JP4427792B2 - Co alloy target material for magnetic recording media - Google Patents
Co alloy target material for magnetic recording media Download PDFInfo
- Publication number
- JP4427792B2 JP4427792B2 JP2004221649A JP2004221649A JP4427792B2 JP 4427792 B2 JP4427792 B2 JP 4427792B2 JP 2004221649 A JP2004221649 A JP 2004221649A JP 2004221649 A JP2004221649 A JP 2004221649A JP 4427792 B2 JP4427792 B2 JP 4427792B2
- Authority
- JP
- Japan
- Prior art keywords
- phase
- target material
- alloy
- magnetic recording
- εco
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000013077 target material Substances 0.000 title claims description 50
- 229910000531 Co alloy Inorganic materials 0.000 title claims description 39
- 229910052758 niobium Inorganic materials 0.000 claims description 12
- 229910052721 tungsten Inorganic materials 0.000 claims description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 73
- 239000000843 powder Substances 0.000 description 18
- 229910000765 intermetallic Inorganic materials 0.000 description 16
- 239000000203 mixture Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- 239000003870 refractory metal Substances 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 239000002184 metal Substances 0.000 description 9
- 229910052715 tantalum Inorganic materials 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910000599 Cr alloy Inorganic materials 0.000 description 2
- 229910000943 NiAl Inorganic materials 0.000 description 2
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229910004356 Ti Raw Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000005300 metallic glass Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Description
本発明は、例えば磁気記録媒体の非磁性基板と磁性層の下地層との間に形成されるシード層の形成に用いられるＣｏ合金ターゲット材に関するものである。 The present invention relates to a Co alloy target material used, for example, for forming a seed layer formed between a nonmagnetic substrate of a magnetic recording medium and an underlayer of a magnetic layer.
ハードディスクドライブ等に利用される磁気記録媒体においては、記録層であるＣｏ系磁性層で高密度な磁気記録が可能となるように発展してきており、その一つの手段として、磁性層の形成にはエピタキシャル成長が利用されている。磁性層をエピタキシャル成長させるため、磁気記録媒体の基板と上記磁性層の間に構成される下地層の格子定数、結晶配向性および膜の均一性の改良が行われている。
例えば、Ｃｏ系磁性層は六方最密充填構造であるため、磁化容易方向、すなわちＣ軸の格子定数とよく整合する、純ＣｒおよびＣｒ合金が下地層として主に用いられている。
Magnetic recording media used in hard disk drives and the like have been developed so that high-density magnetic recording is possible with a Co-based magnetic layer as a recording layer. Epitaxial growth is used. In order to epitaxially grow the magnetic layer, the lattice constant, crystal orientation, and film uniformity of the underlayer formed between the magnetic recording medium substrate and the magnetic layer have been improved.
For example, since the Co-based magnetic layer has a hexagonal close-packed structure, pure Cr and a Cr alloy that match well with the easy magnetization direction, that is, the lattice constant of the C axis, are mainly used as the underlayer.
磁気記録媒体の下地膜に関しては、Ｂ２規則格子金属間化合物を下地膜とする構造を採用することにより高保磁力および低ノイズの磁気記録媒体が得られることが報告されている（例えば、特許文献１参照）。
特に、Ｃｏ系磁性層との相性が良いＣｒ系の下地膜の更に下層として、微細なＢ２規則格子金属間化合物のシード層を形成しておけば、下地層となるＣｒ系の層をエピタキシャル成長させることができ、微細なＣｒ系下地膜を形成することが出来る。これによって、その上層となる磁性層も下地層の微細状態を反映したエピタキシャル成長を起こさせることが出来、高保磁力、低ノイズとなるのである。
As for the underlayer of the magnetic recording medium, it has been reported that a magnetic recording medium having a high coercive force and a low noise can be obtained by adopting a structure in which a B2 ordered lattice intermetallic compound is used as the underlayer (for example, Patent Document 1). reference).
In particular, if a seed layer of a fine B2 ordered lattice intermetallic compound is formed as a lower layer of a Cr-based undercoating film having good compatibility with the Co-based magnetic layer, a Cr-based layer as an underlayer is epitaxially grown. And a fine Cr base film can be formed. Thereby, the magnetic layer as an upper layer can also cause epitaxial growth reflecting the fine state of the underlayer, resulting in high coercive force and low noise.
ＮｉＡｌに代表されるＢ２規則格子金属間化合物のシード層は、下地層として用いられる純Ｃｒ層やＣｒ合金層およびＣｏ系磁性層との整合性が良好であることを確認されているが、近年の磁気記録媒体の高記録密度化に伴い、さらなる高記録密度化を達成する手段が求められている。
そこで、ＮｉＡｌやＲｕＡｌといったＢ２規則格子金属間化合物のシード層に替えて、アモルファスまたは微結晶金属を形成するものとしてＮｂ、Ｖ、Ｍｏ、Ｗ、Ｔｉのいずれか１種類以上の元素にＮｉ、Ｃｏ、Ｆｅ、Ｃｕ等を添加した合金膜が提案されている（例えば、特許文献２参照）。
Therefore, in place of the seed layer of B2 ordered lattice intermetallic compound such as NiAl or RuAl, Ni, Co, or Nb, V, Mo, W, or Ti is used as an element to form amorphous or microcrystalline metal. An alloy film to which Fe, Cu, or the like is added has been proposed (see, for example, Patent Document 2).
上述のアモルファス等のシード層は、一般的にスパッタリング法により形成されており、アモルファスや微結晶を形成する薄膜の組成とほぼ同一の組成を有するターゲット材が必要になる。特に、アモルファスや微結晶を形成する合金組成として有効と考えられるＣｏにＮｂ、Ｗ等の高融点金属元素を添加したＣｏ合金でターゲット材を作製する方法として、溶解鋳造法、粉末焼結法等の方法が考えられる。しかし、高融点金属元素を多量に添加したＣｏ合金を溶解鋳造法で作製しようとする場合には、合金の融点が高いためにＣｏ合金インゴットを作製するのが困難であるという問題がある。また、本願発明者等が、Ｃｏ粉末と高融点金属粉末とを混合後に加圧焼結する粉末冶金法によって作製することを試みたところ、作製したＣｏ合金の焼結体を機械加工する場合に加工が困難であるという問題が発生した。
本発明の目的は、上記の問題を解決し、磁気記録媒体のシード層を形成するためのＣｏ合金ターゲット材を安定的に提供することである。
The above-described seed layer such as amorphous is generally formed by a sputtering method, and a target material having almost the same composition as that of the thin film forming the amorphous or microcrystal is required. In particular, as a method for producing a target material with a Co alloy in which a refractory metal element such as Nb or W is added to Co, which is considered to be effective as an alloy composition for forming an amorphous or microcrystal, a melt casting method, a powder sintering method, etc. Can be considered. However, when a Co alloy to which a large amount of a refractory metal element is added is to be produced by the melt casting method, there is a problem that it is difficult to produce a Co alloy ingot due to the high melting point of the alloy. In addition, when the inventors of the present application tried to produce by a powder metallurgy method in which Co powder and refractory metal powder were mixed and sintered under pressure, when machining the sintered body of the produced Co alloy, The problem that processing was difficult occurred.
An object of the present invention is to solve the above problems and to stably provide a Co alloy target material for forming a seed layer of a magnetic recording medium.
本発明者等は、上記の問題を解決するために、高融点金属元素を含有するＣｏ合金ターゲット材の金属組織の構成を鋭意検討した結果、Ｃｏと高融点金属元素との金属間化合物の硬度が高いために、加工性を阻害していることを発見した。そこで、ターゲット材組織中にＣｏと高融点金属元素との金属間化合物ではない金属Ｃｏ相であるαＣｏ相あるいはεＣｏ相を残存させることで加工性が飛躍的に向上することを見出し本発明に到達した。
すなわち、本発明は、（Ｎｂ、Ｍｏ、Ｗ、Ｔｉ）から選択される１種の元素を４０〜７０原子％含有し、残部Ｃｏ及び不可避的不純物とからなるＣｏ合金ターゲット材において、ターゲット材の組織中にαＣｏ相あるいはεＣｏ相が残存している磁気記録媒体用Ｃｏ合金ターゲット材である。
In order to solve the above problems, the present inventors have intensively studied the structure of the metal structure of the Co alloy target material containing a refractory metal element, and as a result, the hardness of the intermetallic compound of Co and the refractory metal element. It has been found that processability is hindered due to its high value. Therefore, the present inventors have found that workability is dramatically improved by leaving an αCo phase or εCo phase, which is a metallic Co phase that is not an intermetallic compound of Co and a refractory metal element, in the target material structure. did.
That is, the present invention provides a Co alloy target material containing 40 to 70 atomic% of one element selected from (Nb , Mo, W, Ti), and the balance Co and unavoidable impurities. This is a Co alloy target material for magnetic recording media in which an αCo phase or an εCo phase remains in the structure .
好ましくは、ターゲット材のスパッタ面の断面ミクロ組織におけるαＣｏ相あるいはεＣｏ相の最大長径が５００μｍ以下である磁気記録媒体用Ｃｏ合金ターゲット材である。
また、好ましくは、ターゲット材のスパッタ面の断面ミクロ組織において、断面積1ｍｍ２の視野においてαＣｏ相あるいはεＣｏ相の面積率が５％以上である磁気記録媒体用Ｃｏ合金ターゲット材である。
また、好ましくは、ショア硬さが９５ＨＳ以下である磁気記録媒体用Ｃｏ合金ターゲット材である。
Preferably, it is a Co alloy target material for magnetic recording media in which the maximum major axis of the αCo phase or εCo phase in the cross-sectional microstructure of the sputtering surface of the target material is 500 μm or less.
In addition, a Co alloy target material for a magnetic recording medium in which the area ratio of the αCo phase or the εCo phase is 5% or more in a field of view having a cross-sectional area of 1 mm 2 in the cross-sectional microstructure of the sputtering surface of the target material is preferable.
Further, a Co alloy target material for a magnetic recording medium, preferably having a Shore hardness of 95 HS or less.
本発明により、磁気記録媒体のシード層を形成するＣｏ合金ターゲット材を加工性よく実現でき、高保磁力と低ノイズ特性を有する磁気記録媒体を実現できる。 The present invention, a Co alloy target material for forming a seed layer of a magnetic recording medium workability good realized, can realize a magnetic recording medium having a high coercive magnetic force and low noise characteristics.
本発明の重要な特徴は、特定の高融点金属元素を添加したＣｏ合金ターゲット材を加工性の観点から検証した結果、ターゲット材の金属組織中に、Ｃｏと高融点金属元素との金属間化合物相や高融点金属の純金属相あるいはその固溶体相で構成される単体相以外に金属Ｃｏ相であるαＣｏ相あるいはεＣｏ相を残存させることにより、加工性を向上させた点にある。
以下に本発明の詳細に関して説明する。
An important feature of the present invention is that, as a result of verifying a Co alloy target material added with a specific refractory metal element from the viewpoint of workability, an intermetallic compound of Co and a refractory metal element is present in the metal structure of the target material. In addition to a single phase composed of a pure phase of a refractory metal or a high melting point metal or a solid solution phase thereof, the αCo phase or εCo phase, which is a metallic Co phase, is left to improve workability.
Details of the present invention will be described below.
（Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｔｉ）から選択される１種以上の元素とＣｏからなるＣｏ合金は、スパッタした際に金属間化合物を結晶生成の核として微結晶の金属薄膜あるいはアモルファスの金属薄膜を容易に形成することが可能である。このため、Ｃｒ系下地層の配向面を均一にでき、さらにＣｏ系磁性層を微細化することで磁気特性を向上することが可能であるためシード層として利用されている。そして、上記組成のシード層を形成するためには、同一組成のＣｏ合金ターゲット材が使用される。このＣｏ合金の組成系は上述の通り結晶生成の核となる金属間化合物を形成しやすいため、シード層として利用されているが、ターゲット材の金属組織においても、例えば、Ｃｏ７Ｎｂ６、Ｃｏ７Ｔａ６、Ｃｏ７Ｍｏ６、Ｃｏ７Ｗ６、ＣｏＴｉ２といったＣｏ、Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｔｉの単体相に比べて非常に硬度の高い金属間化合物相が形成される。 A Co alloy composed of one or more elements selected from (Nb, Ta, Mo, W, Ti) and Co is a microcrystalline metal thin film or amorphous metal using an intermetallic compound as a nucleus for crystal formation when sputtered. It is possible to easily form a thin film. For this reason, the orientation surface of the Cr-based underlayer can be made uniform, and the magnetic characteristics can be improved by miniaturizing the Co-based magnetic layer, so that it is used as a seed layer. In order to form a seed layer having the above composition, a Co alloy target material having the same composition is used. The composition system of this Co alloy is used as a seed layer because it easily forms an intermetallic compound as a nucleus for crystal formation as described above, but also in the metal structure of the target material, for example, Co 7 Nb 6 , Co Compared with a single phase of Co, Nb, Ta, Mo, W, and Ti, such as 7 Ta 6 , Co 7 Mo 6 , Co 7 W 6 , and CoTi 2 , an intermetallic compound phase having extremely high hardness is formed.
特に、（Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｔｉ）から選択される１種以上の高融点金属元素を２５〜９０原子％含有し、残部実質的にＣｏからなるＣｏ合金組成においては、単純に原料粉末同士を焼結するとこれらの金属間化合物相とＮｂ、Ｔａ、Ｍｏ、Ｗ、Ｔｉの高融点金属の単独相とで形成される合金組織となる可能性が高く、切削や研磨といった機械加工が極めて困難になる。そして、上記の成分組成は、平衡状態において金属Ｃｏ相であるαＣｏ相あるいはεＣｏ相が残存しない成分組成であるため、この領域においてターゲット材の組織制御を行うことが重要である。
そこで、安定的に上記組成のＣｏ合金ターゲット材を製造するためには、金属Ｃｏの単独相で比較的加工性の良好なαＣｏ相あるいはεＣｏ相をターゲット材の組織中に残存させるように組織を制御することで、加工性を向上させる必要がある。
In particular, in a Co alloy composition containing 25 to 90 atomic% of one or more refractory metal elements selected from (Nb, Ta, Mo, W, Ti), and the balance being substantially Co, the raw material is simply When powders are sintered together, there is a high possibility that an alloy structure formed by these intermetallic compound phases and a single phase of a refractory metal of Nb, Ta, Mo, W, Ti will be obtained. It becomes extremely difficult. The component composition described above is a component composition in which the αCo phase or εCo phase, which is a metallic Co phase, does not remain in an equilibrium state. Therefore, it is important to control the structure of the target material in this region.
Therefore, in order to stably produce a Co alloy target material having the above composition, a structure is formed so that an αCo phase or an εCo phase having a relatively good workability in a single phase of metallic Co remains in the structure of the target material. It is necessary to improve workability by controlling.
また、平衡状態において金属Ｃｏ相であるαＣｏ相あるいはεＣｏ相がより残存しない成分組成であるため、より好ましくは、Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｔｉの含有量は４０〜７０原子％である。 Moreover, since it is a component composition in which the αCo phase or εCo phase, which is a metallic Co phase, does not remain in an equilibrium state, the content of Nb, Ta, Mo, W, and Ti is more preferably 40 to 70 atomic%.
また、本発明においては、ターゲット材のスパッタ面の断面ミクロ組織におけるαＣｏ相あるいはεＣｏ相の最大長径が５００μｍ以下である。それは、ターゲット材への加工を施す上では、その金属組織においてはαＣｏ相あるいはεＣｏ相がより微細に均一分散して残存していることが望ましいためである。 In the present invention, the maximum major axis of the αCo phase or εCo phase in the cross-sectional microstructure of the sputtering surface of the target material is 500 μm or less. This is because in processing the target material, it is desirable that the αCo phase or εCo phase remain finely and uniformly dispersed in the metal structure.
また、本発明においては、ターゲット材のスパッタ面の断面ミクロ組織において、断面積1ｍｍ２の視野においてαＣｏ相あるいはεＣｏ相の面積率が５％以上であることが望ましい。それは、ターゲット材への加工を施す上では、ターゲット材の全域に亘ってαＣｏ相あるいはεＣｏ相が均一分散して残存することが望ましいため、上記の面積率を有することが加工性の観点からより望ましいためである。 In the present invention, in the cross-sectional microstructure of the sputtering surface of the target material, it is desirable that the area ratio of the αCo phase or the εCo phase is 5% or more in a visual field having a cross-sectional area of 1 mm 2 . That is, in processing the target material, it is desirable that the αCo phase or the εCo phase remain uniformly dispersed throughout the entire target material, so that the above area ratio is more preferable from the viewpoint of workability. This is desirable.
また、本発明においては、ターゲット材のショア硬さが９５ＨＳ以下であることが好ましい。それは、ターゲット材を加工する超硬およびセラミクス系の切削チップのショア硬さが通常１００ＨＳ前後であり、この切削チップよりも硬度を下げる必要があるためである。切削チップよりも硬度が高くなった場合、ターゲットの強度が切削チップの強度を上回り加工が困難となる為、出来る限りターゲット材のショア硬さを低下させることが好ましい。
なお、ショア硬さとは、ＪＩＳ−Ｚ−２２４６にて定義されるダイヤモンドハンマーを一定高さから落下させ、その跳ね上がり高さに比例する値として求められる硬さをいう。
In the present invention, the Shore hardness of the target material is preferably 95 HS or less. This is because the shore hardness of the carbide and ceramic cutting tips for processing the target material is usually around 100 HS, and the hardness needs to be lower than that of the cutting tips. When the hardness is higher than the cutting tip, the strength of the target exceeds the strength of the cutting tip and it becomes difficult to process. Therefore, it is preferable to reduce the Shore hardness of the target material as much as possible.
The Shore hardness refers to the hardness obtained as a value proportional to the jumping height of a diamond hammer defined by JIS-Z-2246, dropped from a certain height.
また、本発明のターゲット材を作製するための好ましい方法を以下に説明する。
本発明のターゲット材では、強制的にαＣｏ相あるいはεＣｏ相を残存させるために、粉末焼結法が用いられるが、特にαＣｏ相あるいはεＣｏ相を残存させるためには、粉末焼結法に用いられるＣｏ原料粉末の平均粒径は４５μｍ以上とすることが好ましい。それは、Ｃｏ原料粉末の平均粒径が４５μｍよりも微細な場合には、焼結時の原料粉末の固相拡散反応により金属Ｃｏ相であるαＣｏ相あるいはεＣｏ相として残存せずに、金属間化合物相となる可能性が高くなるためである。また、高融点金属元素である（Ｎｂ、Ｔａ、Ｍｏ、Ｗ、Ｔｉ）から選択される１種以上の元素が含まれるため、焼結を効率よく行うためには、ホットプレスや熱間静水圧プレス等の加圧焼結法を利用することが好ましい。特に、熱間静水圧プレスの条件としては、十分な焼結密度が効率良く得られるので温度９００℃以上、圧力１００ＭＰａ以上および保持時間１時間以上とすることが望ましい。
Moreover, the preferable method for producing the target material of this invention is demonstrated below.
In the target material of the present invention, a powder sintering method is used in order to force the αCo phase or εCo phase to remain, but in particular, in order to leave the αCo phase or εCo phase, it is used in the powder sintering method. The average particle diameter of the Co raw material powder is preferably 45 μm or more. When the average particle size of the Co raw material powder is finer than 45 μm, the intermetallic compound does not remain as an αCo phase or εCo phase, which is a metallic Co phase, due to a solid phase diffusion reaction of the raw material powder during sintering. This is because the possibility of becoming a phase increases. In addition, since one or more elements selected from refractory metal elements (Nb, Ta, Mo, W, Ti) are included, hot pressing or hot isostatic pressure is required for efficient sintering. It is preferable to use a pressure sintering method such as a press. In particular, the conditions for hot isostatic pressing are preferably a temperature of 900 ° C. or higher, a pressure of 100 MPa or higher, and a holding time of 1 hour or longer because a sufficient sintered density can be obtained efficiently.
原料粉末として、平均粒径７０μｍのＣｏ原料粉末、平均粒径９５μｍのＮｂ原料粉末、平均粒径１８μｍのＴａ原料粉末、平均粒径９μｍのＭｏ原料粉末、平均粒径８μｍのＷ原料粉末および平均粒径１２０μｍのＴｉ原料粉末を準備した。それぞれ、表１に示す成分組成となるように秤量した後、Ｖ型混合機で混合した混合粉末を軟鋼製の加圧容器に充填し、真空脱気後に封止した。この混合粉末を充填した加圧容器を、Ｎｂ、Ｔａ、Ｍｏ、Ｗの元素が含まれる組成の場合、温度１３００℃、圧力１３０ＭＰａ、１時間の条件で、また、Ｔｉが含まれる組成の場合、温度９００℃、圧力１００ＭＰａ、１時間の条件で熱間静水圧プレスにより加圧焼結して焼結体を作製した。その後、この焼結体を機械加工により直径１８０ｍｍ×１０ｍｍのＣｏ合金ターゲット材を得た。 As raw material powder, Co raw material powder with an average particle size of 70 μm, Nb raw material powder with an average particle size of 95 μm, Ta raw material powder with an average particle size of 18 μm, Mo raw material powder with an average particle size of 9 μm, W raw material powder with an average particle size of 8 μm, and average A Ti raw material powder having a particle size of 120 μm was prepared. After weighing each so as to have the component composition shown in Table 1, the mixed powder mixed by a V-type mixer was filled in a pressure vessel made of mild steel, and sealed after vacuum deaeration. When the pressure vessel filled with this mixed powder is a composition containing elements of Nb, Ta, Mo, W, under conditions of a temperature of 1300 ° C., a pressure of 130 MPa, 1 hour, and a composition containing Ti, A sintered body was produced by pressure sintering by hot isostatic pressing under conditions of a temperature of 900 ° C. and a pressure of 100 MPa for 1 hour. Thereafter, a Co alloy target material having a diameter of 180 mm × 10 mm was obtained by machining the sintered body.
また、比較例として、平均粒径６μｍのＣｏ原料粉末と平均粒径８μｍのＷ原料粉末を原子比率で５０：５０になるように秤量した混合粉末を準備した。その後の工程は、上記と同様にして焼結体を作製した。このＣｏ合金焼結体を直径１８０ｍｍ×１０ｍｍに加工するため、住友電気工業製ＷＸ１２０、ＢＮ６００、およびサンドビック社製６７０、６０８０の切削チップを用い、回転数２３〜２６５ｒｐｍ、送り０．０５〜０．５ｍｍ／ｒｐｍ、切り込み０．１〜０．５ｍｍの切削条件にて旋盤加工を施したが、切削チップが欠ける、焼結体が割れる等の問題により上記の所望寸法のターゲット材に加工することができなかった。 As a comparative example, a mixed powder was prepared by weighing Co raw material powder having an average particle diameter of 6 μm and W raw material powder having an average particle diameter of 8 μm so as to have an atomic ratio of 50:50. Subsequent processes produced the sintered compact like the above. In order to process this Co alloy sintered body to a diameter of 180 mm × 10 mm, a cutting tip of WX120, BN600 manufactured by Sumitomo Electric Industries, Ltd. Lathe was machined under cutting conditions of 5 mm / rpm and a cutting depth of 0.1 to 0.5 mm, but it was processed into a target material of the above desired dimensions due to problems such as chipping of chips and cracking of the sintered body. I could not.
上記で得た各々のＣｏ合金ターゲット材およびＣｏ合金焼結体からそれぞれ１５ｍｍ角の試験片を採取した。各試験片をＸ線回折法で相同定を行い、αＣｏ相あるいはεＣｏ相の有無を確認した結果、表１の試料Ｎｏ．１〜７の本発明例や参考例においてはその存在を確認できたが、試料Ｎｏ．８では確認できなかった。また、各試験片から走査型電子顕微鏡（ＳＥＭ）により１００倍に拡大したミクロ組織を観察し、画像解析によりαＣｏ相およびεＣｏ相、金属間化合物相、添加元素のＮｂ、Ｔａ、Ｍｏ、ＷおよびＴｉの各単体相の面積率を評価した。また、同時に上記のミクロ組織でαＣｏ相あるいはεＣｏ相の最大長径を測定した。さらに、ＪＩＳ−Ｚ−２２４６に基づき、各々のＣｏ合金ターゲット材のショア硬さを測定した。以上、各Ｃｏ合金ターゲット材およびＣｏ合金焼結体の各相の面積率の評価結果を表１に、αＣｏ相あるいはεＣｏ相の最大長径およびショア硬さの測定結果を表２に示す。 A test piece of 15 mm square was collected from each Co alloy target material and Co alloy sintered body obtained above. Each test piece was phase-identified by X-ray diffractometry, and the presence or absence of αCo phase or εCo phase was confirmed. In the present invention examples and reference examples of Nos. 1 to 7, the existence thereof was confirmed. It was not confirmed in 8. Further, the microstructure which was magnified 100 times by a scanning electron microscope (SEM) was observed from each test piece, and αCo phase and εCo phase, intermetallic compound phase, additive elements Nb, Ta, Mo, W and The area ratio of each single phase of Ti was evaluated. At the same time, the maximum major axis of the αCo phase or εCo phase was measured with the above microstructure. Furthermore, the shore hardness of each Co alloy target material was measured based on JIS-Z-2246. Table 1 shows the evaluation results of the area ratio of each phase of each Co alloy target material and Co alloy sintered body, and Table 2 shows the measurement results of the maximum major axis and shore hardness of the αCo phase or εCo phase.
表１から、本発明例の試料Ｎｏ．１〜３および６〜７のＣｏ合金ターゲット材においては、αＣｏ相あるいはεＣｏ相が残存していることが分かる。そして、表２からはαＣｏ相あるいはεＣｏ相の最大長径が３７５μｍ以下、Ｃｏ合金ターゲット材のショア硬さが９０ＨＳ以下であることが分かる。
一方、比較例である試料Ｎｏ．８のＣｏ合金焼結体では、αＣｏ相あるいはεＣｏ相が存在せず、ＣｏＷの金属間化合物相が面積率で９７％を占め、ショア硬さも１１０ＨＳであった。
From Table 1, Sample No. It can be seen that in the Co alloy target materials 1 to 3 and 6 to 7 , the αCo phase or the εCo phase remains. Table 2 shows that the maximum major axis of the αCo phase or εCo phase is 375 μm or less, and the Shore hardness of the Co alloy target material is 90 HS or less.
On the other hand, sample No. which is a comparative example. In the Co alloy sintered body of No. 8, there was no αCo phase or εCo phase, the intermetallic compound phase of CoW accounted for 97% in area ratio, and the Shore hardness was 110 HS.
また、本発明のＣｏ合金ターゲット材の代表的なミクロ組織を示す例として、表１の試料Ｎｏ．１、参考例の試料Ｎｏ．５のＳＥＭで１００倍に拡大したミクロ組織を撮影した写真を、それぞれ図１および２に示す。さらに、比較例の試料Ｎｏ．８のＳＥＭで４００倍に拡大したミクロ組織を撮影した写真を図３に示す。
これらのミクロ組織写真を観察すると、本発明例の図１および参考例の図２においては、濃灰色部で示されるαＣｏ相かεＣｏ相の金属Ｃｏ相が残存しており、淡灰色部で示されるＣｏＷ、ＣｏＴａの金属間化合物相、白色部で示されるＷ単体相、Ｔａ単体相とのそれぞれ３相を有していることが分かる。一方、比較例の図３では、４００倍に拡大したミクロ組織を撮影した写真においても、αＣｏ相あるいはεＣｏ相は確認できず、白色部で示されるＷ相と淡灰色部で示されるＣｏＷの金属間化合物相からなっていることが分かる。
In addition, as an example showing a typical microstructure of the Co alloy target material of the present invention, sample No. 1 Sample No. of Reference Example FIGS. 1 and 2 show photographs of microstructures magnified 100 times with 5 SEM, respectively. Furthermore, sample No. of the comparative example. FIG. 3 shows a photograph of a microstructure magnified 400 times with 8 SEM.
When these microstructure photographs are observed, in FIG. 1 of the present invention example and FIG. 2 of the reference example, the αCo phase or the εCo phase metal Co phase indicated by the dark gray portion remains and is indicated by the light gray portion. It can be seen that each has three phases, ie, an intermetallic compound phase of CoW and CoTa, a W single phase indicated by a white portion, and a Ta single phase. On the other hand, in FIG. 3 of the comparative example, the αCo phase or the εCo phase cannot be confirmed even in a photograph of the microstructure magnified 400 times, and the W phase indicated by the white part and the CoW metal indicated by the light gray part It can be seen that it consists of an intermetallic compound phase.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004221649A JP4427792B2 (en) | 2004-07-29 | 2004-07-29 | Co alloy target material for magnetic recording media |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004221649A JP4427792B2 (en) | 2004-07-29 | 2004-07-29 | Co alloy target material for magnetic recording media |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2006037192A JP2006037192A (en) | 2006-02-09 |
| JP2006037192A5 JP2006037192A5 (en) | 2007-07-26 |
| JP4427792B2 true JP4427792B2 (en) | 2010-03-10 |
Family
ID=35902499
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2004221649A Expired - Lifetime JP4427792B2 (en) | 2004-07-29 | 2004-07-29 | Co alloy target material for magnetic recording media |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4427792B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5248000B2 (en) * | 2006-09-11 | 2013-07-24 | 山陽特殊製鋼株式会社 | CoW-based target material and method for manufacturing the same |
| US20080170959A1 (en) * | 2007-01-11 | 2008-07-17 | Heraeus Incorporated | Full density Co-W magnetic sputter targets |
| JP2015193909A (en) * | 2014-03-25 | 2015-11-05 | Jx日鉱日石金属株式会社 | Sputtering target, manufacturing method thereof, and film formed by sputtering method |
| CN121889531A (en) * | 2024-04-30 | 2026-04-17 | Ｊｘ金属株式会社 | Sputtering component |
-
2004
- 2004-07-29 JP JP2004221649A patent/JP4427792B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2006037192A (en) | 2006-02-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4016399B2 (en) | Method for producing Fe-Co-B alloy target material | |
| US20080083616A1 (en) | Co-Fe-Zr BASED ALLOY SPUTTERING TARGET MATERIAL AND PROCESS FOR PRODUCTION THEREOF | |
| US8523976B2 (en) | Metal powder | |
| JP2020114948A (en) | Mixed powder for metal lamination molding | |
| JP5472688B2 (en) | Fe-Co alloy sputtering target material and method for producing the same | |
| JP5305137B2 (en) | Ni-W sintered target material for forming Ni alloy intermediate layer of perpendicular magnetic recording medium | |
| JP2008189996A (en) | Co-Fe-BASED ALLOY SPUTTERING TARGET MATERIAL AND METHOD FOR PRODUCING THE SAME | |
| JP4953082B2 (en) | Co-Fe-Zr alloy sputtering target material and method for producing the same | |
| JP5370917B2 (en) | Method for producing Fe-Co-Ni alloy sputtering target material | |
| JP5359890B2 (en) | Fe-Co alloy sputtering target material for soft magnetic film formation | |
| EP3515636A1 (en) | Cemented carbide material | |
| JP2005320627A (en) | Co ALLOY TARGET AND ITS PRODUCTION METHOD, SOFT MAGNETIC FILM FOR PERPENDICULAR MAGNETIC RECORDING AND PERPENDICULAR MAGNETIC RECORDING MEDIUM | |
| JP2010111943A (en) | Method for producing sputtering target material | |
| JP4919162B2 (en) | Fe-Co alloy sputtering target material and method for producing Fe-Co alloy sputtering target material | |
| JP2009191359A (en) | Fe-Co-Zr BASED ALLOY TARGET MATERIAL | |
| JP2008260970A (en) | SINTERED SPUTTERING-TARGET MATERIAL OF Co-Zr-BASED ALLOY AND MANUFACTURING METHOD THEREFOR | |
| JP6581780B2 (en) | Ni-based target material with excellent sputtering properties | |
| JP4427792B2 (en) | Co alloy target material for magnetic recording media | |
| JP2018188726A (en) | Sputtering target and production method thereof | |
| JP2008255440A (en) | MoTi ALLOY SPUTTERING TARGET MATERIAL | |
| JP5397755B2 (en) | Fe-Co alloy sputtering target material for soft magnetic film formation | |
| JP2009203537A (en) | Co-Fe-BASED ALLOY SPUTTERING TARGET MATERIAL, AND METHOD FOR PRODUCING THE SAME | |
| JP5403418B2 (en) | Method for producing Co-Fe-Ni alloy sputtering target material | |
| JP2002249801A (en) | High corrosion resistant magnesium alloy and method for producing high corrosion resistant magnesium material | |
| JP2013032573A (en) | METHOD FOR MANUFACTURING Fe-Co-Ta SPUTTERING TARGET MATERIAL AND THE Fe-Co-Ta SPUTTERING TARGET MATERIAL |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20070612 |
|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20070612 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20090723 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20090731 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20090928 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20091120 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20091203 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121225 Year of fee payment: 3 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 4427792 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121225 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131225 Year of fee payment: 4 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term |