JPS60200959A - Production of transparent conductive film - Google Patents

Production of transparent conductive film

Info

Publication number
JPS60200959A
JPS60200959A JP5550484A JP5550484A JPS60200959A JP S60200959 A JPS60200959 A JP S60200959A JP 5550484 A JP5550484 A JP 5550484A JP 5550484 A JP5550484 A JP 5550484A JP S60200959 A JPS60200959 A JP S60200959A
Authority
JP
Japan
Prior art keywords
indium
sputtering
transparent conductive
oxide
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.)
Pending
Application number
JP5550484A
Other languages
Japanese (ja)
Inventor
Kenji Okamoto
謙次 岡元
Takuya Yoshimi
琢也 吉見
Masayuki Wakitani
雅行 脇谷
Kiyotake Sato
佐藤 精威
Terunobu Miura
三浦 照信
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujitsu Ltd
Original Assignee
Fujitsu Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Fujitsu Ltd filed Critical Fujitsu Ltd
Priority to JP5550484A priority Critical patent/JPS60200959A/en
Publication of JPS60200959A publication Critical patent/JPS60200959A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process
    • C23C14/548Controlling the composition

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

PURPOSE:To form a transparent conductive film consisting of indium tin oxide (ITO) having low resistance with good reproducibility by using a mass spectrometric device in such a way that the specified mass spectral ratio between indium and indium oxide is maintained at all times during sputtering. CONSTITUTION:A mass spectrometric device 2 is connected to a chamber 1 of a sputtering device and the spectral intensities of the oxide of indium and indium are taken out of the device 2 and the ratio thereof is monitored in the stage of producing an ITO film by reactive two-pole DC sputtering. A control circuit 4 for controlling a constant current source 5 according to the result thereof is provided and sputtering is executed while the specified ratio of the indium/indium oxide is maintained. The ITO film having low resistance is produced with good reproducibility by the above-mentioned method and the yield is improved.

Description

【発明の詳細な説明】 (1)発明の技術分野 本発明は酸化インジウム錫(ITo)透明導電膜の製造
方法に係り、特に反応性二極直流スパッタリングにより
ITO膜を製造する場合、常時スパッタリング中のイン
ジウムとインジウム酸化物の質量スペクトル比をモニタ
し、再現性よく低抵抗のITO膜を作製することのでき
る透明導電膜の製造方法に関する。
Detailed Description of the Invention (1) Technical Field of the Invention The present invention relates to a method for manufacturing an indium tin oxide (ITo) transparent conductive film, and in particular, when manufacturing an ITO film by reactive bipolar direct current sputtering, it is necessary to constantly perform sputtering. The present invention relates to a method for producing a transparent conductive film that can produce a low-resistance ITO film with good reproducibility by monitoring the mass spectrum ratio of indium and indium oxide.

(2)技術の背景 液晶パネル、プラズマディスプレ等の電極として透明導
電膜が使用されている。この透明導電膜の材料として酸
化錫、酸化インジウム、酸化インジウム錫(ITO)等
があり、その製造方法も蒸着法やスパッタリング法が使
用される。
(2) Background of the technology Transparent conductive films are used as electrodes in liquid crystal panels, plasma displays, and the like. Materials for this transparent conductive film include tin oxide, indium oxide, indium tin oxide (ITO), etc., and vapor deposition and sputtering methods are used for manufacturing the film.

本発明は低抵抗性や透明度が比較的良好で、よく使用さ
れるI’T Oに関するものである。
The present invention relates to I'T O, which is frequently used because of its low resistance and relatively good transparency.

(3)従来技術と問題点 従来金属ターゲットを出発材料として用い、反応性スパ
ッタリングによりITO膜を作製する場合、良好な特性
(抵抗率や透明度)を持つ秋を作製できる条件の範囲が
非常に狭く、再現性よく良好な膜を作ることがきわめて
困難である。
(3) Conventional technology and problems When conventionally producing an ITO film by reactive sputtering using a metal target as a starting material, the range of conditions under which a film with good properties (resistivity and transparency) can be produced is very narrow. It is extremely difficult to make a good film with good reproducibility.

さらにターゲットとして使用するインジウム−錫合金の
表面の酸化の程度によって最適なITO膜が得られる条
件が変化する。従って全く同じ条件でスパツクしたつも
りでも得られた膜の特性は大きく変化して再現性が悪い
Furthermore, the conditions for obtaining an optimal ITO film vary depending on the degree of oxidation on the surface of the indium-tin alloy used as a target. Therefore, even if the film is spun under exactly the same conditions, the properties of the resulting film vary greatly and reproducibility is poor.

なおITO膜の特性はスパッタリングレートに依存し、
この為スパッタリング雰囲気中のアルゴンとインジウム
の発光強度比を用いてスパッタリングレートを制御すれ
ば再現性が向上することが最近報告されているが、この
方法であると、■ アルゴンとインジウムの発光を取り
出す窓にITO膜が蒸着されて色が付くため長時間に亘
りスパッタリングする場合はスパッタリングレー1〜が
正確に制御できない。
Note that the characteristics of the ITO film depend on the sputtering rate.
For this reason, it has recently been reported that reproducibility can be improved by controlling the sputtering rate using the emission intensity ratio of argon and indium in the sputtering atmosphere. Since the ITO film is vapor-deposited on the window and colored, sputtering grays 1 to 1 cannot be accurately controlled when sputtering is performed for a long time.

■ アルゴンとインジウムの発光強度比はスパッタリン
グガス圧の変化に対するスパッタリングレートの変化と
対応しないのでスパッタリングガス圧の安定性を向上さ
せなくてはならないという問題点がある。
(2) Since the emission intensity ratio of argon and indium does not correspond to the change in sputtering rate with respect to the change in sputtering gas pressure, there is a problem that the stability of sputtering gas pressure must be improved.

(4)発明の目的 本発明の目的は上記問題点を解決するもので、質量分析
器を用いスパソクリングチェンハー内のインジウム酸化
物、インジウムの分圧を監視し、インジウム酸化物/イ
ンジウムの比が當に一定となるようにし、酸化インジウ
ム膜中の酸素空孔濃度をコントロールし、より正確な酸
素空孔濃度のコントロールを実現し再現性を向上させる
ことにある。
(4) Purpose of the Invention The purpose of the present invention is to solve the above-mentioned problems, and to monitor the partial pressure of indium oxide and indium in the spa cleaning chamber using a mass spectrometer. The purpose is to control the oxygen vacancy concentration in the indium oxide film by keeping the ratio constant, thereby realizing more accurate control of the oxygen vacancy concentration and improving reproducibility.

(5)発明の構成 上記本発明の目的は、反応性スパッタリングにより酸化
インジウム錫透明導電薄膜を製造する装置において、該
装置に質量分析装置を接続し、該質量分析装置により測
定されるインジウムとインジウムの酸化状態の質量スペ
クトル強度比を一定に保ちつつスパッタリングすること
を特徴とする透明導電膜の製造方法により達成される。
(5) Structure of the Invention The object of the present invention is to provide an apparatus for manufacturing an indium tin oxide transparent conductive thin film by reactive sputtering, in which a mass spectrometer is connected to the apparatus, and indium and indium are measured by the mass spectrometer. This is achieved by a method for producing a transparent conductive film, which is characterized by performing sputtering while keeping the mass spectrum intensity ratio of the oxidation state constant.

(6)発明の実施例 次に図面により本発明の詳細な説明する。(6) Examples of the invention Next, the present invention will be explained in detail with reference to the drawings.

第1図は本発明の実施例によるスパッタリング装置の構
成図、第2図はスパッタリングレートと抵抗率の関係を
示すグラフを示す。
FIG. 1 is a block diagram of a sputtering apparatus according to an embodiment of the present invention, and FIG. 2 is a graph showing the relationship between sputtering rate and resistivity.

第1図に示すように本発明では直流二極スパッタリング
装置のチェンバー1に質量分析装置2を接続し、質量分
析器2からインジウムの酸化物とインジウムとのスペク
トル強度を取り出し、その比をモニタし、その結果によ
り定電流電源5を制御する制御則rj!I4を設置する
。この場合質量分析器のヘッド3はアルゴンプラズマ中
においた方がよい。スパッタリングはチェンバー内にア
ルゴン十酸素(10%)のガスを導入して行ない、ター
ゲット6はインジウム−tFU、 (10%)合金を用
い、ガス圧は5X10−”torrである。
As shown in Figure 1, in the present invention, a mass spectrometer 2 is connected to the chamber 1 of a DC bipolar sputtering device, and the spectral intensities of indium oxide and indium are extracted from the mass spectrometer 2, and the ratio thereof is monitored. , a control law rj! that controls the constant current power supply 5 based on the result. Install I4. In this case, it is better to place the head 3 of the mass spectrometer in argon plasma. Sputtering is carried out by introducing a gas of argon and oxygen (10%) into the chamber, the target 6 is an indium-tFU (10%) alloy, and the gas pressure is 5 x 10-'' torr.

着膜レートとインジウム/インジウム酸化物の比は比例
することがわかっているので、予め着膜レートとインジ
ウム/インジウム酸化物の比の関係を言周ベーζおいて
、スパックリングパワーを2周整して着膜レーI・が1
80人/分になるインジウム/インジウム酸化物の比に
セットする。
Since it is known that the film deposition rate and the ratio of indium/indium oxide are proportional, the relationship between the film deposition rate and the ratio of indium/indium oxide is set in advance as a term base ζ, and the sputtering power is adjusted by two rounds. Then, the deposition layer I is 1
Set the indium/indium oxide ratio to be 80 people/min.

本発明では第2図に示すように100〜250人/分に
着膜レートを設定することにより、良品レベルである4
×10〜4Ω−cm以下の透明導電膜(ドI”0膜)が
再現性よ(得られる。
In the present invention, as shown in Fig. 2, by setting the film deposition rate to 100 to 250 people/min, 4
A transparent conductive film (do I"0 film) having a resistance of 10 to 4 Ω-cm can be obtained with good reproducibility.

なお■′「0の反応性スパッタリングではターゲット6
の状態(酸化の程度)によって放電状態のインピーダン
スが変化し放電電圧が常に変化するため手動または自動
制御により着膜レートのコートロールを行なう。
In addition, in the case of reactive sputtering with
Since the impedance of the discharge state changes depending on the state (degree of oxidation) and the discharge voltage constantly changes, the film deposition rate is coated by manual or automatic control.

本発明は金属ターゲットを用いた反応性スパックリング
を高周波により行なう場合にも通用できる。
The present invention can also be applied to the case where reactive spackling using a metal target is performed using high frequency waves.

(7)発明の効果 本発明によれば低抵抗のITO膜を極めて再現性よく製
造することが可能なql、歩留りが向上し低コスト化に
効果がある。
(7) Effects of the Invention According to the present invention, it is possible to manufacture a low-resistance ITO film with extremely good reproducibility, the yield is improved, and costs are reduced.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は本発明の実施例によるスパッタリング装置構成
図、第2図はスパッタリングレー1〜と抵 ゛抗率の関
係のグラフを示す。 図において1はチェンバー、2は質量分析装置。 3はヘッド、4は制御回路、5ば定電流電源装置。 6はターゲット、を示す。
FIG. 1 is a block diagram of a sputtering apparatus according to an embodiment of the present invention, and FIG. 2 is a graph showing the relationship between sputtering arrays 1 and 1 and resistivity. In the figure, 1 is a chamber, and 2 is a mass spectrometer. 3 is a head, 4 is a control circuit, and 5 is a constant current power supply device. 6 indicates a target.

Claims (1)

【特許請求の範囲】[Claims] 反応性スパッタリングにより酸化インジウム錫透明導電
薄膜を製造する装置において、該装置に質量分析装置を
接続し、該質量分析装置により測定されるインジウムと
インジウムの酸化状態の質量スペクトル強度比を一定に
保ちつつスパッタリングすることを特徴とする透明導電
膜の製造方法。
In an apparatus for producing an indium tin oxide transparent conductive thin film by reactive sputtering, a mass spectrometer is connected to the apparatus, and the mass spectrometer intensity ratio of indium and the oxidation state of indium as measured by the mass spectrometer is kept constant. A method for producing a transparent conductive film, characterized by sputtering.
JP5550484A 1984-03-23 1984-03-23 Production of transparent conductive film Pending JPS60200959A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5550484A JPS60200959A (en) 1984-03-23 1984-03-23 Production of transparent conductive film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5550484A JPS60200959A (en) 1984-03-23 1984-03-23 Production of transparent conductive film

Publications (1)

Publication Number Publication Date
JPS60200959A true JPS60200959A (en) 1985-10-11

Family

ID=13000493

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5550484A Pending JPS60200959A (en) 1984-03-23 1984-03-23 Production of transparent conductive film

Country Status (1)

Country Link
JP (1) JPS60200959A (en)

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