JP2009203537A - Co-Fe-BASED ALLOY SPUTTERING TARGET MATERIAL, AND METHOD FOR PRODUCING THE SAME - Google Patents
Co-Fe-BASED ALLOY SPUTTERING TARGET MATERIAL, AND METHOD FOR PRODUCING THE SAME Download PDFInfo
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Abstract
Description
本発明は、軟磁性膜を形成するためのＣｏ−Ｆｅ系合金スパッタリング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 a Co—Fe-based alloy sputtering target material for forming a soft magnetic film and a method for manufacturing the same.
近年、高度情報化社会により磁気記録の高密度化が強く望まれている。この高密度化を実現する技術として、従来の面内磁気記録方式に代わり垂直磁気記録方式が実用化されている。 In recent years, high recording density has been strongly demanded by an advanced information society. As a technique for realizing this high density, a perpendicular magnetic recording system has been put into practical use instead of the conventional in-plane magnetic recording system.
垂直磁気記録方式とは、磁気記録層の磁化容易軸を媒体面に対して垂直に向けて記録するものであり、記録密度が高いほど反磁界が減少するため、記録再生特性の低下が少ない高記録密度化に適した方式である。垂直磁気記録媒体は、基板／軟磁性裏打ち層／Ｒｕ中間層／ＣｏＰｔＣｒ−ＳｉＯ２磁性層／保護層からなる多層構造が一般的である（例えば、非特許文献１参照）。 Perpendicular magnetic recording is a method in which the easy axis of magnetization of a magnetic recording layer is recorded perpendicularly to the medium surface, and the higher the recording density, the less the demagnetizing field. This method is suitable for increasing the recording density. A perpendicular magnetic recording medium generally has a multilayer structure including a substrate / soft magnetic backing layer / Ru intermediate layer / CoPtCr—SiO 2 magnetic layer / protective layer (see, for example, Non-Patent Document 1).
垂直記録媒体の軟磁性裏打ち層には優れた軟磁気特性が要求されることから、アモルファス軟磁性合金が採用されている。代表的な軟磁性裏打ち層用アモルファス合金として、Ｃｏ−Ｔａ−Ｚｒ合金膜（例えば、特許文献１参照）やＣｏ−Ｚｒ−Ｎｂ合金膜（例えば、非特許文献２参照）などが既に実用化されている。しかしながら、Ｃｏ−Ｔａ−Ｚｒ合金膜やＣｏ−Ｚｒ−Ｎｂ合金膜において、Ｔａ、Ｚｒ、Ｎｂの量が少ない場合には耐食性が低くなり、Ｔａ、Ｚｒ、Ｎｂの量が多い場合には飽和磁束密度が低くなる問題が指摘されている。そこで上記合金膜の代替候補として、飽和磁束密度と耐食性がともに高く、軟磁気特性に優れたＣｏ−Ｆｅ系合金膜が提案されている（例えば、特許文献２参照）。 An amorphous soft magnetic alloy is used because the soft magnetic backing layer of the perpendicular recording medium is required to have excellent soft magnetic characteristics. Co-Ta-Zr alloy films (for example, see Patent Document 1) and Co-Zr-Nb alloy films (for example, see Non-Patent Document 2) have already been put to practical use as typical amorphous alloys for soft magnetic backing layers. ing. However, in a Co—Ta—Zr alloy film or a Co—Zr—Nb alloy film, the corrosion resistance is low when the amount of Ta, Zr, Nb is small, and the saturation magnetic flux is high when the amount of Ta, Zr, Nb is large. The problem of low density has been pointed out. Accordingly, a Co—Fe-based alloy film having high saturation magnetic flux density and corrosion resistance and excellent soft magnetic properties has been proposed as an alternative candidate for the alloy film (see, for example, Patent Document 2).
一般的に、軟磁性裏打ち層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。マグネトロンスパッタリング法とは、ターゲット材と呼ばれる母材の背面に永久磁石を配置し、ターゲット材の表面に磁束を漏洩させて、漏洩磁束領域にプラズマを収束し、高速成膜を可能とする方法である。
しかしながら、マグネトロンスパッタリング法では、プラズマが収束する部分が集中的に侵食されるため、ごく一部しか消費されないままターゲット材を交換することになる。特に、Ｃｏ−Ｆｅ系合金のような強磁性体からなるターゲット材では、ターゲット材の背面に設置した磁石から発生する磁束の大半がターゲット材内部に侵入し、ターゲット材の表面には僅かな磁束しか発生しないため、局部的に深く消耗し、ターゲット材の寿命が極端に短くなるという問題がある。とりわけ、膜厚が１５０〜２００ｎｍと極端に厚い前記垂直磁気記録媒体の軟磁性裏打ち層の形成に際しては、ターゲット材寿命が極端に短いことは深刻な問題となっており、ターゲット材の交換頻度を減らすために、出来る限りターゲット材の厚さを厚く設定しつつ十分な漏洩磁束を得るという矛盾した要求を満たさなければならない。
In general, a magnetron sputtering method is used to form a soft magnetic backing layer. The magnetron sputtering method is a method in which a permanent magnet is placed on the back of a base material called a target material, magnetic flux is leaked to the surface of the target material, plasma is focused on the leakage magnetic flux region, and high-speed film formation is possible. is there.
However, in the magnetron sputtering method, since the portion where the plasma converges is eroded intensively, the target material is replaced while only a small portion is consumed. In particular, in a target material made of a ferromagnetic material such as a Co—Fe-based alloy, most of the magnetic flux generated from a magnet installed on the back surface of the target material penetrates into the target material, and a slight amount of magnetic flux enters the surface of the target material. However, since it occurs only locally, there is a problem that it is locally consumed and the life of the target material becomes extremely short. In particular, in the formation of the soft magnetic backing layer of the perpendicular magnetic recording medium having an extremely thick film thickness of 150 to 200 nm, it is a serious problem that the target material life is extremely short. In order to reduce, the contradictory requirement of obtaining sufficient leakage flux while setting the thickness of the target material as thick as possible must be satisfied.
マグネトロンスパッタリング法ではターゲット材の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プラズマを収束させるのに必要な漏洩磁束を得ることが難しくなる。そこで、十分な漏洩磁束を得るために、ターゲット材自身の透磁率を極力低減することが望まれている。
前記Ｃｏ−Ｆｅ系合金ターゲット材は、一般的に溶解鋳造法で製造されているが、ターゲット材の透磁率が高く、十分な漏洩磁束が得られない問題が指摘されていた。
本発明の目的は、強い漏洩磁束が得られる透磁率が低く使用効率が高いＣｏ−Ｆｅ系合金ターゲット材およびその製造方法を提供することである。
The Co—Fe-based alloy target material is generally manufactured by a melt casting method, but it has been pointed out that the target material has a high magnetic permeability and a sufficient leakage magnetic flux cannot be obtained.
An object of the present invention is to provide a Co—Fe-based alloy target material having a low magnetic permeability and a high use efficiency that provides a strong leakage magnetic flux, and a method for producing the same.
本発明者は、Ｃｏ−Ｆｅ系合金スパッタリングターゲット材の透磁率を低減するために種々の検討を行った結果、Ｃｏ−Ｆｅ系合金スパッタリングターゲット材の組織をＨＣＰ−Ｃｏからなる相とＦｅ２Ｍの非磁性ラーベス相金属間化合物が存在するＦｅを主体とする合金相とからなる組織とすることにより、ターゲット材の透磁率を低減でき、強い漏洩磁束が得られることを見出し本発明に到達した。
すなわち、本発明は、原子比における組成式が（ＣｏＸ−Ｆｅ１００−Ｘ）１００−Ｙ−ＭＹ、２０≦Ｘ≦７０、４≦Ｙ≦２５で表され、前記組成式のＭ元素がＮｂおよび／またはＴａであるスパッタリングターゲット材であって、該スパッタリングターゲット材のミクロ組織がＨＣＰ−Ｃｏからなる相とＦｅを主体とする合金相とからなる焼結組織を有し、前記Ｆｅを主体とする合金相中にＦｅ２Ｍの非磁性ラーベス相金属間化合物が存在することを特徴とするＣｏ−Ｆｅ系合金スパッタリングターゲット材である。
As a result of various studies to reduce the magnetic permeability of the Co—Fe based alloy sputtering target material, the present inventor has found that the structure of the Co—Fe based alloy sputtering target material has a phase composed of HCP—Co and Fe 2 M. It has been found that the magnetic permeability of the target material can be reduced and a strong leakage magnetic flux can be obtained by forming a structure composed of an alloy phase mainly composed of Fe in which the nonmagnetic Laves phase intermetallic compound exists. .
That is, the present invention provides a composition formula in atomic ratio is represented by (Co X -Fe 100-X) 100-Y -M Y, 20 ≦ X ≦ 70,4 ≦ Y ≦ 25, M elements of the composition formula A sputtering target material that is Nb and / or Ta, wherein the microstructure of the sputtering target material has a sintered structure composed of a phase composed of HCP-Co and an alloy phase mainly composed of Fe, and is mainly composed of the Fe And a nonmagnetic Laves phase intermetallic compound of Fe 2 M exists in the alloy phase.
前記ＨＣＰ−Ｃｏからなる相およびＦｅを主体とする合金相の平均粒径が２００μｍ以下であることが好ましい。 The average particle size of the HCP-Co phase and the alloy phase mainly composed of Fe is preferably 200 μm or less.
前記Ｃｏ−Ｆｅ系合金スパッタリングターゲット材は、Ｃｏ粉末と、ＦｅおよびＭ元素を合金化処理した合金粉末とを混合した混合粉末を加圧焼結することにより作製が可能となる。
また、前記合金粉末は、Ｆｅ、ＣｏおよびＭ元素を合金化処理したものでもよい。
また、前記合金化処理は、合金溶湯の急冷凝固処理であることが好ましい。
The Co—Fe based alloy sputtering target material can be manufactured by pressure sintering a mixed powder obtained by mixing Co powder and alloy powder obtained by alloying Fe and M elements.
The alloy powder may be one obtained by alloying Fe, Co and M elements.
The alloying treatment is preferably a rapid solidification treatment of a molten alloy.
本発明は、安定したマグネトロンスパッタリングが行える軟磁性膜形成用のＣｏ−Ｆｅ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Ｃｏ−Ｆｅ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。 INDUSTRIAL APPLICABILITY The present invention can provide a Co-Fe alloy target material for forming a soft magnetic film capable of stable magnetron sputtering, and an industrial product that requires a Co-Fe alloy soft magnetic film such as a perpendicular magnetic recording medium. This is an extremely effective technique for manufacturing.
上述したように、本発明の最も重要な特徴は、原子比における組成式が（ＣｏＸ−Ｆｅ１００−Ｘ）１００−Ｙ−ＭＹ、２０≦Ｘ≦７０、４≦Ｙ≦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Ｃｏ−Ｆｅ系合金ターゲット材の透磁率を低減するために、そのミクロ組織を制御した点にある。すなわち、ターゲット材のミクロ組織において、ＨＣＰ−Ｃｏ相とＦｅを主体とする合金相とからなる焼結組織を有し、Ｆｅを主体とする合金相にＦｅ２Ｍの非磁性ラーベス相金属間化合物を存在させるように制御する点にある。 As described above, the most important feature of the present invention, a composition formula in atomic ratio is represented by (Co X -Fe 100-X) 100-Y -M Y, 20 ≦ X ≦ 70,4 ≦ Y ≦ 25 In order to reduce the magnetic permeability of the Co—Fe based alloy target material in which the M element of the composition formula is Nb and / or Ta, the microstructure is controlled. That is, the microstructure of the target material has a sintered structure composed of an HCP-Co phase and an alloy phase mainly composed of Fe, and the Fe 2 M nonmagnetic Laves phase intermetallic compound is formed in the alloy phase mainly composed of Fe. It is in the point to control to exist.
本発明のＣｏ−Ｆｅ系合金スパッタリングターゲット材の組織をＨＣＰ−Ｃｏからなる相とＦｅを主体とする合金相とからなる焼結組織を有し、Ｆｅを主体とする合金相に非磁性ラーベス相金属間化合物を存在させるように制御する理由を以下に説明する。
一般的にＣｏ合金あるいはＦｅ合金のターゲット材は、溶解鋳造法で作製されている。溶解鋳造法で透磁率を低減するためには、溶解鋳造後に熱処理や圧延等を行い、内部局所応力を増大させ磁壁の移動を阻止する方法が採られている。
The structure of the Co—Fe based alloy sputtering target material of the present invention has a sintered structure composed of a phase composed of HCP—Co and an alloy phase mainly composed of Fe, and the alloy phase mainly composed of Fe includes a nonmagnetic Laves phase. The reason for controlling the intermetallic compound to be present will be described below.
In general, a target material of Co alloy or Fe alloy is produced by a melt casting method. In order to reduce the magnetic permeability by the melt casting method, a method is adopted in which heat treatment, rolling, or the like is performed after melt casting to increase the internal local stress and prevent the domain wall from moving.
本発明者は、Ｃｏ−Ｆｅ系合金ターゲットの漏洩磁束向上のため、上述の手法の適用を試みたが、透磁率を十分に低減することが出来ず、強い漏洩磁束を得ることが出来なかった。
そこで、さらに検討を行った結果、Ｃｏに対してはターゲット材の他の構成元素と合金化させずに純Ｃｏ粉末とし、一方、Ｆｅに対しては少なくともＦｅと非磁性のラーベス相金属間化合物を形成する元素を適量添加し合金化した合金粉とし、これらを混合して焼結した組織とすることで、従来では到達し得なかった極めて低い透磁率を持ったターゲットとなることを見出し、本発明に到達したのである。
The present inventor tried to apply the above-described method to improve the leakage flux of the Co—Fe based alloy target, but could not sufficiently reduce the magnetic permeability and could not obtain a strong leakage flux. .
Therefore, as a result of further investigation, Co was made into pure Co powder without being alloyed with other constituent elements of the target material, while at least Fe and nonmagnetic Laves phase intermetallic compound were used for Fe. By adding an appropriate amount of elements to form an alloyed alloy powder, and by mixing and sintering these powders, it has been found that it becomes a target with extremely low magnetic permeability that could not be achieved conventionally, The present invention has been reached.
本発明は、上述した従来の方法とは全く異なる手法を採用して低い透磁率を持ったターゲットが得られたものであり、その低透磁率化の効果は以下のように考えられる。
一般的に、多結晶体の透磁率には磁気モーメントと磁気異方性が大きく影響し、「磁気モーメント大、磁気異方性小」の場合は高透磁率になり、「磁気モーメント小、磁気異方性大」の場合は低透磁率になることが知られている。
他方、ＣｏとＦｅとを含む合金相の結晶構造には、ＨＣＰ（六方最密格子）、ＦＣＣ（面心立方格子）、ＢＣＣ（体心立方格子）があり、これらの中で最も結晶磁気異方性が大きいのはＨＣＰ相である。また、純Ｃｏは約４２２℃付近の結晶構造変態点を境として変態点以下ではＨＣＰ、変態点以上ではＦＣＣとなることが知られているが、Ｃｏに他の元素を添加して合金化すると室温領域でも結晶磁気異方性が小さいＦＣＣやＢＣＣとなる場合がある。
In the present invention, a target having a low magnetic permeability is obtained by adopting a method completely different from the conventional method described above, and the effect of reducing the magnetic permeability is considered as follows.
In general, the magnetic moment and magnetic anisotropy have a large effect on the magnetic permeability of polycrystals. When the magnetic moment is large and the magnetic anisotropy is small, the magnetic permeability is high. In the case of “high anisotropy”, it is known that the magnetic permeability is low.
On the other hand, the crystal structure of the alloy phase containing Co and Fe includes HCP (hexagonal close-packed lattice), FCC (face-centered cubic lattice), and BCC (body-centered cubic lattice). It is the HCP phase that is highly anisotropic. Pure Co is known to be HCP below the transformation point at the crystal structure transformation point near about 422 ° C. and FCC above the transformation point, but when alloyed by adding other elements to Co Even in the room temperature region, there may be FCC or BCC with small crystal magnetic anisotropy.
本発明では、Ｃｏ−Ｆｅ系合金ターゲット材のミクロ組織を、Ｃｏを他のターゲット材構成元素と合金化させずＨＣＰ−Ｃｏ相として存在させることで磁気異方性を高めている。さらにＣｏとＦｅとの対比で、より磁気モーメントが大きいＦｅを主体とする合金相側に、Ｆｅ２Ｍの非磁性ラーベス相金属間化合物を存在させることで本来強磁性であるＦｅの磁気モーメントをも大幅に低減させることが可能となる。以上の相乗効果によって、ターゲット材全体の磁気モーメントを大幅に低減すると同時に磁気異方性を高めることが可能となり、低い透磁率、強い漏洩磁束を実現できたものと考えられる。
なお、本発明においてＨＣＰ−Ｃｏからなる相とは、不可避的不純物と周囲の拡散層を除いてＣｏからなり結晶構造はＨＣＰからなる相のことである。また、Ｆｅ２Ｍの非磁性ラーベス相金属間化合物とは、化学式がＦｅ２Ｍであらわされるラーベス相からなり、ターゲット材の使用温度領域である室温以上で強磁性を示さない金属間化合物のことである。このような性質をもったＦｅ２Ｍとしては、例えば、常磁性であるＦｅ２Ｎｂ、Ｆｅ２Ｔａを例示できる。なお、ＨＣＰ−Ｃｏ相の結晶構造と非磁性ラーベス相金属間化合物の存在は、例えば、Ｘ線回折法によって判定できる。
また、本発明においてＦｅを主体とする合金相とは、原子比で５０％以上のＦｅとＭ元素から構成される合金相、あるいは原子比で５０％以上のＦｅとＭ元素とＣｏから構成される合金相である。
In the present invention, the magnetic anisotropy is enhanced by allowing the microstructure of the Co—Fe-based alloy target material to exist as an HCP—Co phase without causing Co to be alloyed with other target material constituent elements. In addition, Fe 2 M nonmagnetic Laves phase intermetallic compound is present on the alloy phase side mainly composed of Fe having a larger magnetic moment in comparison with Co and Fe. Can be greatly reduced. Due to the above synergistic effect, it is considered that the magnetic moment of the entire target material can be greatly reduced and the magnetic anisotropy can be increased at the same time, and a low magnetic permeability and a strong leakage magnetic flux can be realized.
In the present invention, the phase composed of HCP-Co refers to a phase composed of Co except for inevitable impurities and surrounding diffusion layers and having a crystal structure composed of HCP. The nonmagnetic Laves phase intermetallic compound of Fe 2 M is an intermetallic compound that consists of a Laves phase represented by the chemical formula Fe 2 M and does not exhibit ferromagnetism at room temperature or higher, which is the operating temperature range of the target material. It is. Examples of Fe 2 M having such properties include paramagnetic Fe 2 Nb and Fe 2 Ta. Note that the crystal structure of the HCP-Co phase and the presence of the nonmagnetic Laves phase intermetallic compound can be determined by, for example, an X-ray diffraction method.
In the present invention, the alloy phase mainly composed of Fe is composed of an alloy phase composed of Fe and M elements with an atomic ratio of 50% or more, or composed of Fe, M elements and Co with an atomic ratio of 50% or more. This is an alloy phase.
なお、本発明のＣｏ−Ｆｅ系合金ターゲット材のミクロ組織において、ＨＣＰ−Ｃｏ相とＦｅを主体とする合金相の比率はターゲット材の化学組成によって変化する。
例えば、Ｃｏの組成比率が低い場合、ＨＣＰ−Ｃｏからなる相とＦｅを主体とする合金相とが分散した組織となり、Ｃｏの組成比率が高い場合、ＨＣＰ−Ｃｏからなる主相に、Ｆｅを主体とする合金相が分散した組織となる。いずれの場合も上述の効果が得られることは言うまでもない。
In the microstructure of the Co—Fe based alloy target material of the present invention, the ratio of the HCP—Co phase and the alloy phase mainly composed of Fe varies depending on the chemical composition of the target material.
For example, when the composition ratio of Co is low, the phase composed of HCP-Co and the alloy phase mainly composed of Fe are dispersed. When the composition ratio of Co is high, Fe is added to the main phase composed of HCP-Co. The main alloy phase is dispersed. In any case, it goes without saying that the above-described effects can be obtained.
また、ＨＣＰ−Ｃｏからなる相とＦｅを主体とする合金相とはそれぞれスパッタリング率が異なる場合があり、粗大な部分が存在するとスパッタリング成膜時に異常放電やパーティクルなどの問題が生じる場合がある。このため、それぞれを微細に分散させることにより、安定したスパッタリングが可能となる。よって、Ｆｅを主体とする合金相とＨＣＰ−Ｃｏからなる相の平均粒径は２００μm以下とすることが好ましい。 In addition, the HCP-Co phase and the alloy phase mainly composed of Fe may have different sputtering rates. If a coarse portion exists, problems such as abnormal discharge and particles may occur during sputtering film formation. For this reason, stable sputtering becomes possible by finely dispersing each of them. Therefore, the average particle size of the alloy phase mainly composed of Fe and the phase composed of HCP-Co is preferably 200 μm or less.
また、本発明のスパッタリングターゲット材の化学組成は、原子比における組成式が（ＣｏＸ−Ｆｅ１００−Ｘ）１００−Ｙ−ＭＹ、２０≦Ｘ≦７０、４≦Ｙ≦２５で表され、前記組成式のＭ元素がＮｂおよび／またはＴａからなるものである。
ＣｏとＦｅとの組成比Ｘを２０≦Ｘ≦７０としたのは、Ｃｏ−Ｆｅ二元系合金膜において、Ｃｏ含有量を原子比で２０〜７０％にすることで高い飽和磁化を持ち軟磁気特性に優れた薄膜を生成できるためである。
Ｍ元素をＮｂおよび／またはＴａとし、その添加量Ｙを４≦Ｙ≦２５としたのは、Ｍ元素をこの範囲で添加することで、薄膜のアモルファス化を促進させる効果や耐食性を向上させる効果があるためである。Ｍ元素の添加量が４％未満であると薄膜が結晶化し、優れた軟磁気特性が得られ難く、さらに耐食性が低下するという問題が生じる。また、２５％を超えると薄膜の飽和磁束密度が低下するという問題が生じる。
他方、Ｍ元素はＦｅとの間で非磁性ラーベス相金属間化合物を形成する元素であるため、Ｍ元素の添加によりターゲット全体の磁気モーメントを低減することが可能である。よって、ターゲット材の特性においてもＭ元素の添加は効果がある。
The chemical composition of the sputtering target material of the present invention, a composition formula in atomic ratio is represented by (Co X -Fe 100-X) 100-Y -M Y, 20 ≦ X ≦ 70,4 ≦ Y ≦ 25, The M element in the composition formula is composed of Nb and / or Ta.
The reason why the composition ratio X of Co and Fe is set to 20 ≦ X ≦ 70 is that in a Co—Fe binary alloy film, the Co content is set to 20 to 70% by atomic ratio so that high saturation magnetization and softness are achieved. This is because a thin film having excellent magnetic properties can be produced.
The reason why the element M is Nb and / or Ta and the addition amount Y is 4 ≦ Y ≦ 25 is that the addition of the element M in this range promotes the effect of promoting the amorphization of the thin film and the corrosion resistance. Because there is. When the amount of M element added is less than 4%, the thin film crystallizes, and it is difficult to obtain excellent soft magnetic properties, and further, the corrosion resistance is lowered. Moreover, when it exceeds 25%, the problem that the saturation magnetic flux density of a thin film falls arises.
On the other hand, since the M element is an element that forms a nonmagnetic Laves phase intermetallic compound with Fe, the addition of the M element can reduce the magnetic moment of the entire target. Therefore, addition of M element is also effective in the characteristics of the target material.
上述の本発明のターゲット材は、所定の組成となるよう調整したＣｏ粉末と、ＦｅとＭ元素を合金化処理した合金粉末とを混合した混合粉末を加圧焼結することで得ることができる。Ｃｏ粉末は上述のように室温領域ではＨＣＰであるが、ＦｅやＭ元素との合金化が進むとＦＣＣやＢＣＣとなる場合があるため、純Ｃｏ粉末のまま他の元素と混合して加圧焼結することで、焼結後のターゲット材の組織にＣｏ相をＨＣＰとして残存させることが重要である。また、ＦｅとＭ元素を合金化処理してＦｅ２Ｍの非磁性ラーベス相金属間化合物が存在する合金粉末とし、この粉末を焼結することで焼結体中にＦｅ２Ｍの非磁性ラーベス相金属間化合物が存在するＦｅを主体とする合金相を効率良く生成することができる。 The target material of the present invention described above can be obtained by pressure sintering a mixed powder obtained by mixing Co powder adjusted to have a predetermined composition and alloy powder obtained by alloying Fe and M elements. . As described above, Co powder is HCP in the room temperature region, but when alloying with Fe or M element proceeds, it may become FCC or BCC. Therefore, pure Co powder is mixed with other elements and pressurized. It is important to leave the Co phase as HCP in the structure of the target material after sintering by sintering. Further, Fe and M elements and the alloy powder present nonmagnetic laves phase intermetallic compound of Fe 2 M by alloying, nonmagnetic laves of Fe 2 M in sintered body by sintering the powder An alloy phase mainly composed of Fe in which a phase intermetallic compound exists can be efficiently generated.
また、Ｆｅ、Ｍ元素からなる合金の液相温度が高く、合金粉末の製造が困難な場合は、Ｃｏの一部を含め、Ｆｅ、Ｃｏ、Ｍ元素を合金化処理したものでもよい。これは、Ｃｏを合金粉末に含有させることによって液相温度を低下させることが可能となるためである。
なお、この場合でも、ターゲット中のＨＣＰ−Ｃｏ相の比率を極力多くするため、Ｆｅを主体とする合金粉末に含まれるＣｏ量は３０原子％以下であることが望ましい。
Moreover, when the liquid phase temperature of the alloy which consists of Fe and M elements is high and manufacture of an alloy powder is difficult, what alloyed Fe, Co, and M element including part of Co may be used. This is because the liquidus temperature can be lowered by including Co in the alloy powder.
Even in this case, in order to increase the ratio of the HCP-Co phase in the target as much as possible, the amount of Co contained in the alloy powder mainly composed of Fe is desirably 30 atomic% or less.
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、熱間押し出しなどの方法を適用することができる。中でも熱間静水圧プレスは加圧圧力が高く、最高温度を低く抑えて拡散層の生成を抑制しても、緻密な焼結体が得られるため、特に好ましい。
なお、加圧焼結時の最高温度は８００℃以上、１２００℃以下の温度に設定することが好ましい。この理由は焼結温度が８００℃を下回ると、緻密な焼結体が得られ難く、１２００℃を超えると焼結中に合金粉末が溶解する場合があるためである。さらに、最高温度が高過ぎると、粉末粒子同士の拡散が進み、ＨＣＰ−Ｃｏ相を十分に残存させづらくなったり、ＨＣＰ−Ｃｏ相とＦｅを主体とする合金相の相間にＣｏ−Ｆｅ拡散相が形成され、磁気モーメントが増加するため、さらに好ましくは９００℃から１１００℃の範囲に設定すると良い。
また、加圧焼結時の最高圧力は２０ＭＰａ以上に設定することが好ましい。その理由は最高圧力が２０ＭＰａを下回ると緻密な焼結体が得られないためである。
In addition, as a pressure sintering method for the mixed powder, methods such as hot pressing, hot isostatic pressing, energizing pressure sintering, and hot extrusion can be applied. Among them, the hot isostatic press is particularly preferable because the pressurization pressure is high and a dense sintered body can be obtained even if the maximum temperature is kept low to suppress the formation of the diffusion layer.
The maximum temperature during pressure sintering is preferably set to a temperature of 800 ° C. or higher and 1200 ° C. or lower. This is because when the sintering temperature is below 800 ° C., a dense sintered body is difficult to obtain, and when it exceeds 1200 ° C., the alloy powder may be dissolved during sintering. Furthermore, if the maximum temperature is too high, the diffusion between the powder particles proceeds, making it difficult to sufficiently leave the HCP-Co phase, or the Co-Fe diffusion phase between the HCP-Co phase and the alloy phase mainly composed of Fe. Is formed, and the magnetic moment is increased. Therefore, the temperature is more preferably set in the range of 900 ° C. to 1100 ° C.
The maximum pressure during pressure sintering is preferably set to 20 MPa or more. The reason is that if the maximum pressure is less than 20 MPa, a dense sintered body cannot be obtained.
本発明の合金化処理としては、微細な組織を得ることができる急冷凝固処理を用いることが好ましい。急冷凝固処理方法としては、不純物の混入が少なく、充填率が高く焼結に適した球状粉末が得られるガスアトマイズ法が好ましい。また、酸化を抑制するには、アトマイズガスとして不活性ガスであるアルゴンガスもしくは窒素ガスを用いると良い。 As the alloying treatment of the present invention, it is preferable to use a rapid solidification treatment capable of obtaining a fine structure. As the rapid solidification treatment method, a gas atomization method is preferred, in which a small amount of impurities is mixed and a spherical powder having a high filling rate and suitable for sintering is obtained. Moreover, in order to suppress oxidation, it is good to use argon gas or nitrogen gas which is inert gas as atomizing gas.
以下の実施例で本発明をさらに詳しく説明する。
以下の実施例では合金組成は全てＦｅ−３０．８Ｃｏ−１２Ｔａ（原子％）とした。表１に示す各粉末をＡｒガスを用いたガスアトマイズ法によって作製した後、得られたアトマイズ粉末を６０メッシュのふるいで分級した。それぞれのアトマイズ粉末を表１の組み合わせで混合粉末の組成がＦｅ−３０．８Ｃｏ−１２Ｔａ（原子％）となるように、秤量し、混合した後、軟鋼カプセルに充填して脱気封止した。次いで、圧力１２２ＭＰａ、温度９５０℃、保持時間１時間の条件で熱間静水圧プレス法により焼結体を作製し、機械加工により直径１９０ｍｍ、厚さ５ｍｍのＣｏ−Ｆｅ系合金ターゲット材を得た。
また、溶解鋳造により同一組成のインゴットを作製した後、機械加工を施して直径１９０ｍｍ、厚さ５ｍｍのＣｏ−Ｆｅ系合金ターゲット材を得た。
The following examples further illustrate the present invention.
In the following examples, the alloy composition was all Fe-30.8Co-12Ta (atomic%). Each powder shown in Table 1 was produced by a gas atomizing method using Ar gas, and then the obtained atomized powder was classified with a 60 mesh sieve. Each atomized powder was weighed so that the composition of the mixed powder in the combination shown in Table 1 was Fe-30.8Co-12Ta (atomic%), mixed, then filled into a mild steel capsule and deaerated and sealed. Next, a sintered body was produced by hot isostatic pressing under conditions of a pressure of 122 MPa, a temperature of 950 ° C., and a holding time of 1 hour, and a Co—Fe based alloy target material having a diameter of 190 mm and a thickness of 5 mm was obtained by machining. .
Moreover, after producing the ingot of the same composition by melt casting, it machined and obtained the Co-Fe type-alloy target material of diameter 190mm and thickness 5mm.
上記試料１と試料２のターゲット材の端材から１０ｍｍ×１０ｍｍの試験片を２個採取しバフ研磨を施した後、一つの試験片はＡｒガスを用いたフラットミリングを施し、走査型電子顕微鏡および光学顕微鏡を用いてミクロ組織観察を行った。もう一つの試験片はＸ線回折測定による相同定を行った。なお、Ｘ線回折測定には（株）リガク製Ｘ線回折装置ＲＩＮＴ２５００Ｖを使用し、線源にＣｏを用いて測定を行った。 After collecting two test pieces of 10 mm × 10 mm from the end materials of the target materials of Sample 1 and Sample 2 and buffing them, one test piece was subjected to flat milling using Ar gas, and a scanning electron microscope The microstructure was observed using an optical microscope. Another test piece was subjected to phase identification by X-ray diffraction measurement. For X-ray diffraction measurement, Rigaku X-ray diffractometer RINT2500V was used, and Co was used as the radiation source.
図１に試料１のミクロ組織の走査型電子顕微鏡像を、図２に試料１のＸ線回折パターンを示す。図１から試料１（本発明例）のミクロ組織は、濃灰色のＣｏ相と薄灰色のＦｅ合金相からなることがわかる。また、図２から試料１（本発明例）のＸ線回折パターンは、ＨＣＰ−Ｃｏ相、αＦｅ相、その他Ｆｅ２Ｔａ金属間化合物に近い相をそれぞれ反映したピークを呈していることから、ミクロ組織中のＣｏ相はＨＣＰ−Ｃｏ相であり、Ｆｅ合金相は、αＦｅ相、非磁性ラーベス相金属間化合物であるＦｅ２Ｔａ金属間化合物相からなると同定できる。
また、図３に試料２のミクロ組織の走査型電子顕微鏡像を、図４に試料２のＸ線回折パターンを示す。図３から試料２（比較例）のミクロ組織は典型的な溶解鋳造組織を示し、薄灰色の初晶部と濃灰色の共晶部からなることがわかる。さらに、図４に示す試料２（比較例）のＸ線回折パターンは、α（Ｃｏ−Ｆｅ）相とその他Ｆｅ２Ｔａ金属間化合物に近い相をそれぞれ反映したピークを呈していることから、ミクロ組織の初晶部はα（Ｃｏ−Ｆｅ）相であり、同じく共晶部はα（Ｃｏ−Ｆｅ）相と金属間化合物相とからなると同定できる。なお、α（Ｃｏ−Ｆｅ）は主にＣｏとＦｅからなる固溶体でＢＣＣ構造の相である。
FIG. 1 shows a scanning electron microscope image of the microstructure of sample 1, and FIG. 2 shows an X-ray diffraction pattern of sample 1. It can be seen from FIG. 1 that the microstructure of sample 1 (example of the present invention) consists of a dark gray Co phase and a light gray Fe alloy phase. In addition, the X-ray diffraction pattern of Sample 1 (Example of the present invention) from FIG. 2 exhibits peaks reflecting HCP-Co phase, αFe phase, and other phases close to Fe 2 Ta intermetallic compound, respectively. The Co phase in the structure is an HCP-Co phase, and the Fe alloy phase can be identified as being composed of an αFe phase and a Fe 2 Ta intermetallic compound phase which is a nonmagnetic Laves phase intermetallic compound.
3 shows a scanning electron microscope image of the microstructure of sample 2, and FIG. 4 shows an X-ray diffraction pattern of sample 2. FIG. 3 shows that the microstructure of Sample 2 (Comparative Example) shows a typical melt-cast structure, and is composed of a light gray primary crystal part and a dark gray eutectic part. Furthermore, since the X-ray diffraction pattern of Sample 2 (Comparative Example) shown in FIG. 4 exhibits peaks reflecting the α (Co—Fe) phase and other phases close to the Fe 2 Ta intermetallic compound, respectively. The primary crystal part of the structure is an α (Co—Fe) phase, and similarly, the eutectic part can be identified as being composed of an α (Co—Fe) phase and an intermetallic compound phase. Α (Co—Fe) is a solid solution mainly composed of Co and Fe and is a phase of the BCC structure.
また、試料１（本発明例）の４００倍の光学顕微鏡像において、ＨＣＰ−Ｃｏからなる相およびＦｅを主体とする合金相のそれぞれの境界を粒界とみなし、直線交差線分法により試料１の平均粒径を求めたところ３２μｍであった。 Further, in the optical microscope image at 400 times that of sample 1 (example of the present invention), each boundary of the phase consisting of HCP-Co and the alloy phase mainly composed of Fe is regarded as a grain boundary, and sample 1 is obtained by the linear crossing line segmentation method. The average particle size was 32 μm.
次に、作製した各ターゲット材の端材から長さ３０ｍｍ、幅１０ｍｍ、厚さ５ｍｍの試験片を採取した。さらに東英工業（株）製直流磁気特性測定装置ＴＲＦ５Ａを使用してこれらの試験片の磁化曲線を測定した。得られた磁化曲線から最大透磁率を求め、表２に示した。表２から、試料１の本発明例のターゲット材では、比較例に比べて格段に低い最大透磁率を示していることがわかる。 Next, a test piece having a length of 30 mm, a width of 10 mm, and a thickness of 5 mm was collected from the end material of each of the prepared target materials. Furthermore, the magnetization curves of these test pieces were measured using a DC magnetic property measuring apparatus TRF5A manufactured by Toei Industry Co., Ltd. The maximum magnetic permeability was determined from the obtained magnetization curve and shown in Table 2. From Table 2, it can be seen that the target material of the present invention example of Sample 1 has a significantly lower maximum magnetic permeability than the comparative example.
次に、作製した各ターゲット材の漏洩磁束（Ｐａｓｓ−Ｔｈｒｏｕｇｈ−Ｆｌｕｘ：以下、ＰＴＦと記す）を測定し表３に示した。ＰＴＦ測定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する方法で、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方法である。実際の測定はＡＳＴＭ Ｆ１７６１−００（Ｓｔａｎｄａｒｄ Ｔｅｓｔ Ｍｅｔｈｏｄ ｆｏｒ Ｐａｓｓ Ｔｈｒｏｕｇｈ Ｆｌｕｘ ｏｆ Ｃｉｒｃｕｌａｒ Ｍａｇｎｅｔｉｃ Ｓｐｕｔｔｅｒｉｎｇ Ｔａｒｇｅｔｓ）に基づいて行い、ＰＴＦは次式より求めた。
（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） （％）
Next, the magnetic flux leakage (Pass-Through-Flux: hereinafter referred to as PTF) of each of the prepared target materials was measured and shown in Table 3. The PTF measurement is a method in which a permanent magnet is disposed on the back surface of the target material and the magnetic flux leaking to the surface of the target material is measured, and the leakage magnetic flux close to the magnetron sputtering apparatus can be measured quantitatively. Actual measurement was performed based on ASTM F1761-00 (Standard Test Method for Pass Through Flux of Circular Magnetic Sputtering Targets), and PTF was calculated from the following equation.
(PTF) = 100 × (Magnetic strength with target material placed) ÷ (Magnetic flux strength with no target material placed) (%)
ＰＴＦの測定結果を示した表３より、試料１（本発明例）のＰＴＦも、高い値を示しており、上述した最大透磁率の測定結果と対応し、非常に強い漏洩磁束が得られることがわかる。
以上より、ミクロ組織がＨＣＰ−Ｃｏからなる相とＦｅ２Ｍ非磁性ラーベス相金属間化合物が存在するＦｅを主体とする合金相とからなる本発明のＣｏ−Ｆｅ系合金ターゲット材は、他の製法のターゲット材に比べ著しく低い透磁率を有し、強い漏洩磁束が得られることが確認できた。
From Table 3 showing the measurement result of PTF, the PTF of sample 1 (example of the present invention) also shows a high value, corresponding to the measurement result of the maximum magnetic permeability described above, and obtaining a very strong leakage magnetic flux. I understand.
From the above, the Co—Fe-based alloy target material of the present invention comprising a phase whose microstructure is composed of HCP—Co and an alloy phase mainly composed of Fe in which a Fe 2 M nonmagnetic Laves phase intermetallic compound exists is It was confirmed that a strong magnetic flux leakage was obtained with a remarkably low permeability compared to the target material of the manufacturing method.
本発明では、Ｃｏ−Ｆｅ系合金スパッタリングターゲット材のミクロ組織をＨＣＰ−Ｃｏ相とＦｅ２Ｍの非磁性ラーベス相金属間化合物が存在するＦｅを主体とする相とからなる焼結組織とすることにより、最大透磁率が低く、漏洩磁束が強いＣｏ−Ｆｅ系合金スパッタリングターゲット材が得られる。この結果、軟磁性膜形成に際して、安定したマグネトロンスパッタリングを行うことが可能となる。 In the present invention, the microstructure of the Co—Fe-based alloy sputtering target material is a sintered structure composed of an HCP-Co phase and a phase mainly composed of Fe in which a nonmagnetic Laves phase intermetallic compound of Fe 2 M exists. Thus, a Co—Fe based alloy sputtering target material having a low maximum magnetic permeability and a strong leakage magnetic flux can be obtained. As a result, stable magnetron sputtering can be performed when forming the soft magnetic film.
Claims (5)
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| JP2010024548A (en) * | 2008-06-17 | 2010-02-04 | Hitachi Metals Ltd | Fe-Co-BASED ALLOY SPUTTERING TARGET MATERIAL FOR FORMING SOFT MAGNETIC FILM |
| JP2010059540A (en) * | 2008-08-04 | 2010-03-18 | Hitachi Metals Ltd | METHOD FOR PRODUCING Co-Fe BASED ALLOY SPUTTERING TARGET MATERIAL AND Co-Fe BASED ALLOY SPUTTERING TARGET MATERIAL |
| JP2010280964A (en) * | 2009-06-05 | 2010-12-16 | Solar Applied Materials Technology Corp | Cobalt-iron alloy sputtering target material having high magnetic field transmittance |
| WO2022041741A1 (en) * | 2020-08-31 | 2022-03-03 | 宁波江丰电子材料股份有限公司 | Iron-cobalt-tantalum alloy powder preparation method, iron-cobalt-tantalum alloy powder and use thereof |
| CN116393688A (en) * | 2023-01-13 | 2023-07-07 | 湖南恒基粉末科技有限责任公司 | A kind of soft magnetic alloy powder and its preparation method and application |
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| CN116393688A (en) * | 2023-01-13 | 2023-07-07 | 湖南恒基粉末科技有限责任公司 | A kind of soft magnetic alloy powder and its preparation method and application |
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