JP6575775B2 - Soft magnetic film - Google Patents
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- JP6575775B2 JP6575775B2 JP2017509306A JP2017509306A JP6575775B2 JP 6575775 B2 JP6575775 B2 JP 6575775B2 JP 2017509306 A JP2017509306 A JP 2017509306A JP 2017509306 A JP2017509306 A JP 2017509306A JP 6575775 B2 JP6575775 B2 JP 6575775B2
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- 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
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
- G11B5/739—Magnetic recording media substrates
- G11B5/73911—Inorganic substrates
- G11B5/73921—Glass or ceramic substrates
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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
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- 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
- G11B5/851—Coating a support with a magnetic layer by sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/16—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing cobalt
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
Description
本発明は、垂直磁気記録方式の磁気媒体等に用いられる軟磁性膜およびこの軟磁性膜を形成するために用いるスパッタリングターゲットに関するものである。 The present invention relates to a soft magnetic film used for a perpendicular magnetic recording type magnetic medium and the like and a sputtering target used to form the soft magnetic film.
近年の磁気記録媒体には記録密度の高密度化のため、従来の面内磁気記録に替わり、垂直磁気記録方式が実用化されている。垂直磁気記録方式とは、垂直磁気記録媒体の磁性膜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。この垂直磁気記録方式において、記録感度を高めた磁気記録膜層と軟磁性膜層とを有する記録媒体が開発されている。
このような磁気記録媒体の軟磁性膜としては、優れた軟磁気特性が要求されることから、アモルファス軟磁性合金が採用されている。この軟磁性膜用のアモルファス合金としては、Ｆｅ、ＣｏあるいはＦｅＣｏ合金に種々の添加元素を含む合金が挙げられる。（例えば、特許文献１参照。）In recent years, a perpendicular magnetic recording system has been put to practical use in place of conventional in-plane magnetic recording in order to increase the recording density of magnetic recording media. Perpendicular magnetic recording is a method in which the magnetic film of a perpendicular magnetic recording medium is formed so that the axis of easy magnetization is oriented perpendicular to the medium surface, and the demagnetizing field in the bit is small even when the recording density is increased. This is a method suitable for high recording density with little deterioration in recording / reproducing characteristics. In this perpendicular magnetic recording system, a recording medium having a magnetic recording film layer and a soft magnetic film layer with improved recording sensitivity has been developed.
As the soft magnetic film of such a magnetic recording medium, an amorphous soft magnetic alloy is adopted because excellent soft magnetic properties are required. Examples of the amorphous alloy for the soft magnetic film include Fe, Co, or an alloy containing various additive elements in the FeCo alloy. (For example, refer to
従来の軟磁性膜には、高い飽和磁束密度（以下、Ｂｓと記す。）と非晶質性が要求されていた。そして、近年では、ドライブ中の読書き用ヘッドの改良や、軟磁性合金の磁束密度を調整し、軟磁性膜とＲｕ膜との交換結合磁界を最適化することにより、従来よりも低い磁束での書込みが可能となってきている。
このように、アモルファス合金を垂直磁気記録媒体の軟磁性膜として用いると、軟磁性膜中の記録磁化が周囲に磁気的な影響を与えることなく、小さなスペースに記録可能となる。そして、このような高いＢｓが要求される軟磁性膜には、ＦｅリッチのＦｅＣｏ合金が利用されている。Conventional soft magnetic films are required to have a high saturation magnetic flux density (hereinafter referred to as Bs) and amorphousness. And in recent years, by improving the read / write head during driving, adjusting the magnetic flux density of the soft magnetic alloy, and optimizing the exchange coupling magnetic field between the soft magnetic film and the Ru film, Can be written.
As described above, when the amorphous alloy is used as the soft magnetic film of the perpendicular magnetic recording medium, the recording magnetization in the soft magnetic film can be recorded in a small space without magnetically affecting the surroundings. For such a soft magnetic film requiring high Bs, an Fe-rich FeCo alloy is used.
本発明者の検討によると、上述したＦｅリッチのＦｅＣｏ合金を用いた軟磁性膜は、温度の上昇に伴うＢｓの低下が大きく、室温（２５℃）より高い温度環境、例えば５０〜１００℃程度では、垂直磁気記録媒体の軟磁性膜としての機能を十分に果たせなくなってしまう場合がある、すなわち、Ｂｓの高温特性に問題があることを確認した。 According to the study of the present inventor, the soft magnetic film using the above-described Fe-rich FeCo alloy has a large decrease in Bs as the temperature rises, and a temperature environment higher than room temperature (25 ° C.), for example, about 50 to 100 ° C. Then, it was confirmed that the function as the soft magnetic film of the perpendicular magnetic recording medium may not be sufficiently performed, that is, there is a problem in the high temperature characteristics of Bs.
本発明の目的は、高温でもＢｓの低下が小さい軟磁性膜、および、この軟磁性膜を形成するために用いるスパッタリングターゲットを提供することである。 An object of the present invention is to provide a soft magnetic film in which a decrease in Bs is small even at a high temperature, and a sputtering target used for forming the soft magnetic film.
本発明者は、Ｂｓの高温特性に関する問題を検討した。そして、軟磁性膜を構成するアモルファス合金にＣｏＦｅＮｂ系合金を採用し、ＣｏとＦｅとの原子比を一定の比率とすることで、Ｂｓの高温特性を大きく改善できることを見出し、本発明に到達した。
すなわち、本発明は、原子比における組成式が、（ＣｏａＦｅ１−ａ）１００−ｂ−ｃＮｂｂＭｃ、０．５０≦ａ≦０．９０、３≦ｂ≦１４、３≦ｃ≦１９、１６≦ｂ＋ｃ≦２４、Ｍは、Ｍｏ、ＣｒおよびＷからなる群から選ばれる１種以上の元素、残部が不可避的不純物からなり、１００℃における飽和磁束密度が０．５０Ｔ以上である軟磁性膜である。The present inventor has examined problems related to the high temperature characteristics of Bs. The present inventors have found that the high temperature characteristics of Bs can be greatly improved by adopting a CoFeNb-based alloy as the amorphous alloy constituting the soft magnetic film and by making the atomic ratio of Co and Fe constant. .
That is, in the present invention, the composition formula in the atomic ratio is (Co a Fe 1-a ) 100- bc Nb b M c , 0.50 ≦ a ≦ 0.90, 3 ≦ b ≦ 14, 3 ≦ c. ≦ 19, 16 ≦ b + c ≦ 24, M is one or more elements selected from the group consisting of Mo, Cr and W, the balance is made of inevitable impurities, and the saturation magnetic flux density at 100 ° C. is 0.50 T or more It is a soft magnetic film.
また、本発明は、前記軟磁性膜を形成するために用いるスパッタリングターゲット材であって、原子比における組成式が、（ＣｏａＦｅ１−ａ）１００−ｂ−ｃＮｂｂＭｃ、０．５０≦ａ≦０．９０、３≦ｂ≦１４、３≦ｃ≦１９、１６≦ｂ＋ｃ≦２４、Ｍは、Ｍｏ、ＣｒおよびＷからなる群から選ばれる１種以上の元素、残部が不可避的不純物からなる軟磁性膜形成用のスパッタリングターゲットである。The present invention also provides a sputtering target material used for forming the soft magnetic film, wherein the composition formula in terms of atomic ratio is (Co a Fe 1-a ) 100- bc Nb b M c , 0. 50 ≦ a ≦ 0.90, 3 ≦ b ≦ 14, 3 ≦ c ≦ 19, 16 ≦ b + c ≦ 24, M is one or more elements selected from the group consisting of Mo, Cr and W, and the remainder is inevitable A sputtering target for forming a soft magnetic film made of impurities.
本発明によれば、室温（２５℃）より高い温度環境でも、Ｂｓの低下が小さく、高温特性に優れるため、垂直磁気記録媒体の使用環境下で軟磁性膜の性能を十分に高めることができるようになり、垂直磁気記録媒体の製造に有用な技術となる。 According to the present invention, even in a temperature environment higher than room temperature (25 ° C.), since the decrease in Bs is small and the high temperature characteristics are excellent, the performance of the soft magnetic film can be sufficiently enhanced under the usage environment of the perpendicular magnetic recording medium. Thus, the technique is useful for manufacturing a perpendicular magnetic recording medium.
本発明の軟磁性膜は、原子比における組成式が、（ＣｏａＦｅ１−ａ）１００−ｂ−ｃＮｂｂＭｃ、０．５０≦ａ≦０．９０、３≦ｂ≦１４、３≦ｃ≦１９、１６≦ｂ＋ｃ≦２４、Ｍは、Ｍｏ、ＣｒおよびＷからなる群から選ばれる１種以上の元素、残部が不可避的不純物からなり、１００℃におけるＢｓが０．５０Ｔ以上であることに特徴を有する。
そして、本発明の軟磁性膜は、垂直磁気記録媒体の使用環境である、室温（２５℃）より高い、１００℃という温度で、Ｂｓの低下を抑制して、Ｂｓを０．５０Ｔ以上とすることにより、垂直磁気記録媒体の軟磁性膜としての機能を十分に果たすことができる。
本発明の上記原子比における組成式中のａ、即ちＣｏの含有比率を０．５０以上とするのは、１００℃におけるＢｓの低下を抑制し、Ｂｓを０．５０Ｔ以上にするためである。また、組成式中のａを０．９０以下にすることで、軟磁気特性の低下を抑制することができる。このため、本発明では、組成式中のａを０．５０≦ａ≦０．９０の範囲にする。中でも、上記と同様の理由から、０．５５≦ａ≦０．７０の範囲が好ましい。The soft magnetic film of the present invention has an atomic ratio of (Co a Fe 1-a ) 100- bc Nb b M c , 0.50 ≦ a ≦ 0.90, 3 ≦ b ≦ 14, 3 ≦ c ≦ 19, 16 ≦ b + c ≦ 24, M is one or more elements selected from the group consisting of Mo, Cr and W, the balance is unavoidable impurities, and Bs at 100 ° C. is 0.50 T or more It has a special feature.
The soft magnetic film of the present invention suppresses the decrease in Bs at a temperature of 100 ° C., which is higher than room temperature (25 ° C.), which is the usage environment of the perpendicular magnetic recording medium, and sets Bs to 0.50 T or more. Thus, the function as a soft magnetic film of the perpendicular magnetic recording medium can be sufficiently achieved.
The reason why the content ratio of a in the composition formula in the above-described atomic ratio of the present invention, that is, Co, is 0.50 or more is to suppress the decrease of Bs at 100 ° C. and to make Bs 0.50 T or more. Moreover, the fall of a soft magnetic characteristic can be suppressed by making a in a composition formula into 0.90 or less. For this reason, in the present invention, a in the composition formula is in the range of 0.50 ≦ a ≦ 0.90. Among these, for the same reason as described above, a range of 0.55 ≦ a ≦ 0.70 is preferable.
本発明の軟磁性膜は、Ｎｂを含有する。Ｎｂを添加元素として選定したのは、電位−ｐＨ図において、ｐＨの広範囲に亘って緻密な不動態被膜を形成することが示されていることから、軟磁性膜の耐食性を向上させるためである。
本発明の軟磁性膜は、組成式中のｂを３以上にすることにより、軟磁性膜をアモルファス構造にすることができる上、耐食性を向上させることができる。また、本発明の軟磁性膜は、組成式中のｂを１４以下にすることにより、脆い金属間化合物相の形成を抑制できる。このため、本発明の軟磁性膜は、組成式中のｂを３≦ｂ≦１４の範囲とする。これにより、本発明の軟磁性膜は、成膜時にアモルファス膜となると同時に、高温環境下であっても軟磁性膜をアモルファス構造に維持でき、結晶化の抑制が可能となる。中でも、上記と同様の理由から、ｂは５以上が好ましく、８以上がより好ましい。また、ｂは１２以下が好ましく、１１以下がより好ましい。The soft magnetic film of the present invention contains Nb. The reason why Nb was selected as the additive element is to improve the corrosion resistance of the soft magnetic film because it is shown in the potential-pH diagram that a dense passive film is formed over a wide range of pH. .
In the soft magnetic film of the present invention, by setting b in the composition formula to 3 or more, the soft magnetic film can have an amorphous structure and corrosion resistance can be improved. Moreover, the soft magnetic film of this invention can suppress formation of a brittle intermetallic compound phase by making b in a composition formula 14 or less. Therefore, in the soft magnetic film of the present invention, b in the composition formula is in the range of 3 ≦ b ≦ 14. Thereby, the soft magnetic film of the present invention becomes an amorphous film at the time of film formation, and at the same time, the soft magnetic film can be maintained in an amorphous structure even under a high temperature environment, and crystallization can be suppressed. Among these, for the same reason as described above, b is preferably 5 or more, and more preferably 8 or more. Further, b is preferably 12 or less, and more preferably 11 or less.
本発明の軟磁性膜は、Ｍ元素としてＭｏ、ＣｒおよびＷからなる群から選ばれる１種以上の元素を含有し、その含有量を３〜１９の範囲とする。
上記のＮｂを添加するのみでは、十分に安定なアモルファス構造と高い耐食性を得ることが困難な場合がある。そこで、本発明の軟磁性膜は、Ｍ元素をＮｂと複合添加することにより、十分に安定なアモルファス構造を形成した上で、軟磁気特性や耐食性を向上させることができる。そして、Ｍ元素の群の中でも、上記と同様の理由から、Ｗが好ましい。
本発明の軟磁性膜は、組成式中のｃを３以上にすることにより、十分に安定なアモルファス構造が得られるとともに、耐食性を向上できる。また、本発明の軟磁性膜は、組成式中のｃを１９以下にすることで、軟磁性膜の軟磁気特性を向上できる。このため、本発明の軟磁性膜は、Ｍ元素の添加量、即ち組成式中のｃを、３≦ｃ≦１９の範囲とする。中でも、上記と同様の理由から、ｃは４以上が好ましく、８以上がより好ましい。また、ｃは１８以下が好ましく、１１以下がより好ましい。The soft magnetic film of the present invention contains one or more elements selected from the group consisting of Mo, Cr and W as the M element, and the content thereof is in the range of 3 to 19.
It may be difficult to obtain a sufficiently stable amorphous structure and high corrosion resistance only by adding the above Nb. Therefore, the soft magnetic film of the present invention can improve soft magnetic properties and corrosion resistance while forming a sufficiently stable amorphous structure by adding M element in combination with Nb. And among the group of M elements, W is preferable for the same reason as described above.
In the soft magnetic film of the present invention, by setting c in the composition formula to 3 or more, a sufficiently stable amorphous structure can be obtained and the corrosion resistance can be improved. The soft magnetic film of the present invention can improve the soft magnetic properties of the soft magnetic film by setting c in the composition formula to 19 or less. Therefore, in the soft magnetic film of the present invention, the amount of M element added, that is, c in the composition formula is in the range of 3 ≦ c ≦ 19. Among these, for the same reason as above, c is preferably 4 or more, and more preferably 8 or more. Further, c is preferably 18 or less, and more preferably 11 or less.
本発明の軟磁性膜は、上記Ｎｂと上記Ｍ元素を複合添加する際に、その含有量、即ち組成式中のｂ＋ｃを、１６≦ｂ＋ｃ≦２４の範囲とする。これは、アモルファス構造を維持したまま、良好な軟磁気特性を得るためである。組成式中のｂ＋ｃを１６以上にすることで、軟磁性膜において安定なアモルファス構造が得られるとともに、耐食性を向上させることができる。また、本発明の軟磁性膜は、組成式中のｂ＋ｃを２４以下にすることにより、軟磁性膜の軟磁気特性を向上できる。中でも、上記と同様の理由から、ｂ＋ｃは１６以上が好ましく、１７以上がより好ましい。また、ｂ＋ｃは２２以下が好ましく、２１以下がより好ましい。 In the soft magnetic film of the present invention, when Nb and M element are added in combination, the content, that is, b + c in the composition formula is set in the range of 16 ≦ b + c ≦ 24. This is to obtain good soft magnetic characteristics while maintaining the amorphous structure. By setting b + c in the composition formula to 16 or more, a stable amorphous structure can be obtained in the soft magnetic film, and the corrosion resistance can be improved. The soft magnetic film of the present invention can improve the soft magnetic properties of the soft magnetic film by setting b + c in the composition formula to 24 or less. Among these, for the same reason as described above, b + c is preferably 16 or more, and more preferably 17 or more. Further, b + c is preferably 22 or less, and more preferably 21 or less.
本発明の軟磁性膜は、ＮｂおよびＭ元素を上記の範囲で含有する以外の残部は、ＦｅとＣｏと不可避的不純物である。不純物の含有量は、できるだけ少ないことが好ましく、例えば、ガス成分である酸素、窒素は１０００質量ｐｐｍ以下、不可避的に含まれるガス成分以外のＮｉ、Ｓｉ等の不純物元素は、合計で１０００質量ｐｐｍ以下であることが好ましい。 In the soft magnetic film of the present invention, the balance other than containing Nb and M elements in the above range is Fe, Co, and unavoidable impurities. The content of impurities is preferably as small as possible. For example, oxygen and nitrogen as gas components are 1000 mass ppm or less, and impurity elements such as Ni and Si other than gas components inevitably contained are 1000 mass ppm in total. The following is preferable.
本発明の上記特性を具備する軟磁性膜の形成には、軟磁性膜の組成と同一組成のスパッタリングターゲットを用いたスパッタリング法が最適である。そして、本発明の別の発明は、原子比における組成式が、（ＣｏａＦｅ１−ａ）１００−ｂ−ｃＮｂｂＭｃ、０．５０≦ａ≦０．９０、３≦ｂ≦１４、３≦ｃ≦１９、１６≦ｂ＋ｃ≦２４、Ｍは、Ｍｏ、ＣｒおよびＷからなる群から選ばれる１種以上の元素、残部が不可避的不純物からなる軟磁性膜形成用スパッタリングターゲットである。A sputtering method using a sputtering target having the same composition as that of the soft magnetic film is optimal for forming the soft magnetic film having the above characteristics of the present invention. In another aspect of the present invention, the composition formula in atomic ratio is (Co a Fe 1-a ) 100- bc Nb b M c , 0.50 ≦ a ≦ 0.90, 3 ≦ b ≦ 14. 3 ≦ c ≦ 19, 16 ≦ b + c ≦ 24, M is a sputtering target for forming a soft magnetic film, wherein one or more elements selected from the group consisting of Mo, Cr, and W, and the balance is unavoidable impurities.
本発明のスパッタリングターゲットの製造方法としては、例えば溶製法や粉末焼結法が適用可能である。溶製法では、鋳造インゴット、もしくは鋳造インゴット中に存在する鋳造欠陥の低減や組織の均一化を図るために、塑性加工や加圧加工を加えてバルク体とし、これに機械加工を施すことで製造できる。
また、粉末焼結法では、原料粉末を例えば熱間静水圧プレス、ホットプレス、放電プラズマ焼結、押し出しプレス焼結等の加圧焼結することにより製造できる。中でも、熱間静水圧プレスは、以下に述べる加圧焼結条件を安定して実現できるため、好適である。As a method for producing the sputtering target of the present invention, for example, a melting method or a powder sintering method can be applied. In the melting method, in order to reduce the casting defects existing in the casting ingot or the casting ingot and to make the structure uniform, plastic processing and pressure processing are applied to form a bulk body, which is then manufactured by machining. it can.
In the powder sintering method, the raw material powder can be manufactured by pressure sintering such as hot isostatic pressing, hot pressing, discharge plasma sintering, extrusion press sintering, and the like. Among these, the hot isostatic press is preferable because it can stably realize the pressure sintering conditions described below.
本発明で粉末焼結法を適用する場合は、原料粉末として、複数の合金粉末や純金属粉末を最終組成になるように混合した混合粉末や、最終組成に調整した合金粉末が適用できる。
また、最終組成に調整した粉末を加圧焼結する方法では、Ｎｂを含有する金属間化合物相を安定的に微細で均一分散できる効果を有する。本発明では、最終組成の合金粉末の紛体組成物を加圧焼結することが好ましい。When the powder sintering method is applied in the present invention, a mixed powder obtained by mixing a plurality of alloy powders or pure metal powders to have a final composition, or an alloy powder adjusted to the final composition can be applied as a raw material powder.
Further, the method of pressure sintering the powder adjusted to the final composition has an effect of stably finely and uniformly dispersing the intermetallic compound phase containing Nb. In the present invention, it is preferable to press-sinter the powder composition of the final alloy powder.
また、上述の加圧焼結に用いる原料粉末は、所望の組成に成分調整した合金溶湯を鋳造したインゴットを粉砕する方法や、上記合金溶湯を不活性ガスにより噴霧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、充填率の高い、焼結に適した球状粉末が得られるガスアトマイズ法が好ましい。尚、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。 Moreover, the raw material powder used for the above-mentioned pressure sintering can be produced by a method of pulverizing an ingot obtained by casting a molten alloy whose components are adjusted to a desired composition, or a gas atomizing method in which the molten alloy is sprayed with an inert gas. Is possible. Of these, the gas atomization method is preferred, in which a spherical powder suitable for sintering having a low filling rate and a high filling rate is obtained. In order to suppress oxidation of the spherical powder, it is preferable to use Ar gas or nitrogen gas, which is an inert gas, as the atomizing gas.
また、上述の加圧焼結における焼結温度は、８００℃以上にすることで、高融点金属であるＮｂやＭ元素を含有する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、焼結温度を１４００℃以下にすることで、合金粉末の溶解を防止できる。このため、本発明では、焼結温度を８００〜１４００℃とすることが好ましい。尚、空孔の形成を最小限に低減した上で、Ｎｂを含有する金属間化合物相の成長を抑制するためには、９００〜１３００℃の温度で焼結することがより好ましい。
また、上述の加圧焼結における加圧圧力は、１００ＭＰａ以上にすることで、焼結の進行を助長し、空孔の発生を抑制することができる。また、加圧圧力を２００ＭＰａ以下にすることで、焼結時にスパッタリング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。このため、本発明では、加圧圧力を１００〜２００ＭＰａとすることが好ましい。尚、より空孔の形成を最小限に低減し、残留応力の導入をさらに抑制するためには、１２０〜１６０ＭＰａの加圧圧力で焼結することがより好ましい。
また、上述の加圧焼結における焼結時間は、１時間以上にすることで、焼結の進行を助長し、空孔の発生を抑制することができる。また、焼結時間を１０時間以下とすることで、製造効率を悪化させないで、Ｎｂを含有する金属間化合物相の成長を抑制して製造できる。このため、本発明では、焼結時間を１〜１０時間とすることが好ましい。尚、空孔の形成を最小限に低減し、Ｎｂを含有する金属間化合物相の成長をさらに抑制するためには、１〜３時間の焼結時間で焼結することがより好ましい。In addition, by setting the sintering temperature in the above-mentioned pressure sintering to 800 ° C. or higher, the sintering of the powder containing Nb or M element, which is a high melting point metal, can be advanced, and the generation of voids can be promoted. Can be suppressed. Moreover, melt | dissolution of alloy powder can be prevented by making sintering temperature into 1400 degrees C or less. For this reason, in this invention, it is preferable that a sintering temperature shall be 800-1400 degreeC. It is more preferable to sinter at a temperature of 900 to 1300 ° C. in order to suppress the formation of voids to a minimum and suppress the growth of the intermetallic compound phase containing Nb.
Moreover, the pressurization pressure in the above-mentioned pressure sintering can be set to 100 MPa or more to promote the progress of sintering and suppress the generation of pores. Moreover, by setting the pressurizing pressure to 200 MPa or less, introduction of residual stress to the sputtering target during sintering can be suppressed, and generation of cracks after sintering can be suppressed. For this reason, in this invention, it is preferable that a pressurization pressure shall be 100-200 MPa. In order to further reduce the formation of pores and further suppress the introduction of residual stress, it is more preferable to sinter at a pressure of 120 to 160 MPa.
In addition, by setting the sintering time in the above-described pressure sintering to 1 hour or longer, the progress of the sintering can be promoted and the generation of pores can be suppressed. Moreover, it can manufacture by suppressing the growth of the intermetallic compound phase containing Nb, without making manufacturing efficiency worse by making sintering time into 10 hours or less. For this reason, in this invention, it is preferable to make sintering time into 1 to 10 hours. In order to reduce the formation of vacancies to the minimum and further suppress the growth of the intermetallic compound phase containing Nb, it is more preferable to sinter with a sintering time of 1 to 3 hours.
（本発明例１）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．７０Ｆｅ０．３０）８２Ｎｂ９Ｗ９の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製し、２５０μｍの篩で分級し、粗粒を除去した。
そして、得られたガスアトマイズ粉末を軟鋼製のカプセルに充填し、脱気封止した後、温度９５０℃、圧力１２２ＭＰａ、保持時間１時間の条件で熱間静水圧プレスによって加圧焼結し、焼結体を作製した。得られた焼結体に機械加工を施し、直径１８０ｍｍ×厚さ５ｍｍの軟磁性膜形成用のスパッタリングターゲットを得た。(Invention Example 1)
First, using a raw material with a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.70 Fe 0.30 ) 82 Nb 9 W 9 in an atomic ratio is melted in vacuo, and Ar gas A gas atomized powder was prepared by a gas atomizing method according to, and classified with a 250 μm sieve to remove coarse particles.
And after filling the obtained gas atomized powder into the capsule made from mild steel and carrying out deaeration sealing, it pressurizes and sinters by hot isostatic pressing on the conditions of temperature 950 degreeC, pressure 122MPa, holding
上記で作製した軟磁性膜形成用スパッタリングターゲットを、キヤノンアネルバ製のＤＣマグネトロンスパッタ装置（Ｃ−３０１０）のチャンバー内に配置し、チャンバ内の真空到達度が２×１０−５Ｐａ以下となるまで排気を行なった後、寸法７５ｍｍ×２５ｍｍのガラス基板上に、Ａｒガス圧０．６Ｐａ、投入電力１０００Ｗの条件で、膜厚３００ｎｍの軟磁性膜をスパッタリング成膜した。The soft magnetic film forming sputtering target produced above is placed in the chamber of a DC magnetron sputtering apparatus (C-3010) manufactured by Canon Anelva, and the vacuum reach in the chamber is 2 × 10 −5 Pa or less. After evacuation, a 300 nm thick soft magnetic film was formed by sputtering on a glass substrate having dimensions of 75 mm × 25 mm under conditions of Ar gas pressure of 0.6 Pa and input power of 1000 W.
（本発明例２）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．５５Ｆｅ０．４５）８２Ｎｂ９Ｍｏ９の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、本発明例１と同様の条件で軟磁性膜形成用のスパッタリングターゲットを作製した。
そして、上記で作製した軟磁性膜形成用スパッタリングターゲットを用いて、実施例１と同様の条件で軟磁性膜をスパッタリング成膜した。(Invention Example 2)
First, using a raw material with a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.55 Fe 0.45 ) 82 Nb 9 Mo 9 in a composition formula in atomic ratio is vacuum-dissolved, and Ar gas A sputtering target for forming a soft magnetic film was produced under the same conditions as in Example 1 of the present invention, except that a gas atomized powder was produced by the gas atomization method according to 1.
Then, a soft magnetic film was formed by sputtering under the same conditions as in Example 1 using the soft magnetic film forming sputtering target prepared above.
（本発明例３）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．７０Ｆｅ０．３０）８２Ｎｂ９Ｃｒ９の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、本発明例１と同様の条件で軟磁性膜形成用のスパッタリングターゲットを作製した。
そして、上記で作製した軟磁性膜形成用スパッタリングターゲットを用いて、実施例１と同様の条件で軟磁性膜をスパッタリング成膜した。(Invention Example 3)
First, using a raw material having a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.70 Fe 0.30 ) 82 Nb 9 Cr 9 in an atomic ratio composition formula is vacuum-dissolved, and Ar gas A sputtering target for forming a soft magnetic film was produced under the same conditions as in Example 1 of the present invention, except that a gas atomized powder was produced by the gas atomization method according to 1.
Then, a soft magnetic film was formed by sputtering under the same conditions as in Example 1 using the soft magnetic film forming sputtering target prepared above.
（本発明例４）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．７０Ｆｅ０．３０）８３Ｎｂ１４Ｗ３の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、本発明例１と同様の条件で軟磁性膜形成用のスパッタリングターゲットを作製した。
そして、上記で作製した軟磁性膜形成用スパッタリングターゲットを用いて、実施例１と同様の条件で軟磁性膜をスパッタリング成膜した。(Invention Example 4)
First, using a raw material having a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.70 Fe 0.30 ) 83 Nb 14 W 3 in an atomic ratio is melted in vacuo, and Ar gas is used. A sputtering target for forming a soft magnetic film was produced under the same conditions as in Example 1 of the present invention, except that a gas atomized powder was produced by the gas atomization method according to 1.
Then, a soft magnetic film was formed by sputtering under the same conditions as in Example 1 using the soft magnetic film forming sputtering target prepared above.
（比較例１）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．３５Ｆｅ０．６５）８１．５Ｔａ１８．５の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、本発明例１と同様の条件で軟磁性膜形成用のスパッタリングターゲットを作製した。
そして、上記で作製した軟磁性膜形成用スパッタリングターゲットを用いて、実施例１と同様の条件で軟磁性膜をスパッタリング成膜した。(Comparative Example 1)
First, using a raw material having a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.35 Fe 0.65 ) 81.5 Ta 18.5 in a composition formula in atomic ratio is vacuum-dissolved, A sputtering target for forming a soft magnetic film was prepared under the same conditions as Example 1 except that gas atomized powder was prepared by a gas atomizing method using Ar gas.
Then, a soft magnetic film was formed by sputtering under the same conditions as in Example 1 using the soft magnetic film forming sputtering target prepared above.
（比較例２）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．３５Ｆｅ０．６５）８２Ｎｂ９Ｗ９の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、本発明例１と同様の条件で軟磁性膜形成用のスパッタリングターゲットを作製した。
そして、上記で作製した軟磁性膜形成用スパッタリングターゲットを用いて、実施例１と同様の条件で軟磁性膜をスパッタリング成膜した。(Comparative Example 2)
First, using a raw material having a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.35 Fe 0.65 ) 82 Nb 9 W 9 in a composition formula in atomic ratio is vacuum-dissolved, and Ar gas A sputtering target for forming a soft magnetic film was produced under the same conditions as in Example 1 of the present invention, except that a gas atomized powder was produced by the gas atomization method according to 1.
Then, a soft magnetic film was formed by sputtering under the same conditions as in Example 1 using the soft magnetic film forming sputtering target prepared above.
（比較例３）
まず、純度９９．９％以上の原料を用いて、原子比における組成式で、（Ｃｏ０．３４Ｆｅ０．６６）６７Ｃｒ２０Ｂ１３の合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、本発明例１と同様の条件で軟磁性膜形成用のスパッタリングターゲットを作製した。
そして、上記で作製した軟磁性膜形成用のスパッタリングターゲットを用いて、実施例１と同様の条件で軟磁性膜をスパッタリング成膜した。(Comparative Example 3)
First, using a raw material having a purity of 99.9% or more, a molten alloy having an alloy composition of (Co 0.34 Fe 0.66 ) 67 Cr 20 B 13 in a composition formula in atomic ratio is vacuum-dissolved, and Ar gas A sputtering target for forming a soft magnetic film was produced under the same conditions as in Example 1 of the present invention, except that a gas atomized powder was produced by the gas atomization method according to 1.
A soft magnetic film was formed by sputtering under the same conditions as in Example 1 using the soft magnetic film forming sputtering target prepared above.
上記で成膜した各軟磁性膜の試料を、さらに寸法６ｍｍ×７ｍｍに加工した後、東英工業株式会社製の振動試料型磁力計（ＶＳＭ−５−２０）を使用し、面内方向に最大磁場８０ｋＡ／ｍを印加したまま、昇温速度０．２℃／ｓｅｃで、室温（２５℃）から４１０℃まで加熱し、Ｂｓを測定した。
代表例として、本発明例１および比較例２の測定結果を図１に示す。また、各軟磁性膜の２５℃および１００℃におけるＢｓの測定結果と、１００℃におけるＢｓの２５℃におけるＢｓからの低下率を表１に示す。Each soft magnetic film sample formed as described above is further processed into a size of 6 mm × 7 mm, and then a vibration sample type magnetometer (VSM-5-20) manufactured by Toei Kogyo Co., Ltd. is used. While applying the maximum magnetic field of 80 kA / m, the sample was heated from room temperature (25 ° C.) to 410 ° C. at a heating rate of 0.2 ° C./sec, and Bs was measured.
As a representative example, the measurement results of Invention Example 1 and Comparative Example 2 are shown in FIG. Table 1 shows the measurement results of Bs at 25 ° C. and 100 ° C. of each soft magnetic film, and the rate of decrease of Bs at 100 ° C. from Bs at 25 ° C.
表１より、本発明の範囲外の比較例となる軟磁性膜は、１００℃におけるＢｓが０．５０Ｔ未満であった。これに対し、本発明の軟磁性膜は、１００℃におけるＢｓが０．５０Ｔ以上であり、Ｂｓの高温特性に優れた軟磁性膜であることが確認できた。
また、本発明の範囲外の比較例となる軟磁性膜は、いずれも２５℃から１００℃におけるＢｓの低下値が０．１０Ｔを超え、低下率は２６％以上であり、大幅な低下であった。これに対し、本発明の軟磁性膜は、２５℃から１００℃におけるＢｓの低下値は０．１０Ｔ未満、低下率は１１％以下であり、Ｂｓの高温特性に優れた軟磁性膜であることが確認できた。
そして、本発明の軟磁性膜は、本発明の軟磁性膜形成用のスパッタリングターゲットにより形成可能であることが確認され、本発明の有効性が確認できた。From Table 1, the Bs at 100 ° C. of the soft magnetic film serving as a comparative example outside the scope of the present invention was less than 0.50T. On the other hand, the soft magnetic film of the present invention has a Bs at 100 ° C. of 0.50 T or more, and was confirmed to be a soft magnetic film excellent in the high temperature characteristics of Bs.
In addition, all of the soft magnetic films as comparative examples outside the scope of the present invention had a Bs decrease value of 0.10 T from 25 ° C. to 100 ° C. and a decrease rate of 26% or more, which was a significant decrease. It was. On the other hand, the soft magnetic film of the present invention is a soft magnetic film excellent in the high temperature characteristics of Bs with a decrease value of Bs of less than 0.10 T and a decrease rate of 11% or less at 25 ° C. to 100 ° C. Was confirmed.
And it was confirmed that the soft magnetic film of this invention can be formed with the sputtering target for soft magnetic film formation of this invention, and the effectiveness of this invention was confirmed.
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| JP6161991B2 (en) * | 2013-08-15 | 2017-07-12 | 山陽特殊製鋼株式会社 | Fe-Co alloy sputtering target material |
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| WO2016157922A1 (en) | 2016-10-06 |
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