものであった。
これに対し焼成法は、スピンコート法やディップコート法、印刷法などにより基材に目的物質の前駆物質を塗布し、これを焼成（熱分解）することで膜を形成するものであり、装置が簡単で生産性に優れ、大面積の成膜が容易であるという利点があるが、通常焼成時に４００℃から５００℃の高温処理を必要とするため基材が限られてしまうという問題点を有していた。
【０００４】
この問題点を解決するための手段として、特開平９−８６９６７号公報に開示されたようにＩＴＯ微粒子がシリケートマトリックス中に分散した膜を２００℃以下で成膜している例があるが、これはエッチング等によるパターンニングが困難であり液晶表示素子等の用途には適していなかった。
【０００５】
従って本発明の目的は、以上のような問題点を解消し、広範な種類の基板を使用可能な２００℃程度の低温での焼成でも透明導電膜を形成することのできる透明導電膜形成用塗布液、及び透明導電膜の形成方法を提供することにある。
【０００６】
【課題を解決するための手段】
即ち本発明は、蟻酸インジウム及び有機錫化合物を溶媒に溶解してなる透明導電膜形成用塗布液であって、有機錫化合物が、蟻酸錫（ II ）、ジｎ−ブチル錫ジ蟻酸塩、テトライソプロポキシ錫及びテトラｔ−ブチル錫からなる群より選択される１種又は２種以上である透明導電膜形成用塗布液である。
さらに本発明は、有機錫化合物がテトラｔ−ブチル錫である前記の透明導電膜形成用塗布液である。
さらにまた本発明は、溶媒がＮ，Ｎ−ジメチルホルムアミドである前記の透明導電膜形成用塗布液である。
また本発明は、前記の透明導電膜形成用塗布液を基板上に塗布し、熱処理することにより透明導電膜を形成することを特徴とする透明導電膜の形成方法である。
さらに本発明は、熱処理が１９０℃〜３５０℃の温度範囲である前記の透明導電膜の形成方法である。
また本発明は、蟻酸インジウム及び有機錫化合物を溶媒に溶解してなる透明導電膜形成用塗布液を基板上に塗布し、１９０℃〜３５０℃の温度範囲で熱処理することにより透明導電膜を形成することを特徴とする透明導電膜の形成方法である。
さらにまた本発明は、熱処理の前に、蟻酸インジウム及び有機錫化合物が熱分解しない温度で予備乾燥する前記の透明導電膜の形成方法である。
【０００７】
【発明の実施の形態】
本発明の塗布液に使用する蟻酸インジウムは、室温空気中で安定であり、２００℃程度に加熱すると熱分解して結晶性の酸化インジウムとなるので、焼成法による塗布液の成分として適している。
又、透明導電膜は膜の特性として硬度の高いものが好ましいが、蟻酸インジウムを使用して得られる透明導電膜は、２００℃程度で熱分解する蟻酸インジウム以外のインジウム化合物を使用した場合に比べて硬度の高い良好な透明導電膜となる。
【０００８】
本発明の塗布液に使用する有機錫化合物としては２００℃程度若しくはそれ以下の温度で熱分解して結晶性の酸化錫となるものであればどのような化合物でもよいが、例えば、錫のアルコキシド、錫の有機酸塩、及び錫の各種有機錯体等を挙げることができる。
このような有機錫化合物として特に好ましいのは、例えば、蟻酸錫（II）、ジｎ−ブチル錫ジ蟻酸塩、テトライソプロポキシ錫、テトラｔ−ブチル錫を挙げることができる。
良好な導電性を得る点で最も好ましいのはテトラｔ−ブチル錫である。
【０００９】
本発明の塗布液中のインジウムと錫の元素数比率は、最終的に形成された透明導電膜中のインジウムと錫の比となるので、透明導電膜を得るに当たって所望とする透明導電膜中のインジウムと錫の比となるように、塗布液に使用する蟻酸インジウム及び有機錫化合物の割合を選択すればが良い。
【００１０】
本発明の塗布液に使用する溶媒としては、蟻酸インジウムと上記有機錫化合物の両方の化合物を溶解、好ましくは室温付近で溶解でき、且つ熱処理時に蟻酸インジウム、上記有機錫化合物と反応しない、若しくは反応し難い難いものであれば任意に選ぶことができる。尚、ここで言う「溶解」とは溶解させようとする温度における溶解度が概ね５（ｇ／１００ｇ）以上であることを意味する。
このような溶媒として好ましいものとしては、例えば、Ｎ，Ｎ−ジメチルホルムアミドを挙げることができる。
【００１１】
本発明の塗布液における、蟻酸インジウムと上記有機錫化合物の濃度は、蟻酸インジウムと有機錫化合物の比率は上記の通りであるので、ここでは蟻酸インジウムと上記有機錫化合物の合計量の濃度で表すことにする。蟻酸インジウムと上記有機錫化合物の合計量の濃度は、従来の焼成法による透明導電膜形成用塗布液中のインジウム化合物と錫化合物の濃度と同程度とすれば支障無いが、例えば、概ね５〜３０重量％であればよく、良好な成膜性を得る点で好ましくは５〜１５重量％とするのが良い。
【００１２】
本発明の透明導電膜の形成方法は、上記塗布液を基板上に塗布し、熱処理することにより透明導電膜を形成するものである。
【００１３】
ここに使用する基板としては、熱処理温度に耐え、かつ使用する溶媒に対して耐性のあるもので有れば任意に選ぶことができ、従来透明導電膜の形成に使用されている基板を使用することができる。例えば、無アルカリガラス基板等のガラス基板は透明導電膜の基板として普及しており、これを使用できる。
【００１４】
本発明の透明導電膜の形成方法における熱処理は、大気中、本発明に使用する上記蟻酸インジウムと有機錫化合物の有効な熱分解が可能な温度で行えばよいが、広範な種類の基板を使用可能であるという本発明の効果を得るためには、好ましくは大気中１９０℃〜３５０℃、好ましくは１９０℃〜２５０℃の温度範囲で行えば良い。
このような温度範囲では上記のガラス基板だけでなく、ポリイミド、ポリアリレート、ポリアリールスルホン、ポリアリーレンスルフィド等の材料も基板として好ましく使用できる。
【００１５】
尚、本発明の透明導電膜の形成方法は、従来より低温で熱処理することができるが、基板材料の選択に制限が無いなど、高温（例えば、従来使用されてきた４００〜５００℃等）での熱処理に耐え得る基板が使用可能であれば、このような高温で熱処理するにあたり何ら支障はなく、この場合、得られる透明導電膜はより低い抵抗値が得られるので、上記本発明の塗布液は従来法のような高温での熱処理での使用に際しても優れた効果を発揮する。
【００１６】
また、本発明の透明導電膜の形成方法は、熱処理の前に１００℃程度の蟻酸インジウム化合物及び有機錫化合物が熱分解しない温度で予備乾燥した方がより平滑な膜面を得ることができるので好ましい。
【００１７】
【実施例】
以下、実施例および比較例により本発明をさらに説明する。
実施例１
蟻酸インジウム及び蟻酸錫（II）を、合計で１０重量％となるようにＮ，Ｎ−ジメチルホルムアミドに溶解させて塗布液とした。
蟻酸インジウムと蟻酸錫（II）の比率は、インジウムと錫の元素数含有比率が、９０：１０となるように調節した。
この塗布液を無アルカリガラス基板上にスピンコート法で塗布し、１００℃で１０分間乾燥させた後、大気中で２００℃で６０分間熱処理して透明導電膜を得た。
得られた膜の特性を下記表１に示す。
【００１８】
実施例２
有機錫化合物としてジｎ−ブチル錫ジ蟻酸塩を使用した以外は、実施例１と同様にして透明導電膜を得た。得られた膜の特性を下記表１に示す。
【００１９】
実施例３
有機錫化合物としてテトライソプロポキシ錫を使用した以外は、実施例１と同様にして透明導電膜を得た。得られた膜の特性を下記表１に示す。
【００２０】
実施例４
有機錫化合物としてテトラｔ−ブチル錫を使用した以外は、実施例１と同様にして透明導電膜を得た。得られた膜の特性を下記表１に示す。
【００２１】
実施例５
熱処理温度を２３０℃とした以外は、実施例４と同様にして透明導電膜を得た。得られた膜の特性を下記表１に示す。
【００２２】
実施例６
基板の材質をポリイミドとした以外は、実施例５と同様にして透明導電膜を得た。得られた膜の特性を下記表１に示す。
【００２３】
実施例７
熱処理温度を５００℃とした以外は、実施例１と同様にして透明導電膜を得た。得られた膜の特性を下記表１に示す。
【００２４】
比較例１
２−エチルヘキサン酸インジウム及び２−エチルヘキサン酸錫を、１０重量％となるようにキシレンに溶解させて塗布液とした。
この塗布液を無アルカリガラス基板上にスピンコート法で塗布し、１００℃で１０分間乾燥させた後、大気中で２００℃で６０分間熱処理したが、インジウム及び錫化合物の熱分解が起こらず、透明導電膜は得られなかった。
【００２５】
【表１】
なお、透過率の測定は、（株）日立製作所製Ｕ−１１００形分光
光度計を用いて、波長５５０ｎｍにおける透明導電膜及び基材の
透過率を読み取った。
【００２６】
【発明の効果】
本発明の効果は、従来の方法の問題となっている真空容器を使用せず大面積の成膜が容易に行え、広範な種類の基板に対し使用可能な２００℃程度の低温での焼成でも透明導電膜を形成することのできる透明導電膜形成用塗布液、及び透明導電膜の形成方法を提供したことにある。
また、本発明によれば、膜特性の良好な透明導電膜を簡便にしかも低温で得られるという効果がある。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a coating solution for forming a transparent conductive film and a method for forming a transparent conductive film, which are suitably used for various electronic devices such as liquid crystal display devices and touch panels.
[0002]
[Prior art]
Conventionally, transparent conductive films have been widely used for liquid crystal display elements, touch panels, electromagnetic shielding materials, infrared reflective films and the like.
Examples of transparent conductive films include indium oxide films doped with tin (ITO), tin oxide films doped with antimony (ATO), and the like by vapor deposition, sputtering, firing (also referred to as coating pyrolysis), etc. Was formed.
[0003]
[Problems to be solved by the invention]
Among the methods for forming a transparent conductive film, the vapor deposition method and the sputtering method are for growing a film by depositing a target substance on a substrate in a gas phase, and since a vacuum vessel is used, the apparatus is large and expensive, Productivity was poor, and film formation of a large area was difficult.
On the other hand, the firing method is to form a film by applying a precursor of a target substance to a substrate by spin coating, dip coating, printing, etc., and firing (thermally decomposing) it. Has the advantage that it is simple, excellent in productivity, and easy to form a film with a large area, but usually requires a high temperature treatment of 400 ° C. to 500 ° C. at the time of firing, so that the base material is limited. Had.
[0004]
As means for solving this problem, there is an example in which a film in which ITO fine particles are dispersed in a silicate matrix is formed at 200 ° C. or lower as disclosed in JP-A-9-86967. Is difficult to pattern by etching or the like, and is not suitable for applications such as liquid crystal display elements.
[0005]
Accordingly, an object of the present invention is to solve the above-mentioned problems and to form a transparent conductive film that can form a transparent conductive film even by baking at a low temperature of about 200 ° C. that can use a wide variety of substrates. It is in providing the formation method of a liquid and a transparent conductive film.
[0006]
[Means for Solving the Problems]
The present invention provides I coating liquid for forming transparent conductive film der the formic indium and an organic tin compound formed by dissolving in a solvent, organic tin compounds, formic acid tin (II), di-n- butyl Suzuji formate, It is the coating liquid for transparent conductive film formation which is 1 type, or 2 or more types selected from the group which consists of tetraisopropoxy tin and tetra t-butyl tin .
Furthermore, the present invention provides the coating liquid for forming a transparent conductive film, wherein the organic tin compound is tetra-t-butyltin.
Furthermore, the present invention is the above-mentioned coating liquid for forming a transparent conductive film, wherein the solvent is N, N-dimethylformamide.
Moreover, this invention is a formation method of a transparent conductive film characterized by forming a transparent conductive film by apply | coating the said coating liquid for transparent conductive film formation on a board | substrate, and heat-processing.
Furthermore, this invention is the formation method of the said transparent conductive film whose heat processing is a temperature range of 190 to 350 degreeC.
In addition, the present invention forms a transparent conductive film by applying a coating liquid for forming a transparent conductive film obtained by dissolving indium formate and an organic tin compound in a solvent and heat-treating the substrate at a temperature range of 190 ° C to 350 ° C. A method of forming a transparent conductive film.
Furthermore, the present invention is the method for forming the transparent conductive film, wherein the transparent conductive film is pre-dried at a temperature at which the indium formate and the organic tin compound are not thermally decomposed before the heat treatment.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
The indium formate used in the coating solution of the present invention is stable in air at room temperature, and is thermally decomposed into crystalline indium oxide when heated to about 200 ° C., so it is suitable as a component of the coating solution by the baking method. .
In addition, the transparent conductive film preferably has a high hardness as a film characteristic, but the transparent conductive film obtained by using indium formate is more in comparison with the case of using an indium compound other than indium formate which is thermally decomposed at about 200 ° C. Therefore, it becomes a good transparent conductive film with high hardness.
[0008]
The organotin compound used in the coating solution of the present invention may be any compound as long as it is thermally decomposed to a crystalline tin oxide at a temperature of about 200 ° C. or lower. For example, a tin alkoxide , Tin organic acid salts, and various organic complexes of tin.
Particularly preferable examples of such an organic tin compound include tin (II) formate, di-n-butyltin diformate, tetraisopropoxytin, and tetra-t-butyltin.
Tetra-t-butyl tin is most preferable in terms of obtaining good conductivity.
[0009]
The ratio of the number of elements of indium and tin in the coating liquid of the present invention is the ratio of indium and tin in the finally formed transparent conductive film. Therefore, in obtaining the transparent conductive film, What is necessary is just to select the ratio of the indium formate and organic tin compound which are used for a coating liquid so that it may become a ratio of an indium and a tin.
[0010]
As the solvent used in the coating solution of the present invention, both indium formate and the above-mentioned organic tin compound can be dissolved, preferably at around room temperature, and indium formate and the above-mentioned organic tin compound do not react or react during heat treatment. If it is difficult and difficult, you can choose any. The term “dissolving” as used herein means that the solubility at the temperature to be dissolved is approximately 5 (g / 100 g) or more.
Preferable examples of such a solvent include N, N-dimethylformamide.
[0011]
The concentration of indium formate and the organic tin compound in the coating solution of the present invention is represented by the concentration of the total amount of indium formate and the organic tin compound because the ratio of indium formate and the organic tin compound is as described above. I will decide. The concentration of the total amount of indium formate and the above organic tin compound is not problematic if the concentration of the indium compound and the tin compound in the coating solution for forming a transparent conductive film by the conventional baking method is approximately the same. It may be 30% by weight, and preferably 5 to 15% by weight from the viewpoint of obtaining good film formability.
[0012]
In the method for forming a transparent conductive film of the present invention, the transparent conductive film is formed by applying the above-mentioned coating solution on a substrate and performing a heat treatment.
[0013]
The substrate used here can be arbitrarily selected as long as it can withstand the heat treatment temperature and is resistant to the solvent used, and a substrate conventionally used for forming a transparent conductive film is used. be able to. For example, glass substrates such as non-alkali glass substrates are widely used as substrates for transparent conductive films and can be used.
[0014]
The heat treatment in the method for forming a transparent conductive film of the present invention may be carried out in the atmosphere at a temperature at which effective thermal decomposition of the indium formate and the organotin compound used in the present invention is possible, but a wide variety of substrates are used. In order to obtain the effect of the present invention that it is possible, it is preferably performed in the air at a temperature range of 190 ° C. to 350 ° C., preferably 190 ° C. to 250 ° C.
In such a temperature range, not only the above glass substrate but also materials such as polyimide, polyarylate, polyarylsulfone, polyarylene sulfide and the like can be preferably used as the substrate.
[0015]
In addition, although the formation method of the transparent conductive film of this invention can heat-process at low temperature conventionally, there is no restriction | limiting in the selection of board | substrate material, for example, high temperature (for example, 400-500 degreeC etc. conventionally used). If a substrate that can withstand this heat treatment can be used, there is no problem in heat treatment at such a high temperature. In this case, the transparent conductive film obtained has a lower resistance value. Exhibits excellent effects when used in heat treatment at a high temperature as in the conventional method.
[0016]
In addition, the method for forming a transparent conductive film of the present invention can obtain a smoother film surface by predrying at a temperature at which the indium formate compound and the organic tin compound at about 100 ° C. are not thermally decomposed before the heat treatment. preferable.
[0017]
【Example】
The present invention will be further described below with reference to examples and comparative examples.
Example 1
Indium formate and tin (II) formate were dissolved in N, N-dimethylformamide to give a total of 10% by weight to obtain a coating solution.
The ratio of indium formate and tin (II) formate was adjusted so that the content ratio of indium and tin was 90:10.
This coating solution was applied onto an alkali-free glass substrate by a spin coating method, dried at 100 ° C. for 10 minutes, and then heat-treated at 200 ° C. for 60 minutes in the air to obtain a transparent conductive film.
The properties of the obtained film are shown in Table 1 below.
[0018]
Example 2
A transparent conductive film was obtained in the same manner as in Example 1 except that di-n-butyltin diformate was used as the organic tin compound. The properties of the obtained film are shown in Table 1 below.
[0019]
Example 3
A transparent conductive film was obtained in the same manner as in Example 1 except that tetraisopropoxytin was used as the organic tin compound. The properties of the obtained film are shown in Table 1 below.
[0020]
Example 4
A transparent conductive film was obtained in the same manner as in Example 1 except that tetra-t-butyltin was used as the organic tin compound. The properties of the obtained film are shown in Table 1 below.
[0021]
Example 5
A transparent conductive film was obtained in the same manner as in Example 4 except that the heat treatment temperature was 230 ° C. The properties of the obtained film are shown in Table 1 below.
[0022]
Example 6
A transparent conductive film was obtained in the same manner as in Example 5 except that the material of the substrate was polyimide. The properties of the obtained film are shown in Table 1 below.
[0023]
Example 7
A transparent conductive film was obtained in the same manner as in Example 1 except that the heat treatment temperature was 500 ° C. The properties of the obtained film are shown in Table 1 below.
[0024]
Comparative Example 1
Indium 2-ethylhexanoate and tin 2-ethylhexanoate were dissolved in xylene so as to be 10% by weight to obtain a coating solution.
This coating solution was applied on a non-alkali glass substrate by a spin coating method, dried at 100 ° C. for 10 minutes, and then heat-treated at 200 ° C. for 60 minutes in the atmosphere, but thermal decomposition of indium and tin compounds did not occur, A transparent conductive film was not obtained.
[0025]
[Table 1]
In addition, the measurement of the transmittance | permeability read the transmittance | permeability of the transparent conductive film and base material in wavelength 550nm using Hitachi Ltd. U-1100 type spectrophotometer.
[0026]
【The invention's effect】
The effect of the present invention is that a large-area film can be easily formed without using a vacuum vessel which is a problem of the conventional method, and can be used for a wide variety of substrates even at a low temperature of about 200 ° C. It is in providing the coating liquid for transparent conductive film formation which can form a transparent conductive film, and the formation method of a transparent conductive film.
Moreover, according to this invention, there exists an effect that the transparent conductive film with a favorable film | membrane characteristic can be obtained simply and at low temperature.
Claims (7)
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