JP2020158806A - Method for manufacturing cylindrical sputtering target - Google Patents

Method for manufacturing cylindrical sputtering target Download PDF

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JP2020158806A
JP2020158806A JP2019057175A JP2019057175A JP2020158806A JP 2020158806 A JP2020158806 A JP 2020158806A JP 2019057175 A JP2019057175 A JP 2019057175A JP 2019057175 A JP2019057175 A JP 2019057175A JP 2020158806 A JP2020158806 A JP 2020158806A
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base treatment
cylindrical
backing tube
target material
treatment layer
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JP7120111B2 (en
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晋 岡野
Susumu Okano
晋 岡野
健志 大友
Kenji Otomo
健志 大友
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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Priority to JP2019057175A priority Critical patent/JP7120111B2/en
Priority to CN202080014649.2A priority patent/CN113423861A/en
Priority to PCT/JP2020/010271 priority patent/WO2020195787A1/en
Priority to KR1020217022973A priority patent/KR20210143161A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/34Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411Constructional aspects of the reactor
    • H01J37/3414Targets
    • H01J37/3423Shape
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes
    • H01J37/34Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3491Manufacturing of targets

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

To provide a method for manufacturing a cylindrical sputtering target, capable of suppressing the influence of an oxide film to prevent poor bonding and improve a yield.SOLUTION: A method for manufacturing a cylindrical sputtering target comprises: a base treatment step of applying a base treatment bonding material to a member on at least one of the inner peripheral surface of the cylindrical target material and the outer peripheral surface of a cylindrical backing tube to form a first surface treatment layer having a thickness of 0.1 mm or more and 0.8 mm or less; and the bonding step of inserting the cylindrical backing tube into the cylindrical target material to fill a space between the cylindrical target material and the cylindrical backing tube with a molten bonding material for filling. The base treatment step includes scratching at least the surface of the first base treatment layer, and the bonding step includes heating the first surface treatment layer until at least the surface of the first surface treatment layer is in a semi-molten state to fill with the bonding material for filling.SELECTED DRAWING: Figure 3

Description

本発明は、スパッタリング装置に用いられる円筒型スパッタリングターゲットの製造方法に関する。 The present invention relates to a method for manufacturing a cylindrical sputtering target used in a sputtering apparatus.

円筒型スパッタリングターゲットを回転させながらスパッタを行うスパッタリング装置が知られている。この種のスパッタリング装置に用いられる円筒型スパッタリングターゲットは、特許文献1に示されるように、円筒型バッキングチューブの外周面に円筒型のターゲット材の内周面が接合されている。
この接合においては、接合面となる円筒型バッキングチューブの外周面及び円筒型ターゲット材の内周面に接合材と同じまたは類似の下地処理接合材を塗布して下地処理被膜を形成し、その後、ターゲット材に円筒型バッキングチューブを挿入して、両者の間に接合部のための隙間を設けるとともに、ターゲット材と円筒型バッキングチューブとを加熱した状態としておき、その隙間に溶融状態の接合材を供給して隙間を充填する接合方法が知られている。接合材としてはインジウム(In)を用いることが多い。
A sputtering apparatus that performs sputtering while rotating a cylindrical sputtering target is known. In the cylindrical sputtering target used in this type of sputtering apparatus, as shown in Patent Document 1, the inner peripheral surface of the cylindrical target material is joined to the outer peripheral surface of the cylindrical backing tube.
In this joining, a base-treated joint material similar to or similar to the joint material is applied to the outer peripheral surface of the cylindrical backing tube to be the joint surface and the inner peripheral surface of the cylindrical target material to form a base-treated coating, and then a base-treated coating is formed. A cylindrical backing tube is inserted into the target material to provide a gap for the joint between the two, and the target material and the cylindrical backing tube are kept in a heated state, and the molten joint material is placed in the gap. A joining method of supplying and filling a gap is known. Indium (In) is often used as the bonding material.

この場合、ターゲット材及び円筒型バッキングチューブの下地処理接合材の表面は、下地処理後の冷却及び両者の隙間へ接合材を充填するための接合前の再加熱等を経て、表面が酸化し、酸化膜が形成される。
この下地処理接合材の表面の酸化膜の形成により、充填する接合材と下地処理接合材との接触が阻害され、接合不良が生じやすい。接合不良となった円筒型スパッタリングターゲットは、全体を加熱して接合材を溶融させた後、ターゲット材をバッキングチューブから取り外し、再度、接合をやり直す作業が必要となる。一方、スパッタされる基板の大型化に伴ってターゲット材は長尺化しており、生産効率の向上の観点から、スパッタ成膜時のパワー密度を上げる傾向にあり、接合強度の向上も望まれている。
In this case, the surface of the base treatment bonding material of the target material and the cylindrical backing tube is oxidized after cooling after the base treatment and reheating before joining to fill the gap between the two. An oxide film is formed.
The formation of an oxide film on the surface of the surface-treated bonding material hinders the contact between the bonding material to be filled and the surface-treated bonding material, and a bonding failure is likely to occur. For a cylindrical sputtering target with poor bonding, it is necessary to heat the entire surface to melt the bonding material, remove the target material from the backing tube, and perform the bonding again. On the other hand, as the size of the substrate to be sputtered increases, the target material becomes longer, and from the viewpoint of improving production efficiency, there is a tendency to increase the power density during sputter film formation, and improvement of bonding strength is also desired. There is.

この対策として、例えば特許文献2においては、円筒型ターゲット材と円筒型バッキングチューブとの隙間に溶融状態の接合材を充填した後に、鋼線や鋼板を差し込んでこれらの間に充填された接合材を撹拌し、充填した接合材と下地処理接合材とを一体化することが開示されている。
特許文献3では、円筒型ターゲット材と円筒型バッキングチューブとの空間に接合材である半田材よりも比重が軽い粉体物質を入れておき、次いで、溶融半田を空間に注入して粉体物質を半田材の液面に浮かせた状態で、粉体物質を振動させながら注入することで半田材を物理的に撹拌している。
特許文献4では、円筒型ターゲット材と円筒型バッキングチューブとの隙間に固体の接合材を充填し、この接合材を加熱して溶融することにより、下地処理面と大気中との接触面積を減らし、ターゲット材と円筒型バッキングチューブの下地処理面の酸化膜の発生を抑制している。
As a countermeasure for this, for example, in Patent Document 2, after filling the gap between the cylindrical target material and the cylindrical backing tube with a bonded material in a molten state, a steel wire or a steel plate is inserted and the bonding material filled between them is inserted. Is disclosed to stir and integrate the filled bonding material and the base-treated bonding material.
In Patent Document 3, a powder substance having a lighter specific gravity than the solder material as a bonding material is put in the space between the cylindrical target material and the cylindrical backing tube, and then molten solder is injected into the space to form the powder substance. Is floated on the liquid surface of the solder material, and the powder material is injected while vibrating to physically stir the solder material.
In Patent Document 4, a solid bonding material is filled in the gap between the cylindrical target material and the cylindrical backing tube, and the bonding material is heated and melted to reduce the contact area between the surface to be treated and the atmosphere. , The generation of oxide film on the base treatment surface of the target material and the cylindrical backing tube is suppressed.

特開2014−37619号公報Japanese Unexamined Patent Publication No. 2014-37619 特許第6341146号公報Japanese Patent No. 6341146 特開2012−177156号公報Japanese Unexamined Patent Publication No. 2012-177156 特開2018−111868号公報Japanese Unexamined Patent Publication No. 2018-11168

しかしながら、特許文献2の場合には、接合材を撹拌するための作業に手間がかかる。しかも、塗布された接合材の酸化膜を全面に亘って除去するために、ターゲット材とバッキングチューブとの隙間全体を撹拌する必要があり、撹拌が不十分な部分では接合不良が発生する可能性が高い。
特許文献3についても同様であり、粉体物質を振動させるための振動源が別の装置として必要になり、粉体物質の振動による半田材の撹拌が十分でない場合には、接合不良につながることがある。
特許文献4の製造方法においては、接合時前に、固体の接合材の外周面やターゲット材及びバッキングチューブの内外周面に酸化膜が付着していると、接合不良の回避が難しくなる。そのため、ターゲット材をバッキングチューブ内に配置する前に、接合材の表面や、ターゲット材、バッキングチューブの内外周面に形成された酸化膜を除去する必要が生じる。
However, in the case of Patent Document 2, it takes time and effort to stir the bonding material. Moreover, in order to remove the oxide film of the applied bonding material over the entire surface, it is necessary to stir the entire gap between the target material and the backing tube, and bonding failure may occur in a portion where the stirring is insufficient. Is high.
The same applies to Patent Document 3, and a vibration source for vibrating the powder material is required as another device, and if the solder material is not sufficiently agitated by the vibration of the powder material, it may lead to poor bonding. There is.
In the manufacturing method of Patent Document 4, if an oxide film adheres to the outer peripheral surface of the solid bonding material and the inner and outer peripheral surfaces of the target material and the backing tube before the bonding, it becomes difficult to avoid the bonding failure. Therefore, before arranging the target material in the backing tube, it is necessary to remove the oxide film formed on the surface of the bonding material, the target material, and the inner and outer peripheral surfaces of the backing tube.

本発明は、このような事情に鑑み、酸化膜の影響を抑制して接合不良の発生を防止し、歩留まりを向上させることを目的としている。 In view of such circumstances, it is an object of the present invention to suppress the influence of the oxide film, prevent the occurrence of bonding defects, and improve the yield.

本発明の円筒型スパッタリングターゲットの製造方法は、円筒型ターゲット材の内周面と該円筒型ターゲット材の内側に挿入した円筒型バッキングチューブの外周面との隙間を接合材で充填して接合する円筒型スパッタリングターゲットの製造方法であって、前記円筒型ターゲット材の内周面と前記円筒側バッキングチューブの外周面との少なくとも何れか一方の部材に下地処理接合材を塗布して0.1mm以上0.8mm以下の第1下地処理層を形成する下地処理工程と、下地処理工程の後、前記円筒型ターゲット材内に前記円筒型バッキングチューブを挿入し、該円筒型ターゲット材と前記円筒型バッキングチューブとの隙間に溶融状態の充填用接合材を充填する接合工程とを有し、前記下地処理工程では、前記第1下地処理層の少なくとも表面に傷を付けておき、前記接合工程では、前記第1下地処理層の少なくとも表面が半溶融状態となるまで加熱した後、前記充填用接合材を充填する。 In the method for manufacturing a cylindrical sputtering target of the present invention, a gap between the inner peripheral surface of the cylindrical target material and the outer peripheral surface of the cylindrical backing tube inserted inside the cylindrical target material is filled with a joining material and joined. A method for manufacturing a cylindrical sputtering target, in which a base treatment bonding material is applied to at least one of the inner peripheral surface of the cylindrical target material and the outer peripheral surface of the cylindrical backing tube to 0.1 mm or more. After the base treatment step of forming the first base treatment layer of 0.8 mm or less and the base treatment step, the cylindrical backing tube is inserted into the cylindrical target material, and the cylindrical target material and the cylindrical backing are inserted. It has a joining step of filling a gap between the tube and a filling bonding material in a molten state, and in the base treatment step, at least the surface of the first base treatment layer is scratched, and in the joining step, the said After heating until at least the surface of the first base treatment layer is in a semi-molten state, the filling bonding material is filled.

下地処理工程で形成される第1下地処理層は、下地処理接合材塗布後の冷却中及び接合工程に際しての再加熱中に表面が酸化され、酸化膜を形成する場合がある。これに対して、第1下地処理層を厚く形成しておいたので、接合工程時に第1下地処理層の表面を少なくとも半溶融状態とすることにより、その表面が垂れ下がった状態となる。このとき、予め第1下地処理層表面に傷を付けておいたことにより、表面に酸化膜が形成されていたとしても、表面部分が垂れ下がる際に、傷の部分で酸化膜が破壊されながら垂れ下がって分断される。この表面が垂れ下がった状態で溶融状態の充填用接合材を充填することにより、酸化膜が分断された第1下地処理層の表面部分に溶融状態の充填用接合材が入り込みながら、これらが混合する。また、酸化膜の一部は充填用接合材の充填により、隙間から押し流される。隙間内に酸化膜の一部が残留したとしても、分断されているので、下地処理接合材と新たな充填用接合材とが一体化し、強固な接合層を形成することができる。
なお、第1下地処理層は全周にわたって垂れ下がり状態となるので、酸化膜を全周にわたって分断させることができる。
The surface of the first base treatment layer formed in the base treatment step may be oxidized during cooling after application of the base treatment bonding material and during reheating during the bonding step to form an oxide film. On the other hand, since the first base treatment layer is formed thick, the surface of the first base treatment layer is at least semi-molten during the joining step, so that the surface is in a hanging state. At this time, even if the oxide film is formed on the surface by scratching the surface of the first base treatment layer in advance, when the surface portion hangs down, the oxide film hangs down while being destroyed at the scratched portion. Is divided. By filling the filled state bonding material in a molten state with the surface hanging down, the molten state filling bonding material is mixed while entering the surface portion of the first base treatment layer in which the oxide film is divided. .. In addition, a part of the oxide film is washed away from the gap by filling the filling bonding material. Even if a part of the oxide film remains in the gap, it is divided, so that the base treatment bonding material and the new filling bonding material can be integrated to form a strong bonding layer.
Since the first base treatment layer is in a hanging state over the entire circumference, the oxide film can be divided over the entire circumference.

この場合、第1下地処理層の厚さが0.1mm未満では、半溶融状態となっても垂れ下がりにくいため、酸化膜が破壊されにくい。第1下地処理層が厚さ0.8mmを超えると、下地処理工程に時間がかかるとともに、自重により垂れ下がったときに、肉厚が大きくなり過ぎて、円筒型ターゲット材に円筒型バッキングチューブを挿入することができなくなるおそれがある。 In this case, if the thickness of the first base treatment layer is less than 0.1 mm, the oxide film is less likely to be broken because it is less likely to hang down even in a semi-molten state. If the thickness of the first base treatment layer exceeds 0.8 mm, the base treatment process takes time, and when it hangs down due to its own weight, the wall thickness becomes too large, and a cylindrical backing tube is inserted into the cylindrical target material. It may not be possible to do so.

円筒型スパッタリングターゲットの製造方法の一つの実施態様として、前記下地処理工程では、前記第1下地処理層が形成された前記一方の部材とは反対側の他方の部材に、前記第1下地処理層よりも薄肉の第2下地処理層を形成しておき、前記第1下地処理層が形成された前記一方の部材に、前記隙間内に径方向に突出して配置可能な掻き取り板を周方向に沿って設けておき、前記接合工程において、前記掻き取り板により前記第2下地処理層の表面に形成された酸化膜の少なくとも一部を掻き取りながら前記円筒型ターゲット材内に前記円筒型バッキングチューブを挿入するとよい。 As one embodiment of the method for manufacturing a cylindrical sputtering target, in the base treatment step, the first base treatment layer is applied to the other member on the side opposite to the one member on which the first base treatment layer is formed. A second base treatment layer having a thickness thinner than that of the first base treatment layer is formed, and a scraping plate that can be arranged so as to project radially in the gap is provided in the circumferential direction on the one member on which the first base treatment layer is formed. In the joining step, the cylindrical backing tube is provided in the cylindrical target material while scraping at least a part of the oxide film formed on the surface of the second surface treatment layer by the scraping plate. Should be inserted.

この製造方法では、厚肉の第1下地処理層とは別に、薄肉の第2下地処理層に対して掻き取り板によって酸化膜の少なくとも一部を除去するようにしているので、新たに充填される接合材と第1下地処理層及び第2下地処理接合材とをより強固に接合できる。しかも、円筒型ターゲット材に円筒型バッキングチューブを挿入する操作によって酸化膜の一部を除去できるので、作業が容易である。 In this manufacturing method, in addition to the thick first base treatment layer, at least a part of the oxide film is removed from the thin second base treatment layer by a scraping plate, so that the thin-walled second base treatment layer is newly filled. The bonding material and the first surface treatment layer and the second surface treatment bonding material can be bonded more firmly. Moreover, since a part of the oxide film can be removed by inserting the cylindrical backing tube into the cylindrical target material, the work is easy.

本発明によれば、酸化膜の影響を抑制して接合不良の発生を防止し、歩留まりを向上させることができる。 According to the present invention, it is possible to suppress the influence of the oxide film, prevent the occurrence of bonding defects, and improve the yield.

第1実施形態の製造方法で製造された円筒型スパッタリングターゲットを示す縦断面図である。It is a vertical sectional view which shows the cylindrical sputtering target manufactured by the manufacturing method of 1st Embodiment. 円筒型スパッタリングターゲットの製造方法を説明するフローチャートである。It is a flowchart explaining the manufacturing method of a cylindrical sputtering target. 下地処理層を形成した円筒型バッキングチューブの縦断面図である。It is a vertical cross-sectional view of the cylindrical backing tube which formed the base treatment layer. 下地処理層を形成した円筒型ターゲット材の縦断面図である。It is a vertical sectional view of the cylindrical target material which formed the base treatment layer. 第1実施形態の製造方法において、円筒型ターゲット材内に円筒型バッキングチューブを挿入して加熱する前の状態を示す縦断面図である。FIG. 5 is a vertical cross-sectional view showing a state before the cylindrical backing tube is inserted into the cylindrical target material and heated in the manufacturing method of the first embodiment. 図5に示す状態から再加熱した状態を示す縦断面図である。It is a vertical cross-sectional view which shows the state which reheated from the state shown in FIG. 図6に示す状態から、円筒型バッキングチューブを降下させた状態を示す縦断面図である。It is a vertical cross-sectional view which shows the state which lowered the cylindrical backing tube from the state shown in FIG. 第2実施形態の製造方法において、円筒型ターゲット材内に円筒型バッキングチューブを挿入する前の状態を示す縦断面図である。It is a vertical cross-sectional view which shows the state before inserting the cylindrical backing tube into the cylindrical target material in the manufacturing method of 2nd Embodiment. 掻き取り板を示す平面図である。It is a top view which shows the scraping plate. 第2実施形態の製造方法で製造された円筒型スパッタリングターゲットの示す縦断面図である。It is a vertical cross-sectional view which shows the cylindrical sputtering target manufactured by the manufacturing method of 2nd Embodiment. 第3実施形態の製造方法において、円筒型ターゲット材内に円筒型バッキングチューブを挿入する前の状態を示す縦断面図である。It is a vertical cross-sectional view which shows the state before inserting the cylindrical backing tube into the cylindrical target material in the manufacturing method of 3rd Embodiment.

以下、本発明に係る円筒型スパッタリングターゲットの製造方法の実施形態を図面を参照しながら説明する。
まず、第1実施形態について説明する。
円筒型スパッタリングターゲット1は、例えば図1に示すように、円筒型ターゲット材(以下、ターゲット材と称す)2内に円筒型バッキングチューブ(以下、バッキングチューブと称す)3が挿入され、これらターゲット材2の内周面と円筒型バッキングチューブ3の外周面との間が接合部4を介して接合される。この場合、ターゲット材2とバッキングチューブ3とは、中心軸が一致した状態で配置される。
Hereinafter, embodiments of a method for manufacturing a cylindrical sputtering target according to the present invention will be described with reference to the drawings.
First, the first embodiment will be described.
In the cylindrical sputtering target 1, for example, as shown in FIG. 1, a cylindrical backing tube (hereinafter referred to as a backing tube) 3 is inserted into a cylindrical target material (hereinafter referred to as a target material) 2, and these target materials are inserted. The inner peripheral surface of 2 and the outer peripheral surface of the cylindrical backing tube 3 are joined via the joint portion 4. In this case, the target material 2 and the backing tube 3 are arranged so that their central axes coincide with each other.

ターゲット材2は長尺状であることから、一般に長さ方向に分割された複数の分割ターゲット材2aを接続することで構成される。 Since the target material 2 has a long shape, it is generally configured by connecting a plurality of divided target materials 2a divided in the length direction.

ターゲット材2及びバッキングチューブ3の材質や寸法は特に限定されないが、例えば、ターゲット材2は、銅、銀等の金属、Al,Znの酸化物焼結体であるAZO等のセラミックスなどからなる内径120mm〜140mmの筒状部材を用いることができ、バッキングチューブ3は、チタン、ステンレス鋼、または銅あるいは銅合金からなる外径119mm〜139mm、長さ0.5m〜4mの筒状部材を用いることができる。この場合、ターゲット材2は、長さ30cm程度の短尺の分割ターゲット材2aを複数連結した状態で円筒型バッキングチューブ3の外周に配置される。ターゲット材2内にバッキングチューブ3を挿入した状態で、ターゲット材2の内周面とバッキングチューブ3の外周面との間には半径方向に0.5mm〜1mmの隙間が形成され、この隙間には、隙間保持のための図示しない棒状スペーサ(図示略)が挿入されていてもよく、この場合、この棒状スペーサとともにターゲット材2及びバッキングチューブ3とが接合部4により一体化される。 The material and dimensions of the target material 2 and the backing tube 3 are not particularly limited. For example, the target material 2 has an inner diameter made of a metal such as copper or silver, or a ceramic such as AZO which is an oxide sintered body of Al or Zn. A tubular member of 120 mm to 140 mm can be used, and the backing tube 3 uses a tubular member having an outer diameter of 119 mm to 139 mm and a length of 0.5 m to 4 m made of titanium, stainless steel, or copper or a copper alloy. Can be done. In this case, the target material 2 is arranged on the outer circumference of the cylindrical backing tube 3 in a state where a plurality of short divided target materials 2a having a length of about 30 cm are connected. With the backing tube 3 inserted in the target material 2, a gap of 0.5 mm to 1 mm is formed in the radial direction between the inner peripheral surface of the target material 2 and the outer peripheral surface of the backing tube 3, and a gap of 0.5 mm to 1 mm is formed in this gap. A rod-shaped spacer (not shown) for holding a gap may be inserted, and in this case, the target material 2 and the backing tube 3 are integrated with the rod-shaped spacer by the joint portion 4.

接合部4は、例えばインジウム含有量が60質量%以上のインジウム合金(例えばIn−Sn合金、In−Bi合金、In−Zn合金)又は純インジウム、錫含有量が60質量%以上の錫合金又は純錫等が用いられる。接合部4は、ターゲット材2、バッキングチューブ3に塗布される下地処理接合材と、これらの隙間に充填される充填用接合材とからなり、これらが一体化して固化することにより設けられる。 The joint 4 is, for example, an indium alloy having an indium content of 60% by mass or more (for example, In—Sn alloy, In—Bi alloy, In—Zn alloy) or pure indium, a tin alloy having a tin content of 60% by mass or more, or a tin alloy. Pure tin or the like is used. The joint portion 4 is composed of a base-treated joint material applied to the target material 2 and the backing tube 3 and a filling joint material filled in the gaps between them, and is provided by integrating and solidifying these.

<円筒型スパッタリングターゲットの製造方法>
この円筒型スパッタリングターゲット1を製造する場合、円筒型バッキングチューブ1の外周面とターゲット材2の内周面とを接合面とし、これら接合面間に設けた接合材で接合する。
図2に示すように、ターゲット材2及びバッキングチューブ3の加熱工程、ターゲット材2及びバッキングチューブ3に下地処理接合材を塗布する下地処理工程、塗布した下地処理接合材を冷却して固化する下地処理接合材冷却工程、固化した下地処理接合材を再加熱する再加熱工程、充填用接合材をターゲット材2とバッキングチューブ3との隙間に充填する接合材充填工程(接合工程)、充填された接合材を冷却して固化する接合材冷却工程を有している。以下、工程順に説明する。
<Manufacturing method of cylindrical sputtering target>
When the cylindrical sputtering target 1 is manufactured, the outer peripheral surface of the cylindrical backing tube 1 and the inner peripheral surface of the target material 2 are used as joint surfaces, and the joint material provided between these joint surfaces is used for joining.
As shown in FIG. 2, a heating step of the target material 2 and the backing tube 3, a base treatment step of applying the base treatment bonding material to the target material 2 and the backing tube 3, and a base treatment for cooling and solidifying the applied base treatment bonding material. Treatment joint material cooling step, reheating step of reheating the solidified base treatment joint material, joint material filling step (joining process) of filling the gap between the target material 2 and the backing tube 3 for filling joint material, filling. It has a joint material cooling process that cools and solidifies the joint material. Hereinafter, the steps will be described in order.

(加熱工程)
ターゲット材2及びバッキングチューブ3を加熱し、これらの接合面となるターゲット材2の内周面及びバッキングチューブ3の外周面を下地処理接合材の融点(又は液相線温度)以上の温度に加熱する。
(Heating process)
The target material 2 and the backing tube 3 are heated, and the inner peripheral surface of the target material 2 and the outer peripheral surface of the backing tube 3 which are the joint surfaces thereof are heated to a temperature equal to or higher than the melting point (or liquidus temperature) of the base-treated joint material. To do.

(下地処理工程)
加熱工程において、加熱状態とした各分割ターゲット材2aの内周面及びバッキングチューブ3の外周面に、それぞれ溶融状態の下地処理接合材を塗布して下地処理層41a,41bをそれぞれ形成する。この場合、ヒータを搭載した超音波はんだコテ(図示略)で超音波振動を加えながら下地処理接合材を塗り込むことにより、分割ターゲット材2aの内周面及びバッキングチューブ3の外周面における汚れや酸化膜の除去などが促進され、これらの表面に下地処理接合材をなじませることができる。
下地処理工程は、大気中で実施してもよいが、アルゴン、窒素等の不活性雰囲気にて実施すると、下地処理接合材によって形成される下地処理層41a,41bの表面の酸化を抑制することができるので、そのような雰囲気で実施することが望ましい。
(Base treatment process)
In the heating step, the base treatment bonding material in the molten state is applied to the inner peripheral surface of each of the divided target materials 2a in the heated state and the outer peripheral surface of the backing tube 3, respectively, to form the base treatment layers 41a and 41b, respectively. In this case, by applying the base treatment bonding material while applying ultrasonic vibration with an ultrasonic soldering iron (not shown) equipped with a heater, dirt on the inner peripheral surface of the divided target material 2a and the outer peripheral surface of the backing tube 3 can be prevented. Removal of the oxide film and the like are promoted, and the surface-treated bonding material can be applied to these surfaces.
The base treatment step may be carried out in the atmosphere, but when carried out in an inert atmosphere such as argon or nitrogen, oxidation of the surfaces of the base treatment layers 41a and 41b formed by the base treatment bonding material is suppressed. It is desirable to carry out in such an atmosphere.

(下地処理接合材冷却工程)
下地処理接合材冷却工程は、下地処理工程後に適宜の冷却手段により行う。これにより、下地処理接合材が固化し、図3及び図4に示すように、各分割ターゲット材2aの内周面及びバッキングチューブ3の外周面に下地処理層41a,41bが形成された状態になる。この下地処理層41a,41bの表面には酸化膜42が形成される。
この場合、下地処理層41a,41bは0.1mm以上0.8mm以下の厚さとなるように形成される。下地処理層41a,41bの厚さが0.1mm未満では、後述する再加熱工程で半溶融状態となっても垂れ下がりにくいため、酸化膜42が破壊されにくい。下地処理層41a,41bを厚さ0.8mmを超えると、下地処理工程に時間がかかるとともに、自重により垂れ下がったときに、下端部の厚さが大きくなり過ぎて、ターゲット材2にバッキングチューブ3を挿入することができなくなるおそれがある。
また、ターゲット材2の内周面とバッキングチューブ3の外周面との両方の下地処理層41a,41bの厚さの和は0.2mm以上0.9mm以下に設定するとよい。これらの厚さの和が0.2mm未満では、いずれかの下地処理層の厚さが0.1mm未満となり、0.9mmを超えると、ターゲット材2にバッキングチューブ3を挿入することができなくなるおそれがある。ターゲット材2の内周面とバッキングチューブ3の外周面との隙間は0.5mm以上1.0mm以下であり、この隙間に対して、下地処理層41a,41bの厚さの和は0.2以上0.9以下の比率とするとよい。例えば、隙間1.0mmの場合は下地処理層の厚さの和が0.2mm以上0.9mmが好ましく、隙間0.5mmの場合は下地処理層の厚さの和が0.10mm以上0.45mm以下が好ましい。すなわち、(下地処理層の厚さの和)/(隙間)=0.2〜0.9であることが好ましい。
(Base treatment joint material cooling process)
The base treatment joint material cooling step is performed by an appropriate cooling means after the base treatment step. As a result, the base treatment bonding material is solidified, and as shown in FIGS. 3 and 4, the base treatment layers 41a and 41b are formed on the inner peripheral surface of each divided target material 2a and the outer peripheral surface of the backing tube 3. Become. An oxide film 42 is formed on the surfaces of the base treatment layers 41a and 41b.
In this case, the base treatment layers 41a and 41b are formed so as to have a thickness of 0.1 mm or more and 0.8 mm or less. If the thickness of the base treatment layers 41a and 41b is less than 0.1 mm, the oxide film 42 is less likely to be destroyed because it is less likely to hang down even if it is in a semi-molten state in the reheating step described later. If the thicknesses of the base treatment layers 41a and 41b exceed 0.8 mm, the base treatment process takes time, and when the base treatment layers hang down due to their own weight, the thickness of the lower end portion becomes too large, and the backing tube 3 is attached to the target material 2. May not be able to be inserted.
Further, the sum of the thicknesses of the base treatment layers 41a and 41b of both the inner peripheral surface of the target material 2 and the outer peripheral surface of the backing tube 3 may be set to 0.2 mm or more and 0.9 mm or less. If the sum of these thicknesses is less than 0.2 mm, the thickness of any of the base treatment layers is less than 0.1 mm, and if it exceeds 0.9 mm, the backing tube 3 cannot be inserted into the target material 2. There is a risk. The gap between the inner peripheral surface of the target material 2 and the outer peripheral surface of the backing tube 3 is 0.5 mm or more and 1.0 mm or less, and the sum of the thicknesses of the base treatment layers 41a and 41b is 0.2 with respect to this gap. The ratio should be 0.9 or more and 0.9 or less. For example, when the gap is 1.0 mm, the sum of the thicknesses of the base treatment layers is preferably 0.2 mm or more and 0.9 mm, and when the gap is 0.5 mm, the sum of the thicknesses of the base treatment layers is 0.10 mm or more and 0. It is preferably 45 mm or less. That is, it is preferable that (sum of thicknesses of the base treatment layer) / (gap) = 0.2 to 0.9.

また、この下地処理層41a,41bが冷却固化された後に、表面の酸化膜42をカッター等によって削り取って除去しておく。この酸化膜42を削り取る作業により、下地処理層41a,41bの表面には傷が付いた状態となる。あるいは、酸化膜42を除去することなく少なくとも表面にカッター等により傷を付けておいてもよい。この傷は、この下地処理層41a,41bに形成される酸化膜42の厚さ以上の深さとなるようにし、酸化膜42の下の接合材にまで達するとよい。 Further, after the base treatment layers 41a and 41b are cooled and solidified, the oxide film 42 on the surface is scraped off by a cutter or the like. By the work of scraping off the oxide film 42, the surfaces of the base treatment layers 41a and 41b are in a scratched state. Alternatively, at least the surface may be scratched by a cutter or the like without removing the oxide film 42. It is preferable that the scratches have a depth equal to or greater than the thickness of the oxide film 42 formed on the base treatment layers 41a and 41b, and reach the bonding material under the oxide film 42.

(再加熱工程)
図5に示す載置台11に、下地処理層41aを形成した分割ターゲット材2aを垂直に連結した状態に載置する。載置台11の表面には、ターゲット材2の内径とほぼ同じ内径の凹部12が設けられ、この凹部12を囲むようにターゲット材2を配置する。一方、バッキングチューブ3の下端部を栓6で塞ぎ、バッキングチューブ3内への接合材の浸入を防ぐようにしておく。
凹部12には充填用接合材40を溶融状態で充填する。この充填用接合材40としては、下地処理接合材と同じ材料を用いるようにし、本例では純インジウム又はインジウム合金を充填している。
(Reheating process)
The divided target material 2a on which the base treatment layer 41a is formed is placed on the mounting table 11 shown in FIG. 5 in a state of being vertically connected. A recess 12 having an inner diameter substantially the same as the inner diameter of the target material 2 is provided on the surface of the mounting table 11, and the target material 2 is arranged so as to surround the recess 12. On the other hand, the lower end of the backing tube 3 is closed with a stopper 6 to prevent the bonding material from entering the backing tube 3.
The recess 12 is filled with the filling bonding material 40 in a molten state. As the filling bonding material 40, the same material as the base treatment bonding material is used, and in this example, pure indium or an indium alloy is filled.

この場合、上下に連結される分割ターゲット材2aの間には、環状スペーサ5を介在させる。環状スペーサ5は、分割ターゲット材2aの長さ方向の寸法誤差や端面の表面粗さを吸収し、これら分割ターゲット材2aを同軸上に配置できる機能と、分割ターゲット材2aの間に生じる隙間を塞ぐパッキンの機能とを有しており、分割ターゲット材2a同士を長さ方向(高さ方向)に正確に接続できる。
この環状スペーサ5としては、弾性を有する樹脂材料などにより形成され、本実施形態ではPTFE(ポリテトラフルオロエチレン)により形成される。
なお、ターゲット材2とバッキングチューブ3とを接合した後には環状スペーサ5は取り外されるため、取り出しやすいように、環状スペーサ5の外径はターゲット材2の外径よりも大きく設定される。
In this case, an annular spacer 5 is interposed between the split target materials 2a connected vertically. The annular spacer 5 absorbs the dimensional error in the length direction of the divided target material 2a and the surface roughness of the end face, and has a function of arranging the divided target material 2a coaxially and a gap generated between the divided target material 2a. It has the function of packing to close, and can accurately connect the divided target materials 2a to each other in the length direction (height direction).
The annular spacer 5 is formed of an elastic resin material or the like, and in the present embodiment, it is formed of PTFE (polytetrafluoroethylene).
Since the annular spacer 5 is removed after the target material 2 and the backing tube 3 are joined, the outer diameter of the annular spacer 5 is set to be larger than the outer diameter of the target material 2 so that it can be easily taken out.

また、ターゲット材2の上端に、ターゲット材2とバッキングチューブ3との隙間からあふれ出た充填用接合材40を受けるための受け皿7を設けておく。
そして、図5に示すように、ターゲット材2の内部にバッキングチューブ3を全体長さの8割程度挿入した状態で同軸上に配置する。この図5に示す状態では、酸化膜42は除去されたものとしているが、下地処理層41a,41bの表面に残存している場合もある。
そして、この図5に示す状態に組み立てた後に、ターゲット材2及びバッキングチューブ3をターゲット材2の周囲に配置したヒータ(図示略)により加熱する。例えば、200℃で1時間〜2時間加熱することにより、下地処理層41a,41bを溶融又は少なくとも半溶融状態とする。このときの再加熱により、下地処理層41a,41bの表面が酸化し、酸化膜42が形成される。前述したように、下地処理層41a,41bは厚さが大きく形成されているとともに、表面に傷が付けられているので、図6に示すように溶融時に自重で垂れ下がって下端部に流れ落ちることにより、酸化膜42が破壊される。
Further, a saucer 7 for receiving the filling joining material 40 overflowing from the gap between the target material 2 and the backing tube 3 is provided at the upper end of the target material 2.
Then, as shown in FIG. 5, the backing tube 3 is coaxially arranged inside the target material 2 with about 80% of the total length inserted. In the state shown in FIG. 5, it is assumed that the oxide film 42 has been removed, but it may remain on the surfaces of the base treatment layers 41a and 41b.
Then, after assembling in the state shown in FIG. 5, the target material 2 and the backing tube 3 are heated by a heater (not shown) arranged around the target material 2. For example, by heating at 200 ° C. for 1 to 2 hours, the base treatment layers 41a and 41b are melted or at least semi-melted. By reheating at this time, the surfaces of the base treatment layers 41a and 41b are oxidized to form an oxide film 42. As described above, the base treatment layers 41a and 41b are formed to have a large thickness and the surface is scratched. Therefore, as shown in FIG. 6, the base treatment layers hang down due to their own weight at the time of melting and flow down to the lower end portion. , The oxide film 42 is destroyed.

(接合材充填工程(接合工程))
図6に矢印で示すように、バッキングチューブ3の下端側を載置台11の凹部12に挿入すると、図7に示すように、溶融状態の充填用接合材40が凹部13から押し出されるようにターゲット材2の内周面とバッキングチューブ3の外周面との隙間を上昇し、ターゲット材2の内周面とバッキングチューブ3の外周面との間に充填用接合材40が充填される。
このとき、下地処理層41a,41b表面の酸化膜42が分断されているので、隙間内を上昇してくる充填用接合材40により押し上げられて、受け皿7内に排出される。また、酸化膜42の一部が充填用接合材40内に残ったとしても、充填用接合材40に分散しながら一体になって隙間内に充填される。
(Joint material filling process (joining process))
As shown by the arrow in FIG. 6, when the lower end side of the backing tube 3 is inserted into the recess 12 of the mounting table 11, the target is pushed out from the recess 13 as shown in FIG. The gap between the inner peripheral surface of the material 2 and the outer peripheral surface of the backing tube 3 is raised, and the filling joining material 40 is filled between the inner peripheral surface of the target material 2 and the outer peripheral surface of the backing tube 3.
At this time, since the oxide film 42 on the surfaces of the base treatment layers 41a and 41b is divided, it is pushed up by the filling bonding material 40 rising in the gap and discharged into the saucer 7. Further, even if a part of the oxide film 42 remains in the filling bonding material 40, it is integrally filled in the gap while being dispersed in the filling bonding material 40.

なお、載置台11の凹部12の容積は、バッキングチューブ3の下端が底面付近まで挿入されたときに、バッキングチューブ3の外周面とターゲット材2の内周面との間に形成される隙間の容積以上あればよく、隙間内を上昇した充填用接合材40がターゲット材2の上端側に若干オーバーフローする程度がよい。
この場合、充填用接合材40がターゲット材2の上端の受け皿7にあふれてきた状態でターゲット材2とバッキングチューブ3との間に充填用接合材40が隙間なく充填されたことが確認できる。
The volume of the recess 12 of the mounting table 11 is the volume of the gap formed between the outer peripheral surface of the backing tube 3 and the inner peripheral surface of the target material 2 when the lower end of the backing tube 3 is inserted near the bottom surface. It suffices to have a volume or more, and it is preferable that the filling joint material 40 that has risen in the gap slightly overflows to the upper end side of the target material 2.
In this case, it can be confirmed that the filling joint material 40 is filled between the target material 2 and the backing tube 3 without a gap in a state where the filling joint material 40 overflows the saucer 7 at the upper end of the target material 2.

このようにしてバッキングチューブ3の下端が凹部12の底面付近まで挿入することにより、ターゲット材2とバッキングチューブ3との隙間に充填用接合材40が隙間なく充填される。
なお、必ずしも限定されるものではないが、前述の再加熱工程、接合材充填工程(少なくとも充填完了までの間)は、不活性雰囲気にて実施するとよく、接合材の酸化を抑制し、さらなる接合強度の向上が可能となる。
By inserting the lower end of the backing tube 3 to the vicinity of the bottom surface of the recess 12 in this way, the filling joining material 40 is filled in the gap between the target material 2 and the backing tube 3 without any gap.
Although not necessarily limited, the above-mentioned reheating step and joining material filling step (at least until the filling is completed) may be carried out in an inert atmosphere to suppress oxidation of the joining material and further join. The strength can be improved.

(接合材冷却工程)
ターゲット材2とバッキングチューブ3との隙間に充填用接合材40を充填した後、これを冷却して固化させることで、これらターゲット材2とバッキングチューブ3とが接合部4により一体化する。
その後、環状スペーサ5や受け皿7、はみ出した接合材等を除去し、清掃することにより円筒型スパッタリングターゲット1が得られる。
(Joint material cooling process)
After filling the gap between the target material 2 and the backing tube 3 with the filling joint material 40, the target material 2 and the backing tube 3 are integrated by the joint portion 4 by cooling and solidifying the joint material 40.
After that, the annular spacer 5, the saucer 7, the protruding joint material, and the like are removed and cleaned to obtain the cylindrical sputtering target 1.

以上説明した方法により、下地処理層41a,41bを厚肉に形成して、表面に傷を付けておき、これを再加熱時に半溶融状態とすることにより、自重で垂れ下がる下地処理層41a,41bの表面で酸化膜42を破壊して分断させ、その後、バッキングチューブ3とターゲット材2との隙間に充填用接合材40を充填する。このため、充填用接合材40と下地処理接合材41a,41bとの一体化が酸化膜42により阻害されることがなく、これらの接合強度を向上しつつ一体化でき、優れた品質の円筒型スパッタリングターゲット1を製造できる。
しかも、ターゲット材2及びバッキングチューブ3に厚肉の下地処理層41a,41bを形成して、その表面に傷を付けておくという簡単な操作で酸化膜42の影響を抑制することができ、ターゲット材2とバッキングチューブ3とを強固に接合することができる。
By the method described above, the base treatment layers 41a and 41b are formed thickly, the surface is scratched, and the base treatment layers 41a and 41b hang down by their own weight by putting them in a semi-molten state at the time of reheating. The oxide film 42 is broken and divided on the surface of the above, and then the gap between the backing tube 3 and the target material 2 is filled with the filling bonding material 40. Therefore, the integration of the filling bonding material 40 and the base-treated bonding materials 41a and 41b is not hindered by the oxide film 42, and these bonding materials can be integrated while being improved, and a cylindrical mold having excellent quality. The sputtering target 1 can be manufactured.
Moreover, the influence of the oxide film 42 can be suppressed by a simple operation of forming thick base treatment layers 41a and 41b on the target material 2 and the backing tube 3 and scratching the surface thereof, and the target. The material 2 and the backing tube 3 can be firmly joined.

図8〜図10は、本発明の第2実施形態の製造方法を示している。なお、この実施形態以降において、前記実施形態と同一部分は同一符号によって表し、その説明を省略する。以下、図11の実施形態においても同様とする。
この第2実施形態では、ターゲット材2の間に設けられている環状スペーサ51の内周部をターゲット材2の内周面より径方向内方に突出させておき、接合材充填工程時のバッキングチューブ3をターゲット材2に挿入する際に、バッキングチューブ3の下地処理層41bの酸化膜42を環状スペーサ51によって掻き取るようにしたものである。
すなわち、ターゲット材2に設けられている環状スペーサ51の内周部が分割ターゲット材2aの径方向内方に突出し、その内径がバッキングチューブ3の外径とほぼ同じ内径(一致した径か、わずかに小径又はわずかに大径)に形成されている。
また、図9に示すように、掻き取り板(環状スペーサ)51には、穴55及び切り込み部56が設けられている。これら穴56及び切り込み部57は、接合工程において、溶融した充填用接合材が穴55及び切り込み部56を通過して流通できるようになっている。なお、穴55及び切り込み部56は、図9に示された形状以外の任意の形状や形成位置及び数により設けるようにしてもよいし、溶融した充填用接合材が通過できるのであれば、穴55又は切り込み部56のいずれか一方のみが形成されるものであってもよい。
8 to 10 show the manufacturing method of the second embodiment of the present invention. In addition, in this embodiment and after, the same part as the said embodiment is represented by the same code, and the description thereof will be omitted. Hereinafter, the same applies to the embodiment shown in FIG.
In this second embodiment, the inner peripheral portion of the annular spacer 51 provided between the target materials 2 is projected inward in the radial direction from the inner peripheral surface of the target material 2, and backing during the joining material filling step is performed. When the tube 3 is inserted into the target material 2, the oxide film 42 of the base treatment layer 41b of the backing tube 3 is scraped off by the annular spacer 51.
That is, the inner peripheral portion of the annular spacer 51 provided on the target material 2 projects inward in the radial direction of the divided target material 2a, and the inner diameter thereof is substantially the same as the outer diameter of the backing tube 3 (matched diameter or slightly). It is formed with a small diameter or a slightly large diameter).
Further, as shown in FIG. 9, the scraping plate (annular spacer) 51 is provided with a hole 55 and a notch 56. In these holes 56 and the cut portion 57, the molten filling bonding material can flow through the holes 55 and the cut portion 56 in the joining step. The holes 55 and the cut portions 56 may be provided in any shape, formation position and number other than the shape shown in FIG. 9, and if the molten filling joint material can pass through, the holes may be provided. Only one of 55 or the notch 56 may be formed.

この第2実施形態の場合は、ターゲット材2の内周面の下地処理層41aは第1実施形態と同様に厚肉に形成するが、バッキングチューブ3の下地処理層41bはターゲット材2の下地処理層41aより薄く形成しておく。この厚肉の下地処理層41aを第1下地処理層、薄肉の下地処理層41bを第2下地処理層とする。したがって、第1実施形態の場合は、両下地処理層41a,41bとも第1下地処理層である。
また、それぞれの下地処理層41a,41bを下地処理接合材冷却工程の後に、表面の酸化膜42を除去するか、少なくとも下地処理層41a,41bに達する傷を付けておく。
In the case of the second embodiment, the base treatment layer 41a on the inner peripheral surface of the target material 2 is formed to be thick as in the first embodiment, but the base treatment layer 41b of the backing tube 3 is the base of the target material 2. It is formed thinner than the treatment layer 41a. The thick base treatment layer 41a is used as the first base treatment layer, and the thin base treatment layer 41b is used as the second base treatment layer. Therefore, in the case of the first embodiment, both the base treatment layers 41a and 41b are the first base treatment layers.
Further, after the base treatment bonding material cooling step, the surface oxide film 42 is removed from each of the base treatment layers 41a and 41b, or at least the base treatment layers 41a and 41b are scratched.

そして、接合工程において、図8に示すようにターゲット材2の上端部にバッキングチューブ3の下端部を挿入した状態でこれらを再加熱する。この再加熱により、両下地処理層41a,41bに酸化膜42が形成され、ターゲット材2の下地処理層41a(第1下地処理層)は厚肉であるため垂れ下がった状態となる。バッキングチューブ3の下地処理層41b(第2下地処理層)にも酸化膜42は形成されるが、下地処理層41bが薄肉であるため垂れ下がることはない。
そして、この加熱状態でターゲット材2にバッキングチューブ3を挿入していくと、ターゲット材2に設けられている掻き取り板51は、その内径がバッキングチューブ3の外径とほぼ同じに形成されているので、バッキングチューブ3が挿入される際に、掻き取り板51の内周部でバッキングチューブ3の外周面上が擦られ、この外周面上の酸化膜42が掻き取られる。掻き取られた酸化膜42は、膜としては破壊された状態となり、隙間内を上昇してくる充填用接合材40により押し上げられて、受け皿7内に排出される。また、酸化膜42の一部が充填用接合材40内に残ったとしても、充填用接合材40に分散しながら一体になって隙間内に充填される。
一方、掻き取り板51により酸化膜42が除去された後のバッキングチューブ3の外周面には、酸化膜42のない下地処理層41bが薄く残り、この下地処理層41bに充填用接合材40が均一になじんで一体化する。
ターゲット材2内周面の下地処理層41a(第1下地処理層)においては、厚肉であるため、第1実施形態と同様に垂れ下がった状態となり、酸化膜42も破壊される。
Then, in the joining step, as shown in FIG. 8, the lower end portion of the backing tube 3 is inserted into the upper end portion of the target material 2 and these are reheated. By this reheating, the oxide film 42 is formed on both the base treatment layers 41a and 41b, and the base treatment layer 41a (first base treatment layer) of the target material 2 is thick and therefore hangs down. The oxide film 42 is also formed on the base treatment layer 41b (second base treatment layer) of the backing tube 3, but it does not hang down because the base treatment layer 41b is thin.
Then, when the backing tube 3 is inserted into the target material 2 in this heated state, the inner diameter of the scraping plate 51 provided on the target material 2 is formed to be substantially the same as the outer diameter of the backing tube 3. Therefore, when the backing tube 3 is inserted, the inner peripheral portion of the scraping plate 51 rubs the outer peripheral surface of the backing tube 3, and the oxide film 42 on the outer peripheral surface is scraped off. The scraped oxide film 42 is in a destroyed state as a film, is pushed up by the filling bonding material 40 rising in the gap, and is discharged into the saucer 7. Further, even if a part of the oxide film 42 remains in the filling bonding material 40, it is integrally filled in the gap while being dispersed in the filling bonding material 40.
On the other hand, on the outer peripheral surface of the backing tube 3 after the oxide film 42 is removed by the scraping plate 51, the base treatment layer 41b without the oxide film 42 remains thin, and the filling bonding material 40 is formed on the base treatment layer 41b. It fits evenly and integrates.
Since the base treatment layer 41a (first base treatment layer) on the inner peripheral surface of the target material 2 is thick, it is in a hanging state as in the first embodiment, and the oxide film 42 is also destroyed.

なお、図8等に示す例では、ターゲット材2を3個の分割ターゲット材2aからなる構成とし、各分割ターゲット材2aの間の各環状スペーサ51を掻き取り板として機能させるように内周部を分割ターゲット材2aから突出させたが、掻き取り板としては、いずれか1個の環状スペーサにその機能を持たせるようにして、他の環状スペーサ5は、第1実施形態のものと同様、内周縁を分割ターゲット材2aと同じ内径に形成してもよいし、すべての環状スペーサの内周部を分割ターゲット材2aから径方向内方に突出させて掻き取り板として機能させるようにしてもよい。
なお、接合後に環状スペーサ51を除去することで、図10に示すように、環状スペーサ51を設けていた部分は接合部4の厚さが薄くなる。
また、ターゲット材2の上端の受け皿7の内周部を環状スペーサ51と同様に径方向内方に突出させて、その内周部を掻き取り板として利用してもよい。この場合、掻き取り板としての環状スペーサ51と併用してもよい。
In the example shown in FIG. 8 and the like, the target material 2 is composed of three divided target materials 2a, and each annular spacer 51 between the divided target materials 2a functions as a scraping plate. Was projected from the split target material 2a, but as a scraping plate, any one of the annular spacers was provided with the function, and the other annular spacer 5 was the same as that of the first embodiment. The inner peripheral edge may be formed to have the same inner diameter as the split target material 2a, or the inner peripheral portions of all the annular spacers may be projected inward in the radial direction from the split target material 2a to function as a scraping plate. Good.
By removing the annular spacer 51 after joining, the thickness of the joint portion 4 becomes thinner in the portion where the annular spacer 51 is provided, as shown in FIG.
Further, the inner peripheral portion of the saucer 7 at the upper end of the target material 2 may be projected inward in the radial direction in the same manner as the annular spacer 51, and the inner peripheral portion thereof may be used as a scraping plate. In this case, it may be used in combination with the annular spacer 51 as a scraping plate.

図11は、本発明の第3実施形態の製造方法の製造途中の状態を示している。
前述した第2実施形態では、バッキングチューブ3の下地処理層41bの酸化膜を掻き取るようにしたが、この第3実施形態では、ターゲット材2の下地処理層41aの酸化膜42を除去するようにしている。すなわち、掻き取り板8をバッキングチューブ3の下端に設けておき、ターゲット材2にバッキングチューブ3を挿入する際に、掻き取り板8の外周部でターゲット材2の内周面上の下地処理層41aの酸化膜42を掻き取るようにしたものである。ターゲット材2の下地処理層41aは薄肉に形成され、バッキングチューブ3の下地処理層41bは厚肉に形成される。つまり、この実施形態では、ターゲット材2の下地処理層41aが第2下地処理層であり、バッキングチューブ3の下地処理層41bが第1下地処理層である。
この場合、前述した栓6に掻き取り板8を固定すればよい。この掻き取り板8は、外径がターゲット材2の内径とほぼ同じ(一致した径か、わずかに小径又はわずかに大径)に形成される。
FIG. 11 shows a state in the middle of manufacturing the manufacturing method according to the third embodiment of the present invention.
In the second embodiment described above, the oxide film of the base treatment layer 41b of the backing tube 3 is scraped off, but in this third embodiment, the oxide film 42 of the base treatment layer 41a of the target material 2 is removed. I have to. That is, the scraping plate 8 is provided at the lower end of the backing tube 3, and when the backing tube 3 is inserted into the target material 2, the base treatment layer on the inner peripheral surface of the target material 2 is formed at the outer peripheral portion of the scraping plate 8. The oxide film 42 of 41a is scraped off. The base treatment layer 41a of the target material 2 is formed to be thin, and the base treatment layer 41b of the backing tube 3 is formed to be thick. That is, in this embodiment, the base treatment layer 41a of the target material 2 is the second base treatment layer, and the base treatment layer 41b of the backing tube 3 is the first base treatment layer.
In this case, the scraping plate 8 may be fixed to the stopper 6 described above. The scraping plate 8 is formed so that the outer diameter is substantially the same as the inner diameter of the target material 2 (matched diameter, slightly smaller diameter, or slightly larger diameter).

掻き取り板8によりターゲット材2の内周面から掻き取られた酸化膜42は、凹部12に流れ込み、この凹部12に充填されている充填用接合材40に混入するが、膜としては破壊されているので、再び膜状に形成されることはない。
バッキングチューブ3の下地処理層41bに形成された酸化膜42は、下地処理層41bが厚肉に形成されていたため、再加熱により垂れ下がって破壊される。
The oxide film 42 scraped from the inner peripheral surface of the target material 2 by the scraping plate 8 flows into the recess 12 and mixes with the filling bonding material 40 filled in the recess 12, but the film is destroyed. Therefore, it is not formed into a film again.
The oxide film 42 formed on the base treatment layer 41b of the backing tube 3 hangs down and is destroyed by reheating because the base treatment layer 41b is formed thick.

なお、前述の実施形態では、ターゲット材2とバッキングチューブ3との両方に下地処理接合材を塗布したが、いずれかの表面が充填用接合材40と濡れやすい状態であれば、その表面については下地処理接合材の塗布を省略してもよい。言い換えれば、接合工程時において、下地処理接合材は、ターゲット材2とバッキングチューブ3との少なくとも何れか一方に塗布して下地処理層11を形成するようにしてもよい。 In the above-described embodiment, the base treatment bonding material is applied to both the target material 2 and the backing tube 3, but if either surface is easily wetted with the filling bonding material 40, the surface thereof The application of the base treatment bonding material may be omitted. In other words, at the time of the joining step, the base treatment bonding material may be applied to at least one of the target material 2 and the backing tube 3 to form the base treatment layer 11.

本発明の効果を確認するため、実験を行った。ターゲット材及びバッキングチューブに表1の材種のものを用い、それぞれ下地処理接合層を表1の厚さで形成した。なお実施例6のターゲット種であるSIZとは、Si、In、Zrの酸化物焼結体であり、実施例7のAZOは、Al、Znの酸化物焼結体であり、実施例8のCuGaはCu、Gaの合金であり、実施例9のCuNiとはCu、Niの合金であり、実施例10のCuCuOとはCu、CuOの焼結体である。ターゲット材とバッキングチューブとの隙間は1.0mmとした。
下地処理接合材としてはInはんだ材を用いた。下地処理に際しては、表面温度が240℃〜260℃に達するまで温風にて加熱し、大気雰囲気中で超音波はんだコテを用いながら下地処理接合材を塗布し、表面が均一に濡れたところで、溶融した接合材を滴下し、ターゲット材及びバッキングチューブを回転しながら厚塗りし、常温まで冷却した。
下地処理層の厚さは、下地処理層を形成する前後でターゲット材とバッキングチューブの厚さを任意の8点でそれぞれ測定して、8点の平均値を算出し、(下地処理層形成後の厚さの平均値−下地処理層形成前の厚さの平均値)により下地処理層の厚さを求めた。
接合後、超音波探傷検査装置により接合面積率を計測した。接合面積率は、ターゲット材とバッキングチューブとの接合面の総面積に対して、接合不良個所を除いた接合済面積の比率である。接合面積率が90%以上で合格とできる。
An experiment was conducted to confirm the effect of the present invention. As the target material and the backing tube, those of the materials shown in Table 1 were used, and the base-treated joint layer was formed to the thickness shown in Table 1, respectively. SIZ, which is the target species of Example 6, is an oxide sintered body of Si, In, and Zr, and AZO of Example 7 is an oxide sintered body of Al, Zn, and is of Example 8. CuGa is an alloy of Cu and Ga, CuNi of Example 9 is an alloy of Cu and Ni, and CuCuO of Example 10 is a sintered body of Cu and CuO. The gap between the target material and the backing tube was 1.0 mm.
An In solder material was used as the base treatment bonding material. In the base treatment, heat with warm air until the surface temperature reaches 240 ° C to 260 ° C, apply the base treatment bonding material in the air atmosphere using an ultrasonic soldering iron, and when the surface is uniformly wet, The molten bonding material was dropped, and the target material and the backing tube were thickly coated while rotating, and cooled to room temperature.
For the thickness of the base treatment layer, the thickness of the target material and the backing tube was measured at any 8 points before and after the base treatment layer was formed, and the average value of the 8 points was calculated (after the base treatment layer was formed). The thickness of the base treatment layer was determined by (the average value of the thickness before formation of the base treatment layer-the average value of the thickness before the formation of the base treatment layer).
After joining, the joining area ratio was measured by an ultrasonic flaw detection inspection device. The joint area ratio is the ratio of the joined area excluding the defective joint to the total area of the joint surface between the target material and the backing tube. It can be passed when the joint area ratio is 90% or more.

また、実施例1〜10、比較例1、2では掻き取り板を設置せず、掻き取りは行わなかった。実施例11は図11のように掻き取り板を設置し、ターゲット内周面を掻き取りした。実施例12は図8のように掻き取り板を設置し、バッキングチューブ外周面を掻き取りした。
これらの結果を表1に示す。表中、BTはバッキングチューブ、TGはターゲット材を示す。
Further, in Examples 1 to 10 and Comparative Examples 1 and 2, the scraping plate was not installed and scraping was not performed. In Example 11, a scraping plate was installed as shown in FIG. 11, and the inner peripheral surface of the target was scraped. In Example 12, a scraping plate was installed as shown in FIG. 8, and the outer peripheral surface of the backing tube was scraped.
These results are shown in Table 1. In the table, BT indicates a backing tube and TG indicates a target material.

Figure 2020158806
Figure 2020158806

表1からわかるように、ターゲット材及びバッキングチューブの少なくともいずれか一方の下地処理層の厚さが0.1mm以上0.8mm以下の場合、いずれも接合面積率が90%以上であった。
これに対して、比較例1及び比較例2は、ターゲット材及びバッキングチューブとも下地処理層の厚さが小さいため、接合率が90%未満であった。
As can be seen from Table 1, when the thickness of at least one of the base treatment layer of the target material and the backing tube was 0.1 mm or more and 0.8 mm or less, the joint area ratio was 90% or more.
On the other hand, in Comparative Example 1 and Comparative Example 2, the bonding ratio was less than 90% because the thickness of the base treatment layer was small for both the target material and the backing tube.

1 円筒型スパッタリングターゲット
2 円筒型ターゲット材
2a 分割ターゲット材
3 円筒型バッキングチューブ
4 接合部
40 充填用接合材
41a,41b 下地処理層
42 酸化膜
5 環状スペーサ
51 環状スペーサ(掻き取り板)
55 穴
56 切り込み部
6 栓
7 受け皿
8 掻き取り板
11 載置台
12 凹部
1 Cylindrical sputtering target 2 Cylindrical target material 2a Divided target material 3 Cylindrical backing tube 4 Joint 40 Filling joint material 41a, 41b Base treatment layer 42 Oxidation film 5 Circular spacer 51 Circular spacer (scraping plate)
55 Hole 56 Notch 6 Plug 7 Receiving tray 8 Scraping plate 11 Mounting stand 12 Recess

Claims (2)

円筒型ターゲット材の内周面と該円筒型ターゲット材の内側に挿入した円筒型バッキングチューブの外周面との隙間を接合材で充填して接合する円筒型スパッタリングターゲットの製造方法であって、前記円筒型ターゲット材の内周面と前記円筒側バッキングチューブの外周面との少なくとも何れか一方の部材に下地処理接合材を塗布して0.1mm以上0.8mm以下の第1下地処理層を形成する下地処理工程と、下地処理工程の後、前記円筒型ターゲット材内に前記円筒型バッキングチューブを挿入し、該円筒型ターゲット材と前記円筒型バッキングチューブとの隙間に溶融状態の充填用接合材を充填する接合工程とを有し、前記下地処理工程では、前記第1下地処理層の少なくとも表面に傷を付けておき、前記接合工程では、前記第1下地処理層の少なくとも表面が半溶融状態となるまで加熱した後、前記充填用接合材を充填することを特徴とする円筒型スパッタリングターゲットの製造方法。 A method for manufacturing a cylindrical sputtering target, wherein the gap between the inner peripheral surface of the cylindrical target material and the outer peripheral surface of the cylindrical backing tube inserted inside the cylindrical target material is filled with a joining material to join. A base treatment bonding material is applied to at least one member of the inner peripheral surface of the cylindrical target material and the outer peripheral surface of the cylindrical backing tube to form a first base treatment layer of 0.1 mm or more and 0.8 mm or less. After the base treatment step and the base treatment step, the cylindrical backing tube is inserted into the cylindrical target material, and a bonding material for filling in a molten state is inserted in the gap between the cylindrical target material and the cylindrical backing tube. In the base treatment step, at least the surface of the first base treatment layer is scratched, and in the joining step, at least the surface of the first base treatment layer is in a semi-molten state. A method for producing a cylindrical sputtering target, which comprises filling the filling bonding material after heating until 前記下地処理工程では、前記第1下地処理層が形成された前記一方の部材とは反対側の他方の部材に、前記第1下地処理層よりも薄肉の第2下地処理層を形成しておき、前記第1下地処理層が形成された前記一方の部材に、前記隙間内に径方向に突出して配置可能な掻き取り板を周方向に沿って設けておき、前記接合工程において、前記掻き取り板により前記第2下地処理層の表面に形成された酸化膜の少なくとも一部を掻き取りながら前記円筒型ターゲット材内に前記円筒型バッキングチューブを挿入することを特徴とする請求項1記載の円筒型スパッタリングターゲットの製造方法。
In the base treatment step, a second base treatment layer thinner than the first base treatment layer is formed on the other member on the opposite side of the one member on which the first base treatment layer is formed. A scraping plate that can be arranged so as to project radially in the gap is provided along the circumferential direction on the one member on which the first surface treatment layer is formed, and the scraping is performed in the joining step. The cylinder according to claim 1, wherein the cylindrical backing tube is inserted into the cylindrical target material while scraping at least a part of the oxide film formed on the surface of the second surface treatment layer by the plate. Manufacturing method of type sputtering target.
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