JP7552604B2 - target - Google Patents
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- JP7552604B2 JP7552604B2 JP2021546593A JP2021546593A JP7552604B2 JP 7552604 B2 JP7552604 B2 JP 7552604B2 JP 2021546593 A JP2021546593 A JP 2021546593A JP 2021546593 A JP2021546593 A JP 2021546593A JP 7552604 B2 JP7552604 B2 JP 7552604B2
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- 239000000203 mixture Substances 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 230000005291 magnetic effect Effects 0.000 description 34
- 239000000843 powder Substances 0.000 description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 25
- 230000004907 flux Effects 0.000 description 16
- 238000000034 method Methods 0.000 description 16
- 238000005245 sintering Methods 0.000 description 16
- 239000002184 metal Substances 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 14
- 229910052742 iron Inorganic materials 0.000 description 11
- 238000004544 sputter deposition Methods 0.000 description 9
- 239000002775 capsule Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011812 mixed powder Substances 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 238000009689 gas atomisation Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910001080 W alloy Inorganic materials 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 238000003825 pressing Methods 0.000 description 3
- 238000012935 Averaging Methods 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 230000003313 weakening effect Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Powder Metallurgy (AREA)
- Magnetic Record Carriers (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Valve Device For Special Equipments (AREA)
Description
本発明は、例えば、磁気記録媒体のシード層を形成するためのターゲットに関するものである。 The present invention relates, for example, to a target for forming a seed layer of a magnetic recording medium.
磁気記録媒体の記録密度を向上させる手段として、垂直磁気記録方式が実用化されている。この垂直磁気記録方式とは、磁気記録層を媒体面に対して磁化容易軸が垂直方向に配向するように形成したものであり、記録密度を上げていってもビット内の反磁界が小さく、記録再生特性の低下が少ない高記録密度に適した方法である。
そして、磁気記録層を媒体面に対して磁化容易軸が垂直方向に配向させるため、中間層としてＲｕを適用し、シード層としてＮｉ合金を用いることが提案されている。
As a means of improving the recording density of magnetic recording media, the perpendicular magnetic recording method has been put to practical use. This perpendicular magnetic recording method is a method in which the magnetic recording layer is formed so that the axis of easy magnetization is oriented perpendicular to the medium surface, and is suitable for high recording density because the demagnetizing field within the bit is small even when the recording density is increased, and the deterioration of recording and reproduction characteristics is small.
In order to orient the magnetic easy axis of the magnetic recording layer perpendicular to the medium surface, it has been proposed to use Ru as the intermediate layer and a Ni alloy as the seed layer.
このような磁気記録媒体のシード層として用いられるＮｉ合金は、ｆｃｃ構造、（１１１）面への配向性を備える軟磁性材で構成され、磁気ヘッドから発生する磁界を引き込む役割と、中間層の結晶性と、磁気記録層の酸化物の粒界偏析を制御することが求められており、例えば、Ｎｉ－Ｆｅ－Ｗ合金が提案されている（特許文献１参照）。
そして、このＮｉ－Ｆｅ－Ｗ合金からなるシード層の形成には、一般的にターゲットを用いたスパッタリング法が適用されている。
The Ni alloy used as the seed layer of such magnetic recording media is composed of a soft magnetic material with an fcc structure and orientation to the (111) plane, and is required to attract the magnetic field generated by the magnetic head, as well as to control the crystallinity of the intermediate layer and the grain boundary segregation of oxides in the magnetic recording layer; for example, a Ni-Fe-W alloy has been proposed (see Patent Document 1).
In order to form the seed layer made of the Ni--Fe--W alloy, a sputtering method using a target is generally applied.
特許文献１に開示されるシード層は、磁気記録層の磁気特性の劣化を抑制でき、中間層の厚い場合でも書き込み性能を改善できるという点で有用な技術である。
しかしながら、本発明者の検討によると、特許文献１に開示されるＮｉ－Ｆｅ－Ｗ合金からなるターゲットを用いて、スパッタリングによりシード層を成膜したところ、漏洩磁束が低く、高速での成膜が困難になり、ターゲットの使用効率が低くなる場合があることを確認した。また、特許文献１に開示されるＮｉ－Ｆｅ－Ｗ合金からなるターゲットを用いて、スパッタリングによりシード層を成膜する際に、パーティクルと呼ばれる欠陥が多く発生する場合があることを確認した。
The seed layer disclosed in Patent Document 1 is a useful technique in that it can suppress deterioration of the magnetic characteristics of the magnetic recording layer and can improve the write performance even when the intermediate layer is thick.
However, according to the study by the present inventors, when a seed layer is formed by sputtering using a target made of the Ni-Fe-W alloy disclosed in Patent Document 1, it has been confirmed that leakage flux is low, making it difficult to form a film at high speed, and the use efficiency of the target may be low. In addition, it has been confirmed that when a seed layer is formed by sputtering using a target made of the Ni-Fe-W alloy disclosed in Patent Document 1, many defects called particles may be generated.
本発明の目的は、高い漏洩磁束を有し、スパッタリングの際にパーティクルの発生量が少なく、例えば、磁気記録媒体の製造に有用なターゲットを提供することである。The object of the present invention is to provide a target which has high leakage magnetic flux and generates a small amount of particles during sputtering, and which is useful, for example, in the manufacture of magnetic recording media.
本発明のターゲットは、原子比における組成式がＮｉ１００－Ｘ－Ｙ－ＦｅＸ－ＷＹ、５≦Ｘ≦４０、１≦Ｙ≦１５で表わされ、残部が不可避的不純物からなり、ＮｉＷからなるマトリックス相中にＦｅＷ相が分散している。 The target of the present invention has a composition formula in atomic ratio expressed as Ni100-XY-FeX - WY , where 5≦X≦40 and 1≦Y≦15, with the remainder being unavoidable impurities, and has an FeW phase dispersed in a matrix phase made of NiW.
本発明のターゲットは、０．１２ｍｍ２当たりで、４００μｍ以上の内接円直径を有するＦｅＷ相が１個未満であることが好ましい。 The target of the present invention preferably contains less than one FeW phase having an inscribed circle diameter of 400 μm or more per 0.12 mm2 .
本発明のターゲットは、０．１２ｍｍ２当たりで、１５μｍ以上の内接円直径を有するＷ相が１個未満であることが好ましい。 The target of the present invention preferably contains less than one W phase having an inscribed circle diameter of 15 μm or more per 0.12 mm2 .
本発明は、高い漏洩磁束を有し、スパッタリングの際にパーティクルの発生量が少なく、例えば、磁気記録媒体の製造に有用なターゲットを提供することができる。 The present invention can provide a target that has high leakage magnetic flux and generates low amounts of particles during sputtering, making it useful, for example, for the production of magnetic recording media.
本発明のターゲットは、ＮｉＷからなるマトリックス相中にＦｅＷ相を分散させる。
ＮｉとＦｅが合金化すると、磁性（透磁率）が高くなり、高い漏洩磁束が得られなくなる。このため、本発明のターゲットは、ＮｉとＦｅの合金化を抑制して、ＮｉＷからなるマトリックス相中にＦｅＷ相を分散させた金属組織とする。具体的には、本発明のターゲットは、非磁性のＷを、強磁性体であるＮｉおよびＦｅと、それぞれ合金化させ、マトリックスをＮｉＷ相とし、ＦｅＷ相を分散させることにより、各相の磁性を弱めることができ、高い漏洩磁束が得られ、高速での成膜が可能となる、すなわちターゲットの使用効率を高くすることができる。
尚、ターゲットの金属組織中にＮｉＦｅＷ相やＮｉＦｅ相が存在すると、ＮｉとＦｅの合金化により磁性が高くなり、高い漏洩磁束が得られなくなる。また、ターゲットの金属組織中に、Ｆｅ相が存在すると、非磁性のＷによる磁性を弱める効果が得られず、漏洩磁束が低くなる。このため、本発明の実施形態に係るターゲットは、金属組織中に、ＮｉＦｅＷ相、ＮｉＦｅ相およびＦｅ相がなく、ＮｉＷ相、ＦｅＷ相およびＷ相で構成されることが好ましい。
In the target of the present invention, an FeW phase is dispersed in a matrix phase made of NiW.
When Ni and Fe are alloyed, the magnetism (magnetic permeability) becomes high, and high leakage magnetic flux cannot be obtained. Therefore, the target of the present invention suppresses the alloying of Ni and Fe, and has a metal structure in which the FeW phase is dispersed in the matrix phase made of NiW. Specifically, the target of the present invention is alloyed with non-magnetic W and ferromagnetic Ni and Fe, respectively, to make the matrix into a NiW phase, and to disperse the FeW phase, thereby weakening the magnetism of each phase, obtaining a high leakage magnetic flux, and enabling high-speed film formation, i.e., the utilization efficiency of the target can be increased.
If the NiFeW phase or NiFe phase exists in the metal structure of the target, the magnetism becomes high due to the alloying of Ni and Fe, and high leakage magnetic flux cannot be obtained. Also, if the Fe phase exists in the metal structure of the target, the effect of weakening the magnetism by non-magnetic W cannot be obtained, and the leakage magnetic flux becomes low. Therefore, it is preferable that the target according to the embodiment of the present invention does not have the NiFeW phase, NiFe phase, and Fe phase in the metal structure, and is composed of the NiW phase, FeW phase, and W phase.
本発明のターゲットは、Ｎｉ、ＦｅおよびＷを含有し、残部が不可避的不純物で構成される。Ｎｉ、Ｆｅ、Ｗの含有量は、シード層として必要とされるｆｃｃ構造、（１１１）面への配向性等の軟磁気特性を大きく損なわない範囲で適宜調整することができ、具体的には、原子比における組成式がＮｉ１００－Ｘ－Ｙ－ＦｅＸ－ＷＹ、５≦Ｘ≦４０、１≦Ｙ≦１５で表わされ、残部が不可避的不純物からなる。
本発明のターゲットは、Ｆｅの含有量、すなわち組成式のＸを５以上にすることにより、低い保磁力を備えるシード層を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｘを１０以上にすることが好ましい。
また、本発明のターゲットは、Ｘを４０以下にすることにより、安定したｆｃｃ構造、（１１１）面への配向性を備えるシード層を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｘを２０以下にすることが好ましい。
The target of the present invention contains Ni, Fe and W, with the remainder being unavoidable impurities. The contents of Ni, Fe and W can be appropriately adjusted within a range that does not significantly impair the soft magnetic properties, such as the fcc structure required for a seed layer and the orientation to the (111) plane, and specifically, the composition formula in atomic ratio is expressed as Ni100-X-Y - FeX - WY , 5≦X≦40, 1≦Y≦15, with the remainder being unavoidable impurities.
In the target of the present invention, a seed layer having low coercivity can be obtained by setting the Fe content, i.e., X in the composition formula, to 5 or more. For the same reasons as above, it is preferable that the target according to the embodiment of the present invention has X set to 10 or more.
Moreover, in the target of the present invention, a seed layer having a stable fcc structure and orientation to the (111) plane can be obtained by setting X to 40 or less. And, in the target according to the embodiment of the present invention, it is preferable to set X to 20 or less for the same reason as above.
本発明のターゲットは、Ｗの含有量、すなわち組成式のＹを１以上にすることにより、安定したｆｃｃ構造、（１１１）面への配向性を備えるシード層を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｙを２以上にすることが好ましい。
また、本発明のターゲットは、Ｙを１５以下にすることにより、高い飽和磁束密度を有するシード層を得ることができる。そして、本発明の実施形態に係るターゲットは、上記と同様の理由から、Ｙを８以下にすることが好ましい。
In the target of the present invention, a seed layer having a stable fcc structure and orientation to the (111) plane can be obtained by setting the W content, i.e., Y in the composition formula, to 1 or more. For the same reasons as above, it is preferable that the target according to the embodiment of the present invention has Y of 2 or more.
Furthermore, in the target of the present invention, a seed layer having a high saturation magnetic flux density can be obtained by setting Y to 15 or less. And, in the target according to the embodiment of the present invention, it is preferable to set Y to 8 or less for the same reason as above.
本発明の実施形態に係るターゲットは、０．１２ｍｍ２当たりで、４００μｍ以上の内接円直径を有するＦｅＷ相を１個未満とすることが好ましい。これにより、本発明のターゲットは、パーティクルの発生を抑制することができる。
ＦｅＷ相は、本発明のターゲットを構成する金属組織（ＮｉＷ相、ＦｅＷ相、Ｗ相）の中で、最も磁性が強くなる。そして、ＦｅＷ相のうち、内接円直径が４００μｍ以上という粗大なＦｅＷ相が存在すると、局所的に漏洩磁束が低くなり過ぎてしまい、スパッタリングが進行し難くなり、ターゲット表面にノジュールと呼ばれる凸部が発生する場合があり、アーキングと呼ばれる異常放電の起点となる虞がある。このため、本発明の実施形態に係るターゲットは、内接円直径が３００μｍ以上のＦｅＷ相を１個未満とすることがより好ましい。
ここで、本発明でいう内接円直径は、ある輪郭形状の内部に描くことのできる、その輪郭の少なくとも一点で接する円のうちで、最大の面積（直径）を有するものの直径のことである。そして、本発明でいうＦｅＷ相の内接円直径は、ターゲットのスパッタ面となる面の、任意の０．１２ｍｍ２となる視野において、走査型電子顕微鏡による反射電子像の濃灰色で示されるＦｅＷ相を撮影して測定することができる。そして、４００μｍ以上の内接円直径を有するＦｅＷ相の個数は、スパッタ面となる面で０．１２ｍｍ２となる１視野の観察を行ない、その視野に存在する内接円直径が４００μｍ以上のＦｅＷ相の個数をカウントすることで得られる。また、パーティクルの発生を抑制する観点から、４００μｍ以上の内接円直径を有するＦｅＷ相の個数は、スパッタ面となる面で０．１２ｍｍ２となる視野を複数視野（例えば５視野）で観察を行ない、各視野に存在する内接円直径が４００μｍ以上のＦｅＷ相の個数をカウントして、その平均値としてもよい。
In the target according to the embodiment of the present invention, it is preferable that the number of FeW phases having an inscribed circle diameter of 400 μm or more per 0.12 mm 2 is less than one. This makes it possible for the target of the present invention to suppress the generation of particles.
The FeW phase is the most magnetic of the metal structures (NiW phase, FeW phase, W phase) constituting the target of the present invention. If a coarse FeW phase with an inscribed circle diameter of 400 μm or more is present among the FeW phases, the leakage magnetic flux becomes too low locally, making it difficult for sputtering to proceed, and protrusions called nodules may occur on the target surface, which may become the starting point of abnormal discharge called arcing. For this reason, it is more preferable that the target according to the embodiment of the present invention has less than one FeW phase with an inscribed circle diameter of 300 μm or more.
Here, the inscribed circle diameter in the present invention refers to the diameter of the circle that has the largest area (diameter) among the circles that can be drawn inside a certain contour shape and that touch at least one point of the contour. The inscribed circle diameter of the FeW phase in the present invention can be measured by photographing the FeW phase shown in dark gray in the backscattered electron image by a scanning electron microscope in an arbitrary field of view of 0.12 mm2 on the surface that will become the sputtering surface of the target. The number of FeW phases having an inscribed circle diameter of 400 μm or more can be obtained by observing one field of view of 0.12 mm2 on the surface that will become the sputtering surface and counting the number of FeW phases with an inscribed circle diameter of 400 μm or more that exist in that field of view. From the viewpoint of suppressing particle generation, the number of FeW phases having an inscribed circle diameter of 400 μm or more may be determined by observing a plurality of fields (e.g., five fields) of 0.12 mm2 on the surface to be sputtered, counting the number of FeW phases having an inscribed circle diameter of 400 μm or more present in each field, and averaging the results.
本発明の実施形態に係るターゲットは、０．１２ｍｍ２当たりで、１５μｍ以上の内接円直径を有するＷ相を１個未満とすることが好ましい。これにより、本発明のターゲットは、パーティクルの発生を抑制することができる。
ＷのＡｒイオンに対するスパッタリング率は、ＮｉやＦｅに比べて極端に低く、内接円直径が１５μｍ以上のＷ相が存在すると、ターゲット表面にＷ相の凸部が発生する場合があり、アーキングの起点となる虞がある。このため、本発明の実施形態に係るターゲットは、内接円直径が１０μｍ以上のＷ相を１個未満とすることがより好ましい。
ここで、本発明でいうＷ相の内接円直径は、ターゲットのスパッタ面となる面の、任意の０．１２ｍｍ２となる視野において、走査型電子顕微鏡による反射電子像の白色で示されるＷ相を撮影して測定することができる。そして、１５μｍ以上の内接円直径を有するＷ相の個数は、スパッタ面となる面で０．１２ｍｍ２となる１視野の観察を行ない、その視野に存在する内接円直径が１５μｍ以上のＷ相の個数をカウントすることで得られる。また、パーティクルの発生を抑制する観点から、１５μｍ以上の内接円直径を有するＷ相の個数は、スパッタ面となる面で０．１２ｍｍ２となる視野を複数視野（例えば５視野）で観察を行ない、各視野に存在する内接円直径が１５μｍ以上のＷ相の個数をカウントして、その平均値としてもよい。
In the target according to the embodiment of the present invention, it is preferable that the number of W phases having an inscribed circle diameter of 15 μm or more per 0.12 mm2 is less than one. Thereby, the target of the present invention can suppress the generation of particles.
The sputtering rate of W with respect to Ar ions is extremely low compared to Ni and Fe, and if a W phase with an inscribed circle diameter of 15 μm or more is present, a convex portion of the W phase may be generated on the target surface, which may become a starting point for arcing. For this reason, it is more preferable that the target according to the embodiment of the present invention has less than one W phase with an inscribed circle diameter of 10 μm or more.
Here, the inscribed circle diameter of the W phase in the present invention can be measured by photographing the W phase shown in white in a backscattered electron image by a scanning electron microscope in an arbitrary field of view of 0.12 mm2 on the surface to be sputtered of the target. The number of W phases having an inscribed circle diameter of 15 μm or more can be obtained by observing one field of view of 0.12 mm2 on the surface to be sputtered and counting the number of W phases having an inscribed circle diameter of 15 μm or more present in that field of view. In addition, from the viewpoint of suppressing the generation of particles, the number of W phases having an inscribed circle diameter of 15 μm or more can be obtained by observing multiple fields of view (e.g., five fields of view) of 0.12 mm2 on the surface to be sputtered, counting the number of W phases having an inscribed circle diameter of 15 μm or more present in each field of view, and averaging them.
本発明のターゲットは、例えば、粉末焼結法で得ることができる。具体的には、ＮｉＷ合金粉末とＦｅＷ合金粉末を混合した混合粉末を加圧焼結することにより得ることができる。各合金粉末の製造方法としては、合金溶湯を鋳造したインゴットを粉砕して作製する方法や、合金溶湯を不活性ガスにより噴霧することで粉末を形成するガスアトマイズ法によって作製することが可能である。中でも、不純物の混入が少なく、充填率が高く、焼結に適した球状粉末が得られるガスアトマイズ法を用いることが好ましい。ここで、球状粉末の酸化を抑制するためには、アトマイズガスとして不活性ガスであるＡｒガスもしくは窒素ガスを用いることが好ましい。
そして、加圧焼結としては、例えば、熱間静水圧プレス（ＨＩＰ）法、ホットプレス法、通電焼結法等を適用することができる。
The target of the present invention can be obtained, for example, by a powder sintering method. Specifically, the target can be obtained by pressure sintering a mixed powder obtained by mixing NiW alloy powder and FeW alloy powder. As a manufacturing method for each alloy powder, it is possible to manufacture the target by a method of crushing an ingot cast from an alloy melt, or a gas atomization method in which the alloy melt is sprayed with an inert gas to form a powder. Among them, it is preferable to use the gas atomization method, which has a small amount of impurities, a high filling rate, and can obtain spherical powder suitable for sintering. Here, in order to suppress oxidation of the spherical powder, it is preferable to use an inert gas such as Ar gas or nitrogen gas as the atomization gas.
The pressure sintering can be performed by, for example, a hot isostatic press (HIP) method, a hot press method, an electric current sintering method, or the like.
加圧焼結は、焼結温度７００～１３００℃、加圧圧力３０～２００ＭＰａ、１～１０時間の条件で行なうことが好ましい。
焼結温度は、７００℃以上にすることで、粉末の焼結を進行させることができ、空孔の発生を抑制することができる。また、焼結温度は、１３００℃以下にすることで、粉末の溶解を抑制できる。そして、空孔の発生を抑制しつつ、ＮｉＷ合金粉末とＦｅＷ合金粉末の拡散を抑制するためには、８５０～１０５０℃の温度で焼結することが好ましい。
また、加圧圧力は、３０ＭＰａ以上にすることで、焼結の進行を促進し、空孔の発生を抑制することができる。また、加圧圧力は、２００ＭＰａ以下にすることで、焼結時にターゲットへの残留応力の導入が抑制され、焼結後の割れの発生を抑制することができる。
また、焼結時間は、１時間以上にすることで、焼結の進行を促進し、空孔の発生を抑制することができる。また、焼結時間は、１０時間以下にすることで、製造効率の低下を抑制できる。
The pressure sintering is preferably carried out under conditions of a sintering temperature of 700 to 1300° C., a pressing pressure of 30 to 200 MPa, and a time of 1 to 10 hours.
By setting the sintering temperature at 700° C. or higher, the sintering of the powder can be promoted and the generation of voids can be suppressed. By setting the sintering temperature at 1300° C. or lower, the dissolution of the powder can be suppressed. In order to suppress the generation of voids while suppressing the diffusion of the NiW alloy powder and the FeW alloy powder, it is preferable to sinter at a temperature of 850 to 1050° C.
Furthermore, by setting the pressing pressure to 30 MPa or more, the progress of sintering can be promoted and the generation of voids can be suppressed, and by setting the pressing pressure to 200 MPa or less, the introduction of residual stress into the target during sintering can be suppressed, and the generation of cracks after sintering can be suppressed.
Moreover, by setting the sintering time to 1 hour or more, the progress of sintering can be promoted and the generation of voids can be suppressed, and by setting the sintering time to 10 hours or less, the decrease in manufacturing efficiency can be suppressed.
Ａｒガスを用いたガスアトマイズ法によって、原子比における組成式がＮｉ９６．９８Ｗ３．０２粉末とＦｅ９７．１２Ｗ２．８８粉末を製造した。得られた粉末をそれぞれ２５０μｍの篩にて粗粉を除去後、原子比における組成式がＮｉ８２Ｆｅ１５Ｗ３となるように、秤量した後にＶ型混合機で混合して混合粉末を得た。
そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。この焼結体を機械加工により直径１８０ｍｍ、厚さ７ｍｍの本発明例１となるターゲットを得た。
A gas atomization method using Ar gas was used to produce powders with a composition formula of Ni 96.98 W 3.02 and Fe 97.12 W 2.88 . After removing coarse powders from each of the obtained powders using a 250 μm sieve, the powders were weighed so that the composition formula in the atomic ratio was Ni 82 Fe 15 W 3 , and then mixed in a V-type mixer to obtain a mixed powder.
The mixed powder was then filled into a capsule made of soft iron and degassed and sealed at 450° C. for 4 hours. The capsule was then pressure-sintered by HIP at 950° C., 122 MPa, and 1 hour to produce a sintered body. The sintered body was machined to obtain a target having a diameter of 180 mm and a thickness of 7 mm, which was to be Example 1 of the present invention.
Ａｒガスを用いたガスアトマイズ法によって、原子比における組成式がＮｉ９６．２０Ｗ３．８０粉末とＦｅ９７．１２Ｗ２．８８粉末を製造した。得られた粉末をそれぞれ２５０μｍの篩にて粗粉を除去後、原子比における組成式がＮｉ９１．２５Ｆｅ５Ｗ３．７５となるように、秤量した後にＶ型混合機で混合して混合粉末を得た。
そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。この焼結体を機械加工により直径１８０ｍｍ、厚さ７ｍｍの本発明例２となるターゲットを得た。
A gas atomization method using Ar gas was used to produce powders with a composition formula of Ni 96.20 W 3.80 and Fe 97.12 W 2.88 . After removing coarse powders from each of the obtained powders using a 250 μm sieve, the powders were weighed so that the composition formula in atomic ratio was Ni 91.25 Fe 5 W 3.75 , and then mixed in a V-type mixer to obtain a mixed powder.
The mixed powder was then filled into a capsule made of soft iron and degassed and sealed at 450° C. for 4 hours. The capsule was then pressure-sintered by HIP at 950° C., 122 MPa, and 1 hour to produce a sintered body. The sintered body was machined to obtain a target having a diameter of 180 mm and a thickness of 7 mm, which was to be Example 2 of the present invention.
Ａｒガスを用いたガスアトマイズ法によって、原子比における組成式がＮｉ９６．２０Ｗ３．８０粉末とＦｅ９７．１２Ｗ２．８８粉末を製造した。得られた粉末をそれぞれ２５０μｍの篩にて粗粉を除去後、原子比における組成式がＮｉ５６．５８Ｆｅ４０Ｗ３．４２となるように、秤量した後にＶ型混合機で混合して混合粉末を得た。
そして、この混合粉末を軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、９５０℃、１２２ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。この焼結体を機械加工により直径１８０ｍｍ、厚さ７ｍｍの本発明例３となるターゲットを得た。
A gas atomization method using Ar gas was used to produce powders with a composition formula of Ni 96.20 W 3.80 and Fe 97.12 W 2.88 . After removing coarse powders from each of the obtained powders using a 250 μm sieve, the powders were weighed so that the composition formula in atomic ratio was Ni 56.58 Fe 40 W 3.42 , and then mixed in a V-type mixer to obtain a mixed powder.
The mixed powder was then filled into a capsule made of soft iron and degassed and sealed at 450° C. for 4 hours. The capsule was then pressure-sintered by HIP at 950° C., 122 MPa, and 1 hour to produce a sintered body. The sintered body was machined to obtain a target having a diameter of 180 mm and a thickness of 7 mm, which was to be Example 3 of the present invention.
Ａｒガスを用いたガスアトマイズ法によって、原子比における組成式がＮｉ８２Ｆｅ１５Ｗ３粉末を製造した。
得られた粉末を２５０μｍの篩にて粗粉を除去後、軟鉄製のカプセルに充填して、４５０℃、４時間の条件で脱ガス封止をした。そして、１２５０℃、１４６ＭＰａ、１時間の条件で、ＨＩＰによって上記カプセルを加圧焼結して、焼結体を作製した。この焼結体を機械加工により直径１８０ｍｍ、厚さ７ｍｍの比較例となるターゲットを得た。
Powder having a composition formula of Ni 82 Fe 15 W 3 in terms of atomic ratio was produced by a gas atomization method using Ar gas.
The obtained powder was sieved through a 250 μm sieve to remove coarse powder, then filled into a soft iron capsule and degassed and sealed at 450° C. for 4 hours. The capsule was then pressure-sintered by HIP at 1250° C., 146 MPa, and 1 hour to produce a sintered body. This sintered body was machined to obtain a target having a diameter of 180 mm and a thickness of 7 mm, which serves as a comparative example.
上記で作製した本発明例１～３および比較例のターゲットの漏洩磁束を以下の方法で測定した。先ず、馬蹄型永久磁石の上部にガウスメータを配置し、馬蹄型永久磁石とガウスメータの間にターゲットを置かない際の磁束を１００Ｇに設定する。次に、馬蹄型永久磁石とガウスメータとの間にターゲットを置いた際の中心の磁束を測定した。そして、ターゲットを置いた際の測定した磁束を上記で設定した１００Ｇで除して漏洩磁束とした。その結果を表１に示す。The leakage magnetic flux of the targets of the present invention examples 1 to 3 and the comparative example prepared above was measured by the following method. First, a gaussmeter was placed above the horseshoe-shaped permanent magnet, and the magnetic flux when no target was placed between the horseshoe-shaped permanent magnet and the gaussmeter was set to 100 G. Next, the magnetic flux at the center was measured when the target was placed between the horseshoe-shaped permanent magnet and the gaussmeter. The measured magnetic flux when the target was placed was then divided by the 100 G set above to obtain the leakage magnetic flux. The results are shown in Table 1.
上記で作製した各ターゲットの端材から１０ｍｍ×１０ｍｍ×５ｍｍの試験片を採取し、１０ｍｍ×１０ｍｍとなる面にバフ研磨を施した。本発明例１および比較例の試験片は、株式会社日立ハイテクノロジーズの走査型電子顕微鏡Ｓ－３６００Ｎを用いて、本発明例２および本発明例３の試験片は、日本電子株式会社の走査型電子顕微鏡ＪＳＭ－６６１０ＬＡを用いて金属組織観察を行なった。また、本発明例１～３および比較例の試験片について、エネルギー分散型Ｘ線分光法により構成される相の存在を確認した。金属組織観察は、各試料のスパッタ面となる面の走査型電子顕微鏡の反射電子像で、任意の視野のうち、０．１２ｍｍ２となる視野を１視野観察し、視野内に存在するＦｅＷ相およびＷ相の内接円直径を測定し、内接円直径が４００μｍ以上のＦｅＷ相と、内接円直径が１５μｍ以上のＷ相の個数をカウントした。
本発明例１～３となるターゲットのエロ―ジョン面となる面の金属組織を図１～図３に、また、比較例となるターゲットのエロ―ジョン面となる面の金属組織を図４に示す。
A test piece measuring 10 mm x 10 mm x 5 mm was taken from the end material of each target prepared above, and the surface measuring 10 mm x 10 mm was subjected to buffing. The test pieces of the present invention example 1 and the comparative example were observed for metal structure using a scanning electron microscope S-3600N manufactured by Hitachi High-Technologies Corporation, and the test pieces of the present invention example 2 and the present invention example 3 were observed for metal structure using a scanning electron microscope JSM-6610LA manufactured by JEOL Ltd. In addition, the presence of the phases constituted by the test pieces of the present invention examples 1 to 3 and the comparative example was confirmed by energy dispersive X-ray spectroscopy. The metal structure observation was performed by observing one field of view of 0.12 mm2 out of any field of view using a backscattered electron image of a scanning electron microscope of the surface that would be the sputtered surface of each sample, measuring the inscribed circle diameter of the FeW phase and the W phase present in the field of view, and counting the number of FeW phases with an inscribed circle diameter of 400 μm or more and W phases with an inscribed circle diameter of 15 μm or more.
The metal structures of the eroded surfaces of the targets of Examples 1 to 3 of the present invention are shown in FIGS. 1 to 3, and the metal structure of the eroded surface of the target of the comparative example is shown in FIG.
本発明例１～３となるターゲットは、図１～３に示すように、いずれも、薄灰色で示されるＮｉＷのマトリックス相に、濃灰色で示されるＦｅＷ相が分散しており、０．１２ｍｍ２となる視野において、４００μｍ以上の内接円直径を有するＦｅＷ相はなく、白色で示される１５μｍ以上の内接円直径を有するＷ相もなく、５．０％以上という高い漏洩磁束が得られていた。
一方、比較例のターゲットは、図４に示すように、ＮｉＦｅＷ相からなり、漏洩磁束が５．０％未満という低い値を示したことを確認した。
As shown in FIGS. 1 to 3, in the targets of Examples 1 to 3 of the present invention, the FeW phase shown in dark gray was dispersed in the NiW matrix phase shown in light gray, and in a field of view of 0.12 mm2 , there was no FeW phase having an inscribed circle diameter of 400 μm or more, and no W phase having an inscribed circle diameter of 15 μm or more shown in white, and a high leakage magnetic flux of 5.0% or more was obtained.
On the other hand, it was confirmed that the target of the comparative example was made of a NiFeW phase as shown in FIG. 4, and exhibited a low leakage flux of less than 5.0%.
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| CN104651788A (en) | 2013-11-21 | 2015-05-27 | 安泰科技股份有限公司 | Ni-Fe-W alloy target and manufacturing method thereof |
| JP2016145394A (en) | 2015-02-09 | 2016-08-12 | 山陽特殊製鋼株式会社 | Ni-based target material with excellent sputtering properties |
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| SG172268A1 (en) * | 2009-04-17 | 2011-07-28 | Jx Nippon Mining & Metals Corp | Barrier film for semiconductor wiring, sintered compact sputtering target and method of producing the sputtering target |
| TWI387661B (en) * | 2009-07-22 | 2013-03-01 | China Steel Corp | Manufacturing method of nickel alloy target |
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