JP2016145394A - Nickel based target material excellent in sputtering property - Google Patents
Nickel based target material excellent in sputtering property Download PDFInfo
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- 239000013077 target material Substances 0.000 title claims abstract description 60
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title abstract 8
- 238000004544 sputter deposition Methods 0.000 title description 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims abstract description 41
- 229910052742 iron Inorganic materials 0.000 claims abstract description 28
- 238000005477 sputtering target Methods 0.000 claims abstract description 26
- 230000004907 flux Effects 0.000 claims abstract description 18
- 229910018062 Ni-M Inorganic materials 0.000 claims abstract description 16
- 239000011159 matrix material Substances 0.000 claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 6
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 229910001080 W alloy Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 20
- 229910017061 Fe Co Inorganic materials 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 35
- 238000000034 method Methods 0.000 description 19
- 230000005389 magnetism Effects 0.000 description 17
- 238000001755 magnetron sputter deposition Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 229910020598 Co Fe Inorganic materials 0.000 description 3
- 229910002519 Co-Fe Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000009689 gas atomisation Methods 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910021472 group 8 element Inorganic materials 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
- G11B5/7368—Non-polymeric layer under the lowermost magnetic recording layer
- G11B5/7379—Seed layer, e.g. at least one non-magnetic layer is specifically adapted as a seed or seeding layer
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Magnetic Record Carriers (AREA)
- Thin Magnetic Films (AREA)
Abstract
Description
本発明は、強い漏洩磁束が得られる透磁率が低く使用効率が高いＮｉ系合金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 Ni-based alloy sputtering target material having a low magnetic permeability and a high use efficiency that can provide a strong leakage magnetic flux.
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. .
そして、垂直磁気記録方式においては、記録密度を高めた磁気記録膜相と軟磁性膜相とを有する記録媒体が開発されており、このような媒体構造では、軟磁性層と磁気記録層の間にシード層や下地膜層が製膜された記録媒体が開発されている。この垂直磁気記録方式用のシード層には一般に、ＮｉＷ系の合金が用いられている。 In the perpendicular magnetic recording system, a recording medium having a magnetic recording film phase and a soft magnetic film phase with an increased recording density has been developed. In such a medium structure, a recording medium between the soft magnetic layer and the magnetic recording layer has been developed. In addition, a recording medium on which a seed layer and a base film layer are formed has been developed. In general, a NiW-based alloy is used for the seed layer for the perpendicular magnetic recording system.
一方、ハードディスクドライブの磁気記録特性を改善する一つの手法として、シード層に磁性を持たせる方法が提案されており、例えば、特開２０１２−１２８９３３号（特許文献１）に開示されているように、磁性を有するＶＩＩＩ族の元素であるＦｅ，Ｃｏを添加することで、磁性を持ったシード層が提案されている。 On the other hand, as one method for improving the magnetic recording characteristics of a hard disk drive, a method of imparting magnetism to a seed layer has been proposed. For example, as disclosed in Japanese Patent Application Laid-Open No. 2012-128933 (Patent Document 1). A seed layer having magnetism has been proposed by adding Fe, Co, which is a group VIII element having magnetism.
上述したシード層の成膜には、一般にマグネトロンスパッタリング法が用いられている。この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を収束させ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。しかしながら、上述でのターゲット材では透磁率が高いため漏洩磁束が低く、スパッタ性に乏しい点が課題である。 Magnetron sputtering is generally used for the formation of the seed layer described above. This magnetron sputtering method is a sputtering method that enables high-speed film formation by placing a magnet behind the target material, leaking magnetic flux to the surface of the target material, and converging the plasma in the leakage magnetic flux region. . This magnetron sputtering method is characterized by leakage of magnetic flux to the sputtering surface of the target material. Therefore, if the magnetic permeability of the target material itself is high, sufficient magnetic flux leakage necessary for the magnetron sputtering method is formed on the sputtering surface of the target material. It becomes difficult to do. Therefore, the permeability of the target material itself must be reduced as much as possible. However, the above-described target material has a problem that the magnetic permeability is high, the leakage magnetic flux is low, and the sputtering property is poor.
一方、透磁率を低減する手法の一例として、特開２０１０−５９５４０号（特許文献２）のように、純Ｃｏスパッタリングターゲット材において、原料に純Ｃｏ粉末を用いることで透磁率を低くする方法がある。しかし、特許文献２の方法は軟磁性相用Ｃｏ−Ｆｅ系合金ターゲット材にのみ適応でき、シード層用Ｎｉ系合金ターゲット材などには対応していない。さらに、Ｆｅ源には合金を使用しており、純Ｆｅ粉末を用いた粉末焼結法の検討は行われていない。 On the other hand, as an example of a technique for reducing the magnetic permeability, there is a method of reducing the magnetic permeability by using pure Co powder as a raw material in a pure Co sputtering target material as disclosed in JP 2010-59540 A (Patent Document 2). is there. However, the method of Patent Document 2 can be applied only to the Co—Fe based alloy target material for the soft magnetic phase, and does not correspond to the Ni based alloy target material for the seed layer. Furthermore, an alloy is used as the Fe source, and a powder sintering method using pure Fe powder has not been studied.
そこで、本発明では原料粉末としてＮｉ−Ｍ系合金粉末、純Ｆｅ粉末、純Ｃｏ粉末を用いて、シード層用Ｎｉ−Ｃｏ−Ｆｅ系合金ターゲット材の製造方法を検討した結果、強い漏洩磁束が得られるＮｉ−Ｃｏ−Ｆｅ系合金ターゲット材を見出した。 Therefore, in the present invention, as a result of studying a method for producing a Ni-Co-Fe alloy target material for a seed layer using Ni-M alloy powder, pure Fe powder, and pure Co powder as raw material powder, strong leakage magnetic flux is found. The obtained Ni—Co—Fe alloy target material was found.
（１）Ｎｉ系スパッタリングターゲット材は（Ｎｉx −ＦｅY −ＣｏZ ）100-W −ＭW合金からなり、同合金はａｔ．％で、Ｍ１元素はＷ、Ｍｏ、Ｔａ、Ｃｒ、Ｖ、Ｎｂから選ばれる１種又は２種以上の元素であり、Ｍ１元素の合計量Ｗは２〜２０ａｔ．％であり。残部がＮｉ、Ｆｅ、Ｃｏおよび不可避的不純物からなり、かつＮｉ、Ｆｅ、Ｃｏの含有量の内訳は２０≦Ｘ≦９８、０≦Ｙ≦５０、０≦Ｚ≦６０であって、かつミクロ組織はマトリックス相がＮｉ−Ｍ相でマトリックス相中にＦｅ相および／またはＣｏ相が分散していることを特徴とするＮｉ系スパッタリングターゲット材。 (1) Ni-based sputtering target material is made of (Nix -Fe Y -Co Z) 100 -W -M W alloy, the alloy at. %, The M1 element is one or more elements selected from W, Mo, Ta, Cr, V, and Nb, and the total amount W of the M1 element is 2 to 20 at. %. The balance is Ni, Fe, Co and inevitable impurities, and the breakdown of the contents of Ni, Fe, Co is 20 ≦ X ≦ 98, 0 ≦ Y ≦ 50, 0 ≦ Z ≦ 60, and the microstructure Is a Ni-type sputtering target material characterized in that the matrix phase is Ni-M phase and the Fe phase and / or Co phase is dispersed in the matrix phase.
（２）前記（１）に記載されたＮｉ−Ｆｅ−Ｃｏ−Ｍ合金で、ＦｅとＣｏの合計量が１．５ａｔ％以上含有すること特徴とするＮｉ系スパッタリングターゲット材。
（３）前記（１）または（２）に記載されたＮｉ−Ｆｅ−Ｃｏ−Ｍ合金に、更にＭ２元素としてＡｌ，Ｇａ，Ｉｎ，Ｓｉ，Ｇｅ，Ｓｎ，Ｚｒ，Ｔｉ，Ｈｆ，Ｂ，Ｃｕ，Ｐ，Ｃ，Ｒｕから選ばれる１種又は２種以上の元素を合計で０超え〜１０ａｔ．％含有することを特徴とするＮｉ系スパッタリングターゲット材。
(2) The Ni-Fe-Co-M alloy described in (1) above, wherein the total amount of Fe and Co is 1.5 at% or more.
(3) In addition to the Ni—Fe—Co—M alloy described in (1) or (2) above, Al, Ga, In, Si, Ge, Sn, Zr, Ti, Hf, B, Cu as M2 elements , P, C, Ru selected from a total of more than 0 to 10 at. % Ni-based sputtering target material characterized by containing.
（４）ｆｃｃまたはｈｃｐ相のＣｏを含むことを特徴とする前記（１）〜（３）のいずれか１に記載のＮｉ系スパッタリングターゲット材。
（５）ｆｃｃまたはｂｃｃ相のＦｅを含むことを特徴とする前記（１）〜（３）のいずれか１に記載のＮｉ系スパッタリングターゲット材。
（６）漏洩磁束が１０％以上であることを特徴とする前記（１）〜（３）のいずれか１に記載のＮｉ系スパッタリングターゲット材にある。
(4) The Ni-based sputtering target material according to any one of (1) to (3), wherein the Ni-based sputtering target material contains Co of fcc or hcp phase.
(5) The Ni-based sputtering target material according to any one of (1) to (3), wherein the Ni-based sputtering target material contains fcc or bcc phase Fe.
(6) The Ni-based sputtering target material according to any one of (1) to (3), wherein the leakage magnetic flux is 10% or more.
本発明によれば、効率よくマグネトロンスパッタリングが行えるＮｉ−Ｆｅ−Ｃｏ−Ｍ系合金スパッタリングターゲット材を提供でき、垂直磁気記録媒体のようにＮｉ−Ｆｅ−Ｃｏ系合金のシード層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。 INDUSTRIAL APPLICABILITY According to the present invention, an Ni—Fe—Co—M alloy sputtering target material capable of efficiently performing magnetron sputtering can be provided, and an industry that requires a Ni—Fe—Co alloy seed layer as in a perpendicular magnetic recording medium. This is an extremely effective technology for manufacturing products.
以下、本発明について詳細に説明する。
上述したように、本発明の最も重要な特徴は、シード層用スパッタリングターゲット材において、原料粉末としてＮｉ−Ｍ系合金粉末、純Ｆｅ粉末、純Ｃｏ粉末を用いて混合し、成形することで、磁性が弱い、または磁性を持たないＮｉ系合金中に、磁性を有するＦｅやＣｏを切り離して混在させた点にある。
Hereinafter, the present invention will be described in detail.
As described above, the most important feature of the present invention is that, in the sputtering target material for the seed layer, Ni-M alloy powder, pure Fe powder, and pure Co powder are mixed and molded as a raw material powder, This is in that Fe or Co having magnetism is separated and mixed in a Ni-based alloy having weak magnetism or no magnetism.
また、Ｎｉ−Ｆｅ−Ｃｏ−Ｍ合金において、Ｗ，Ｍｏ，Ｔａ，Ｃｒ，Ｖ，Ｎｂを以下Ｍ１元素と称すると、このＭ１元素は、高融点を持つｂｃｃ系金属であり、本発明で規定する成分範囲でｆｃｃであるＮｉ−Ｆｅ−Ｃｏ系に添加することにより、そのメカニズムは明確ではないが、シード層に求められる（１１１）面への配向性を改善させ、かつ結晶粒を微細化させる元素である。このＷ，Ｍｏ，Ｔａ，Ｃｒ，Ｖ，Ｎｂの１種または２種以上をａｔ％量で、２〜２０％とする。しかし、２％未満ではその効果が十分でなく、また、２０％を超えると化合物が析出するか、アモルファス化する。シード層用合金としてはｆｃｃ単相である事が求められることから、その範囲を２〜２０％とする。好ましくは５〜１５％とする。 In the Ni—Fe—Co—M alloy, when W, Mo, Ta, Cr, V, and Nb are hereinafter referred to as M1 elements, these M1 elements are bcc metals having a high melting point, and are defined by the present invention. Although the mechanism is not clear by adding to the Ni-Fe-Co system which is fcc in the component range to be improved, the orientation to the (111) plane required for the seed layer is improved and the crystal grains are made finer It is an element to be made. One or two or more of W, Mo, Ta, Cr, V, and Nb is 2% to 20% in terms of at%. However, if it is less than 2%, the effect is not sufficient, and if it exceeds 20%, the compound precipitates or becomes amorphous. Since the alloy for the seed layer is required to be an fcc single phase, its range is made 2 to 20%. Preferably it is 5 to 15%.
本発明に係るＮｉ−Ｆｅ−Ｃｏ−Ｍ合金において、Ｎｉ、Ｆｅ、Ｃｏの比率である、Ｎｉ：Ｆｅ：Ｃｏ＝α：β：γとすると、α：９８〜２０とする。９８以下とした理由は、β＋γが１．５未満では保磁力が高くなる。また、２０以上とした理由は、２０未満では、上記同様保磁力が高くなる。したがって、その範囲を９８〜２０とした。好ましくは９８〜６０とする。 In the Ni—Fe—Co—M alloy according to the present invention, when Ni: Fe: Co = α: β: γ, which is the ratio of Ni, Fe, and Co, α: 98-20. The reason why it is 98 or less is that when β + γ is less than 1.5, the coercive force becomes high. Moreover, if it is 20 or more, if it is less than 20, the coercive force is increased as described above. Therefore, the range was set to 98-20. Preferably it is set to 98-60.
ａｔ比β：０〜５０
Ｆｅは、保磁力を低減する元素であり、かつ、膜の配向性を改善する元素でもある。しかし、５０を超えると保磁力が高くなることから、その範囲を０〜５０とした。好ましくは２〜５０％、より好ましくは１０〜４０とする。
ａｔ比γ：０〜６０
Ｃｏは、（１１１）方向の保磁力を低減する元素である。しかし、６０を超えると保磁力が高くなることから、その上限を６０とした。好ましくは４０以下とする。
at ratio β: 0 to 50
Fe is an element that reduces the coercive force and also improves the orientation of the film. However, since coercive force will become high when it exceeds 50, the range was made into 0-50. Preferably it is 2 to 50%, more preferably 10 to 40.
at ratio γ: 0 to 60
Co is an element that reduces the coercivity in the (111) direction. However, since the coercive force increases when it exceeds 60, the upper limit is set to 60. Preferably it is 40 or less.
磁性を有するＦｅ相および／またはＣｏ相が、磁性が弱い、または磁性を持たないＮｉ−Ｍ相中に、分散することで、母材の磁性を低減させ、透磁率を低下させる。透磁率の低下により、強い漏洩磁束が得られ、スパッタリング性が向上する。ＦｅとＣｏの合計量が１．５ａｔ％より少ない場合では、Ｎｉ系中間層に十分な磁性を持たせることができない。したがって、ＦｅとＣｏの含有合計量を１．５ａｔ％以上とした。 The Fe phase and / or Co phase having magnetism are dispersed in the Ni-M phase having weak magnetism or no magnetism, thereby reducing the magnetism of the base material and lowering the magnetic permeability. Due to the decrease in the magnetic permeability, a strong leakage magnetic flux is obtained and the sputtering property is improved. When the total amount of Fe and Co is less than 1.5 at%, the Ni-based intermediate layer cannot have sufficient magnetism. Therefore, the total content of Fe and Co is set to 1.5 at% or more.
Ｍ２元素は、（１１１）面を配向させる元素であり、また、結晶粒を微細化する元素である。このＭ２元素の１種または２種以上をａｔ％量で、０〜１０％とする。しかし、１０％を超えると化合物が生じたり、アモルファス化することから、その上限を１０％とする。好ましくは５％とする。また、Ｍ１＋Ｍ２は好ましくは、２５ａｔ％以下、さらに好ましくは２０ａｔ％以下とする。 The M2 element is an element that orients the (111) plane and is an element that refines crystal grains. One or two or more of these M2 elements are made at 0% to 10% in the amount of at%. However, if it exceeds 10%, a compound is formed or becomes amorphous, so the upper limit is made 10%. Preferably it is 5%. M1 + M2 is preferably 25 at% or less, more preferably 20 at% or less.
Ｃｏは、マトリックス相であるＮｉ−Ｍ系合金と合金化せずに、ｆｃｃまたはｈｃｐ相の単一で存在することで、透磁率の低いスパッタリング性に優れたターゲット材となる。Ｆｅは、マトリックス相であるＮｉ−Ｍ系合金と合金化せずに、ｆｃｃまたはｈｃｐ相の単一で存在することで、透磁率の低いスパッタ性に優れたターゲット材となる。
磁性が弱い、または磁性を持たないＮｉＷ系合金中に、磁性を有するＦｅやＣｏを切り離して混在させ、１０％以上の漏洩磁束を得ることで、スパッタ性に優れたターゲット材となる。
Co does not form an alloy with a Ni-M alloy that is a matrix phase, but exists as a single fcc or hcp phase, and thus becomes a target material with low permeability and excellent sputtering properties. Fe does not form an alloy with the Ni-M alloy that is the matrix phase, but exists as a single fcc or hcp phase, so that it becomes a target material with low permeability and excellent sputterability.
A NiW-based alloy having weak magnetism or no magnetism is mixed with Fe and Co having magnetism separately to obtain a leakage magnetic flux of 10% or more, thereby obtaining a target material having excellent sputterability.
本発明においては、Ｎｉ−Ｆｅ−Ｃｏ−Ｍ合金スパッタリングターゲット材において、Ｎｉ−Ｍ合金溶湯を急冷凝固処理した粉末と純Ｆｅ、純Ｃｏ粉末を所定の組成比率に混合し成形し機械加工することで、透磁率の低くスパッタ性に優れたＮｉ系ターゲットの製造方法を見出した。 In the present invention, in a Ni—Fe—Co—M alloy sputtering target material, a powder obtained by rapidly solidifying a Ni—M alloy molten metal and pure Fe and pure Co powder are mixed in a predetermined composition ratio and molded and machined. Thus, a method for producing a Ni-based target having low magnetic permeability and excellent sputterability was found.
本発明に係る純Ｃｏについては、ｆｃｃまたはｈｃｐ構造を形成しており、また、純Ｆ
ｅはｆｃｃまたはｂｃｃ構造を形成している。したがって、本発明のように、Ｎｉ−Ｍ系合金粉末、純Ｆｅ粉末、純Ｃｏ粉末を用いて混合し、作製したターゲット材では、ｆｃｃまたはｈｃｐ相の純Ｃｏやｆｃｃまたはｂｃｃ相の純Ｆｅが存在していることがＸ線回折より明確に観測することができる。一方、合金化したＦｅやＣｏではこれらのピークは観測しないことが判明した。
The pure Co according to the present invention has an fcc or hcp structure, and is pure F
e forms an fcc or bcc structure. Therefore, as in the present invention, the target material prepared by mixing using Ni-M alloy powder, pure Fe powder, and pure Co powder has fcc or hcp phase pure Co or fcc or bcc phase pure Fe. The existence can be clearly observed from X-ray diffraction. On the other hand, it has been found that these peaks are not observed in alloyed Fe and Co.
作製した合金粉末は５００μｍ以下に分級した粉末が好ましい。粉末の作製は、ガスア
トマイズ法、水アトマイズ法や回転ディスク式アトマイズ法などを適用することができる。作製したターゲット材の漏洩磁束（Ｐａｓｓ−Ｔｈｒｏｕｇｈ−Ｆｌｕｘ、以下ＰＴＦと記す）の測定に当たっては、ターゲット材の裏面に永久磁石を配置し、ターゲット材表面に漏洩する磁束を測定した。この方法は、マグネトロンスパッタ装置に近い状態の漏洩磁束を定量的に測定できる。実際の測定はＡＳＴＭ Ｆ２８０６−０１（Ｓｔａｎｄａｒｄ Ｔｅｓｔ Ｍｅｔｈｏｄ ｆｏｒ Ｐａｓｓ Ｔｈｒｏｕｇｈ Ｆｌｕｘ ｏｆ Ｃｉｒｃｕｌａｒ Ｍａｇｎｅｔｉｃ Ｓｐｕｔｔｅｒｉｎｇ Ｔａｒｇｅｔｓ Ｍｅｔｈｏｄ２）に基づいて行い、次式よりＰＴＦを求めた。（ＰＴＦ）＝１００×（ターゲット材を置いた状態での磁束の強さ）÷（ターゲット材を置かない状態での磁束の強さ）（％）
The produced alloy powder is preferably a powder classified to 500 μm or less. For the production of the powder, a gas atomizing method, a water atomizing method, a rotating disk atomizing method, or the like can be applied. In measuring the leakage magnetic flux (Pass-Through-Flux, hereinafter referred to as PTF) of the produced target material, a permanent magnet was disposed on the back surface of the target material, and the magnetic flux leaking to the target material surface was measured. This method can quantitatively measure the leakage magnetic flux in a state close to a magnetron sputtering apparatus. Actual measurement was performed based on ASTM F2806-01 (Standard Test Method for Pass Through Flux of Circular Magnetic Sputtering Targets Method 2), and PTF was obtained from the following equation. (PTF) = 100 × (Magnetic strength with target material placed) ÷ (Magnetic strength with no target material placed) (%)
以下、本発明についてさらに実施例により具体的に説明する。
原料粉末において、純Ｆｅ粉末、純Ｃｏ粉末、Ｎｉ−Ｍ系合金粉末は、ガスアトマイズ法によって作製した。ガスアトマイズ法の条件は、ガス種類がアルゴンガス、ノズル径が６ｍｍ、ガス圧が５ＭＰａの条件で行った。
Hereinafter, the present invention will be described more specifically with reference to examples.
In the raw material powder, pure Fe powder, pure Co powder, and Ni-M alloy powder were produced by a gas atomization method. The gas atomization method was performed under the conditions that the gas type was argon gas, the nozzle diameter was 6 mm, and the gas pressure was 5 MPa.
上述したＮｉ−Ｍ系合金粉末に対して、純Ｆｅ粉末、純Ｃｏ粉末の各混合粉末をＳＣ材質からなる封入缶に充填し、到達真空度１０-1Ｐａ以上で脱気真空封入した後、加圧焼結方法にて、温度１１００Ｋ、１４７ＭＰａ、保持時間５時間の条件、ないしは温度９５０Ｋ、１４７ＭＰａ、保持時間５時間の条件で、成形体を作製し、次いで機械加工により最終形状として外径１８０ｍｍ、厚み７ｍｍのターゲット材を得た。混合粉末は、純Ｆｅ粉末、純Ｃｏ粉末、Ｎｉ−Ｍ系合金粉末をＶ型混合機により１時間攪拌したものを使用した。また、混合粉末の加圧焼結方法としては、ホットプレス、熱間静水圧プレス、通電加圧焼結、熱間押し出しなどを適用することができる。 After filling the above-mentioned Ni-M alloy powder with a mixed powder of pure Fe powder and pure Co powder in a sealed can made of SC material, and after deaeration vacuum sealing at an ultimate vacuum of 10 -1 Pa or higher, A compact is produced by pressure sintering at a temperature of 1100 K, 147 MPa and a holding time of 5 hours, or a temperature of 950 K, 147 MPa and a holding time of 5 hours, and then machined to obtain a final shape with an outer diameter of 180 mm. A target material having a thickness of 7 mm was obtained. As the mixed powder, pure Fe powder, pure Co powder, and Ni-M alloy powder were stirred for 1 hour with a V-type mixer. Moreover, as a pressure sintering method of the mixed powder, hot pressing, hot isostatic pressing, energizing pressure sintering, hot extrusion, and the like can be applied.
得られたターゲット材の特性についての測定、評価について述べる。
［透磁率］
作製したターゲット材の透磁率の測定に当たっては、外径１５ｍｍ、内径１０ｍｍ、高さ５ｍｍのリング試験片を製作し、ＢＨトレーサーを用いて、８ｋＡ／ｍの印加磁場にて最大透磁率を測定した。最大透磁率が１０００以下を○、１０００を超えるものを×とした。
Measurement and evaluation of the characteristics of the obtained target material will be described.
[Permeability]
In measuring the permeability of the prepared target material, a ring test piece having an outer diameter of 15 mm, an inner diameter of 10 mm, and a height of 5 mm was manufactured, and the maximum permeability was measured with a BH tracer in an applied magnetic field of 8 kA / m. . The maximum magnetic permeability was 1000 or less, and the case where the maximum permeability exceeded 1000 was rated as x.
［ＰＴＦ］
作製したターゲット材のＰＴＦの測定に当たっては、ターゲット材の裏面に永久磁石を配置し、ターゲット材表面に漏洩する磁束を測定した。比較例のターゲット材のＰＴＦは１０％以下であったが、本発明の実施例のターゲット材はいずれも１０％以上のＰＴＦを示した。
[PTF]
In measuring the PTF of the produced target material, a permanent magnet was placed on the back surface of the target material, and the magnetic flux leaking to the target material surface was measured. The PTF of the target material of the comparative example was 10% or less, but all of the target materials of the examples of the present invention showed 10% or more of PTF.
［Ｆｅ相、Ｃｏ相］
作製したターゲット材のＣｏ相やＦｅ相の観測に当たっては、幅１０ｍｍ、長さ２０ｍｍ、厚み５ｍｍの試験片を製作し、Ｘ線回折装置にて回折パターンを得た。Ｘ源はＣｕ−α線でスキャンスピード４°／ｍｉｎで測定した。実施例のターゲット材のＸＲＤパターンでは、メインピークと共にｆｃｃまたはｈｃｐのＣｏ相や、ｆｃｃまたはｂｃｃのＦｅ相に起因するピークを観測した。ＸＲＤによりｆｃｃまたはｈｃｐのＣｏ相や、ｆｃｃまたはｂｃｃのＦｅ相を観測したものを○、観測しなかったものを×とする。
[Fe phase, Co phase]
In observing the Co phase and Fe phase of the prepared target material, a test piece having a width of 10 mm, a length of 20 mm, and a thickness of 5 mm was produced, and a diffraction pattern was obtained using an X-ray diffractometer. The X source was Cu-α ray and measured at a scan speed of 4 ° / min. In the XRD pattern of the target material of the example, a peak due to the fcc or hcp Co phase or the fcc or bcc Fe phase was observed together with the main peak. The case where the Co phase of fcc or hcp or the Fe phase of fcc or bcc was observed by XRD is indicated by ◯, and the case where the fcc or bcc Fe phase is not observed is indicated by ×.
［成分偏析］
作製したターゲット材の成分分布測定に当たっては、幅１０ｍｍ、長さ２０ｍｍ、厚み５ｍｍの試験片を製作し、ＥＰＭＡ（電子ブローブマイクロアナライザ）より各主成分の分布を観測した。比較例のターゲット材において、Ｆｅ、Ｃｏが均一に存在していたが、実施例のターゲット材においては、Ｆｅ、Ｃｏ成分の分布に偏りがあり、Ｎｉ−Ｍ系中にＦｅ、Ｃｏの単一相が切り離された状態で混在していることを観測した。ＥＰＭＡよりＦｅ、Ｃｏ成分の分布に偏りがあるものを○、Ｆｅ、Ｃｏが均一に存在しているものを×と示した。
[Component segregation]
In measuring the component distribution of the prepared target material, a test piece having a width of 10 mm, a length of 20 mm, and a thickness of 5 mm was manufactured, and the distribution of each main component was observed with an EPMA (electronic probe microanalyzer). In the target material of the comparative example, Fe and Co existed uniformly, but in the target material of the example, the distribution of Fe and Co components was uneven, and the single Fe and Co in the Ni-M system. It was observed that the phases were separated and separated. The case where the distribution of Fe and Co components is biased from EPMA is indicated by ◯, and the case where Fe and Co are uniformly present is indicated by ×.
表２に示すように、比較例３１〜４１は、磁性を有するＮｉ系シード層用合金ターゲッ
ト材の原料として、単にＦｅ源やＣｏ源に合金のみを用いることで、磁性を持つＦｅ、Ｃｏが均一に存在するため、１０００μｍを超える透磁率を観測し、ＰＴＦは１０％未満であった。また、ＦｅやＣｏは合金の状態で存在しており、ＸＲＤによるそれぞれ固有のピークは観測しなかった。
As shown in Table 2, in Comparative Examples 31 to 41, as a raw material for the alloy target material for the Ni-based seed layer having magnetism, Fe and Co having magnetism can be obtained simply by using an alloy for the Fe source and Co source. Since it exists uniformly, the magnetic permeability exceeding 1000 micrometers was observed and PTF was less than 10%. Fe and Co existed in an alloy state, and no unique peak was observed by XRD.
これに対し、本発明例Ｎｏ．１〜３０においては、いずれも原料粉末としてＮｉ−Ｍ系合金粉末、純Ｆｅ粉末、純Ｃｏ粉末を用いて混合し、成形することで、磁性が弱い、または磁性を持たないＮｉ系合金中に、磁性を有するＦｅやＣｏを切り離して混在しているため、１０００μｍ以下の透磁率を示し、１０％以上のＰＴＦを示した。また、ＦｅやＣｏは単体で存在しており、Ｘ線回折よりｆｃｃまたはｈｃｐ相のＣｏやｆｃｃまたはｂｃｃ相のＦｅを観測した。この結果、本発明についてのＮｏ．１〜３０のいずれも純Ｆｅ粉末、純Ｃｏ粉末を成形に使用し、Ｎｉ−Ｍ系中にＦｅ、Ｃｏの単一相が切り離された状態で混在しているスパッタリングターゲット材は、透磁率の低下していることがわかる。 On the other hand, the present invention example No. 1 to 30, all are mixed using Ni-M alloy powder, pure Fe powder, and pure Co powder as raw material powders, and formed into a Ni-based alloy that is weak or non-magnetic. Since Fe and Co having magnetism are separated and mixed, the magnetic permeability is 1000 μm or less, and the PTF is 10% or more. Fe and Co exist alone, and fcc or hcp phase Co or fcc or bcc phase Fe was observed by X-ray diffraction. As a result, no. 1 to 30 use pure Fe powder and pure Co powder for molding, and the sputtering target material in which a single phase of Fe and Co is separated in the Ni-M system is magnetic permeability. It turns out that it has fallen.
以上述べたように、本発明では、Ｎｉ−Ｆｅ−Ｃｏ−Ｍ合金であって、Ｎｉ、Ｆｅ、Ｃｏの比率がａｔ％で、Ｎｉ：Ｆｅ：Ｃｏ＝９８〜２０：０〜５０：０〜６０、Ｆｅ＋Ｃｏ≧１．５であり、かつ、Ｍ元素としてＷ，Ｍｏ，Ｔａ，Ｃｒ，Ｖ，Ｎｂの１種または２種以上を２〜２０ａｔ％含有するスパッタリングターゲット材であって、Ｎｉ−Ｍ系中にＦｅ、Ｃｏの単一相が切り離された状態で混在することで、漏洩磁束が強くスパッタ性に優れたＮｉ系合金スパッタリングターゲット材が得られ、優れた結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 the present invention, the Ni—Fe—Co—M alloy has a ratio of Ni, Fe, and Co of at%, and Ni: Fe: Co = 98 to 20: 0 to 50: 0 to 60, Fe + Co ≧ 1.5, and a sputtering target material containing 2 to 20 at% of one or more of W, Mo, Ta, Cr, V, and Nb as M element, By mixing Fe and Co in a state where a single phase of Fe and Co is separated in the system, a Ni-based alloy sputtering target material having a strong leakage magnetic flux and excellent sputterability can be obtained, and an excellent result can be obtained.
Patent Applicant Sanyo Special Steel Co., Ltd.
Attorney: Attorney Shiina
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| JP2015023101A JP6581780B2 (en) | 2015-02-09 | 2015-02-09 | Ni-based target material with excellent sputtering properties |
| SG11201706370SA SG11201706370SA (en) | 2015-02-09 | 2016-02-04 | Ni-BASED TARGET MATERIAL EXCELLENT IN SPUTTERING PROPERTY |
| SG10201906538UA SG10201906538UA (en) | 2015-02-09 | 2016-02-04 | Ni-BASED TARGET MATERIAL EXCELLENT IN SPUTTERING PROPERTY |
| CN201680006203.9A CN107250424A (en) | 2015-02-09 | 2016-02-04 | The excellent Ni series target materials of sputtering |
| PCT/JP2016/053350 WO2016129492A1 (en) | 2015-02-09 | 2016-02-04 | Ni BASED TARGET MATERIAL WITH EXCELLENT SPUTTERING PROPERTIES |
| MYPI2017702870A MY188184A (en) | 2015-02-09 | 2016-02-04 | Ni-based target material excellent in sputtering property |
| TW105104154A TW201700742A (en) | 2015-02-09 | 2016-02-05 | Ni based target material with excellent sputtering properties |
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| CN115161603B (en) * | 2022-05-17 | 2023-02-21 | 广东欧莱高新材料股份有限公司 | Production process of high-purity multi-element alloy rotary sputtering target for high-definition liquid crystal display of high generation |
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| JP2005530925A (en) * | 2002-06-07 | 2005-10-13 | ヘラエウス インコーポレーテッド | High PTF sputtering target and manufacturing method thereof |
| JP2010095794A (en) * | 2008-09-22 | 2010-04-30 | Hitachi Metals Ltd | METHOD FOR PRODUCING Co-Fe-Ni-BASED ALLOY SPUTTERING TARGET MATERIAL |
| JP2010248603A (en) * | 2009-04-20 | 2010-11-04 | Hitachi Metals Ltd | METHOD FOR PRODUCING Fe-Co-Ni-BASED ALLOY SPUTTERING TARGET MATERIAL |
| JP2012128933A (en) * | 2010-11-22 | 2012-07-05 | Sanyo Special Steel Co Ltd | Alloy for seed layer of magnetic recording medium, and sputtering target material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021054136A1 (en) * | 2019-09-19 | 2021-03-25 | 日立金属株式会社 | Target |
| JP7552604B2 (en) | 2019-09-19 | 2024-09-18 | 株式会社プロテリアル | target |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6581780B2 (en) | 2019-09-25 |
| SG10201906538UA (en) | 2019-08-27 |
| MY188184A (en) | 2021-11-24 |
| TW201700742A (en) | 2017-01-01 |
| WO2016129492A1 (en) | 2016-08-18 |
| CN107250424A (en) | 2017-10-13 |
| SG11201706370SA (en) | 2017-09-28 |
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