JPS63314714A - Manufacture of transparent electricity conducting film - Google Patents
Manufacture of transparent electricity conducting filmInfo
- Publication number
- JPS63314714A JPS63314714A JP15191287A JP15191287A JPS63314714A JP S63314714 A JPS63314714 A JP S63314714A JP 15191287 A JP15191287 A JP 15191287A JP 15191287 A JP15191287 A JP 15191287A JP S63314714 A JPS63314714 A JP S63314714A
- Authority
- JP
- Japan
- Prior art keywords
- film
- conducting film
- electricity conducting
- transparent electricity
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 230000005611 electricity Effects 0.000 title abstract 5
- 230000001678 irradiating effect Effects 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 11
- 239000011521 glass Substances 0.000 abstract description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052738 indium Inorganic materials 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 2
- 238000005245 sintering Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 150000002894 organic compounds Chemical class 0.000 description 7
- 238000000053 physical method Methods 0.000 description 6
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- ARHIRDSNQLUBHR-UHFFFAOYSA-K 2-ethylhexanoate;indium(3+) Chemical compound [In+3].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O ARHIRDSNQLUBHR-UHFFFAOYSA-K 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002736 metal compounds Chemical group 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は各種表示デバイス用電極材料、発熱体、熱線反
射材料などの目的に使用される透明導電膜の製造方法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for manufacturing transparent conductive films used for various purposes such as electrode materials for display devices, heating elements, and heat ray reflecting materials.
従来の技術
従来より、透明導電膜は各種表示デバイス用電極、発熱
体、熱線反射材料などの目的に使用されてきた。BACKGROUND OF THE INVENTION Conventionally, transparent conductive films have been used for various purposes such as electrodes for display devices, heating elements, and heat ray reflective materials.
従来のこれら透明導電膜は主として蒸着、スパッタ等の
物理的手法により製造されてきたが、装置コストや生産
性等の向上を目的として金属を含有した有機化合物の熱
分解による製造方法の研究も広く行なわれている。Conventionally, these transparent conductive films have been mainly manufactured using physical methods such as vapor deposition and sputtering, but research has also been widely conducted on manufacturing methods using thermal decomposition of organic compounds containing metals, with the aim of improving equipment costs and productivity. It is being done.
発明が解決しようとする問題点
しかしながら、金属を含有した有機化合物の熱分解によ
る製造方法においては生成した透明導電膜の導電性が蒸
着、スパッタ等の物理的手法のよるものに比して劣るも
のであった。Problems to be Solved by the Invention However, the conductivity of the produced transparent conductive film is inferior to that produced by physical methods such as vapor deposition and sputtering in the manufacturing method by thermal decomposition of organic compounds containing metals. Met.
それ故に、本発明の目的は金属を含有した有機化合、物
の熱分解による製造方法における利点を維持しつつ、物
理的手法により得られる透明導電膜により近い導電性を
有する透明導電膜の製造方法を提供することである。Therefore, the object of the present invention is to maintain the advantages of the manufacturing method by thermal decomposition of metal-containing organic compounds and materials, and to produce a transparent conductive film having conductivity closer to that obtained by physical methods. The goal is to provide the following.
問題点を解決するだめの手段
本発明においては上記、金属を含有した有機化合物の熱
分解による透明導電膜の製造方法における問題を解決す
るための手段として、熱分解、焼結の完了した透明導電
膜に空気中で、または空気との接触を遮断した状態で紫
外線を発生するランプで光を照射して抵抗値の調節をす
ることを特徴とする。すなわち、上記照射により透明導
電膜の抵抗値が製造直後よりも著しく低下し、物理的手
法により製造されたものにより近い抵抗値の透明導電膜
が得られる。Means for Solving the Problems In the present invention, as a means for solving the problems in the above-mentioned method for manufacturing a transparent conductive film by thermal decomposition of an organic compound containing a metal, a transparent conductive film that has been thermally decomposed and sintered is used. It is characterized by adjusting the resistance value by irradiating the film with light from a lamp that generates ultraviolet rays in the air or in a state where contact with the air is blocked. That is, the resistance value of the transparent conductive film is significantly lowered by the above-mentioned irradiation than that immediately after production, and a transparent conductive film having a resistance value closer to that produced by a physical method can be obtained.
従来より、例えば特公昭６０−１９６１０号公報に記載
されているごとく、金属含有有機化合物の熱分解の過程
において、または熱分解の予備工程として紫外線により
有機化合物の結合を切断して熱分解を補助しようとする
考えはあり、かつ現在、主として使用されている酸化イ
ンジウムや酸化スズ等は光導電性を有するゆえに紫外線
の照射によシ抵抗値を低下させようとする試みは良く行
なわれているが、実際には単に紫外線照射による抵抗値
低下は一時的なものであって例えば、１日放置すること
によシ抵抗値は元の値またはそれに近い値にまで戻る傾
向にあった。Conventionally, as described in Japanese Patent Publication No. 60-19610, thermal decomposition has been assisted by breaking the bonds of organic compounds with ultraviolet rays during the process of thermal decomposition of metal-containing organic compounds or as a preliminary step for thermal decomposition. There are ideas to lower the resistance value of the materials currently used, such as indium oxide and tin oxide, which have photoconductivity. However, in reality, the decrease in resistance value due to UV irradiation is only temporary, and the resistance value tends to return to its original value or a value close to it by leaving it for one day, for example.
本発明者らは上記熱分解型により製造された透明導電膜
を空気中でまたは空気との接触を遮断した状態で紫外線
を発生するランプで一定時間以上光を照射することによ
り、上記透明導電膜の抵抗値が低下し、かつ、低下した
抵抗値が安定に持続することを見いだし、本発明に至っ
たものである。The present inventors irradiated the transparent conductive film produced by the above pyrolysis method with light for a certain period of time using a lamp that generates ultraviolet rays in the air or with the contact with the air cut off. The inventors have discovered that the resistance value of the material decreases, and that the decreased resistance value continues stably, leading to the present invention.
ここに使用される紫外線を発生するランプとしては通常
紫外線の発生に使用されている低圧、中圧、高圧、超高
圧水銀灯やキセノンランプ、ハライドランプ等が使用で
きるが、紫外線のみでなく、可視光線、赤外線も同時に
発生するものが好ましい。すなわち、紫外線のみの照射
では永続的な抵抗値の低下は期待できない。The lamps that generate ultraviolet rays used here can include low-pressure, medium-pressure, high-pressure, and ultra-high-pressure mercury lamps, xenon lamps, and halide lamps, which are normally used to generate ultraviolet rays, but in addition to ultraviolet rays, visible rays can also be used. , one that also generates infrared rays at the same time is preferable. That is, irradiation with only ultraviolet rays cannot be expected to permanently reduce the resistance value.
紫外線を発生するランプによる照射時間は最低でも１分
間は必要であって、十分な効果を必要とする場合は３分
間以上の照射が好ましい。The irradiation time using a lamp that generates ultraviolet rays is required to be at least 1 minute, and if a sufficient effect is required, irradiation for 3 minutes or more is preferred.
上記ランプによる照射時の雰囲気は通常の空気中でも良
いが、空気を遮断して照射すると更に良好な結果が得ら
れる。The atmosphere during irradiation with the above lamp may be normal air, but even better results can be obtained if irradiation is performed with air blocked.
上記、照射時の空気遮断条件としては特に厳しい条件は
不要であって、実施例で示す通９、プラスチックスフィ
ルム、紙、ガラス板、セラミックス板、金属板などで透
明導電膜表面を覆うだけで十分な効果があるため、大量
生産にも十分に対応できる有用な手段と言える。As mentioned above, there is no need for particularly severe air-blocking conditions during irradiation; simply cover the surface of the transparent conductive film with a plastic film, paper, glass plate, ceramic plate, metal plate, etc. as shown in Example 9. Since it is sufficiently effective, it can be said to be a useful method that can be used for mass production.
本発明にかかる抵抗値低下処理をした透明導電膜は処理
後もプラスチックスフィルム製の袋に保存する程度の簡
単な保管条件で抵抗値の増加もなく安定なものである。The transparent conductive film subjected to the resistance value lowering treatment according to the present invention remains stable without any increase in resistance value even after treatment under simple storage conditions such as storing in a plastic film bag.
作用
金属を含有した有機化合物の熱分解により製造した透明
導電膜に、空気中で、または空気との接触を遮断した状
態で紫外線を発生するランプで最低１分間以上光を照射
することによシ、透明導電膜の抵抗値が低下し、かつ、
低下した抵抗値が安定に持続するため、物理的手法で作
られた透明導電膜と同等の特性の透明導電膜が得られる
。A transparent conductive film produced by thermal decomposition of an organic compound containing a working metal is irradiated with light for at least 1 minute using a lamp that generates ultraviolet light in the air or in a state where contact with the air is blocked. , the resistance value of the transparent conductive film decreases, and
Since the reduced resistance value remains stable, a transparent conductive film with properties equivalent to those made by physical methods can be obtained.
本発明にかかる処理による抵抗値低下の機構としては、
熱分解により生じた酸化物超微粒子の表面に強く吸着さ
れた酸素原子またはイオンが紫外線を放射するランプの
照射による紫外線および熱振動により脱着されるものと
推定される。透明導電膜に吸着された酸素量および、脱
着後の酸素含有量は実施例に述べるごとく還元ガス中に
おける熱分析や、ラザフォード後方散乱の測定によシ実
測することができる。The mechanism of resistance value reduction due to the treatment according to the present invention is as follows:
It is presumed that oxygen atoms or ions strongly adsorbed on the surface of ultrafine oxide particles produced by thermal decomposition are desorbed by ultraviolet rays and thermal vibrations caused by irradiation from a lamp that emits ultraviolet rays. The amount of oxygen adsorbed on the transparent conductive film and the oxygen content after desorption can be measured by thermal analysis in reducing gas or measurement of Rutherford backscattering, as described in the Examples.
実施例 以下、実施例により説明する。Example Examples will be explained below.
実施例１
２−エチルヘキサン酸インジウムに６モルチの２−エチ
ルヘキサン酸スズを添加し、石油系溶剤に溶解してイン
キを製造した。本インキをガラス板上に印刷してのち、
５３０’Ｃで焼成して透明導電膜を製造した。Example 1 An ink was prepared by adding 6 mol of tin 2-ethylhexanoate to indium 2-ethylhexanoate and dissolving it in a petroleum solvent. After printing this ink on a glass plate,
A transparent conductive film was manufactured by firing at 530'C.
本透明導電膜に直接、または透明導電膜を有する側のガ
ラス面上に各種材料を載せて３０ｃｍの距離よりＩ Ｋ
ｗ高圧水銀灯で照射した結果を表１に示す。なお、表１
中で耐熱性の不十分な材料の場合およびセラばツクス、
金属板のごとき不透明な材料の場合は透明導電膜の反対
側のガラス面より照射した。IK from a distance of 30 cm by placing various materials directly on the transparent conductive film or on the glass surface on the side with the transparent conductive film.
Table 1 shows the results of irradiation with a high-pressure mercury lamp. In addition, Table 1
In the case of materials with insufficient heat resistance in and ceramics,
In the case of an opaque material such as a metal plate, the light was irradiated from the glass surface on the opposite side of the transparent conductive film.
続いて、表１においてポリイミドフィルムを介して照射
したサンプルと、焼成したままのサンプルの２種につい
て還元ガス中の熱重量分析とラザフォード後方散乱の測
定を行なった。Subsequently, in Table 1, thermogravimetric analysis in reducing gas and Rutherford backscattering measurements were performed on two types of samples: the sample irradiated through the polyimide film and the as-fired sample.
この結果、どちらの測定においても照射サンプルにおい
てはインジウム１原子当り１．５個の酸素原子が観測さ
れたのに対し、焼成したままのサンプルにおいてはイン
ジウム１原子当り２個の酸素原子が観測された。As a result, in both measurements, 1.5 oxygen atoms per indium atom were observed in the irradiated sample, whereas 2 oxygen atoms were observed per indium atom in the as-fired sample. Ta.
この結果よシ、金属化合物の熱分解時に過剰に吸着され
た酸素原子が本発明にかかる処理により脱着して化合物
本来の抵抗値にまで低下するものと推察される。As a result, it is inferred that the oxygen atoms excessively adsorbed during the thermal decomposition of the metal compound are desorbed by the treatment according to the present invention, and the resistance value is reduced to the original resistance value of the compound.
実施例２
実施例１において高圧水銀灯に代えてＩ Ｋｗのキセノ
ンランプを使用した場合も実施例１と同様の結果が得ら
れた。Example 2 The same results as in Example 1 were obtained when an I Kw xenon lamp was used in place of the high-pressure mercury lamp in Example 1.
（以下余 白）
表 １
発明の効果
以上実施例および比較例から判るごとく、本発明にかか
る透明導電膜の製造方法は極めて簡単な方法で熱分解透
明導電膜の抵抗値を低下でき、その抵抗値も従来の物理
的手法によるものと同等のものであり、産業上の効果は
大である。(Leaving space below) Table 1 Effects of the Invention As can be seen from the Examples and Comparative Examples, the method for producing a transparent conductive film according to the present invention can reduce the resistance value of a pyrolyzed transparent conductive film in an extremely simple manner. The values are also equivalent to those obtained by conventional physical methods, and the industrial effects are significant.
Claims (2)
光を照射して抵抗値の調節を行う透明導電膜の製造方法
。(1) A method for producing a transparent conductive film in which the resistance value is adjusted by irradiating light with a lamp that generates ultraviolet rays for at least 1 minute.
間以上光を照射して抵抗値の調節を行う特許請求の範囲
第１項に記載の透明導電膜の製造方法。(2) The method for manufacturing a transparent conductive film according to claim 1, wherein the resistance value is adjusted by irradiating light for at least 1 minute or more in a state where contact with air is cut off.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62151912A JP2589695B2 (en) | 1987-06-18 | 1987-06-18 | Method for producing transparent conductive film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62151912A JP2589695B2 (en) | 1987-06-18 | 1987-06-18 | Method for producing transparent conductive film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63314714A true JPS63314714A (en) | 1988-12-22 |
| JP2589695B2 JP2589695B2 (en) | 1997-03-12 |
Family
ID=15528911
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62151912A Expired - Fee Related JP2589695B2 (en) | 1987-06-18 | 1987-06-18 | Method for producing transparent conductive film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2589695B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008041551A1 (en) * | 2006-10-02 | 2008-04-10 | National Institute Of Advanced Industrial Science And Technology | Method for fabricating transparent conductive tin oxide film |
| JP2012174600A (en) * | 2011-02-23 | 2012-09-10 | Fujifilm Corp | Method for producing conductive sheet, conductive sheet and touch panel |
| US8963146B2 (en) | 2009-11-05 | 2015-02-24 | Sumitomo Metal Mining Co., Ltd. | Method of manufacturing transparent conductive film, the transparent conductive substrate using the film, as well as device using the substrate |
| US9701849B2 (en) | 2010-02-17 | 2017-07-11 | Sumitomo Metal Mining Co., Ltd. | Method of manufacturing transparent conductive film, the transparent conductive film, element and transparent conductive substrate using the film, as well as device using the substrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5684809A (en) * | 1979-12-14 | 1981-07-10 | Hitachi Ltd | Method of forming transparent conductive film |
| JPS59193488A (en) * | 1983-04-19 | 1984-11-02 | シチズン時計株式会社 | Manufacture of panel substrate for display body |
| JPS61290421A (en) * | 1985-06-19 | 1986-12-20 | Hitachi Ltd | Production of liquid crystal display element |
-
1987
- 1987-06-18 JP JP62151912A patent/JP2589695B2/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5684809A (en) * | 1979-12-14 | 1981-07-10 | Hitachi Ltd | Method of forming transparent conductive film |
| JPS59193488A (en) * | 1983-04-19 | 1984-11-02 | シチズン時計株式会社 | Manufacture of panel substrate for display body |
| JPS61290421A (en) * | 1985-06-19 | 1986-12-20 | Hitachi Ltd | Production of liquid crystal display element |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008041551A1 (en) * | 2006-10-02 | 2008-04-10 | National Institute Of Advanced Industrial Science And Technology | Method for fabricating transparent conductive tin oxide film |
| JP5057476B2 (en) * | 2006-10-02 | 2012-10-24 | 独立行政法人産業技術総合研究所 | Manufacturing method of tin oxide transparent conductive film |
| US8963146B2 (en) | 2009-11-05 | 2015-02-24 | Sumitomo Metal Mining Co., Ltd. | Method of manufacturing transparent conductive film, the transparent conductive substrate using the film, as well as device using the substrate |
| US9701849B2 (en) | 2010-02-17 | 2017-07-11 | Sumitomo Metal Mining Co., Ltd. | Method of manufacturing transparent conductive film, the transparent conductive film, element and transparent conductive substrate using the film, as well as device using the substrate |
| JP2012174600A (en) * | 2011-02-23 | 2012-09-10 | Fujifilm Corp | Method for producing conductive sheet, conductive sheet and touch panel |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2589695B2 (en) | 1997-03-12 |
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