JP2006176808A - METHOD FOR PRODUCING CoCrPt-SIO2 SPUTTERING TARGET FOR DEPOSITING MAGNETIC RECORDING FILM - Google Patents
METHOD FOR PRODUCING CoCrPt-SIO2 SPUTTERING TARGET FOR DEPOSITING MAGNETIC RECORDING FILM Download PDFInfo
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この発明は、ハードディスクの高密度磁気記録媒体に適用される磁気記録膜、特に垂直磁気記録媒体に適用されるＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜を形成するための微細組織を有するＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法に関するものである
The present invention relates to a CoCrPt—SiO 2 sputtering having a microstructure for forming a magnetic recording film applied to a high-density magnetic recording medium of a hard disk, particularly a CoCrPt—SiO 2 granular magnetic recording film applied to a perpendicular magnetic recording medium. Relates to a method of manufacturing the target
ハードディスク装置は一般にコンピュータやデジタル家電等の外部記録装置として用いられており、記録密度の一層の向上が求められている。そのため、近年、超高密度の記録を実現できる垂直磁気記録方式が注目されてきた。この垂直磁気記録方式は、高密度化するほど記録磁化が安定すると言われており、この垂直磁気記録方式を備えた磁気記録媒体には磁気記録膜が積層されており、この磁気記録膜は高性能な磁気記録膜であることが必要である。これに適用可能な磁気記録膜の一つとしてＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜が提案されており、このＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜はＣｒおよびＰｔを含むＣｏ基焼結合金相とシリカ相の混合相を有する複合ターゲットを用いてＲＦマグネトロンスパッタ法により作製することができることが知られている（非特許文献１参照）。 Hard disk devices are generally used as external recording devices such as computers and digital home appliances, and further improvement in recording density is required. Therefore, in recent years, a perpendicular magnetic recording system that can realize ultra-high density recording has attracted attention. In this perpendicular magnetic recording system, it is said that the recording magnetization becomes more stable as the density is increased, and a magnetic recording film provided with this perpendicular magnetic recording system is laminated with a magnetic recording film. It must be a high performance magnetic recording film. As one of the magnetic recording films applicable to this, a CoCrPt—SiO 2 granular magnetic recording film has been proposed. This CoCrPt—SiO 2 granular magnetic recording film has a Co-based sintered alloy phase containing Cr and Pt and a silica phase. It is known that it can be produced by an RF magnetron sputtering method using a composite target having a mixed phase of (see Non-Patent Document 1).
この複合ターゲットは、通常は、ＳｉＯ２粉末：４〜２０原子％、Ｃｒ粉末：５〜２０原子％、Ｐｔ粉末：５〜３０原子％を含有し、残部：Ｃｏ粉末からなる組成となるように配合し混合したのち、得られた混合体を加圧焼結することにより作製される。この場合、シリカ粉末の粒径が大きいと、スパッタリングしたときにパーティクルが発生し易いので、シリカ粉末の粒径を１０μｍ以下とすることが好ましいとされている（特許文献１参照）。
しかし、粒径：１０μｍ以下の微細なＳｉＯ２粉末を使用し、この微細なＳｉＯ２粉末を通常の粒径を有するＣｒ粉末、Ｐｔ粉末、Ｃｏ粉末などとともに混合し、得られた混合粉末を加圧焼結することにより得られたターゲットは、加圧焼結中に粒成長して粗大な金属粒が生成し、それに伴って、微細なＳｉＯ２粉末は粗大な金属粒を取り囲むように粗大な金属粒の周囲に偏析し、この粗大な金属粒の周囲に偏析したＳｉＯ２相は集合して偏析しているために異常放電を起こし易く、異常放電が起きると、ＳｉＯ２相は破壊されてパーティクルとなり、さらにＳｉＯ２相に囲まれた粗大金属粒が剥離、飛散して数十μレベルの巨大なパーティクルになりやすいという問題点があった。 However, a fine SiO 2 powder having a particle size of 10 μm or less is used, and this fine SiO 2 powder is mixed with Cr powder, Pt powder, Co powder, etc. having a normal particle size, and the resulting mixed powder is added. The target obtained by pressure sintering grows grains during pressure sintering to produce coarse metal grains, and accordingly, the fine SiO 2 powder is coarse so as to surround the coarse metal grains. Since the SiO 2 phase segregated around the metal particles and segregated around the coarse metal particles aggregates and segregates, abnormal discharge is likely to occur. When abnormal discharge occurs, the SiO 2 phase is destroyed. There is a problem that the particles become particles, and the coarse metal particles surrounded by the SiO 2 phase are easily separated and scattered to form huge particles of several tens of microns.
そこで、本発明者らは、かかる課題を解決すべく研究を行なったところ、
原料粉末であるＣｒ粉末、Ｐｔ粉末、Ｃｏ粉末およびＳｉＯ２粉末を目標配合組成となるように混合し、得られた混合粉末を真空または不活性ガス雰囲気中で予め仮焼処理し、この仮焼処理した混合粉末をホットプレスまたは熱間静水圧プレスなどの方法で加圧焼結することにより得られたターゲットは、従来のＣｒ粉末、Ｐｔ粉末、Ｃｏ粉末およびＳｉＯ２粉末を混合して得られた混合粉末をただちに加圧焼結することにより得られたターゲットに比べて、金属粒が粗大化することなく、またＳｉＯ２相が集合して偏析することなく微細に均一分散している組織を有し、この全体が微細な組織を有するターゲットを用いてスパッタリングを行うと、パーティクルの発生を減少させることができる、という研究結果が得られたのである。
Therefore, the present inventors conducted research to solve this problem,
Raw material powders such as Cr powder, Pt powder, Co powder and SiO 2 powder are mixed so as to have a target composition, and the obtained mixed powder is pre-calcined in a vacuum or an inert gas atmosphere. The target obtained by pressure-sintering the treated mixed powder by a method such as hot pressing or hot isostatic pressing is obtained by mixing conventional Cr powder, Pt powder, Co powder and SiO 2 powder. Compared to the target obtained by immediately pressure-sintering the mixed powder, the structure is finely and uniformly dispersed without coarsening of the metal grains and without aggregation and segregation of the SiO 2 phase. In other words, it was found that the generation of particles can be reduced when sputtering is performed using a target having a fine structure as a whole.
この発明は、かかる研究結果に基づいてなされたものであって、
（１）Ｐｔ粉末、Ｃｒ粉末、Ｃｏ粉末およびＳｉＯ２粉末を混合し、得られた混合粉末を真空または不活性ガス雰囲気中で予め仮焼処理して仮焼処理粉末を作製し、この仮焼処理粉末を加圧焼結する磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法、に特徴を有するものである。
The present invention was made based on the results of such research,
(1) Pt powder, Cr powder, Co powder and SiO 2 powder are mixed, and the obtained mixed powder is calcined in advance in a vacuum or an inert gas atmosphere to prepare a calcined powder. This method is characterized by a method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film in which a treated powder is pressure-sintered.
前記（１）記載の磁気記録膜形成用スパッタリングターゲットを製造する方法において、Ｃｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＳｉＯ２粉末を目標とする配合組成となるように配合し混合して混合粉末を作製し、この混合粉末を仮焼処理したのち加圧焼結することが最も好ましいが、Ｐｔ粉末、ＳｉＯ２粉末、Ｃｒ粉末およびＣｏ粉末が目標配合組成より少ない配合組成の混合粉末であっても良く、この混合粉末はＰｔ粉末を目標配合量の８０質量％以上、ＳｉＯ２粉末を目標配合量の２０質量％以上含むことが必要であるが、Ｃｒ粉末およびＣｏ粉末は一部含まれていても含まれなくても良い。 In the method for producing a sputtering target for forming a magnetic recording film according to (1) above, Co powder, Cr powder, Pt powder and SiO 2 powder are blended and mixed so as to have a target blending composition to produce a mixed powder. It is most preferable that the mixed powder is subjected to calcination treatment and then pressure-sintered. However, the mixed powder may have a blending composition in which Pt powder, SiO 2 powder, Cr powder and Co powder are less than the target blending composition. This mixed powder needs to contain 80% by mass or more of the target compounding amount of Pt powder and 20% by mass or more of the target compounding amount of SiO 2 powder, although Cr powder and Co powder are partially contained. It does not have to be included.
したがって、この発明は、
（２）目標配合量のＰｔ粉末、目標配合量のＳｉＯ２粉末、目標配合量の０〜１００質量％（０も含む）のＣｒ粉末および目標配合量の０〜１００質量％（０も含む）のＣｏ粉末を含むＣｏおよびＣｒの内の１種または２種が目標配合組成より少ない配合組成の混合粉末（以下、一部不足混合粉末という）を作製し、この一部不足混合粉末を真空または不活性ガス雰囲気中で予め仮焼処理して一部不足仮焼処理粉末を作製し、この一部不足仮焼処理粉末にＣｒ粉末およびＣｏ粉末を添加して目標配合組成を有する混合粉末を作製し、この混合粉末を加圧焼結する磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法、
（３）目標配合量の８０質量％以上のＰｔ粉末、目標配合量の２０質量％以上の微細なＳｉＯ２粉末、目標配合量の０〜１００質量％（０も含む）のＣｒ粉末および目標配合量の０〜１００質量％（０も含む）のＣｏ粉末を含むＰｔ粉末、ＳｉＯ２粉末、Ｃｒ粉末およびＣｏ粉末が目標配合組成より少ない配合組成の混合粉末（以下、不足混合粉末という）を作製し、この不足混合粉末を真空または不活性ガス雰囲気中で予め仮焼処理して不足仮焼処理粉末を作製し、この不足仮焼処理粉末にＰｔ粉末、ＳｉＯ２粉末、Ｃｒ粉末およびＣｏ粉末を添加して目標成分組成を有する混合粉末を作製し、この混合粉末を加圧焼結する磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法、に特徴を有するものである。
Therefore, the present invention
(2) Target blending amount of Pt powder, target blending amount of SiO 2 powder, target blending amount of 0-100% by mass (including 0) Cr powder and target blending amount of 0-100% by mass (including 0) A mixed powder (hereinafter referred to as “partially deficient mixed powder”) having one or two of Co and Cr containing less than the target compounded composition is prepared, and the partially deficient mixed powder is vacuum or Preliminarily calcined in an inert gas atmosphere to produce a partially deficient calcined powder, and Cr powder and Co powder are added to the partially deficient calcined powder to produce a mixed powder having the target composition And a method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film, wherein the mixed powder is subjected to pressure sintering,
(3) Pt powder of 80% by weight or more of the target blending amount, fine SiO 2 powder of 20% by weight or more of the target blending amount, 0 to 100% by weight (including 0) Cr powder of the target blending amount and the target blending Preparation of mixed powder (hereinafter referred to as insufficient mixed powder) of Pt powder, SiO 2 powder, Cr powder and Co powder containing 0 to 100 mass% (including 0) of Co powder of the amount less than the target blend composition The insufficiently mixed powder is preliminarily calcined in a vacuum or an inert gas atmosphere to prepare an insufficiently calcined powder, and Pt powder, SiO 2 powder, Cr powder and Co powder are added to the insufficiently calcined powder. It is characterized by a method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film in which a mixed powder having a target component composition is added and the mixed powder is pressure-sintered.
本発明者らは、前記仮焼処理した混合粉末を加圧焼結することにより得られたターゲットは、その組織が一層微細化することについての理由を究明すべくさらに研究を行った。その結果、
（ｂ）原料粉末であるＣｒ粉末、Ｐｔ粉末、Ｃｏ粉末などの金属粉末の内でもＰｔ粉末は加圧焼結中に最も凝集しやすく、そのためにＰｔ粉末は加圧焼結中に凝集して粗大なＰｔ粉末に成長し、粗大なＰｔ粒になりやすいこと、
（ｃ）このＰｔ粉末が凝集し粗大化するのを阻止することにより、焼結体素地の金属粒の粗大化を阻止することができ、それに伴って、ＳｉＯ２相が粒界に集合して偏析することを阻止することができ、かかる阻止を行うことにより微細な金属粒および偏析の少ない微細なＳｉＯ２相が均一分散した組織を有するターゲットを作製することができること、
（ｄ）Ｐｔ粉末の加圧焼結工程における凝集および粗大化を阻止するには、予めＰｔ粉末と微細なＳｉＯ２粉末を混合して得られた混合粉末を仮焼処理することによりＰｔ粉末の外周に微細なＳｉＯ２粉末が固着したＰｔ−ＳｉＯ２仮焼処理粉末を形成し、このＰｔ粉末の外周に微細なＳｉＯ２粉末が固着したＰｔ−ＳｉＯ２仮焼処理粉末にＣｒ粉末およびＣｏ粉末を添加混合して目標成分組成を有する混合粉末を作製し、この混合粉末を加圧焼結すると、Ｐｔ粉末の外周に固着しているＳｉＯ２粉末がＰｔ粉末の凝集を阻止するために、加圧焼結中にＰｔ粉末が凝集して粗大化するのを防止することができるとともに偏析の少ない微細なＳｉＯ２相からなる組織を有するターゲットを得ることができる、などの研究結果が得られたのである。
The inventors of the present invention further studied to find out the reason why the microstructure of the target obtained by pressure-sintering the calcined mixed powder was further refined. as a result,
(B) Among metal powders such as Cr powder, Pt powder, and Co powder, which are raw material powders, Pt powder is most easily aggregated during pressure sintering. Therefore, Pt powder is aggregated during pressure sintering. It grows into coarse Pt powder and tends to become coarse Pt grains.
(C) By preventing the Pt powder from agglomerating and coarsening, it is possible to prevent the metal grains of the sintered body from coarsening, and as a result, the SiO 2 phase aggregates at the grain boundaries. Segregation can be prevented, and by performing such inhibition, a target having a structure in which fine metal particles and a fine SiO 2 phase with little segregation are uniformly dispersed can be produced.
(D) In order to prevent agglomeration and coarsening in the pressure sintering process of Pt powder, the mixed powder obtained by previously mixing Pt powder and fine SiO 2 powder is calcined to obtain Pt powder. periphery to form a Pt-SiO 2 calcinated treated powder fine SiO 2 powder is stuck, Cr powder and Co powder Pt-SiO 2 calcinated treated powder fine SiO 2 powder on the outer circumference is stuck in the Pt powder When a mixed powder having a target component composition is prepared by mixing and pressure-sintering the mixed powder, the SiO 2 powder fixed to the outer periphery of the Pt powder prevents the Pt powder from aggregating. Research results have been obtained, such as being able to prevent the Pt powder from agglomerating and coarsening during pressure sintering and to obtain a target having a structure composed of a fine SiO 2 phase with little segregation. Because is there.
この発明は、かかる研究結果に基づいてなされたものであって、
（４）Ｐｔ粉末と微細なＳｉＯ２粉末を混合して得られた混合粉体を仮焼処理することにより、Ｐｔ−ＳｉＯ２仮焼処理粉末を作製し、このＰｔ−ＳｉＯ２仮焼処理粉末にＣｒ粉末およびＣｏ粉末を混合して加圧焼結する磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法、に特徴を有するものである。
The present invention was made based on the results of such research,
(4) Pt powder and by calcining processes a mixed powder obtained by mixing a fine SiO 2 powder, to prepare a Pt-SiO 2 calcinated treated powder, the Pt-SiO 2 calcinated treated powder And a method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film, in which Cr powder and Co powder are mixed and pressure-sintered.
さらに、前記（４）記載の磁気記録膜形成用スパッタリングターゲットを製造する方法において、原料粉末であるＰｔ粉末を目標配合量の８０質量％以上、ＳｉＯ２粉末を目標配合量の２０質量％以上を混合して得られた混合粉末を仮焼処理することにより、目標成分組成より少ない組成を有するＰｔ粉末の外周に微細なＳｉＯ２粉末が固着したＰｔ−ＳｉＯ２仮焼処理粉末（以下、一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末という）を作製し、この一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末にＣｒ粉末、Ｃｏ粉末、Ｐｔ粉末およびＳｉＯ２粉末を添加して目標成分組成を有する混合粉末を作製し、この目標成分組成を有する混合粉末を加圧焼結することにより素地全体に微細な金属粒と偏析の少ない微細なＳｉＯ２相からなる組織を有するターゲットを得ることもできる。 Furthermore, in the method for producing a sputtering target for forming a magnetic recording film according to the above (4), Pt powder as a raw material powder is 80% by mass or more of the target compounding amount, and SiO 2 powder is 20% by mass or more of the target compounding amount. By calcining the mixed powder obtained by mixing, Pt-SiO 2 calcined powder (hereinafter, partly) in which fine SiO 2 powder is fixed to the outer periphery of Pt powder having a composition smaller than the target component composition to prepare a) that lack Pt-SiO 2 calcinated treated powder, mixed with a target component composition this part insufficient Pt-SiO 2 calcinated treated powder to Cr powder, Co powder, was added to Pt powder and SiO 2 powder A powder having a structure composed of fine metal particles and a fine SiO 2 phase with little segregation is formed on the entire substrate by pressure sintering the mixed powder having the target component composition. You can also get a get.
したがって、この発明は、
（５）Ｐｔ粉末を目標配合量の８０質量％以上、微細なＳｉＯ２粉末を目標配合量の２０質量％以上を混合して得られた混合粉末を仮焼処理することにより、目標成分組成より少ない組成のＰｔ−ＳｉＯ２仮焼処理粉末（以下、一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末という）を作製し、この一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末にＣｒ粉末、Ｃｏ粉末、Ｐｔ粉末およびＳｉＯ２粉末を添加して目標成分組成を有する混合粉末を作製し、この混合粉末を加圧焼結することを特徴とする磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法、に特徴を有するものである。
Therefore, the present invention
(5) By calcining a mixed powder obtained by mixing Pt powder with 80% by mass or more of the target blending amount and fine SiO 2 powder with 20% by mass or more of the target blending amount, Pt-SiO 2 calcinated treated powder of less composition (hereinafter, referred to as a part deficient Pt-SiO 2 calcinated treated powder) was prepared, Cr powder to the part lack Pt-SiO 2 calcinated treated powder, Co powder, A method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film, comprising adding a Pt powder and a SiO 2 powder to produce a mixed powder having a target component composition, and pressure-sintering the mixed powder, It has the characteristics.
この発明の前記（１）、（２）、（３）、（４）および（５）記載の磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法において使用する原料粉末は、Ｃｏ粉末、Ｃｒ粉末およびＰｔ粉末の平均粒径（ただし、平均粒径とは累積５０％の中心粒径を意味する。以下同じ）がいずれも５０μｍ以下であり、ＳｉＯ２粉末の平均粒径が１０μｍ以下であり、かつＳｉＯ２粉末の平均粒径はＰｔ粉末の平均粒径よりも小さく、ＳｉＯ２粉末とＰｔ粉末の平均粒径比が１／２００〜１／５の範囲内にあることが一層好ましい。Ｃｏ粉末、Ｃｒ粉末およびＰｔ粉末の平均粒径がいずれかが５０μｍを越えると、微細な組織が得られず、またＳｉＯ２粉末の平均粒径が１０μｍを越えると異常放電が発生し易くなり、したがってパーティクルの発生が多くなるからである。 The raw material powder used in the method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film according to (1), (2), (3), (4) and (5) of the present invention is Co powder, Cr The average particle size of the powder and the Pt powder (however, the average particle size means a central particle size of 50% cumulative. The same applies hereinafter) is 50 μm or less, and the average particle size of the SiO 2 powder is 10 μm or less. , and the average particle size of the SiO 2 powder is smaller than the average particle diameter of Pt powder, it is more preferable that the average particle size ratio of SiO 2 powder and Pt powder is in the range of 1 / 200-1 / 5. If any of the average particle diameter of Co powder, Cr powder and Pt powder exceeds 50 μm, a fine structure cannot be obtained, and if the average particle diameter of SiO 2 powder exceeds 10 μm, abnormal discharge is likely to occur. This is because the generation of particles increases.
また、ＳｉＯ２粉末とＰｔ粉末の平均粒径比が１／２００よりも小さい場合、ＳｉＯ２粉末の平均粒径が０．１μｍよりも小さくなって超微粒となり、かかる超微粒は混合時に凝集を起こしやすく、焼結をするとかえって巨大なＳｉＯ２の塊となってしまうので実用上適切ではない。一方、ＳｉＯ２粉末とＰｔ粉末の平均粒径比が１／５よりも大きいと、Ｐｔ粉末表面が十分にＳｉＯ２粉末で覆われないため、加圧焼結時におけるＰｔ粉末の凝集を阻止することができず、したがって、金属粒が粗大化し、微細なＳｉＯ２粉末が均一分散した組織が得られなくなるので好ましくない。 In addition, when the average particle size ratio of the SiO 2 powder and the Pt powder is smaller than 1/200, the average particle size of the SiO 2 powder becomes smaller than 0.1 μm and becomes ultrafine particles. It is easy to cause, and when sintered, it becomes a huge lump of SiO 2 , which is not suitable for practical use. On the other hand, if the average particle size ratio between the SiO 2 powder and the Pt powder is larger than 1/5, the surface of the Pt powder is not sufficiently covered with the SiO 2 powder, thereby preventing the aggregation of the Pt powder during pressure sintering. Therefore, the metal grains are coarsened, and a structure in which fine SiO 2 powder is uniformly dispersed cannot be obtained.
したがって、この発明は、
（６）原料粉末は、Ｃｏ粉末、Ｃｒ粉末およびＰｔ粉末の平均粒径（ただし、平均粒径とは累積５０％の中心粒径を意味する。以下同じ）がいずれも５０μｍ以下であり、ＳｉＯ２粉末の平均粒径が１０μｍ以下であり、かつＳｉＯ２粉末の平均粒径はＰｔ粉末の平均粒径よりも小さく、ＳｉＯ２粉末とＰｔ粉末の平均粒径比が１／２００〜１／５の範囲内にある前記（１）、（２）、（３）、（４）または（５）記載の磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法、に特徴を有するものである。
Therefore, the present invention
(6) The raw material powder has an average particle diameter of Co powder, Cr powder and Pt powder (however, the average particle diameter means a central particle diameter of 50% cumulative. The same applies hereinafter) is 50 μm or less. the average particle size of 2 powder is at 10μm or less, and the average particle size of the SiO 2 powder is smaller than the average particle diameter of the Pt powder, the average particle size ratio of SiO 2 powder and Pt powder 1/200 to 1/5 (1), (2), (3), (4) or (5) described above, the method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film is characterized.
この発明の磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法において、不足混合粉末および一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末に含まれるＰｔ粉末を目標配合量の８０質量％以上、ＳｉＯ２粉末を目標配合量の２０質量％以上とした理由は、Ｐｔ粉末が目標配合量の８０質量％未満ではＳｉＯ２粉末が固着してないＰｔ粉末の量が多くなり、このＳｉＯ２粉末が固着してないＰｔ粉末の量の多い粉末を加圧焼結すると、粗大粒が多く生成する原因になるので好ましくないからである。一方、ＳｉＯ２粉末の目標配合量を２０質量％未満にすると、ＳｉＯ２粉末の量が少なすぎてＰｔ粉末全量の表面を覆うに十分でなく、仮焼処理してもＳｉＯ２粉末が固着していないＰｔ粉末が多く存在することになり、粗大粒発生の原因になるので好ましくないからである。 In the method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film of the present invention, the Pt powder contained in the deficient mixed powder and the partially deficient Pt—SiO 2 calcined powder is 80% by mass or more of the target blending amount, SiO 2 reason for the 2 powder was not less than 20 mass% of the target amount, the amount of Pt powder SiO 2 powder is not fixed increases is less than 80 wt% of Pt powder target amount, the SiO 2 powder is fixed This is because pressure sintering a powder with a large amount of Pt powder that is not done is not preferable because it causes a large amount of coarse particles to be formed. On the other hand, if the target blending amount of SiO 2 powder is less than 20% by mass, the amount of SiO 2 powder is too small to cover the entire surface of Pt powder, and the SiO 2 powder is fixed even if calcined. This is because a large amount of Pt powder that is not present is present, which causes generation of coarse grains, which is not preferable.
この発明の磁気記録膜形成用ＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットの製造方法において、仮焼処理は温度：５００〜１０００℃、真空または不活性ガス雰囲気中、１０分以上保持の条件で行うことが好ましい。仮焼処理温度が５００℃未満ではＰｔ粉末の周りにＳｉＯ２粉末を十分に固着させることができず、したがってＰｔ粉末の凝集および粗大化を避けることができないので好ましくなく、一方、仮焼処理温度が１０００℃を越えると、ＳｉＯ２粉末同士が仮焼処理中に焼結し粗大化してしまう恐れがあるからである。仮焼処理温度の一層好ましい範囲は６００〜９００℃である。 In the method for producing a CoCrPt—SiO 2 sputtering target for forming a magnetic recording film according to the present invention, the calcination treatment is preferably performed at a temperature of 500 to 1000 ° C. in a vacuum or an inert gas atmosphere for 10 minutes or more. If the calcining temperature is less than 500 ° C., it is not preferable because the SiO 2 powder cannot be sufficiently fixed around the Pt powder, and therefore aggregation and coarsening of the Pt powder cannot be avoided. If the temperature exceeds 1000 ° C., the SiO 2 powders may be sintered and coarsened during the calcination treatment. A more preferable range of the calcining temperature is 600 to 900 ° C.
また、仮焼処理雰囲気は、Ｃｏ粉末およびＣｒ粉末を含む混合粉末の場合、Ｃｏ粉末およびＣｒ粉末の酸化を防ぐために真空または不活性ガス雰囲気で行うことが必要であるが、Ｐｔ−ＳｉＯ２仮焼処理粉末および一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末を作製する雰囲気は大気雰囲気であっても良い。仮焼処理時間は１時間以上行うことが一層好ましいが、生産性を考慮すると、４８時間以下が好ましい。 Further, calcination treatment atmosphere in the case of a mixed powder comprising Co powder and Cr powder, it is necessary to carried out in vacuum or inert gas atmosphere to prevent oxidation of the Co powder and Cr powder, Pt-SiO 2 Provisional The atmosphere for producing the calcined powder and the partially deficient Pt—SiO 2 calcined powder may be an air atmosphere. The calcination time is more preferably 1 hour or longer, but 48 hours or shorter is preferable in consideration of productivity.
加圧焼結は、１０００℃以上、１２５０℃以下の温度で実施することが好ましい。１０００℃未満では焼結体の密度が低く空孔を多く含むようになり、この焼結体を用いて作製したターゲットは異常放電やパーティクルが発生しやすいからである。一方、１２５０℃を越えて加圧焼結すると、ＣｏＣｒＰｔが溶融してしまう恐れがあるからである。 The pressure sintering is preferably performed at a temperature of 1000 ° C. or higher and 1250 ° C. or lower. If the temperature is lower than 1000 ° C., the sintered body has a low density and contains many voids, and a target produced using this sintered body is likely to generate abnormal discharge and particles. On the other hand, if the pressure sintering exceeds 1250 ° C., CoCrPt may be melted.
この発明は、パーティクル発生の少ないＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜を形成するためのＣｏＣｒＰｔ−ＳｉＯ２スパッタリングターゲットを簡単に製造することができ、コンピューター並びにデジタル家電等の産業の発展に大いに貢献し得るものである。 The present invention can easily produce a CoCrPt—SiO 2 sputtering target for forming a CoCrPt—SiO 2 granular magnetic recording film with less generation of particles, and can greatly contribute to the development of industries such as computers and digital home appliances. Is.
原料粉末として、平均粒径：１２μｍを有する市販のＣｏ粉末、平均粒径：３５μｍを有する市販のＣｒ粉末、平均粒径：３５μｍを有する市販のＰｔ粉末を用意した。さらに原料粉末として平均粒径：３μｍを有するＳｉＯ２粉末を用意した。 As the raw material powder, a commercially available Co powder having an average particle size of 12 μm, a commercially available Cr powder having an average particle size of 35 μm, and a commercially available Pt powder having an average particle size of 35 μm were prepared. Furthermore, SiO 2 powder having an average particle size: 3 μm was prepared as a raw material powder.
実施例１
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＳｉＯ２粉末を、Ｃｒ粉末：７．２原子％、Ｐｔ粉末：１８原子％、ＳｉＯ２粉末：１０原子％、残部：Ｃｏ粉末となるように秤量して配合し、Ａｒ雰囲気中、乾式ボールミルで８時間乾式混合し、得られた混合粉末を真空中：温度：７００℃で１時間保持の条件で仮焼処理を行った。この仮焼処理により一部焼結した部分が有る場合は軽く解砕して仮焼処理粉末を作製し、この仮焼処理粉末を直径：１６５ｍｍのカーボンモールドに充填し、真空雰囲気中、温度：１２００℃、圧力：２０ＭＰａ、３時間保持の条件で真空ホットプレスすることにより加圧焼結体を作製した。この加圧焼結体を機械加工することにより直径：１５２．４ｍｍ、厚さ：２ｍｍの寸法を有するターゲットを作製することにより本発明法１を実施した。
Example 1
The previously prepared Co powder, Cr powder, Pt powder and SiO 2 powder should be Cr powder: 7.2 atomic%, Pt powder: 18 atomic%, SiO 2 powder: 10 atomic%, and the balance: Co powder. The mixture was weighed and blended, and dry mixed in an Ar atmosphere with a dry ball mill for 8 hours. The obtained mixed powder was calcined under the conditions of keeping in vacuum: temperature: 700 ° C. for 1 hour. When there is a part sintered partly by this calcination treatment, it is crushed lightly to prepare a calcination treatment powder, this calcination treatment powder is filled in a carbon mold having a diameter of 165 mm, and in a vacuum atmosphere, temperature: A pressure sintered body was produced by vacuum hot pressing under conditions of 1200 ° C., pressure: 20 MPa, and 3 hours. The pressure-sintered body was machined to produce a target having a diameter of 152.4 mm and a thickness of 2 mm.
実施例２
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＳｉＯ２粉末を、Ｃｒ粉末：７．７原子％、Ｐｔ粉末：１６原子％、ＳｉＯ２粉末：６原子％、残部：Ｃｏ粉末となるように秤量して配合し、Ａｒ雰囲気中、乾式ボールミルで８時間乾式混合することにより一部不足混合粉末を作製し、得られた一部不足混合粉末を真空中：温度：７００℃で１時間保持の条件で仮焼処理を行うことにより一部不足仮焼処理粉末を作製した。この一部不足仮焼処理粉末にＰｔ粉末およびＳｉＯ２粉末を添加し混合してＣｒ粉末：７．２原子％、Ｐｔ粉末：１８原子％、ＳｉＯ２粉末：１０原子％、残部：Ｃｏ粉末からなる目標成分の混合粉末を作製し、得られた混合粉末を直径：１６５ｍｍのカーボンモールドに充填し、真空雰囲気中、温度：１２００℃、圧力：２０ＭＰａ、３時間保持の条件で真空ホットプレスすることにより加圧焼結体を作製した。この加圧焼結体を機械加工することにより直径：１５２．４ｍｍ、厚さ：２ｍｍの寸法を有するターゲットを作製することにより本発明法２を実施した。
Example 2
The previously prepared Co powder, Cr powder, Pt powder and SiO 2 powder should be Cr powder: 7.7 atomic%, Pt powder: 16 atomic%, SiO 2 powder: 6 atomic%, and the balance: Co powder. Weighing and blending, and preparing a partially deficient mixed powder by dry mixing in an Ar atmosphere with a dry ball mill for 8 hours. The resulting partially deficient mixed powder is kept in vacuum: temperature: 700 ° C. for 1 hour. A partially short calcined powder was produced by performing a calcining treatment under conditions. Pt powder and SiO 2 powder are added to and mixed with the partially calcined powder, Cr powder: 7.2 atomic%, Pt powder: 18 atomic%, SiO 2 powder: 10 atomic%, and the remainder: Co powder A mixed powder of the target component is prepared, and the obtained mixed powder is filled in a carbon mold having a diameter of 165 mm, and is vacuum hot pressed in a vacuum atmosphere at a temperature of 1200 ° C., a pressure of 20 MPa, and maintained for 3 hours. Thus, a pressure sintered body was produced. The pressure-sintered body was machined to produce a target having dimensions of diameter: 152.4 mm and thickness: 2 mm, and the present method 2 was carried out.
実施例３
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＳｉＯ２粉末を、Ｃｒ粉末：７．２原子％、Ｐｔ粉末：１８原子％、ＳｉＯ２粉末：１０原子％、残部：Ｃｏ粉末となるように秤量し、この内のＰｔ粉末およびＳｉＯ２粉末のみを大気中、乾式ボールミルで８時間乾式混合し、得られた混合粉末を大気中：温度：７００℃で１時間保持の条件で仮焼処理を行うことによりＰｔ−ＳｉＯ２仮焼処理粉末を作製した。この時、一部焼結した部分が有る場合は軽く解砕した。このようにして作製したＰｔ−ＳｉＯ２仮焼処理粉末に先に秤量したＣｒ粉末およびＣｏ粉末を添加し混合して混合粉末を作製し、この混合粉末を直径：１６５ｍｍのカーボンモールドに充填し、真空雰囲気中、温度：１２００℃、圧力：２０ＭＰａ、３時間保持の条件で真空ホットプレスすることにより加圧焼結体を作製した。この加圧焼結体を機械加工することにより直径：１５２．４ｍｍ、厚さ：２ｍｍの寸法を有するターゲットを作製することにより本発明法３を実施した。
Example 3
The previously prepared Co powder, Cr powder, Pt powder and SiO 2 powder should be Cr powder: 7.2 atomic%, Pt powder: 18 atomic%, SiO 2 powder: 10 atomic%, and the balance: Co powder. Weigh and dry-mix only the Pt powder and SiO 2 powder in the atmosphere with a dry ball mill for 8 hours in the atmosphere, and subject the resulting mixed powder to a calcination treatment in the atmosphere: temperature: held at 700 ° C. for 1 hour. to prepare a Pt-SiO 2 calcinated treated powder by performing. At this time, when there was a partially sintered part, it was crushed lightly. The thus-prepared Pt—SiO 2 calcined powder was mixed with the previously weighed Cr powder and Co powder to produce a mixed powder, and this mixed powder was filled into a carbon mold having a diameter of 165 mm, A pressure-sintered body was produced by vacuum hot pressing in a vacuum atmosphere at a temperature of 1200 ° C. and a pressure of 20 MPa for 3 hours. The pressure-sintered body was machined to produce a target having a diameter of 152.4 mm and a thickness of 2 mm, and the present invention method 3 was carried out.
実施例４
先に用意したＰｔ粉末およびＳｉＯ２粉末を目標配合量の９０質量％、ＳｉＯ２粉末を目標配合量の６０質量％を混合し、得られた混合粉末をＡｒ雰囲気中、乾式ボールミルで８時間乾式混合したのち真空中：温度：７００℃で１時間保持の条件で仮焼処理を行うことにより目標成分組成より少ない組成の一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末を作製し、この一部不足Ｐｔ−ＳｉＯ２仮焼処理粉末にＣｒ粉末、Ｃｏ粉末、Ｐｔ粉末およびＳｉＯ２粉末を添加して目標成分組成のＣｒ：７．２原子％、Ｐｔ：１８原子％、ＳｉＯ２：１０原子％、残部：Ｃｏからなる混合粉末を作製し、この混合粉末を直径：１６５ｍｍのカーボンモールドに充填し、真空雰囲気中、温度：１２００℃、圧力：２０ＭＰａ、３時間保持の条件で真空ホットプレスすることにより加圧焼結体を作製した。この加圧焼結体を機械加工することにより直径：１５２．４ｍｍ、厚さ：２ｍｍの寸法を有するターゲットを作製することにより本発明法４を実施した。
Example 4
The previously prepared Pt powder and SiO 2 powder were mixed with 90% by mass of the target compounding amount, and SiO 2 powder was mixed with 60% by mass of the target compounding amount. The resulting mixed powder was dry-dried in an Ar atmosphere in a dry ball mill for 8 hours. After mixing, in vacuum: Temperature: calcination under the condition of holding at 700 ° C. for 1 hour to produce a partially insufficient Pt—SiO 2 calcination powder with a composition less than the target component composition, and this partially insufficient Cr powder, Co powder, Pt powder and SiO 2 powder are added to the Pt—SiO 2 calcined powder, and the target component composition is Cr: 7.2 atomic%, Pt: 18 atomic%, SiO 2 : 10 atomic%, The balance: Co mixed powder made of Co was prepared, and this mixed powder was filled into a carbon mold having a diameter of 165 mm, and vacuum hot-pressed in a vacuum atmosphere at a temperature of 1200 ° C., a pressure of 20 MPa, and maintained for 3 hours. The pressure-sintered body was produced by reducing. The pressure-sintered body was machined to produce a target having a diameter of 152.4 mm and a thickness of 2 mm, and the present invention method 4 was carried out.
従来例１
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＳｉＯ２粉末を、Ｃｒ粉末：７．２原子％、Ｐｔ粉末：１８原子％、ＳｉＯ２粉末：１０原子％、残部：Ｃｏ粉末となるように秤量して配合し、ジルコニアボールによる乾式ボールミルで８時間乾式混合し、得られた混合粉末を直径：１６５ｍｍのカーボンモールドに充填し、真空雰囲気中、温度：１２００℃、圧力：２０ＭＰａ、３時間保持の条件で真空ホットプレスすることにより加圧焼結体を作製した。この加圧焼結体を機械加工することにより直径：１５２．４ｍｍ、厚さ：２ｍｍの寸法を有するターゲットを作製することにより従来法１を実施した。
Conventional Example 1
The previously prepared Co powder, Cr powder, Pt powder and SiO 2 powder should be Cr powder: 7.2 atomic%, Pt powder: 18 atomic%, SiO 2 powder: 10 atomic%, and the balance: Co powder. Weigh and mix, dry-mix for 8 hours in a dry ball mill with zirconia balls, fill the resulting mixed powder into a carbon mold with a diameter of 165 mm, hold in a vacuum atmosphere at a temperature of 1200 ° C., a pressure of 20 MPa, and hold for 3 hours. A pressure sintered body was prepared by vacuum hot pressing under the conditions of: Conventional method 1 was carried out by producing a target having dimensions of diameter: 152.4 mm and thickness: 2 mm by machining this pressure sintered body.
さらに実施例１〜４の本発明法１〜４を実施することにより得られたターゲットおよび従来例１の従来法１を実施することにより得られたターゲットをそれぞれバッキングプレートにろう付けし、これを市販のスパッタ装置に装着し、
到達真空度：＜５×１０−５Ｐａ、
基板加熱：無し、
ターゲット−基板間距離：６０ｍｍ、
Ａｒガス圧：２．０Ｐａ、
放電電力：ＲＦ６５０ｗ、
の条件で３０分間のプレスパッタ後、市販の直径：６インチ、Ｓｉウエハ上にＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜を厚さ：１００ｎｍになるように２５枚の基板に成膜した。得られた基板について、市販の異物検査装置により基板上の異物数を計数し、２５枚の平均値を求め、その結果を表１に示した。なお、この成膜は、前もって成膜と同じ条件で３時間のプレスパッタを行い、ターゲット表層の機械加工跡を除去し、一端装置を大気開放してチャンバーを十分クリーニングしてから行った。
Further, the target obtained by carrying out the inventive methods 1 to 4 of Examples 1 to 4 and the target obtained by carrying out the conventional method 1 of Conventional Example 1 are brazed to the backing plate, respectively. Attached to a commercially available sputtering device,
Ultimate vacuum: <5 × 10 −5 Pa,
Substrate heating: None,
Target-substrate distance: 60 mm,
Ar gas pressure: 2.0 Pa,
Discharge power: RF650w,
After pre-sputtering for 30 minutes under the above conditions, a commercially available diameter: 6 inches, a CoCrPt—SiO 2 granular magnetic recording film was formed on 25 substrates on a Si wafer to a thickness of 100 nm. About the obtained board | substrate, the number of the foreign materials on a board | substrate was counted with the commercially available foreign material test | inspection apparatus, the average value of 25 sheets was calculated | required, and the result was shown in Table 1. This film formation was performed in advance by performing pre-sputtering for 3 hours under the same conditions as the film formation, removing the machining trace of the target surface layer, opening the one-end device to the atmosphere, and sufficiently cleaning the chamber.
表１に示される結果から、本発明法１〜４を実施することにより得られたターゲットは、従来法１を実施することにより得られたターゲットに比べて、スパッタリング時に発生するパーティクルの数が格段に少ないことが分かる。 From the results shown in Table 1, the target obtained by carrying out the inventive methods 1 to 4 has a remarkably large number of particles generated during sputtering compared to the target obtained by carrying out the conventional method 1. It can be seen that there are few.
さらに、スパッタによる成膜後、バッキングプレートからターゲットを剥がし、そこから組織観察用のサンプルを切り出し、樹脂に埋めこみ、研磨したのち５００倍の光学顕微鏡で断面組織を観察し、その組織写真を撮影し、前記実施例１〜４および従来例１で作製したターゲットの組織写真を図１〜５に示した。
図１〜５から明らかなように、実施例１〜４の本発明法１〜４を実施することにより得られたターゲットは金属粒（白色部）が微細であり、さらのＳｉＯ２相（黒色部）が微細に均一分散しているに対し、従来例１の従来法１を実施することにより得られたターゲットは金属粒（白色部）が粗大であり、さらのＳｉＯ２相（黒色部）が粗大な金属粒の周囲を囲むように集合して偏析していることがわかる。
Furthermore, after film formation by sputtering, the target is peeled off from the backing plate, and a sample for observing the structure is cut out from it, embedded in resin, polished, and then observed for a cross-sectional structure with a 500 × optical microscope, and a photograph of the structure is taken. The structure photographs of the targets prepared in Examples 1 to 4 and Conventional Example 1 are shown in FIGS.
As is apparent from FIGS. 1 to 5, the target obtained by carrying out the inventive methods 1 to 4 of Examples 1 to 4 has fine metal particles (white part) and further SiO 2 phase (black). Part) is finely and uniformly dispersed, the target obtained by carrying out Conventional Method 1 of Conventional Example 1 has coarse metal particles (white part), and further SiO 2 phase (black part) It can be seen that segregates around the periphery of coarse metal grains.
Claims (6)
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