JP2006265654A - Fe-Co-B-BASED ALLOY TARGET MATERIAL AND METHOD FOR PRODUCING THE SAME - Google Patents
Fe-Co-B-BASED ALLOY TARGET MATERIAL AND METHOD FOR PRODUCING THE SAME Download PDFInfo
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- 239000013077 target material Substances 0.000 title claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 37
- 239000000956 alloy Substances 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 230000005291 magnetic effect Effects 0.000 claims abstract description 56
- 229910020674 Co—B Inorganic materials 0.000 claims abstract description 29
- 230000035699 permeability Effects 0.000 claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 230000005415 magnetization Effects 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- 238000009689 gas atomisation Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910017061 Fe Co Inorganic materials 0.000 claims description 3
- 238000007712 rapid solidification Methods 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 abstract description 7
- 238000000151 deposition Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 21
- 238000001755 magnetron sputter deposition Methods 0.000 description 6
- 230000004907 flux Effects 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 229910002058 ternary alloy Inorganic materials 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
本発明は、軟磁性膜を形成するためのＦｅ−Ｃｏ−Ｂ系合金ターゲット材およびその製造方法に関するものである。 The present invention relates to an Fe—Co—B alloy target material for forming a soft magnetic film and a method for producing the same.
近年、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いる。しかしながら、現在広く世の中で使用されている面内磁気記録方式の磁気記録媒体では、高記録密度化を実現しようとすると、記録ビットが微細化し、記録ヘッドで記録できないほどの高保磁力が要求される。そこで、これらの問題を解決し、記録密度を向上させる手段として垂直磁気記録方式が検討されている。 In recent years, the progress of magnetic recording technology has been remarkable, and the recording density of magnetic recording media has been increased to increase the capacity of drives. However, in the magnetic recording medium of the in-plane magnetic recording system that is currently widely used in the world, if a high recording density is to be realized, the recording bit becomes fine and a high coercive force that cannot be recorded by the recording head is required. . Therefore, a perpendicular magnetic recording method has been studied as a means for solving these problems and improving the recording density.
垂直磁気記録方式とは、垂直磁気記録媒体の磁性膜中に媒体面に対して磁気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、記録密度を上げて行っ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。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。
そして、２層記録媒体の軟磁性膜として、Ｆｅ−Ｃｏ−Ｂ系合金の軟磁性膜を用いることが提案されている（例えば、特許文献１参照）。
Perpendicular magnetic recording is a method in which a magnetic easy axis is oriented in the perpendicular direction with respect to the medium surface in a magnetic film of a perpendicular magnetic recording medium. This method is suitable for a high recording density with a small magnetic field and little deterioration in recording / reproducing characteristics. 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.
It has been proposed to use a Fe—Co—B alloy soft magnetic film as the soft magnetic film of the two-layer recording medium (see, for example, Patent Document 1).
また、一般的に、２層媒体の軟磁性膜の成膜にはマグネトロンスパッタリング法が用いられることが知られている。マグネトロンスパッタリング法とは、ターゲット材の背後に磁石を配置し、ターゲット材の表面に磁束を漏洩させて、その漏洩磁束領域にプラズマが収束されることにより高速成膜を可能とするスパッタリング法である。このマグネトロンスパッタリング法はターゲット材のスパッタ表面に磁束を漏洩させることに特徴があるため、ターゲット材自身の透磁率が高い場合にはターゲット材のスパッタ表面にマグネトロンスパッタリング法に必要十分な漏洩磁束を形成するのが難しくなる。そこで、ターゲット材自身の透磁率を極力低減しなければならないという要求がある。例えば、Ｆｅ−Ｃｏ−Ｂの三元系合金ターゲット材において透磁率を低減することが提案されている（例えば、特許文献２、非特許文献１参照）。
本発明者等が、特許文献２に記載されている低透磁率化を検討した結果、Ｆｅ−Ｃｏ−Ｂ三元系合金では、ＢはＦｅやＣｏへはほとんど固溶しないため、ターゲットの持つ磁化は、ＦｅやＣｏの磁化の体積平均値より低くすることは物理的に困難であり、安定的かつ効率的にスパッタリングを行う上では、なお課題を有している
本発明の目的は、垂直磁気記録媒体等に用いられる軟磁性膜を成膜するためのＦｅ−Ｃｏ−Ｂ系合金ターゲット材に関して、良好なスパッタリング特性を有する低透磁率のＦｅ−Ｃｏ−Ｂ系合金ターゲット材を提供することである。
As a result of studying the low magnetic permeability described in Patent Document 2 by the present inventors, in the Fe—Co—B ternary alloy, since B hardly dissolves in Fe or Co, the target has It is physically difficult to make the magnetization lower than the volume average value of the magnetization of Fe or Co, and there is still a problem in performing stable and efficient sputtering. To provide a low-permeability Fe-Co-B alloy target material having good sputtering characteristics with respect to an Fe-Co-B alloy target material for forming a soft magnetic film used for a magnetic recording medium or the like. It is.
本発明者らは、軟磁性膜成膜用のＦｅ−Ｃｏ−Ｂ系合金ターゲット材の透磁率に関して種々の検討を行った結果、Ｆｅ−Ｃｏ−Ｂ系合金ターゲット材に適正な合金元素を適正量添加することにより、ターゲット材の磁化を低下させることが可能となり、その結果、ターゲット材の透磁率を低減出来ることを見出し本発明に到達した。 As a result of various studies on the magnetic permeability of the Fe—Co—B alloy target material for forming the soft magnetic film, the present inventors have found that an appropriate alloy element is suitable for the Fe—Co—B alloy target material. By adding the amount, it became possible to lower the magnetization of the target material, and as a result, it was found that the magnetic permeability of the target material can be reduced, and the present invention has been achieved.
すなわち、本発明は、元素Ｍが、４ａ族、５ａ族、６ａ族、７ａ族および８族（ＦｅおよびＣｏを除く）から選ばれる元素であり、原子比における組成式が（（ＦｅＸＣｏ（１００−Ｘ））１００−ＹＭＹ）１００−ＺＢＺ、５５≦Ｘ≦７５、０＜Ｙ≦２０、５≦Ｚ≦１５で表されるＦｅ−Ｃｏ−Ｂ系合金ターゲット材である。
また、ターゲット材は飽和磁化が１．０（Ｔ）から１．８Ｔの範囲であること、最大比透磁率が２５０以下であることが好ましく、板厚が５ｍｍ以上のターゲット材に好適である。
また、前記Ｆｅ−Ｃｏ−Ｂ系合金ターゲット材は、合金の溶湯を急冷凝固処理した合金粉末を加圧焼結することにより作製可能となる。好ましくは、急冷凝固処理はガスアトマイズであり、加圧焼結は熱間静水圧プレスおよびプラズマ通電焼結である。
That is, in the present invention, the element M is an element selected from the group 4a, 5a, 6a, 7a, and 8 (excluding Fe and Co), and the composition formula in the atomic ratio is ((Fe X Co ( 100-X)) is a 100-Y M Y) 100- Z B Z, 55 ≦ X ≦ 75,0 <Fe-Co-B -based alloy target material represented by Y ≦ 20,5 ≦ Z ≦ 15.
The target material preferably has a saturation magnetization in the range of 1.0 (T) to 1.8 T, a maximum relative permeability of 250 or less, and is suitable for a target material having a plate thickness of 5 mm or more.
The Fe—Co—B alloy target material can be produced by pressure sintering an alloy powder obtained by rapidly solidifying a molten alloy. Preferably, the rapid solidification treatment is gas atomization, and the pressure sintering is hot isostatic pressing and plasma electric current sintering.
本発明により、安定したマグネトロンスパッタリングが行なえる軟磁性膜形成用のＦｅ−Ｃｏ−Ｂ系合金ターゲット材を提供でき、垂直磁気記録媒体のようにＦｅ−Ｃｏ−Ｂ系合金の軟磁性膜を必要とする工業製品を製造する上で極めて有効な技術となる。 According to the present invention, an Fe—Co—B alloy target material for forming a soft magnetic film capable of performing stable magnetron sputtering can be provided, and an Fe—Co—B alloy soft magnetic film as in a perpendicular magnetic recording medium is required. This is an extremely effective technique for manufacturing industrial products.
本発明の最も重要な特徴は、Ｆｅ−Ｃｏ−Ｂ系合金ターゲット材の透磁率を低減させるために、元素添加を行い、その添加元素とその添加量を制御する点にある。Ｆｅ−Ｃｏ系合金のスパッタ薄膜は、比較的大きな飽和磁化を有することより、垂直磁気記録媒体用軟磁性膜として膜厚を薄く出来るメリットがある。また、軟磁性膜としては、Ｆｅ−Ｃｏ系合金にＢを添加することにより非晶質もしくは微結晶のスパッタ薄膜とすることで、記録媒体の読み書き時に結晶粒界に起因するノイズ発生を抑制することが可能となる。
このように垂直磁気記録の軟磁性膜として好適な軟磁気特性を有するＦｅ−Ｃｏ−Ｂ膜を形成するためのターゲット材として、薄膜の軟磁気特性の低下を極力招くことなく、ターゲット材の低透磁率化を実現するためには、ターゲット材の金属組織において、マトリックス相を構成するＦｅやＣｏに固溶する元素を添加させることで、ターゲット材の磁化を低減させて透磁率を低減することが可能となる。
The most important feature of the present invention is that an element is added in order to reduce the magnetic permeability of the Fe—Co—B based alloy target material, and the added element and its added amount are controlled. Since the sputtered thin film of Fe—Co alloy has a relatively large saturation magnetization, there is an advantage that the film thickness can be reduced as a soft magnetic film for a perpendicular magnetic recording medium. Further, as the soft magnetic film, an amorphous or microcrystalline sputtered thin film is formed by adding B to the Fe—Co alloy, thereby suppressing the generation of noise caused by crystal grain boundaries during reading and writing of the recording medium. It becomes possible.
Thus, as a target material for forming an Fe—Co—B film having soft magnetic characteristics suitable as a soft magnetic film for perpendicular magnetic recording, the target material is reduced without causing a decrease in the soft magnetic characteristics of the thin film as much as possible. In order to achieve magnetic permeability, by adding an element that dissolves in Fe or Co constituting the matrix phase in the metal structure of the target material, the magnetization of the target material is reduced to reduce the magnetic permeability. Is possible.
そこで、本発明のＦｅ−Ｃｏ−Ｂ系合金ターゲット材においては、Ｆｅ相やＣｏ相に固溶し磁化を低減させる添加元素Ｍとして、元素周期律表における４ａ族（Ｔｉ、Ｚｒ、Ｈｆ）、５ａ族（Ｖ、Ｎｂ、Ｔａ）、６ａ族（Ｃｒ、Ｍｏ、Ｗ）、７ａ族（Ｍｎ、Ｔｃ、Ｒｅ）および８族（ＦｅおよびＣｏを除く、Ｎｉ、Ｒｕ、Ｒｈ、Ｐｄ、Ｏｓ、Ｉｒ、Ｐｔ）から選ばれる元素を選択するとともに、さらに原子比における組成式が（（ＦｅＸＣｏ（１００−Ｘ））１００−ＹＭＹ）１００−ＺＢＺ、５５≦Ｘ≦７５、０＜Ｙ≦２０、５≦Ｚ≦１５で表される成分組成とした。なお、上記の成分範囲とした理由は、添加元素Ｍの添加量が少ないと磁化低減の効果が薄く、添加量が多いと膜の磁気特性が劣化するためである。 Therefore, in the Fe—Co—B based alloy target material of the present invention, as an additive element M that dissolves in the Fe phase or Co phase and reduces magnetization, group 4a (Ti, Zr, Hf) in the periodic table of elements, Group 5a (V, Nb, Ta), Group 6a (Cr, Mo, W), Group 7a (Mn, Tc, Re) and Group 8 (excluding Fe and Co, Ni, Ru, Rh, Pd, Os, Ir , together with selecting the element selected from Pt), a composition formula in further atomic ratio ((Fe X Co (100- X)) 100-Y M Y) 100-Z B Z, 55 ≦ X ≦ 75,0 < It was set as the component composition represented by Y <= 20 and 5 <= Z <= 15. The reason why the above component range is adopted is that the effect of reducing magnetization is small when the additive amount of the additive element M is small, and the magnetic properties of the film are deteriorated when the additive amount is large.
また、本発明において、ターゲット材の飽和磁化は、１．８（Ｔ）以下であることが好ましいが、飽和磁化が１．０（Ｔ）未満となると、軟磁性膜としての磁化自体も低下するため軟磁性膜としては十分な特性を満足しなくなるため、ターゲット材の飽和磁化が１．０（Ｔ）以上、１．８（Ｔ）以下であることが好ましい。また、ターゲット材の最大透磁率は、可能な限り低いことが好ましく、マグネトロンスパッタで安定してスパッタ放電するためには、２５０以下が好ましく、より好ましくは２００以下であり、さらに好ましくは１００以下である。
さらに、本発明のターゲット材は、従来のＦｅ−Ｃｏ−Ｂ三元系合金のターゲット材と比較し透磁率が低く、ターゲット材表面の漏洩磁束が大きくなるため、板厚の大きなターゲット材の安定放電に有効であり、特に板厚が５ｍｍ以上のターゲット材でも放電が安定するため有効である。
In the present invention, the saturation magnetization of the target material is preferably 1.8 (T) or less. However, when the saturation magnetization is less than 1.0 (T), the magnetization itself as the soft magnetic film also decreases. Therefore, the saturation magnetization of the target material is preferably 1.0 (T) or more and 1.8 (T) or less because the soft magnetic film does not satisfy sufficient characteristics. Further, the maximum permeability of the target material is preferably as low as possible, and is preferably 250 or less, more preferably 200 or less, and still more preferably 100 or less, in order to stably perform sputtering discharge by magnetron sputtering. is there.
Furthermore, since the target material of the present invention has a lower magnetic permeability than the conventional Fe—Co—B ternary alloy target material and increases the leakage flux on the surface of the target material, the stability of the target material having a large plate thickness is improved. It is effective for discharge, and particularly effective for target materials having a plate thickness of 5 mm or more because the discharge is stable.
本発明のターゲット材は、真空溶解法、粉末焼結法等の各種製法で製造可能であるが、低透磁率のターゲット材を製造するためには、微細な金属組織とすることが望ましく、本発明のＦｅ−Ｃｏ−Ｂ系合金の溶湯を急冷凝固処理した合金粉末を加圧焼結して作製することが好ましい。なお、さらに、ターゲット材においては透磁率を低減するため、加圧焼結する原料の粉末を、Ｆｅ基合金の急冷凝固粉末とＣｏ基合金の急冷凝固粉末とを混合した粉末とすることが好ましい。それは、ＦｅとＣｏの完全な合金化を抑制することができるため、ターゲット材の飽和磁化の上昇を抑制することができるためである。
また、急冷凝固処理としては、低不純物で焼結体製造に適した球状粉末を得られるガスアトマイズが好ましい。より好ましくは、アルゴンガスもしくは窒素ガスを用いたガスアトマイズである。
The target material of the present invention can be manufactured by various manufacturing methods such as a vacuum melting method and a powder sintering method, but in order to manufacture a low magnetic permeability target material, it is desirable to have a fine metal structure. It is preferable to produce by pressurizing and sintering an alloy powder obtained by rapidly solidifying the molten Fe-Co-B alloy of the invention. Further, in order to reduce the magnetic permeability in the target material, it is preferable that the raw material powder to be pressure-sintered is a powder obtained by mixing rapidly solidified powder of Fe-based alloy and rapidly solidified powder of Co-based alloy. . This is because complete alloying of Fe and Co can be suppressed, and an increase in saturation magnetization of the target material can be suppressed.
Moreover, as the rapid solidification treatment, gas atomization that can obtain a spherical powder suitable for manufacturing a sintered body with low impurities is preferable. More preferred is gas atomization using argon gas or nitrogen gas.
また、本発明の加圧焼結としては、高圧力で焼結が可能な熱間静水圧プレスおよび短時間で焼結を完了させることが可能なプラズマ通電焼結を用いることが好ましい。それは、これらの方法によれば、比較的に高温や長時間の焼結処理を避けながら高密度な焼結体を得ることができるため、急冷凝固した合金粉末の微細組織の粗大化およびＦｅとＣｏの合金化の抑制がより可能となるためである。 In addition, as the pressure sintering of the present invention, it is preferable to use a hot isostatic press capable of sintering at a high pressure and plasma electric current sintering capable of completing the sintering in a short time. According to these methods, it is possible to obtain a high-density sintered body while avoiding a relatively high temperature and long-time sintering treatment, so that the microstructure of the rapidly solidified alloy powder is coarsened and Fe and This is because the alloying of Co can be further suppressed.
また、本発明のターゲット材を用いることにより、板厚の厚いターゲットを効率よく使用することが可能となり、垂直磁気記録用軟磁性膜が安定して成膜することができると共に、垂直磁気記録媒体の製造が安定に資することとなる。 Further, by using the target material of the present invention, it becomes possible to efficiently use a thick target, and a soft magnetic film for perpendicular magnetic recording can be stably formed, and a perpendicular magnetic recording medium can be used. This will contribute to stable production.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010007980A1 (en) * | 2008-07-14 | 2010-01-21 | 山陽特殊製鋼株式会社 | Alloys for soft magnetic film layers in vertical magnetic recording media, sputtering target materials and manufacturing method therefore |
| CN112371987A (en) * | 2020-11-13 | 2021-02-19 | 河南东微电子材料有限公司 | Preparation method of iron-cobalt-boron-chromium-aluminum alloy powder |
| KR20220124147A (en) * | 2020-01-06 | 2022-09-13 | 산요오도꾸슈세이꼬 가부시키가이샤 | Manufacturing method of sputtering target material |
| CN119912265A (en) * | 2025-01-22 | 2025-05-02 | 宁波江丰电子材料股份有限公司 | A CoFeB target material and preparation method thereof |
-
2005
- 2005-03-24 JP JP2005086853A patent/JP2006265654A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010007980A1 (en) * | 2008-07-14 | 2010-01-21 | 山陽特殊製鋼株式会社 | Alloys for soft magnetic film layers in vertical magnetic recording media, sputtering target materials and manufacturing method therefore |
| JP2010018869A (en) * | 2008-07-14 | 2010-01-28 | Sanyo Special Steel Co Ltd | Alloy for soft magnetic film layer in perpendicular magnetic recording medium, sputtering target material and method for producing the same |
| KR20220124147A (en) * | 2020-01-06 | 2022-09-13 | 산요오도꾸슈세이꼬 가부시키가이샤 | Manufacturing method of sputtering target material |
| KR102883192B1 (en) | 2020-01-06 | 2025-11-06 | 산요오도꾸슈세이꼬 가부시키가이샤 | Method for manufacturing sputtering target material |
| CN112371987A (en) * | 2020-11-13 | 2021-02-19 | 河南东微电子材料有限公司 | Preparation method of iron-cobalt-boron-chromium-aluminum alloy powder |
| CN119912265A (en) * | 2025-01-22 | 2025-05-02 | 宁波江丰电子材料股份有限公司 | A CoFeB target material and preparation method thereof |
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