JP3286954B2 - Method for producing tin-added indium oxide ternary functional film - Google Patents
Method for producing tin-added indium oxide ternary functional filmInfo
- Publication number
- JP3286954B2 JP3286954B2 JP28210696A JP28210696A JP3286954B2 JP 3286954 B2 JP3286954 B2 JP 3286954B2 JP 28210696 A JP28210696 A JP 28210696A JP 28210696 A JP28210696 A JP 28210696A JP 3286954 B2 JP3286954 B2 JP 3286954B2
- Authority
- JP
- Japan
- Prior art keywords
- tin
- indium oxide
- substrate
- functional film
- film
- 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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Links
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- Surface Treatment Of Glass (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Non-Insulated Conductors (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は高配向性、低抵抗及
び透明性を有するために透明電極ばかりでなく結晶基板
としても各種デバイスや機能性結晶膜の形成に適した錫
添加酸化インジウム膜及びその製造方法に関する。The present invention relates to a tin-doped indium oxide film which has high orientation, low resistance and transparency and is suitable not only as a transparent electrode but also as a crystal substrate for forming various devices and functional crystal films. It relates to the manufacturing method.
【０００２】[0002]
【従来技術】半導体デバイスや機能性薄膜を形成する結
晶基板として、バルク結晶から切り出した基板を用いる
ことが一般であるが、バルク単結晶を出発素材とする場
合、バルク単結晶素材が高価であり、このような素材か
らスライスして必要とする結晶方位の材料に加工する際
の素材の歩留が低く、経済的でない等の問題があった。
また、スライスする際に生じる結晶歪みなどの影響も無
視できなかった。2. Description of the Related Art Generally, a substrate cut from a bulk crystal is used as a crystal substrate for forming a semiconductor device or a functional thin film. However, when a bulk single crystal is used as a starting material, the bulk single crystal material is expensive. However, when such a material is sliced and processed into a material having a required crystal orientation, the yield of the material is low, and there is a problem that it is not economical.
In addition, the influence of crystal distortion generated during slicing could not be ignored.
【０００３】これに対して、ガラスなどの基板上に必要
とする結晶方位の薄膜を直接形成することによって、経
済的でかつ素材結晶の形態に制約されない、任意の結晶
方位を有する結晶基板を得ることが提案されており、こ
のような基板として、ガラス基板上に酸化錫膜（ＴＯ）
を形成した基板がある。しかしながら、ガラス基板上に
形成された酸化錫膜の結晶性が基板の表面性状の影響を
強く受けるということから、前記したような単結晶に替
わり得るような結晶配向性のものを得ることが困難であ
った。基板の材質としては、デバイスや構造上の利点か
らガラスや酸化ケイ素などの透明非晶質のものが用いら
れるが、これらの表面の構造が非晶質であることから、
その影響によって、スパッター法などによって酸化錫膜
を形成しても、酸化錫膜の結晶成長が阻害され、好適な
結晶面の配向特性の膜が得られなかった。On the other hand, by directly forming a thin film having the required crystal orientation on a substrate such as glass, a crystal substrate having an arbitrary crystal orientation that is economical and is not restricted by the form of the material crystal is obtained. It has been proposed that a tin oxide film (TO) is formed on a glass substrate as such a substrate.
There is a substrate on which is formed. However, since the crystallinity of the tin oxide film formed on the glass substrate is strongly affected by the surface properties of the substrate, it is difficult to obtain a crystal orientation that can replace the single crystal as described above. Met. As the material of the substrate, a transparent amorphous material such as glass or silicon oxide is used for device and structural advantages, but since the structure of these surfaces is amorphous,
Due to the influence, even if a tin oxide film is formed by a sputtering method or the like, the crystal growth of the tin oxide film is inhibited, and a film having a suitable crystal plane orientation characteristic cannot be obtained.
【０００４】しかし、本発明者等は、先にスプレー熱分
解法によりガラス基板上に高配向の酸化錫膜を形成し得
ることを見い出したが、この酸化錫膜は、その配向性及
び透明性に優れたものであるが、抵抗率が８．８×１０
~1Ωｃｍであり、導電性が要求される用途には高過ぎる
抵抗値を示す欠点があった。そこで、酸化錫膜（ＴＯ）
について、その電気的抵抗を低くするため、アンチモン
（Ｓｂ）やフッ素（Ｆ）を添加することは知られている
が、これらの添加元素を含む酸化錫膜（ＡＴＯ、ＦＴ
Ｏ）は電気抵抗は小さいが、結晶の配向性も低下してし
まうため、デバイスの特性から好ましいものではなかっ
た。このように基板上に形成する酸化錫膜において、低
抵抗でかつ高結晶配向性の両者の特性を実現することは
困難であった。However, the present inventors have previously found that a highly oriented tin oxide film can be formed on a glass substrate by a spray pyrolysis method. But with a resistivity of 8.8 × 10
11 Ωcm, which is a drawback in that the resistance is too high for applications requiring conductivity. Therefore, tin oxide film (TO)
It is known to add antimony (Sb) or fluorine (F) in order to lower the electrical resistance of the film. However, tin oxide films (ATO, FT) containing these added elements are known.
O) is not preferable in view of the characteristics of the device because the electrical resistance is small, but the crystal orientation is also reduced. As described above, it is difficult to realize both characteristics of low resistance and high crystal orientation in the tin oxide film formed on the substrate.
【０００５】しかし、本発明者は、基板上に形成する酸
化錫膜において、低抵抗でかつ高結晶配向性の両者の特
性を実現するため、ガラス基板上にジブチル錫ジアセテ
ートの熱分解法によって（２００）面に選択的に配向し
た酸化錫膜（ＴＯ）を形成し、この酸化錫膜上に、アン
チモン又はフッ素等の錫又は酸素より最外殻電子数が一
つ多い元素を含み、且つ、（２００）面に選択的に配向
した酸化錫膜（ＴＯ）を形成した酸化錫とすることによ
って一応の解決を見た。However, in order to realize both low resistance and high crystal orientation characteristics in a tin oxide film formed on a substrate, the present inventor has proposed a method of thermally decomposing dibutyltin diacetate on a glass substrate. Forming a selectively oriented tin oxide film (TO) on the (200) plane, containing on the tin oxide film an element having one more outermost shell electron than tin or oxygen such as antimony or fluorine, and A tentative solution was found by using tin oxide in which a selectively oriented tin oxide film (TO) was formed on the (200) plane.
【０００６】他方、錫添加酸化インジウム（ＩＴＯ）膜
も透明電極として、透明電極として表示ディスプレーを
初めとして電子デバイスにいろいろ利用されている。し
かし、この場合もまた、酸化錫膜同様の問題があった。On the other hand, a tin-doped indium oxide (ITO) film is also used as a transparent electrode, and as a transparent electrode, is variously used in electronic devices such as display displays. However, also in this case, there was a problem similar to the tin oxide film.
【０００７】[0007]
【発明が解決しようとする課題】そこで、本発明者は、
錫添加酸化インジウム（ＩＴＯ）膜について、高配向
性、低抵抗及び透明性の三元機能を有する錫添加酸化イ
ンジウム（ＩＴＯ）膜を得べく種々検討した結果、本発
明を完成したもので、本発明の目的は、高配向性、低抵
抗及び透明性の三元機能を有する錫添加酸化インジウム
（ＩＴＯ）膜及び基板上に高度に配向した低抵抗及び透
明性の錫添加酸化インジウム膜を容易に且つ確実に製膜
することを可能にする錫添加酸インジウム膜の製造方法
を提供する。Therefore, the present inventor has proposed:
As a result of various studies on a tin-doped indium oxide (ITO) film having a ternary function of high orientation, low resistance, and transparency, the present invention was completed. An object of the present invention is to easily form a tin-doped indium oxide (ITO) film having a ternary function of high orientation, low resistance and transparency and a highly oriented low-resistance and transparency tin-doped indium oxide film on a substrate. Provided is a method for producing a tin-added indium oxide film that enables reliable film formation.
【０００８】[0008]
【課題を解決するための手段】請求項１の発明の要旨
は、有機インジウム化合物及び有機錫化合物を含有する
アルコール溶液を、Ｉｎ原子１００に対してＳｎ原子５
〜３０の割合になるように、加熱された基板上に間歇的
に噴霧して、（１１１）面配向を有し、８０％以上の光
透過率及び１．０×１０ -3 〜１．０×１０ -4 Ωｃｍとい
う低抵抗を有する錫添加酸化インジウム三元機能膜の製
造方法であり、好ましい有機インジウム化合物がＩｎ
（Ｃ5Ｈ7Ｏ2）3 であり、有機錫化合物が（Ｃ4Ｈ9）2Ｓ
ｎ（ＯＣＯＣＨ3）2 である。Summary of the Invention for 請 Motomeko 1 Means for Solving the Problems] is an alcohol solution containing the organic indium compound and an organic tin compound, Sn atom relative In atoms 100 5
Intermittently on a heated substrate to a ratio of ~ 30
Was sprayed on, (111) has a plane orientation of 80% or more of light
Transmittance and 1.0 × 10 −3 to 1.0 × 10 −4 Ωcm
Of Tin-doped Indium Oxide Ternary Functional Film with Low Resistance
A manufacturing method, organic indium compound has preferably an In
(C 5 H 7 O 2 ) 3 and the organotin compound is (C 4 H 9 ) 2 S
n (OCOCH 3) 2.
【０００９】[0009]
【発明の実施の形態】次に本発明について詳細に述べ
る。本発明で使用する有機インジウム化合物及び有機錫
化合物として使用できるものは有機溶剤に可溶性を有す
るものであれば、何れでも可能であるが、特に好ましい
化合物としては有機インジウム化合物としてはＩｎ（Ｃ
5Ｈ7Ｏ2）3、有機錫化合物として（Ｃ4Ｈ9）2Ｓｎ（Ｏ
ＣＯＣＨ3）2である。そして、両者の割合としてＩｎ原
子１００に対してＳｎ原子５〜３０の割合で使用する。
そして、この際に使用し得る有機溶媒としては有機イン
ジウム化合物及び有機錫化合物を溶解するものであれば
良く、特に制約はないが、好ましい有機溶媒としてはア
ルコール類化合物であり、特に好ましい溶媒はエチルア
ルコールである。Next, the present invention will be described in detail. As the organic indium compound and the organic tin compound used in the present invention, any compounds can be used as long as they have solubility in an organic solvent, but a particularly preferable compound is In (C
5 H 7 O 2 ) 3 , (C 4 H 9 ) 2 Sn (O
COCH 3) is 2. And, as the ratio of both, Sn atoms are used in a ratio of 5 to 30 with respect to 100 In atoms.
The organic solvent that can be used at this time is not particularly limited as long as it can dissolve the organic indium compound and the organic tin compound, but a preferable organic solvent is an alcohol compound, and a particularly preferable solvent is ethyl. Alcohol.
【００１０】本発明では先ず、上記の有機インジウム化
合物と有機錫化合物とを含有する原料溶液を作る。この
場合、原料溶液としては有機インジウム化合物を１〜４
重量％含有するものが好ましい。原料溶液を基板に噴霧
させるに際しては、基板としてはガラス板を使用し、基
板の温度としては通常４５０〜５００℃前後に保ち、一
回の噴霧量は０．５ｃｍ3であって、所定の厚さになる
ように１０〜１００回程度繰り返して行う。噴霧によっ
て基板温度が低下するため基板の温度低かが１０℃程度
以下になるように、噴霧は時間間隔をおいて行う。In the present invention, first, a raw material solution containing the above-mentioned organic indium compound and organic tin compound is prepared. In this case, as the raw material solution, the organic indium compound is 1 to 4
What contains by weight is preferable. When the raw material solution is sprayed on the substrate, a glass plate is used as the substrate, and the temperature of the substrate is usually maintained at around 450 to 500 ° C., and the amount of one spray is 0.5 cm 3 , and a predetermined thickness is applied. The process is repeated about 10 to 100 times so as to obtain the best results. The spraying is performed at intervals so that the temperature of the substrate is reduced to about 10 ° C. or less because the temperature of the substrate is reduced by the spraying.
【００１１】このような操作によって得られた錫添加酸
化インジウム被膜は高度の配向性及び透明性を有し、低
抵抗であって、例えば２５ｍｍ×２５ｍｍ、膜厚２００
ｎｍという大面積化が可能となり、透明電極として表示
ディスプレイをはじめとして電子デバイスにいろいろ使
用することが可能である。The tin-added indium oxide film obtained by such an operation has a high degree of orientation and transparency, has low resistance, and has a thickness of, for example, 25 mm × 25 mm and a thickness of 200 mm.
A large area of nm can be achieved, and the transparent electrode can be used in a variety of electronic devices including display displays.
【００１２】[0012]
【実施例及び比較例】次に実施例をもって本発明を更に
具体的に説明する。 実施例１ Ｉｎ（Ｃ5Ｈ7Ｏ2）3及びＩｎに対するＳｎの比が８原子
％の量の（Ｃ4Ｈ9）2Ｓｎ（ＯＣＯＣＨ3）2をエタノー
ルに溶解し、３重量％の溶液を調整した。この溶液を５
００℃に熱したガラス基板に噴霧した。このとき、ガラ
ス基板の温度が低下し過ぎないように時間間隔をおい
て、溶液の噴霧を膜厚が２００ｎｍになるまで繰り返し
た後、自然冷却した。配向度を次式で評価した。Examples and Comparative Examples Next, the present invention will be described more specifically with reference to examples. Example 1 In (C 5 H 7 O 2 ) 3 and (C 4 H 9 ) 2 Sn (OCOCH 3 ) 2 in an amount of 8 atomic% of Sn to In were dissolved in ethanol to prepare a 3 % by weight solution. Was adjusted. This solution is
It was sprayed on a glass substrate heated to 00 ° C. At this time, spraying of the solution was repeated at time intervals so that the temperature of the glass substrate did not excessively decrease until the film thickness became 200 nm, and then cooled naturally. The degree of orientation was evaluated by the following equation.
【００１３】[0013]
【数１】 (Equation 1)
【００１４】ここでＩ（ｈｋ１）及びＩ0（ｈｋ１）は
それぞれ（ｈｋ１）面のＸ線回析強度及びＪＣＰＤＳの
標準強度である。得られた膜についてα＝６３％となり
（１１１）面に強い選択配向が生じたことを示した。ま
たこのとき抵抗率は３．５×１０~4Ωｃｍという低い値
を示し、可視域での光透過率も８０％以上であった。Here, I (hk1) and I 0 (hk1) are the X-ray diffraction intensity of the (hk1) plane and the standard intensity of JCPDS, respectively. Α = 63% for the obtained film, indicating that strong selective orientation occurred on the (111) plane. At this time, the resistivity showed a low value of 3.5 × 10 to 4 Ωcm, and the light transmittance in the visible region was 80% or more.
【００１５】実施例２ Ｉｎに対するＳｎの比が３２原子％の量の（Ｃ4Ｈ9）2
Ｓｎ（ＯＣＯＣＨ3）2をエタノールに溶解し、その他の
条件は実施例１と同じにして製膜を行った。得られた膜
についてα＝８０％となり（１１１）面に更に強い選択
配向が生じたことを示した。またこのとき抵抗率は１．
０×１０~3Ωｃｍという低い値を示し、可視域での光透
過率も８０％以上であった。Example 2 (C 4 H 9 ) 2 with a ratio of Sn to In of 32 atomic%
Sn (OCOCH 3 ) 2 was dissolved in ethanol, and the other conditions were the same as in Example 1 to form a film. Α = 80% was obtained for the obtained film, indicating that stronger selective orientation occurred on the (111) plane. At this time, the resistivity is 1.
It showed a low value of 0 × 10 to 3 Ωcm, and the light transmittance in the visible region was 80% or more.
【００１６】[0016]
【発明の効果】以上述べたように、本発明は、例えば、
Ｉｎ（Ｃ5Ｈ7Ｏ2）3及び（Ｃ4Ｈ9）2Ｓｎ（ＯＣＯＣ
Ｈ3）2を含有するアルコール溶液を、加熱された基板上
に噴霧、熱分解することによって高度の配向性を有し、
透明性に優れ、また低抵抗の錫添加酸化インジウム膜を
製膜することができ、大面積化が可能であって各種の電
子ディバイスに利用することができる。As described above, the present invention provides, for example,
In (C 5 H 7 O 2 ) 3 and (C 4 H 9 ) 2 Sn (OCOC
A high degree of orientation by spraying and pyrolyzing an alcohol solution containing H 3 ) 2 onto a heated substrate;
A tin-added indium oxide film having excellent transparency and low resistance can be formed, and can have a large area, and can be used for various electronic devices.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平４−276078（ＪＰ，Ａ) 特開 昭60−157109（ＪＰ，Ａ) 特開 平６−150724（ＪＰ，Ａ) 特開 平８−253318（ＪＰ，Ａ) 特開 平７−122766（ＪＰ，Ａ) 特開 平７−25615（ＪＰ，Ａ) 特開 昭63−89436（ＪＰ，Ａ) 兼安一成 外３名，スプレー法により 作成した酸化インジウム膜の電気的，光 学的特性，電気化学および工業物理化 学，日本，Ｖｏｌ．55，Ｎｏ．３，ｐ. 245−250 (58)調査した分野(Int.Cl.7，ＤＢ名) C30B 1/00 - 35/00 C01G 15/00 C01G 19/00 C03C 17/25 H01B 5/14 H01B 13/00 ＣＡ（ＳＴＮ) ＪＩＣＳＴファイル（ＪＯＩＳ)──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-4-276078 (JP, A) JP-A-60-157109 (JP, A) JP-A-6-150724 (JP, A) JP-A 8- 253318 (JP, A) JP-A-7-122766 (JP, A) JP-A-7-25615 (JP, A) JP-A-63-89436 (JP, A) Electrical and optical properties of the prepared indium oxide film, electrochemical and industrial physics, Japan, Vol. 55, No. 3, p. 245-250 (58) Fields investigated (Int. Cl. 7 , DB name) C30B 1/00-35/00 C01G 15/00 C01G 19/00 C03C 17/25 H01B 5/14 H01B 13 / 00 CA (STN) JICST file (JOIS)
Claims (1)
Ｏ 2 ） 3 及び有機錫化合物として（Ｃ 4 Ｈ 9 ） 2 Ｓｎ（ＯＣ
ＯＣＨ 3 ） 2 を含有するアルコール溶液を、Ｉｎ原子１０
０に対してＳｎ原子５〜３０の割合になるように、加熱
された基板上に間歇的に噴霧して、（１１１）面配向を
有し、８０％以上の光透過率及び１．０×１０-3〜１．
０×１０-4Ωｃｍという低抵抗を有する錫添加酸化イン
ジウム三元機能膜の製造方法。1. An organic indium compound comprising In (C 5 H 7)
O 2 ) 3 and (C 4 H 9 ) 2 Sn (OC
The alcohol solution containing OCH 3 ) 2 was washed with 10 In atoms.
It is intermittently sprayed onto a heated substrate so as to have a Sn atom ratio of 5 to 30 with respect to 0, has a (111) plane orientation, a light transmittance of 80% or more, and 1.0 × 10 -3 to 1.
A method for producing a tin-added indium oxide ternary functional film having a low resistance of 0 × 10 −4 Ωcm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28210696A JP3286954B2 (en) | 1996-10-24 | 1996-10-24 | Method for producing tin-added indium oxide ternary functional film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28210696A JP3286954B2 (en) | 1996-10-24 | 1996-10-24 | Method for producing tin-added indium oxide ternary functional film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10130097A JPH10130097A (en) | 1998-05-19 |
| JP3286954B2 true JP3286954B2 (en) | 2002-05-27 |
Family
ID=17648210
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28210696A Expired - Fee Related JP3286954B2 (en) | 1996-10-24 | 1996-10-24 | Method for producing tin-added indium oxide ternary functional film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3286954B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4260494B2 (en) | 2002-02-26 | 2009-04-30 | 株式会社フジクラ | Manufacturing method of transparent electrode substrate, manufacturing method of photoelectric conversion element, and manufacturing method of dye-sensitized solar cell |
| DE602004007089T2 (en) | 2003-11-14 | 2008-02-21 | Sharp K.K. | Apparatus for producing thin films |
| JP2007289874A (en) * | 2006-04-25 | 2007-11-08 | Matsushita Electric Works Ltd | Coating application method |
| JP2012150904A (en) * | 2011-01-17 | 2012-08-09 | Sharp Corp | Transparent conductive film |
-
1996
- 1996-10-24 JP JP28210696A patent/JP3286954B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 兼安一成 外３名，スプレー法により作成した酸化インジウム膜の電気的，光学的特性，電気化学および工業物理化学，日本，Ｖｏｌ．５５，Ｎｏ．３，ｐ．２４５−２５０ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10130097A (en) | 1998-05-19 |
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