JPS6217325B2 - - Google Patents
Info
- Publication number
- JPS6217325B2 JPS6217325B2 JP13031480A JP13031480A JPS6217325B2 JP S6217325 B2 JPS6217325 B2 JP S6217325B2 JP 13031480 A JP13031480 A JP 13031480A JP 13031480 A JP13031480 A JP 13031480A JP S6217325 B2 JPS6217325 B2 JP S6217325B2
- Authority
- JP
- Japan
- Prior art keywords
- paste
- transparent conductive
- conductive film
- acetope
- dimethyltin
- 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
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- 229910052738 indium Inorganic materials 0.000 claims description 12
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229940007550 benzyl acetate Drugs 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- PWEVMPIIOJUPRI-UHFFFAOYSA-N dimethyltin Chemical compound C[Sn]C PWEVMPIIOJUPRI-UHFFFAOYSA-N 0.000 description 14
- 229910052718 tin Inorganic materials 0.000 description 11
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 8
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 8
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000007650 screen-printing Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 4
- 229910006404 SnO 2 Inorganic materials 0.000 description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 description 4
- 150000003606 tin compounds Chemical class 0.000 description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- -1 indium organic acids Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OJVAMHKKJGICOG-UHFFFAOYSA-N 2,5-hexanedione Chemical compound CC(=O)CCC(C)=O OJVAMHKKJGICOG-UHFFFAOYSA-N 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 2
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 2
- 229960001826 dimethylphthalate Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002471 indium Chemical class 0.000 description 2
- 150000002472 indium compounds Chemical class 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 2
- 229920001220 nitrocellulos Polymers 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- SMEGJBVQLJJKKX-HOTMZDKISA-N [(2R,3S,4S,5R,6R)-5-acetyloxy-3,4,6-trihydroxyoxan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@@H]1[C@H]([C@@H]([C@H]([C@@H](O1)O)OC(=O)C)O)O SMEGJBVQLJJKKX-HOTMZDKISA-N 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 229940081735 acetylcellulose Drugs 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229940095102 methyl benzoate Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Non-Insulated Conductors (AREA)
Description
【発明の詳細な説明】
本発明は、スクリーン印刷と焼成によりガラス
等の基板上に金属酸化物よりなる透明導電性被膜
を所望の形状に形成するための透明導電性被膜形
成用ペーストに関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a transparent conductive film forming paste for forming a transparent conductive film made of a metal oxide into a desired shape on a substrate such as glass by screen printing and baking.
ガラス、セラミツクなどの基板上に形成した
Cd，In，Sn等の酸化物被膜は透明で良好な導電
性を示すことはよく知られており、半導体素子、
液晶表示装置に使用されたり、或は、窓ガラス等
の氷結防止用導電膜として利用されたりして近年
益々応用範囲が拡大してきている。このような金
属酸化物透明導電性被膜の形成方法としては、化
学スプレー法、真空蒸着法、スクリーン印刷法な
どがある。 formed on a substrate such as glass or ceramic
It is well known that oxide films such as Cd, In, and Sn are transparent and exhibit good conductivity, and are used in semiconductor devices,
In recent years, the range of applications has been expanding more and more, such as being used in liquid crystal display devices or as a conductive film for preventing icing on window glass and the like. Methods for forming such a metal oxide transparent conductive film include a chemical spray method, a vacuum evaporation method, and a screen printing method.
化学スプレー法は、比較的大面積の形状の被膜
を得るには有利であるが、微細で複雑な形状のも
のを得るには、フオトエツチングなど余分な工程
が必要となり経済的ではない。真空蒸着法は、最
近マスク蒸着法が発達しフオトエツチング処理は
必要でなくなつたが、同時に多量の蒸着ができな
いので量産向きではない。スクリーン印刷法で
は、かかる問題がなく、目的形状のものを印刷焼
成することができ、エツチング処理にともなう廃
液処理の必要もないという利点がある。しかし、
従来は、透明導電性被膜形成用ペースト自体の安
定性が良くないため、スクリーン印刷時の作業性
も悪く、形成された被膜の導電性の良否にもバラ
ツキが大きいという欠点があつた。 Although the chemical spray method is advantageous in obtaining a film with a relatively large area, it is not economical to obtain a film with a fine and complex shape because it requires extra steps such as photo etching. The vacuum evaporation method has recently developed a mask evaporation method and no longer requires photoetching, but it is not suitable for mass production because a large amount cannot be deposited at the same time. The screen printing method has the advantage that it does not have such problems, can print and bake objects in the desired shape, and does not require waste liquid treatment associated with etching. but,
Conventionally, the stability of the paste for forming a transparent conductive film itself was poor, so the workability during screen printing was poor, and the conductivity of the formed film varied widely.
従来、この種ペーストにおいてはオクチル酸イ
ンジウム（C7H15CO2）3In等のイオン結合性の強
い有機酸インジウムを主体に用いていたが、有機
酸インジウムは加水分解し易く、又ペーストとし
た場合、ペーストのゲル化を促進する等比較的容
易に化学変化するという欠点を持つているため、
ペースト自体の寿命を短かくし、スクリーン印刷
時の作業性を悪くする原因となつていた。 Conventionally, in this type of paste, indium organic acids with strong ionic bonding properties such as indium octylate (C 7 H 15 CO 2 ) 3 In have been mainly used, but indium organic acids are easily hydrolyzed and are not compatible with pastes. However, it has the disadvantage that it undergoes chemical changes relatively easily, such as promoting gelation of the paste.
This shortens the life of the paste itself and causes poor workability during screen printing.
本発明者らは、これら欠点をなくすため、前出
願（出願番号55−36624、及出願番号55−
101752）に示す如く、焼成により金属酸化物被膜
を与える化合物として、例えば、アセチルアセト
ン（Hacac）の配位したトリスアセチルアセトナ
ートインジウム（In（acac）3）などの有機イン
ジウム錯体を使用したり、又抵抗値調整用スズ化
合物として、例えば、ジメチルスズアセトープ
（CH3）2Sn（acac）2などの有機スズ錯体を用いて
ペーストの安定性を高め、好結果を得ているが、
抵抗値調整用スズ化合物として、有機スズ錯体を
用いた場合、形成された透明導電性被膜の抵抗値
が、わずかながらばらつく欠点があつた。 In order to eliminate these drawbacks, the present inventors have proposed the previous application (application number 55-36624, and application number 55-36624).
101752), organic indium complexes such as indium trisacetylacetonate (In(acac) 3 ) coordinated with acetylacetone (Hacac) are used as compounds that provide a metal oxide film upon firing, or As a tin compound for adjusting the resistance value, organic tin complexes such as dimethyltin acetope (CH 3 ) 2 Sn (acac) 2 have been used to improve the stability of the paste, and good results have been obtained.
When an organic tin complex is used as the tin compound for adjusting the resistance value, there is a drawback that the resistance value of the formed transparent conductive film varies slightly.
本発明は、叙上の欠点を解消し、抵抗値が低く
ばらつきのない透明導電性被膜を提供するために
なされたものである。 The present invention has been made in order to eliminate the above-mentioned drawbacks and to provide a transparent conductive film having a low resistance value and no variation.
本発明の特徴は、主成分であるトリアセチルア
セトナートインジウムに、抵抗値調整用として
有機スズ錯体を、Sn原子百分率（Sn／（In＋
Sn）×100）が20At％となるように添加したこと
にある。 The feature of the present invention is that an organic tin complex is added to the main component, indium triacetylacetonate, to adjust the resistance value.
The reason is that Sn) × 100) was added to 20 At%.
第１図は、主成分としてのIn（acac）3有機イン
ジウム錯体に、抵抗値調整用としてオクチル酸ス
ズ、又は、ジメチルスズアセトープ、又はジブチ
ルスズジラウレートを用いて作成したペーストを
焼成して得られる透明導電性被膜中のSnO2の残
存率を示すグラフである。このグラフより、オク
チル酸スズを用いて作成したペーストでは、
SnO2の残存率が30.0％であるが、ジメチルスズ
アセトープの場合は、17.6％とSnO2の残存率が
低くいことがわかる。故に、ジメチルスズアセト
ープを、抵抗値調整用スズ化合物として用いる場
合、オクチル酸スズと同じ抵抗値調整効果を持た
せるには、オクチル酸スズ添加量より、多量のジ
メチルスズアセトープを添加する必要がある。 Figure 1 shows the paste obtained by baking a paste made using In(acac) 3 organic indium complex as the main component and tin octylate, dimethyltin acetope, or dibutyltin dilaurate for resistance adjustment. It is a graph showing the residual rate of SnO 2 in a transparent conductive film. From this graph, the paste made using tin octylate has
It can be seen that the residual rate of SnO 2 is 30.0%, but in the case of dimethyltin acetope, the residual rate of SnO 2 is low at 17.6%. Therefore, when dimethyltin acetope is used as a tin compound for adjusting resistance, in order to have the same resistance adjusting effect as tin octylate, it is necessary to add a larger amount of dimethyltin acetope than tin octylate. There is.
そこで、本発明者らは、種々の実験の結果、
Sn／（In＋Sn）百分率が20At％となるように、
ジメチルスズアセトープを添加すると、得られる
透明導電性被膜のシート抵抗が最小となることを
見出した。このことは、前出願（出願番号55−
36624）で述べたごとく、Sn／（In＋Sn）百分率
が10〜13At％となるように、オクチル酸スズを
添加した場合、得られる透明導電性被膜のシート
抵抗が最小となるが、ジメチルスズアセトープを
用いた場合は、Sn／（In＋Sn）百分率が20At％
となるように、ジメチルスズアセトープを添加し
なければ、オクチル酸スズ添加の場合と同様の効
果がえられないためであると判断できる。 Therefore, as a result of various experiments, the present inventors found that
So that the Sn/(In+Sn) percentage is 20At%,
It has been found that addition of dimethyltin acetope minimizes the sheet resistance of the resulting transparent conductive coating. This means that the previous application (application number 55-
36624), when tin octylate is added so that the Sn/(In+Sn) percentage is 10 to 13 At%, the sheet resistance of the resulting transparent conductive film is minimized, but dimethyltin acetope When using Sn/(In+Sn) percentage is 20At%
Therefore, it can be concluded that this is because the same effect as when adding tin octylate cannot be obtained unless dimethyltin acetope is added.
透明導電性被膜形成用ペーストは、インジウム
化合物に、抵抗値調整用としてのスズ化合物、粘
性剤、溶媒を混合して作成されるが、本発明で
は、インジウム化合物として、トリアセチルアセ
トナートインジウムを、抵抗値調整用として、
ジブチルスズジラウレート、ジメチルスズアセト
ープなどの有機スズ錯体を用いている。 The paste for forming a transparent conductive film is created by mixing an indium compound with a tin compound for adjusting the resistance value, a viscous agent, and a solvent. In the present invention, indium triacetylacetonate is used as the indium compound, For adjusting resistance value,
Organotin complexes such as dibutyltin dilaurate and dimethyltin acetope are used.
次に粘性剤であるが、融点の低いソーダ硝子へ
の適用を考慮すれば500℃以下でほぼ完全に熱分
解するものでなければならない。例えばエチルセ
ルローズ、ニトロセルローズ、アセチルセルロー
ズ、ベンジルセルローズなどが適用できる。次に
溶媒であるが、有機インジウム錯体や有機スズ錯
体に対して反応性が乏しく、前記粘性剤に対して
溶解能が良く蒸気圧が常温で１mmHg以下で、沸
点180〜350℃の性質があるものでなくてはならな
い。この溶媒として、２−エチルヘキシルアルコ
ール、ベンジルアルコール、ｄ−４−テルピネノ
ール等の高沸点アルコール、アセト酢酸エチル、
酢酸ベンジル、安息香酸メチル、フタル酸ジメチ
ル、フタル酸ジエチル、フタル酸ジブチル等の高
沸点エステル、アセトニルアセトン、イソホロン
等の高沸点ケトン、メチルカルビトール、カルビ
トール、カルビトールアセテート等のカルビトー
ル群等が適用できる。これら溶媒は単独で、又は
二種以上混合して使用してよい。 Next is the viscosity agent, which must be almost completely thermally decomposed at temperatures below 500°C, considering its application to soda glass, which has a low melting point. For example, ethylcellulose, nitrocellulose, acetylcellulose, benzylcellulose, etc. can be used. Next, regarding the solvent, it has poor reactivity with organic indium complexes and organotin complexes, has good dissolving power for the above-mentioned viscous agents, has a vapor pressure of 1 mmHg or less at room temperature, and has a boiling point of 180 to 350°C. It has to be something. As the solvent, high boiling point alcohols such as 2-ethylhexyl alcohol, benzyl alcohol, d-4-terpinenol, ethyl acetoacetate,
High boiling point esters such as benzyl acetate, methyl benzoate, dimethyl phthalate, diethyl phthalate, dibutyl phthalate, high boiling point ketones such as acetonylacetone and isophorone, carbitol group such as methyl carbitol, carbitol, carbitol acetate, etc. etc. can be applied. These solvents may be used alone or in combination of two or more.
次にペーストの製造方法を説明する。まず、In
（acac）3を秤量し、これに前記各溶媒を添加す
る。次に適当量のHacacを添加し130〜180℃の温
度で加熱し、Hacacにより一度完全に溶解せしめ
る。さらに同じ温度で加熱を続けHacacを完全に
除去する。Hacacが完全に除去されたか否かは溶
液の重量変化を調べることにより判明する。
Hacacを完全に除いたものは安定であり、In
（acac）3に対する溶解力のさほど大でない溶媒系
でも溶解状態は良好となる。次に、粘性剤である
セルローズ化合物を添加し、50〜60℃でよく撹拌
する。最後に有機スズ錯体を添加し撹拌してペー
ストを完成する。このようにして作成したペース
トは、スクリーン印刷法で目的形状に印刷し、
130〜170℃で予備乾燥後、400〜600℃で焼成する
ことにより、透明で良導電性の被膜を得ることが
できる。 Next, a method for producing the paste will be explained. First, In
(acac) 3 is weighed, and each of the above-mentioned solvents is added to it. Next, an appropriate amount of Hacac is added and heated at a temperature of 130 to 180°C to completely dissolve it once with Hacac. Further heating is continued at the same temperature to completely remove Hacac. Whether or not Hacac has been completely removed can be determined by examining the change in weight of the solution.
Completely excluding Hacac is stable and In
(acac) 3 can be dissolved in a good state even in a solvent system that does not have a very strong dissolving power. Next, a cellulose compound as a viscosity agent is added and stirred well at 50 to 60°C. Finally, the organic tin complex is added and stirred to complete the paste. The paste created in this way is printed into the desired shape using the screen printing method, and
A transparent and highly conductive film can be obtained by pre-drying at 130-170°C and then firing at 400-600°C.
以下、実施例により更に詳しく説明する。 A more detailed explanation will be given below using examples.
次の組成比で、ペーストを作成した。 A paste was prepared with the following composition ratio.
金属部
（In（acac）3、ジメチルスズアセトープ）
5.0wt％
溶媒部 84.0wt％
酢酸ベンジル 47.4wt％
ベンジルアルコール 17.8wt％
フタル酸ジメチル 17.8wt％
粘性剤（ニトロセルローズ粘度120秒）
11.0wt％
ここで、抵抗値調整用としてのジメチルスズア
セトープの添加比率を変化させ、得られた透明導
電性被膜のシート抵抗値を調べた結果が、第２図
に示したグラフである。このグラフから、抵抗値
調整用にジメチルスズアセトープを、Sn／（In
＋Sn）百分率が20At％となるように添加して得
られるペーストを用いて作製した透明導電性被膜
のシート抵抗が、最小となることがわかる。ジブ
チルスズジラウレートでも同じ結果を得ている。 Metal part (In(acac) 3 , dimethyltin acetope)
5.0wt% Solvent part 84.0wt% Benzyl acetate 47.4wt% Benzyl alcohol 17.8wt% Dimethyl phthalate 17.8wt% Viscous agent (nitrocellulose viscosity 120 seconds)
11.0wt% Here, the graph shown in FIG. 2 is the result of examining the sheet resistance value of the transparent conductive film obtained by changing the addition ratio of dimethyltin acetope for resistance value adjustment. From this graph, we can see that dimethyltin acetope is used for resistance adjustment.
It can be seen that the sheet resistance of the transparent conductive film produced using the paste obtained by adding Sn+Sn to 20 At% is the minimum. The same results were obtained with dibutyltin dilaurate.
なお、ペーストの焼成条件は、予備乾燥150
℃、20分で、焼成510℃、30分であり、形成され
た被膜厚は1500Åである。トリアセチルアセトナ
ートインジウムを有機インジウム錯体として用
いることにより、ペーストに用いる高沸点溶媒に
対し溶解度が高まつてペースト製造が容易とな
り、焼成後の透明導電性被膜は均質で歩留り良く
得られた。 The firing conditions for the paste are pre-drying at 150°C.
℃ for 20 minutes and calcination at 510℃ for 30 minutes, and the formed film thickness was 1500 Å. By using indium triacetylacetonate as an organic indium complex, the solubility in the high boiling point solvent used in the paste was increased, making it easier to manufacture the paste, and the transparent conductive film after firing was homogeneous and obtained with a good yield.
第１図は有機インジウム錯体に、抵抗値調整用
としてオクチル酸スズ、又はジメチルスズアセト
ープ、又はジブチルスズジラウレートを用いて作
成したペーストを焼成して得られる透明導電性被
膜中のSnO2残存率を示すグラフ、第２図は、本
発明の実施例で、ジメチルスズアセトープ添加比
率を変化させて得られた透明導電性被膜のシート
抵抗値を示すグラフである。
Figure 1 shows the SnO 2 residual rate in a transparent conductive film obtained by firing a paste made using tin octylate, dimethyltin acetope, or dibutyltin dilaurate for resistance adjustment in an organic indium complex. The graph shown in FIG. 2 is a graph showing sheet resistance values of transparent conductive coatings obtained by varying the addition ratio of dimethyltin acetope in Examples of the present invention.
Claims (1)
としてセルローズ化合物と、酢酸ベンジルなどの
溶媒と、抵抗値調整用として有機スズ錯体を
Sn／（In＋Sn）百分率（Sn原子百分率）が20At
％となるように添加混合した事を特徴とする透明
導電性被膜形成用ペースト。1 Add a cellulose compound as a viscosity agent, a solvent such as benzyl acetate, and an organic tin complex as a resistance value adjustment to the main component, an organic indium complex.
Sn/(In+Sn) percentage (Sn atomic percentage) is 20At
A paste for forming a transparent conductive film, which is characterized by being added and mixed so that
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13031480A JPS5755011A (en) | 1980-09-19 | 1980-09-19 | Transparent conductive film forming paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13031480A JPS5755011A (en) | 1980-09-19 | 1980-09-19 | Transparent conductive film forming paste |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5755011A JPS5755011A (en) | 1982-04-01 |
| JPS6217325B2 true JPS6217325B2 (en) | 1987-04-17 |
Family
ID=15031353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13031480A Granted JPS5755011A (en) | 1980-09-19 | 1980-09-19 | Transparent conductive film forming paste |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5755011A (en) |
-
1980
- 1980-09-19 JP JP13031480A patent/JPS5755011A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5755011A (en) | 1982-04-01 |
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