JP2003249132A - Manufacturing method of low resistance transparent conductive film - Google Patents
Manufacturing method of low resistance transparent conductive filmInfo
- Publication number
- JP2003249132A JP2003249132A JP2002050299A JP2002050299A JP2003249132A JP 2003249132 A JP2003249132 A JP 2003249132A JP 2002050299 A JP2002050299 A JP 2002050299A JP 2002050299 A JP2002050299 A JP 2002050299A JP 2003249132 A JP2003249132 A JP 2003249132A
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- Prior art keywords
- transparent conductive
- conductive film
- oxide
- metal
- gas
- 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.)
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Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、低抵抗透明導電膜
の製造法に関する。得られた低抵抗透明導電膜は、LC
D、有機EL等のフラットパネルディスプレイ用透明導
電膜として利用できる。TECHNICAL FIELD The present invention relates to a method for producing a low resistance transparent conductive film. The obtained low resistance transparent conductive film is LC
It can be used as a transparent conductive film for flat panel displays such as D and organic EL.
【0002】[0002]
【従来の技術】従来より、LCDや有機EL等のフラッ
トパネルディスプレイ用透明導電膜は、蒸着法、イオン
プレーティング法、スパッタリング法等によって、ガラ
ス基板上に金属酸化物を付着せしめることにより製造さ
れている。しかしながら、これらの方法では、装置が大
がかりになり装置コストが高くなると共に、製造コスト
が高くなる等のため、簡単な装置で安価に製造する方法
が求められていた。2. Description of the Related Art Conventionally, a transparent conductive film for a flat panel display such as LCD and organic EL is manufactured by depositing a metal oxide on a glass substrate by a vapor deposition method, an ion plating method, a sputtering method or the like. ing. However, in these methods, the size of the device becomes large, the cost of the device becomes high, and the manufacturing cost becomes high. Therefore, there has been a demand for a method of inexpensively manufacturing with a simple device.
【0003】そのために、フラットパネルディスプレイ
用透明導電膜を簡単な装置で安価に製造することを目的
として、従来のスパッタ成膜法等に代えて、近年、IT
O膜等の透明導電膜をスピン塗布、スプレー塗布、イン
クジェット塗布で形成することが提案されている。この
場合、透明導電膜形成材料としては、例えば、ITO等
の微粒子を有機溶媒に分散した分散液が使用される。こ
の分散液を上記塗布方法で基板に塗布した後加熱して、
有機溶媒の除去とITO微粒子の焼結とを行い、基板上
に薄膜状のITO膜を形成する。Therefore, in order to manufacture a transparent conductive film for a flat panel display with a simple apparatus at a low cost, in recent years, instead of the conventional sputtering film forming method, etc.
It has been proposed to form a transparent conductive film such as an O film by spin coating, spray coating, or inkjet coating. In this case, as the transparent conductive film forming material, for example, a dispersion liquid in which fine particles such as ITO are dispersed in an organic solvent is used. This dispersion is applied to the substrate by the above coating method and then heated,
The organic solvent is removed and the ITO fine particles are sintered to form a thin ITO film on the substrate.
【0004】[0004]
【発明が解決しようとする課題】上記塗布法で用いられ
る従来の材料は、低温加熱では焼結後の電気抵抗(シー
ト抵抗)が数kΩ/□と大きく、また、電気抵抗が小さ
いものを得ようとすると焼結の際に高温加熱(例えば、
300℃程度以上)が必要なため、LCD、有機EL等
のフラットパネルディスプレイの分野における透明導電
膜の形成には使用できないという問題がある。そのた
め、低温で焼結でき、低抵抗値を有する透明導電膜の製
造法が求められている。The conventional materials used in the above coating method have a large electric resistance (sheet resistance) of several kΩ / □ after sintering at low temperature heating and a small electric resistance. If so, high temperature heating during sintering (for example,
Since it requires about 300 ° C. or higher), it cannot be used for forming a transparent conductive film in the field of flat panel displays such as LCD and organic EL. Therefore, there is a demand for a method of manufacturing a transparent conductive film which can be sintered at a low temperature and has a low resistance value.
【0005】本発明の課題は、上記従来技術の問題点を
解決することにあり、焼結温度が低く、かつ、焼結後の
電気抵抗(シート抵抗)が小さい薄膜状透明導電膜の製造
法を提供することにある。An object of the present invention is to solve the above-mentioned problems of the prior art, and a method for producing a thin film transparent conductive film having a low sintering temperature and a small electric resistance (sheet resistance) after sintering. To provide.
【0006】[0006]
【課題を解決するための手段】本発明者らは、低抵抗透
明導電膜を得るために、その材料及び製造プロセスにつ
いて鋭意研究・開発を行ってきた。その結果、低温加熱
(250℃以下)で電気抵抗を大幅に下げることができる
低抵抗透明導電膜の製造法を見出し、本発明を完成させ
るに至った。[Means for Solving the Problems] The inventors of the present invention have conducted extensive research and development on materials and manufacturing processes for obtaining a low-resistance transparent conductive film. As a result, low temperature heating
The inventors have found a method for producing a low-resistance transparent conductive film capable of significantly reducing the electric resistance (at 250 ° C. or lower), and completed the present invention.
【0007】本発明の低抵抗透明導電膜の製造法は、透
明導電膜形成用金属酸化物の各成分金属の少なくとも1
種の金属の微粒子又は該各成分金属からなる少なくとも
1種の合金の微粒子の分散液を調製し、この分散液を被
処理基板上に塗布した後、大気圧の酸素ガス若しくはオ
ゾンガス雰囲気中、又は不活性ガス、例えば、ヘリウム
等の希ガス等に酸素ガス若しくはオゾンガスを添加した
ガスの大気圧プラズマのようなプラズマ雰囲気中、15
0〜250℃で加熱し、酸化と燒結とを同時に行い、金
属酸化物からなる透明導電膜を形成することからなる。
焼結温度が150℃未満であると充分焼結せず、また、
250℃を超えるとディスプレイ製造工程上問題が生じ
る。The method for producing a low-resistance transparent conductive film of the present invention comprises at least one of the component metals of the metal oxide for forming the transparent conductive film.
After preparing a dispersion liquid of fine particles of one kind of metal or fine particles of at least one alloy consisting of the respective component metals, and applying this dispersion liquid on a substrate to be treated, in an oxygen gas or ozone gas atmosphere at atmospheric pressure, or In a plasma atmosphere such as an atmospheric pressure plasma of an inert gas, for example, a gas obtained by adding oxygen gas or ozone gas to a rare gas such as helium, 15
It consists of heating at 0 to 250 ° C. and simultaneously performing oxidation and sintering to form a transparent conductive film made of a metal oxide.
If the sintering temperature is less than 150 ° C., it will not be sufficiently sintered, and
If it exceeds 250 ° C, a problem occurs in the display manufacturing process.
【0008】分散液は、酸化インジウム、酸化錫、酸化
亜鉛、酸化カドミウム、酸化ガリウム、In2O3(Z
nO)m、及びInGaO3(ZnO)m等や、これら酸
化物にドーパントを添加した錫添加酸化インジウム(I
TO)、アンチモン添加酸化錫(ATO)、亜鉛添加酸化
インジウム(IZO)及びアルミニウム添加酸化亜鉛(A
ZO)から選ばれた金属酸化物の各成分金属の少なくと
も1種の金属の微粒子分散液又は該各成分金属からなる
少なくとも1種の合金の微粒子分散液をである。IT
O、ATO、IZO、ZnO、SnO2、CaWO4か
ら選ばれるものが好ましい。上記製造法において、酸化
と燒結との工程で酸化性雰囲気中に紫外線照射を行うこ
とが好ましい。本発明の方法で製造した低抵抗透明導電
膜は、ガラス基板や有機樹脂材料からなる基板との密着
性も併せ持つという特徴を有する。The dispersion is indium oxide, tin oxide, zinc oxide, cadmium oxide, gallium oxide, In 2 O 3 (Z
nO) m , InGaO 3 (ZnO) m, and the like, and tin-containing indium oxide (I
TO), antimony added tin oxide (ATO), zinc added indium oxide (IZO) and aluminum added zinc oxide (A
A fine particle dispersion of at least one metal of each component metal of the metal oxide selected from ZO) or a fine particle dispersion of at least one alloy of each of the component metals. IT
Those selected from O, ATO, IZO, ZnO, SnO 2 and CaWO 4 are preferable. In the above-mentioned manufacturing method, it is preferable to perform ultraviolet irradiation in an oxidizing atmosphere in the steps of oxidizing and sintering. The low resistance transparent conductive film produced by the method of the present invention has a feature that it also has adhesion to a glass substrate or a substrate made of an organic resin material.
【0009】[0009]
【発明の実施の形態】本発明によれば、上記したよう
に、透明導電膜形成用金属酸化物の各成分金属の少なく
とも1種の金属の微粒子又は該各成分金属からなる少な
くとも1種の合金の微粒子の分散液を被処理基板上に、
例えば、スピン塗布、スプレー塗布、インクジェット塗
布、浸漬塗布、ロールコート法、スクリーン印刷法等の
公知の方法を用いて塗布した後、酸化性雰囲気中で、通
常の透明導電膜形成用材料の微粒子を単体で焼結するの
に必要な温度(一般に、500〜700℃)よりはるかに
低温(150〜250℃)で加熱し、酸化と燒結とを同時
に行って成膜することにより透明導電膜が得られる。こ
の製造法において、燒結前に、分散液を塗布した基板を
所定の温度で乾燥してもよい。According to the present invention, as described above, fine particles of at least one metal of each component metal of the metal oxide for forming a transparent conductive film, or at least one alloy of each component metal. On the substrate to be treated,
For example, spin coating, spray coating, ink jet coating, dip coating, roll coating method, after applying a known method such as screen printing method, in an oxidizing atmosphere, fine particles of a normal transparent conductive film forming material A transparent conductive film is obtained by heating at a temperature (150 to 250 ° C.) far lower than the temperature required for sintering alone (generally 500 to 700 ° C.) and simultaneously performing oxidation and sintering to form a film. To be In this manufacturing method, the substrate coated with the dispersion may be dried at a predetermined temperature before sintering.
【0010】本発明における分散液は、上記微粒子を有
機溶媒に分散させたものである。用いる有機溶媒として
は、使用する微粒子によって適宜選択すればよく、例え
ば、次のようなものがある。すなわち、メタノール、エ
タノール、プロパノール、イソプロピルアルコール、及
びブタノール等のアルコール類、エチレングリコール等
のグリコール類、アセトン、メチルエチルケトン及びジ
エチルケトン等のケトン類、酢酸エチル、酢酸ブチル及
び酢酸ベンジル等のエステル類、メトキシエタノール及
びエトキシエタノール等のエーテルアルコール類、ジオ
キサン及びテトラヒドロフラン等のエーテル類、N,N
−ジメチルホルムアミド等の酸アミド類、トルエン、キ
シレン等の芳香族炭化水素類等を挙げることができる。
さらに、本発明では、この有機溶媒中には水も含まれる
ものとする。The dispersion in the present invention is a dispersion of the above fine particles in an organic solvent. The organic solvent to be used may be appropriately selected depending on the fine particles to be used, and examples thereof include the following. That is, alcohols such as methanol, ethanol, propanol, isopropyl alcohol and butanol, glycols such as ethylene glycol, ketones such as acetone, methyl ethyl ketone and diethyl ketone, esters such as ethyl acetate, butyl acetate and benzyl acetate, methoxy. Ether alcohols such as ethanol and ethoxyethanol, ethers such as dioxane and tetrahydrofuran, N, N
Examples thereof include acid amides such as dimethylformamide and aromatic hydrocarbons such as toluene and xylene.
Further, in the present invention, water is also included in this organic solvent.
【0011】上記有機溶媒の使用量は、使用する微粒子
に応じて、塗布しやすく、かつ所望の膜厚を得ることが
できるように適宜選択すればよい。例えば、溶媒に対し
微粒子1〜10wt%である。分散液を塗布する被処理
基板としての支持体には、通常用いられるガラス基板や
有機樹脂材料からなる基板を挙げることができ、その形
状としては平板、立体物、フィルム等であってもよい。
有機樹脂材料としては、例えば、セルロースアセテート
類、ポリスチレン、ポリエチレンテレフタレート、ポリ
スチレン類、ポリエーテル類、ポリイミド、エポキシ樹
脂、フェノキシ樹脂、ポリカーボネート、ポリフッ化ビ
ニリデン、テフロン(登録商標)等を用いることができ
る。これらを単独又は貼り合わせて支持体として用いて
もよい。この被処理基板は、分散液を塗布する前に、純
水や超音波等を用いて洗浄することが好ましい。The amount of the organic solvent used may be appropriately selected depending on the fine particles used so that the coating can be easily performed and a desired film thickness can be obtained. For example, the amount of fine particles is 1 to 10 wt% with respect to the solvent. Examples of the support as a substrate to be treated to which the dispersion liquid is applied include a glass substrate and a substrate made of an organic resin material that are commonly used, and the shape thereof may be a flat plate, a three-dimensional object, a film, or the like.
As the organic resin material, for example, cellulose acetate, polystyrene, polyethylene terephthalate, polystyrene, polyethers, polyimide, epoxy resin, phenoxy resin, polycarbonate, polyvinylidene fluoride, Teflon (registered trademark) and the like can be used. These may be used alone or as a support by laminating them. This substrate to be processed is preferably washed with pure water, ultrasonic waves or the like before applying the dispersion liquid.
【0012】本発明によれば、酸化性雰囲気中で所定の
温度で加熱することにより、酸化と焼結が同時に進行し
て透明導電膜の成膜が可能となる。この際に、金属微粒
子は、一般的な透明導電膜材料である金属酸化物の場合
よりもはるかに低温で緻密に焼結するため、低温で電気
抵抗の小さな透明導電膜を製造することができる。ま
た、焼結と酸化とは、酸化性雰囲気中で同時に行われ、
この際、同時にUVランプ照射を行うと、時間短縮・低
温化の面でさらに効果がある。されらにまた、本発明の
製造法には、大気圧プラズマ等を用いた、いわゆるプラ
ズマ焼結として知られている方法も有効である。According to the present invention, by heating at a predetermined temperature in an oxidizing atmosphere, oxidation and sintering proceed at the same time and a transparent conductive film can be formed. At this time, since the metal fine particles are densely sintered at a much lower temperature than in the case of a metal oxide which is a general transparent conductive film material, a transparent conductive film having a low electric resistance can be manufactured at a low temperature. . Further, sintering and oxidation are performed simultaneously in an oxidizing atmosphere,
At this time, irradiation with UV lamps at the same time is more effective in terms of time reduction and temperature reduction. Moreover, a method known as so-called plasma sintering using atmospheric pressure plasma or the like is also effective for the production method of the present invention.
【0013】[0013]
【実施例】以下、本発明の実施例を説明する。
(実施例1)Snを5%含むIn合金微粒子(粒径1μm
以下)を濃度が5重量%となるように酢酸n−ブチルに
分散して分散液を調製した。この分散液をスピンコート
法によりガラス基板に塗布した後、大気圧の酸素ガス雰
囲気中で250℃に加熱して、膜厚約150nmの透明
導電膜を形成した。得られた透明導電膜は緻密化し、以
下述べるように電気抵抗も小さい。上記製造法におい
て、加熱時間を5、10分、酸素ガス濃度を50、10
0容量%に設定して加熱し、得られた透明電導膜に対
し、シート抵抗(Ω/□)を測定した。その結果を表1に
示す。EXAMPLES Examples of the present invention will be described below. (Example 1) In alloy fine particles containing 5% Sn (particle size 1 μm
The following) was dispersed in n-butyl acetate to have a concentration of 5% by weight to prepare a dispersion liquid. This dispersion was applied on a glass substrate by spin coating and then heated to 250 ° C. in an oxygen gas atmosphere at atmospheric pressure to form a transparent conductive film having a film thickness of about 150 nm. The obtained transparent conductive film is densified and has a low electric resistance as described below. In the above manufacturing method, the heating time is 5 and 10 minutes, and the oxygen gas concentration is 50 and 10
The transparent conductive film thus obtained was heated at 0% by volume, and the sheet resistance (Ω / □) was measured. The results are shown in Table 1.
【0014】(表1) (Table 1)
【0015】表1から明らかなように、本実施例記載の
方法によれば、シート抵抗の低い透明導電膜が得られて
いる。このシート抵抗は、対照としてITO微粒子を大
気中で500℃で焼結して得られた透明導電膜のシート
抵抗(15〜30KΩ/□)と比べて、極めて低い値であ
った。その他の上記各成分金属微粒子を用いた場合も、
上記方法に従えば、低温燒結で同様に低いシート抵抗を
有する透明導電膜が得られる。As is clear from Table 1, according to the method described in this example, a transparent conductive film having a low sheet resistance was obtained. This sheet resistance was an extremely low value as compared with the sheet resistance (15 to 30 KΩ / □) of the transparent conductive film obtained by sintering ITO fine particles at 500 ° C. in the air as a control. In the case of using the other metal fine particles of each of the above,
According to the above method, a transparent conductive film having low sheet resistance can be obtained by sintering at low temperature.
【0016】(実施例2)Snを5%含むIn合金微粒
子(粒径1μm以下)を濃度が5重量%となるように酢
酸n−ブチルに分散して分散液を調製した。この分散液
をスピンコート法によりガラス基板に塗布した後、ヘリ
ウムガスに酸素ガスを添加した大気圧プラズマによるプ
ラズマ焼結(燒結条件:放電電力1KW、He+3%O
2、トータル流量10SLM、放電周波数13.56M
Hz)を行い、膜厚約150nmの透明導電膜を形成し
た。なお、酸素ガス添加量は、ヘリウムガスの3容量%
とした。また、ガラス基板に設けた熱電対により基板温
度を測定し、基板温度が250℃となるように大気圧プ
ラズマの放電電力及びプラズマヘッド−基板間距離を調
整した。Example 2 In alloy fine particles (particle size: 1 μm or less) containing 5% Sn were dispersed in n-butyl acetate to a concentration of 5% by weight to prepare a dispersion liquid. This dispersion was applied to a glass substrate by spin coating and then plasma-sintered by atmospheric pressure plasma in which oxygen gas was added to helium gas (sintering condition: discharge power 1 KW, He + 3% O
2 , total flow rate 10 SLM, discharge frequency 13.56M
Hz) to form a transparent conductive film having a film thickness of about 150 nm. The amount of oxygen gas added is 3% by volume of helium gas.
And Further, the substrate temperature was measured by a thermocouple provided on the glass substrate, and the discharge power of the atmospheric pressure plasma and the distance between the plasma head and the substrate were adjusted so that the substrate temperature was 250 ° C.
【0017】得られた透明導電膜は緻密化し、以下述べ
るように電気抵抗も小さい。上記製造方法において、加
熱時間を5、10、20分に設定して加熱し、得られた
透明電導膜に対し、シート抵抗(Ω/□)を測定した。そ
の結果を表2に示す。
(表2)
The transparent conductive film obtained is densified and has a low electric resistance as described below. In the above-mentioned manufacturing method, the heating time was set to 5, 10 and 20 minutes for heating, and the sheet resistance (Ω / □) of the obtained transparent conductive film was measured. The results are shown in Table 2. (Table 2)
【0018】表2から明らかなように、本実施例記載の
方法によれば、シート抵抗の低い透明導電膜が得られて
いる。このシート抵抗は、対照としてITO微粒子を大
気中で500℃で焼結して得られた透明導電膜のシート
抵抗(15〜30KΩ/□)と比べて、極めて低い値であ
った。その他の上記各成分金属微粒子を用いた場合も、
上記方法に従えば、低温燒結で同様に低いシート抵抗を
有する透明導電膜が得られる。As is apparent from Table 2, according to the method described in this example, a transparent conductive film having a low sheet resistance was obtained. This sheet resistance was an extremely low value as compared with the sheet resistance (15 to 30 KΩ / □) of the transparent conductive film obtained by sintering ITO fine particles at 500 ° C. in the air as a control. In the case of using the other metal fine particles of each of the above,
According to the above method, a transparent conductive film having low sheet resistance can be obtained by sintering at low temperature.
【0019】[0019]
【発明の効果】本発明の低抵抗透明導電膜の製造法によ
れば、透明導電膜形成用金属酸化物の各成分金属の微粒
子又はその合金の微粒子を用いて、酸化性雰囲気中で酸
化と燒結とを同時に行うので、低い焼結温度で、焼結後
の電気抵抗が小さい薄膜状透明導電膜を簡単な装置で安
価に製造することができる。According to the method for producing a low-resistance transparent conductive film of the present invention, fine particles of each component metal of the metal oxide for forming a transparent conductive film or fine particles of an alloy thereof are used to oxidize in an oxidizing atmosphere. Since the sintering is performed at the same time, the thin film transparent conductive film having a low electric resistance after sintering can be manufactured at a low sintering temperature at a low cost with a simple apparatus.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 石橋 暁 千葉県山武郡山武町横田523 株式会社ア ルバック千葉超材料研究所内 Fターム(参考) 2H092 HA04 MA05 MA06 MA10 NA25 PA01 3K007 AB05 AB18 CB01 DB03 FA01 5G323 BA01 BA02 BB02 BC01 BC03 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Akira Ishibashi 523 Yokota, Sanmu-cho, Sanmu-gun, Chiba Prefecture Lubac Chiba Institute for Materials Research F-term (reference) 2H092 HA04 MA05 MA06 MA10 NA25 PA01 3K007 AB05 AB18 CB01 DB03 FA01 5G323 BA01 BA02 BB02 BC01 BC03
Claims (3)
属の少なくとも1種の金属の微粒子又は該各成分金属か
らなる少なくとも1種の合金の微粒子の分散液を調製
し、この分散液を被処理基板上に塗布した後、大気圧の
酸素ガス若しくはオゾンガス雰囲気中、又は不活性ガス
に酸素ガス若しくはオゾンガスを添加したガスのプラズ
マ雰囲気中、150〜250℃で加熱し、酸化と燒結と
を同時に行い、金属酸化物からなる透明導電膜を形成す
ることを特徴とする低抵抗透明導電膜の製造法。1. A dispersion liquid of fine particles of at least one metal of each component metal of a metal oxide for forming a transparent conductive film or fine particles of at least one alloy of each component metal is prepared, and the dispersion liquid is prepared. After coating on the substrate to be processed, it is heated at 150 to 250 ° C. in an oxygen gas or ozone gas atmosphere at atmospheric pressure, or in a plasma atmosphere of a gas in which oxygen gas or ozone gas is added to an inert gas to oxidize and sinter. A method for producing a low-resistance transparent conductive film, which is performed at the same time to form a transparent conductive film made of a metal oxide.
錫、酸化亜鉛、酸化カドミウム、酸化ガリウム、In2
O3(ZnO)m、及びInGaO3(ZnO)m等や、こ
れら酸化物にドーパントを添加した錫添加酸化インジウ
ム(ITO)、アンチモン添加酸化錫(ATO)、亜鉛添加
酸化インジウム(IZO)及びアルミニウム添加酸化亜鉛
(AZO)から選ばれた金属酸化物の各成分金属の少なく
とも1種の金属の微粒子分散液又は該各成分金属からな
る少なくとも1種の合金の微粒子分散液であることを特
徴とする請求項1記載の低抵抗透明導電膜の製造法。2. The dispersion comprises indium oxide, tin oxide, zinc oxide, cadmium oxide, gallium oxide, In 2
O 3 (ZnO) m , InGaO 3 (ZnO) m, etc., tin added indium oxide (ITO) obtained by adding a dopant to these oxides, antimony added tin oxide (ATO), zinc added indium oxide (IZO) and aluminum Zinc oxide added
A fine particle dispersion of at least one metal of each component metal of a metal oxide selected from (AZO) or a fine particle dispersion of at least one alloy of each component metal. A method for producing a low-resistance transparent conductive film as described above.
性雰囲気中に紫外線照射を行うことを特徴とする請求項
1又は2記載の低抵抗透明導電膜の製造法。3. The method for producing a low resistance transparent conductive film according to claim 1, wherein in the steps of oxidizing and sintering, ultraviolet irradiation is performed in an oxidizing atmosphere.
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JP2006324105A (en) * | 2005-05-18 | 2006-11-30 | Sumitomo Osaka Cement Co Ltd | Transparent conductive film forming method and transparent conductive film |
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WO2011055856A1 (en) * | 2009-11-05 | 2011-05-12 | 住友金属鉱山株式会社 | Transparent conductive film and manufacturing method for same, element using same, transparent conductive substrate and device using same |
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JP2006324105A (en) * | 2005-05-18 | 2006-11-30 | Sumitomo Osaka Cement Co Ltd | Transparent conductive film forming method and transparent conductive film |
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