JP2011181140A - Fe-Co BASED ALLOY SOFT MAGNETIC FILM FOR MAGNETIC RECORDING MEDIUM - Google Patents
Fe-Co BASED ALLOY SOFT MAGNETIC FILM FOR MAGNETIC RECORDING MEDIUM Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 64
- 239000000956 alloy Substances 0.000 title claims abstract description 64
- 229910017061 Fe Co Inorganic materials 0.000 title claims abstract description 48
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000002425 crystallisation Methods 0.000 abstract description 18
- 230000008025 crystallization Effects 0.000 abstract description 18
- 239000010408 film Substances 0.000 description 64
- 238000002441 X-ray diffraction Methods 0.000 description 21
- 239000000843 powder Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 17
- 238000000034 method Methods 0.000 description 15
- 239000013077 target material Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 10
- 239000011521 glass Substances 0.000 description 7
- 238000005477 sputtering target Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 229910052715 tantalum Inorganic materials 0.000 description 5
- 238000009689 gas atomisation Methods 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 3
- 239000002775 capsule Substances 0.000 description 3
- 229910020674 Co—B Inorganic materials 0.000 description 2
- 229910005335 FePt Inorganic materials 0.000 description 2
- 229910001362 Ta alloys Inorganic materials 0.000 description 2
- 238000005280 amorphization Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 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
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Magnetic Record Carriers (AREA)
- Thin Magnetic Films (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
本発明は、磁気記録媒体に用いられるＦｅ−Ｃｏ系合金軟磁性膜に関するものである。 The present invention relates to an Fe—Co alloy soft magnetic film used for a magnetic recording medium.
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、使用されている垂直磁気記録方式の磁気記録媒体で、記録密度を高めるために記録ビットを微細化していくと、磁気的に記録したデータが周囲の熱の影響で消える熱揺らぎの問題がある。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熱アシスト磁気記録方式が検討されている。
熱アシスト磁気記録方式とは、熱揺らぎ対策のために磁気の保磁力を高めた媒体にヘッドから微細な熱を照射し、その部分の磁気保磁力を下げてデータの記録を行う方式である。この、熱アシスト磁気記録方式においては、高い保磁力を有するＦｅＰｔ規則合金等の記録層と軟磁性膜層とを有する記録媒体が開発されている。
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 perpendicular magnetic recording type magnetic recording medium that is currently used, if the recording bits are made finer to increase the recording density, the magnetically recorded data disappears due to the influence of ambient heat. There's a problem. Therefore, a heat-assisted magnetic recording method has been studied as a means for solving these problems and improving the recording density.
The heat-assisted magnetic recording system is a system in which data is recorded by irradiating a medium with a high magnetic coercive force from a head to reduce thermal fluctuation from the head and lowering the magnetic coercive force of that portion. In this thermally assisted magnetic recording system, a recording medium having a recording layer such as an FePt ordered alloy having a high coercive force and a soft magnetic film layer has been developed.
このような磁気記録媒体の軟磁性膜としては、高い飽和磁束密度を有することが要求されており、飽和磁束密度が大きいＦｅ−Ｃｏ合金が一般的に利用されている。また、優れた軟磁気特性を有するためと、軟磁性膜表面の凹凸部からのノイズ発生を抑制するためにアモルファス性の高い合金膜が望まれている。アモルファスとは、結晶のように原子配列が規則的ではなく、短距離秩序はあるが、長距離秩序がないと定義されているが、より短距離秩序をなくす、つまりアモルファス性が高いことが上述の点で好ましい。さらに、熱アシスト磁気記録方式においては、記録層であるＦｅＰｔ合金等を規則化させるために高温アニール処理が必要であり、それに伴って軟磁性膜が結晶化してアモルファスから結晶質膜に変化し、高周波透磁率が低下し記録の際に高転送レートでの書込性が劣化してしまうという問題が指摘されている。（例えば、特許文献１参照）。
また、これまでの一般的な垂直磁気記録媒体のアモルファスの軟磁性膜としては、Ｆｅ−Ｃｏ−Ｔａ合金膜（例えば、特許文献２参照）やＦｅ−Ｃｏ−Ｂ合金膜（例えば、特許文献３参照）が提案されている。
The soft magnetic film of such a magnetic recording medium is required to have a high saturation magnetic flux density, and an Fe—Co alloy having a high saturation magnetic flux density is generally used. In addition, an alloy film having high amorphous property is desired in order to have excellent soft magnetic properties and to suppress noise generation from the uneven portions on the surface of the soft magnetic film. Amorphous is defined as having no short-range order, although the atomic arrangement is not regular like crystals, but there is no long-range order. This is preferable. Furthermore, in the thermally assisted magnetic recording system, a high temperature annealing process is necessary to order the recording layer such as an FePt alloy, and accordingly, the soft magnetic film is crystallized to change from an amorphous to a crystalline film, A problem has been pointed out that the high-frequency magnetic permeability decreases and the writeability at a high transfer rate deteriorates during recording. (For example, refer to Patent Document 1).
Further, as an amorphous soft magnetic film of a conventional general perpendicular magnetic recording medium, an Fe—Co—Ta alloy film (for example, refer to Patent Document 2) or an Fe—Co—B alloy film (for example, Patent Document 3). Have been proposed).
本発明者らの検討によれば、上述の特許文献２に開示される軟磁性膜形成用ターゲット材を用いて成膜したＦｅ−Ｃｏ−Ｔa合金軟磁性膜では、Ｆｅ−Ｃｏ合金にＴａを添加することにより高い結晶化温度を有していたものの、アモルファス性が低いことを確認した。一方、上述の特許文献３に開示されるＦｅ−Ｃｏ−Ｂ合金軟磁性膜では、アモルファス性、結晶化温度とも低いことを確認した。
本発明の目的は、上記の問題を解決し、アモルファス性が高く、かつ高い結晶化温度を有する磁気記録媒体に用いられるＦｅ−Ｃｏ系合金軟磁性膜を提供することである。
According to the study by the present inventors, in the Fe—Co—Ta alloy soft magnetic film formed using the soft magnetic film forming target material disclosed in the above-mentioned Patent Document 2, Ta is added to the Fe—Co alloy. Although it had high crystallization temperature by adding, it confirmed that amorphous nature was low. On the other hand, it was confirmed that the Fe—Co—B alloy soft magnetic film disclosed in Patent Document 3 described above has low amorphous properties and a low crystallization temperature.
An object of the present invention is to solve the above-described problems and provide an Fe—Co alloy soft magnetic film used for a magnetic recording medium having a high amorphous property and a high crystallization temperature.
本発明者らは、磁気記録媒体に用いられるＦｅ−Ｃｏ系合金軟磁性膜について、Ｆｅ−Ｃｏ系合金への添加元素について種々の検討を行った結果、Ｎｂおよび／またはＴａとＢを複合添加し、そして、それぞれの好適な添加範囲を見出し本発明に到達した。 As a result of various studies on the additive elements to the Fe—Co alloy, the inventors have added Nb and / or Ta and B in combination. And the suitable addition range of each was found and the present invention was reached.
すなわち、本発明は、原子比における組成式が（（ＦｅＸ−Ｃｏ１００−Ｘ）１００−ＹＮｉＹ）１００−ａ−ｂ−Ｍａ−Ｂｂ、１０≦Ｘ≦７０、０≦Ｙ≦２５、７≦ａ、１≦ｂ≦５、１３≦ａ＋ｂ≦２５で表され、前記組成式のＭ元素がＮｂおよび／またはＴａである磁気記録媒体用軟磁性膜であって、膜厚が１０〜５００ｎｍの磁気記録媒体用Ｆｅ−Ｃｏ系合金軟磁性膜である。 That is, the present invention provides a composition formula in the atomic ratio ((Fe X -Co 100-X ) 100-Y Ni Y) 100-a-b -M a -B b, 10 ≦ X ≦ 70,0 ≦ Y ≦ 25, 7 ≦ a, 1 ≦ b ≦ 5, 13 ≦ a + b ≦ 25, and a soft magnetic film for a magnetic recording medium in which the M element of the composition formula is Nb and / or Ta, and the film thickness is 10 It is a Fe-Co alloy soft magnetic film for magnetic recording media of ˜500 nm.
本発明により、アモルファス性が高く、かつ高い結晶化温度を有する磁気記録媒体に用いられるＦｅ−Ｃｏ系合金軟磁性膜を提供でき、磁気記録媒体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 alloy soft magnetic film used for a magnetic recording medium having a high amorphous property and a high crystallization temperature can be provided, which is an extremely effective technique for manufacturing a magnetic recording medium.
本発明の最も重要な特徴は、軟磁性膜としてＦｅ−Ｃｏ系合金中に、アモルファス性と結晶化温度を高めるための最適な元素としてＮｂおよび／またはＴａとＢとを選択し、さらに上記の効果を実現するためのそれぞれの最適な添加量を見出した点にある。 The most important feature of the present invention is that Nb and / or Ta and B are selected as the optimum elements for increasing the amorphous nature and the crystallization temperature in the Fe-Co alloy as the soft magnetic film, and It is the point which discovered each optimal addition amount for implement | achieving an effect.
まず、本発明のベースとなるＦｅ−Ｃｏ系合金に関して説明する。
本発明の合金のベースとなるＦｅ−Ｃｏ合金は、原子比による組成式が（（ＦｅＸ−Ｃｏ１００−Ｘ）１００−ＹＮｉＹ）、１０≦Ｘ≦７０、０≦Ｙ≦２５で表される組成である。それは、この組成範囲にあるＦｅ−Ｃｏ合金は飽和磁化が大きく、軟磁性膜として適切であるためである。なお、Ｆｅ−Ｃｏ合金に対して、最大２５原子％のＮｉで置換することも可能である。Ｎｉをこの範囲で含有させることで、磁歪が低減でき、薄膜の軟磁気特性を向上させる効果があるためである。なお、高い飽和磁化膜が要求される場合にはＮｉは含有させない方が好ましい。また、Ｎｉの組成比が原子比で２５％を超えると飽和磁化の低下が大きくなる。
First, the Fe—Co alloy used as the base of the present invention will be described.
The Fe—Co alloy serving as the base of the alloy of the present invention has a composition formula based on an atomic ratio represented by ((Fe X -Co 100-X ) 100-Y Ni Y ), 10 ≦ X ≦ 70, 0 ≦ Y ≦ 25. Composition. This is because an Fe—Co alloy in this composition range has a large saturation magnetization and is suitable as a soft magnetic film. Note that it is possible to replace the Fe—Co alloy with a maximum of 25 atomic% Ni. This is because inclusion of Ni in this range can reduce magnetostriction and improve the soft magnetic properties of the thin film. When a high saturation magnetization film is required, it is preferable not to contain Ni. Further, when the composition ratio of Ni exceeds 25% by atomic ratio, the saturation magnetization is greatly reduced.
本発明のＦｅ−Ｃｏ系合金では、上述のＦｅ−Ｃｏ合金にＭ元素としてＮｂおよび／またはＴａを７原子％以上含有するものである。それは、Ｍ元素の添加によりＦｅ−Ｃｏ合金がアモルファス化すると同時に、Ｍ元素自身の融点も高い上、Ｆｅ−Ｃｏ合金の融点を上昇させることができるため軟磁性膜が結晶質化する温度である結晶化温度を高めることが可能となるためである。なお、Ｍ元素の添加量が７原子％に満たない場合には、Ｆｅ−Ｃｏ合金のアモルファス化が困難となる。 In the Fe—Co alloy of the present invention, the above-described Fe—Co alloy contains 7 atom% or more of Nb and / or Ta as M elements. This is the temperature at which the soft magnetic film crystallizes because the Fe-Co alloy becomes amorphous by the addition of the M element and at the same time the melting point of the M element itself is high and the melting point of the Fe-Co alloy can be increased. This is because the crystallization temperature can be increased. Note that when the amount of M element added is less than 7 atomic%, it becomes difficult to make the Fe—Co alloy amorphous.
本発明のＦｅ−Ｃｏ系合金では、上述のＭ元素であるＮｂやＴａを含有するＦｅ−Ｃｏ系合金にアモルファス性をさらに効果的に向上させる必須元素としてＢを１原子％以上５原子％以下で、かつＭ元素との合計で１３〜２５原子％含有する。Ｂは、Ｆｅ−Ｃｏ系合金のアモルファス化を促進させる元素であり、特に原子半径の異なるＭ元素と複合的に含有させることで、Ｆｅ−Ｃｏ系合金のアモルファス化をさらに促進させることが可能となる。なお、ＢとＭ元素との合計が１３原子％に満たない場合には、アモルファス化と結晶化温度を高める効果が少なく、２５原子％を超えると飽和磁化の低下が大きくなるため、１３〜２５原子％の範囲に制御することが重要である。 In the Fe—Co based alloy of the present invention, B is 1 atomic% or more and 5 atomic% or less as an essential element for further effectively improving the amorphousness in the Fe—Co based alloy containing the above-mentioned M element Nb or Ta. And 13 to 25 atomic% in total with M element. B is an element that promotes the amorphization of the Fe—Co-based alloy. In particular, B can be further promoted to amorphize the Fe—Co-based alloy by compounding with M elements having different atomic radii. Become. When the total of B and M elements is less than 13 atomic%, the effect of increasing the amorphization and crystallization temperature is small, and when it exceeds 25 atomic%, the saturation magnetization is greatly reduced. It is important to control to the atomic% range.
また、本発明の磁気記録媒体用軟磁性膜においては、Ｂの含有量を５原子％以下とする。それは、５原子％を超えるＢを添加すると結晶化温度が低下するためである。さらに、Ｂを多量に含む軟磁性膜を形成するためには、軟磁性膜を形成するために用いられるスパッタリングターゲット材中に多量のＢを含有させる必要がある。Ｂを多量に含むターゲット材ではＢがミクロ組織中に硼化物として存在することとなるため、この硼化物がスパッタリング時の異常放電やパーティクルなどの問題の原因となる場合がある。そこで、Ｆｅ−Ｃｏ系合金軟磁性膜のスパッタリング成膜時の問題を抑制するためにも、Ｂの含有量は５原子％以下とした。 In the soft magnetic film for a magnetic recording medium of the present invention, the B content is 5 atomic% or less. This is because the crystallization temperature is lowered when B exceeding 5 atomic% is added. Furthermore, in order to form a soft magnetic film containing a large amount of B, it is necessary to include a large amount of B in the sputtering target material used for forming the soft magnetic film. In a target material containing a large amount of B, since B exists as a boride in the microstructure, the boride may cause problems such as abnormal discharge and particles during sputtering. Therefore, the B content is set to 5 atomic% or less in order to suppress problems during sputtering of the Fe—Co alloy soft magnetic film.
また、本発明の磁気記録媒体用軟磁性膜においては、膜厚を１０〜５００ｎｍとする。それは、膜厚が１０ｎｍ未満であると、膜厚が薄いために、磁気記録における記録効率低下が顕著になり、記録ビットの磁化反転が確実に行えない問題が生じる場合がある。一方、膜厚が５００ｎｍを超えると膜応力が大きくなり膜が剥れやすくなり、さらに膜を形成するのに時間がかかり、生産性が低下するためである。 In the soft magnetic film for a magnetic recording medium of the present invention, the film thickness is 10 to 500 nm. That is, if the film thickness is less than 10 nm, the film thickness is so thin that the recording efficiency is significantly reduced in magnetic recording, and there is a problem that the magnetization reversal of the recording bit cannot be performed reliably. On the other hand, when the film thickness exceeds 500 nm, the film stress increases and the film is easily peeled off, and further, it takes time to form the film and the productivity is lowered.
上述したＦｅ−Ｃｏ系合金膜を形成する方法としては、真空蒸着法、スパッタリング法および化学気相成長法を用いることができる。中でも高速に安定した膜が形成できるため、Ｆｅ−Ｃｏ系合金軟磁性膜と同一組成のターゲット材をスパッタリングして薄膜を形成するスパッタリング法が好ましい。 As a method for forming the above-described Fe—Co alloy film, a vacuum deposition method, a sputtering method, and a chemical vapor deposition method can be used. In particular, since a stable film can be formed at high speed, a sputtering method in which a thin film is formed by sputtering a target material having the same composition as that of the Fe—Co alloy soft magnetic film is preferable.
上述したＦｅ−Ｃｏ系合金軟磁性膜を形成するために用いられるスパッタリングターゲット材の製造方法としては、溶解鋳造法や粉末焼結法が適用可能である。溶解鋳造法では、鋳造インゴット、もしくは、鋳造インゴットに塑性加工や加圧加工を加えたバルク体とすることで製造可能となる。また、粉末焼結法では、ガスアトマイズ法でＦｅ−Ｃｏ系合金の最終組成の合金粉末を製造し原料粉末とすることや、複数の合金粉末や純金属粉末をＦｅ−Ｃｏ系合金の最終組成となるように混合した混合粉末を原料粉末とすることが可能である。原料粉末の焼結方法としては、熱間静水圧プレス、ホットプレス、放電プラズマ焼結、押し出しプレス焼結等の加圧焼結を用いることが可能である。 As a manufacturing method of the sputtering target material used for forming the Fe—Co alloy soft magnetic film described above, a melt casting method or a powder sintering method can be applied. In the melt casting method, it is possible to produce a cast ingot or a bulk body obtained by applying plastic processing or pressure processing to the cast ingot. In the powder sintering method, an alloy powder having the final composition of the Fe-Co alloy is manufactured by a gas atomization method and used as a raw material powder, or a plurality of alloy powders and pure metal powders are combined with the final composition of the Fe-Co alloy. The mixed powder thus mixed can be used as a raw material powder. As a method for sintering the raw material powder, it is possible to use pressure sintering such as hot isostatic pressing, hot pressing, discharge plasma sintering, and extrusion press sintering.
以下の実施例で本発明を更に詳しく説明する。
（実施例１）
まず、純度９９．９％以上の原料を用い（Ｆｅ３０−Ｃｏ７０）８７−Ｔａ１０−Ｂ３（原子％）合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製し、２５０μｍの篩で分級した。そして得られたガスアトマイズ粉末を軟鋼カプセルに充填し、脱気封止した後、温度９５０℃、圧力１２２ＭＰａ、保持時間１時間の条件で熱間静水圧プレスによって焼結し、焼結体を作製した。得られた焼結体に機械加工を施し直径１８０ｍｍ×厚さ５ｍｍのＦｅ−Ｃｏ系合金スパッタリングターゲット材を作製した。
上記で作製したターゲット材をＤＣマグネトロンスパッタ装置（アネルバ社製３０１０）のチャンバ内に配置し、チャンバ内を真空到達温度２×１０−５Ｐａ以下となるまで排気を行った後、寸法７５×２５ｍｍのガラス基板上にＡｒガス圧０．６Ｐａ、投入電力５００Ｗの条件にて膜厚２００ｎｍの軟磁性膜を形成した。
The following examples further illustrate the present invention.
Example 1
First, using a raw material having a purity of 99.9% or more, (Fe 30 -Co 70 ) 87 -Ta 10 -B 3 (atomic%) alloy melt having an alloy composition is vacuum-dissolved, and gas atomized powder is formed by a gas atomizing method using Ar gas. It produced and classified with the sieve of 250 micrometers. The obtained gas atomized powder was filled into a mild steel capsule and degassed and sealed, and then sintered by hot isostatic pressing under conditions of a temperature of 950 ° C., a pressure of 122 MPa, and a holding time of 1 hour to prepare a sintered body. . The obtained sintered body was machined to produce a Fe—Co alloy sputtering target material having a diameter of 180 mm × thickness of 5 mm.
The target material prepared above is placed in the chamber of a DC magnetron sputtering apparatus (3010 manufactured by Anerva), the inside of the chamber is evacuated to a vacuum ultimate temperature of 2 × 10 −5 Pa or less, and then a size of 75 × 25 mm. A soft magnetic film having a thickness of 200 nm was formed on the glass substrate under the conditions of Ar gas pressure 0.6 Pa and input power 500 W.
（比較例１）
純度９９．９％以上の原料を用い（Ｆｅ３０−Ｃｏ７０）８７−Ｔａ５−Ｂ８（原子％）合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、実施例１と同様の条件で直径１８０ｍｍ×厚さ５ｍｍのＦｅ−Ｃｏ系合金スパッタリングターゲット材を作製した。また、作製したターゲット材を使用して、実施例１と同一の条件で、寸法７５×２５ｍｍのガラス基板上に膜厚２００ｎｍの軟磁性膜を形成した。
(Comparative Example 1)
A raw material having a purity of 99.9% or more is used to melt (Fe 30 -Co 70 ) 87 -Ta 5 -B 8 (atomic%) in an alloy melt in a vacuum, and a gas atomized powder is produced by a gas atomizing method using Ar gas. A Fe—Co alloy sputtering target material having a diameter of 180 mm and a thickness of 5 mm was produced under the same conditions as in Example 1. A soft magnetic film having a film thickness of 200 nm was formed on a glass substrate having a size of 75 × 25 mm under the same conditions as in Example 1 using the prepared target material.
（比較例２）
それそれ純度９９．９％以上のＦｅ原料粉末（１５０μｍアンダー）、Ｃｏ原料粉末（２５０μｍアンダー）、Ｔａ原料粉末（４５μｍアンダー）を準備し、（Ｆｅ３０−Ｃｏ７０）８７−Ｔａ１３（原子％）合金組成となるように、秤量、混合して混合粉末を作製した。得られた混合粉末を軟鋼カプセルに充填し、脱気封止した後、温度１２５０℃、圧力１２２ＭＰａ、保持時間２時間の条件で熱間静水圧プレスによって焼結し、焼結体を作製した。得られた焼結体に機械加工を施し直径１８０ｍｍ×厚さ５ｍｍのＦｅ−Ｃｏ系合金スパッタリングターゲット材を作製した。また、作製したターゲット材を使用して、実施例１と同一の条件で、寸法７５×２５ｍｍのガラス基板上に膜厚２００ｎｍの軟磁性膜を形成した。
(Comparative Example 2)
Fe raw material powder (under 150 μm), Co raw material powder (under 250 μm), and Ta raw material powder (under 45 μm) having a purity of 99.9% or more were prepared, and (Fe 30 -Co 70 ) 87 -Ta 13 (atomic%) ) Weighed and mixed so as to have an alloy composition to prepare a mixed powder. The obtained mixed powder was filled into a mild steel capsule and sealed by deaeration, and then sintered by hot isostatic pressing under conditions of a temperature of 1250 ° C., a pressure of 122 MPa, and a holding time of 2 hours to prepare a sintered body. The obtained sintered body was machined to produce a Fe—Co alloy sputtering target material having a diameter of 180 mm × thickness of 5 mm. A soft magnetic film having a film thickness of 200 nm was formed on a glass substrate having a size of 75 × 25 mm under the same conditions as in Example 1 using the prepared target material.
上記で形成した実施例１、比較例１、比較例２の軟磁性膜を形成した各ガラス基板を５個（寸法２５×２５ｍｍ）に切断した試料を作製した。各試料について、以下の測定を行った。
（１）Ｘ線回折による半価幅測定
各例の試料のうち１個を（株）リガク製Ｘ線回折装置ＲＩＮＴ２５００Ｖを使用し、線源にＣｏを用いて軟磁性膜のＸ線回折測定を行った。得られたＸ線回折パターンから２θ＝５２°付近のブロードなピークの半価幅を求め、表１に示した。ここで、半価幅とは、Ｘ線回折ピークの１／２強度におけるピーク幅であり、アモルファス性の高い膜では、原子配列の短距離秩序がよりなくなるため、Ｘ線回折ピークがブロードになり、半価幅は大きくなる。
（２）結晶化温度の測定
各例の試料のうち４個を使用して、０．５Ｐａ以下に減圧した真空雰囲気で、それぞれ３００℃×１０分、３５０℃×１０分、４００℃×１０分、４５０℃×１０分の加熱処理を施した後、Ｘ線回折測定を行った。図１に実施例１のＸ線回折パターンを、図２に比較例１のＸ線回折パターンを、図３に比較例２のＸ線回折パターンをそれぞれ示す。図１〜３から、結晶化温度を求め、表１に示した。
Samples were prepared by cutting each glass substrate on which the soft magnetic films of Example 1, Comparative Example 1, and Comparative Example 2 formed above were cut into five pieces (25 × 25 mm). The following measurements were performed for each sample.
(1) Half width measurement by X-ray diffraction One sample of each example was measured using a Rigaku X-ray diffractometer RINT2500V, and Co was used as a radiation source for X-ray diffraction measurement of a soft magnetic film. went. The half-value width of a broad peak near 2θ = 52 ° was determined from the obtained X-ray diffraction pattern and is shown in Table 1. Here, the half width is a peak width at half the intensity of the X-ray diffraction peak. In a highly amorphous film, the short-range order of the atomic arrangement is further lost, so the X-ray diffraction peak becomes broad. The full width at half maximum increases.
(2) Measurement of crystallization temperature Using four of the samples of each example, in a vacuum atmosphere reduced to 0.5 Pa or less, 300 ° C. × 10 minutes, 350 ° C. × 10 minutes, 400 ° C. × 10 minutes, respectively. After the heat treatment at 450 ° C. for 10 minutes, X-ray diffraction measurement was performed. FIG. 1 shows the X-ray diffraction pattern of Example 1, FIG. 2 shows the X-ray diffraction pattern of Comparative Example 1, and FIG. 3 shows the X-ray diffraction pattern of Comparative Example 2. The crystallization temperature was determined from FIGS.
表１から、実施例１のＦｅ−Ｃｏ系合金軟磁性膜と比較例１のＦｅ−Ｃｏ系合金軟磁性膜は、比較例２のＦｅ−Ｃｏ系合金軟磁性膜より半価幅が大きいためアモルファス性が高いことが分かる。また、実施例1のＦｅ−Ｃｏ系合金軟磁性膜と比較例２のＦｅ−Ｃｏ系合金軟磁性膜は、比較例１のＦｅ−Ｃｏ系合金軟磁性膜より高い結晶化温度を有していることが分かる。
よって、ＴａとＢとを適量添加した本発明のＦｅ−Ｃｏ系合金軟磁性膜は、アモルファス性が高く、かつ高い結晶化温度を有していることが確認できた。
From Table 1, the Fe—Co alloy soft magnetic film of Example 1 and the Fe—Co alloy soft magnetic film of Comparative Example 1 have a larger half width than the Fe—Co alloy soft magnetic film of Comparative Example 2. It can be seen that the amorphous property is high. In addition, the Fe—Co alloy soft magnetic film of Example 1 and the Fe—Co alloy soft magnetic film of Comparative Example 2 have higher crystallization temperatures than the Fe—Co alloy soft magnetic film of Comparative Example 1. I understand that.
Therefore, it was confirmed that the Fe—Co alloy soft magnetic film of the present invention to which appropriate amounts of Ta and B were added had high amorphousness and a high crystallization temperature.
（実施例２）
純度９９．９％以上の原料を用い（Ｆｅ６５−Ｃｏ３５）８７−Ｔａ８−Ｂ５（原子％）合金組成となる合金溶湯を真空溶解し、Ａｒガスによるガスアトマイズ法によってガスアトマイズ粉末を作製する以外は、実施例１と同様の条件で直径１８０ｍｍ×厚さ５ｍｍのＦｅ−Ｃｏ系合金スパッタリングターゲット材を作製した。また、作製したターゲット材を使用して、実施例１と同一の条件で、寸法７５×２５ｍｍのガラス基板上に膜厚２００ｎｍの軟磁性膜を形成した。
(Example 2)
Using a raw material with a purity of 99.9% or more, (Fe 65 -Co 35 ) 87 -Ta 8 -B 5 (atomic%) is melted in a vacuum with an alloy composition, and a gas atomized powder is produced by a gas atomizing method using Ar gas. A Fe—Co alloy sputtering target material having a diameter of 180 mm and a thickness of 5 mm was produced under the same conditions as in Example 1. A soft magnetic film having a film thickness of 200 nm was formed on a glass substrate having a size of 75 × 25 mm under the same conditions as in Example 1 using the prepared target material.
（比較例３）
それそれ純度９９．９％以上のＦｅ原料粉末（１５０μｍアンダー）、Ｆｅ８８−Ｂ１２（原子％）合金ガスアトマイズ粉末、Ｃｏ８８−Ｂ１２（原子％）合金ガスアトマイズ粉末を準備し、（Ｆｅ６５−Ｃｏ３５）８７−Ｂ１３（原子％）合金組成となるように、秤量、混合して混合粉末を作製した。得られた混合粉末を軟鋼カプセルに充填し、脱気封止した後、温度１２５０℃、圧力１２２ＭＰａ、保持時間２時間の条件で熱間静水圧プレスによって焼結し、焼結体を作製した。得られた焼結体に機械加工を施し直径１８０ｍｍ×厚さ５ｍｍのＦｅ−Ｃｏ系合金スパッタリングターゲット材を作製した。また、作製したターゲット材を使用して、実施例１と同一の条件で、寸法７５×２５ｍｍのガラス基板上に膜厚２００ｎｍの軟磁性膜を形成した。
(Comparative Example 3)
Fe raw material powder (under 150 μm) having a purity of 99.9% or more, Fe 88 -B 12 (atomic%) alloy gas atomized powder, Co 88 -B 12 (atomic%) alloy gas atomized powder were prepared, and (Fe 65 − A mixed powder was prepared by weighing and mixing to obtain a Co 35 ) 87 -B 13 (atomic%) alloy composition. The obtained mixed powder was filled into a mild steel capsule and sealed by deaeration, and then sintered by hot isostatic pressing under conditions of a temperature of 1250 ° C., a pressure of 122 MPa, and a holding time of 2 hours to prepare a sintered body. The obtained sintered body was machined to produce a Fe—Co alloy sputtering target material having a diameter of 180 mm × thickness of 5 mm. A soft magnetic film having a film thickness of 200 nm was formed on a glass substrate having a size of 75 × 25 mm under the same conditions as in Example 1 using the prepared target material.
上記で形成した実施例２、比較例３の軟磁性膜を形成した各ガラス基板を５個（寸法２５×２５ｍｍ）に切断した試料を作製した。各試料について、以下の測定を行った。
（１）Ｘ線回折による半価幅測定
各例の試料のうち１個を（株）リガク製Ｘ線回折装置ＲＩＮＴ２５００Ｖを使用し、線源にＣｏを用いてＸ線回折測定を行った。得られたＸ線回折パターンから２θ＝５２°付近のブロードなピークの半価幅を求め、表２に示した。
（２）結晶化温度の測定
各例の試料のうち４個を使用して、０．５Ｐａ以下に減圧した真空雰囲気で、それぞれ３００℃×１０分、３５０℃×１０分、４００℃×１０分、４５０℃×１０分の加熱処理を施した後、Ｘ線回折測定を行った。図４に実施例２のＸ線回折パターンを、図５に比較例３のＸ線回折パターンをそれぞれ示す。図４、５から、結晶化温度を求め、表２に示した。
Samples were prepared by cutting each glass substrate on which the soft magnetic films of Example 2 and Comparative Example 3 formed above were formed into five pieces (size: 25 × 25 mm). The following measurements were performed for each sample.
(1) Half width measurement by X-ray diffraction One sample of each example was subjected to X-ray diffraction measurement using Rigaku X-ray diffraction apparatus RINT2500V and using Co as a radiation source. The half-value width of a broad peak near 2θ = 52 ° was determined from the obtained X-ray diffraction pattern and is shown in Table 2.
(2) Measurement of crystallization temperature Using four of the samples of each example, in a vacuum atmosphere reduced to 0.5 Pa or less, 300 ° C. × 10 minutes, 350 ° C. × 10 minutes, 400 ° C. × 10 minutes, respectively. After the heat treatment at 450 ° C. for 10 minutes, X-ray diffraction measurement was performed. FIG. 4 shows the X-ray diffraction pattern of Example 2, and FIG. 5 shows the X-ray diffraction pattern of Comparative Example 3. 4 and 5, the crystallization temperature was obtained and shown in Table 2.
表２から、実施例２のＦｅ−Ｃｏ系合金軟磁性膜は、比較例３のＦｅ−Ｃｏ系合金軟磁性膜より半価幅が大きいためアモルファス性が高く、かつ高い結晶化温度を有していることが分かる。
よって、ＴａとＢとを適量添加した本発明のＦｅ−Ｃｏ系合金軟磁性膜は、アモルファス性が高く、かつ高い結晶化温度を有していることが確認できた。
From Table 2, the Fe—Co alloy soft magnetic film of Example 2 has a higher half-value width than the Fe—Co alloy soft magnetic film of Comparative Example 3, and thus has high amorphousness and a high crystallization temperature. I understand that
Therefore, it was confirmed that the Fe—Co alloy soft magnetic film of the present invention to which appropriate amounts of Ta and B were added had high amorphousness and a high crystallization temperature.
本発明のＦｅ−Ｃｏ系合金軟磁性膜は、アモルファス性が高く、かつ高い結晶化温度を有しているため、磁気記録媒体等の軟磁性膜として有用であり、適用が可能である。 The Fe—Co alloy soft magnetic film of the present invention is highly amorphous and has a high crystallization temperature. Therefore, the Fe—Co alloy soft magnetic film is useful as a soft magnetic film for magnetic recording media and can be applied.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012108997A (en) * | 2010-10-26 | 2012-06-07 | Sanyo Special Steel Co Ltd | Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium |
| JP2013161497A (en) * | 2012-02-03 | 2013-08-19 | Sanyo Special Steel Co Ltd | Alloy for soft magnetic film layer having low saturation magnetic flux density to be used for magnetic recording medium, and sputtering target material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012108997A (en) * | 2010-10-26 | 2012-06-07 | Sanyo Special Steel Co Ltd | Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium |
| JP2013161497A (en) * | 2012-02-03 | 2013-08-19 | Sanyo Special Steel Co Ltd | Alloy for soft magnetic film layer having low saturation magnetic flux density to be used for magnetic recording medium, and sputtering target material |
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