JP6125689B1 - Indium oxide-zinc oxide (IZO) sputtering target - Google Patents

Indium oxide-zinc oxide (IZO) sputtering target Download PDF

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JP6125689B1
JP6125689B1 JP2016071381A JP2016071381A JP6125689B1 JP 6125689 B1 JP6125689 B1 JP 6125689B1 JP 2016071381 A JP2016071381 A JP 2016071381A JP 2016071381 A JP2016071381 A JP 2016071381A JP 6125689 B1 JP6125689 B1 JP 6125689B1
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target
sintered body
temperature
sputtering
sintering
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JP2017179536A (en
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崇 掛野
崇 掛野
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JX Nippon Mining and Metals Corp
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Priority to TW105137428A priority patent/TWI645059B/en
Priority to TW107122136A priority patent/TWI661069B/en
Priority to KR1020160163661A priority patent/KR20170112970A/en
Priority to CN201611242711.5A priority patent/CN107267936A/en
Priority to CN201810723839.6A priority patent/CN108930015A/en
Priority to CN202210337974.3A priority patent/CN114752901A/en
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Priority to KR1020180077156A priority patent/KR101956506B1/en
Priority to KR1020190017109A priority patent/KR20190019104A/en
Priority to KR1020200017636A priority patent/KR102322184B1/en
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    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract

【課題】焼結体の反りが少なく、反り低減のための研削によるバルク抵抗率の面内ばらつきが抑制された酸化インジウム−酸化亜鉛系酸化物（ＩＺＯ）焼結体ターゲット及びその製造方法を提供する。【解決手段】ＺｎとＩｎの原子比が０．０５≦Ｚｎ／（Ｉｎ＋Ｚｎ）≦０．３０を満たし、該ターゲットのスパッタ面におけるバルク抵抗率の標準偏差が０．１ｍΩ・ｃｍ以下であるスパッタリングターゲットであって、原料粉末をプレス成形した成形体を室温から焼結温度まで昇温する工程において、途中保持温度を６００〜８００℃とし、１〜１０時間保持する工程、当該途中保持温度から焼結温度まで０．２〜２．０℃／ｍｉｎで昇温する工程、焼結温度を１３５０〜１５００℃とし、焼結保持時間を１〜１００時間で焼結するＩＺＯ焼結体からなるスパッタリングターゲットの製造方法。【選択図】なしAn object of the present invention is to provide an indium oxide-zinc oxide-based oxide (IZO) sintered body target with less warpage of the sintered body and suppressed in-plane variation of bulk resistivity due to grinding for reducing warpage, and a method for producing the same. To do. A sputtering target in which an atomic ratio of Zn and In satisfies 0.05 ≦ Zn / (In + Zn) ≦ 0.30, and a standard deviation of bulk resistivity on a sputtering surface of the target is 0.1 mΩ · cm or less. In the step of raising the temperature of the compact formed by pressing the raw material powder from room temperature to the sintering temperature, the intermediate holding temperature is set to 600 to 800 ° C., and the step of holding for 1 to 10 hours, sintering from the intermediate holding temperature. The step of raising the temperature to 0.2 to 2.0 ° C./min up to the temperature, the sintering temperature of 1350 to 1500 ° C., and the sputtering target made of an IZO sintered body that sinters the sintering holding time in 1 to 100 hours Production method. [Selection figure] None

Description

本発明は、酸化インジウム−酸化亜鉛系（ＩＺＯ）スパッタリングターゲット及びその製造方法に関し、特には、ターゲットのスパッタ面内におけるバルク抵抗率の差が小さく、膜の形成に好適なスパッタリングターゲット及びその製造方法に関する。   The present invention relates to an indium oxide-zinc oxide based (IZO) sputtering target and a method for producing the same, and more particularly, a sputtering target suitable for forming a film with a small difference in bulk resistivity within the sputtering surface of the target and a method for producing the same. About.

いくつかの金属複合酸化物からなる透明導電膜は、高導電性と可視光透過性を有しているので、液晶表示装置、薄膜エレクトロルミネッセンス表示装置、有機ＥＬ、放射性検出装置、端末機器の透明タブレット、窓ガラスの結露防止用発熱膜、帯電防止膜あるいは太陽光集熱器用選択透過膜、タッチパネルの電極などの多岐に亘る用途に使用されている。このような金属複合酸化物からなる透明導電膜の中でも最も普及しているものはＩＴＯと呼ばれている酸化インジウム−酸化錫からなる透明導電膜である。   The transparent conductive film made of some metal complex oxides has high conductivity and visible light transmission, so it is transparent for liquid crystal display devices, thin film electroluminescence display devices, organic EL, radioactive detection devices, and terminal devices. It is used in a wide variety of applications such as tablets, heat generation films for preventing condensation on window glass, antistatic films or selective permeation films for solar collectors, and electrodes for touch panels. Among the transparent conductive films made of such metal composite oxides, the most popular one is a transparent conductive film made of indium oxide-tin oxide called ITO.

一方、ＩＴＯ膜よりもエッチング速度が大きいインジウム及び亜鉛の複合酸化物（「ＩＺＯ」と称する）を主成分とする透明導電膜の需要が増加しつつある。ＩＺＯ膜を製造する際には、焼結体スパッタリングターゲットが使用されるが、このＩＺＯ焼結体は、焼結過程で反りが発生するという問題があった。反りが発生したターゲットは、製品形状を整えるために、その両面を、平面になるよう研削する必要があるが、研削処理によってターゲット面内のバルク抵抗率が大きく変動し、スパッタリングの際、異常放電等が生じるという問題があった。   On the other hand, there is an increasing demand for transparent conductive films composed mainly of a composite oxide of indium and zinc (referred to as “IZO”), which has a higher etching rate than the ITO film. When manufacturing an IZO film, a sintered body sputtering target is used, but this IZO sintered body has a problem that warpage occurs in the sintering process. In order to adjust the product shape, it is necessary to grind both sides of the target that is warped so that it is flat. However, the bulk resistivity in the target surface varies greatly due to the grinding process, and abnormal discharge occurs during sputtering. There was a problem that it occurred.

次に、ＩＺＯ焼結体スパッタリングに関する先行技術について説明する。特許文献１には、酸化インジウムと酸化亜鉛とを混合し、これをコールドプレス及び静水圧冷間圧縮により成形した後、酸素雰囲気中又は大気中で１３００〜１５００℃で加熱焼結することが開示されている。また、特許文献２には、Ｉｎ２Ｏ３とＺｎＯの粉末を混合するに先立ちＺｎＯ粉末のみを仮焼することが開示されている。 Next, the prior art regarding IZO sintered compact sputtering is demonstrated. Patent Document 1 discloses that indium oxide and zinc oxide are mixed, formed by cold pressing and isostatic pressing, and then heated and sintered at 1300 to 1500 ° C. in an oxygen atmosphere or in the air. Has been. Patent Document 2 discloses that only ZnO powder is calcined prior to mixing In 2 O 3 and ZnO powder.

特許文献３には、酸化インジウム粉末と酸化亜鉛粉末とを特定の性状にすることが記載されている。また、特許文献４には、ＩＺＯを焼結する際、１２００℃に達するまで、酸素濃度２１％容量以上とし、１２００〜１４５０℃では、酸素濃度２１％容量未満の雰囲気で焼結することが記載されている。特許文献５には、原料粉末を微細に粉砕することでターゲットにおける結晶粒径を制御することが記載されている。   Patent Document 3 describes that indium oxide powder and zinc oxide powder have specific properties. Patent Document 4 describes that when IZO is sintered, the oxygen concentration is set to 21% capacity or more until reaching 1200 ° C., and the sintering is performed in an atmosphere of less than 21% oxygen concentration at 1200 to 1450 ° C. Has been. Patent Document 5 describes that the crystal grain size in the target is controlled by finely pulverizing the raw material powder.

しかしながら、これら従来の製造工程の下では、焼結時の加熱による熱膨張、熱収縮に伴い、作製した焼結体に反りが発生していた。反りの大きな焼結体はターゲット形状に加工する際、ターゲットのスパッタ面における抵抗率の差が大きくなることがあった。このような、ターゲット面内の抵抗率のばらつきはスパッタ時にアーキング（異常放電）等を引き起こし、製品の製造歩留まりを低下させる問題があった。特に、近年のスパッタリングターゲットの大面積化に伴い、上記のような問題は顕著になっていた。   However, under these conventional manufacturing processes, the produced sintered body warps due to thermal expansion and contraction due to heating during sintering. When a sintered body having a large warp is processed into a target shape, the difference in resistivity on the sputtering surface of the target may become large. Such variations in the resistivity within the target surface cause arcing (abnormal discharge) during sputtering, resulting in a problem that the production yield of the product is lowered. In particular, with the increase in area of sputtering targets in recent years, the above problems have become prominent.

特開２００１−１３１７３６号公報JP 2001-131736 A 特開平９−１１１４４４号公報JP-A-9-111444 特開２００７−８７８０号公報JP 2007-8780 A 特開２００７−８７７２号公報Japanese Patent Laid-Open No. 2007-8772 国際公開第２００１／０３８５９９号International Publication No. 2001/038599

本発明は上記課題を解決するためになされたものであり、スパッタリングの際にアーキング（異常放電）の発生を抑制することができる、スパッタ面内のバルク抵抗率の差が小さい、スパッタリングターゲット及びその製造方法を提供することを課題とする。特に、大面積であっても、バルク抵抗率の面内の差が小さいスパッタリングターゲットを提供することを課題とする。   The present invention has been made to solve the above-described problems, and can suppress the occurrence of arcing (abnormal discharge) during sputtering, and has a small difference in bulk resistivity within the sputtering surface, and a sputtering target thereof It is an object to provide a manufacturing method. In particular, it is an object of the present invention to provide a sputtering target having a small in-plane difference in bulk resistivity even in a large area.

本発明者は、上記の課題を解決するために鋭意研究を行った結果、ＩＺＯの収縮が開始する或いは開始したところで一旦温度を保持して、焼結体内の温度分布を小さくし、これにより、焼結体の反り量を大幅に抑制することができることを見出した。その結果、ターゲット形状に整えるため、その両面を平面になるように研削等しても、面内のバルク抵抗率の差が小さいスパッタリングターゲットを得ることができるとの知見が得られた。   As a result of earnest research to solve the above-mentioned problems, the present inventor has held the temperature once when the shrinkage of IZO starts or starts, thereby reducing the temperature distribution in the sintered body. It has been found that the amount of warpage of the sintered body can be greatly suppressed. As a result, it was found that a sputtering target with a small in-plane bulk resistivity difference could be obtained even if the both surfaces were ground so as to be in a flat shape.

このような知見に基づき、本願は、以下の発明を提供する。
１）Ｉｎ、Ｚｎ、Ｏからなるスパッタリングターゲットであって、ＺｎとＩｎの原子比が０．０５≦Ｚｎ／（Ｉｎ＋Ｚｎ）≦０．３０を満たし、該ターゲットのスパッタ面におけるバルク抵抗率の標準偏差が１．０ｍΩ・ｃｍ以下であることを特徴とするスパッタリングターゲット。
２）バルク抵抗率が１．０〜１０ｍΩ・ｃｍであることを特徴とする上記１）記載のスパッタリングターゲット。
３）相対密度が９８％以上であることを特徴とする上記１）又は２）記載のスパッタリングターゲット。
４）スパッタ面の面積が６００００ｍｍ２〜４０００００ｍｍ２であることを特徴とする上記１）〜３）のいずれか一に記載のスパッタリングターゲット。
５）Ｉｎ、Ｚｎ、Ｏからなる焼結体であって、ＺｎとＩｎの原子比が０．０５≦Ｚｎ／（Ｉｎ＋Ｚｎ）≦０．３０を満たし、反り量が２．０ｍｍ以内であることを特徴とするＩＺＯ焼結体。
６）原料粉末をプレス成形した成形体を焼結して製造される、ＩＺＯ焼結体からなるスパッタリングターゲットの製造方法であって、室温から焼結温度まで昇温する工程において、途中保持温度を６００〜８００℃とし、１〜１０時間保持する工程、当該途中保持温度から焼結温度まで０．２〜２．０℃／ｍｉｎで昇温する工程、焼結温度を１３５０〜１５００℃とし、焼結保持時間を１〜１００時間で焼結する工程からなることを特徴とするスパッタリングターゲットの製造方法。
７）焼結温度を１３８０〜１４２０℃とすることを特徴とする上記６）記載のスパッタリングターゲットの製造方法。
８）焼結保持時間を５〜３０時間で焼結することを特徴とする上記６）又は７）記載のスパッタリングターゲットの製造方法。
９）１．０〜５．０℃／ｍｉｎで降温することを特徴とする上記６）〜８）のいずれか一に記載のスパッタリングターゲットの製造方法。
のスパッタリングターゲットの製造方法。
１０）途中保持温度から焼結温度まで０．５〜１．５℃／ｍｉｎで昇温することを特徴とする上記６）〜９）のいずれか一に記載のスパッタリングターゲットの製造方法。 Based on such knowledge, the present application provides the following inventions.
1) A sputtering target composed of In, Zn, and O, wherein the atomic ratio of Zn and In satisfies 0.05 ≦ Zn / (In + Zn) ≦ 0.30, and the standard deviation of the bulk resistivity on the sputtering surface of the target Is 1.0 mΩ · cm or less.
2) The sputtering target according to 1) above, wherein the bulk resistivity is 1.0 to 10 mΩ · cm.
3) The sputtering target according to 1) or 2) above, wherein the relative density is 98% or more.
4) The sputtering target according to any one of 1) to 3) above, wherein the area of the sputtering surface is 60000 mm 2 to 400000 mm 2 .
5) A sintered body made of In, Zn, and O, wherein an atomic ratio of Zn and In satisfies 0.05 ≦ Zn / (In + Zn) ≦ 0.30, and a warpage amount is within 2.0 mm. A featured IZO sintered body.
6) A method for producing a sputtering target comprising an IZO sintered body produced by sintering a molded body obtained by press-molding a raw material powder, and in the step of raising the temperature from room temperature to the sintering temperature, A step of holding at 600 to 800 ° C. for 1 to 10 hours, a step of raising the temperature from the intermediate holding temperature to the sintering temperature at 0.2 to 2.0 ° C./min, a sintering temperature of 1350 to 1500 ° C., A method for producing a sputtering target, comprising a step of sintering for a holding time of 1 to 100 hours.
7) The method for producing a sputtering target according to 6) above, wherein the sintering temperature is 1380 to 1420 ° C.
8) Sintering holding time is 5 to 30 hours, The manufacturing method of the sputtering target of the said 6) or 7) description characterized by the above-mentioned.
9) The method for producing a sputtering target according to any one of 6) to 8) above, wherein the temperature is lowered at 1.0 to 5.0 ° C./min.
A method for manufacturing a sputtering target.
10) The method for producing a sputtering target according to any one of the above 6) to 9), wherein the temperature is raised from an intermediate holding temperature to a sintering temperature at 0.5 to 1.5 ° C./min.

本発明は、酸化インジウム−酸化亜鉛系酸化物（ＩＺＯ）焼結体の製造方法において、従来と異なる製造条件、すなわち、焼結条件のうち、特定の温度で保持することが反りの低減に有効であることを見出し、スパッタ面内におけるバルク抵抗率差の小さいターゲットを作製することができ、その結果、アーキングなどの発生が少なく良好なスパッタリングを可能とし、形成した膜の特性を向上させることができるという優れた効果を有する。本発明は、特に大面積のＩＺＯスパッタリングターゲットにおいて有効である。   According to the present invention, in the method for producing an indium oxide-zinc oxide-based oxide (IZO) sintered body, it is effective for reducing warpage to hold at a specific temperature among the production conditions different from the conventional one, that is, the sintering conditions. As a result, it is possible to produce a target having a small bulk resistivity difference in the sputtering surface, and as a result, it is possible to perform good sputtering with less occurrence of arcing and the like, and to improve the characteristics of the formed film. It has an excellent effect of being able to. The present invention is particularly effective for a large area IZO sputtering target.

本発明のスパッタリングターゲット（角型）のバルク抵抗率の測定箇所を示す図である。It is a figure which shows the measurement location of the bulk resistivity of the sputtering target (square shape) of this invention. 本発明のスパッタリングターゲット（円盤型）のバルク抵抗率の測定箇所を示す図である。It is a figure which shows the measurement location of the bulk resistivity of the sputtering target (disk type) of this invention. 本発明のスパッタリングターゲットの反り量の測定を示す模式図である。It is a schematic diagram which shows the measurement of the curvature amount of the sputtering target of this invention.

本発明のスパッタリングターゲットの成分組成は、インジウム（Ｉｎ）、亜鉛（Ｚｎ）、酸素（Ｏ）からなり、ＺｎとＩｎとの原子比が０．０５≦Ｚｎ／（Ｉｎ＋Ｚｎ）≦０．３０の条件を満たすものである。本発明のターゲットは、主としてインジウムと亜鉛の複合酸化物から構成されているが、酸化インジウムや酸化亜鉛の単独の酸化物を含んでもよい。また、本発明の特性を損なわない範囲で他の元素を含んでもよい。上記Ｚｎの原子比はターゲットを用いて形成される膜の導電性等の観点から決定されるものであり、この範囲を超えると所望の特性が得られない。   The component composition of the sputtering target of the present invention is composed of indium (In), zinc (Zn), and oxygen (O), and the atomic ratio between Zn and In is 0.05 ≦ Zn / (In + Zn) ≦ 0.30. It satisfies. The target of the present invention is mainly composed of a complex oxide of indium and zinc, but may include a single oxide of indium oxide or zinc oxide. Moreover, you may contain another element in the range which does not impair the characteristic of this invention. The atomic ratio of Zn is determined from the viewpoint of the conductivity of the film formed using the target, and if it exceeds this range, desired characteristics cannot be obtained.

本発明は、前記スパッタリングターゲットのスパッタ面におけるバルク抵抗率の標準偏差が１．０ｍΩ・ｃｍ以下であることを特徴とする。焼結体の反りが大きい場合、ターゲットのスパッタ面のバルク抵抗率のばらつきが大きくなるため、形成した膜特性（特に膜抵抗）の均一性を阻害する問題があった。本発明では、焼結条件を調整することで焼結体の反りを著しく低減し、これにより、スパッタ面内のバルク抵抗率の標準偏差を１．０ｍΩ・ｃｍ以下まで低減することを可能としている。なお、スパッタ面とは、焼結体を研削し、スパッタリングターゲットに加工した結果、スパッタ装置にてスパッタされる面のことを意味する。   The present invention is characterized in that the standard deviation of the bulk resistivity on the sputtering surface of the sputtering target is 1.0 mΩ · cm or less. When the warp of the sintered body is large, the variation in the bulk resistivity of the sputtering surface of the target becomes large, and there is a problem that the uniformity of the formed film characteristics (particularly film resistance) is hindered. In the present invention, the warping of the sintered body is remarkably reduced by adjusting the sintering conditions, thereby making it possible to reduce the standard deviation of the bulk resistivity in the sputtering surface to 1.0 mΩ · cm or less. . In addition, a sputter | spatter surface means the surface sputter | spatter | spattered with a sputtering device as a result of grinding a sintered compact and processing it into a sputtering target.

本発明のバルク抵抗率は、１．０ｍΩ・ｃｍ以上、１０ｍΩ・ｃｍ以下であることが好ましい。バルク抵抗率が高い場合、スパッタ放電を不安定にすることがある。本発明のバルク抵抗率は、四探針法により、ターゲットのスパッタ面を等間隔に１６点以上（角型ターゲットの場合）又は９点以上（円盤型ターゲットの場合）を測定し、その平均値及び標準偏差を算出する。例えば、図１、２に示すように、ターゲット端から２０ｍｍ以上内側の部分を５０ｍｍ〜６０ｍｍの等間隔で１５ｍｍ角の部位を３回測定し、その平均をその部位のバルク抵抗率とする。但し、ターゲットの面積が小さい場合は、測定間隔を狭めることで、測定点数を９点以上又は１６点以上確保する。なお、ターゲットのバルク抵抗率を測定する際は、必要に応じて研削しても良い。   The bulk resistivity of the present invention is preferably 1.0 mΩ · cm or more and 10 mΩ · cm or less. When the bulk resistivity is high, the sputter discharge may become unstable. The bulk resistivity of the present invention is determined by measuring at least 16 points (in the case of a square target) or 9 points or more (in the case of a disk type target) at equal intervals on the sputtering surface of the target by the four-point probe method, and the average value thereof. And calculate the standard deviation. For example, as shown in FIGS. 1 and 2, a 15 mm square part is measured three times at an equal interval of 50 mm to 60 mm at an inner portion of 20 mm or more from the target end, and the average is defined as the bulk resistivity of the part. However, when the area of the target is small, the number of measurement points is ensured to be 9 or more or 16 or more by narrowing the measurement interval. In addition, when measuring the bulk resistivity of a target, you may grind as needed.

一般に、焼結体の面積が大きくなるほど、反り量も大きくなる。本発明は、大面積の焼結体であっても、その反り量を２．０ｍｍ以内に抑制することができることを特徴とするものである。本発明は、特に、ターゲットのスパッタ面における面積が６００００ｍｍ２〜４０００００ｍｍ２と大面積であっても、スパッタ面内の抵抗率差を上記範囲に抑えることができる点で優れたものである。ここで、反りの測定には、レーザー式変位センサーを用い、そのレーザーをプローブとして焼結体の大きさに合わせて、図２に示すように焼結体のいずれか一方の面をレーザーで走査しながら、その高さを測定する。そして、面内における最大の高さと最小の高さの差異を最大反り量とする。 In general, the larger the area of the sintered body, the greater the warpage. The present invention is characterized in that even if the sintered body has a large area, the amount of warpage can be suppressed within 2.0 mm. The present invention is particularly excellent in that the difference in resistivity within the sputtering surface can be kept within the above range even if the area of the sputtering surface of the target is as large as 60000 mm 2 to 400000 mm 2 . Here, for the measurement of warpage, a laser displacement sensor is used, and the laser is used as a probe to match the size of the sintered body, and as shown in FIG. 2, one surface of the sintered body is scanned with a laser. While measuring the height. The difference between the maximum height and the minimum height in the plane is set as the maximum warpage amount.

また、本発明のスパッタリングターゲットは、相対密度が９８％以上と高密度であることを特徴とするものである。高密度ターゲットは、スパッタリングの際のパーティクル等を低減することができ、良好な特性を備えた膜を形成することが可能となる。相対密度は、（アルキメデス法で測定した焼結体の実際の密度）／（酸化物の組成から計算した理論密度）×１００＝相対密度（％）で示したものである。ここで、酸化物の組成から計算した理論密度とは、原料を構成する元素から算出した理論的な密度のことであり、例えば酸化インジウム（Ｉｎ２Ｏ３）粉、酸化亜鉛（ＺｎＯ）粉を原料とし、酸化インジウム：酸化亜鉛の重量比を９０ｗｔ％：１０ｗｔ％とした場合、酸化物の組成から計算した理論密度＝（酸化インジウムの理論密度×９０＋酸化亜鉛の理論密度×１０）／１００（ｇ／ｃｍ３）として算出する。 The sputtering target of the present invention is characterized in that the relative density is as high as 98% or more. The high-density target can reduce particles and the like during sputtering, and can form a film with good characteristics. The relative density is expressed by (actual density of sintered body measured by Archimedes method) / (theoretical density calculated from oxide composition) × 100 = relative density (%). Here, the theoretical density calculated from the composition of the oxide is a theoretical density calculated from the elements constituting the raw material. For example, indium oxide (In 2 O 3 ) powder, zinc oxide (ZnO) powder is used. When the weight ratio of indium oxide: zinc oxide is 90 wt%: 10 wt% as a raw material, the theoretical density calculated from the oxide composition = (theoretical density of indium oxide × 90 + theoretical density of zinc oxide × 10) / 100 ( g / cm 3 ).

本発明の酸化インジウム−酸化亜鉛系酸化物（ＩＺＯ）焼結体ターゲットは、以下、原料の混合、粉砕、成型、焼結の各プロセスを経て作製することができる。
（原料の混合、粉砕、造粒、成型の条件）
原料粉として、酸化インジウム（Ｉｎ２Ｏ３）粉、酸化亜鉛（ＺｎＯ）粉を準備する。原料粉は、比表面積が約５ｍ２／ｇのものを使用するのが好ましい。
具体的には、酸化インジウム粉は、かさ密度：０．５〜０．７ｇ／ｃｍ３、メジアン径（Ｄ５０）：１．０〜２．１μｍ、比表面積：４．０〜５．７ｍ２／ｇ、酸化亜鉛粉：かさ密度：０．２〜０．６ｇ／ｃｍ３、メジアン径（Ｄ５０）：１．０〜２．５μｍ、比表面積：３．０〜６．０ｍ２／ｇを使用する。 The indium oxide-zinc oxide-based oxide (IZO) sintered compact target of the present invention can be produced through the following processes of mixing, crushing, molding and sintering of raw materials.
(Raw material mixing, grinding, granulation, molding conditions)
As raw material powder, indium oxide (In 2 O 3 ) powder and zinc oxide (ZnO) powder are prepared. The raw material powder preferably has a specific surface area of about 5 m 2 / g.
Specifically, the indium oxide powder has a bulk density of 0.5 to 0.7 g / cm 3 , a median diameter (D 50 ) of 1.0 to 2.1 μm, and a specific surface area of 4.0 to 5.7 m 2. / G, zinc oxide powder: bulk density: 0.2 to 0.6 g / cm 3 , median diameter (D 50 ): 1.0 to 2.5 μm, specific surface area: 3.0 to 6.0 m 2 / g use.

次に、各原料粉を所望の組成比となるように秤量後、混合粉砕を行う。粉砕方法には求める粒度、被粉砕物質に応じて様々な方法があるが、ビーズミル等の湿式媒体攪拌ミルが適している。これは、粉体を水に分散させたスラリーを、硬度の高い材料であるジルコニア、アルミナ等の粉砕媒体と共に強制的に攪拌するものであり、高効率で粉砕粉を得ることが出来る。しかし、この際に粉砕媒体も磨耗するために、粉砕粉に粉砕媒体自身が不純物として混入するので、長時間の処理は好ましくない。   Next, each raw material powder is weighed so as to have a desired composition ratio, and then mixed and ground. There are various pulverization methods depending on the desired particle size and the material to be pulverized, but a wet medium stirring mill such as a bead mill is suitable. In this method, a slurry in which powder is dispersed in water is forcibly stirred together with a grinding medium such as zirconia or alumina, which is a material with high hardness, and a pulverized powder can be obtained with high efficiency. However, since the pulverizing medium is also worn at this time, the pulverizing medium itself is mixed as an impurity in the pulverized powder.

粉砕量を粉砕前後の比表面積の差で定義すれば、湿式媒体攪拌ミルでは粉砕量は粉体に対する投入エネルギーにほぼ比例する。従って、粉砕を行う際には、湿式媒体攪拌ミルは積算電力を管理することが重要である。粉砕前後の比表面積の差（ΔＢＥＴ）は、０．５〜３．０ｍ２／ｇ、粉砕後のメジアン径（Ｄ５０）は、１．０μｍ以下とする。 If the pulverization amount is defined by the difference in specific surface area before and after pulverization, the pulverization amount is almost proportional to the input energy to the powder in the wet medium stirring mill. Therefore, when performing pulverization, it is important that the wet medium stirring mill manages the integrated power. The difference in specific surface area before and after pulverization (ΔBET) is 0.5 to 3.0 m 2 / g, and the median diameter (D 50 ) after pulverization is 1.0 μm or less.

次に、微粉砕したスラリーの造粒を行う。これは、造粒により粉体の流動性を向上させることで、次工程のプレス成型時に粉体を均一に金型へ充填し、均質な成形体を得るためである。造粒には様々な方式があるが、プレス成型に適した造粒粉を得る方法の一つに、噴霧式乾燥装置（スプレードライヤー）を用いる方法がある。これは粉体をスラリーとして、熱風中に液滴として分散させ、瞬間的に乾燥させる方法であり、１０〜５００μｍの球状の造粒粉が連続的に得ることが出来る。   Next, the finely pulverized slurry is granulated. This is because by improving the fluidity of the powder by granulation, the powder is uniformly filled in the mold at the time of press molding in the next step, and a homogeneous molded body is obtained. There are various types of granulation, and one method for obtaining granulated powder suitable for press molding is a method using a spray-type drying device (spray dryer). This is a method in which powder is dispersed as slurry in hot air and dried instantaneously, and spherical granulated powder of 10 to 500 μm can be continuously obtained.

スプレードライヤーによる乾燥では、熱風の入口温度、および出口温度の管理が重要である。入口と出口との温度差が大きければ単位時間当たりの乾燥量が増加し生産性が向上するが、入口温度が高すぎる場合には粉体、および添加したバインダーが熱により変質し、望まれる特性が得られない場合がある。また、出口温度が低すぎる場合は造粒粉が十分に乾燥されない場合がある。   In drying with a spray dryer, it is important to control the inlet temperature and outlet temperature of hot air. If the temperature difference between the inlet and outlet is large, the amount of drying per unit time will increase and the productivity will improve, but if the inlet temperature is too high, the powder and added binder will change in quality due to heat, and the desired characteristics May not be obtained. In addition, when the outlet temperature is too low, the granulated powder may not be sufficiently dried.

また、スラリー中にポリビニルアルコール（ＰＶＡ）等のバインダーを添加し造粒粉中に含有させることで、成形体強度を向上させることが出来る。ＰＶＡの添加量は、ＰＶＡ６ｗｔ．％含有水溶液を原料粉に対して５０〜２５０ｃｃ／ｋｇ添加する。さらに、バインダーに適した可塑剤も添加することで、プレス成型時の造粒粉の圧壊強度を調節することも出来る。また、得られた造粒粉に、少量の水を添加し湿潤させることで成形体強度を向上する方法もある。   Moreover, a molded object intensity | strength can be improved by adding binders, such as polyvinyl alcohol (PVA), in a slurry, and making it contain in granulated powder. The amount of PVA added was PVA 6 wt. % Aqueous solution is added to the raw material powder at 50 to 250 cc / kg. Furthermore, the crushing strength of the granulated powder during press molding can be adjusted by adding a plasticizer suitable for the binder. There is also a method for improving the strength of the molded body by adding a small amount of water to the obtained granulated powder and moistening it.

次に、プレス成型を行う。造粒粉を金型に充填し、４００〜１０００ｋｇｆ／ｃｍ２の圧力を、１〜３分間保持して成形する。圧力４００ｋｇｆ／ｃｍ２未満であると、充分な強度と密度の成形体を得ることができず、また圧力１０００ｋｇｆ／ｃｍ２以上では、成形体を金型から取り出す際に、成形体自身が圧力から解放されることによる変形のため破壊する場合があり、生産上好ましくない。 Next, press molding is performed. The granulated powder is filled into a mold, and molded by holding a pressure of 400 to 1000 kgf / cm 2 for 1 to 3 minutes. When the pressure is less than 400 kgf / cm 2 , a molded body having sufficient strength and density cannot be obtained. When the pressure is 1000 kgf / cm 2 or more, the molded body itself is out of pressure when taken out from the mold. It may break due to deformation due to being released, which is not preferable in production.

（焼結工程）
電気炉を使用し、酸素雰囲気中で成形体を焼結し、焼結体を得る。焼結温度１３５０〜１５００℃まで昇温する。昇温途中で、焼結体内の温度分布を小さくするために保持工程を導入する。途中保持温度は、反応が始まる前の温度帯で焼結体内の温度分布を小さくするため、６００〜８００℃の温度で導入すると良い。６００℃未満では温度が低温過ぎて効果がみられず、９００℃より高温の場合は、すでにある程度反応が進んでいるため、反り低減の効果が得られない。途中保持時間は１〜１０時間、好ましくは４〜６時間、とする。保持時間が短すぎると、反応の進行を十分に抑制できず、一方、保持時間が長すぎると生産性が低下するため好ましくない。 (Sintering process)
Using an electric furnace, the molded body is sintered in an oxygen atmosphere to obtain a sintered body. The sintering temperature is raised to 1350-1500 ° C. In the middle of the temperature increase, a holding process is introduced to reduce the temperature distribution in the sintered body. The intermediate holding temperature is preferably introduced at a temperature of 600 to 800 ° C. in order to reduce the temperature distribution in the sintered body in the temperature zone before the reaction starts. If the temperature is lower than 600 ° C., the temperature is too low and no effect is seen. If the temperature is higher than 900 ° C., the reaction has already progressed to some extent, so that the effect of reducing warpage cannot be obtained. The intermediate holding time is 1 to 10 hours, preferably 4 to 6 hours. If the holding time is too short, the progress of the reaction cannot be sufficiently suppressed. On the other hand, if the holding time is too long, productivity is lowered, which is not preferable.

そして、途中保持温度から焼結温度まで０．２〜２．０℃／ｍｉｎで昇温する。途中保持温度から焼結温度まで昇温速度が０．２℃／ｍｉｎより小さいと、所定温度になるまでに不必要に時間を要してしまうことと、密度が上がらないことがあり、昇温速度が２．０℃／ｍｉｎより大きいと、焼結体内の温度分布が小さくならずに、むらが生じたり、焼結体が割れてしまったりする。好ましくは、０．５〜１．５℃／ｍｉｎである。   And it heats up at 0.2-2.0 degrees C / min from holding temperature on the way to sintering temperature. If the heating rate from the holding temperature to the sintering temperature is less than 0.2 ° C / min, it may take time unnecessarily to reach the predetermined temperature and the density may not increase. When the speed is higher than 2.0 ° C./min, the temperature distribution in the sintered body is not reduced, and unevenness occurs or the sintered body is cracked. Preferably, it is 0.5 to 1.5 ° C./min.

焼結温度は１３５０〜１５００℃として、１〜１００時間ほど保持し、その後、炉冷または降温速度１．０〜５．０℃／ｍｉｎで降温する。焼結温度が１３５０℃より低いと、高密度の焼結体を得ることが出来ない。また、１５００℃以上の焼結温度では、酸化亜鉛の揮発により、焼結密度の低下や組成ずれが生じ、また炉ヒーター寿命が低下してしまうというコスト的問題もあるので、上限は１５００℃とすることが望ましい。好ましくは、１３８０〜１４２０℃である。また焼結温度における保持時間が１時間より短いと、焼結が充分進まず、焼結体の密度が充分高くならなかったり、焼結体が反ってしまったりする。保持時間が１００時間を越えても、不必要なエネルギーと時間を要する無駄が生じて生産上好ましくない。好ましくは、５〜３０時間である。   The sintering temperature is set to 1350 to 1500 ° C. and held for about 1 to 100 hours. When the sintering temperature is lower than 1350 ° C., a high-density sintered body cannot be obtained. At a sintering temperature of 1500 ° C. or higher, volatilization of zinc oxide causes a decrease in sintering density and a composition shift, and there is a cost problem that the life of the furnace heater is reduced. Therefore, the upper limit is 1500 ° C. It is desirable to do. Preferably, it is 1380-1420 degreeC. On the other hand, if the holding time at the sintering temperature is shorter than 1 hour, the sintering does not proceed sufficiently, the density of the sintered body does not become sufficiently high, or the sintered body is warped. Even if the holding time exceeds 100 hours, unnecessary energy and time is wasted, which is not preferable for production. Preferably, it is 5 to 30 hours.

次に、本発明の実施例について説明する。実施例、比較例では、酸化インジウム−酸化亜鉛系酸化物（ＩＺＯ）焼結体の原料粉末をプレス成形した成形体を作製する工程は、前記段落００２０〜００２６に記載する条件で実施し、さらに焼結工程は、段落００２７〜段落００２９に記載する条件の範囲で適宜設定して実施した。それぞれの焼結体の組成は表１に示す通りである。   Next, examples of the present invention will be described. In the examples and comparative examples, the step of producing a molded body obtained by press-molding the raw material powder of the indium oxide-zinc oxide based oxide (IZO) sintered body is performed under the conditions described in the paragraphs 0020 to 0026, The sintering process was carried out by appropriately setting within the range of conditions described in paragraphs 0027 to 0029. The composition of each sintered body is as shown in Table 1.

実施例等におけるアーキング試験は、シンクロン製マグネトロンスパッタ装置（型番：ＢＳＣ７０１１）を使用し、ＤＣパワー密度：２．３Ｗ／ｃｍ２、ガス圧：０．６Ｐａ、ガス流量３００ｓｃｃｍの条件で、アルゴン雰囲気中、３５時間連続してスパッタを行い、アーキングの発生状態を調べた。アーキングの検出は、ランドマークテクノロジー製マイクロアークモニター（ＭＡＭ ｇｅｎｅｓｉｓ）を用い、アーキング（マイクロアーク）発生回数（回）を測定した。アーキング判定基準は、検出電圧１００Ｖ以上、放出エネルギー（アーク放電が発生しているときのスパッタ電圧×スパッタ電流×発生時間）が２０ｍＪ以下のアーキングをカウントし、１０回以下であれば〇、それを超える場合は×とした。 The arcing test in Examples and the like uses a SYNCHRON magnetron sputtering apparatus (model number: BSC7011), DC power density: 2.3 W / cm 2 , gas pressure: 0.6 Pa, gas flow rate 300 sccm, in an argon atmosphere. Sputtering was continued for 35 hours, and the occurrence of arcing was examined. The arcing was detected by measuring the number of occurrences of arcing (microarc) using a Landmark Technology micro arc monitor (MAM genesis). The arcing criterion is that arcing with a detection voltage of 100 V or more and emission energy (sputtering voltage when the arc discharge is occurring × sputtering current × generation time) is 20 mJ or less. When exceeding, it was set as x.

（実施例１）
実施例１では、最高焼結温度を１４００℃、焼結保持時間を１０時間、途中保持温度を８００℃、とした。その結果、焼結体の密度は９８．４１％で、最大反り値は１．３９ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率は、２．４３ｍΩ・ｃｍ、その標準偏差は０．７８ｍΩ・ｃｍであった。実施例１では、このように焼結体の反り量が少なく、ターゲットのバルク抵抗率のばらつきが小さくという良好な結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生はほとんど見られなかった。以上の結果を、表１に示す。 Example 1
In Example 1, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, and the intermediate holding temperature was 800 ° C. As a result, the density of the sintered body was 98.41%, and the maximum warpage value was 1.39 mm. In addition, in order to adjust the sintered body to the target shape, both surfaces of the sintered body were ground so that they were flat. The target bulk resistivity was 2.43 mΩ · cm, and its standard deviation was 0.78 mΩ · cm. . In Example 1, good results were obtained that the amount of warpage of the sintered body was small and the variation in the bulk resistivity of the target was small. Moreover, when the target thus prepared was sputtered, almost no arcing was observed. The results are shown in Table 1.

（実施例２−１５）
実施例２−１５では、焼結体の組成、最高焼結温度、焼結保持時間、途中保持温度、途中保持時間、途中保持温度から焼結保持温度までの昇温速度、焼結体の面積、の各条件をそれぞれ変化させた。その結果、表１に示す通り、いずれの焼結体も密度が９８％以上であり、最大反り値は２．０ｍｍ以内であった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、いずれのターゲットのバルク抵抗率は、１．０〜１０．０ｍΩ・ｃｍであり、その標準偏差は１．０ｍΩ・ｃｍ以内であった。実施例２−１５では、このように焼結体の反り量が少なく、ターゲットのバルク抵抗率のばらつきが小さくという良好な結果が得られた。また、これらのターゲットをスパッタしたところ、アーキングの発生はほとんど見られなかった。 (Example 2-15)
In Example 2-15, the composition of the sintered body, the maximum sintering temperature, the sintering holding time, the intermediate holding temperature, the intermediate holding time, the heating rate from the intermediate holding temperature to the sintering holding temperature, the area of the sintered body Each condition was changed. As a result, as shown in Table 1, the density of each sintered body was 98% or more, and the maximum warpage value was within 2.0 mm. Moreover, in order to arrange the sintered body into the target shape, both surfaces of the sintered body were ground so as to be flat. The bulk resistivity of any target was 1.0 to 10.0 mΩ · cm, and the standard deviation was It was within 1.0 mΩ · cm. In Example 2-15, good results were obtained that the amount of warpage of the sintered body was small and the variation in the bulk resistivity of the target was small. Further, when these targets were sputtered, almost no arcing was observed.

（比較例１）
比較例１では、最高焼結温度を１４００℃、焼結保持時間を１０時間とし、途中保持は行わなかった。その結果、焼結体の最大反り値は２．３０ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．４０ｍΩ・ｃｍであった。比較例１では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 1)
In Comparative Example 1, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, and no intermediate holding was performed. As a result, the maximum warpage value of the sintered body was 2.30 mm. Further, in order to adjust the sintered body to the target shape, both surfaces of the sintered body were ground so that the standard deviation of the target bulk resistivity was 1.40 mΩ · cm. In Comparative Example 1, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例２）
比較例２では、最高焼結温度を１４００℃、焼結保持時間を１０時間とし、途中保持温度を５００℃と低くした。その結果、焼結体の最大反り値は２．０６ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．１８ｍΩ・ｃｍであった。比較例２では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 2)
In Comparative Example 2, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, and the intermediate holding temperature was lowered to 500 ° C. As a result, the maximum warpage value of the sintered body was 2.06 mm. Further, when the sintered body was ground so as to have a flat target shape, the standard deviation of the target bulk resistivity was 1.18 mΩ · cm. In Comparative Example 2, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例３）
比較例３では、最高焼結温度を１４００℃、焼結保持時間を１０時間とし、途中保持温度を９００℃と高くした。その結果、焼結体の最大反り値は２．１４ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．２４ｍΩ・ｃｍであった。比較例３では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 3)
In Comparative Example 3, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, and the holding temperature was as high as 900 ° C. As a result, the maximum warpage value of the sintered body was 2.14 mm. Further, in order to prepare the sintered body in a target shape, both surfaces of the sintered body were ground so as to be flat, and the standard deviation of the target bulk resistivity was 1.24 mΩ · cm. In Comparative Example 3, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例４）
比較例４では、最高焼結温度を１４００℃、焼結保持時間を１０時間とし、途中保持温度を１１００℃と高くした。その結果、焼結体の最大反り値は２．１１ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．１１ｍΩ・ｃｍであった。比較例４では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 4)
In Comparative Example 4, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, and the intermediate holding temperature was as high as 1100 ° C. As a result, the maximum warpage value of the sintered body was 2.11 mm. Further, when the sintered body was ground so as to be flat in order to prepare the sintered body, the standard deviation of the bulk resistivity of the target was 1.11 mΩ · cm. In Comparative Example 4, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例５）
比較例５では、最高焼結温度を１４００℃、焼結保持時間を１０時間、途中保持温度を８００℃とし、途中保持温度から最高焼結温度までの昇温速度を５℃／ｍｉｎと速くした。その結果、焼結体の最大反り値は２．２３ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．２６ｍΩ・ｃｍであった。比較例５では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 5)
In Comparative Example 5, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, the intermediate holding temperature was 800 ° C., and the rate of temperature increase from the intermediate holding temperature to the maximum sintering temperature was increased to 5 ° C./min. . As a result, the maximum warpage value of the sintered body was 2.23 mm. Further, in order to adjust the sintered body to the target shape, both surfaces of the sintered body were ground so as to be flat, and the standard deviation of the bulk resistivity of the target was 1.26 mΩ · cm. In Comparative Example 5, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例６）
比較例６では、最高焼結温度を１４００℃、焼結保持時間を１０時間、途中保持温度を８００℃とし、途中保持時間を１時間と短くした。その結果、焼結体の最大反り値は２．３１ｍｍとなった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．３１ｍΩ・ｃｍであった。比較例６では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 6)
In Comparative Example 6, the maximum sintering temperature was 1400 ° C., the sintering holding time was 10 hours, the intermediate holding temperature was 800 ° C., and the intermediate holding time was shortened to 1 hour. As a result, the maximum warpage value of the sintered body was 2.31 mm. Further, in order to prepare the sintered body in a target shape, both surfaces of the sintered body were ground so as to be flat, and the standard deviation of the target bulk resistivity was 1.31 mΩ · cm. In Comparative Example 6, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例７）
比較例７では、途中保持温度を８００℃とし、最高焼結温度を１６００℃と高くした。その結果、焼結体の最大反り量は２．３３ｍｍであり、相対密度が９７．５％であった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．４２ｍΩ・ｃｍであった。比較例７では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 7)
In Comparative Example 7, the intermediate holding temperature was 800 ° C., and the maximum sintering temperature was 1600 ° C. As a result, the maximum warpage amount of the sintered body was 2.33 mm, and the relative density was 97.5%. Further, in order to prepare the sintered body in a target shape, both surfaces of the sintered body were ground so as to be flat, and the standard deviation of the target bulk resistivity was 1.42 mΩ · cm. In Comparative Example 7, the result was that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large. Further, when the target thus produced was sputtered, arcing was frequently generated.

（比較例８）
比較例８では、途中保持温度を８００℃とし、最高焼結温度を１５００℃と高くした。その結果、焼結体の最大反り量は２．３７ｍｍであった。また、焼結体をターゲット形状に整えるために、その両面を平面になるように研削したところ、ターゲットのバルク抵抗率の標準偏差は１．５３ｍΩ・ｃｍであった。比較例８では、このように焼結体の反り量が大きく、ターゲットのバルク抵抗率のばらつきが大きいという結果が得られた。また、このようにして作製したターゲットをスパッタしたところ、アーキングの発生が多かった。 (Comparative Example 8)
In Comparative Example 8, the intermediate holding temperature was set to 800 ° C., and the maximum sintering temperature was increased to 1500 ° C. As a result, the maximum warpage amount of the sintered body was 2.37 mm. Further, in order to prepare the sintered body in a target shape, both surfaces of the sintered body were ground so as to be flat, and the standard deviation of the bulk resistivity of the target was 1.53 mΩ · cm. In Comparative Example 8, the result that the amount of warpage of the sintered body was large and the variation in the bulk resistivity of the target was large was obtained. Further, when the target thus produced was sputtered, arcing was frequently generated.

上記の通り、本発明は、従来と異なる焼結条件により、反りが小さい焼結体を歩留まりよく作製することができ、これにより、生産性を著しく向上させることができるという優れた効果を有する。また、本発明は、焼結体の反りを低減することで、該焼結体を加工した後のターゲットのスパッタ面のバルク抵抗率のばらつきが小さくことができ、特性が均一な膜を形成することができるという優れた効果を有する。本発明のスパッタリングターゲットは、液晶表示装置、薄膜エレクトロルミネッセンス表示装置、有機ＥＬなどに使用される透明導電膜の形成に有用である。
As described above, the present invention can produce a sintered body with a small warp with a high yield under different sintering conditions, and has an excellent effect that the productivity can be remarkably improved. In addition, the present invention reduces the warpage of the sintered body, thereby reducing the variation in the bulk resistivity of the sputtering surface of the target after processing the sintered body, and forming a film with uniform characteristics. It has an excellent effect of being able to. The sputtering target of this invention is useful for formation of the transparent conductive film used for a liquid crystal display device, a thin film electroluminescent display device, organic EL, etc.

Claims (3)

Ｉｎ、Ｚｎ、Ｏからなるスパッタリングターゲットであって、ＺｎとＩｎの原子比が０．０５≦Ｚｎ／（Ｉｎ＋Ｚｎ）≦０．３０を満たし、該ターゲットのスパッタ面の面積が６００００ｍｍ２以上で、スパッタ面におけるバルク抵抗率の標準偏差が１．０ｍΩ・ｃｍ以下であり、相対密度が９８％以上であることを特徴とするスパッタリングターゲット。 A sputtering target composed of In, Zn, and O, wherein the atomic ratio of Zn and In satisfies 0.05 ≦ Zn / (In + Zn) ≦ 0.30, the area of the sputtering surface of the target is 60000 mm 2 or more, and sputtering A sputtering target characterized in that the standard deviation of bulk resistivity on the surface is 1.0 mΩ · cm or less and the relative density is 98% or more. バルク抵抗率が１．０〜１０ｍΩ・ｃｍであることを特徴とする請求項１記載のスパッタリングターゲット。   2. The sputtering target according to claim 1, wherein the bulk resistivity is 1.0 to 10 mΩ · cm. スパッタ面の面積が６００００ｍｍ２〜４０００００ｍｍ２であることを特徴とする請求項１又は２に記載のスパッタリングターゲット。 The sputtering target according to claim 1 or 2 area of the sputtering surface is characterized by a 60000mm 2 ~400000mm 2.
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TW105137428A TWI645059B (en) 2016-03-31 2016-11-16 Indium oxide-zinc oxide (IZO) sputtered palladium and manufacturing method thereof
TW107122136A TWI661069B (en) 2016-03-31 2016-11-16 Manufacturing method of sputtering target
KR1020160163661A KR20170112970A (en) 2016-03-31 2016-12-02 Indium zinc oxide (izo) based sputtering target, and method for producing same
CN201810723839.6A CN108930015A (en) 2016-03-31 2016-12-28 Zinc-oxide-based (IZO) sputtering target of indium oxide-and its manufacturing method
CN202210337974.3A CN114752901A (en) 2016-03-31 2016-12-28 Indium oxide-zinc oxide (IZO) sputtering target and method for producing same
CN201611242711.5A CN107267936A (en) 2016-03-31 2016-12-28 Indium oxide is Zinc-oxide-based（IZO）Sputtering target and its manufacture method
KR1020180077156A KR101956506B1 (en) 2016-03-31 2018-07-03 Indium zinc oxide (izo) based sputtering target, and method for producing same
KR1020190017109A KR20190019104A (en) 2016-03-31 2019-02-14 Indium zinc oxide (izo) based sputtering target, and method for producing same
KR1020200017636A KR102322184B1 (en) 2016-03-31 2020-02-13 Indium zinc oxide (izo) based sputtering target, and method for producing same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6523510B1 (en) * 2018-03-30 2019-06-05 Ｊｘ金属株式会社 Sputtering target
JP2020143359A (en) * 2019-03-08 2020-09-10 Ｊｘ金属株式会社 Manufacturing method of sputtering target member, and sputtering target member
CN113555451A (en) * 2020-04-23 2021-10-26 南方科技大学 Preparation method of transparent photoelectric device and transparent photoelectric device
JP7162647B2 (en) * 2020-09-15 2022-10-28 Ｊｘ金属株式会社 Cu-W-O sputtering target and oxide thin film
CN113956022A (en) * 2021-11-30 2022-01-21 郑州大学 Zinc-doped indium oxide powder, sputtering target material and preparation method thereof
CN116177993A (en) * 2022-12-15 2023-05-30 先导薄膜材料（广东）有限公司 Indium zinc oxide sintered target and preparation method thereof
CN116162908A (en) * 2022-12-15 2023-05-26 先导薄膜材料（广东）有限公司 Indium zinc oxide target and preparation method thereof
CN116199496A (en) * 2022-12-15 2023-06-02 先导薄膜材料（广东）有限公司 Indium zinc oxide doped rare earth metal target material and preparation method thereof
CN116041047A (en) * 2022-12-15 2023-05-02 先导薄膜材料（广东）有限公司 IZO doped target material for sputtering and preparation method thereof
CN117247273B (en) * 2023-11-17 2024-02-23 江苏迪纳科精细材料股份有限公司 Preparation method and device of X-IZO magnetron sputtering target material with high mobility

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001131736A (en) * 1999-11-09 2001-05-15 Nikko Materials Co Ltd Sputtering target and method of manufacture
JP3721080B2 (en) * 1999-05-10 2005-11-30 株式会社日鉱マテリアルズ Sputtering target and manufacturing method thereof
US20060151321A1 (en) * 2004-03-05 2006-07-13 Tosoh Corporation Cylindrical sputtering target, ceramic sintered body, and process for producing sintered body
US20070117237A1 (en) * 2003-05-20 2007-05-24 Idemitsu Kosan Co., Ltd. Amorphous transparent conductive film, sputtering target as its raw material, amorphous transparent electrode substrate, process for producing the same and color filter for liquid crystal display
JP2008001554A (en) * 2006-06-22 2008-01-10 Idemitsu Kosan Co Ltd Sintered body, film, and organic electroluminescent element
JP2010024087A (en) * 2008-07-18 2010-02-04 Idemitsu Kosan Co Ltd Method for manufacturing oxide sintered compact, methods for manufacturing oxide sintered compact, sputtering target, oxide thin film and thin film transistor, and semiconductor device
JP2013147423A (en) * 2008-06-06 2013-08-01 Idemitsu Kosan Co Ltd Sputtering target for oxide thin film and process for producing the same
JP2014043598A (en) * 2012-08-24 2014-03-13 Ulvac Japan Ltd METHOD FOR MANUFACTURING InZnO BASED SPUTTERING TARGET
JP2015021165A (en) * 2013-07-19 2015-02-02 三菱マテリアル株式会社 Sputtering target and production method thereof

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3734540B2 (en) 1995-10-13 2006-01-11 三井金属鉱業株式会社 Manufacturing method of indium oxide-zinc oxide based sintered compact target
KR100849258B1 (en) 1999-11-25 2008-07-29 이데미쓰 고산 가부시키가이샤 Sputtering target and transparent conductive oxide
CN1320155C (en) * 2001-06-26 2007-06-06 三井金属矿业株式会社 Sputtering target for high resistance transparent conductive membrane and mfg. method of high resistance transparent conductive membrane
JP5156181B2 (en) 2005-06-30 2013-03-06 出光興産株式会社 Method for producing indium oxide / zinc oxide sintered body
JP4758697B2 (en) 2005-07-01 2011-08-31 出光興産株式会社 Manufacturing method of IZO sputtering target
CN102191465A (en) * 2010-03-18 2011-09-21 中国科学院福建物质结构研究所 Indium-doped zinc oxide target material and preparation method of transparent conducting film
CN103518003A (en) * 2011-05-10 2014-01-15 出光兴产株式会社 In2O3-ZnO sputtering target
KR101973873B1 (en) * 2013-03-29 2019-04-29 제이엑스금속주식회사 Igzo sputtering target and igzo film

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3721080B2 (en) * 1999-05-10 2005-11-30 株式会社日鉱マテリアルズ Sputtering target and manufacturing method thereof
JP2001131736A (en) * 1999-11-09 2001-05-15 Nikko Materials Co Ltd Sputtering target and method of manufacture
US20070117237A1 (en) * 2003-05-20 2007-05-24 Idemitsu Kosan Co., Ltd. Amorphous transparent conductive film, sputtering target as its raw material, amorphous transparent electrode substrate, process for producing the same and color filter for liquid crystal display
US20060151321A1 (en) * 2004-03-05 2006-07-13 Tosoh Corporation Cylindrical sputtering target, ceramic sintered body, and process for producing sintered body
JP2008001554A (en) * 2006-06-22 2008-01-10 Idemitsu Kosan Co Ltd Sintered body, film, and organic electroluminescent element
JP2013147423A (en) * 2008-06-06 2013-08-01 Idemitsu Kosan Co Ltd Sputtering target for oxide thin film and process for producing the same
JP2010024087A (en) * 2008-07-18 2010-02-04 Idemitsu Kosan Co Ltd Method for manufacturing oxide sintered compact, methods for manufacturing oxide sintered compact, sputtering target, oxide thin film and thin film transistor, and semiconductor device
JP2014043598A (en) * 2012-08-24 2014-03-13 Ulvac Japan Ltd METHOD FOR MANUFACTURING InZnO BASED SPUTTERING TARGET
JP2015021165A (en) * 2013-07-19 2015-02-02 三菱マテリアル株式会社 Sputtering target and production method thereof

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