JPS6228712B2 - - Google Patents
Info
- Publication number
- JPS6228712B2 JPS6228712B2 JP9873980A JP9873980A JPS6228712B2 JP S6228712 B2 JPS6228712 B2 JP S6228712B2 JP 9873980 A JP9873980 A JP 9873980A JP 9873980 A JP9873980 A JP 9873980A JP S6228712 B2 JPS6228712 B2 JP S6228712B2
- Authority
- JP
- Japan
- Prior art keywords
- transparent conductive
- conductive film
- indium
- compound
- resistance
- 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
Links
- 238000000034 method Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 7
- 150000002472 indium compounds Chemical class 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 10
- 150000003606 tin compounds Chemical class 0.000 description 8
- -1 tin alkoxides Chemical class 0.000 description 6
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 5
- 229910052738 indium Inorganic materials 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-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
- 239000000919 ceramic Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- MCXZOLDSEPCWRB-UHFFFAOYSA-N triethoxyindigane Chemical compound [In+3].CC[O-].CC[O-].CC[O-] MCXZOLDSEPCWRB-UHFFFAOYSA-N 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- ONIKNECPXCLUHT-UHFFFAOYSA-N 2-chlorobenzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1Cl ONIKNECPXCLUHT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PKKGKUDPKRTKLJ-UHFFFAOYSA-L dichloro(dimethyl)stannane Chemical compound C[Sn](C)(Cl)Cl PKKGKUDPKRTKLJ-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 150000001261 hydroxy acids Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
- Laminated Bodies (AREA)
Description
本発明は、ガラス、セラミツクス等の耐熱性基
板上に透明導電膜を形成する方法に関するもので
ある。
透明導電膜は、液晶デイスプレイ素子、エレク
トロルミネツセンスデイスプレイ素子、エレクト
ロクロミツクデイスプレイ素子などのデイスプレ
イ素子の電極に広く用いられている。また、太陽
電池、光電池、航空機や自動車の防曇窓にも用い
られる。従来、透明導電膜の製造方法とし次の方
法がある。
(イ) 真空蒸着法
(ロ) スパツタ法
(ハ) CVD法
(ニ) 塗布法
上記(イ),(ロ)の方法は低抵抗の透明導電膜が得ら
れる長所をもつ方法であるが、同時に、真空系を
用いるために連続生産が困難であることからバツ
チ方式がとられているため生産コストが高くなる
という欠点をあわせもつ。(ハ)の方法では連続生産
が可能であり、上記(イ)(ロ)の方法の欠点を解消でき
る可能性があるが、蒸気流のコントロールが困難
であり、均質な透明導電膜を連続して生産し難い
という欠点をもつ。(ニ)の方法は上記欠点を解消す
る可能性があるが、従来用いられている材料では
低抵抗の膜は得難いという欠点がある。
本発明の目的は、上記した従来技術の欠点をな
くし、実用に供し得る低抵抗の透明導電膜の安価
な製造方法を提供するにある。
塗布法により、実用に供し得る低抵抗の透明導
電膜を製造するために本発明はドーピングスズ化
合物として、一般式RSn−SnR(ここでRは炭素
数1〜8のアルキル基)で表わされるジチン化合
物を用いることを特徴とする。
透明導電膜としてはSnをドープしたIn2O3、あ
るいはSbをドープしたSnO2が知られているが、
より低抵抗であること、パターン化のためのエツ
チングが容易であることから、前者が一般的に用
いられている。塗布法によりSnをドープした
In2O3からなる透明導電膜の製造のための材料
は、インジウム化合物、スズ化合物および溶媒で
ある。塗布法により得られる透明導電膜は、従来
の材料を用いると実用に耐え得る程度の低抵抗と
はなり難い。塗布法により得られる透明導電膜の
抵抗値は、用いる材料の種類により異なるが、ド
ーピングスズ化合物の種類による影響が最も大き
い。例えば無機スズ化合物である塩化第一スズ
(SuCl2)や塩化第二スズ(SnCl4)を用いた場合に
は、塗布後焼成した際に塩素が残り易く高抵抗の
原因となる。また有機スズ化合物であるジメチル
スズジクロリド((CH3)2SnCl2)などは昇華性で
あるために、焼成途中で揮散し高抵抗となる。ま
たジアルキルスズジカルボキシレート、トリアル
キルスズモノカルボキシレートなどのスズ化合物
は固体物質であるため、塗膜に一様に分散し難
く、高抵抗の原因となる。またテトラエトキシス
ズ(Sn(OCH2CH3)4)、エトラメトキシスズ
(Sn(OCH3)4)などのスズアルコキシドは加水分
解を受け易く塗布液が白濁し易いという欠点をも
つ。
上記したように従来用いられているドーピング
スズ化合物はいずれも難点をもつため、得られた
透明導電膜は抵抗が高く実用に耐え難い。しかる
に、本発明によるジチン化合物を用いることによ
り、従来のドーピングスズ化合物が持つている上
記問題点をすべて解消し、塗布法により実用レベ
ルの低抵抗の透明導電膜を安価に製造することが
できる。すなわち、ジチン化合物は、液体である
ためインジウム化合物中に一様に分散した塗膜を
作ることができ、しかも蒸発や昇華により揮散す
る前に有機成分が完全に焼成するため、低抵抗の
透明導電膜を得ることができる。本発明に用いら
れるジチン化合物はアルキルが炭素数1〜8が望
ましい。炭素数がこれより多いと得られる透明導
電膜の緻密性が損なわれ高抵抗となる。またドー
ピング量はインジウム化合物に対して5〜30重量
%が適当である。ドーピング量が5%より少ない
と抵抗値が高くなり、30%より多いと膜が白濁し
易く、また抵抗値が高くなる。
インジウム化合物としては、トリエトキシイン
ジウム(In(OC2H5)3)などのインジウムアルコ
キシド、ジエトキシモノブチルインジウム
(C4H9In(OC2H5)2)などのアルキルインジウム
アルコキシド、トリ(マーエチルヘキサン酸)イ
ンジウム(In(OCOC7H15)3)などのインジウム
カーボキシレートなどを用いることができる。ま
た硝酸インジウム、塩化インジウムなどの無機イ
ンジウム化合物と、モノカルボン酸、ジカルボン
酸、ヒドロキシ酸、ジカルボン酸モノエステルな
どの配位子から形成されるインジウム化合物を用
いることもできる。本発明に適する溶媒は、メタ
ノール、エタノール、プロパノールなどのアルコ
ール、セロソルブ、カルビトール、グリコール、
アセトン、メチルエチルケトン、酢酸メチル、酢
酸エチルなどがある。焼成温度はガラス基板を用
いる場合には300〜700℃が望ましい。温度が300
℃より低いと有機物の燃焼が不完全であり、また
700℃より高いとガラスが変形する。アルミナな
どのセラミツク基板を用いる場合には300℃以上
の焼成温度が適する。
次に本発明を実施例により説明する。
実施例 1〜7
オクチル酸インジウム、ジチン化合物、エチル
セロソルブをそれぞれ第1表に示す量だけ秤量
し、塗布液とした。この塗布液をスピンナにより
ガラス基板上に塗布し、ついで乾燥させた後500
℃で1時間焼成した。得られた透明導電膜のシー
ト抵抗値と膜厚を第1表に示す。
The present invention relates to a method for forming a transparent conductive film on a heat-resistant substrate such as glass or ceramics. Transparent conductive films are widely used in electrodes of display devices such as liquid crystal display devices, electroluminescent display devices, and electrochromic display devices. It is also used in solar cells, photovoltaic cells, and anti-fog windows of aircraft and automobiles. Conventionally, there are the following methods for manufacturing transparent conductive films. (a) Vacuum deposition method (b) Sputtering method (c) CVD method (d) Coating method The above methods (a) and (b) have the advantage of producing a transparent conductive film with low resistance, but at the same time Since continuous production is difficult due to the use of a vacuum system, the batch method is adopted, which also has the disadvantage of increasing production costs. Method (c) allows continuous production and may eliminate the drawbacks of methods (a) and (b) above, but it is difficult to control the vapor flow and it is difficult to continuously produce a homogeneous transparent conductive film. The disadvantage is that it is difficult to produce. Although method (d) has the potential to eliminate the above-mentioned drawback, it has the drawback that it is difficult to obtain a low-resistance film using conventionally used materials. An object of the present invention is to eliminate the drawbacks of the above-mentioned conventional techniques and to provide an inexpensive manufacturing method for a transparent conductive film with low resistance that can be put to practical use. In order to produce a transparent conductive film with a low resistance that can be used practically by a coating method, the present invention uses a ditin compound represented by the general formula RSn-SnR (where R is an alkyl group having 1 to 8 carbon atoms) as a doping tin compound. It is characterized by using a compound. In 2 O 3 doped with Sn or SnO 2 doped with Sb are known as transparent conductive films.
The former is generally used because it has lower resistance and can be easily etched for patterning. Doped with Sn by coating method
The materials for producing a transparent conductive film made of In 2 O 3 are an indium compound, a tin compound and a solvent. A transparent conductive film obtained by a coating method cannot easily have a resistance low enough to withstand practical use if conventional materials are used. The resistance value of a transparent conductive film obtained by a coating method varies depending on the type of material used, but is most influenced by the type of doping tin compound. For example, when inorganic tin compounds such as stannous chloride (SuCl 2 ) or stannic chloride (SnCl 4 ) are used, chlorine tends to remain when baked after coating, causing high resistance. Furthermore, since dimethyltin dichloride ((CH 3 ) 2 SnCl 2 ), which is an organic tin compound, is sublimable, it volatilizes during firing, resulting in high resistance. Further, since tin compounds such as dialkyltin dicarboxylate and trialkyltin monocarboxylate are solid substances, they are difficult to uniformly disperse in the coating film, causing high resistance. Furthermore, tin alkoxides such as tetraethoxytin (Sn(OCH 2 CH 3 ) 4 ) and etramethoxytin (Sn(OCH 3 ) 4 ) have the disadvantage that they are easily hydrolyzed and the coating solution tends to become cloudy. As mentioned above, all of the conventionally used doping tin compounds have drawbacks, and the resulting transparent conductive film has a high resistance and is difficult to put into practical use. However, by using the ditin compound according to the present invention, all of the above-mentioned problems of conventional doped tin compounds can be solved, and a transparent conductive film with a practical level of low resistance can be manufactured at low cost by a coating method. In other words, since the ditin compound is a liquid, it is possible to create a coating film that is uniformly dispersed in the indium compound, and since the organic component is completely baked before being volatilized by evaporation or sublimation, it is a transparent conductor with low resistance. membrane can be obtained. In the ditin compound used in the present invention, the alkyl preferably has 1 to 8 carbon atoms. If the number of carbon atoms is larger than this, the density of the resulting transparent conductive film will be impaired and the resistance will be high. The appropriate doping amount is 5 to 30% by weight based on the indium compound. When the doping amount is less than 5%, the resistance value becomes high, and when it is more than 30%, the film tends to become cloudy and the resistance value becomes high. Indium compounds include indium alkoxides such as triethoxyindium (In(OC 2 H 5 ) 3 ), alkylindium alkoxides such as diethoxymonobutyl indium (C 4 H 9 In(OC 2 H 5 ) 2 ), tri( Indium carboxylates such as indium mer-ethylhexanoate (In(OCOC 7 H 15 ) 3 ) can be used. Further, an indium compound formed from an inorganic indium compound such as indium nitrate or indium chloride and a ligand such as a monocarboxylic acid, a dicarboxylic acid, a hydroxy acid, or a dicarboxylic acid monoester can also be used. Solvents suitable for the present invention include alcohols such as methanol, ethanol, propanol, cellosolve, carbitol, glycols,
Examples include acetone, methyl ethyl ketone, methyl acetate, and ethyl acetate. When using a glass substrate, the firing temperature is preferably 300 to 700°C. temperature is 300
If it is lower than ℃, the combustion of organic matter is incomplete, and
If the temperature is higher than 700℃, the glass will deform. When using a ceramic substrate such as alumina, a firing temperature of 300°C or higher is suitable. Next, the present invention will be explained by examples. Examples 1 to 7 Indium octylate, ditin compound, and ethyl cellosolve were each weighed in amounts shown in Table 1 to prepare a coating solution. This coating solution was applied onto a glass substrate using a spinner, and after drying,
It was baked at ℃ for 1 hour. The sheet resistance value and film thickness of the obtained transparent conductive film are shown in Table 1.
【表】
実施例 8
トリエトキシインジウム(15g)、ヘキサメチ
ルジチン(1.5g)、エチルセロソルブ(100g)
から塗布液を調製し、ついで実施例1〜7と同様
にして透明導電膜を形成した。シート抵抗値は
0.8KΩ/□、膜厚は710Åであつた。
実施例 9〜15
硝酸インジウム、配位子、ヘキサメチルジチ
ン、エチルセロソルブを第2表に示す量だけ秤量
し塗布液とした。ついで実施例1〜7と同様にし
て透明導電膜を形成した。
実施例 16
オクチル酸インジウム(15g)、ヘキサメチル
ジチン(1.5g)、エチルセロソルブ(100g)か
ら塗布液を調製した。この塗布液をアルミナ基板
上にスピンナにより塗布し、ついで900℃で10分
間焼成した。得られた透明導電膜のシート抵抗値
は0.4Ω/□であつた。[Table] Example 8 Triethoxyindium (15g), hexamethylditine (1.5g), ethyl cellosolve (100g)
A coating solution was prepared from the above, and then a transparent conductive film was formed in the same manner as in Examples 1 to 7. The sheet resistance value is
The resistance was 0.8KΩ/□, and the film thickness was 710Å. Examples 9 to 15 Indium nitrate, a ligand, hexamethylditine, and ethyl cellosolve were weighed in amounts shown in Table 2 to prepare a coating solution. Then, a transparent conductive film was formed in the same manner as in Examples 1 to 7. Example 16 A coating solution was prepared from indium octylate (15 g), hexamethylditine (1.5 g), and ethyl cellosolve (100 g). This coating liquid was applied onto an alumina substrate using a spinner, and then baked at 900°C for 10 minutes. The sheet resistance value of the obtained transparent conductive film was 0.4Ω/□.
【表】
本発明により、実用に供し得る低抵抗の透明導
電膜を安価に製造することができ、工業的意義が
大きい。[Table] According to the present invention, a practically usable, low-resistance transparent conductive film can be manufactured at low cost, and it has great industrial significance.
Claims (1)
でRは炭素数1〜8のアルキル基)で表わされる
ジチン化合物、および有機溶媒を必須成分とする
溶液を基板上に塗布した後、これを加熱すること
を特徴とする透明導電膜形成法。1 After applying a solution containing an indium compound, a ditin compound represented by the general formula RSn-SnR (where R is an alkyl group having 1 to 8 carbon atoms), and an organic solvent as essential components onto a substrate, this is heated. A transparent conductive film forming method characterized by the following.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9873980A JPS5724678A (en) | 1980-07-21 | 1980-07-21 | Method of forming transparent electroconductive film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9873980A JPS5724678A (en) | 1980-07-21 | 1980-07-21 | Method of forming transparent electroconductive film |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS5724678A JPS5724678A (en) | 1982-02-09 |
JPS6228712B2 true JPS6228712B2 (en) | 1987-06-22 |
Family
ID=14227853
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9873980A Granted JPS5724678A (en) | 1980-07-21 | 1980-07-21 | Method of forming transparent electroconductive film |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5724678A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2842917B2 (en) * | 1990-02-09 | 1999-01-06 | 株式会社日立製作所 | Electronic device mounting structure |
-
1980
- 1980-07-21 JP JP9873980A patent/JPS5724678A/en active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS5724678A (en) | 1982-02-09 |
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