JP2002363615A - METHOD FOR MANUFACTURING Co-TYPE SPUTTERING TARGET MATERIAL WITH LOW MAGNETIC PERMEABILITY FOR MAGNETIC RECORDING MEDIUM - Google Patents
METHOD FOR MANUFACTURING Co-TYPE SPUTTERING TARGET MATERIAL WITH LOW MAGNETIC PERMEABILITY FOR MAGNETIC RECORDING MEDIUMInfo
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- JP2002363615A JP2002363615A JP2002079529A JP2002079529A JP2002363615A JP 2002363615 A JP2002363615 A JP 2002363615A JP 2002079529 A JP2002079529 A JP 2002079529A JP 2002079529 A JP2002079529 A JP 2002079529A JP 2002363615 A JP2002363615 A JP 2002363615A
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- target material
- magnetic
- magnetic permeability
- temperature
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、主として磁気記録
媒体用スパッタリングターゲット材の製造方法に関し、
特に低透磁率のスパッタリングＣｏ系ターゲット材の製
造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a sputtering target material for a magnetic recording medium.
In particular, the present invention relates to a method of manufacturing a sputtering target material having a low magnetic permeability.
【０００２】[0002]
【従来の技術】従来、電子機器材料の分野のなかでもコ
ンピューターのハードディスクなどの磁気記録媒体用薄
膜の需要は急激な増加の傾向にあり、使用される薄膜の
記録密度もますます高密度化しつつあり、Ｃｏ−Ｃｒ系
合金に加えてＣｏ−Ｃｒ−Ｔａ系合金、Ｃｏ−Ｐｔ系合
金およびＣｏ−Ｃｒ−Ｐｔ系合金薄膜が使用されつつあ
る。このような磁気記録媒体用薄膜の作製には、主とし
てスパッタリング工法が用いられている。このスパッタ
リングに使用されるターゲット材は、従来鋳造、鋳造→
圧延等の工法により成形され、切り出した後、所望の形
状および表面状態に機械加工をし、また必要に応じてバ
ッキングプレートにインジウムなどでろう付けして完成
品とされる。2. Description of the Related Art In the field of electronic device materials, the demand for thin films for magnetic recording media such as computer hard disks has been increasing rapidly, and the recording density of thin films used has been increasing. In addition, Co-Cr-Ta alloys, Co-Pt alloys, and Co-Cr-Pt alloy thin films are being used in addition to Co-Cr alloys. For manufacturing such a thin film for a magnetic recording medium, a sputtering method is mainly used. The target material used for this sputtering is conventionally casting, casting →
After being formed by a method such as rolling, and cut out, it is machined into a desired shape and surface state, and if necessary, brazed to a backing plate with indium or the like to obtain a finished product.
【０００３】さらに、一部には粉末冶金法によっても均
一性に優れた高品位のスパッタリングターゲット材の製
造が試みられている。このようなスパッタリングによる
磁気記録媒体用薄膜の製造においては、工業的にはマグ
ネトロン方式のスパッタリング装置が主として使用さ
れ、そのスパッタリング効果を高め、低コストでの薄膜
製造を目的として、スパッタリングターゲット材の低透
磁率化への試みが種々行われてきている。[0003] Further, some attempts have been made to produce high-quality sputtering target materials having excellent uniformity even by powder metallurgy. In the production of a thin film for a magnetic recording medium by such sputtering, a magnetron type sputtering apparatus is mainly used industrially, and the sputtering target material is reduced for the purpose of enhancing the sputtering effect and producing the thin film at low cost. Various attempts have been made to increase the permeability.
【０００４】[0004]
【発明が解決しようとする課題】この透磁率の低いター
ゲット材の製造には、目的組成の合金の溶解時に、低透
磁率化を達成するために、主成分以外の元素を添加させ
る方法があるが、スパッタリングにより作製した薄膜の
本質的な特性であるところの記録および再生特性に対し
て好影響を与えることなく、劣化させる可能性を含んで
いることから望ましくない。In the production of a target material having a low magnetic permeability, there is a method in which an element other than the main component is added in order to achieve a low magnetic permeability when an alloy having a desired composition is melted. However, this method is not desirable because it includes the possibility of deteriorating the recording and reproduction characteristics, which are essential characteristics of the thin film formed by sputtering, without having a favorable effect.
【０００５】これに対してターゲット材に冷間加工時あ
るいは熱間加工時に機械的に歪みを加え、透磁率の低減
を行うという方法は、薄膜の磁気特性を劣化させること
なく有効であるが、鋳造法で作製した鋳塊から切り出し
たターゲット材はその凝固時に生じる凝固偏析を避ける
ことができず、プレス機などにより機械的な歪みを加え
る際には成分の不均一に起因するところの機械的強度の
劣化に基づく割れなどの問題点を生じ易い。On the other hand, a method of mechanically applying strain to a target material during cold working or hot working to reduce the magnetic permeability is effective without deteriorating the magnetic properties of the thin film. The target material cut from the ingot produced by the casting method cannot avoid solidification segregation that occurs at the time of solidification, and when applying mechanical strain with a press machine etc., mechanical properties caused by non-uniform components Problems such as cracks due to deterioration in strength are likely to occur.
【０００６】さらにはターゲット材に与える歪み量のコ
ントロールは難しく、工業的に安定かつ容易な方法とは
言えがたい。この不均一な歪みの導入はろう付け時の際
の加熱時あるいはスパッタリング中にターゲットに加わ
る熱により、ターゲット本体に反りなどの機械的な寸法
変化を生じさせるなどの問題点がある。本発明はこのよ
うな状況の下でなされたものであって、その目的とする
ところは、従来技術に見られる種々の問題点を発生させ
ることなく、高性能な薄膜の作製を可能にする低透磁率
ターゲットの作製の実現を提供することにある。Further, it is difficult to control the amount of strain applied to the target material, and it is not industrially stable and easy. The introduction of the non-uniform distortion has a problem that the target body undergoes mechanical dimensional change such as warpage due to heat applied to the target during heating during brazing or during sputtering. The present invention has been made under such a circumstance, and an object of the present invention is to provide a low-performance thin film capable of producing a high-performance thin film without causing various problems found in the prior art. An object of the present invention is to provide a realization of a magnetic permeability target.
【０００７】[0007]
【課題を解決するための手段】上記の問題点を解決した
本発明の方法の要旨とするところは、Ｃｏ−Ｃｒ−Ｔａ
系合金のガスアトマイズ粉末を金属製の容器に充填・封
入し、これを加圧圧縮用金型内で高温高圧プレスして固
化成形した後、冷却途中にて８００℃〜１２５０℃の温
度範囲で低透磁率化のための熱処理を行い、冷却し、所
定の形状に機械加工することを特徴とするもので、この
方法は従来の機械的に歪みを導入する方法とは異なり、
特に熱処理により金属組織学的に構成相をコントロール
することにより低透磁率化を実現することを特徴とする
ものである。SUMMARY OF THE INVENTION The gist of the method of the present invention which has solved the above problems is that of Co-Cr-Ta.
After filling and enclosing the gas atomized powder of the base alloy in a metal container and pressing it in a pressurizing and compression mold at a high temperature and a high pressure for solidification molding, the temperature is lowered in the temperature range of 800 ° C to 1250 ° C during cooling. It is characterized by performing heat treatment for permeability, cooling, and machining into a predetermined shape.This method is different from the conventional method of introducing mechanical strain,
In particular, it is characterized by realizing a low magnetic permeability by controlling the constituent phases in a metallographic manner by heat treatment.
【０００８】[0008]
【発明の実施の形態】本発明における熱処理によるター
ゲット材の低透磁率化は、所望の熱処理中にＣｏＣｒ相
つまりσ相が析出するとともに、マトリックス中のＣｏ
量が減少し、その結果として透磁率が低下することによ
る。本発明において熱処理温度の下限を８００℃に限定
した理由は、８００℃未満では元素の拡散が遅く、Ｃｏ
Ｃｒ相の析出に長時間を要し実用的でないことによる。
上限温度を１２５０℃に限定した理由は、平衡状態図か
らもＣｏＣｒ相つまりσ相は１２８０℃まで分解するこ
とはないが、必要以上の高温までの加熱は、結晶粒を粗
大化させるなどの問題点が生じるので実質的には１２５
０℃以下が好ましいからである。アトマイズにおいては
粉末は急速凝固により作製されるため、組成的には鋳造
材と比較して格段に優れており、また熱間での固化成形
時にも均一化されるため、熱処理時の均熱後実質的には
３０分でその効果は現れることを確認した。DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, the target material is made to have a low magnetic permeability by a heat treatment.
Due to the reduced volume and consequently the permeability. The reason why the lower limit of the heat treatment temperature is limited to 800 ° C. in the present invention is that the diffusion of elements is slow below 800 ° C.
This is because it takes a long time to precipitate the Cr phase and is not practical.
The reason that the upper limit temperature is limited to 1250 ° C. is that the CoCr phase, that is, the σ phase does not decompose to 1280 ° C. even from the equilibrium diagram, but heating to a higher temperature than necessary causes the crystal grains to become coarse. Since the point is generated, it is substantially 125
This is because the temperature is preferably 0 ° C. or lower. In atomization, powder is produced by rapid solidification, so its composition is much better than that of cast material.Because it is uniform during hot solidification molding, it is uniform after heat treatment. It was confirmed that the effect appeared substantially in 30 minutes.
【０００９】[0009]
【実施例】実施例１ Ｃｏ−Ｃｒ12−Ｔａ4 の合金粉末をガスアトマイズ法で
作製し、金属製の容器に充填・ロータリー式真空ポンプ
で脱気後、押出し装置により１２００℃で径２１０ｍ
ｍ、長さ１５０ｍｍの成形材を作製した後、その冷却途
中にて８００℃、２時間熱処理を行い、水冷し、機械加
工を経てターゲット材に作製した。同一の成形材から透
磁率測定用試料を切り出し、透磁率を測定し、図１に示
すように熱処理を行っていないＢ部の透磁率と比較し、
透磁率が１０％低減していることを確認した。すなわ
ち、図１はＣｏ−Ｃｒ−Ｔａの場合の熱処理温度と透磁
率との変化を示す図であり、熱処理なしを１００とした
時の磁場１ｋＯｅにおける透磁率の相対値として表して
いる。また、図２はＣｏ−Ｃｒ−Ｔａの場合の熱処理温
度とＣｏＣｒ相の析出に伴うＸ線の回析強度の変化を示
す図である。これにより熱処理条件の違いによりＸ線相
対強度に変化があることが判る。EXAMPLE 1 Co-Cr 12 alloy powder -Ta 4 produced by the gas atomizing method, after degassing by filling and rotary vacuum pump in a metal container, the diameter at 1200 ° C. The extrusion apparatus 210m
After preparing a molded material having a length of 150 mm and a length of 150 mm, a heat treatment was performed at 800 ° C. for 2 hours in the middle of the cooling, followed by water cooling, followed by mechanical processing to prepare a target material. A sample for measuring the magnetic permeability was cut out from the same molding material, the magnetic permeability was measured, and compared with the magnetic permeability of the part B not subjected to the heat treatment as shown in FIG.
It was confirmed that the magnetic permeability was reduced by 10%. That is, FIG. 1 is a diagram showing a change between the heat treatment temperature and the magnetic permeability in the case of Co—Cr—Ta, and is expressed as a relative value of the magnetic permeability at a magnetic field of 1 kOe when no heat treatment is taken as 100. FIG. 2 is a graph showing the change in the X-ray diffraction intensity accompanying the heat treatment temperature and the CoCr phase precipitation in the case of Co—Cr—Ta. This indicates that there is a change in the X-ray relative intensity due to the difference in the heat treatment conditions.
【００１０】実施例２ Ｃｏ−Ｃｒ14−Ｔａ6 の合金粉末をガスアトマイズ法で
作製し、金属製の容器に充填・ロータリー式真空ポンプ
で脱気後、押出し装置により１２００℃で径２１０ｍ
ｍ、長さ１００ｍｍの成形材を作製した後、その冷却途
中にて１０００℃、２時間熱処理を行い、油冷し、機械
加工を経てターゲット材に作製した。同一の成形材から
透磁率測定用試料を切り出し、透磁率を測定し、実施例
１に示す図１と同様に、熱処理を行っていないＢ部の透
磁率と比較し、透磁率が１５％低減していることを確認
した。Example 2 An alloy powder of Co—Cr 14 —Ta 6 was prepared by a gas atomization method, filled in a metal container, deaerated by a rotary vacuum pump, and extruded at 1200 ° C. with a diameter of 210 m by an extruder.
After forming a molded material having a length of 100 mm and a length of 100 mm, a heat treatment was performed at 1000 ° C. for 2 hours in the course of cooling, followed by oil-cooling, followed by machining to prepare a target material. A sample for measuring the magnetic permeability was cut out from the same molding material, and the magnetic permeability was measured, and the magnetic permeability was reduced by 15% as compared with the magnetic permeability of the part B not subjected to the heat treatment, similarly to FIG. 1 shown in Example 1. I confirmed that.
【００１１】実施例３ Ｃｏ−Ｃｒ14−Ｐｔ8 の合金粉末をガスアトマイズ法で
作製し、金属製の容器に充填・ロータリー式真空ポンプ
で脱気後、押出し装置により１２００℃で径１６０ｍ
ｍ、長さ１００ｍｍの成形材を作製した後、その冷却途
中にて１０５０℃、１時間熱処理を行い、油冷し、機械
加工を経てターゲット材に作製した。同一の成形材から
透磁率測定用試料を切り出し、透磁率を測定し、実施例
１に示す図１と同様に、熱処理を行っていないＢ部の透
磁率と比較し、透磁率が２０％低減していることを確認
した。Example 3 An alloy powder of Co—Cr 14 —Pt 8 was prepared by a gas atomization method, filled in a metal container, deaerated by a rotary vacuum pump, and then extruded at 1200 ° C. to a diameter of 160 m by an extruder.
After forming a molded material having a length of 100 mm and a length of 100 mm, a heat treatment was performed at 1050 ° C. for 1 hour in the course of cooling, oil-cooled, and machined to produce a target material. A sample for permeability measurement was cut out from the same molding material, the permeability was measured, and the permeability was reduced by 20% as compared with the permeability of the part B not subjected to the heat treatment as in FIG. 1 shown in Example 1. I confirmed that.
【００１２】実施例４ Ｃｏ−Ｃｒ13−Ｔａ3 −Ｐｔ13の合金粉末をガスアトマ
イズ法で作製し、金属製の容器に充填・ロータリー式真
空ポンプで脱気後、押出し装置により１２００℃で径２
１０ｍｍ、長さ２００ｍｍの成形材を作製した後、その
冷却途中にて１０５０℃、１時間熱処理を行い、油冷
し、機械加工を経てターゲット材に作製した。同一の成
形材から透磁率測定用試料を切り出し、透磁率を測定
し、実施例１に示す図１と同様に、熱処理を行っていな
いＢ部の透磁率と比較し、透磁率が２０％低減している
ことを確認した。Example 4 An alloy powder of Co—Cr 13 —Ta 3 —Pt 13 was prepared by a gas atomization method, filled in a metal container, deaerated by a rotary vacuum pump, and then extruded at 1200 ° C. by an extruder.
After a molded material having a length of 10 mm and a length of 200 mm was produced, a heat treatment was performed at 1050 ° C. for 1 hour in the course of cooling, oil-cooled, and machined to produce a target material. A sample for permeability measurement was cut out from the same molding material, the permeability was measured, and the permeability was reduced by 20% as compared with the permeability of the part B not subjected to the heat treatment as in FIG. 1 shown in Example 1. I confirmed that.
【００１３】[0013]
【発明の効果】以上述べたように、本発明によるスパッ
タリングにより作製された薄膜の磁気特性を劣化させる
ことなく、ターゲット材の透磁率は実質１０〜２０％低
減された。この低透磁率化されたターゲットは機械的な
歪みが導入されておらず、ろう付け時の加熱によって
も、またスパッタリング中にもターゲット材に反りが発
生することなく、効率良く薄膜を作製することができる
ようになった。As described above, the magnetic permeability of the target material was substantially reduced by 10 to 20% without deteriorating the magnetic properties of the thin film produced by sputtering according to the present invention. This low-permeability target does not introduce mechanical strain, and can efficiently produce a thin film without heating during brazing and without warping of the target material during sputtering. Is now available.
【図１】Ｃｏ−Ｃｒ−Ｔａの場合の熱処理温度と透磁率
との変化を示す図である。FIG. 1 is a diagram showing changes in heat treatment temperature and magnetic permeability in the case of Co—Cr—Ta.
【図２】Ｃｏ−Ｃｒ−Ｔａの場合の熱処理温度とＣｏＣ
ｒ相の析出に伴うＸ線の回析強度との変化を示す図であ
る。FIG. 2 shows the heat treatment temperature and CoC for Co—Cr—Ta.
It is a figure which shows the change with the diffraction intensity of X-ray accompanying precipitation of r phase.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 国脇 嘉春 兵庫県姫路市飾磨区中島字一文字3007番地 山陽特殊製鋼株式会社内 (72)発明者 田中 義和 兵庫県姫路市飾磨区中島字一文字3007番地 山陽特殊製鋼株式会社内 Ｆターム(参考） 4K018 AA10 BA04 BB10 EA16 FA01 FA08 KA29 4K029 BA24 BC06 BD11 CA05 DC04 DC09 5D112 FA04 FB06 ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Yoshiharu Kuniwaki 3007 character, Nakajima character, Shima, Himeji City, Hyogo Prefecture Inside Sanyo Special Steel Co., Ltd. (72) Inventor Yoshikazu Tanaka 3007 character, Nakashima character, Himeji City, Hyogo Prefecture Address Sanyo Special Steel Co., Ltd. F term (reference) 4K018 AA10 BA04 BB10 EA16 FA01 FA08 KA29 4K029 BA24 BC06 BD11 CA05 DC04 DC09 5D112 FA04 FB06
Claims (3)
ズ粉末を金属製の容器に充填・封入し、これを加圧圧縮
用金型内で高温高圧プレスして固化成形した後、冷却途
中にて８００℃〜１２５０℃の温度で低透磁率化のため
の熱処理を行ってから、室温まで冷却し、所定の形状に
機械加工することを特徴とする磁気記録媒体用低透磁率
スパッタリングＣｏ系ターゲット材の製造方法。Claims 1. A gas atomized powder of a Co-Cr-Ta-based alloy is filled and sealed in a metal container, and this is solidified and formed by high-temperature and high-pressure pressing in a pressurizing mold, and then, during cooling. A low-magnetic-permeability sputtering Co-based target material for a magnetic recording medium, which is heat-treated at a temperature of 800 ° C. to 1250 ° C. to lower the magnetic permeability, then cooled to room temperature, and machined into a predetermined shape. Manufacturing method.
ズ粉末を金属製の容器に充填・封入し、これを加圧圧縮
用金型内で高温高圧プレスして固化成形した後、冷却途
中にて８００℃〜１２５０℃の温度で低透磁率化のため
の熱処理を行い、冷却し、所定の形状に機械加工するこ
とを特徴とする磁気記録媒体用低透磁率スパッタリング
Ｃｏ系ターゲット材の製造方法。2. A gas atomized powder of a Co—Cr—Pt-based alloy is filled and sealed in a metal container, and is solidified by high-temperature and high-pressure pressing in a metal mold for pressurization and compression. A method for producing a low-magnetic-permeability sputtering Co-based target material for a magnetic recording medium, comprising performing a heat treatment at a temperature of 800 ° C. to 1250 ° C. for lowering the magnetic permeability, cooling, and machining into a predetermined shape.
トマイズ粉末を金属製の容器に充填・封入し、これを加
圧圧縮用金型内で高温高圧プレスして固化成形した後、
容器を除去し該合金成形材部分を取り出し、冷却途中に
て８００℃〜１２５０℃の温度で低透磁率化のための熱
処理を行い、冷却し、所定の形状に機械加工することを
特徴とする磁気記録媒体用低透磁率スパッタリングＣｏ
系ターゲット材の製造方法。3. A gas atomized powder of a Co—Cr—Ta—Pt alloy is filled and sealed in a metal container, and is solidified by high-temperature and high-pressure pressing in a metal mold for pressure compression.
The method is characterized in that the container is removed, the alloy molding material portion is taken out, heat treatment for lowering the magnetic permeability is performed at a temperature of 800 ° C. to 1250 ° C. during cooling, cooling, and machining to a predetermined shape. Low permeability sputtering Co for magnetic recording media
Method of manufacturing a target material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002079529A JP2002363615A (en) | 2002-03-20 | 2002-03-20 | METHOD FOR MANUFACTURING Co-TYPE SPUTTERING TARGET MATERIAL WITH LOW MAGNETIC PERMEABILITY FOR MAGNETIC RECORDING MEDIUM |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002079529A JP2002363615A (en) | 2002-03-20 | 2002-03-20 | METHOD FOR MANUFACTURING Co-TYPE SPUTTERING TARGET MATERIAL WITH LOW MAGNETIC PERMEABILITY FOR MAGNETIC RECORDING MEDIUM |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16347596A Division JPH108243A (en) | 1996-06-24 | 1996-06-24 | Production of low permeability sputtering cobalt base target material for magnetic recording medium |
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| JP2002363615A true JP2002363615A (en) | 2002-12-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005012591A1 (en) * | 2003-08-05 | 2005-02-10 | Nikko Materials Co., Ltd. | Sputtering target and method for production thereof |
| JP2011214039A (en) * | 2010-03-31 | 2011-10-27 | Sanyo Special Steel Co Ltd | Method for producing sputtering target material |
| US8663439B2 (en) | 2004-11-15 | 2014-03-04 | Jx Nippon Mining & Metals Corporation | Sputtering target for producing metallic glass membrane and manufacturing method thereof |
| WO2014097911A1 (en) * | 2012-12-18 | 2014-06-26 | Jx日鉱日石金属株式会社 | Sintered sputtering target |
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2002
- 2002-03-20 JP JP2002079529A patent/JP2002363615A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005012591A1 (en) * | 2003-08-05 | 2005-02-10 | Nikko Materials Co., Ltd. | Sputtering target and method for production thereof |
| CN100457963C (en) * | 2003-08-05 | 2009-02-04 | 日矿金属株式会社 | Sputtering target and method for production thereof |
| US8430978B2 (en) | 2003-08-05 | 2013-04-30 | Jx Nippon Mining & Metals Corporation | Sputtering target and method for production thereof |
| US8663439B2 (en) | 2004-11-15 | 2014-03-04 | Jx Nippon Mining & Metals Corporation | Sputtering target for producing metallic glass membrane and manufacturing method thereof |
| JP2011214039A (en) * | 2010-03-31 | 2011-10-27 | Sanyo Special Steel Co Ltd | Method for producing sputtering target material |
| WO2014097911A1 (en) * | 2012-12-18 | 2014-06-26 | Jx日鉱日石金属株式会社 | Sintered sputtering target |
| JP5960287B2 (en) * | 2012-12-18 | 2016-08-02 | Ｊｘ金属株式会社 | Sintered sputtering target |
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