JP6210503B2 - Soft magnetic alloy for magnetic recording and sputtering target material - Google Patents
Soft magnetic alloy for magnetic recording and sputtering target material Download PDFInfo
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- JP6210503B2 JP6210503B2 JP2012179238A JP2012179238A JP6210503B2 JP 6210503 B2 JP6210503 B2 JP 6210503B2 JP 2012179238 A JP2012179238 A JP 2012179238A JP 2012179238 A JP2012179238 A JP 2012179238A JP 6210503 B2 JP6210503 B2 JP 6210503B2
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- 238000005477 sputtering target Methods 0.000 title claims description 17
- 239000013077 target material Substances 0.000 title claims description 10
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims description 8
- 239000012535 impurity Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 description 12
- 239000000956 alloy Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 230000035939 shock Effects 0.000 description 8
- 230000004907 flux Effects 0.000 description 7
- 238000010791 quenching Methods 0.000 description 7
- 230000000171 quenching effect Effects 0.000 description 7
- 238000004544 sputter deposition Methods 0.000 description 7
- 238000005336 cracking Methods 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 229910052735 hafnium Inorganic materials 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910002546 FeCo Inorganic materials 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 125000001475 halogen functional group Chemical group 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910017061 Fe Co Inorganic materials 0.000 description 2
- 238000005280 amorphization Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 101000993059 Homo sapiens Hereditary hemochromatosis protein Proteins 0.000 description 1
- 229910015234 MoCo Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
- G11B5/64—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent
- G11B5/66—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent the record carriers consisting of several layers
- G11B5/667—Record carriers characterised by the selection of the material comprising only the magnetic material without bonding agent the record carriers consisting of several layers including a soft magnetic layer
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
-
- 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
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- 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
- H01F41/183—Sputtering targets therefor
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Magnetic Record Carriers (AREA)
- Soft Magnetic Materials (AREA)
- Thin Magnetic Films (AREA)
Description
本発明は、磁気記録媒体における軟磁性薄膜層用アモルファス合金およびスパッタリングターゲット材に関する。 The present invention relates to amorphous alloys and sputtering target material for soft magnetic thin film layer in the magnetic recording medium.
近年、垂直磁気記録の進歩は著しく、ドライブの大容量化のために、磁気記録媒体の高記録密度化が進められており、従来普及していた面内磁気記録媒体により、さらに高記録密度が実現できる、垂直磁気記録方式が実用化されている。ここで、垂直磁気記録方式とは、垂直磁気記録媒体の磁性膜中の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、高記録密度に適した方法である。 In recent years, the progress of perpendicular magnetic recording has been remarkable, and in order to increase the capacity of the drive, the recording density of the magnetic recording medium has been increased. A realizable perpendicular magnetic recording system has been put into practical use. Here, the perpendicular magnetic recording method is a method suitable for high recording density, in which the easy axis of magnetization is oriented perpendicularly to the medium surface in the magnetic film of the perpendicular magnetic recording medium. .
そこで、最近では１０ｋＧ程度の比較的小さい磁性（Ｂｓ）の合金組成を持つ軟磁性薄膜が使用されつつある。例えば、特開２０１１−１８１１４０号公報（特許文献１）に開示されているように、軟磁性膜としてＦｅ−Ｃｏ系合金中にアモルファス性と結晶化温度を高めるための最適な元素としてＮｂおよび／またはＴａとＢとを選択し、アモルファス性が高く、かつ高い結晶化温度を有する磁気記録媒体に用いられるＦｅ−Ｃｏ系合金軟磁性膜が提案されている。 Therefore, recently, a soft magnetic thin film having a relatively small magnetic (Bs) alloy composition of about 10 kG is being used. For example, as disclosed in Japanese Patent Application Laid-Open No. 2011-181140 (Patent Document 1), Nb and / or as an optimum element for increasing the amorphous nature and the crystallization temperature in an Fe—Co alloy as a soft magnetic film. Alternatively, an Fe—Co alloy soft magnetic film has been proposed in which Ta and B are selected and used for a magnetic recording medium having a high amorphous property and a high crystallization temperature.
また、特開２０１１−８６３５６号公報（特許文献２）に開示されているように、下地層の飽和磁束密度（Ｍｓ）を高めつつ、中間層の核発生を抑制する効果を維持することによって、優れたオーバーライト（ＯＷ）特性を得ることを可能とした垂直磁気記録媒体、並びにそのような垂直磁気記録媒体を備えた磁気記録再生装置が提案されている。 Further, as disclosed in Japanese Patent Application Laid-Open No. 2011-86356 (Patent Document 2), by increasing the saturation magnetic flux density (Ms) of the underlayer while maintaining the effect of suppressing the nucleation of the intermediate layer, A perpendicular magnetic recording medium capable of obtaining an excellent overwrite (OW) characteristic and a magnetic recording / reproducing apparatus including such a perpendicular magnetic recording medium have been proposed.
また、特開２００８−２９９０５号公報（特許文献３）に開示されているように、飽和磁束密度、非晶質性、耐候性に優れた垂直磁気記録媒体における軟磁性膜層用合金が提案されている。しかし、その合金の成分組成がＺｒ，Ｈｆ，Ｎｂ，ＴａにＡｌ，Ｃｒを含有させたＦｅＣｏ系合金であって、ＦｅＣｏ系合金に主成分とするＭｏ，Ｗを含有させたものではない。 Further, as disclosed in Japanese Patent Application Laid-Open No. 2008-29905 (Patent Document 3), an alloy for a soft magnetic film layer in a perpendicular magnetic recording medium excellent in saturation magnetic flux density, amorphousness, and weather resistance has been proposed. ing. However, the component composition of the alloy is an FeCo alloy in which Al and Cr are contained in Zr, Hf, Nb, and Ta, and the MoCo and the main components are not contained in the FeCo alloy.
また、特開２０１１−２０８２６５号公報（特許文献４）や特開２０１１−２１４０３９号公報（特許文献５）には、磁気記録媒体や光磁気（ＭＯ）記録媒体の製造に利用され、高い磁場透過率（ＰＴＦ）を有するスパッタリングターゲットの製造方法において、Ｆｅ，Ｃｏ，Ｎｉを主成分とし、これに主成分以外の１つの元素を含む粉末原料を熱間で成形し、冷却したターゲットの製造方法や、さらに機械加工した後熱処理し、透過率を低減したターゲットの製造方法が提案されている。この方法に係る成分組成は、いずれもＭｏ，Ｗの含有量が低いためにＢｓが高すぎ、本発明が特徴とする１０ｋＧ以下の小さいＢｓを有する組成とは異なる。 Japanese Patent Application Laid-Open No. 2011-208265 (Patent Document 4) and Japanese Patent Application Laid-Open No. 2011-214039 (Patent Document 5) are used for manufacturing a magnetic recording medium and a magneto-optical (MO) recording medium, and have high magnetic field transmission. In a method for producing a sputtering target having a rate (PTF), a raw material containing Fe, Co, Ni as a main component and one element other than the main component is hot-formed and cooled, Further, a method for manufacturing a target in which the heat treatment is performed after further machining and the transmittance is reduced has been proposed. The component composition according to this method is different from the composition having a small Bs of 10 kG or less, which is characterized by the present invention, because Bs is too high because the contents of Mo and W are low.
また、特開２０１２−４８７６７号公報（特許文献６）には、垂直磁気記録媒体における軟磁性層膜として用いるＣｏ−（Ｚｒ，Ｈｆ）−Ｂ系合金およびスパッタリングターゲット材並びに磁気記録媒体が提案されている。しかし、この特許文献はＺｒ，Ｈｆの含有量を５ａｔ％以上と高い成分組成を対象としたものである。 Japanese Patent Laying-Open No. 2012-48767 (Patent Document 6) proposes a Co— (Zr, Hf) —B alloy, a sputtering target material, and a magnetic recording medium used as a soft magnetic layer film in a perpendicular magnetic recording medium. ing. However, this patent document is intended for a component composition having a high Zr and Hf content of 5 at% or more.
さらに、特開２０１２−１０８９９７号公報（特許文献７）には、垂直磁気記録媒体における軟磁性層膜として用いるＣｏ−（Ｔｉ，Ｚｒ，Ｈｆ）系合金およびスパッタリングターゲット材並びに磁気記録媒体が提案されている。しかし、この合金成分の場合も、上記特許文献６と同様に、Ｔｉ，Ｚｒ，Ｈｆの含有量が５ａｔ％以上と高い成分組成を対象としたものである。
その一方で、このようにＴａやＮｂを１０％を超えて多量に添加したスパッタリングターゲットや、Ｔｉ，Ｚｒ，Ｈｆのような５％以上を超えて多量に添加したスパッタリングターゲットでは、スパッタリングターゲットを使用、すなわち、スパッタリング中にスパッタリングターゲットが割れる現象が起きることがある。その理由は明確ではないが、スパッタリング中にはスパッタリングターゲットのスパッタされる面では数百度から１０００℃を超えると推定されるように加熱される一方、反対側の面はスパッタリング装置の冷却板に密着しており、常温に維持されているように、スパッタリングターゲットの厚みの中に大きな熱勾配を有すると共に、スパッタリングが数秒単位でオンオフが繰り返されるような、厳しい熱環境が割れの原因と推定される。このような熱環境下でも割れないスパッタリングターゲットの特性を、「耐サーマルショック性」と呼ぶことにする。 On the other hand, a sputtering target in which Ta or Nb is added in a large amount exceeding 10%, or a sputtering target added in a large amount exceeding 5% such as Ti, Zr, or Hf uses a sputtering target. That is, a phenomenon that the sputtering target breaks during sputtering may occur. The reason is not clear, but during sputtering, the surface to be sputtered is heated so that the surface to be sputtered is estimated to be several hundred degrees to over 1000 ° C., while the opposite surface is in close contact with the cooling plate of the sputtering apparatus. As it is maintained at room temperature, a severe thermal environment in which the sputtering target has a large thermal gradient in the thickness and the sputtering is repeatedly turned on and off in units of several seconds is presumed to cause cracking. . The characteristic of a sputtering target that does not break under such a thermal environment is referred to as “thermal shock resistance”.
上述した問題を解消するために鋭意開発を進めた結果、ＭｏＷはＦｅＣｏに固溶度を有し、それ故生成する金属間化合物量が低減すること、およびＦｅＣｏ固溶体にＭｏＷが固溶して熱膨張率が金属間化合物に近づくことにより、耐サーマルショック性が改善されることを見出し発明に至った。その発明の要旨とするところは
（１）ａｔ．％比で、１００Ｆｅ／（Ｆｅ＋Ｃｏ）：３０〜７０、ただし、Ｆｅ＞２０．４、かつ下記（Ａ）群の各種元素の１種または２種を１０〜３０％含有し、残部Ｃｏおよび不可避的不純物からなることを特徴とする磁気記録用軟磁性合金。
（Ａ）Ｍｏ，Ｗ
As a result of diligent development to solve the above-mentioned problems, MoW has a solid solubility in FeCo, thus reducing the amount of intermetallic compound to be generated, and MoW is dissolved in FeCo solid solution and heated. It has been found that the thermal shock resistance is improved when the expansion coefficient approaches that of an intermetallic compound, leading to the invention. The gist of the invention is (1) at. % Ratio, 100Fe / (Fe + Co): 30 to 70, Fe> 20.4, and 10 to 30% of one or two kinds of various elements in group (A) below , with the remainder being Co and inevitable A soft magnetic alloy for magnetic recording, characterized by comprising impurities.
(A) Mo, W
（２）前記（１）に記載した磁気記録用軟磁性合金を用いたスパッタリングターゲット材にある。 (2) in the sputtering target material using the magnetic recording soft magnetic alloy according to (1).
以上述べたように、本発明は、耐サーマルショック性に優れた軟磁性合金およびそのスパッタリングターゲット材を提供することにある。 As described above, the present invention is to provide a soft magnetic alloy excellent in thermal shock resistance and a sputtering target material thereof.
以下、本発明に係わる成分組成の限定理由を説明する。
ａｔ．％比で、１００Ｆｅ／（Ｆｅ＋Ｃｏ）：３０〜７０、ただし、Ｆｅ＞２０．４
Ｆｅ、Ｃｏは、軟磁性材料を得るための元素である。しかし、ａｔ．％比で、７０を超えると、耐食性が劣化するために、その上限を７０とした。
Hereinafter, the reasons for limiting the component composition according to the present invention will be described.
at. % Ratio, 100Fe / (Fe + Co): 30 to 70, but Fe> 20.4
Fe and Co are elements for obtaining a soft magnetic material. However, at. If the percentage exceeds 70, the corrosion resistance deteriorates, so the upper limit was set to 70.
（Ａ）群の各種元素の１種または２種を１０〜３０％
（Ａ）群であるＭｏ，Ｗは、Ｃｏ合金において、非晶質化（アモルファス化性）を確保するための元素であり、その元素の１種または２種の合計含有量が、１０％未満では磁性が高すぎ、また、３０％を超えると、非磁性となることから、その範囲を１０〜３０％とした。
(A) 10-30% of one or two of the various elements in the group
Mo and W which are (A) groups are elements for ensuring amorphization (amorphization) in a Co alloy, and the total content of one or two of the elements is less than 10%. Then, the magnetism is too high, and if it exceeds 30%, it becomes non-magnetic, so the range was made 10-30%.
以下、本発明に係る合金について実施例によって具体的に説明する。
通常、垂直磁気記録媒体における薄膜は、その成分と同じ成分のスパッタリングターゲット材をスパッタし、ガラス基板などの上に成膜し得られる。ここでスパッタにより成膜された薄膜は急冷されている。これに対し、本発明では実施例、比較例の供試材として、単ロール式の液体急冷装置にて作製した急冷薄帯を用いている。これは実際にスパッタにより急冷され成膜された薄膜の、成分による諸特性への影響を、簡易的に液体急冷薄帯により評価したものである。
Hereinafter, the alloy according to the present invention will be specifically described with reference to examples.
Usually, a thin film in a perpendicular magnetic recording medium can be formed on a glass substrate by sputtering a sputtering target material having the same component. Here, the thin film formed by sputtering is rapidly cooled. On the other hand, in this invention, the quenching thin strip produced with the single roll type liquid quenching apparatus is used as a test material of an Example and a comparative example. This is a simple evaluation of the influence of the components on various properties of a thin film formed by quenching by sputtering in a simple manner using a liquid quenching ribbon.
［急冷薄帯の作製条件］
表１〜表３に示す成分組成に秤量した原料３０ｇを内径が１０ｍｍで深さが４０ｍｍ程度の水冷銅型に挿入して減圧したＡｒ雰囲気中でアーク溶解して凝固させ、急冷薄帯の溶解母材とした。急冷薄帯の作製条件は、単ロール方式で、内径１５ｍｍの石英管中にてこの溶解母材をセットし、出湯ノズルの内径を１ｍｍとし、雰囲気気圧を６１ｋＰａ、噴霧差圧を６９ｋＰａ、銅ロール（径３００ｍｍ）の回転数を３０００ｒｐｍ、銅ロールと出湯ノズルのギャップを０．３ｍｍにして溶解母材を溶解後出湯した。出湯温度は各溶解母材の溶け落ち直後の温度とした。このようにして作製した急冷薄帯を供試材とし、以下の項目を評価した。
[Conditions for quenching ribbon]
30 g of raw materials weighed to the composition shown in Tables 1 to 3 were inserted into a water-cooled copper mold having an inner diameter of 10 mm and a depth of about 40 mm, and arc-melted in a reduced Ar atmosphere to solidify and melt the rapidly cooled ribbon A base material was used. The conditions for preparing the quenching ribbon are a single roll method, this molten base material is set in a quartz tube having an inner diameter of 15 mm, the inner diameter of the tap nozzle is 1 mm, the atmospheric pressure is 61 kPa, the spray differential pressure is 69 kPa, and the copper roll (The diameter of 300 mm) was set to 3000 rpm, the gap between the copper roll and the hot water nozzle was set to 0.3 mm, and the molten base material was melted to discharge hot water. The hot water temperature was the temperature immediately after each molten base material was melted. The following items were evaluated using the thus prepared quenched ribbon as a test material.
［急冷薄帯の飽和磁束密度の評価］
急冷薄帯の飽和磁束密度（Ｂｓ）の評価としては、ＶＳＭ装置（振動試料型磁力計）にて、印加磁場１２００ｋＡ／ｍ、供試材の重量は１５ｍｇ程度で飽和磁束密度を測定した。
[Evaluation of saturation magnetic flux density of quenched ribbon]
For the evaluation of the saturation magnetic flux density (Bs) of the quenched ribbon, the saturation magnetic flux density was measured with an applied magnetic field of 1200 kA / m and a weight of the test material of about 15 mg with a VSM apparatus (vibrating sample magnetometer).
［急冷薄帯の構造］
急冷薄帯の非晶質性の評価としては、通常、非晶質材料のＸ線回折パターンを測定すると、回折ピークが見られず、非晶質特有のハローパターンとなる。また、完全な非晶質でない場合は、回折ピークは見られるものの、結晶材料と比較してピーク高さが低くなり、かつハローパターンも見られる。そこで下記の方法にて非晶質性の評価とした。
[Structure of quenched ribbon]
As an evaluation of the amorphous property of the quenched ribbon, usually, when an X-ray diffraction pattern of an amorphous material is measured, a diffraction peak is not seen and a halo pattern peculiar to an amorphous state is obtained. Moreover, when it is not completely amorphous, although a diffraction peak is seen, a peak height becomes low compared with a crystalline material, and a halo pattern is also seen. Therefore, the amorphous property was evaluated by the following method.
［非晶質性の評価］
非晶質性の評価としては、ガラス板に両面テープで供試材を貼り付け、Ｘ線回折装置にて回折パターンを得た。このとき、測定面は急冷薄帯の銅ロール接触面となるように供試材を貼り付けた。Ｘ線源はＣｕ−α線で、スキャンスピード４°／ｍｉｎで測定した。この回折パターンにハローパターンが確認できるものを○、全くハローパターンが見られないものを×として非晶質性の評価とした。
[Amorphous evaluation]
For evaluation of amorphousness, a test material was attached to a glass plate with a double-sided tape, and a diffraction pattern was obtained with an X-ray diffractometer. At this time, the test material was affixed so that a measurement surface might become a copper roll contact surface of a rapidly cooled ribbon. The X-ray source was Cu-α ray, and measurement was performed at a scan speed of 4 ° / min. In this diffraction pattern, the evaluation of the amorphous property was evaluated as ◯ when the halo pattern could be confirmed, and x when no halo pattern was observed.
［急冷薄帯の耐食性評価（ＮａＣｌ）］
ガラスペレットに急冷薄帯を両面テープで貼り付けた試料にて、塩水噴霧試験（５％ＮａＣｌ水溶液で３５℃にて１６時間噴霧）を実施した評価で、発錆が認められなかったものを○、発錆が認められたものを×とした。
[Evaluation of corrosion resistance of quenched ribbon (NaCl)]
A sample in which a quenching ribbon was attached to a glass pellet with a double-sided tape, and a salt spray test (sprayed at 35 ° C. for 16 hours with a 5% NaCl aqueous solution) was conducted. The case where rusting was observed was rated as x.
耐サーマルショック性はターゲットを作製し、所定の温度からの水冷により割れるか割れないかを評価した。
［ターゲット作製方法］
表１〜表３に示す組成をガスアトマイズ法により軟磁性合金粉末を作製した。得られた粉末を５００μｍ以下に分級し、ＨＩＰ（熱間等方圧プレス）による固化成形加工の原料粉末として用いた。ＨＩＰ成形用ビレットは、直径２５０ｍｍ、長さ５０ｍｍの炭素鋼製の缶に原料粉末を充填したのち、蓋をして、真空脱気を施し、その後脱気孔を封入し作製した。この粉末を充填したビレットを１１５０℃に加熱した後、内径２３０ｍｍの拘束型コンテナ内に装入し、５００ＭＰａの加圧にて成形した。上記方法で作製した固化成形耐を、ワイヤーカットで切り出し、旋盤加工にて直径および厚さの寸法を調整し、平面研磨により厚さと表面粗さの仕上げを行って、直径１８０ｍｍ、厚さ７ｍｍの円盤状に加工し、スパッタリングターゲット材を作製した。
For thermal shock resistance, a target was prepared and evaluated whether it was cracked or not cracked by water cooling from a predetermined temperature.
[Target production method]
Soft magnetic alloy powders having the compositions shown in Tables 1 to 3 were prepared by gas atomization. The obtained powder was classified to 500 μm or less and used as a raw material powder for solidification molding by HIP (hot isostatic pressing). The billet for HIP molding was prepared by filling a raw material powder into a carbon steel can having a diameter of 250 mm and a length of 50 mm, and then covering the can with a vacuum, vacuum deaeration, and then enclosing the deaeration holes. The billet filled with this powder was heated to 1150 ° C., and then charged into a constraining container having an inner diameter of 230 mm and molded under a pressure of 500 MPa. The solidification resistance produced by the above method is cut out by wire cutting, the diameter and thickness are adjusted by lathe processing, and the thickness and surface roughness are finished by surface polishing, and the diameter is 180 mm and the thickness is 7 mm. A sputtering target material was fabricated by processing into a disk shape.
［耐サーマルショック性の評価］
上記で得たターゲットを３００℃から５０℃きざみで、７００℃までの各温度で１時間保持した後、水中へ投入することで急冷し、割れの発生状況を確認した。割れの発生した温度を割れ温度として評価した。割れ温度が４５０℃以上を耐サーマルショック性が良いとした。
[Evaluation of thermal shock resistance]
The target obtained above was held at 300 ° C. to 50 ° C. at each temperature up to 700 ° C. for 1 hour, and then rapidly cooled by throwing it into water to confirm the occurrence of cracks. The temperature at which cracking occurred was evaluated as the cracking temperature. A cracking temperature of 450 ° C. or higher was regarded as good thermal shock resistance.
表２に示す比較例Ｎｏ．２９、３０はＦｅ含有量が多いために、耐食性悪い。比較例Ｎｏ．３１は（Ａ）群のＭｏ元素の含有量が少ないために、Ｂｓが高い。比較例Ｎｏ．３２、３３、３４は（Ａ）群のＭｏ、Ｗ元素の含有量が多いために、割れ温度が低い。 Comparative Example No. 2 shown in Table 2 29 and 30 have poor corrosion resistance due to the high Fe content. Comparative Example No. No. 31 has a high Bs because the content of the Mo element in group (A) is small. Comparative Example No. 32 , 33 , and 34 have a low cracking temperature because they contain a large amount of Mo and W elements in group (A).
これに対して、本発明であるＮｏ．１〜２８は、いずれも本発明の条件を満足していることから、１０ｋＧ以下の比較的小さい飽和磁束密度（Ｂｓ）を得ることが可能となり、かつアモルファス性、耐食性および本発明の最大の特徴とする割れ温度が高く、所謂耐サーマルショック性に優れた合金を提供することができる。 On the other hand, No. which is the present invention. Since Nos. 1 to 28 all satisfy the conditions of the present invention, it is possible to obtain a relatively small saturation magnetic flux density (Bs) of 10 kG or less, and amorphous characteristics, corrosion resistance, and the greatest features of the present invention. An alloy having a high cracking temperature and excellent in so-called thermal shock resistance can be provided.
以上述べたように、本発明により、特に飽和磁束密度、非晶質性（アモルファス性）、および耐食性を確保し、かつ耐サーマルショック性に優れた磁気記録用軟磁性用合金およびそれを用いたスパッタリングターゲット材並びに磁気記録媒体を得ることを可能とした極めて優れた効果を奏するものである。
特許出願人 山陽特殊製鋼株式会社
代理人 弁理士 椎 名 彊
As described above, in accordance with the present invention, a soft magnetic alloy for magnetic recording and the use thereof, which particularly ensure saturation magnetic flux density, amorphousness (amorphousness), corrosion resistance, and excellent thermal shock resistance, are used. An extremely excellent effect is obtained that makes it possible to obtain a sputtering target material and a magnetic recording medium.
Patent Applicant Sanyo Special Steel Co., Ltd.
Attorney: Attorney Shiina
Claims (2)
（Ａ）Ｍｏ，Ｗ at. % Ratio, 100Fe / (Fe + Co): 30 to 70, but Fe> 20.4, and 10 to 30% of one or two kinds of various elements of group (A) below, with the remainder Co and unavoidable A soft magnetic alloy for magnetic recording, characterized by comprising impurities.
(A) Mo, W
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| JP2012179238A JP6210503B2 (en) | 2012-08-13 | 2012-08-13 | Soft magnetic alloy for magnetic recording and sputtering target material |
| SG11201408798PA SG11201408798PA (en) | 2012-08-13 | 2013-08-08 | Soft magnetic alloy for magnetic recording purposes, sputtering target material, and magnetic recording medium |
| PCT/JP2013/071484 WO2014027601A1 (en) | 2012-08-13 | 2013-08-08 | Soft magnetic alloy for magnetic recording purposes, sputtering target material, and magnetic recording medium |
| CN201380039614.4A CN104488029B (en) | 2012-08-13 | 2013-08-08 | Magnetic recording non-retentive alloy and sputtering target material and magnetic recording media |
| MYPI2015000091A MY171479A (en) | 2012-08-13 | 2013-08-08 | Soft magnetic alloy for magnetic recording purposes, sputtering target material, and magnetic recording medium |
| SG10201700410WA SG10201700410WA (en) | 2012-08-13 | 2013-08-08 | Soft magnetic alloy for magnetic recording purposes, sputtering target material, and magnetic recording medium |
| TW102128832A TWI478183B (en) | 2012-08-13 | 2013-08-12 | A magneto-magnetic recording medium for magnetic recording and a sputtering target, and a magnetic recording medium |
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| JP2012179238A JP6210503B2 (en) | 2012-08-13 | 2012-08-13 | Soft magnetic alloy for magnetic recording and sputtering target material |
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| CN104766685A (en) * | 2014-05-21 | 2015-07-08 | 北京北冶功能材料有限公司 | High-performance iron-cobalt soft magnetic alloy forging material |
| JP6506659B2 (en) * | 2015-08-24 | 2019-04-24 | 山陽特殊製鋼株式会社 | Amorphous alloy for magnetic recording, sputtering target material and magnetic recording medium |
| JP2017208147A (en) * | 2016-05-16 | 2017-11-24 | 日立金属株式会社 | Sputtering target for forming soft magnetic ground layer and soft magnetic ground layer |
| CN111850431B (en) * | 2019-09-23 | 2022-02-22 | 宁波中科毕普拉斯新材料科技有限公司 | Iron-based amorphous alloy containing sub-nanoscale ordered clusters, preparation method and nanocrystalline alloy derivative thereof |
| WO2024128075A1 (en) * | 2022-12-16 | 2024-06-20 | 株式会社プロテリアル | Sputtering target and production method therefor |
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| JP2524514B2 (en) * | 1987-09-21 | 1996-08-14 | 日立マクセル株式会社 | Magnetic recording media |
| JP2635402B2 (en) * | 1988-11-02 | 1997-07-30 | アルプス電気株式会社 | Soft magnetic alloy film |
| JPH0555036A (en) * | 1991-08-26 | 1993-03-05 | Tdk Corp | Soft magnetic thin film and its manufacture, soft magnetic multilayer film and its manufacture as well as magnetic head |
| JPH07272223A (en) * | 1994-03-29 | 1995-10-20 | Tdk Corp | Magneto-resistance effect type head |
| US20060110626A1 (en) * | 2004-11-24 | 2006-05-25 | Heraeus, Inc. | Carbon containing sputter target alloy compositions |
| JP4380577B2 (en) * | 2005-04-07 | 2009-12-09 | 富士電機デバイステクノロジー株式会社 | Perpendicular magnetic recording medium |
| JP4331182B2 (en) * | 2006-04-14 | 2009-09-16 | 山陽特殊製鋼株式会社 | Soft magnetic target material |
| JP4953082B2 (en) * | 2006-10-10 | 2012-06-13 | 日立金属株式会社 | Co-Fe-Zr alloy sputtering target material and method for producing the same |
| WO2009133921A1 (en) * | 2008-04-30 | 2009-11-05 | 山陽特殊製鋼株式会社 | Sputtering target material for producing intermediate layer film of perpendicular magnetic recording medium and thin film produced by using the same |
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| TW201413758A (en) | 2014-04-01 |
| CN104488029A (en) | 2015-04-01 |
| WO2014027601A1 (en) | 2014-02-20 |
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| TWI478183B (en) | 2015-03-21 |
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