JP5672537B2 - Cylindrical sputtering target and manufacturing method thereof - Google Patents
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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、スパッタリングターゲット材の接合面に電解還元により金属層から成る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 to the production thereof, and relates to a sputtering target in which a base layer made of a metal layer is provided on the joint surface of a sputtering target material by electrolytic reduction.
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、例えば、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, for example, 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できない。一方、支持基材は、材料が金属であっても接合時には接合材の融点以上に加熱されるため表面酸化が進行し、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。 Originally, ceramics and metals are difficult to join, and cannot be joined simply by melting a bonding material such as a low melting point solder and bringing it into contact with the ceramic to cool and solidify. On the other hand, the supporting base material is heated to the melting point or higher of the bonding material at the time of bonding even if the material is metal, so that the surface oxidation proceeds and the wettability with the molten bonding material becomes worse, and the bonding material after cooling and solidification The adhesive strength of is reduced.
こ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酸でスパッタリングターゲットの表面を処理した後、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 this problem, after the surface of the sputtering target is previously treated with a metal such as aluminum or aluminum alloy or an acid, 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へ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、低融点半田との濡れ性が低下するため、これらの金属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 with the low melting point solder is lowered, so that sufficient bonding strength cannot be obtained even if an underlayer is formed of 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、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、ターゲット材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）。 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 of Cu, a method has been proposed in which a part of a solder material to be bonded to both surfaces of a target material and a supporting substrate is soldered by an ultrasonic metallizing method to firmly bond the target material and the supporting substrate. (See Patent Document 3).
しかしこの方法は、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周側半径が小さい場合、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において、接合面に超音波メタライジングの超音波振動子が有効に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。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。 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 peripheral radius of the cylindrical target material is small or the central axis of the cylindrical target material is used. When the length in the direction is long, a portion where the ultrasonic metallizing ultrasonic transducer cannot be effectively brought into contact with the bonding surface is generated, and it is difficult to perform the ultrasonic metalizing process all over the bonding surface. 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、円筒形のセラミックスのターゲット材の接合面を電解還元することによって金属層を形成させ、これを下地層とすることによって、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強度が得られ、スパッタリング中の熱の影響で剥離や割れのない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 layer by electrolytic reduction of the joint surface of a cylindrical ceramic target material, and by using this as a base layer, cooling can be performed without pressing the joint during joining. It is an object of the present invention to provide a sputtering target and a method for manufacturing the sputtering target, which can obtain a sufficient bonding rate and strength only by solidification and are free from peeling and cracking due to 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、以下のことを見出し、本発明を完成するに至った。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周面に円筒形セラミックスターゲット材を接合してなる円筒形スパッタリングターゲットにおいて、ターゲット材の内周面にターゲット材の還元金属から成る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）下地層の上に１層以上の金属層を有する、（１）に記載の円筒形スパッタリングターゲット。
（３）金属層の１層がスズ（Ｓｎ）から成る、（２）に記載の円筒形スパッタリングターゲット。
（４）金属層の厚みが１０〜３００μｍである、（２）または（３）に記載のスパッタリングターゲット。
（５）インジウム合金半田により接合してなる、（１）から（４）いずれかに記載の円筒形スパッタリングターゲット。
（６）円筒形セラミックスターゲット材の内周面を電界還元して、ターゲット材の還元金属から成る下地層を形成し、次いで円筒形支持基材の外周面に円筒形セラミックスターゲット材を接合することを特徴とする、（１）に記載の円筒形スパッタリングターゲットの製造方法。
As a result of intensive studies in order to solve the above problems, the present inventors have found the following and completed the present invention. That is, the present invention is as follows.
(1) A cylindrical sputtering target formed by bonding a cylindrical ceramic target material to the outer peripheral surface of a cylindrical support base material, and having an underlayer made of a reduced metal of the target material on the inner peripheral surface of the target material A cylindrical sputtering target.
(2) The cylindrical sputtering target according to (1), having one or more metal layers on the underlayer.
(3) The cylindrical sputtering target according to (2), wherein one metal layer is made of tin (Sn).
(4) The sputtering target according to (2) or (3), wherein the metal layer has a thickness of 10 to 300 μm.
(5) The cylindrical sputtering target according to any one of (1) to (4), which is joined by indium alloy solder.
(6) Electric field reduction is performed on the inner peripheral surface of the cylindrical ceramic target material to form a base layer made of the reduced metal of the target material, and then the cylindrical ceramic target material is joined to the outer peripheral surface of the cylindrical support base material. The manufacturing method of the cylindrical sputtering target as described in (1) characterized by these.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明おける円筒形のセラミックスのターゲット材は、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。 The target material of the cylindrical ceramic in the present invention is not particularly limited. For example, ITO (Indium Tin Oxide), ZnO (Zinc Oxide), AZO, which are optical thin film materials used for transparent conductive films and the like. (Aluminum Zinc Oxide), IZO (Indium Zinc Oxide), Ta 2 O 5 , Nb 2 O 5 , TiO 2 and the like can be given.
支持基材としては、ステンレス、チタン、チタン合金、銅、銅合金などである。支持基材は濡れ性を改善するため、接合する前に十分に洗浄しておくおことが望ましい。 Examples of the supporting substrate include stainless steel, titanium, titanium alloy, copper, and copper alloy. In order to improve the wettability, it is desirable that the support substrate be thoroughly washed before bonding.
接合には、例えば低融点半田が用いられ、より好ましくは鉛フリーのインジウム（融点１５７℃）や錫−インジウム合金（１１７℃）が用いられる。 For the bonding, for example, low melting point solder is used, and lead-free indium (melting point 157 ° C.) or tin-indium alloy (117 ° C.) is more preferably used.
ターゲット材の内周面にターゲット材の還元金属から成る下地層を形成する方法には特に限定はないが、例えば、ターゲット材の内周面を電界還元する方法があげられる。このとき、ターゲット材の内周面は、良好な金属面を得る為に予め洗浄しておくことが好ましい。電解還元して金属層を形成するに際し、還元剤としては水酸化ナトリウムなどの水溶液が望ましく、電流密度は低いと還元に時間を要し、余り高いと時間の制御が難しくなるので０．５〜５Ａ／ｄｍ２が望ましく、より好ましくは２Ａ／ｄｍ２である。また、電解時間は電流密度、還元剤の濃度にもよるが生産性を考慮すると概ね１〜１０分程度が好ましい。 There is no particular limitation on the method of forming the base layer made of the reduced metal of the target material on the inner peripheral surface of the target material. At this time, the inner peripheral surface of the target material is preferably washed in advance in order to obtain a good metal surface. When forming a metal layer by electrolytic reduction, an aqueous solution such as sodium hydroxide is desirable as the reducing agent. If the current density is low, it takes time for reduction, and if it is too high, it becomes difficult to control the time. 5 A / dm 2 is desirable, more preferably 2 A / dm 2 . The electrolysis time is preferably about 1 to 10 minutes in consideration of productivity although it depends on the current density and the concentration of the reducing agent.
この方法により、例えばセラミックスターゲット材としてＩＴＯを用いた場合、ターゲット材内周面の最表面は還元されてインジウム−スズ合金層が形成されているものと推定される。 By this method, for example, when ITO is used as the ceramic target material, it is presumed that the outermost surface of the inner peripheral surface of the target material is reduced to form an indium-tin alloy layer.
ターゲット材の内周面を電解還元してターゲット材の還元金属から成る下地層を形成させ、ターゲット材と支持基材とを接合する。またターゲット材の下地層の上に、スパッタ法、蒸着法、メッキ法などで１層以上の金属層を形成してから、支持基材を接合してもよい。 The inner peripheral surface of the target material is electrolytically reduced to form a base layer made of the reduced metal of the target material, and the target material and the support base material are joined. Further, after forming one or more metal layers on the base layer of the target material by sputtering, vapor deposition, plating, or the like, the supporting base material may be bonded.
この金属層は接合層とは異なるものであり、ニッケル（Ｎｉ）、クロム（Ｃｒ）、銅（Ｃｕ）、スズ（Ｓｎ）などが好ましい。金属層の厚みとしては余り薄いと効果がなく、厚過ぎると形成に時間がかかるので、１０〜３００μｍが望ましい。 This metal layer is different from the bonding layer, and nickel (Ni), chromium (Cr), copper (Cu), tin (Sn) and the like are preferable. If the thickness of the metal layer is too thin, there is no effect, and if it is too thick, it takes time to form, so 10 to 300 μm is desirable.
円筒型ターゲット材を円筒形支持基材に接合するには、円筒形支持基材の外側に、内周面に金属下地層を形成した円筒形ターゲット材を配置し、接合すればよい。接合方法としてはターゲット材を加熱し、円筒形ターゲット材の内周面と円筒形基材の外周面の間に形成される空隙に溶融させた半田を注入し、冷却固化させればよい。このとき、両者の中心軸が一致するように接合してもよいし、また複数のターゲット材を接合する場合には、隣接するターゲット材の表面の段差ができるだけ小さくなるように接合してもよい。 In order to join the cylindrical target material to the cylindrical support base material, a cylindrical target material having a metal base layer formed on the inner peripheral surface may be disposed outside the cylindrical support base material and joined. As a joining method, the target material is heated, and molten solder is injected into a gap formed between the inner peripheral surface of the cylindrical target material and the outer peripheral surface of the cylindrical base material, and then cooled and solidified. At this time, they may be joined so that their central axes coincide with each other, and when joining a plurality of target materials, they may be joined so that the level difference between the surfaces of the adjacent target materials is as small as possible. .
本発明によれば、接合率と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、スパッタ時の剥離や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 peeling and cracking during sputtering is significantly suppressed.
以下、本発明の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。
Examples of the present invention will be described below, but the present invention is not limited thereto.
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個用意した。円筒形ＩＴＯターゲット材およびＴｉ製円筒基材を十分に洗浄した。円筒形ＩＴＯターゲット材の電解還元は水酸化ナトリム１０％水溶液を還元剤とし、ターゲット材を陰極、カーボン電極を陽極として繋ぎ、２５℃、電流密度２Ａ／ｄｍ２の条件で５分間行い、ターゲット材内周面に金属下地層を形成した。また、Ｔｉ製円筒基材については、外周面を超音波メタライジング処理によってＩｎ半田を下塗りした。
Example 1
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) were prepared. . The cylindrical ITO target material and the Ti cylindrical substrate were thoroughly cleaned. Electrolytic reduction of the cylindrical ITO target material is carried out for 5 minutes under the conditions of 25 ° C. and current density of 2 A / dm 2 with a 10% aqueous solution of sodium hydroxide as the reducing agent, the target material as the cathode and the carbon electrode as the anode. A metal underlayer was formed on the inner peripheral surface. In addition, for the Ti cylindrical substrate, the outer peripheral surface was primed with In solder by ultrasonic metallizing treatment.
Ｔｉ製円筒形基材を垂直に立て、その外側に円筒形ＩＴＯターゲット材を配置し、両者の中心軸が一致するように組み合わせ、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空隙に溶融させた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放電試験を行なった結果、割れは認められなかった。 A cylindrical cylindrical substrate made of Ti was set up vertically, and a cylindrical ITO target material was arranged on the outside thereof, and they were combined and fixed so that their central axes coincided. This assembly is heated to 180 ° C. using a ribbon heater, and molten In solder is poured into a gap formed between the inner peripheral surface of the cylindrical ITO target material and the outer peripheral surface of the Ti cylindrical base material, Thereafter, it was cooled and solidified. As a result of conducting a discharge test on the cylindrical ITO sputtering target produced by this method, no cracks were observed.
（実施例２）
実施例１において、円筒形ＩＴＯターゲット材の金属下地層の上に、Ｓｎをスパッタ法で１０μｍ形成した以外は、実施例１と同様に作製した。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放電試験を行なった結果、割れは認められなかった。
(Example 2)
In Example 1, it produced similarly to Example 1 except having formed 10 micrometers of Sn by the sputtering method on the metal base layer of the cylindrical ITO target material. As a result of conducting a discharge test on the cylindrical ITO sputtering target produced by this method, no cracks were observed.
（実施例３）
実施例１において、円筒形ＩＴＯターゲット材の金属下地層の上に、Ｎｉ層を５μｍ、次いでＳｎ層を１５μｍの厚みに電気めっきで形成した以外は、実施例１と同様に作製した。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放電試験を行なった結果、割れは認められなかった。
Example 3
In Example 1, it produced similarly to Example 1 except having formed the Ni layer into the thickness of 5 micrometers on the metal base layer of the cylindrical ITO target material, and then forming the Sn layer into the thickness of 15 micrometers by electroplating. As a result of conducting a discharge test on the cylindrical ITO sputtering target produced by this method, no cracks were observed.
（比較例１）
実施例１において、円筒形ＩＴＯターゲット材の内周面を電解還元することなく、直接Ｉｎ半田を流し込み作製したところ、ターゲット材内周面の濡れ性が悪く、基材と全く接合できなかった。
(Comparative Example 1)
In Example 1, the inner peripheral surface of the cylindrical ITO target material was directly poured into In solder without electrolytic reduction. As a result, the wettability of the inner peripheral surface of the target material was poor and the substrate could not be joined at all.
（比較例２）
実施例１において、電界還元を行わずに、円筒形ＩＴＯターゲット材内周面についても超音波メタライジング処理によりＩｎ半田を下塗りし、それ以外は実施例１と同様にしてＩｎ半田の流し込みを行った。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ったところ、ターゲット表面の一部に割れが観察された。
(Comparative Example 2)
In Example 1, In solder was primed by ultrasonic metallizing treatment on the inner peripheral surface of the cylindrical ITO target material without performing electric field reduction, and In solder was poured in the same manner as in Example 1 except that. It was. When a discharge test was performed on the cylindrical ITO sputtering target, cracks were observed on a part of the target surface.
１１：円筒形支持基材
２１：円筒形セラミックスターゲット材
３１：電解還元金属下地層
４１：金属層（１）
５１：金属層（２）
６１：空隙
11: Cylindrical support base material 21: Cylindrical ceramic target material 31: Electrolytic reduction metal base layer 41: Metal layer (1)
51: Metal layer (2)
61: Air gap
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| KR101502513B1 (en) * | 2013-06-20 | 2015-03-16 | (주)태광테크 | Sputtering target assembly and method of manufacturing the same |
| JP5937731B2 (en) * | 2014-10-07 | 2016-06-22 | Ｊｘ金属株式会社 | Sputtering target |
| JP5944024B1 (en) * | 2015-02-27 | 2016-07-05 | Ｊｘ金属株式会社 | Rotary sputtering target and manufacturing method thereof |
| KR102206547B1 (en) | 2015-03-18 | 2021-01-22 | 바이탈 씬 필름 머티리얼즈 (광동) 캄파니 리미티드 | Method of forming a rotating sputtering target |
| JP6756283B2 (en) * | 2016-04-12 | 2020-09-16 | 三菱マテリアル株式会社 | Cylindrical sputtering target |
| JP6658937B2 (en) | 2018-03-15 | 2020-03-04 | 三菱マテリアル株式会社 | Cylindrical sputtering target, sputtering target material, and method for manufacturing cylindrical sputtering target |
| WO2019176677A1 (en) * | 2018-03-15 | 2019-09-19 | 三菱マテリアル株式会社 | Cylindrical sputtering target, sputtering target material, and method for manufacturing cylindrical sputtering target |
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