WO2013047321A1 - Alloy used in soft-magnetic thin-film layer on perpendicular magnetic recording medium, sputtering-target material, and perpendicular magnetic recording medium having soft-magnetic thin-film layer - Google Patents

Alloy used in soft-magnetic thin-film layer on perpendicular magnetic recording medium, sputtering-target material, and perpendicular magnetic recording medium having soft-magnetic thin-film layer Download PDF

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WO2013047321A1
WO2013047321A1 PCT/JP2012/074065 JP2012074065W WO2013047321A1 WO 2013047321 A1 WO2013047321 A1 WO 2013047321A1 JP 2012074065 W JP2012074065 W JP 2012074065W WO 2013047321 A1 WO2013047321 A1 WO 2013047321A1
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alloy
recording medium
tla
film layer
magnetic recording
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PCT/JP2012/074065
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French (fr)
Japanese (ja)
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澤田　俊之
慶明 松原
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山陽特殊製鋼株式会社
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Priority to CN201280046629.9A priority Critical patent/CN103875035B/en
Priority to SG11201400805SA priority patent/SG11201400805SA/en
Publication of WO2013047321A1 publication Critical patent/WO2013047321A1/en

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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
    • G11B5/64—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
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • 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
    • 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
    • H01F10/126—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing rare earth metals
    • 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

Definitions

  • the present invention relates to a (Co, Fe) -lanthanoid alloy and a sputtering target material for a soft magnetic thin film layer in a perpendicular magnetic recording medium.
  • the progress of magnetic recording technology has been remarkable, and in order to increase the capacity of the drive, the recording density of the magnetic recording medium has been increased, and a higher recording density can be realized than the in-plane magnetic recording medium that has been popular in the past.
  • a perpendicular magnetic recording system has been put into practical use.
  • the perpendicular magnetic recording system is a method suitable for high recording density, in which the easy magnetization axis is oriented in the perpendicular direction with respect to the medium surface in the magnetic film of the perpendicular magnetic recording medium.
  • a two-layer recording medium having a magnetic recording film layer and a soft magnetic film layer with improved recording sensitivity has been developed.
  • a CoCrPt—SiO 2 alloy is used for the magnetic recording film layer.
  • a conventional soft magnetic film layer needs to have a high saturation magnetic flux density (hereinafter referred to as Bs) and an amorphous property. Further, depending on the application and use environment of the perpendicular magnetic recording medium, it has high corrosion resistance and high hardness. Various characteristics have been additionally required. For example, in Japanese Patent Application Laid-Open No. 2008-299905 (Patent Document 1), high Bs is obtained by adding Fe, and high hardness is obtained by adding B. In JP 2011-68985 (Patent Document 2), the corrosion resistance (weather resistance) is improved by adding Y or Ti.
  • an amorphous alloy having a low Bs is used for the soft magnetic layer of the perpendicular magnetic recording medium as described above. That is, an amorphous alloy having low Bs has a large decrease range of Bs as the temperature rises, and Bs under a temperature environment (for example, about 70 to 150 ° C.) higher than room temperature to which the drive is exposed becomes remarkably low. The function as the soft magnetic layer of the perpendicular magnetic recording medium cannot be sufficiently performed.
  • the present inventors have examined various additive elements in detail for Bs and temperature characteristics of the soft magnetic film alloy of the perpendicular magnetic recording medium. It was found that there is an inverse correlation between the Bs of B and the decrease in Bs from room temperature to 150 ° C. However, the addition of an element belonging to the lanthanoid deviates from this inverse correlation, and the present inventors found that the Bs reduction range up to 150 ° C. can be significantly reduced compared with an alloy having the same Bs at room temperature. .
  • an object of the present invention is to provide a soft magnetic alloy for perpendicular magnetic recording media having a high saturation magnetic flux density at a high temperature relative to a saturation magnetic flux density at room temperature, and a sputtering target material for producing a thin film of this alloy. is there.
  • a soft magnetic thin film layer made of the above alloy is provided.
  • a perpendicular magnetic recording medium having the soft magnetic thin film layer is provided.
  • a sputtering target material comprising the above alloy is provided.
  • the soft magnetic alloy for perpendicular magnetic recording media has a small decrease in Bs at a high temperature relative to Bs at room temperature, that is, a high temperature of about 70 to 150 ° C. at which the drive is exposed during use. , And a sputtering target material for producing a thin film of this alloy.
  • the alloy of the present invention in a perpendicular magnetic recording medium, the magnetic properties of the soft magnetic alloy can be fully exhibited, and the function of the soft magnetic thin film layer can be sufficiently enhanced. This can lead to an improvement in the performance of the magnetic recording medium.
  • FIG. 3 is a diagram showing an X-ray diffraction pattern of a 39% Co-39% Fe-8% Zr-6% B-8% (additive element) alloy made of a quenched ribbon. It is the figure which plotted Bs and Bs ratio of room temperature in Table 1. It is the figure which plotted Bs and Bs ratio of room temperature in Table 2.
  • Bs at room temperature and its temperature characteristics of the soft magnetic film alloy of the perpendicular magnetic recording medium were examined in detail for various additive elements. As a result, Bs at room temperature and Bs from room temperature to 150 ° C. It was found that there was an inverse correlation between the drop widths. However, when an element belonging to a lanthanoid was added, it was found that the inverse correlation relationship was removed, and the Bs decrease width up to 150 ° C. was significantly reduced as compared with an alloy having an equivalent Bs at room temperature.
  • the characteristics and operation of the amorphous soft magnetic alloy found by the present invention based on the above findings and having a small Bs decrease width at high temperatures relative to Bs at room temperature will be described below.
  • the elements belonging to the lanthanoids having atomic numbers 57 to 71 are La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu.
  • TLA 0.5 ⁇ TLA ⁇ 15 (TLA is the total amount of elements added to the lanthanoids having atomic numbers 57 to 71)
  • TAM Y + Ti + Zr + Hf + V + Nb + Ta + B / 2) Total amount of addition amount, B alone being 1/2 times the value.
  • TLA + TAM + TNM ⁇ 30 C + Al + Si + P + Cr + Mn + Ni + Cu + Zn + Ga + Ge + Mo + Sn + W total%)
  • the element belonging to the lanthanoids having atomic numbers of 57 to 71 is an essential element for reducing Bs at room temperature and suppressing the decrease of Bs at high temperature, and also has an amorphous promoting effect.
  • the material of the alloy composition of the present invention when crystalline it is also an element that forms brittle intermetallic compounds with Co and / or Fe.
  • Y, Ti, Zr, Hf, V, Nb, Ta, and B are elements that lower Bs at room temperature and have an amorphous promoting effect.
  • C, Al, Si, P, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Mo, Sn, and W are elements added to lower Bs at room temperature. Therefore, if the TLA is less than 0.5, the effect of suppressing the decrease in Bs at high temperatures is not sufficient, and if it exceeds 15, a large amount of brittle intermetallic compounds are produced. Processing becomes difficult. Further, if TLA + TAM is less than 5, the amorphous promoting effect is not sufficient. Further, when TLA + TAM + TNM exceeds 30, Bs at room temperature becomes excessively low.
  • the preferable range of each formula is as follows.
  • formula (1) preferably 1 ⁇ TLA ⁇ 13, more preferably 2 ⁇ TLA ⁇ 11.
  • formula (2) preferably 6 ⁇ TLA + TAM, more preferably 7 ⁇ TLA + TAM.
  • the range of the ratio of the Fe content and the total content of Fe and Co (hereinafter referred to as “Fe% / (Fe% + Co%)”) is not particularly limited, but the softness of the perpendicular magnetic recording medium is not limited.
  • the magnetic film those more than 0 and 0.90 or less are often used, and those having a value of 0.30 or more and 0.65 or less are more used.
  • a soft magnetic film layer in a perpendicular magnetic recording medium can be formed on a glass substrate or the like by sputtering a sputtering target material having the same component as that component.
  • the thin film formed by sputtering is rapidly cooled.
  • a quenching ribbon manufactured by a single roll type liquid quenching apparatus is used as a specimen. 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.
  • Experiment C a sputtering target material was actually produced, and a thin film produced by sputtering was evaluated.
  • 30 g of raw material weighed to a predetermined component was arc-melted in reduced-pressure Ar using a water-cooled copper mold having a diameter of about 10 mm and a depth of about 40 mm, to obtain a molten preform for the quenched ribbon. .
  • the conditions for preparing the quenched ribbon are a single roll method, set in this molten base material in a quartz tube having a diameter of 15 mm, the diameter of the hot water nozzle is 1 mm, the atmospheric pressure is 61 kPa, the spray differential pressure is 69 kPa, the copper roll (diameter is 300 mm). ) was set at 3000 rpm and the gap between the copper roll and the hot water nozzle was set to 0.3 mm, and the hot water was discharged.
  • the hot water temperature is not particularly limited, and the hot water is discharged immediately after each molten base material is completely melted.
  • the quenched ribbon thus prepared was used as a test material, and Bs and amorphous properties at room temperature and high temperature were evaluated.
  • Bs ratio the closer this Bs ratio is to 100%, the smaller the decrease in Bs from 30 ° C to 150 ° C.
  • 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, amorphousness was evaluated by the following method. The test material was attached to a glass plate with a double-sided tape, and a diffraction pattern was obtained with an X-ray diffractometer.
  • the test material was affixed on the glass plate so that the measurement surface was a copper roll contact surface of a quenched ribbon.
  • the X-ray source was Cu-k ⁇ ray, and the scan speed was 4 ° / min.
  • the evaluation of the amorphous property was evaluated as ⁇ when the halo pattern could be confirmed, and x when no halo pattern was observed.
  • machinability For the evaluation of the machinability of the sputtering target material, 5 kg of a base material weighed to a predetermined component was induction-melted in a refractory crucible under a reduced Ar atmosphere and then solidified. The size of the crucible is 120 mm in diameter and 150 mm in height. From the lower part of the ingot, a sputtering target material having a diameter of 95 mm and a thickness of 2 mm was produced by lathe processing, wire cutting processing, and plane polishing processing. Machinability was evaluated by the occurrence of chips and cracks during these processes.
  • the atmospheric pressure in the chamber was evacuated to 1 ⁇ 10 ⁇ 4 Pa or less, and Ar gas having a purity of 99.9% was added until the pressure reached 0.6 Pa to perform sputtering.
  • the thin film was formed on the glass substrate so as to have a thickness of 1.5 ⁇ m.
  • Bs and Bs ratio, and the crystal structure were evaluated similarly to the quenched ribbon.
  • two basic compositions were selected, a certain amount of additive element was added to each, and changes in Bs and Bs ratio at room temperature depending on the type of additive element were evaluated. The results are shown as Experiment A and Experiment B.
  • Table 1 shows various properties of the quenched ribbon with various elements added.
  • No. Nos. 1 to 10 are examples of the present invention.
  • Reference numerals 11 to 31 are comparative examples.
  • FIG. 2 shows a plot of room temperature Bs and Bs ratio in Table 1.
  • FIG. 2 shows that the composition added with an element other than the element belonging to the lanthanoid shows a correlation in which the Bs ratio also decreases with a decrease in Bs at room temperature, whereas the composition added with the element belonging to the lanthanoid clearly It can be seen that the Bs ratio is high despite the low Bs at room temperature.
  • Experiment B is an alloy in which Co is 39.6%, Fe is 48.4%, Ti is 3%, Zr is 2%, Nb is 3%, Ta is 2%, and the balance is 2%. And the effect of the type of additive element under a constant addition amount was evaluated.
  • No. 11 is an alloy containing no additive elements and blended so that Co, Fe, Ti, Zr, Nb, and Ta are 40.5 to 49.5 to 3 to 2 to 3 to 2.
  • Table 2 shows various properties of the quenched ribbon with various elements added.
  • No. 1-4 are examples of the present invention.
  • Reference numerals 5 to 14 are comparative examples.
  • FIG. 3 shows a plot of room temperature Bs and Bs ratio in Table 2.
  • FIG. 3 shows that the composition in which an element other than the element belonging to the lanthanoid is added has a correlation in which the Bs ratio also decreases with a decrease in Bs at room temperature. It can be seen that the Bs ratio is high despite the low Bs at room temperature.
  • Table 3 shows various properties of the sputtered thin film.
  • a to J are examples of the present invention, and a to j are comparative examples.
  • Comparative Example a is an example in which 5% Zr is added in place of 2% Nd and 3% Gd added in Invention Example A.
  • TLA the element belonging to the lanthanoid of the present invention example
  • the difference in Bs at room temperature is as small as 0.08 T or less.
  • the Bs ratio is 0.2% or less in the composition containing 0.5% or more of the element belonging to the lanthanoid in the pair other than J and j (samples from A to I) than in the composition (samples from a to i). 1 to 10% higher.
  • all of the sputtering target materials A to I and a to i could be processed without chipping.
  • the sample of J was not chipped during machining, but the sample of j was made of three sputtering target materials, but two of them were broken and could not be made, and the other one was made but chipped. There has occurred. Furthermore, since the sample of j has a large TLA + TAM + TNM of 31, Bs at room temperature is excessively low.

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Abstract

Provided is a soft-magnetic alloy for use in a perpendicular magnetic recording medium, said alloy having a high saturation flux density at high temperatures with respect to the saturation flux density thereof at room temperature. Said alloy contains the following: one or more lanthanide elements, which have atomic numbers from 57 to 71; and one or more elements selected from among yttrium, titanium, zirconium, hafnium, vanadium, niobium, tantalum, and boron and/or one or more elements selected from among carbon, aluminum, silicon, phosphorus, chromium, manganese, nickel, copper, zinc, gallium, germanium, molybdenum, tin, and tungsten. The remainder of said alloy comprises cobalt, iron, and unavoidable impurities. The atomic percentages of the constituent elements satisfy each of the following relations: (1) 0.5 ≤ TLA ≤ 15, (2) 5 ≤ TLA+TAM, and (3) TLA+TAM+TNM ≤ 30, with TLA representing the sum of the atomic percentages of the lanthanide elements, TAM representing Y+Ti+Zr+Hf+V+Nb+Ta+B/2 (with only the atomic percentage of boron halved), and TNM representing C+Al+Si+P+Cr+Mn+Ni+Cu+Zn+Ga+Ge+Mo+Sn+W.

Description

垂直磁気記録媒体における軟磁性薄膜層に用いる合金およびスパッタリングターゲット材並びに軟磁性薄膜層を有する垂直磁気記録媒体Alloy and sputtering target material used for soft magnetic thin film layer in perpendicular magnetic recording medium and perpendicular magnetic recording medium having soft magnetic thin film layer 関連出願の相互参照Cross-reference of related applications
　この出願は、２０１１年９月２６日に出願された日本国特許出願２０１１－２０９８５６号に基づく優先権を主張するものであり、その全体の開示内容が参照により本明細書に組み込まれる。 This application claims priority based on Japanese Patent Application No. 2011-209856 filed on Sep. 26, 2011, the entire disclosure of which is incorporated herein by reference.
　本発明は、垂直磁気記録媒体における軟磁性薄膜層用（Ｃｏ，Ｆｅ）－ランタノイド系合金およびスパッタリングターゲット材に関するものである。 The present invention relates to a (Co, Fe) -lanthanoid alloy and a sputtering target material for a soft magnetic thin film layer in a perpendicular magnetic recording medium.
　磁気記録技術の進歩は著しく、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、過去に普及していた面内磁気記録媒体より更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。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。そして、垂直磁気記録方式においては、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２層記録媒体が開発されている。この磁気記録膜層には一般的にＣｏＣｒＰｔ－ＳｉＯ2 系合金が用いられている。 The progress of magnetic recording technology has been remarkable, and in order to increase the capacity of the drive, the recording density of the magnetic recording medium has been increased, and a higher recording density can be realized than the in-plane magnetic recording medium that has been popular in the past. A perpendicular magnetic recording system has been put into practical use. The perpendicular magnetic recording system is a method suitable for high recording density, in which the easy magnetization axis is oriented in the perpendicular direction with respect to the medium surface in the magnetic film of the perpendicular magnetic recording medium. In the perpendicular magnetic recording system, a two-layer recording medium having a magnetic recording film layer and a soft magnetic film layer with improved recording sensitivity has been developed. In general, a CoCrPt—SiO 2 alloy is used for the magnetic recording film layer.
　一方、従来の軟磁性膜層には、高い飽和磁束密度（以下、Ｂｓと記す）と非晶質性が必要であり、さらに垂直磁気記録媒体の用途や使用環境によっては、高耐食性、高硬度など様々な特性が付加的に要求されてきた。例えば、特開２００８－２９９９０５号公報（特許文献１）では、Ｆｅを添加することにより高いＢｓを得ており、Ｂを添加することにより高い硬度を得ている。また、特開２０１１－６８９８５号公報（特許文献２）では、ＹやＴｉの添加により耐食性（耐候性）を改善している。 On the other hand, a conventional soft magnetic film layer needs to have a high saturation magnetic flux density (hereinafter referred to as Bs) and an amorphous property. Further, depending on the application and use environment of the perpendicular magnetic recording medium, it has high corrosion resistance and high hardness. Various characteristics have been additionally required. For example, in Japanese Patent Application Laid-Open No. 2008-299905 (Patent Document 1), high Bs is obtained by adding Fe, and high hardness is obtained by adding B. In JP 2011-68985 (Patent Document 2), the corrosion resistance (weather resistance) is improved by adding Y or Ti.
　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き込みが可能となってきている。したがって、記録層の下に配置される軟磁性層として、従来のような高Ｂｓではなく、比較的低Ｂｓの非晶質合金が検討されるようになってきた。このように低Ｂｓ合金を垂直磁気記録媒体の軟磁性層として用いると、軟磁性膜中の記録磁化が、過度に周囲に磁気的な影響を与えることがなく、結果として小さなスペースに記録可能となる。この現象は、「書き滲み」の低減による、見かけ上の記録密度改善と考えられている。 In recent years, writing with a lower magnetic flux than before has been achieved by improving the read / write head during driving and adjusting the magnetic flux density of the soft magnetic alloy to optimize the exchange coupling magnetic field between the soft magnetic film and the Ru film. It has become possible. Therefore, as a soft magnetic layer disposed under the recording layer, an amorphous alloy having a relatively low Bs instead of the conventional high Bs has been studied. When a low Bs alloy is used as a soft magnetic layer of a perpendicular magnetic recording medium in this way, the recording magnetization in the soft magnetic film does not excessively affect the surroundings and can be recorded in a small space as a result. Become. This phenomenon is considered to improve the apparent recording density by reducing the “writing blur”.
特開２００８－２９９９０５号公報JP 2008-299905 A 特開２０１１－６８９８５号公報JP 2011-68985 A
　しかしながら、上述したように低いＢｓを持つ非晶質合金を垂直磁気記録媒体の軟磁性層に用いると、新たな課題があることが明らかになってきた。すなわち、低いＢｓを有する非晶質合金は温度の上昇に伴うＢｓの低下幅が大きく、ドライブが曝される室温より高い温度環境（例えば７０～１５０℃程度）の下におけるＢｓが著しく低くなり、垂直磁気記録媒体の軟磁性層としての機能を十分に果たせなくなってしまう。 However, it has become clear that there is a new problem when an amorphous alloy having a low Bs is used for the soft magnetic layer of the perpendicular magnetic recording medium as described above. That is, an amorphous alloy having low Bs has a large decrease range of Bs as the temperature rises, and Bs under a temperature environment (for example, about 70 to 150 ° C.) higher than room temperature to which the drive is exposed becomes remarkably low. The function as the soft magnetic layer of the perpendicular magnetic recording medium cannot be sufficiently performed.
　上述のような問題を解消するために、本発明者らは垂直磁気記録媒体の軟磁性膜用合金の室温でのＢｓとその温度特性について、様々な添加元素を詳細に検討した結果、室温でのＢｓと室温から１５０℃までのＢｓの低下幅には逆の相関があることがわかった。しかしながら、ランタノイドに属する元素を添加すると、この逆相関の関係から外れ、室温で同等のＢｓを有する合金と比較し、著しく１５０℃までのＢｓ低下幅が小さく抑えられることを見出し本発明に至った。 In order to solve the above-mentioned problems, the present inventors have examined various additive elements in detail for Bs and temperature characteristics of the soft magnetic film alloy of the perpendicular magnetic recording medium. It was found that there is an inverse correlation between the Bs of B and the decrease in Bs from room temperature to 150 ° C. However, the addition of an element belonging to the lanthanoid deviates from this inverse correlation, and the present inventors found that the Bs reduction range up to 150 ° C. can be significantly reduced compared with an alloy having the same Bs at room temperature. .
　したがって、本発明の目的は、室温での飽和磁束密度に対する高温での飽和磁束密度が大きい垂直磁気記録媒体用軟磁性合金、およびこの合金の薄膜を作製するためのスパッタリングターゲット材を提供することにある。 Accordingly, an object of the present invention is to provide a soft magnetic alloy for perpendicular magnetic recording media having a high saturation magnetic flux density at a high temperature relative to a saturation magnetic flux density at room temperature, and a sputtering target material for producing a thin film of this alloy. is there.
　本発明の一態様によれば、垂直磁気記録媒体における軟磁性薄膜層に用いる合金であって、前記合金が、ａｔ％で、
　原子番号が５７～７１のランタノイドに属する元素を１種以上と、
　Ｙ，Ｔｉ，Ｚｒ，Ｈｆ，Ｖ，Ｎｂ，Ｔａ，Ｂの１種もしくは２種以上または／およびＣ，Ａｌ，Ｓｉ，Ｐ，Ｃｒ，Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｇａ，Ｇｅ，Ｍｏ，Ｓｎ，Ｗの１種もしくは２種以上と、残部Ｃｏ，Ｆｅおよび不可避的不純物を含んでなり（comprising）、好ましくはこれらの元素のみから実質的になり（consisting essentially of）、より好ましくはこれらの元素のみからなり（consisting of）、下記の式（１）～（３）：
（１）０．５≦ＴＬＡ≦１５
（２）５≦ＴＬＡ＋ＴＡＭ
（３）ＴＬＡ＋ＴＡＭ＋ＴＮＭ≦３０
（式中、ＴＬＡは原子番号５７～７１のランタノイドに属する元素の添加量の合計％であり、ＴＡＭ＝Ｙ＋Ｔｉ＋Ｚｒ＋Ｈｆ＋Ｖ＋Ｎｂ＋Ｔａ＋Ｂ／２の添加量の合計％（なお、Ｂのみ１／２倍の値）であり、ＴＮＭ＝Ｃ＋Ａｌ＋Ｓｉ＋Ｐ＋Ｃｒ＋Ｍｎ＋Ｎｉ＋Ｃｕ＋Ｚｎ＋Ｇａ＋Ｇｅ＋Ｍｏ＋Ｓｎ＋Ｗの添加量の合計％である）
を全て満たす、合金が提供される。 According to one aspect of the present invention, an alloy used for a soft magnetic thin film layer in a perpendicular magnetic recording medium, wherein the alloy is at%,
One or more elements belonging to lanthanoids with atomic numbers 57-71,
One or more of Y, Ti, Zr, Hf, V, Nb, Ta, B or / and C, Al, Si, P, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Mo, Sn , W, and the remainder Co, Fe, and inevitable impurities (comprising), preferably consisting essentially of these elements, more preferably these elements Consisting of the following formulas (1) to (3):
(1) 0.5 ≦ TLA ≦ 15
(2) 5 ≦ TLA + TAM
(3) TLA + TAM + TNM ≦ 30
(In the formula, TLA is the total addition amount of elements belonging to the lanthanoids of atomic numbers 57 to 71, and is the total addition amount of TAM = Y + Ti + Zr + Hf + V + Nb + Ta + B / 2 (note that only B is a value of 1/2). , TNM = C + Al + Si + P + Cr + Mn + Ni + Cu + Zn + Ga + Ge + Mo + Sn + W
An alloy is provided that satisfies all of the following:
　本発明の他の一態様によれば、上記合金からなる軟磁性薄膜層が提供される。本発明の更に別の態様によれば、上記軟磁性薄膜層を有する垂直磁気記録媒体が提供される。本発明の更にまた別の態様によれば、上記合金からなるスパッタリングターゲット材が提供される。 According to another aspect of the present invention, a soft magnetic thin film layer made of the above alloy is provided. According to still another aspect of the present invention, there is provided a perpendicular magnetic recording medium having the soft magnetic thin film layer. According to still another aspect of the present invention, a sputtering target material comprising the above alloy is provided.
　このような本発明によれば、室温でのＢｓに対する高温、つまり使用中にドライブが曝される７０～１５０℃程度の高温の下でのＢｓの低下幅が小さい垂直磁気記録媒体用軟磁性合金、およびこの合金の薄膜を作製するためのスパッタリングターゲット材を提供することができる。また、本発明の合金を垂直磁気記録媒体に用いることにより、軟磁性合金のもつ磁気特性を如何なく発揮し、軟磁性薄膜層の機能を十分に高めることが出来るようになり、その結果として垂直磁気記録媒体の性能向上に繋げることができる。 According to the present invention as described above, the soft magnetic alloy for perpendicular magnetic recording media has a small decrease in Bs at a high temperature relative to Bs at room temperature, that is, a high temperature of about 70 to 150 ° C. at which the drive is exposed during use. , And a sputtering target material for producing a thin film of this alloy. In addition, by using the alloy of the present invention in a perpendicular magnetic recording medium, the magnetic properties of the soft magnetic alloy can be fully exhibited, and the function of the soft magnetic thin film layer can be sufficiently enhanced. This can lead to an improvement in the performance of the magnetic recording medium.
急冷リボン製の３９％Ｃｏ－３９％Ｆｅ－８％Ｚｒ－６％Ｂ－８％（添加元素）の合金のＸ線回折パターンを示す図である。FIG. 3 is a diagram showing an X-ray diffraction pattern of a 39% Co-39% Fe-8% Zr-6% B-8% (additive element) alloy made of a quenched ribbon. 表１における室温のＢｓとＢｓ比をプロットした図である。It is the figure which plotted Bs and Bs ratio of room temperature in Table 1. 表２における室温のＢｓとＢｓ比をプロットした図である。It is the figure which plotted Bs and Bs ratio of room temperature in Table 2.
　以下、本発明について詳細に説明する。特段の明示が無いかぎり、本明細書において「％」又は単位無しの数字はａｔ％を意味する。 Hereinafter, the present invention will be described in detail. Unless otherwise specified, “%” or a number without a unit in this specification means at%.
　上述したように、垂直磁気記録媒体の軟磁性膜用合金の室温でのＢｓとその温度特性について、様々な添加元素を詳細に検討した結果、室温でのＢｓと室温から１５０℃までのＢｓの低下幅には逆の相関があることがわかった。しかしながら、ランタノイドに属する元素を添加すると、この逆相関の関係から外れ、室温で同等のＢｓを有する合金と比較し、著しく１５０℃までのＢｓ低下幅が小さく抑えられることが分かった。 As described above, Bs at room temperature and its temperature characteristics of the soft magnetic film alloy of the perpendicular magnetic recording medium were examined in detail for various additive elements. As a result, Bs at room temperature and Bs from room temperature to 150 ° C. It was found that there was an inverse correlation between the drop widths. However, when an element belonging to a lanthanoid was added, it was found that the inverse correlation relationship was removed, and the Bs decrease width up to 150 ° C. was significantly reduced as compared with an alloy having an equivalent Bs at room temperature.
　上記現象についての詳細な理由は不明であるが、以下のことが推測される。Ｂｓの温度特性には交換積分（Ｊｅ）が影響すると考えられており、結晶質金属の場合、原理は不明ながら３ｄ電子軌道と原子間距離によりＪｅは変化する可能性が示唆されている（いわゆるベーテ・スレーター曲線）。ここで、本発明においてＢｓの温度特性を改善する効果が見られたランタノイドに属する元素は、結晶における原子半径が１．７３～１．９９×１０-10 ｍと、他の元素に対し著しく大きい。したがって、これらランタノイドに属する元素を添加した非晶質合金は、平均の原子間距離が広がると考えられ、これにより結晶質合金における原子間距離増加によるＪｅ増大と同じような効果が現れ、Ｂｓの高温特性が改善されると推察される。 Although the detailed reason for the above phenomenon is unknown, the following is presumed. The exchange integral (Je) is considered to affect the temperature characteristics of Bs. In the case of crystalline metals, the principle is unknown, but it is suggested that Je may change depending on the 3d electron orbit and interatomic distance (so-called). Bethe-Slater curve). Here, the element belonging to the lanthanoid, in which the effect of improving the temperature characteristic of Bs in the present invention was observed, has an atomic radius in the crystal of 1.73 to 1.99 × 10 −10 m, which is significantly larger than other elements. . Therefore, it is considered that the average interatomic distance is increased in the amorphous alloy to which the element belonging to these lanthanoids is added. As a result, the same effect as the increase in Je due to the increase in the interatomic distance in the crystalline alloy appears. It is assumed that the high temperature characteristics are improved.
　実際、図１に急冷薄帯試料のＸ線回折の例を示す通り、ランタノイドに属する元素を添加した場合、他の元素を添加した場合と比較し、ハローパターンの低角側の裾が、緩やかに拡大していることが確認される。これは、原子半径の大きいランタノイドに属する元素を添加することにより、非晶質合金の平均原子間距離が広げられたことを示唆している。 In fact, as shown in the example of the X-ray diffraction of the quenched ribbon sample in FIG. 1, when the element belonging to the lanthanoid is added, the skirt on the low angle side of the halo pattern is gentler than when adding other elements. It is confirmed that it has expanded. This suggests that the average interatomic distance of the amorphous alloy was increased by adding an element belonging to a lanthanoid having a large atomic radius.
　上記した知見を基に本発明により見出した、室温でのＢｓに対する高温でのＢｓ低下幅が小さい非晶質軟磁性合金における特徴と作用を以下に述べる。なお、原子番号が５７～７１のランタノイドに属する元素とは、Ｌａ，Ｃｅ，Ｐｒ，Ｎｄ，Ｐｍ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕを指す。
式（１）０．５≦ＴＬＡ≦１５（ＴＬＡは原子番号５７～７１のランタノイドに属する元素の添加量の合計％）
式（２）５≦ＴＬＡ＋ＴＡＭ（ＴＡＭ＝Ｙ＋Ｔｉ＋Ｚｒ＋Ｈｆ＋Ｖ＋Ｎｂ＋Ｔａ＋Ｂ／２の添加量の合計％、なお、Ｂのみ１／２倍の値。
式（３）ＴＬＡ＋ＴＡＭ＋ＴＮＭ≦３０（ＴＮＭ＝Ｃ＋Ａｌ＋Ｓｉ＋Ｐ＋Ｃｒ＋Ｍｎ＋Ｎｉ＋Ｃｕ＋Ｚｎ＋Ｇａ＋Ｇｅ＋Ｍｏ＋Ｓｎ＋Ｗの添加量の合計％） The characteristics and operation of the amorphous soft magnetic alloy found by the present invention based on the above findings and having a small Bs decrease width at high temperatures relative to Bs at room temperature will be described below. The elements belonging to the lanthanoids having atomic numbers 57 to 71 are La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu.
Formula (1) 0.5 ≦ TLA ≦ 15 (TLA is the total amount of elements added to the lanthanoids having atomic numbers 57 to 71)
Formula (2) 5 ≦ TLA + TAM (TAM = Y + Ti + Zr + Hf + V + Nb + Ta + B / 2) Total amount of addition amount, B alone being 1/2 times the value.
Formula (3) TLA + TAM + TNM ≦ 30 (TNM = C + Al + Si + P + Cr + Mn + Ni + Cu + Zn + Ga + Ge + Mo + Sn + W total%)
　本発明合金において、原子番号５７～７１のランタノイドに属する元素は、室温でのＢｓを低下させ、高温でのＢｓの低下を抑制するための必須元素であるとともに、非晶質促進効果も有する。また、結晶質の場合の本発明合金組成の材料においては、Ｃｏおよび／またはＦｅと脆性な金属間化合物を生成する元素でもある。本発明合金において、Ｙ，Ｔｉ，Ｚｒ，Ｈｆ，Ｖ，Ｎｂ，Ｔａ，Ｂは、室温でのＢｓを低下させるとともに、非晶質促進効果を有する元素である。 In the alloy of the present invention, the element belonging to the lanthanoids having atomic numbers of 57 to 71 is an essential element for reducing Bs at room temperature and suppressing the decrease of Bs at high temperature, and also has an amorphous promoting effect. Moreover, in the material of the alloy composition of the present invention when crystalline, it is also an element that forms brittle intermetallic compounds with Co and / or Fe. In the alloy of the present invention, Y, Ti, Zr, Hf, V, Nb, Ta, and B are elements that lower Bs at room temperature and have an amorphous promoting effect.
　本発明合金において、Ｃ，Ａｌ，Ｓｉ，Ｐ，Ｃｒ，Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｇａ，Ｇｅ，Ｍｏ，Ｓｎ，Ｗは、室温でのＢｓを低下させるために添加する元素である。したがって、ＴＬＡが０．５未満では高温でのＢｓの低下抑制効果が十分でなく、１５を超えると脆性な金属間化合物が多く生成するため、結晶質となる本合金組成のスパッタリングターゲット材の機械加工が困難となる。また、ＴＬＡ＋ＴＡＭが５未満では非晶質促進効果が十分でない。さらに、ＴＬＡ＋ＴＡＭ＋ＴＮＭが３０を超えると室温でのＢｓが過度に低くなる。なお、各式の好ましい範囲は下記の通りである。 In the alloy of the present invention, C, Al, Si, P, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Mo, Sn, and W are elements added to lower Bs at room temperature. Therefore, if the TLA is less than 0.5, the effect of suppressing the decrease in Bs at high temperatures is not sufficient, and if it exceeds 15, a large amount of brittle intermetallic compounds are produced. Processing becomes difficult. Further, if TLA + TAM is less than 5, the amorphous promoting effect is not sufficient. Further, when TLA + TAM + TNM exceeds 30, Bs at room temperature becomes excessively low. In addition, the preferable range of each formula is as follows.
　式（１）について好ましくは、１≦ＴＬＡ≦１３、より好ましくは、２≦ＴＬＡ≦１１である。式（２）について好ましくは、６≦ＴＬＡ＋ＴＡＭ、より好ましくは、７≦ＴＬＡ＋ＴＡＭである。式（３）について好ましくは、ＴＬＡ＋ＴＡＭ＋ＴＮＭ≦２８、より好ましくは、ＴＬＡ＋ＴＡＭ＋ＴＮＭ≦２６である。なお、Ｆｅの含有量とＦｅとＣｏを合計した含有量の比（以下「Ｆｅ％／（Ｆｅ％＋Ｃｏ％）」と記す。）の範囲については特に制限はないが、垂直磁気記録媒体の軟磁性膜としては、０を超え０．９０以下のものが多く使用されており、０．３０以上、０．６５以下のものがより多く使用されている。 For formula (1), preferably 1 ≦ TLA ≦ 13, more preferably 2 ≦ TLA ≦ 11. For formula (2), preferably 6 ≦ TLA + TAM, more preferably 7 ≦ TLA + TAM. Preferably about Formula (3), it is TLA + TAM + TNM <= 28, More preferably, it is TLA + TAM + TNM <= 26. The range of the ratio of the Fe content and the total content of Fe and Co (hereinafter referred to as “Fe% / (Fe% + Co%)”) is not particularly limited, but the softness of the perpendicular magnetic recording medium is not limited. As the magnetic film, those more than 0 and 0.90 or less are often used, and those having a value of 0.30 or more and 0.65 or less are more used.
　以下、本発明について実施例によって具体的に説明する。 Hereinafter, the present invention will be specifically described with reference to examples.
　通常、垂直磁気記録媒体における軟磁性膜層は、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、以下に示す実験ＡおよびＢでは、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。 Usually, a soft magnetic film layer in a perpendicular magnetic recording medium can be formed on a glass substrate or the like by sputtering a sputtering target material having the same component as that component. Here, the thin film formed by sputtering is rapidly cooled. On the other hand, in the experiments A and B shown below, a quenching ribbon manufactured by a single roll type liquid quenching apparatus is used as a specimen. 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.
　次いで実験Ｃとして、実際にスパッタリングターゲット材を作製し、これをスパッタして作製した薄膜について評価した。急冷薄帯の作製条件については、所定の成分に秤量した原料３０ｇを径が１０ｍｍで深さが４０ｍｍ程度の水冷銅鋳型にて減圧Ａｒ中でアーク溶解し、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、径１５ｍｍの石英管中にこの溶解母材にセットし、出湯ノズルの径を１ｍｍとし、雰囲気圧６１ｋＰａ、噴霧差圧６９ｋＰａ、銅ロール（径３００ｍｍ）の回転数は３０００ｒｐｍで、銅ロールと出湯ノズルのギャップ０．３ｍｍに設定して出湯した。出湯温度は特に限定せず、出湯するタイミングは各溶解母材が完全に溶け落ちた直後とした。このようにして作製した急冷薄帯を供試材とし、室温と高温でのＢｓと非晶質性を評価した。 Next, as Experiment C, a sputtering target material was actually produced, and a thin film produced by sputtering was evaluated. Regarding the conditions for preparation of the quenched ribbon, 30 g of raw material weighed to a predetermined component was arc-melted in reduced-pressure Ar using a water-cooled copper mold having a diameter of about 10 mm and a depth of about 40 mm, to obtain a molten preform for the quenched ribbon. . The conditions for preparing the quenched ribbon are a single roll method, set in this molten base material in a quartz tube having a diameter of 15 mm, the diameter of the hot water nozzle is 1 mm, the atmospheric pressure is 61 kPa, the spray differential pressure is 69 kPa, the copper roll (diameter is 300 mm). ) Was set at 3000 rpm and the gap between the copper roll and the hot water nozzle was set to 0.3 mm, and the hot water was discharged. The hot water temperature is not particularly limited, and the hot water is discharged immediately after each molten base material is completely melted. The quenched ribbon thus prepared was used as a test material, and Bs and amorphous properties at room temperature and high temperature were evaluated.
　急冷薄帯の室温でのＢｓおよび高温（１５０℃）におけるＢｓ低下幅の評価については、ＶＳＭ装置（振動試料型磁力計）にて、印加磁場１２００ｋＡ／ｍで室温（３０℃）および１５０℃のＢｓを測定した。なお、高温におけるＢｓの低下幅は３０℃でのＢｓに対する１５０℃でのＢｓの百分率、すなわち、式で示せば（１５０℃でのＢｓ）／（３０℃でのＢｓ）×１００％により評価した。（以下、「Ｂｓ比」と記す）。すなわち、このＢｓ比が１００％に近いほど、３０℃から１５０℃におけるＢｓの低下幅が小さいことを示す。 Regarding the evaluation of Bs at room temperature and the Bs decrease width at high temperature (150 ° C.) of the quenched ribbon, using a VSM apparatus (vibrating sample type magnetometer) with an applied magnetic field of 1200 kA / m at room temperature (30 ° C.) and 150 ° C. Bs was measured. In addition, the decrease width of Bs at high temperature was evaluated by the percentage of Bs at 150 ° C. with respect to Bs at 30 ° C., that is, (Bs at 150 ° C.) / (Bs at 30 ° C.) × 100%. . (Hereinafter referred to as “Bs ratio”). That is, the closer this Bs ratio is to 100%, the smaller the decrease in Bs from 30 ° C to 150 ° C.
　急冷薄帯の非晶質性の評価については、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を評価した。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ガラス板に貼り付けた。Ｘ線源はＣｕ－ｋα線で、スキャンスピードを４°／ｍｉｎとして測定した。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。 Regarding the 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, amorphousness was evaluated by the following method. The 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 on the glass plate so that the measurement surface was a copper roll contact surface of a quenched ribbon. The X-ray source was Cu-kα ray, and the scan speed was 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.
　スパッタリングターゲット材の機械加工性の評価については、所定の成分に秤量した５ｋｇの母材を耐火物坩堝中で、減圧したＡｒ雰囲気の下で誘導溶解した後、凝固させた。坩堝のサイズは、直径１２０ｍｍ、高さ１５０ｍｍである。このインゴットの下部から、旋盤加工、ワイヤーカット加工、平面研磨加工にて、直径９５ｍｍ、厚さ２ｍｍのスパッタリングターゲット材を作製した。これらの加工時における、欠けや割れの発生により機械加工性を評価した。 For the evaluation of the machinability of the sputtering target material, 5 kg of a base material weighed to a predetermined component was induction-melted in a refractory crucible under a reduced Ar atmosphere and then solidified. The size of the crucible is 120 mm in diameter and 150 mm in height. From the lower part of the ingot, a sputtering target material having a diameter of 95 mm and a thickness of 2 mm was produced by lathe processing, wire cutting processing, and plane polishing processing. Machinability was evaluated by the occurrence of chips and cracks during these processes.
　スパッタ膜の評価については、チャンバー内の気圧を１×１０-4Ｐａ以下に真空排気し、純度が９９．９％のＡｒガスを０．６Ｐａになるまで投入しスパッタを行なった。薄膜はガラス基板上に１．５μｍの厚さとなるように生成させた。この薄膜試料について、急冷薄帯と同様にＢｓおよびＢｓ比と結晶構造を評価した。まず初めに、基本組成を２種選定し、それぞれに一定量の添加元素を添加し、添加元素の種類による室温でのＢｓとＢｓ比の変化について評価した。その結果を、実験Ａおよび実験Ｂとして示す。実験Ａは、Ｃｏが３９％で、Ｆｅが３９％、Ｚｒが８％、Ｂが６％で、残部の８％が添加元素となる合金を作成し、添加量が一定の下での添加元素種類の影響を評価した。なお、Ｎｏ．１１は添加元素がなく、ＣｏとＦｅ、Ｚｒ、Ｂが４３対４３対８対６になるように配合した合金である。 For the evaluation of the sputtered film, the atmospheric pressure in the chamber was evacuated to 1 × 10 −4 Pa or less, and Ar gas having a purity of 99.9% was added until the pressure reached 0.6 Pa to perform sputtering. The thin film was formed on the glass substrate so as to have a thickness of 1.5 μm. About this thin film sample, Bs and Bs ratio, and the crystal structure were evaluated similarly to the quenched ribbon. First, two basic compositions were selected, a certain amount of additive element was added to each, and changes in Bs and Bs ratio at room temperature depending on the type of additive element were evaluated. The results are shown as Experiment A and Experiment B. In Experiment A, an alloy in which Co is 39%, Fe is 39%, Zr is 8%, B is 6%, and the remaining 8% is an additive element, and the additive element under a constant addition amount is prepared. The effect of type was evaluated. In addition, No. 11 is an alloy containing no additive elements and blended so that Co, Fe, Zr, and B are 43: 43: 8: 6.
Figure JPOXMLDOC01-appb-T000001
 　表１は、様々な元素を添加した急冷薄帯の諸特性を示す。Ｎｏ．１～１０は本発明例であり、Ｎｏ．１１～３１は比較例である。
Figure JPOXMLDOC01-appb-T000001
 Table 1 shows various properties of the quenched ribbon with various elements added. No. Nos. 1 to 10 are examples of the present invention. Reference numerals 11 to 31 are comparative examples.
　表１における、室温のＢｓとＢｓ比をプロットした図を図２に示す。図２より、ランタノイドに属する元素以外の元素を添加した組成は、概ね室温でのＢｓ低下にともないＢｓ比も低下する相関が見られるのに対し、ランタノイドに属する元素を添加した組成は、明らかに低い室温でのＢｓにもかかわらずＢｓ比が高いことがわかる。実験Ｂは、Ｃｏが３９．６％で、Ｆｅが４８．４％、Ｔｉが３％、Ｚｒが２％、Ｎｂが３％、Ｔａが２％で、残部の２％が添加元素となる合金を作成し、添加量が一定の下での添加元素種類の影響を評価した。なお、Ｎｏ．１１は添加元素がなく、ＣｏとＦｅ、Ｔｉ、Ｚｒ、Ｎｂ、Ｔａが４０．５対４９．５対３対２対３対２になるように配合した合金である。 FIG. 2 shows a plot of room temperature Bs and Bs ratio in Table 1. FIG. 2 shows that the composition added with an element other than the element belonging to the lanthanoid shows a correlation in which the Bs ratio also decreases with a decrease in Bs at room temperature, whereas the composition added with the element belonging to the lanthanoid clearly It can be seen that the Bs ratio is high despite the low Bs at room temperature. Experiment B is an alloy in which Co is 39.6%, Fe is 48.4%, Ti is 3%, Zr is 2%, Nb is 3%, Ta is 2%, and the balance is 2%. And the effect of the type of additive element under a constant addition amount was evaluated. In addition, No. 11 is an alloy containing no additive elements and blended so that Co, Fe, Ti, Zr, Nb, and Ta are 40.5 to 49.5 to 3 to 2 to 3 to 2.
Figure JPOXMLDOC01-appb-T000002
 　表２は、様々な元素を添加した急冷薄帯の諸特性を示す。Ｎｏ．１～４は本発明例であり、Ｎｏ．５～１４は比較例である。
Figure JPOXMLDOC01-appb-T000002
 Table 2 shows various properties of the quenched ribbon with various elements added. No. 1-4 are examples of the present invention. Reference numerals 5 to 14 are comparative examples.
　表２における、室温のＢｓとＢｓ比をプロットした図を図３に示す。図３より、ランタノイドに属する元素以外の元素を添加した組成は、概ね室温でのＢｓ低下にともないＢｓ比も低下する相関が見られるのに対し、ランタノイドに属する元素を添加した組成は、明らかに低い室温でのＢｓにもかかわらずＢｓ比が高いことがわかる。 FIG. 3 shows a plot of room temperature Bs and Bs ratio in Table 2. FIG. 3 shows that the composition in which an element other than the element belonging to the lanthanoid is added has a correlation in which the Bs ratio also decreases with a decrease in Bs at room temperature. It can be seen that the Bs ratio is high despite the low Bs at room temperature.
　以上の実験Ａ，Ｂによりランタノイドに属する元素を添加した場合、その他の元素を添加した場合と比較し、同程度のＢｓを有する組成に対し、高いＢｓ比が得られることが明らかとなった。次に、様々な組成において、ランタノイドに属する元素を添加した組成と、添加していない組成で、ほぼ同等のＣｏおよびＦｅ量を持つ１０対の組成について、スパッタリングターゲット材を作製し、これを用いたスパッタ薄膜の評価を実施した（実験Ｃ）。 From the above experiments A and B, it was found that when an element belonging to a lanthanoid was added, a higher Bs ratio was obtained for a composition having the same degree of Bs as compared with the case where another element was added. Next, in various compositions, sputtering target materials were prepared and used for 10 pairs of compositions in which the elements belonging to the lanthanoids were added and the compositions in which the elements were not added and having almost the same amount of Co and Fe. The sputtered thin film was evaluated (Experiment C).
　なお、実験ＣにおけるＡ～Ｊとａ～ｊについては、同等のＣｏおよびＦｅ量を持つ組成を対にして比較することで、ほぼ同等のＦｅ％／（Ｆｅ％＋Ｃｏ％）と室温でのＢｓを持ちながら、ランタノイドに属する元素を０．５％以上含むか含まないかにより、Ｂｓ比が変化することを確認したものである。実験Ｃは、様々な組成におけるスパッタ膜の室温でのＢｓ、Ｂｓ比、非晶質性の評価をした。 Note that A to J and a to j in Experiment C are compared by comparing compositions having equivalent amounts of Co and Fe in pairs, so that the equivalent Fe% / (Fe% + Co%) and Bs at room temperature. It has been confirmed that the Bs ratio changes depending on whether or not 0.5% or more of the element belonging to the lanthanoid is contained. Experiment C evaluated the Bs, Bs ratio, and amorphous property of the sputtered film having various compositions at room temperature.
Figure JPOXMLDOC01-appb-T000003
 　表３は、スパッタ薄膜の諸特性を示す。Ａ～Ｊは本発明例であり、ａ～ｊは比較例である。
Figure JPOXMLDOC01-appb-T000003
 Table 3 shows various properties of the sputtered thin film. A to J are examples of the present invention, and a to j are comparative examples.
　比較例では本発明例のランタノイドに属する元素（表中のＴＬＡ）を他の添加元素に置き換えたものである。例えば、比較例ａは本発明例Ａで添加している２％のＮｄと３％のＧｄに代え、Ｚｒを５％添加した例である。このように、ＴＬＡを他の添加元素に置き換えることによりＴＬＡの効果を検証した。 In the comparative example, the element belonging to the lanthanoid of the present invention example (TLA in the table) is replaced with another additive element. For example, Comparative Example a is an example in which 5% Zr is added in place of 2% Nd and 3% Gd added in Invention Example A. Thus, the effect of TLA was verified by replacing TLA with other additive elements.
Figure JPOXMLDOC01-appb-T000004
 　表４のように、それぞれ対となる組成は、ほぼ同等のＣｏおよびＦｅ量であることから、室温でのＢｓの差は０．０８Ｔ以下と小さい。一方、Ｂｓ比は、Ｊとｊ以外の対においてランタノイドに属する元素を０．５％以上含む組成（Ａ～Ｉの試料）の方が０．２％以下の組成（ａ～ｉの試料）より、１～１０％高いことが分かる。また、Ａ～Ｉおよびａ～ｉのスパッタリングターゲット材はいずれも欠けなく加工可能であった。
Figure JPOXMLDOC01-appb-T000004
 As shown in Table 4, since the paired compositions have almost the same amount of Co and Fe, the difference in Bs at room temperature is as small as 0.08 T or less. On the other hand, the Bs ratio is 0.2% or less in the composition containing 0.5% or more of the element belonging to the lanthanoid in the pair other than J and j (samples from A to I) than in the composition (samples from a to i). 1 to 10% higher. In addition, all of the sputtering target materials A to I and a to i could be processed without chipping.
　なお、Ｊの試料は機械加工時に欠けは発生しなかったが、ｊの試料は３枚のスパッタリングターゲット材を作製したが、うち２枚は割れたため作製できず、残り１枚は作製したが欠けが発生した。さらに、ｊの試料はＴＬＡ＋ＴＡＭ＋ＴＮＭが３１と大きいため、室温でのＢｓが過度に低い。 The sample of J was not chipped during machining, but the sample of j was made of three sputtering target materials, but two of them were broken and could not be made, and the other one was made but chipped. There has occurred. Furthermore, since the sample of j has a large TLA + TAM + TNM of 31, Bs at room temperature is excessively low.

Claims (8)

  1. 　垂直磁気記録媒体における軟磁性薄膜層に用いる合金であって、前記合金が、ａｔ％で、
    　原子番号が５７～７１のランタノイドに属する元素を１種以上と、
    　Ｙ，Ｔｉ，Ｚｒ，Ｈｆ，Ｖ，Ｎｂ，Ｔａ，Ｂの１種もしくは２種以上または／およびＣ，Ａｌ，Ｓｉ，Ｐ，Ｃｒ，Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｇａ，Ｇｅ，Ｍｏ，Ｓｎ，Ｗの１種もしくは２種以上と
    　残部Ｃｏ，Ｆｅおよび不可避的不純物を含んでなり、下記の式（１）～（３）：
    （１）０．５≦ＴＬＡ≦１５
    （２）５≦ＴＬＡ＋ＴＡＭ
    （３）ＴＬＡ＋ＴＡＭ＋ＴＮＭ≦３０
    （式中、ＴＬＡは原子番号５７～７１のランタノイドに属する元素の添加量の合計％であり、ＴＡＭ＝Ｙ＋Ｔｉ＋Ｚｒ＋Ｈｆ＋Ｖ＋Ｎｂ＋Ｔａ＋Ｂ／２の添加量の合計％（なお、Ｂのみ１／２倍の値）であり、ＴＮＭ＝Ｃ＋Ａｌ＋Ｓｉ＋Ｐ＋Ｃｒ＋Ｍｎ＋Ｎｉ＋Ｃｕ＋Ｚｎ＋Ｇａ＋Ｇｅ＋Ｍｏ＋Ｓｎ＋Ｗの添加量の合計％である）
    を全て満たす、合金。     An alloy used for a soft magnetic thin film layer in a perpendicular magnetic recording medium, wherein the alloy is at%,
    One or more elements belonging to lanthanoids with atomic numbers 57-71,
    One or more of Y, Ti, Zr, Hf, V, Nb, Ta, B or / and C, Al, Si, P, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Mo, Sn , W and the balance Co, Fe and unavoidable impurities, and the following formulas (1) to (3):
    (1) 0.5 ≦ TLA ≦ 15
    (2) 5 ≦ TLA + TAM
    (3) TLA + TAM + TNM ≦ 30
    (In the formula, TLA is the total addition amount of elements belonging to the lanthanoids of atomic numbers 57 to 71, and is the total addition amount of TAM = Y + Ti + Zr + Hf + V + Nb + Ta + B / 2 (note that only B is a value of 1/2). , TNM = C + Al + Si + P + Cr + Mn + Ni + Cu + Zn + Ga + Ge + Mo + Sn + W
    An alloy that meets all requirements.
  2. 　前記合金が、ａｔ％で、
    　原子番号が５７～７１のランタノイドに属する元素を１種以上と、
    　Ｙ，Ｔｉ，Ｚｒ，Ｈｆ，Ｖ，Ｎｂ，Ｔａ，Ｂの１種もしくは２種以上または／およびＣ，Ａｌ，Ｓｉ，Ｐ，Ｃｒ，Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｇａ，Ｇｅ，Ｍｏ，Ｓｎ，Ｗの１種もしくは２種以上と
    　残部Ｃｏ，Ｆｅおよび不可避的不純物のみから実質的になる、請求項１に記載の合金。     The alloy is at%,
    One or more elements belonging to lanthanoids with atomic numbers 57-71,
    One or more of Y, Ti, Zr, Hf, V, Nb, Ta, B or / and C, Al, Si, P, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Mo, Sn The alloy according to claim 1, consisting essentially of only one or more of W, W and the balance Co, Fe and inevitable impurities.
  3. 　前記合金が、ａｔ％で、
    　原子番号が５７～７１のランタノイドに属する元素を１種以上と、
    　Ｙ，Ｔｉ，Ｚｒ，Ｈｆ，Ｖ，Ｎｂ，Ｔａ，Ｂの１種もしくは２種以上または／およびＣ，Ａｌ，Ｓｉ，Ｐ，Ｃｒ，Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｇａ，Ｇｅ，Ｍｏ，Ｓｎ，Ｗの１種もしくは２種以上と
    　残部Ｃｏ，Ｆｅおよび不可避的不純物のみからなる、請求項１に記載の合金。     The alloy is at%,
    One or more elements belonging to lanthanoids with atomic numbers 57-71,
    One or more of Y, Ti, Zr, Hf, V, Nb, Ta, B or / and C, Al, Si, P, Cr, Mn, Ni, Cu, Zn, Ga, Ge, Mo, Sn The alloy according to claim 1, comprising only one or more of W, W and the balance Co, Fe and inevitable impurities.
  4. 　請求項１に記載の合金からなる軟磁性薄膜層。 A soft magnetic thin film layer made of the alloy according to claim 1.
  5. 　請求項４に記載の軟磁性薄膜層を有する垂直磁気記録媒体。 A perpendicular magnetic recording medium having the soft magnetic thin film layer according to claim 4.
  6. 　請求項１に記載の合金からなるスパッタリングターゲット材。 A sputtering target material comprising the alloy according to claim 1.
  7. 　請求項６に記載のスパッタリングターゲット材から成膜された軟磁性薄膜層。 A soft magnetic thin film layer formed from the sputtering target material according to claim 6.
  8. 　請求項７に記載の軟磁性薄膜層を有する垂直磁気記録媒体。 A perpendicular magnetic recording medium having the soft magnetic thin film layer according to claim 7.
PCT/JP2012/074065 2011-09-26 2012-09-20 Alloy used in soft-magnetic thin-film layer on perpendicular magnetic recording medium, sputtering-target material, and perpendicular magnetic recording medium having soft-magnetic thin-film layer WO2013047321A1 (en)

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JP6405261B2 (en) * 2014-05-01 2018-10-17 山陽特殊製鋼株式会社 Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium
JP2020135907A (en) * 2019-02-18 2020-08-31 山陽特殊製鋼株式会社 Spattering target for forming soft magnetic layer of perpendicular magnetic recording medium, and perpendicular magnetic recording medium, and soft magnetic layer thereof

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