JPH0696619A - Composition for forming transparent conductive film and method therefor - Google Patents

Composition for forming transparent conductive film and method therefor

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Publication number
JPH0696619A
JPH0696619A JP24485492A JP24485492A JPH0696619A JP H0696619 A JPH0696619 A JP H0696619A JP 24485492 A JP24485492 A JP 24485492A JP 24485492 A JP24485492 A JP 24485492A JP H0696619 A JPH0696619 A JP H0696619A
Authority
JP
Japan
Prior art keywords
compound
indium
magnesium
conductive film
transparent conductive
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
Application number
JP24485492A
Other languages
Japanese (ja)
Inventor
Yoshihiro Hori
堀  喜博
Akiyoshi Hattori
章良 服部
Akihiko Yoshida
昭彦 吉田
Original Assignee
Matsushita Electric Ind Co Ltd
松下電器産業株式会社
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Matsushita Electric Ind Co Ltd, 松下電器産業株式会社 filed Critical Matsushita Electric Ind Co Ltd
Priority to JP24485492A priority Critical patent/JPH0696619A/en
Publication of JPH0696619A publication Critical patent/JPH0696619A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To stably form a transparent conductive film having low resistance and high transmissivity. CONSTITUTION:By heating an organic solution composed of an inorganic indium compound, a magnesium compound, and an organic compound capable of coordination in indium, the inorganic indium compound and magnesium compound, where a part of the organic compound are coordinated, react with crystal water including an inorganic indium salt. Partial hydrolysis of the magnesium compound allows an intermediate composite compound of indium and magnesium to be formed. The resultant composition is applied and baked so that an MgIn2O4-x film having spinel structure can be obtained, thus realizing conductivity and high transmissivity.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、ガラス、セラミックス
等の基板上に形成する透明導電膜の形成用組成物及び透
明導電膜の形成方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a composition for forming a transparent conductive film formed on a substrate such as glass or ceramics and a method for forming the transparent conductive film.

【0002】[0002]

【従来の技術】液晶表示素子、エレクトロルミネッセン
ス(EL)表示素子などの表示素子類の電極や、自動
車、航空機、建築物などの窓ガラスの防曇または氷結防
止のための発熱抵抗体において、可視光に対して高透過
性を有する電極材料が使用されている。
Visible in electrodes of display elements such as liquid crystal display elements and electroluminescence (EL) display elements, and heating resistors for preventing fogging or icing of window glass of automobiles, aircraft, buildings, etc. An electrode material having high transparency to light is used.

【0003】このような透明導電性材料としては、酸化
スズ・酸化アンチモン系(ATO)や酸化インジウム・
酸化スズ系(ITO)などが知られており、これらの金
属酸化物はガラスまたはセラミック基板上に容易に被膜
を形成し、透明導電膜とすることができる。
Such transparent conductive materials include tin oxide / antimony oxide (ATO) and indium oxide.
Tin oxide (ITO) and the like are known, and these metal oxides can easily form a film on a glass or ceramic substrate to form a transparent conductive film.

【0004】またそれら透明導電膜の形成方法として
は、次の方法が知られている。 (1) 真空蒸着法 (2) スパッタリング法 (3) CVD法 (4) 塗布法
The following methods are known as methods for forming these transparent conductive films. (1) Vacuum evaporation method (2) Sputtering method (3) CVD method (4) Coating method

【0005】[0005]

【発明が解決しようとする課題】しかし、上記の(1)、
(2)、(3)の方法は、装置が複雑かつ高価で、コストと量
産性に問題がある。また、(4)の方法は、上記の(1)、
(2)、(3)の方法の課題を解決する可能性を有しているも
のの、実用に耐えうる膜を形成することが困難であっ
た。
[Problems to be Solved by the Invention] However, the above (1),
In the methods (2) and (3), the device is complicated and expensive, and there are problems in cost and mass productivity. Further, the method of (4), the above (1),
Although there is a possibility of solving the problems of the methods (2) and (3), it is difficult to form a film that can be used practically.

【0006】さらに、酸化スズ・アンチモン系(AT
O)は抵抗率が比較的高いこと、化学的に安定であるた
め、酸によってエッチングすることが難しい等の課題が
あった。
Further, tin oxide / antimony type (AT
Since O) has a relatively high resistivity and is chemically stable, there is a problem that it is difficult to etch with O.

【0007】また、酸化インジウム・酸化スズ系(IT
O)は抵抗率が低く、酸によって容易にエッチングが可
能であるが、環境条件に対する安定性の悪さから、透光
性の低下、抵抗率の増加という課題があった。
Further, indium oxide / tin oxide (IT
O) has a low resistivity and can be easily etched with an acid, but has problems such as a decrease in translucency and an increase in resistivity due to its poor stability against environmental conditions.

【0008】本発明は、上記従来の透明導電膜の形成の
課題を解決するもので、高透過率の透明導電膜を安定し
て形成することが可能な透明導電膜形成用組成物と透明
導電膜の形成方法を提供することを目的とする。
The present invention solves the above-mentioned problems of forming a conventional transparent conductive film, and a composition for forming a transparent conductive film and a transparent conductive film capable of stably forming a transparent conductive film having a high transmittance. An object is to provide a method for forming a film.

【0009】[0009]

【課題を解決するための手段】本発明は、無機インジウ
ム化合物と、マグネシウム化合物と、インジウムに配位
可能な有機化合物とを含む透明導電膜形成用組成物であ
る。
The present invention is a composition for forming a transparent conductive film containing an inorganic indium compound, a magnesium compound and an organic compound capable of coordinating with indium.

【0010】また、本発明は、この組成物を基板に塗
布、乾燥した後、焼成する透明導電膜形成方法である。
Further, the present invention is a method for forming a transparent conductive film, which comprises coating the composition on a substrate, drying the composition, and then baking the composition.

【0011】[0011]

【作用】本発明は、無機インジウム化合物と、マグネシ
ウム化合物と、インジウムに配位可能な有機化合物とを
含む有機溶液を加熱処理することにより、有機化合物が
1部配位した無機インジウム化合物とマグネシウム化合
物と無機インジウム化合物が含有する結晶水が反応し、
無機インジウム化合物とマグネシウム化合物が部分的に
加水分解されて、インジウムとマグネシウムの中間複合
化合物を形成し、この組成物を塗布・焼成することによ
り、スピネル構造を有するMgIn2O4-x膜を得ることで、
高い導電性、透過率を可能にするものである。
In the present invention, an organic solution containing an inorganic indium compound, a magnesium compound, and an organic compound capable of coordinating with indium is heat-treated to form an inorganic indium compound and a magnesium compound in which one part of the organic compound is coordinated. And the water of crystallization contained in the inorganic indium compound reacts,
An inorganic indium compound and a magnesium compound are partially hydrolyzed to form an intermediate composite compound of indium and magnesium, and this composition is applied and baked to obtain a MgIn 2 O 4-x film having a spinel structure. By that,
It enables high conductivity and transmittance.

【0012】[0012]

【実施例】以下、本発明の実施例について図面を参照し
て説明する。
Embodiments of the present invention will be described below with reference to the drawings.

【0013】本発明の透明導電膜形成用組成物は、例え
ば以下のようにして合成される。まず最初に、無機イン
ジウム化合物に配位可能な有機化合物を混合する。ここ
で、この無機インジウム化合物はインジウムやマグネシ
ウムと配位可能な有機化合物と置換できる配位子をもつ
ものであればよい。例えば、硝酸インジウム、塩化イン
ジウム、あるいは硫酸インジウムが挙げられ、さらに結
晶水を有しているものが好ましい。また、インジウムに
配位可能な有機化合物はインジウムとマグネシウムに1
部配位して、インジウムとマグネシウムの中間化合物の
形成を助け、有機溶剤に対する溶解性をもたせるために
必要であり、例えば、β−ジケトン類、α−またはβ−
ケトン酸類、前記ケトン酸類のエステル類、α−または
β−アミノアルコ−ル類が挙げられる。
The transparent conductive film-forming composition of the present invention is synthesized, for example, as follows. First, an organic compound capable of coordinating with an inorganic indium compound is mixed. Here, the inorganic indium compound may be any compound having a ligand capable of substituting an organic compound capable of coordinating with indium or magnesium. Examples thereof include indium nitrate, indium chloride, and indium sulfate, and those having crystallization water are preferable. The organic compound that can be coordinated to indium is 1 to indium and magnesium.
It is necessary in order to facilitate the formation of an intermediate compound of indium and magnesium by having a partial coordination and to have solubility in an organic solvent, for example, β-diketones, α- or β-
Examples thereof include ketone acids, esters of the above ketone acids, and α- or β-amino alcohols.

【0014】次に、前記溶液に有機溶剤とマグネシウム
化合物を加え、撹拌する。このときの撹拌は、加熱処理
しながら行うことが好ましい。ここで、前記マグネシウ
ム化合物としては、空気中では比較的安定ではあるが、
加熱処理により容易に加水分解しやすいものであればよ
い。例えば、硝酸マグネシウム、塩化マグネシウム、硫
酸マグネシウム、シュウ酸マグネシウム、酢酸マグネシ
ウムなどが好ましい。また、前記有機溶剤としては、本
発明で用いる有機化合物や無機化合物を溶解するもので
あればよい。例えば、トルエン、キシレン等の芳香族炭
化水素、エタノ−ル、イソプロパノ−ル、等のアルコ−
ル類、酢酸エチル、酢酸ブチル等の酢酸エステル類、ア
セトン、ジエチルケトン等のケトン類、メトキシエタノ
−ル、エトキシエタノ−ル等のエ−テル類、テトラヒド
ロフラン等が挙げられる。さらに、加熱処理の温度とし
ては、無機インジウム化合物とマグネシウム化合物とそ
れらの配位可能な有機化合物とからなる有機溶液の還流
温度もしくは還流温度付近が好ましい。
Next, an organic solvent and a magnesium compound are added to the solution and stirred. It is preferable that the stirring at this time is performed while heating. Here, although the magnesium compound is relatively stable in air,
Any substance that can be easily hydrolyzed by heat treatment may be used. For example, magnesium nitrate, magnesium chloride, magnesium sulfate, magnesium oxalate, magnesium acetate and the like are preferable. Further, the organic solvent may be any solvent that dissolves the organic compound or the inorganic compound used in the present invention. For example, aromatic hydrocarbons such as toluene and xylene, alcohols such as ethanol and isopropanol, and the like.
And acetic acid esters such as ethyl acetate and butyl acetate, ketones such as acetone and diethyl ketone, ethers such as methoxyethanol and ethoxyethanol, and tetrahydrofuran. Further, the temperature of the heat treatment is preferably at or near the reflux temperature of the organic solution containing the inorganic indium compound, the magnesium compound and the organic compound capable of coordinating them.

【0015】そして、加熱処理後の有機溶液を室温付近
まで冷却し、得られた有機溶液を透明導電膜形成用組成
物とする。ここで、有機溶液の増粘効果と、透明導電膜
形成用組成物を基板に塗布・乾燥して得られる被膜の安
定性を与えるために、透明導電膜形成用組成物に多価の
アルコ−ルを加えることが好ましい。例えば、多価のア
ルコ−ルとしては、グリコ−ル類や3価のアルコ−ル類
が挙げられるが、炭素数が小さく、熱分解時の炭素残留
の恐れの少ない、エチレングリコ−ルやグリセリンが好
ましい。
The organic solution after the heat treatment is cooled to around room temperature, and the obtained organic solution is used as a composition for forming a transparent conductive film. Here, in order to give the thickening effect of the organic solution and the stability of the coating film obtained by coating and drying the composition for forming a transparent conductive film on a substrate, the composition for forming a transparent conductive film contains a polyvalent alcohol. Is preferably added. For example, polyvalent alcohols include glycols and trivalent alcohols, but ethylene glycol and glycerin have a small number of carbons and are less likely to leave carbon residue during thermal decomposition. Is preferred.

【0016】このようにして、得られた透明透明導電膜
形成組成物を基板に塗布・乾燥した後、焼成して、透明
導電膜を形成する。ここで、透明導電膜形成用組成物の
塗布には、スクリ−ン印刷法、ロ−ルコ−ト法、ディッ
プコ−ト法、スピンコ−ト法、等を用いることができる
が、ディップコ−ト法、スピンコ−ト法が好ましい。ま
た、焼成温度としては、透明導電膜形成用組成物が、分
解する温度以上で、かつ基板の変形温度以下であればよ
く、400〜700℃が好ましい。
The transparent transparent conductive film-forming composition thus obtained is applied to a substrate, dried, and then baked to form a transparent conductive film. Here, for the coating of the composition for forming a transparent conductive film, a screen printing method, a roll coat method, a dip coat method, a spin coat method, or the like can be used, and a dip coat method. The spin coat method is preferred. The firing temperature may be higher than or equal to the decomposition temperature of the composition for forming a transparent conductive film and lower than the deformation temperature of the substrate, and is preferably 400 to 700 ° C.

【0017】以下、本発明のさらに詳細な具体的実施例
を説明する。
Hereinafter, more detailed specific examples of the present invention will be described.

【0018】(実施例1)1 lの三角フラスコに、45
gの硝酸インジウム(化1)を秤量し、50gのアセチル
アセトンを加えて、室温で混合・溶解させた。その溶液
に、0[(数1)で0wt%]〜8.1g[(数1)で30wt%]
のシュウ酸マグネシウム(化2)とアセトンを加えて還
流した。その還流後の溶液を、室温付近まで冷却し、10
gのグリセリンを加えて、撹拌・混合し、透明導電膜形
成用組成物を合成した。その透明導電膜形成用組成物
に、SiO2コート並ガラス基板を60cm/minの引き上げ速度
でディップコートした。その基板を5分間室温で放置
し、100℃で5分間乾燥した後、500℃で1時間焼成し
た。得られた膜の厚みは0.05μmで、それらのシ−ト抵
抗並びに透過率を図1に示す。
(Example 1) In a 1 l Erlenmeyer flask, 45
g of indium nitrate (Chemical Formula 1) was weighed, 50 g of acetylacetone was added, and mixed and dissolved at room temperature. In the solution, 0 [(Equation 1) 0 wt%] to 8.1 g [(Equation 1) 30 wt%]
Magnesium oxalate (Chemical Formula 2) and acetone were added and the mixture was refluxed. The solution after reflux is cooled to near room temperature,
G glycerin was added, and the mixture was stirred and mixed to synthesize a composition for forming a transparent conductive film. The transparent conductive film-forming composition was dip-coated with a SiO 2 -coated glass substrate at a pulling rate of 60 cm / min. The substrate was left at room temperature for 5 minutes, dried at 100 ° C. for 5 minutes, and then baked at 500 ° C. for 1 hour. The thickness of the obtained film was 0.05 μm, and their sheet resistance and transmittance are shown in FIG.

【0019】[0019]

【化1】 In(NO3)3・3H2O[Chemical 1] In (NO 3 ) 3・ 3H 2 O

【0020】[0020]

【化2】 MgC2O4・2H2O (実施例2)無機インジウム化合物として、硝酸インジ
ウムを、マグネシウム化合物として、硝酸マグネシウム
(化3)を用い、(数1)で10wt%となるようにした。
他は実施例1に同じ。
## STR00002 ## MgC 2 O 4 .2H 2 O (Example 2) Indium nitrate was used as the inorganic indium compound, and magnesium nitrate (Chemical formula 3) was used as the magnesium compound, so that 10 wt% was obtained in (Equation 1). did.
Others are the same as in Example 1.

【0021】[0021]

【化3】 Mg(NO3)2・6H2O (実施例3)無機インジウム化合物として、塩化インジ
ウム(化4)を、マグネシウム化合物として、硝酸マグ
ネシウムを用い、(数1)で10wt%となるようにした。
他は実施例1に同じ。
## STR00003 ## Mg (NO 3 ) 2 .6H 2 O (Example 3) Indium chloride (Chemical Formula 4) was used as the inorganic indium compound, and magnesium nitrate was used as the magnesium compound. I did it.
Others are the same as in Example 1.

【0022】[0022]

【化4】 InCl3・3H2O (実施例4)無機インジウム化合物として、塩化インジ
ウム(化4)を、マグネシウム化合物として、シュウ酸
マグネシウムを用い、(数1)で10wt%となるようにし
た。他は実施例1と同じである。
## STR00004 ## InCl 3 .3H 2 O (Example 4) Indium chloride (Chemical formula 4) was used as the inorganic indium compound, and magnesium oxalate was used as the magnesium compound, so that 10 wt% was obtained in (Equation 1). . Others are the same as in the first embodiment.

【0023】(比較例1)1 lの三角フラスコに、45
gの硝酸インジウム(化1)と5.4g[(数1)で10wt
%]のシュウ酸第1スズ(化5)とアセトンを加えて、
撹拌・混合し、透明導電膜形成用組成物を合成した。そ
の透明導電膜形成用組成物に、SiO2コート並ガラス基板
を60cm/minの引き上げ速度でディップコートした。その
基板を5分間室温で放置し、100℃で5分間乾燥した後、5
00℃で1時間焼成した。
(Comparative Example 1) In a 1 l Erlenmeyer flask, 45
g of indium nitrate (Chemical formula 1) and 5.4 g [(Equation 1) 10 wt.
%] Stannous oxalate (formula 5) and acetone are added,
The mixture was stirred and mixed to synthesize a composition for forming a transparent conductive film. The transparent conductive film-forming composition was dip-coated with a SiO 2 -coated glass substrate at a pulling rate of 60 cm / min. Allow the substrate to sit at room temperature for 5 minutes, dry at 100 ° C for 5 minutes, then
It was baked at 00 ° C for 1 hour.

【0024】[0024]

【化5】 SnC2O4 (表1)に実施例1〜4、比較例1の結果を示す。Embedded image SnC 2 O 4 (Table 1) shows the results of Examples 1 to 4 and Comparative Example 1.

【0025】[0025]

【表1】 [Table 1]

【0026】このように、比較例に比べて高透過率の透
明導電膜を得ることが出来る。
In this way, a transparent conductive film having a higher transmittance than that of the comparative example can be obtained.

【0027】[0027]

【発明の効果】以上述べたところから明らかなように、
本発明は、導電性と可視領域における透過性に優れた透
明導電膜を容易にかつ安価で得ることができる。
As is apparent from the above description,
INDUSTRIAL APPLICABILITY The present invention makes it possible to easily and inexpensively obtain a transparent conductive film having excellent conductivity and transparency in the visible region.

【0028】従って、本発明にかかる透明導電膜は表示
素子や発熱抵抗体等の透明電極等の用途に最適なもので
ある。
Therefore, the transparent conductive film according to the present invention is most suitable for use as a transparent electrode such as a display element or a heating resistor.

【図面の簡単な説明】[Brief description of drawings]

【図1】実施例1のシュウ酸マグネシウム添加量による
シ−ト抵抗及び透過率の変化を示すグラフである。
FIG. 1 is a graph showing changes in sheet resistance and transmittance according to the amount of magnesium oxalate added in Example 1.

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】無機インジウム化合物と、マグネシウム化
合物と、インジウムに配位可能な有機化合物とを含む有
機溶液であることを特徴とする透明導電膜形成用組成
物。
1. A composition for forming a transparent conductive film, which is an organic solution containing an inorganic indium compound, a magnesium compound, and an organic compound capable of coordinating with indium.
【請求項2】無機インジウム化合物に対するマグネシウ
ムの配合比が、下記(数1)で5〜20wt%の範囲にある
ことを特徴とする請求項1記載の透明導電膜形成用組成
物。 【数1】 Mg/(In+Mg)×100
2. The composition for forming a transparent conductive film according to claim 1, wherein the compounding ratio of magnesium to the inorganic indium compound is in the range of 5 to 20 wt% in the following (Formula 1). [Equation 1] Mg / (In + Mg) × 100
【請求項3】無機インジウム化合物が硝酸インジウム、
塩化インジウム、又は硫酸インジウムであることを特徴
とする請求項1記載の透明導電膜形成用組成物。
3. The inorganic indium compound is indium nitrate,
The composition for forming a transparent conductive film according to claim 1, which is indium chloride or indium sulfate.
【請求項4】マグネシウム化合物が硝酸マグネシウム、
塩化マグネシウム、硫酸マグネシウム、シュウ酸マグネ
シウム、酢酸マグネシウムからなる群から選ばれたもの
であることを特徴とする請求項1記載の透明導電膜形成
用組成物。
4. The magnesium compound is magnesium nitrate,
The composition for forming a transparent conductive film according to claim 1, which is selected from the group consisting of magnesium chloride, magnesium sulfate, magnesium oxalate, and magnesium acetate.
【請求項5】配位可能な有機化合物が、β−ジケトン
類、α−またはβ−ケトン酸類、前記ケトン酸類のエス
テル類、α−またはβ−アミノアルコール類からなる群
から選ばれるものであることを特徴とする請求項1記載
の透明導電膜形成用組成物。
5. The coordinating organic compound is selected from the group consisting of β-diketones, α- or β-ketone acids, esters of the ketone acids, and α- or β-amino alcohols. The composition for forming a transparent conductive film according to claim 1, wherein
【請求項6】無機インジウム化合物と、マグネシウム化
合物と、インジウムに配位可能な有機化合物とを含む透
明導電膜形成用組成物を、基板に塗布、乾燥した後、焼
成することを特徴とする透明導電膜の形成方法。
6. A transparent conductive film-forming composition comprising an inorganic indium compound, a magnesium compound, and an organic compound capable of coordinating with indium, coated on a substrate, dried, and then baked. Method for forming conductive film.
JP24485492A 1992-09-14 1992-09-14 Composition for forming transparent conductive film and method therefor Pending JPH0696619A (en)

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Application Number Priority Date Filing Date Title
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Publications (1)

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JPH0696619A true JPH0696619A (en) 1994-04-08

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JP2014120712A (en) * 2012-12-19 2014-06-30 Ricoh Co Ltd Coating liquid for metal oxide film formation, metal oxide film, field effect transistor, and process of manufacturing field effect transistor
KR20140097475A (en) 2011-11-30 2014-08-06 가부시키가이샤 리코 Coating liquid for forming metal oxide thin film, metal oxide thin film, field-effect transistor, and method for manufacturing field-effect transistor
KR20180067738A (en) 2010-11-29 2018-06-20 가부시키가이샤 리코 Coating liquid for forming metal oxide thin film, metal oxide thin film, field effect transistor, and method for producing the field effect transistor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20180067738A (en) 2010-11-29 2018-06-20 가부시키가이샤 리코 Coating liquid for forming metal oxide thin film, metal oxide thin film, field effect transistor, and method for producing the field effect transistor
KR20140097475A (en) 2011-11-30 2014-08-06 가부시키가이샤 리코 Coating liquid for forming metal oxide thin film, metal oxide thin film, field-effect transistor, and method for manufacturing field-effect transistor
US9418842B2 (en) 2011-11-30 2016-08-16 Ricoh Company, Ltd. Coating liquid for forming metal oxide thin film, metal oxide thin film, field-effect transistor, and method for manufacturing field-effect transistor
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