JP2012132065A - Cylindrical sputtering target and method for manufacturing the same - Google Patents
Cylindrical sputtering target and method for manufacturing the same Download PDFInfo
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本発明は、マグネトロン型回転カソードスパッタリング装置等に用いられる円筒形セラミックススパッタリングターゲットおよびその製造に関するものであり、少なくともスパッタリングターゲット材内周面に２層の金属下地層を設けたスパッタリングターゲットに関する。 The present invention relates to a cylindrical ceramic sputtering target used in a magnetron type rotary cathode sputtering apparatus and the like, and its production, and more particularly to a sputtering target in which two metal underlayers are provided on the inner peripheral surface of a sputtering target material.
マグネトロン型回転カソードスパッタリング装置等に用いられるセラミックスターゲットの製造方法としては、別途作製したセラミックス焼結体からなる円筒形ターゲット材を円筒形支持基材に組み込み、低融点半田等の接合材を用いて接合する方法がある（特許文献１参照）。この形態の円筒形ターゲットは比較的低コストで作製でき、高密度のセラミックス焼結体を使用できることから高品位な成膜が可能であり、今後の普及が見込まれている。 As a method of manufacturing a ceramic target used in a magnetron type rotary cathode sputtering apparatus or the like, a cylindrical target material made of a separately prepared ceramic sintered body is incorporated into a cylindrical support base material, and a bonding material such as a low melting point solder is used. There is a method of joining (see Patent Document 1). A cylindrical target of this form can be produced at a relatively low cost, and since a high-density ceramic sintered body can be used, high-quality film formation is possible, and it is expected to spread in the future.
しかし、一方で、この形態の円筒形ターゲットは熱膨張率の異なる二つの円筒形状物を組み合わせ、その間隙を接合材で固定するため、高温となる接合時と冷却固化後では双方の体積収縮量の違いから内部応力が生じ、接合部に剥離等の不具合が発生しやすい。接合が不十分な状態のターゲットでスパッタリングを行なうと、ターゲット材の冷却効率が低下し、ターゲット材が割れる恐れがある。それゆえ、接合率および接合強度を高められる簡便な接合方法の開発が望まれている。 However, on the other hand, this type of cylindrical target combines two cylindrical objects with different coefficients of thermal expansion, and the gap is fixed with a bonding material. Therefore, both volume shrinkage during high temperature bonding and after cooling and solidification Due to the difference, internal stress is generated and defects such as peeling are likely to occur at the joint. When sputtering is performed with a target with insufficient bonding, the cooling efficiency of the target material is lowered, and the target material may be broken. Therefore, development of a simple joining method capable of increasing the joining rate and joining strength is desired.
元来、セラミックスと金属は接合しづらく、低融点半田等の接合材を溶融し、セラミックスに接触させ冷却固化しただけでは接合が難しい。一方、支持基材は金属製であっても、接合時に接合材の融点以上に加熱されるため表面の酸化が進行し、このため溶融した接合材との濡れ性が悪くなり、冷却固化後の接合材の密着力が低下する恐れがある。 Originally, ceramics and metals are difficult to bond, and it is difficult to bond them simply by melting a bonding material such as low melting point solder and bringing it into contact with ceramics and solidifying by cooling. On the other hand, even if the support substrate is made of metal, the surface is oxidized because it is heated to the melting point of the bonding material at the time of bonding, so that the wettability with the molten bonding material deteriorates, and after cooling and solidification There is a possibility that the adhesion of the bonding material may be reduced.
これらの問題を解決する手段として、予めアルミまたはアルミ合金等の金属またはスパッタリングターゲットの表面を酸処理した後、スパッタリングターゲット材の接合面または、スパッタリングターゲット材と支持基体の両接合表面に半田層を電気メッキにより形成した後、半田層を溶融させた状態で両接合面を密着させ、一体化した状態で冷却して固着する方法が知られている（特許文献２参照）。しかしこの方法では、スパッタリングターゲットの材料がセラミックスである場合、電気メッキにより形成した半田層はセラミックスへの密着力が弱く、十分な接合強度を得ることが困難である。 As a means for solving these problems, a metal such as aluminum or aluminum alloy or the surface of a sputtering target is previously acid-treated, and then a solder layer is formed on the bonding surface of the sputtering target material or both the bonding surfaces of the sputtering target material and the support substrate. A method is known in which, after forming by electroplating, both joining surfaces are brought into close contact with each other in a molten state, and then cooled and fixed in an integrated state (see Patent Document 2). However, in this method, when the material of the sputtering target is ceramic, the solder layer formed by electroplating has weak adhesion to the ceramic, and it is difficult to obtain sufficient bonding strength.
一般に、セラミックスに金属をめっきする場合、密着性がよい金属は限られており、それらはニッケル（Ｎｉ）や銅（Ｃｕ）などである。ただし、ＮｉやＣｕは接合時に表面酸化が進行し、接合材の低融点半田との濡れ性が低下するため、これらの金属だけで下地層を形成しても十分な接合強度を得ることはできない。 In general, when metal is plated on ceramics, metals having good adhesion are limited, such as nickel (Ni) and copper (Cu). However, Ni and Cu undergo surface oxidation at the time of bonding, and the wettability of the bonding material with the low-melting-point solder decreases, so that sufficient bonding strength cannot be obtained even if the base layer is formed with only these metals. .
また、接合強度の高いスパッタリングターゲットを得る接合方法として、チタン（Ｔｉ）またはチタン合金（Ｔｉ合金）のスパッタリングターゲット材およびＣｕ、Ｃｕ合金、ＴｉおよびＴｉ合金などの支持基材両接合面にＮｉあるいはＣｕをメッキ処理した後、スパッタリングターゲット材および支持基材両面に接合する半田材の一部分を超音波メタライジング法により半田処理し、スパッタリングターゲットと支持基材とを強固に接合する方法が提案されている（特許文献３参照）。しかしこの方法では、スパッタリングターゲットが平板構造である場合においては可能な手段であるが、たとえば円筒形ターゲットに関しては、円筒形ターゲット材の内径が小さい場合、あるいは円筒形ターゲット材の中心軸方向の長さが長い場合は、接合面に超音波メタライジング装置の超音波発信端が接触できない部分が生じ、接合面全体にくまなく超音波メタライジング処理を施すことが困難となる。 Further, as a joining method for obtaining a sputtering target having a high joining strength, Ni or Ti on a joining surface of both a sputtering base material of titanium (Ti) or a titanium alloy (Ti alloy) and a supporting base material such as Cu, Cu alloy, Ti and Ti alloy. After plating Cu, a method is proposed in which a part of a solder material to be bonded to both sides of a sputtering target material and a supporting substrate is soldered by an ultrasonic metallizing method to firmly bond the sputtering target and the supporting substrate. (See Patent Document 3). However, this method is possible when the sputtering target has a flat plate structure. For example, in the case of a cylindrical target, when the inner diameter of the cylindrical target material is small or the length of the cylindrical target material in the central axis direction is long. When the length is long, a portion where the ultrasonic wave transmitting end of the ultrasonic metallizing device cannot contact is formed on the bonding surface, and it is difficult to perform the ultrasonic metallizing process all over the bonding surface.
また、平板構造のターゲットを接合する場合、ターゲット材と支持基材の間隙に溶融した接合材を満たし、ターゲット材と支持基材を互いに近づけるように押圧することで接合材の密着性を高めることも可能であるが、円筒形ターゲットでは構造上、そのような押圧操作が行えないということも接合が難しい要因となっている。 In addition, when joining flat-plate targets, the gap between the target material and the supporting base material is filled with the molten joining material, and the target material and the supporting base material are pressed closer together to increase the adhesiveness of the joining material. However, due to the structure of the cylindrical target, such a pressing operation cannot be performed, which makes it difficult to join.
本発明の課題は、円筒形状のセラミックス焼結体からなるターゲット材と円筒形支持基材の接合に際し、接合面に２層の金属下地層を形成することにより、接合の際に接合部を押圧しなくても冷却固化させるだけで十分な接合率および接合強度が得られ、スパッタリング中に熱の影響を受けても割れの発生を著しく低減できるスパッタリングターゲットおよびその製造方法を提供することにある。 An object of the present invention is to form a metal base layer of two layers on a joining surface when joining a target material made of a cylindrical ceramic sintered body and a cylindrical support base material, thereby pressing the joining portion during joining. It is an object of the present invention to provide a sputtering target and a method for manufacturing the sputtering target that can obtain a sufficient bonding rate and bonding strength only by cooling and solidification, and can significantly reduce the occurrence of cracks even under the influence of heat during sputtering.
本発明者らは、上記課題を解決するために鋭意検討を行った結果、本発明を完成するに至った。 As a result of intensive studies to solve the above problems, the present inventors have completed the present invention.
即ち本発明は、以下のとおりである。
（１）円筒形支持基材の外側に、円筒形状のセラミックス焼結体からなるターゲット材を接合材で接合した円筒形スパッタリングターゲットであって、ターゲット材の内周面に、またはターゲット材の内周面と円筒形支持基材の外周面の両方に、ニッケルまたは銅からなる第１の下地層を有し、その第１の下地層の上に、スズからなる第２の下地層を有することを特徴とする、円筒形スパッタリングターゲット。
（２）第１の下地層と第２の下地層の合計の厚みが１０〜２００μｍである、（１）に記載のターゲット。
（３）円筒形状のセラミックス焼結体からなるターゲット材の内周面に、または円筒形状のセラミックス焼結体からなるターゲット材の内周面と円筒形支持基材の外周面の両方に、ニッケルまたは銅からなる第１の下地層を形成し、その第１の下地層の上に、スズからなる第２の下地層を形成し、次いで、そのターゲット材を円筒形支持基材の外側に配置し、両者を接合材で接合することを特徴とする、（１）または（２）に記載のターゲットの製造方法。
That is, the present invention is as follows.
(1) A cylindrical sputtering target in which a target material composed of a cylindrical ceramic sintered body is bonded to the outer side of a cylindrical support base material with a bonding material, and is formed on the inner peripheral surface of the target material or inside the target material. Having a first underlayer made of nickel or copper on both the peripheral surface and the outer peripheral surface of the cylindrical support base, and having a second underlayer made of tin on the first underlayer A cylindrical sputtering target.
(2) The target according to (1), wherein the total thickness of the first underlayer and the second underlayer is 10 to 200 μm.
(3) Nickel on the inner peripheral surface of the target material made of a cylindrical ceramic sintered body or on both the inner peripheral surface of the target material made of a cylindrical ceramic sintered body and the outer peripheral surface of the cylindrical support substrate Alternatively, a first base layer made of copper is formed, a second base layer made of tin is formed on the first base layer, and then the target material is disposed outside the cylindrical support base material. And both are joined with a joining material, The manufacturing method of the target as described in (1) or (2) characterized by the above-mentioned.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明において、円筒形状のセラミックス焼結体からなるターゲット材は特に限定されるものではないが、例えば透明導電膜などに用いられる光学薄膜材料である、ＩＴＯ（Ｉｎｄｉｕｍ Ｔｉｎ Ｏｘｉｄｅ）、ＺｎＯ（Ｚｉｎｃ Ｏｘｉｄｅ）、ＡＺＯ（Ａｌｕｍｉｎｉｕｍ Ｚｉｎｃ Ｏｘｉｄｅ）、ＩＺＯ（Ｉｎｄｉｕｍ Ｚｉｎｃ Ｏｘｉｄｅ）、Ｔａ２Ｏ５、Ｎｂ２Ｏ５、ＴｉＯ２等を挙げることができる。 In the present invention, the target material made of a cylindrical ceramic sintered body is not particularly limited. For example, ITO (Indium Tin Oxide) and ZnO (Zinc Oxide), which are optical thin film materials used for transparent conductive films and the like, are used. ), AZO (Aluminum Zinc Oxide), IZO (Indium Zinc Oxide), Ta 2 O 5 , Nb 2 O 5 , TiO 2 and the like.
円筒形支持基材の材質としては、例えばステンレス（ＳＵＳ）、チタン（Ｔｉ）、チタン合金（Ｔｉ合金）などである。 Examples of the material of the cylindrical support base include stainless steel (SUS), titanium (Ti), titanium alloy (Ti alloy), and the like.
接合材としては融点が約２３０℃よりも低い低融点半田などが用いられ、例えば鉛フリーのインジウム（融点１５７℃）やスズ―インジウム合金（１１７℃）が用いられる。 As the bonding material, a low melting point solder having a melting point lower than about 230 ° C. is used. For example, lead-free indium (melting point: 157 ° C.) or tin-indium alloy (117 ° C.) is used.
第１の下地層には、接合材よりも融点が高くセラミックスターゲット材に対して密着性のよいＮｉ（融点１４５５℃）またはＣｕ（融点１０８４℃）が選ばれる。第１の下地層の上に第２の下地層を形成するが、第２の下地層は接合材より融点が高く、第１の下地層との密着性がよく、かつ接合材との濡れ性がよい金属であるスズ（Ｓｎ：融点２３２℃）を用いる。特にＳｎは接合時の高温においても表面酸化が進行しないため、接合材との濡れ性が低下しない。
第１および第２の下地層の形成法としては、スパッタリング法、イオンプレーティング法、蒸着法、メッキ法などがあるが、セラミックスターゲット材に下地層を形成する方法としてはメッキ法が好ましい。メッキ法としては特に限定されるものではなく、電解メッキまたは無電解メッキのいずれであってもよい。
For the first underlayer, Ni (melting point 1455 ° C.) or Cu (melting point 1084 ° C.) having a melting point higher than that of the bonding material and good adhesion to the ceramic target material is selected. The second underlayer is formed on the first underlayer. The second underlayer has a higher melting point than the bonding material, good adhesion to the first underlayer, and wettability with the bonding material. However, tin (Sn: melting point 232 ° C.) which is a good metal is used. In particular, Sn does not proceed with surface oxidation even at a high temperature during bonding, so that the wettability with the bonding material does not decrease.
As a method for forming the first and second underlayers, there are a sputtering method, an ion plating method, a vapor deposition method, a plating method, and the like. A plating method is preferable as a method for forming the underlayer on the ceramic target material. The plating method is not particularly limited, and may be either electrolytic plating or electroless plating.
第１および第２の下地層の厚みは密着性や作業時間を考慮し、それぞれ５〜１００μｍが好ましい。 The thickness of the first and second underlayers is preferably 5 to 100 μm in consideration of adhesion and working time.
本発明においては、第１および第２の下地層は円筒形状のセラミックス焼結体からなるターゲット材の内周面だけでなく、円筒形支持基材の外周面にも形成することが好ましい。その形成方法には前述と同様の方法を用いることができ、これにより円筒形支持基材の濡れ性を改善することができる。 In the present invention, the first and second underlayers are preferably formed not only on the inner peripheral surface of the target material made of a cylindrical ceramic sintered body but also on the outer peripheral surface of the cylindrical support substrate. As the forming method, the same method as described above can be used, whereby the wettability of the cylindrical support substrate can be improved.
上述のように第１および第２の下地層を形成した後、円筒形支持基材の外側に円筒形状のターゲット材を配置する。このとき、両者の中心軸が合うように配置してもよく、また複数の円筒形状のターゲット材を用いる場合は、それらの外周面ができるだけそろうように配置してもよい。その後、円筒形状のターゲット材および円筒形支持基材を接合材の融点以上に加熱し、両者の隙間に溶融した接合材を注入し、冷却固化させることにより接合する。 After forming the first and second underlayers as described above, a cylindrical target material is disposed outside the cylindrical support base material. At this time, they may be arranged so that the central axes of the two are aligned, and when a plurality of cylindrical target materials are used, they may be arranged so that their outer peripheral surfaces are as close as possible. Thereafter, the cylindrical target material and the cylindrical support substrate are heated to the melting point or higher of the bonding material, and the molten bonding material is injected into the gap between the two, and bonded by cooling and solidifying.
このような方法においては、形成した下地層が接合作業中に溶融することを防ぐため、下地層を構成する金属は接合材よりも高融点であることが必要であるが、本発明の第１の下地層に用いられるＮｉやＣｕ、および第２の下地層に用いられるＳｎは、いずれも前述のように融点が高いため問題はない。そしてこれらの金属で接合面に二層の下地層を形成することにより、接合率および接合強度が高い円筒形スパッタリングターゲットを得ることができる。 In such a method, in order to prevent the formed underlayer from melting during the bonding operation, the metal constituting the underlayer needs to have a higher melting point than the bonding material. Any of Ni and Cu used for the underlying layer and Sn used for the second underlying layer have no problem since they have a high melting point as described above. A cylindrical sputtering target having a high bonding rate and high bonding strength can be obtained by forming a two-layer underlayer on the bonding surface using these metals.
本発明によれば、接合率および接合強度が高い円筒形セラミックスのターゲットを得ることができ、スパッタリング時の割れの発生が著しく抑制される。 According to the present invention, a cylindrical ceramic target having a high bonding rate and bonding strength can be obtained, and the occurrence of cracks during sputtering is significantly suppressed.
以下、本発明について実施例をもって説明するが、本発明はこれに限定されるものではない。なお、放電試験はスパッタリングガスにアルゴンを使用し、スパッタリング圧力：０．３Ｐａ、電力４５００Ｗで行った。 Hereinafter, although an example explains the present invention, the present invention is not limited to this. The discharge test was performed using argon as a sputtering gas and at a sputtering pressure of 0.3 Pa and a power of 4500 W.
（実施例１）
円筒形ＩＴＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、Ｔｉ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＩＴＯターゲット材の内周面およびＴｉ製円筒形基材の外周面に、第１の下地層としてＮｉを膜厚５μｍ、第１の下地層の上に第２の下地層としてＳｎを膜厚１５μｍ、それぞれ電気メッキ法で形成した。Ｔｉ製円筒形基材を垂直に立て、その外側に円筒形ＩＴＯターゲット材を両者の中心軸が一致するように配置し固定した。この組み立て品をリボンヒーターを用いて１８０℃まで加熱し、円筒形ＩＴＯターゲット材の内周面とＴｉ製円筒形基材の外周面の間に形成されるクリアランスに溶融させたＩｎ半田を流し込み、その後、冷却固化させた。この方法によって作製した円筒形ＩＴＯスパッタリングターゲットを超音波探傷装置（日本クラウトクレーマー製）で測定したところ、接合率は９７％であった。この円筒形ＩＴＯスパッタリングターゲットの放電試験を行なった結果、使用率８０％においても割れは認められなかった。
Example 1
Prepare one cylindrical ITO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one Ti cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) On the inner peripheral surface of the cylindrical ITO target material and the outer peripheral surface of the Ti cylindrical substrate, Ni is used as a first underlayer with a film thickness of 5 μm, and Sn as a second underlayer on the first underlayer. A film thickness of 15 μm was formed by electroplating. A cylindrical cylindrical substrate made of Ti was set up vertically, and a cylindrical ITO target material was arranged and fixed on the outside thereof so that the central axes of both coincided. This assembly is heated to 180 ° C. using a ribbon heater, and molten In solder is poured into the clearance formed between the inner peripheral surface of the cylindrical ITO target material and the outer peripheral surface of the Ti cylindrical substrate, Thereafter, it was cooled and solidified. When the cylindrical ITO sputtering target produced by this method was measured with an ultrasonic flaw detector (manufactured by Nippon Kraut Kramer), the joining rate was 97%. As a result of conducting a discharge test of this cylindrical ITO sputtering target, no crack was observed even at a usage rate of 80%.
（比較例１）
円筒形ＩＴＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、Ｔｉ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＩＴＯターゲット材の内周面およびＴｉ製円筒形基材の外周面に下地層としてＮｉを膜厚５μｍで電気メッキ法にて形成した。実施例１と同様にして、円筒形ＩＴＯターゲット材とＴｉ製円筒形基材をＩｎ半田で接合し、円筒形ＩＴＯスパッタリングターゲットを作製した。この方法によって作製した円筒形ＩＴＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、３５％であった。この円筒形ＩＴＯスパッタリングターゲットの放電試験を行なった結果、放電中に割れが発生した。
(Comparative Example 1)
Prepare one cylindrical ITO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one Ti cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) Then, Ni was formed as an underlayer on the inner peripheral surface of the cylindrical ITO target material and the outer peripheral surface of the Ti cylindrical substrate by electroplating with a film thickness of 5 μm. In the same manner as in Example 1, a cylindrical ITO target material and a Ti cylindrical substrate were joined with In solder to produce a cylindrical ITO sputtering target. When the joining rate of the cylindrical ITO sputtering target produced by this method was measured in the same manner as in Example 1, it was 35%. As a result of conducting a discharge test of this cylindrical ITO sputtering target, cracks occurred during discharge.
（比較例２）
実施例１と同様にして、但し円筒形ＩＴＯターゲット材およびＴｉ製円筒形基材に下地層を形成せずにＩｎ半田で接合を試みたが、濡れ性が悪く、両者は接合できなかった。.
（実施例２）
円筒形ＡＺＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、ＳＵＳ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＡＺＯターゲット材の内周面に第１の下地層としてＣｕを膜厚５μｍ、第１の下地層の上に第２の下地層としてＳｎを膜厚１５μｍ、それぞれ電気メッキ法で形成した。また、ＳＵＳ製円筒形基材の外周面に第１の下地層としてＮｉを膜厚５μｍ、第１の下地層の上に第２の下地層としてＳｎを膜厚１５μｍ、それぞれ電気メッキ法で形成した。ＳＵＳ製円筒形基材を垂直に立て、その外側に円筒形ＡＺＯターゲット材を両者の中心軸が一致するように配置し固定した。この組み立て品をリボンヒーターを用いて１８０℃まで加熱し、円筒形ＡＺＯターゲット材の内周面とＳＵＳ製円筒形基材の外周面の間に形成されるクリアランスに溶融させたＩｎ半田を流し込み、その後、冷却固化させた。この方法によって作製した円筒形ＡＺＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、９５％であった。この円筒形ＡＺＯスパッタリングターゲットの放電試験を行なった結果、使用率８１％においても割れは認められなかった。
(Comparative Example 2)
In the same manner as in Example 1, however, joining was attempted with In solder without forming an underlayer on the cylindrical ITO target material and the Ti cylindrical base material, but the wettability was poor and both could not be joined. .
(Example 2)
Prepare one cylindrical AZO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one SUS cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) In addition, Cu was formed as a first underlayer on the inner peripheral surface of the cylindrical AZO target material with a thickness of 5 μm, and Sn was formed as a second underlayer on the first underlayer with a thickness of 15 μm by an electroplating method. . Further, Ni is formed as a first underlayer on the outer peripheral surface of the SUS cylindrical base material with a thickness of 5 μm, and Sn is formed as a second underlayer on the first underlayer with a thickness of 15 μm by an electroplating method. did. A SUS cylindrical base material was set up vertically, and a cylindrical AZO target material was arranged and fixed on the outer side thereof so that the central axes of both coincided. This assembly is heated to 180 ° C. using a ribbon heater, and molten In solder is poured into the clearance formed between the inner peripheral surface of the cylindrical AZO target material and the outer peripheral surface of the SUS cylindrical base material, Thereafter, it was cooled and solidified. When the joining ratio of the cylindrical AZO sputtering target produced by this method was measured in the same manner as in Example 1, it was 95%. As a result of conducting a discharge test of this cylindrical AZO sputtering target, no crack was observed even at a usage rate of 81%.
（比較例３）
円筒形ＡＺＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、ＳＵＳ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＡＺＯターゲット材の内周面に下地層としてＣｕを膜厚５μｍで電気メッキ法にて形成し、ＳＵＳ製円筒形基材の外周面には下地層としてＮｉを膜厚５μｍで電気メッキ法にて形成した。実施例２と同様にして円筒形ＡＺＯターゲット材とＳＵＳ製円筒形基材をＩｎ半田で接合し、円筒形ＡＺＯスパッタリングターゲットを作製した。この円筒形ＡＺＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、２９％であった。この円筒形ＡＺＯスパッタリングターゲットの放電試験を行なった結果、放電中に割れが発生した。
(Comparative Example 3)
Prepare one cylindrical AZO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one SUS cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) Then, Cu is formed on the inner peripheral surface of the cylindrical AZO target material as an underlayer by electroplating with a film thickness of 5 μm, and Ni is formed on the outer peripheral surface of the SUS cylindrical base material as an underlayer with a film thickness of 5 μm. Formed by the method. In the same manner as in Example 2, the cylindrical AZO target material and the SUS cylindrical base material were joined with In solder to produce a cylindrical AZO sputtering target. When the joining rate of this cylindrical AZO sputtering target was measured in the same manner as in Example 1, it was 29%. As a result of conducting a discharge test of this cylindrical AZO sputtering target, cracks occurred during discharge.
（比較例４）
実施例２において、円筒形ＡＺＯターゲット材およびＳＵＳ製円筒形基材に下地層を形成せずにＩｎ半田で接合を試みたが、濡れ性が悪く、接合できなかった。
(Comparative Example 4)
In Example 2, joining was attempted with In solder without forming an underlayer on the cylindrical AZO target material and the cylindrical base material made of SUS, but the wettability was poor and joining was not possible.
（実施例３）
円筒形ＩＺＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、Ｔｉ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＩＺＯターゲット材の内周面およびＴｉ製円筒形基材の外周面に、第１の下地層としてＮｉを膜厚５μｍ、第１の下地層の上に第２の下地層としてＳｎを膜厚１５μｍ、それぞれ電気メッキ法で形成した。Ｔｉ製円筒形基材を垂直に立て、その外側に円筒形ＩＺＯターゲット材を両者の中心軸が一致するように配置し固定した。この組み立て品をリボンヒーターを用いて１８０℃まで加熱し、円筒形ＩＺＯターゲット材の内周面とＴｉ製円筒形基材の外周面の間に形成されるクリアランスに溶融させたＩｎ半田を流し込み、その後、冷却固化させた。この方法によって作製した円筒形ＩＺＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、９６％であった。この円筒形ＩＺＯスパッタリングターゲットの放電試験を行なった結果、使用率８０％においても割れは認められなかった。
(Example 3)
Prepare one cylindrical IZO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one Ti cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) On the inner peripheral surface of the cylindrical IZO target material and the outer peripheral surface of the Ti cylindrical base material, Ni is formed as a first underlayer with a film thickness of 5 μm, and Sn is formed as a second underlayer on the first underlayer. A film thickness of 15 μm was formed by electroplating. A Ti cylindrical base material was set up vertically, and a cylindrical IZO target material was arranged and fixed on the outside thereof so that the central axes of both coincided. This assembly is heated to 180 ° C. using a ribbon heater, and molten In solder is poured into the clearance formed between the inner peripheral surface of the cylindrical IZO target material and the outer peripheral surface of the Ti cylindrical base material, Thereafter, it was cooled and solidified. When the joining rate of the cylindrical IZO sputtering target produced by this method was measured in the same manner as in Example 1, it was 96%. As a result of conducting a discharge test of this cylindrical IZO sputtering target, no crack was observed even at a usage rate of 80%.
（比較例５）
円筒形ＩＺＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、Ｔｉ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＩＺＯターゲット材の内周面およびＴｉ製円筒形基材の外周面に、下地層としてＮｉを膜厚５μｍで電気メッキ法にて形成した。実施例３と同様にして円筒形ＩＺＯターゲット材とＴｉ製円筒形基材をＩｎ半田で接合し、円筒形ＩＺＯスパッタリングターゲットを作製した。この円筒形ＩＺＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、２７％であった。この円筒形ＩＺＯスパッタリングターゲットの放電試験を行なった結果、放電中に割れが発生した。
(Comparative Example 5)
Prepare one cylindrical IZO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one Ti cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) As a base layer, Ni was formed by electroplating with a film thickness of 5 μm on the inner peripheral surface of the cylindrical IZO target material and the outer peripheral surface of the Ti cylindrical base material. In the same manner as in Example 3, a cylindrical IZO target material and a Ti cylindrical substrate were joined with In solder to produce a cylindrical IZO sputtering target. When the joining ratio of this cylindrical IZO sputtering target was measured in the same manner as in Example 1, it was 27%. As a result of conducting a discharge test of this cylindrical IZO sputtering target, cracks occurred during discharge.
（比較例６）
実施例３において、円筒形ＩＺＯターゲット材およびＴｉ製円筒形基材に下地層を形成せずにＩｎ半田で接合を試みたが、濡れ性が悪く、両者は接合できなかった。
(Comparative Example 6)
In Example 3, joining was attempted with In solder without forming an underlayer on the cylindrical IZO target material and the Ti cylindrical base material, but the wettability was poor and both could not be joined.
（実施例４）
円筒形ＩＴＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、ＳＵＳ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＩＴＯターゲット材の内周面に、第１の下地層としてＮｉを膜厚５μｍ、第１の下地層の上に第２の下地層としてＳｎを膜厚１５μｍ、それぞれ電気メッキ法で形成した。ＳＵＳ製円筒形基材の外周面には超音波半田ごてを使用してＩｎ半田を下塗りした。ＳＵＳ製円筒形基材を垂直に立て、その外側に円筒形ＩＴＯターゲット材を両者の中心軸が一致するように配置し固定した。この組み立て品をリボンヒーターを用いて１８０℃まで加熱し、円筒形ＩＴＯターゲット材の内周面とＳＵＳ製円筒形基材の外周面の間に形成されるクリアランスに溶融させたＩｎ半田を流し込み、その後、冷却固化させた。この方法によって作製した円筒形ＩＴＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、９５％であった。この円筒形ＩＴＯスパッタリングターゲットの放電試験を行なった結果、使用率８１％においても割れは認められなかった。
Example 4
Prepare one cylindrical ITO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one SUS cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) On the inner surface of the cylindrical ITO target material, Ni is formed as a first underlayer with a thickness of 5 μm, and Sn is formed as a second underlayer with a thickness of 15 μm on the first underlayer by electroplating. did. An In solder was undercoated on the outer peripheral surface of the SUS cylindrical base material using an ultrasonic soldering iron. A SUS cylindrical base material was set up vertically, and a cylindrical ITO target material was arranged and fixed on the outside thereof so that the central axes of both coincided. This assembly is heated to 180 ° C. using a ribbon heater, and molten In solder is poured into the clearance formed between the inner peripheral surface of the cylindrical ITO target material and the outer peripheral surface of the SUS cylindrical base material, Thereafter, it was cooled and solidified. When the joining rate of the cylindrical ITO sputtering target produced by this method was measured in the same manner as in Example 1, it was 95%. As a result of conducting a discharge test of this cylindrical ITO sputtering target, no crack was observed even at a usage rate of 81%.
（実施例５）
円筒形ＡＺＯターゲット材（外径：１５０ｍｍφ、内径：１３０ｍｍφ、長さ：３００ｍｍ）を１個、ＳＵＳ製円筒形基材（外径：１２８ｍｍφ、内径：１２２ｍｍφ、長さ：４００ｍｍ）を１個用意し、円筒形ＡＺＯターゲット材の内周面に、第１の下地層としてＣｕを膜厚５μｍ、第１の下地層の上に第２の下地層としてＳｎを膜厚１５μｍ、それぞれ電気メッキ法で形成した。ＳＵＳ製円筒形基材の外周面には超音波半田ごてを使用してＩｎ半田を下塗りした。ＳＵＳ製円筒形基材を垂直に立て、その外側に円筒形ＡＺＯターゲット材を両者の中心軸が一致するように配置し固定した。この組み立て品をリボンヒーターを用いて１８０℃まで加熱し、円筒形ＡＺＯターゲット材の内周面とＳＵＳ製円筒形基材の外周面の間に形成されるクリアランスに溶融させたＩｎ半田を流し込み、その後、冷却固化させた。この方法によって作製した円筒形ＡＺＯスパッタリングターゲットの接合率を実施例１と同様にして測定したところ、９６％であった。この円筒形ＡＺＯスパッタリングターゲットの放電試験を行なった結果、使用率８０％においても割れは認められなかった。
(Example 5)
Prepare one cylindrical AZO target material (outer diameter: 150 mmφ, inner diameter: 130 mmφ, length: 300 mm) and one SUS cylindrical substrate (outer diameter: 128 mmφ, inner diameter: 122 mmφ, length: 400 mm) On the inner peripheral surface of the cylindrical AZO target material, Cu is formed as a first underlayer with a thickness of 5 μm, and Sn is formed as a second underlayer with a thickness of 15 μm on the first underlayer by electroplating. did. An In solder was undercoated on the outer peripheral surface of the SUS cylindrical base material using an ultrasonic soldering iron. A SUS cylindrical base material was set up vertically, and a cylindrical AZO target material was arranged and fixed on the outer side thereof so that the central axes of both coincided. This assembly is heated to 180 ° C. using a ribbon heater, and molten In solder is poured into the clearance formed between the inner peripheral surface of the cylindrical AZO target material and the outer peripheral surface of the SUS cylindrical base material, Thereafter, it was cooled and solidified. When the joining ratio of the cylindrical AZO sputtering target produced by this method was measured in the same manner as in Example 1, it was 96%. As a result of conducting a discharge test of this cylindrical AZO sputtering target, no crack was observed even at a usage rate of 80%.
１０：円筒形支持基材
２０：円筒形状のセラミックス焼結体からなるターゲット材
３０：第１の下地層
４０：第２の下地層
５０：クリアランス
10: Cylindrical support base material 20:
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