JP2013204074A - Transparent conductive film and method for manufacturing the same - Google Patents
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Abstract
Description
本発明は、ＩＴＯ並みに低抵抗な透明導電膜及びその製造方法に関する。 The present invention relates to a transparent conductive film as low as ITO and a method for producing the same.
液晶ディスプレイ等のフラットパネルディスプレイ用の透明導電膜として、通常ＩＴＯ（Indium Tin Oxide：酸化インジウムスズ）が用いられている。このＩＴＯでは、Ｉｎを使用するため、資源的に将来不足する可能性があり、その代替材料としてＡＺＯ(Al-Zn-O：Aluminum doped Zinc Oxide：アルミニウム添加酸化亜鉛）などのＺｎＯ系の透明導電膜が活発に検討されている。 As a transparent conductive film for a flat panel display such as a liquid crystal display, ITO (Indium Tin Oxide) is usually used. Since this ITO uses In, there is a possibility that it will lack resources in the future. As an alternative material, ZnO-based transparent conductivity such as AZO (Al-Zn-O: Aluminum doped Zinc Oxide) is used. Membranes are being actively investigated.
ＩＴＯの代替えのためには、抵抗率をＩＴＯ並みに低下させる必要があるが、ＺｎＯ系の透明導電膜の抵抗を下げる方法として、従来はスパッタリング法などで結晶性の良いｃ軸配向（（０００１）配向）の膜を作製することが良いとされていた（特許文献１〜３参照）。 In order to substitute for ITO, it is necessary to reduce the resistivity to the same level as that of ITO. However, as a method for reducing the resistance of a ZnO-based transparent conductive film, conventionally, c-axis orientation ((0001 ) Orientation) film is considered good (see Patent Documents 1 to 3).
上記従来の技術には、以下の課題が残されている。
すなわち、従来のｃ軸配向のＺｎＯ系の膜では、フラットパネルディスプレイで標準的な１００〜２００ｎｍ程度の膜厚で、抵抗率がＩＴＯ並みの２．５×１０−４Ω・ｃｍ以下に低下しないという問題があった。したがって、ＩＴＯ代替のためには、２００ｎｍ以下の膜厚でＩＴＯと同程度に抵抗を低下させる必要がある。
The following problems remain in the conventional technology.
That is, in the conventional c-axis oriented ZnO-based film, the resistivity is not reduced to 2.5 × 10 −4 Ω · cm or less, which is the same as that of ITO, with a standard film thickness of about 100 to 200 nm in a flat panel display. There was a problem. Therefore, in order to replace ITO, it is necessary to reduce the resistance to the same extent as that of ITO with a film thickness of 200 nm or less.
本発明は、前述の課題に鑑みてなされたもので、ＩＴＯ並みの低抵抗を有したＺｎＯ系の透明導電膜及びその製造方法を提供することを目的とする。 The present invention has been made in view of the above-described problems, and an object thereof is to provide a ZnO-based transparent conductive film having a low resistance comparable to that of ITO and a method for manufacturing the same.
本発明は、前記課題を解決するために以下の構成を採用した。すなわち、第１の発明に係る透明導電膜は、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した六方晶のＺｎＯ系酸化物膜からなり、ｍ軸方向に配向したことを特徴とする。 The present invention employs the following configuration in order to solve the above problems. That is, the transparent conductive film according to the first invention is a hexagonal crystal having a composition of Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, with the balance being composed of Zn and inevitable impurities. It is made of a ZnO-based oxide film and is oriented in the m-axis direction.
このＺｎＯ系の透明導電膜では、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した六方晶のＺｎＯ系酸化物膜からなり、ｍ軸方向に配向しているので、ＩＴＯ並みの低抵抗を有するＡＺＯ膜となる。すなわち、伝導率は電子の流れる結晶方位によって異なり、ｃ軸方向（＜０、０、０、１＞方向）の配向よりも伝導率が高くなるｍ軸方向（＜１、０、−１、０＞方向）の配向となっていること、およびＡｌの良好なドーピング量によって、２．５×１０−４Ω・ｃｍ以下の抵抗率となる。 In this ZnO-based transparent conductive film, hexagonal ZnO-based oxide having a component composition containing Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, with the balance being composed of Zn and inevitable impurities. Since it consists of a film and is oriented in the m-axis direction, it becomes an AZO film having a low resistance comparable to that of ITO. That is, the conductivity varies depending on the crystal orientation in which electrons flow, and the m-axis direction (<1, 0, −1, 0) in which the conductivity is higher than the orientation in the c-axis direction (<0, 0, 0, 1> direction). > Direction) and a good doping amount of Al, the resistivity is 2.5 × 10 −4 Ω · cm or less.
なお、Ａｌの含有量を上記範囲に設定した理由は、０．１ｗｔ％未満であると、Ａｌのドーピング量が少なくて膜中のキャリア濃度が低下するためであり、２．０ｗｔ％を超えると、Ａｌのドーピング量が増えすぎて、結晶欠陥が増加し、移動度が低下してしまうためである。 The reason why the Al content is set in the above range is that when it is less than 0.1 wt%, the Al doping amount is small and the carrier concentration in the film decreases, and when it exceeds 2.0 wt% This is because the amount of Al doping increases too much, resulting in an increase in crystal defects and a decrease in mobility.
また、第２の発明に係る透明導電膜の製造方法は、上記本発明の透明導電膜を製造する方法であって、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した酸化物の焼結体からなるスパッタリングターゲットを用い、面方位（表面に平行な格子面）がｍ面（｛1、０、−１、０｝面）の六方晶のＺｎＯ単結晶基板又は同様の面方位のサファイア（Ａｌ２Ｏ３）単結晶基板の上に２００〜４００℃の成膜温度でスパッタすることを特徴とする。 Moreover, the manufacturing method of the transparent conductive film which concerns on 2nd invention is a method of manufacturing the transparent conductive film of the said invention, Comprising: Al: 0.1-2.0 wt% is contained with respect to the total amount of metal components And a sputtering target made of an oxide sintered body having a component composition consisting of Zn and inevitable impurities as the balance, and the plane orientation (lattice plane parallel to the surface) is m-plane ({1, 0, -1, Sputtering is performed at a film forming temperature of 200 to 400 ° C. on a (0} plane) hexagonal ZnO single crystal substrate or a sapphire (Al 2 O 3 ) single crystal substrate having the same plane orientation.
すなわち、この透明導電膜の製造方法では、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した酸化物の焼結体からなるスパッタリングターゲットを用い、面方位がｍ面の六方晶のＺｎＯ単結晶基板又は同様の面方位のサファイア単結晶基板の上に２００〜４００℃の成膜温度でスパッタするので、ｍ軸配向した低抵抗のＡＺＯ膜である上記透明導電膜を成膜することができる。 That is, in this method for producing a transparent conductive film, sintering of an oxide having a component composition containing Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, with the balance being Zn and inevitable impurities. Since sputtering is performed on a hexagonal ZnO single crystal substrate having a m-plane orientation or a sapphire single crystal substrate having a similar plane orientation at a film forming temperature of 200 to 400 ° C., an m-axis orientation is performed. The transparent conductive film which is an AZO film having a low resistance can be formed.
なお、成膜温度を上記範囲に設定した理由は、２００℃未満または４００℃を超えた温度であると、膜の結晶性が悪くなり、キャリア濃度及び移動度が低下して所望の低抵抗を得ることができないためである。
また、Ａｌの含有量を上記範囲内に設定した理由は、成膜した透明導電膜中のＡｌ含有量を上述した設定範囲内とするためである。
The reason why the film formation temperature is set in the above range is that if the temperature is less than 200 ° C. or more than 400 ° C., the crystallinity of the film is deteriorated, the carrier concentration and mobility are lowered, and a desired low resistance is obtained. It is because it cannot be obtained.
The reason why the Al content is set within the above range is that the Al content in the formed transparent conductive film is within the above-described setting range.
本発明によれば、以下の効果を奏する。
すなわち、本発明に係る透明導電膜及びその製造方法によれば、ｍ軸方向に配向した六方晶のＡＺＯ膜となるので、従来のＡＺＯ膜に比べて抵抗率が低下し、ＩＴＯ並みの低抵抗が得られる。
The present invention has the following effects.
That is, according to the transparent conductive film and the method of manufacturing the same according to the present invention, the hexagonal AZO film is oriented in the m-axis direction. Therefore, the resistivity is lower than that of the conventional AZO film, and the resistance is as low as that of ITO. Is obtained.
以下、本発明に係る透明導電膜及びその製造方法における一実施形態を説明する。 Hereinafter, an embodiment of a transparent conductive film and a method for producing the same according to the present invention will be described.
本実施形態の透明導電膜は、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した六方晶のＺｎＯ系酸化物膜からなり、ｍ軸方向に配向した薄膜である。
この透明導電膜は、抵抗率が２．５×１０−４Ω・ｃｍ以下であり、六方晶の結晶構造を有している。
The transparent conductive film of the present embodiment contains Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, and the remainder is a hexagonal ZnO-based oxide having a component composition consisting of Zn and inevitable impurities. A thin film made of a film and oriented in the m-axis direction.
This transparent conductive film has a resistivity of 2.5 × 10 −4 Ω · cm or less and has a hexagonal crystal structure.
なお、上記抵抗率は、膜厚計による膜厚測定と、抵抗測定装置によるシート抵抗測定により求められる。膜中のＡｌの含有量はＥＰＭＡ（電子線プローブ微小分析装置）による定量分析から求めることができる。また、ｍ軸配向（（１０−１０）配向）となっているかどうかは、Ｘ線回折（ＸＲＤ）測定により得られる回折パターンでの（１０−１０）ピークの相対強度比の大小から確認できる。 In addition, the said resistivity is calculated | required by the film resistance measurement by a film thickness meter, and the sheet resistance measurement by a resistance measuring apparatus. The Al content in the film can be determined from quantitative analysis using EPMA (electron probe microanalyzer). Moreover, it can be confirmed from the magnitude of the relative intensity ratio of the (10-10) peak in the diffraction pattern obtained by X-ray diffraction (XRD) measurement whether it is m-axis orientation ((10-10) orientation).
この透明導電膜は、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した酸化物の焼結体からなるスパッタリングターゲットを用い、面方位がｍ面の六方晶のＺｎＯ単結晶基板又は同様の面方位のサファイア単結晶基板の上に２００〜４００℃の成膜温度でスパッタすることで得られる。
なお、透明導電膜は、Ｘ線回折測定で、ｍ面に対応する（１０−１０）等の回折ピーク以外の回折ピークが観測されない程度にｍ軸方向に配向していることが好ましい。
This transparent conductive film contains Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, and the sputtering target is made of an oxide sintered body having a component composition consisting of Zn and inevitable impurities. And is sputtered onto a hexagonal ZnO single crystal substrate having an m-plane orientation or a sapphire single crystal substrate having a similar plane orientation at a film forming temperature of 200 to 400 ° C.
The transparent conductive film is preferably oriented in the m-axis direction to such an extent that no diffraction peak other than the diffraction peak corresponding to the m-plane (10-10) is observed by X-ray diffraction measurement.
このように、本実施形態の透明導電膜は、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した六方晶のＺｎＯ系酸化物膜からなり、ｍ軸方向に配向しているので、ＩＴＯ並みの低抵抗を有するＡＺＯ膜となる。すなわち、伝導率は電子の流れる結晶方位によって異なり、ｃ軸方向の配向よりも伝導率が高くなるｍ軸方向の配向となっていること、およびＡｌの良好なドーピング量によって、２．５×１０−４Ω・ｃｍ以下の抵抗率となる。 Thus, the transparent conductive film of this embodiment contains Al: 0.1 to 2.0 wt% with respect to the total metal component amount, and the hexagonal crystal has a component composition with the balance consisting of Zn and inevitable impurities. Since it is made of a ZnO-based oxide film and oriented in the m-axis direction, it becomes an AZO film having a resistance as low as that of ITO. In other words, the conductivity varies depending on the crystal orientation in which electrons flow, and the orientation is in the m-axis direction, where the conductivity is higher than the orientation in the c-axis direction. The resistivity is -4 Ω · cm or less.
また、この透明導電膜の製造方法では、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した酸化物の焼結体からなるスパッタリングターゲットを用い、面方位がｍ面の六方晶のＺｎＯ単結晶基板又は同様の面方位のサファイア単結晶基板の上にの上に２００〜４００℃の成膜温度でスパッタするので、ｍ軸配向した低抵抗のＡＺＯ膜である上記透明導電膜を成膜することができる。 Further, in this method for producing a transparent conductive film, sintering of an oxide having a component composition containing Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, with the balance being Zn and inevitable impurities. Since sputtering is performed on a hexagonal ZnO single crystal substrate having a m-plane orientation or a sapphire single crystal substrate having a similar plane orientation at a film forming temperature of 200 to 400 ° C. using a sputtering target composed of a body, The transparent conductive film which is an m-axis-oriented low-resistance AZO film can be formed.
次に、本発明に係る透明導電膜及びその製造方法について、上記実施形態に基づいて作製した実施例を評価した結果について説明する。 Next, the result of evaluating the example produced based on the said embodiment about the transparent conductive film which concerns on this invention, and its manufacturing method is demonstrated.
まず、全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した六方晶のＺｎＯ系酸化物の焼結体からなるスパッタリングターゲットを用い、３００℃の成膜温度でＤＣスパッタにて、表面の面方位がｍ面のＺｎＯ単結晶基板又は同様の面方位のサファイア（Ａｌ２Ｏ３）単結晶基板の上にｍ軸配向したＡＺＯ膜を２００ｎｍ成膜し、その抵抗率を測定した。その際のターゲット及び膜における全金属成分量に対するＡｌの割合、単結晶基板の面方位、抵抗率を表１及び表２に示す。 First, sputtering comprising a sintered body of hexagonal ZnO-based oxide containing Al: 0.1 to 2.0 wt% with respect to the total amount of metal components, with the balance being a component composition comprising Zn and inevitable impurities. M-axis orientation on a ZnO single crystal substrate having a surface orientation of m-plane or a sapphire (Al 2 O 3 ) single crystal substrate having a similar plane orientation by DC sputtering at a film forming temperature of 300 ° C. using a target. The AZO film formed was formed to a thickness of 200 nm, and the resistivity was measured. Tables 1 and 2 show the ratio of Al to the total amount of metal components in the target and film, the plane orientation of the single crystal substrate, and the resistivity.
なお、上記抵抗率は、膜厚測定（アルバック社製の膜厚計ＤＥＫＴＡＫを使用）と抵抗測定（三菱化学社製の抵抗率計ロレスタを使用）から、また、ターゲット及び膜におけるＡｌの含有量はＥＰＭＡ測定（日本電子社製の電子線ブローブ微小分析装置を使用）による定量分析から求めた。 In addition, the above-mentioned resistivity is based on film thickness measurement (using ULVAC film thickness meter DEKTAK) and resistance measurement (using Mitsubishi Chemical Corporation resistivity meter Loresta), and the target and film Al content. Was obtained from quantitative analysis by EPMA measurement (using an electron beam probe microanalyzer manufactured by JEOL Ltd.).
また、比較例として、面方位がｃ面のＺｎＯ単結晶基板又は同様の面方位のサファイア単結晶基板の上にｃ軸配向したＡＺＯ膜を同様の条件で成膜し、その抵抗率を測定した。その際のターゲット及び膜における全金属成分量に対するＡｌの割合、単結晶基板の面方位、抵抗率を表１及び表２に示す。抵抗率やＡｌの含有量の測定は実施例と同様にして行なった。
なお、これら実施例及び比較例において、膜の配向面の方位が各単結晶基板の表面の面方位と同じであることは、ＸＲＤ測定（ブルカー社製のＸ線回折装置を使用）で、各単結晶基板の表面の面方位と同じ方位の回折ピークのみが膜において観測されたことにより確認した。
Further, as a comparative example, a c-axis oriented AZO film was formed on a c-plane ZnO single crystal substrate or a sapphire single crystal substrate having a similar plane orientation under the same conditions, and the resistivity was measured. . Tables 1 and 2 show the ratio of Al to the total amount of metal components in the target and film, the plane orientation of the single crystal substrate, and the resistivity. The resistivity and Al content were measured in the same manner as in the examples.
In these examples and comparative examples, the orientation of the orientation plane of the film is the same as the orientation of the surface of each single crystal substrate. In XRD measurement (using a Bruker X-ray diffractometer), Only a diffraction peak having the same orientation as the surface orientation of the surface of the single crystal substrate was observed in the film.
なお、スパッタリング成膜条件、ターゲット作製方法は以下のとおりである。
＜ターゲット作製方法＞
原料粉末として、平均粒径が０．５μｍ以下で純度が９９．９％以上の酸化亜鉛粉末、酸化アルミニウム粉末を用意し、所望のＡｌ含有量となるようそれぞれ配合し、乾式ボールミルにより混合して混合粉末を作製した。この混合粉末を金型に入れ、ＣＩＰ（冷間静水圧プレス）による緻密化処理を行い、成形体に加工した。さらに、得られた成形体を大気中、１４００℃で５時間焼成することにより、焼結体を作製した。得られた焼結体を研削して、直径１０１．６ｍｍ、厚さ６ｍｍの寸法を有するタ−ゲットを作製した。
The sputtering film forming conditions and the target manufacturing method are as follows.
<Target preparation method>
Prepare zinc oxide powder and aluminum oxide powder with an average particle size of 0.5 μm or less and a purity of 99.9% or more as raw material powders, mix each with a desired Al content, and mix by dry ball mill. A mixed powder was prepared. This mixed powder was put into a mold and subjected to densification treatment by CIP (cold isostatic pressing) to process into a molded body. Furthermore, the obtained molded body was fired at 1400 ° C. for 5 hours in the air to prepare a sintered body. The obtained sintered body was ground to prepare a target having a diameter of 101.6 mm and a thickness of 6 mm.
＜スパッタリング成膜条件＞
・スパッタリング装置：ＤＣスパッタリングスパッタ装置（アルバック社製）
・磁界強度：１０００Ｇａｕｓｓ（ターゲット直上、垂直成分）
・スパッタリングターゲット：ＡＺＯ（ＺｎＯ＋Ａｌ２Ｏ３）焼結ターゲット（焼結密度９８．５％）
・到達真空度：５×１０−５Ｐａ未満
・スパッタリングガス：Ａｒ
・スパッタリングガス圧：０．５Ｐａ
・スパッタリングパワー：ＤＣ２００Ｗ
<Sputtering film formation conditions>
・ Sputtering equipment: DC sputtering sputtering equipment (manufactured by ULVAC)
Magnetic field strength: 1000 Gauss (directly above the target, vertical component)
Sputtering target: AZO (ZnO + Al 2 O 3 ) sintered target (sintering density 98.5%)
・ Achieving vacuum: less than 5 × 10 −5 Pa ・ Sputtering gas: Ar
・ Sputtering gas pressure: 0.5 Pa
・ Sputtering power: DC200W
これらの結果、比較例に比べて面方位がｍ面のＺｎＯ単結晶基板又は同様の面方位のサファイア単結晶基板の上に所定Ａｌ含有量で成膜した本発明の実施例は、抵抗率が低く、ＩＴＯ並みの２．５×１０−４Ω・ｃｍ以下の値が得られている。
なお、成膜温度を１８０℃及び４２０℃として同様に上記成膜を行った結果、ＺｎＯ単結晶又はサファイア単結晶のいずれの面方位を持つ基板を用いても、抵抗率が２．５×１０−４Ω・ｃｍを超えた値となることを確認した。
As a result, compared to the comparative example, the embodiment of the present invention formed with a predetermined Al content on a ZnO single crystal substrate having an m-plane orientation or a sapphire single crystal substrate having a similar plane orientation has a resistivity of A value of 2.5 × 10 −4 Ω · cm or less, which is as low as ITO, is obtained.
Note that, as a result of performing the above film formation in the same manner at a film formation temperature of 180 ° C. and 420 ° C., the resistivity is 2.5 × 10 10 regardless of whether the substrate has any plane orientation of ZnO single crystal or sapphire single crystal. It was confirmed that the value exceeded −4 Ω · cm.
なお、本発明の技術範囲は上記実施形態及び実施例に限定されるものではなく、本発明の趣旨を逸脱しない範囲において種々の変更を加えることが可能である。 The technical scope of the present invention is not limited to the above-described embodiments and examples, and various modifications can be made without departing from the spirit of the present invention.
Claims (2)
全金属成分量に対してＡｌ：０．１〜２．０ｗｔ％を含有し、残部がＺｎおよび不可避不純物からなる成分組成を有した酸化物の焼結体からなるスパッタリングターゲットを用い、面方位がｍ面の六方晶のＺｎＯ単結晶基板又は同様の面方位のサファイア単結晶基板の上に２００〜４００℃の成膜温度でスパッタすることを特徴とする透明導電膜の製造方法。 A method for producing the transparent conductive film according to claim 1,
Using a sputtering target made of an oxide sintered body having a component composition of Al and 0.1 to 2.0 wt% with respect to the total metal component amount, the balance being Zn and inevitable impurities, the plane orientation is A method for producing a transparent conductive film, comprising sputtering at a film forming temperature of 200 to 400 ° C. on an m-plane hexagonal ZnO single crystal substrate or a sapphire single crystal substrate having a similar plane orientation.
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| JPS5023918B1 (en) * | 1970-10-06 | 1975-08-12 | ||
| JP2010215948A (en) * | 2009-03-13 | 2010-09-30 | Hitachi Metals Ltd | Method for manufacturing transparent conductive film |
| JP2010219084A (en) * | 2009-03-13 | 2010-09-30 | Mitsubishi Materials Corp | SOLAR CELL HAVING CONSTITUENT LAYER OF (Zn, Al)O-BASED TRANSPARENT ELECTRODE LAYER AND ZnO-Al2O3-BASED SPUTTERING TARGET USED FOR FORMING THE (Zn, Al)O-BASED TRANSPARENT ELECTRODE LAYER |
| WO2011002086A1 (en) * | 2009-07-03 | 2011-01-06 | 株式会社カネカ | Crystalline silicon type solar cell and process for manufacture thereof |
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| JPS5023918B1 (en) * | 1970-10-06 | 1975-08-12 | ||
| JP2010215948A (en) * | 2009-03-13 | 2010-09-30 | Hitachi Metals Ltd | Method for manufacturing transparent conductive film |
| JP2010219084A (en) * | 2009-03-13 | 2010-09-30 | Mitsubishi Materials Corp | SOLAR CELL HAVING CONSTITUENT LAYER OF (Zn, Al)O-BASED TRANSPARENT ELECTRODE LAYER AND ZnO-Al2O3-BASED SPUTTERING TARGET USED FOR FORMING THE (Zn, Al)O-BASED TRANSPARENT ELECTRODE LAYER |
| WO2011002086A1 (en) * | 2009-07-03 | 2011-01-06 | 株式会社カネカ | Crystalline silicon type solar cell and process for manufacture thereof |
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