JP2009155722A - Ni-W BASED SINTERED TARGET MATERIAL - Google Patents
Ni-W BASED SINTERED TARGET MATERIAL Download PDFInfo
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Abstract
Description
本発明は、垂直磁気記録媒体のNi合金中間層を形成するためのNi−W系焼結ターゲット材に関するものである。 The present invention relates to a Ni—W sintered target material for forming a Ni alloy intermediate layer of a perpendicular 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、現在広く世の中で使用されている面内磁気記録方式の磁気記録媒体では、高記録密度化を実現しようとすると、記録ビットが微細化し、記録ヘッドで記録できないほどの高保磁力が要求される。そこで、これらの問題を解決し、記録密度を向上させる手段として垂直磁気記録方式が検討されている。 In recent years, the progress of magnetic recording technology has been remarkable, and the recording density of magnetic recording media has been increased to increase the capacity of drives. However, in the magnetic recording medium of the in-plane magnetic recording system that is currently widely used in the world, when trying to achieve a high recording density, the recording bit becomes finer and a high coercive force that cannot be recorded by the recording head is required. . Therefore, a perpendicular magnetic recording method has been studied as a means for solving these problems and improving the recording density.
垂直磁気記録方式とは、垂直磁気記録媒体の磁性膜中に媒体面に対して磁気容易軸が垂直方向に配向するように形成したものであり、記録密度を上げて行ってもビット内の反磁界が小さく、記録再生特性の低下が少ない高記録密度に適した方法である。そして、垂直磁気記録方式においては、記録感度を高めた磁気記録膜層と軟磁性膜層とを有する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中間層や下地層が成膜された記録媒体が開発されている。
そして、このような記録媒体の中間層としては、中間層上に形成される下地層や磁気記録層の配向を制御する作用が要求されており、Ni−W系などのNi合金を適用することが提案されている(例えば、特許文献1)。
As an intermediate layer of such a recording medium, an action for controlling the orientation of the underlayer or magnetic recording layer formed on the intermediate layer is required, and a Ni alloy such as a Ni—W system is applied. Has been proposed (for example, Patent Document 1).
特許文献1に記載されるNi−W系合金膜を形成するためのスパッタリング用ターゲット材は、一般的にNi−W系合金の溶解鋳造インゴットに圧延を施して作製されている。本願発明者らの検討によれば、溶解鋳造−圧延で作製されるNi−W系合金ターゲット材を使用してマグネトロンスパッタリングによって膜厚の薄い中間層を形成したところ、膜のバラツキが確認された。
本発明の目的は、上記の問題を解決し、スパッタリングによって成膜される垂直磁気記録媒体の中間層用Ni−W系合金膜のバラツキを抑制することが可能なNi−W系ターゲット材を提供することである。
The sputtering target material for forming the Ni—W alloy film described in Patent Document 1 is generally produced by rolling a Ni—W alloy melt casting ingot. According to the study by the present inventors, when a thin intermediate layer was formed by magnetron sputtering using a Ni-W alloy target material produced by melt casting-rolling, variation in the film was confirmed. .
An object of the present invention is to provide a Ni-W-based target material that can solve the above-described problems and can suppress variations in the Ni-W-based alloy film for an intermediate layer of a perpendicular magnetic recording medium formed by sputtering. It is to be.
本発明者らは、上記の問題に関して種々の検討を行った結果、Ni−W系ターゲット材の配向組織を、主成分となるNiのランダム配向に近似した配向組織に制御することで、Ni−W系合金膜のバラツキを抑制可能であることを見出し本発明に到達した。 As a result of various investigations on the above problems, the present inventors have controlled the orientation structure of the Ni—W target material to be an orientation structure that approximates the random orientation of Ni as the main component. The inventors have found that it is possible to suppress variations in the W-based alloy film, and have reached the present invention.
すなわち、本発明は、Wを3〜15原子%含み、残部Niおよび不可避的不純物からなる焼結ターゲット材であって、前記焼結ターゲット材のX線回折におけるfcc相であるNi固溶体の強度比が、0.30≦I(200)/I(111)≦0.50、0.10≦I(220)/I(111)≦0.30であるNi-W系焼結ターゲット材である。
また、さらに、好ましくは、IVa族、Va族、VIa族、VIIa族、IIIb族、IVb族から選択される1種または2種以上の添加元素を20原子%以下含むNi-W系焼結ターゲット材である。また、前記添加元素として、少なくともCrを含むことがさらに好ましい。
That is, the present invention is a sintered target material containing 3 to 15 atomic% of W, the balance being Ni and inevitable impurities, and the strength ratio of the Ni solid solution that is the fcc phase in the X-ray diffraction of the sintered target material Is a Ni—W based sintered target material satisfying 0.30 ≦ I (200) / I (111) ≦ 0.50 and 0.10 ≦ I (220) / I (111) ≦ 0.30.
Further preferably, the Ni—W-based sintering target preferably contains 20 atomic% or less of one or more additive elements selected from IVa group, Va group, VIa group, VIIa group, IIIb group, and IVb group. It is a material. Further, it is more preferable that the additive element contains at least Cr.
本発明により、安定したマグネトロンスパッタリングが行なえる垂直磁気記録媒体の中間層を成膜するためのNi−W系ターゲット材を提供でき、垂直磁気記録媒体を製造する上で極めて有効な技術となる。 The present invention can provide a Ni—W-based target material for forming an intermediate layer of a perpendicular magnetic recording medium capable of performing stable magnetron sputtering, which is an extremely effective technique for producing a perpendicular magnetic recording medium.
本発明の最も重要な特徴は、マグネトロンスパッタの安定化のために等方的組織を有するNi-W系焼結ターゲット材とすることにある。具体的には、ターゲット材の結晶組織をX線回折における強度比を0.30≦I(200)/I(111)≦0.50かつ0.10≦I(220)/I(111)≦0.30と、当該ターゲット材の主成分であるNiのランダム配向に近い配向に制御することで、マグネトロンスパッタにおける成膜の安定化が図られる。 The most important feature of the present invention is to provide a Ni—W sintered target material having an isotropic structure for stabilizing magnetron sputtering. Specifically, the intensity ratio in X-ray diffraction of the crystal structure of the target material is 0.30 ≦ I (200) / I (111) ≦ 0.50 and 0.10 ≦ I (220) / I (111) ≦ By controlling the orientation to 0.30, which is close to the random orientation of Ni, which is the main component of the target material, film formation in magnetron sputtering can be stabilized.
本発明のNi−W系ターゲット材は、面心立方構造(fcc)を維持しつつ、Niが元来有する磁性を低下させることが好ましいため、3〜15原子%のWが添加された残部Niおよび不可避的不純部からなる組成とすることが効果的である。 Since the Ni-W-based target material of the present invention preferably maintains the face-centered cubic structure (fcc) and lowers the magnetic properties inherent in Ni, the remaining Ni to which 3 to 15 atomic% W is added is added. In addition, it is effective to have a composition comprising inevitable impure parts.
スパッタリングにおいては、Ar+イオンがターゲット材表面に衝突した際、原子間に割り込み、その周囲の原子を激しく振動させる。振動はターゲット材の結晶最密方向に最も伝播されやすく、表面原子が最密方向へ放出される。そのため、スパッタリング中の原子放出はターゲット材の結晶構造に依存する。したがって、優先放出方向に対応する部分の成膜速度が高く、非優先方向に対応する部分の成膜速度が低くなる。この成膜速度の差により、多結晶構造を有するターゲット材の膜厚分布の均一性が支配される。よって、多結晶組織のターゲット材であっても、結晶粒が均一微細で、かつその結晶配向がランダムであれば、優先方位の成膜速度が相殺され、統計的にはあらゆるポイントに到着するスパッタ粒子の速度が同一であると考えられ、その結果、均一な成膜速度が実現可能となると考えられる。よって、スパッタ膜のバラツキを抑制するためには、均一微細な結晶粒を有するランダム配向のターゲット材とすることが望ましい。 In sputtering, when Ar + ions collide with the surface of a target material, they are interrupted between atoms and vigorously vibrate surrounding atoms. The vibration is most easily propagated in the crystal close-packed direction of the target material, and surface atoms are released in the close-packed direction. For this reason, atomic emission during sputtering depends on the crystal structure of the target material. Therefore, the film formation speed of the part corresponding to the priority release direction is high, and the film formation speed of the part corresponding to the non-priority direction is low. Due to the difference in film formation rate, the uniformity of the film thickness distribution of the target material having a polycrystalline structure is governed. Therefore, even if the target material has a polycrystalline structure, if the crystal grains are uniform and fine and the crystal orientation is random, the deposition rate in the preferred orientation is offset, and the spatter that arrives at any point statistically. It is considered that the speed of the particles is the same, and as a result, a uniform film forming speed can be realized. Therefore, in order to suppress variations in the sputtered film, it is desirable to use a randomly oriented target material having uniform fine crystal grains.
本発明のWを3〜15原子%含み、残部Niおよび不可避的不純物からなるターゲット材組成において、ランダム配向に近い状態を維持するためには、fcc相であるNiのランダム配向時のメインピークである(111)面、(200)面、(220)面のX線回折強度の比がランダム配向時に近いことが望ましい。つまりは、fcc相であるNi固溶体の(111)面と(200)面のX線回折における強度比であるI(200)/I(111)が0.30〜0.50であり、かつfcc相であるNi固溶体の(111)面と(220)面のX線回折における強度比であるI(220)/I(111)が0.10〜0.30であることが必要である。
JCPDS(Joint Comittee on Powder Diffrection Standards)カードの純Niから、ランダム配向時のNi(111)面と(200)面のX線回折強度比[I(200)/I(111)]は約0.42であり、(111)面と(220)面のX線回折強度比[I(220)/I(111)]は約0.21であるので、それぞれのX線回折強度比が上記範囲を大きく超えると特定方向の結晶配向が強くなり、スパッタ膜のバラツキが顕著に現れだす。
また、スパッタ膜のバラツキを抑制するには、ターゲットの平均結晶粒径は500μm以下が好ましく、より好ましくは100μm以下である。
In order to maintain a state close to random orientation in the target material composition containing 3 to 15 atomic% of W of the present invention and comprising the balance Ni and unavoidable impurities, the main peak at the time of random orientation of Ni as the fcc phase is used. It is desirable that the ratio of X-ray diffraction intensities of a certain (111) plane, (200) plane, and (220) plane is close to that during random orientation. That is, I (200) / I (111), which is the intensity ratio in the X-ray diffraction between the (111) plane and the (200) plane of the Ni solid solution that is the fcc phase, is 0.30 to 0.50, and fcc It is necessary that I (220) / I (111), which is the intensity ratio in the X-ray diffraction between the (111) plane and the (220) plane of the Ni solid solution as the phase, is 0.10 to 0.30.
From the pure Ni of JCPDS (Joint Committee on Powder Direction Standards) card, the X-ray diffraction intensity ratio [I (200) / I (111)] between the Ni (111) plane and the (200) plane at random orientation is about 0. 42, and the X-ray diffraction intensity ratio [I (220) / I (111)] between the (111) plane and the (220) plane is about 0.21, so that each X-ray diffraction intensity ratio falls within the above range. If it exceeds a large value, the crystal orientation in a specific direction becomes strong, and the variation of the sputtered film appears remarkably.
In addition, in order to suppress variations in the sputtered film, the average crystal grain size of the target is preferably 500 μm or less, more preferably 100 μm or less.
本発明のNi−W系ターゲット材は、粉末冶金技術を用いることにより達成が可能となる。具体的には、原料粉末として、Ni粉末とW粉末を所定の組成となるように混合した混合粉末、ガスアトマイズなどで作製したNi−W合金粉末、組成の異なる複数のNi−W合金粉末を混合した混合粉末などを用いることが出来る。また、各原料粉末を焼結する方法としては、熱間性水圧プレス法やホットプレス法などの加圧焼結が適当できるが、熱間性水圧プレス法を用いるがより望ましい。それは、熱間静水圧プレス法であれば、原料粉末に等方的な圧力を付与することが可能となるので、よりランダム配向を維持した上で、親密度に近い焼結組織のターゲット材を作製できるためである。 The Ni—W target material of the present invention can be achieved by using powder metallurgy technology. Specifically, as a raw material powder, a mixed powder in which Ni powder and W powder are mixed so as to have a predetermined composition, a Ni-W alloy powder produced by gas atomization, and a plurality of Ni-W alloy powders having different compositions are mixed. The mixed powder can be used. In addition, as a method of sintering each raw material powder, pressure sintering such as a hot hydraulic press method or a hot press method can be used, but it is more preferable to use a hot hydraulic press method. If it is a hot isostatic pressing method, it is possible to apply an isotropic pressure to the raw material powder. Therefore, while maintaining a more random orientation, a target material having a sintered structure close to the intimacy can be obtained. This is because it can be manufactured.
さらにIVa族(Ti、Zr、Hf)、Va族(V、Nb、Ta)、VIa族(Cr、Mo、W)、VIIa族(Mn、Tc、Re)、IIIb族(B、Al、Ga、In、Tl)、IVb族(C、Si、Ge、Sn、Pb)から選択される1種または2種以上の添加元素を20原子%以下含むことが望ましい。それは、Ni−W系焼結ターゲット材に上記の添加元素を含有することにより、スパッタにより得られるNi−W合金膜の配向性、結晶粒径や磁性を調整することが可能となるためである。また、ターゲット材の製造に関しては、上記の添加元素は、各純金属粉末として添加した上で加圧焼結するか、または、Ni等に添加して合金粉末とした上で、加圧焼結することも可能である。 Further, Group IVa (Ti, Zr, Hf), Group Va (V, Nb, Ta), Group VIa (Cr, Mo, W), Group VIIa (Mn, Tc, Re), Group IIIb (B, Al, Ga, It is desirable to contain 20 atomic% or less of one or more additive elements selected from In, Tl) and IVb groups (C, Si, Ge, Sn, Pb). This is because the orientation, crystal grain size, and magnetism of the Ni-W alloy film obtained by sputtering can be adjusted by including the above-mentioned additive element in the Ni-W sintered target material. . Regarding the production of the target material, the above additive elements are added as pure metal powders and then sintered under pressure, or added to Ni or the like to form alloy powders and then sintered under pressure. It is also possible to do.
なお、Ni−W系合金への添加元素としては、特にCrが望ましい。それは、Ni-W系合金にCrが添加された場合に密着性および耐食性といった膜特性が改善されるためである。 Note that Cr is particularly desirable as an additive element to the Ni-W alloy. This is because film properties such as adhesion and corrosion resistance are improved when Cr is added to the Ni—W alloy.
図1に示すスパッタ面を直径164mmとする円板形状のNi−W系ターゲット材を表1に示す製造工程で作製した。作製したターゲット材のX線回折による配向性評価を実施した。ターゲット材中のfcc相であるNi固溶体の(111)面、(200)面、(220)面から得られる相対強度と強度比を表2および表3に示す。表2および3中には、参考としてJCPDS(Joint Comittee on Powder Diffrection Standards)カードの純Niのデータをランダムな配向例として記載する。表2および表3から、粉末冶金法で作製した実施例1および2は、Niのランダム配向に近似した配向組織を有しているのに対して、比較例のターゲット材では、Niのランダム配向から大きく乖離した配向組織となっていることがわかる。 また、実施例3のミクロ組織の一例を図2に示す。実施例3の平均結晶粒径は79μmであった。なお、ミクロ組織は鏡面研磨後に塩化第二鉄水溶液で化学腐食を行い、光学顕微鏡で観察を行い、平均結晶粒径は、JIS G551の切断法に準じて測定した1結晶粒当たりの平均線分長とした。 A disc-shaped Ni—W-based target material with a sputter surface shown in FIG. 1 having a diameter of 164 mm was produced by the manufacturing process shown in Table 1. The orientation evaluation by X-ray diffraction of the prepared target material was performed. Tables 2 and 3 show the relative strengths and strength ratios obtained from the (111), (200), and (220) planes of the Ni solid solution that is the fcc phase in the target material. In Tables 2 and 3, pure Ni data of JCPDS (Joint Committee on Powder Direction Standards) card is described as a random orientation example as a reference. From Tables 2 and 3, Examples 1 and 2 produced by powder metallurgy have an orientation structure that approximates the random orientation of Ni, whereas the target material of the comparative example has a random orientation of Ni. It can be seen that the orientation structure is greatly deviated. An example of the microstructure of Example 3 is shown in FIG. The average crystal grain size of Example 3 was 79 μm. The microstructure was mirror-polished and then chemically corroded with a ferric chloride aqueous solution and observed with an optical microscope. The average crystal grain size was the average line segment per crystal grain measured according to the cutting method of JIS G551. It was long.
本発明のNi−W系焼結ターゲット材は垂直磁気記録媒体のNi合金中間層を安定形成するのに優れているため、垂直磁気記録媒体の安定製造に不可欠な技術となる。
Since the Ni—W sintered target material of the present invention is excellent in stably forming the Ni alloy intermediate layer of the perpendicular magnetic recording medium, it is an indispensable technique for stable production of the perpendicular magnetic recording medium.
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