JPH0751745B2 - Method for producing transparent conductive film - Google Patents
Method for producing transparent conductive filmInfo
- Publication number
- JPH0751745B2 JPH0751745B2 JP63198882A JP19888288A JPH0751745B2 JP H0751745 B2 JPH0751745 B2 JP H0751745B2 JP 63198882 A JP63198882 A JP 63198882A JP 19888288 A JP19888288 A JP 19888288A JP H0751745 B2 JPH0751745 B2 JP H0751745B2
- Authority
- JP
- Japan
- Prior art keywords
- target
- transparent conductive
- conductive film
- substrate
- sputtering
- 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 - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3421—Cathode assembly for sputtering apparatus, e.g. Target using heated targets
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroluminescent Light Sources (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Electric Cables (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は液晶表示装置等に使用されるIn１−ＸSnx系透
明導電膜の製造方法及び製造装置に関する。TECHNICAL FIELD The present invention relates to a method and an apparatus for manufacturing an In 1-X Snx-based transparent conductive film used in a liquid crystal display device or the like.
（従来の技術） 従来、この種の透明導電膜の製造方法として、スパッタ
法、蒸着法、CVD法等が知られており、該透明導電膜の
用途によってこれらの方法のうち適当な方法を採用して
いる。このうちスパッタ法は、In−Sn合金ターゲットを
用いる場合と、In2O3−SnO2系配化物ターゲットを用い
る場合とがあるが、導電性と光透過率が安定した膜が得
られる利点のある後者の方が多く使われている。(Prior Art) Conventionally, as a method for producing this kind of transparent conductive film, a sputtering method, a vapor deposition method, a CVD method, etc. have been known, and an appropriate method among these methods is adopted depending on the use of the transparent conductive film. is doing. Among the sputtering method, the case of using the In-Sn alloy target, there are a case of using In 2 O 3 -SnO 2 based distribution product target, conductivity and light transmittance of the advantages stable film can be obtained The latter one is used more often.
後者のスパッタ法について更に説明すると、In2O3−SnO
2系酸化物ターゲットをCuやSUS製のバッキングプレート
に低融点金属のロウ材によりボンティングし、そのバッ
キングプレートを真空室内の基板と対向するスパッタカ
ソードに取付け、該カソードに負の電圧を印加してスパ
ッタを行う。この場合、該真空室には、プラズマ放電を
発生させるためのガスとして、Ar等の不活性ガスにO2ガ
スを適当量含有させた混合ガスが導入される。そしてO2
ガスの混合量を変化させ、最適の導電性と光透過率をも
った透明導電膜を基板上に得る。この際、ターゲット
は、Arイオンによりボンバードされて発熱するので、バ
ッキングプレートの背面から水冷される。To further explain the latter sputtering method, In 2 O 3 --SnO
A 2 type oxide target is bonded to a Cu or SUS backing plate with a brazing material of a low melting point metal, the backing plate is attached to a sputter cathode facing the substrate in the vacuum chamber, and a negative voltage is applied to the cathode. To sputter. In this case, a mixed gas of an inert gas such as Ar containing an appropriate amount of O 2 gas is introduced into the vacuum chamber as a gas for generating plasma discharge. And O 2
By changing the mixed amount of gas, a transparent conductive film having optimum conductivity and light transmittance is obtained on the substrate. At this time, the target is bombarded by Ar ions and generates heat, so that the target is water-cooled from the back surface of the backing plate.
（発明が解決しようとする課題） 前記従来のスパッタ法で透明導電膜を製造する場合、連
続的にスパッタを行なっていると、In2O3−SnO2系酸化
物ターゲットの表面が黒色に変色し、その程度や面積が
スパッタ時間とともに増加する現象が起る。そして、そ
の結果、基板上への透明導電膜の析出速度が低下し、作
製した該膜の導電性と光透過率が悪化するという問題が
生ずる。(Problems to be Solved by the Invention) When a transparent conductive film is manufactured by the conventional sputtering method, if the sputtering is continuously performed, the surface of the In 2 O 3 —SnO 2 -based oxide target turns black. However, there occurs a phenomenon that the degree and the area increase with the sputtering time. Then, as a result, the deposition rate of the transparent conductive film on the substrate decreases, and the conductivity and the light transmittance of the prepared film deteriorate.
この問題の原因について、発明者は種々の検討の結果、
次のようなことであることが究明された。即ち、前記タ
ーゲットの表面の黒色物は、In（Sn）Ｏの組成に近い非
晶質の物質で、InやSnは２価になっているものが多く、
その電気抵抗はIn2O3やSnO2に較べて極めて高いこと、
そして該黒色物は、スパッタ中にターゲットより飛び出
したInやSn原子がＯ原子と共に再度ターゲット表面に析
出することにより生成され、一旦この物質が生成する
と、電気抵抗が高いためスパッタされにくく、その上に
続々と析出するので、スパッタ時間と共に黒色物が増加
し、これに伴なって析出速度が低下すること、が原因で
あると分かった。従って、長時間連続して多数枚の基板
に順次透明導電膜を作製している時には、その膜厚が徐
々に薄くなるという問題が生じる。Regarding the cause of this problem, the inventor has made various studies and found that
It has been clarified that it is as follows. That is, the black substance on the surface of the target is an amorphous substance having a composition close to that of In (Sn) O, and In and Sn are often divalent.
Its electrical resistance is extremely higher than that of In 2 O 3 and SnO 2 ,
The black matter is generated by the precipitation of In and Sn atoms, which are ejected from the target during sputtering, again on the surface of the target together with O atoms. Once this substance is generated, it is difficult to be sputtered because of its high electric resistance. It was found that the cause is that black matter increases with the sputtering time, and the deposition rate decreases with the increase in the spattering time. Therefore, when a transparent conductive film is successively formed on a large number of substrates continuously for a long period of time, there arises a problem that the film thickness is gradually reduced.
また該黒色非晶物質も幾分スパッタされ、該膜中に混入
するが、該物質は電気抵抗が高く黒色であるため、形成
される透明導電膜の導電性と透過率が悪化する原因であ
ることも分った。特に透過率の悪化の問題は基板の温度
が低い場合に著しい。Further, the black amorphous substance is also sputtered to some extent and mixes into the film, but since the substance has a high electric resistance and is black, it is a cause of deterioration of conductivity and transmittance of the transparent conductive film to be formed. I also understood that. Particularly, the problem of deterioration of the transmittance is remarkable when the temperature of the substrate is low.
本発明は、In１−ＸSnx系透明導電膜の製造に伴なう前
記問題点を解決する製造方法と装置を提案することを目
的とするものである。It is an object of the present invention to propose a manufacturing method and apparatus for solving the above problems associated with manufacturing an In 1-X Snx-based transparent conductive film.
（課題を解決するための手段） 本発明では、In2O3−SnO2系酸化物ターゲットを高温に
加熱して該ターゲットの表面に非晶質物質が析出するこ
とを抑制しながら該ターゲットをスパッタし、基板上に
In１−ＸSnx酸化物系（０≦ｘ≦１）透明導電膜を形成
することにより、導電性と光透過率の良い透明導電膜を
迅速に作製するようにした。(Means for Solving the Problems) In the present invention, an In 2 O 3 —SnO 2 -based oxide target is heated to a high temperature to suppress the precipitation of an amorphous substance on the surface of the target while controlling the target. Sputter on the substrate
By forming an In 1-X Snx oxide-based (0 ≦ x ≦ 1) transparent conductive film, a transparent conductive film having good conductivity and light transmittance was promptly produced.
（作用） 真空室内の基板に対向して設けられたスパッタカソード
上にIn2O3−SnO2系酸化物ターゲットを設け、該真空室
内にO2ガスを混入したArガスを導入し、該カソードに負
の電位を与えてスパッタにより該基板上に透明導電膜を
形成することは従来の場合と同様であるが、本発明で
は、この場合該ターゲットをヒータ又は熱媒体による加
熱装置で100℃以上に加熱し乍らスパッタするもので、
この加熱により該ターゲット上に前記従来のもののよう
な黒色の非晶質物質が析出することが防止される。これ
は、該非晶質物質は、非平衡物質であるため、100℃以
上では存在できないためであり、100℃以上では結晶質
のIn2O3−SnO2になるか或はわずかの金属InとIn2O3−Sn
O2になる。そして金属InはIn2O3−SnO2にくらべてスパ
ッタ率が高いので、すぐスパッタされてしまい、ターゲ
ット上に析出しない。(Function) An In 2 O 3 —SnO 2 -based oxide target is provided on the sputter cathode provided to face the substrate in the vacuum chamber, Ar gas mixed with O 2 gas is introduced into the vacuum chamber, and the cathode is introduced. It is the same as the conventional case to form a transparent conductive film on the substrate by applying a negative potential to the substrate by sputtering, but in the present invention, in this case, the target is 100 ° C. or higher by a heater or a heating device using a heating medium. It is heated to and sputtered,
This heating prevents deposition of a black amorphous substance on the target, unlike the conventional one. This is because the amorphous substance is a non-equilibrium substance and cannot exist at 100 ° C. or higher, and becomes crystalline In 2 O 3 —SnO 2 at 100 ° C. or higher, or a slight amount of metallic In. In 2 O 3 −Sn
It becomes O 2 . The metal In Due to the high sputtering rate as compared with In 2 O 3 -SnO 2, will be immediately sputtered, not deposited on the target.
従って基板上に析出するIn2O3−SnO2は、ターゲットと
同質の物質であるから、導電性に富み、透過性もよく比
較的迅速に透明導電膜を形成出来る。Therefore, since In 2 O 3 —SnO 2 deposited on the substrate is a substance of the same quality as the target, it is rich in conductivity, has good permeability, and can form a transparent conductive film relatively quickly.
（実施例） 本発明の実施例を別紙図面につき説明するに、第１図及
び第２図に於て、符号（１）は、適当な真空排気手段に
接続される排気口（２）と、ArガスにO2ガスを混入した
スパッタガスの導入口（３）を備えた真空室、（４）及
び（５）は該真空室（１）内に互に対向して設けた基板
及びスパッタカソードを示し、該基板（４）の背後にこ
れを加熱するヒータ（６）を設けるようにした。また該
スパッタカソード（５）はバッキングプレート（７）の
背後に磁石（８）を収容した容筐（９）を備えるものと
し、該磁石（８）により該バッキングプレート（７）の
前面にロウ材でボンディングしたIn2O3−SnO3系酸化物
ターゲット（10）の表面に磁界を形成してマグネトロン
式のスパッタを行なえるようにした。（11）はアースシ
ールド、（12）は防着板である。(Embodiment) An embodiment of the present invention will be described with reference to the attached drawings. In FIGS. 1 and 2, reference numeral (1) indicates an exhaust port (2) connected to an appropriate vacuum exhaust means, A vacuum chamber provided with a sputtering gas inlet (3) in which O 2 gas is mixed with Ar gas, and (4) and (5) are a substrate and a sputtering cathode provided in the vacuum chamber (1) so as to face each other. The heater (6) for heating the substrate (4) is provided behind the substrate (4). Further, the sputter cathode (5) is provided with a housing (9) which houses a magnet (8) behind the backing plate (7), and the magnet (8) allows a brazing material on the front surface of the backing plate (7). A magnetic field was formed on the surface of the In 2 O 3 —SnO 3 based oxide target (10) bonded in step 2 so that magnetron-type sputtering could be performed. (11) is an earth shield, and (12) is a protective plate.
該ターゲット（10）は、第１図示の場合、ターゲット
（10）の前方に設けたシース型ニクロム線ヒータやタン
タル線ヒータ等のヒータ（13）により100℃以上に加熱
されるようにし、この場合、該容筐（９）に冷却水を配
管（14）（14）を介して循環させ、バッキングプレート
（７）を水冷した。該ヒータ（13）は可変変圧器に接続
され、加熱温度を調節するように構成される。In the case of the first illustration, the target (10) is heated to 100 ° C. or higher by a heater (13) such as a sheath type nichrome wire heater or a tantalum wire heater provided in front of the target (10). Then, cooling water was circulated through the casing (9) through the pipes (14) and (14) to cool the backing plate (7) with water. The heater (13) is connected to a variable transformer and is configured to regulate the heating temperature.
第２図示の場合、該ターゲット（10）は、高融点のロウ
材によりバッキングプレート（７）にボンディングさ
れ、その背後の容筐（９）に配管（14）（14）を介して
循環される例えばオイル系の耐熱温度が300℃以上の熱
媒体（15）により加熱され、この場合、好ましくは該熱
媒体は自動温度調節式の加熱器により加熱される。In the case of the second illustration, the target (10) is bonded to the backing plate (7) with a high melting point brazing material, and circulated in the container (9) behind it through the pipes (14) (14). For example, the oil system is heated by a heat medium (15) having a heat resistant temperature of 300 ° C. or higher. In this case, the heat medium is preferably heated by an automatic temperature control type heater.
第１図示の装置に於いて、カソード（５）に、現在最も
代表的なIn2O3に10％SnO2が混入した酸化物ターゲット
（10）を設置し、ヒータ（13）で全く加熱せずに25時間
の連続スパッタを行ない、ターゲット（10）の表面に充
分に黒色の非晶質物質を析出させた。この状態ではター
ゲト（10）の表面に抵抗の大きい非晶質物質が析出して
いるので、スパッタ時の放電インピーダンスが高い。具
体的には、真空室（１）のArガス圧が５×10-3Torr、導
入酸素ガス分圧が４×10-5Torr、ターゲット（10）の寸
法が５インチ×16インチである場合、410V一定で放電さ
せると、上記黒色状態のターゲット（10）では、放電電
流が1.9Aであった。In the apparatus shown in FIG. 1, an oxide target (10) containing 10% SnO 2 mixed with In 2 O 3 which is the most typical one at present is installed on the cathode (5) and heated by a heater (13). Without doing this, continuous sputtering was carried out for 25 hours to sufficiently deposit a black amorphous substance on the surface of the target (10). In this state, since the amorphous substance having a high resistance is deposited on the surface of the target (10), the discharge impedance during sputtering is high. Specifically, when the Ar gas pressure in the vacuum chamber (1) is 5 × 10 -3 Torr, the introduced oxygen gas partial pressure is 4 × 10 -5 Torr, and the target (10) dimensions are 5 inches × 16 inches. When the target (10) in the black state was discharged at a constant voltage of 410 V, the discharge current was 1.9 A.
次に、基板（４）を代え、ヒータ（13）で加熱して黒色
のターゲット（10）の表面を50℃から200℃まで順次加
熱して30分間保持し、前記具体例と同条件で410Vで放電
させて電流値を測定した。ターゲット（10）の表面温度
はサーモラベルを用いて測定した。その結果は第３図示
の如くであった。この結果から分かるように、100℃よ
り放電電流の増大の効果が表われはじめ、150℃以上で
は一定となり、2.2Aの電流が得られた。そして、この放
電の後には、ターゲット（10）の表面に析出していた黒
色物質は消失していた。この時の基板（４）に形成され
た透明導電膜の析出速度、電気抵抗率及び550nmにおけ
る光透過率は第４図示の如くであった。尚、基板（４）
の温度は200℃一定とした。ターゲット（10）の加熱用
ヒータ（13）によっても基板（４）が加熱されるので、
あらかじめ基板（４）の温度が200℃になるように、そ
れぞれのターゲット表面温度に対して基板加熱ヒータ
（６）の出力を調節した。Next, the substrate (4) is replaced, and the surface of the black target (10) is heated from 50 ° C to 200 ° C by heating with the heater (13) and held for 30 minutes, and 410 V under the same conditions as the above specific example. Was discharged and the current value was measured. The surface temperature of the target (10) was measured using a thermo label. The result was as shown in FIG. As can be seen from this result, the effect of increasing the discharge current began to appear from 100 ° C, and became constant at 150 ° C or higher, and a current of 2.2 A was obtained. Then, after this discharge, the black substance deposited on the surface of the target (10) disappeared. At this time, the deposition rate of the transparent conductive film formed on the substrate (4), the electrical resistivity and the light transmittance at 550 nm were as shown in FIG. The substrate (4)
The temperature was constant at 200 ° C. Since the substrate (4) is also heated by the heater (13) for heating the target (10),
The output of the substrate heater (6) was adjusted in advance for each target surface temperature so that the temperature of the substrate (4) reached 200 ° C.
第４図の結果から明らかなように、ターゲット（10）の
温度が100℃から析出速度は増加し、電気抵抗率は減少
し、光透過率は増加する。そして150℃以上で一定とな
る。As is clear from the results of FIG. 4, when the temperature of the target (10) is 100 ° C., the deposition rate increases, the electrical resistivity decreases, and the light transmittance increases. And it becomes constant above 150 ℃.
第２図示のカソード（３）を使用して前記の場合と同様
の実験を行なったが、同様の結果が得られた。An experiment similar to the above was carried out using the cathode (3) shown in FIG. 2, but similar results were obtained.
（発明の効果） 以上のように本発明の方法によるときは、In2O3−SnO3
系酸化物ターゲットを100℃以上に加熱し乍らスパッタ
するようにしたので、該ターゲット上に黒色物質を析出
することなくスパッタを行なえ、迅速に透明導電膜を製
造できると共に導電性と光透過性の良い透明導電膜が得
られる効果がある。(Effects of the Invention) As described above, when the method of the present invention is used, In 2 O 3 —SnO 3
Since the system oxide target was heated to 100 ° C or higher for sputtering, sputtering can be performed without precipitating a black substance on the target, and a transparent conductive film can be rapidly manufactured, and conductivity and light transmission can be achieved. There is an effect that a good transparent conductive film can be obtained.
第１図及び第２図は本発明の方法の実施に使用した製造
装置の断面図、第３図はターゲットの温度と放電電流の
関係を示す線図、第４図は本発明の方法により作製され
た透明導電膜の特性を示す線図である。 （１）……真空室、（４）……基板 （10）……In2O3−SnO2系酸化物ターゲット （13）……ヒータ、（15）……熱媒体1 and 2 are cross-sectional views of a manufacturing apparatus used for carrying out the method of the present invention, FIG. 3 is a diagram showing the relationship between the temperature of the target and the discharge current, and FIG. 4 is prepared by the method of the present invention. It is a diagram which shows the characteristic of the transparent conductive film which was carried out. (1) …… Vacuum chamber, (4) …… Substrate (10) …… In 2 O 3 —SnO 2 type oxide target (13) …… Heater, (15) …… Heating medium
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭62−186417（ＪＰ，Ａ) 特開 昭62−93804（ＪＰ，Ａ) 特開 昭61−47645（ＪＰ，Ａ) 特開 昭63−162864（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-62-186417 (JP, A) JP-A-62-93804 (JP, A) JP-A-61-47645 (JP, A) JP-A-63- 162864 (JP, A)
Claims (1)
加熱して該ターゲットの表面に非晶質物質が析出するこ
とを抑制しながら該ターゲットをスパッタし、基板上に
In１−ＸSnx酸化物系（０≦ｘ≦１）透明導電膜を形成
することを特徴とする透明導電膜の製造方法。1. An In 2 O 3 —SnO 2 -based oxide target is heated to a high temperature to sputter the target while suppressing precipitation of an amorphous substance on the surface of the target.
A method of manufacturing a transparent conductive film, which comprises forming an In 1-X Snx oxide-based (0 ≦ x ≦ 1) transparent conductive film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63198882A JPH0751745B2 (en) | 1988-08-11 | 1988-08-11 | Method for producing transparent conductive film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63198882A JPH0751745B2 (en) | 1988-08-11 | 1988-08-11 | Method for producing transparent conductive film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0250951A JPH0250951A (en) | 1990-02-20 |
| JPH0751745B2 true JPH0751745B2 (en) | 1995-06-05 |
Family
ID=16398496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63198882A Expired - Fee Related JPH0751745B2 (en) | 1988-08-11 | 1988-08-11 | Method for producing transparent conductive film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0751745B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100101937A1 (en) * | 2008-10-29 | 2010-04-29 | Applied Vacuum Coating Technologies Co., Ltd. | Method of fabricating transparent conductive film |
| KR20120093952A (en) * | 2009-11-06 | 2012-08-23 | 가부시키가이샤 한도오따이 에네루기 켄큐쇼 | Method for manufacturing semiconductor element and semiconductor device, and deposition apparatus |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6042629B2 (en) * | 1976-09-20 | 1985-09-24 | 日本プレシジヨン・サ−キツツ株式会社 | Input/output protection circuit for MOS integrated circuits |
| US4299678A (en) * | 1979-07-23 | 1981-11-10 | Spin Physics, Inc. | Magnetic target plate for use in magnetron sputtering of magnetic films |
| JPS6147645A (en) * | 1984-08-15 | 1986-03-08 | Toshiba Corp | Formation of thin film |
| JPH0664935B2 (en) * | 1985-10-18 | 1994-08-22 | ティーディーケイ株式会社 | Transparent conductive film and method for forming the same |
| JPS62186417A (en) * | 1986-02-10 | 1987-08-14 | 日本板硝子株式会社 | Manufacture of transparent conductive film |
| JPH086177B2 (en) * | 1986-12-26 | 1996-01-24 | 松下電器産業株式会社 | Reactive sputtering method |
| JPH01132760A (en) * | 1987-11-19 | 1989-05-25 | Matsushita Electric Ind Co Ltd | Sputter film deposition method and film deposition equipment |
-
1988
- 1988-08-11 JP JP63198882A patent/JPH0751745B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0250951A (en) | 1990-02-20 |
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