JP2009001862A - Sputtering target for use in forming film of perpendicular magnetic recording medium having low relative magnetic permeability - Google Patents
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 46
- 230000035699 permeability Effects 0.000 title claims abstract description 26
- 238000005477 sputtering target Methods 0.000 title claims abstract description 24
- 229910002058 ternary alloy Inorganic materials 0.000 claims abstract description 31
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 3
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 3
- 229910003452 thorium oxide Inorganic materials 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 abstract description 8
- 239000000843 powder Substances 0.000 description 59
- 239000011812 mixed powder Substances 0.000 description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 16
- 229910004298 SiO 2 Inorganic materials 0.000 description 13
- 238000005520 cutting process Methods 0.000 description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 9
- 229910010413 TiO 2 Inorganic materials 0.000 description 9
- 230000004907 flux Effects 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 238000010894 electron beam technology Methods 0.000 description 8
- 238000004453 electron probe microanalysis Methods 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 238000005211 surface analysis Methods 0.000 description 8
- 238000007731 hot pressing Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- 229910001260 Pt alloy Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- -1 Ta 2 O 5 Inorganic materials 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
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Abstract
Description
この発明は、ハードディスクの高密度磁気記録媒体に適用される磁気記録膜、特に垂直磁気記録媒体に適用される磁気記録膜を形成するための比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲットに関するものである。 The present invention relates to a sputtering target for forming a perpendicular magnetic recording medium film having a low relative permeability for forming a magnetic recording film applied to a high-density magnetic recording medium of a hard disk, particularly a magnetic recording film applied to a perpendicular magnetic recording medium. It is about.
ハードディスク装置は一般にコンピューターやデジタル家電等の外部記録装置として用いられており、記録密度の一層の向上が求められている。そのため、近年、超高密度記録を実現できる垂直磁気記録方式が注目されてきた。この垂直磁気記録方式は、従来の面内記録方式と異なり、原理的に高密度化するほど記録磁化が安定すると言われており、すでに実用化されている。この垂直磁気記録方式のハードディスク媒体の記録層に適用する材料の有力な候補としてＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜が提案されており、このＣｏＣｒＰｔ−ＳｉＯ２グラニュラ磁気記録膜はＣｏ−Ｃｒ−Ｐｔ三元系焼結合金相と二酸化珪素相との混合相を有するスパッタリングターゲットを用いてマグネトロンスパッタすることにより作製することが知られている（非特許文献１参照）。
このスパッタリングターゲットは、通常、二酸化珪素粉末、Ｃｒ粉末、Ｐｔ粉末およびＣｏ粉末を、二酸化珪素：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％を含有し、残部：Ｃｏからなる組成となるように配合し混合したのち、真空ホットプレスまたは熱間静水圧プレスすることにより作製されることが知られており、その他に市販のＣｏ−Ｃｒ−Ｐｔ三元系合金粉末または急冷凝固して作製したＣｏ−Ｃｒ−Ｐｔ三元系合金粉末と二酸化珪素粉末を二酸化珪素：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％を含有し、残部：Ｃｏからなる組成となるように配合し混合したのち、真空ホットプレスまたは熱間静水圧プレスすることにより作製されることが知られている（特許文献１、特許文献２などを参照）。
さらに前記二酸化珪素のほかにＴｉＯ、Ｃｒ２Ｏ３、ＴｉＯ２、Ｔａ２Ｏ５、Ａｌ２Ｏ３、ＢｅＯ２、ＭｇＯ、ＴｈＯ２、ＺｒＯ２、ＣｅＯ２、Ｙ２Ｏ３などの非磁性酸化物が使用できることが知られている（特許文献３、４参照）。
This sputtering target usually contains silicon dioxide powder, Cr powder, Pt powder and Co powder, silicon dioxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%. The remainder: It is known to be prepared by mixing and mixing so as to have a composition consisting of Co, and then vacuum hot pressing or hot isostatic pressing, and in addition, commercially available Co-Cr-Pt ternary Alloy powder or Co—Cr—Pt ternary alloy powder prepared by rapid solidification and silicon dioxide powder: silicon dioxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol It is known that it is prepared by blending and mixing so as to have a composition consisting of Co, the balance: Co, and then vacuum hot pressing or hot isostatic pressing (Patent Document 1, Patent Document). See, eg, 2).
In addition to silicon dioxide, nonmagnetic oxidation such as TiO, Cr 2 O 3 , TiO 2 , Ta 2 O 5 , Al 2 O 3 , BeO 2 , MgO, ThO 2 , ZrO 2 , CeO 2 , Y 2 O 3, etc. It is known that products can be used (see Patent Documents 3 and 4).
この従来の磁気記録媒体膜形成用スパッタリングターゲットは、強磁性合金であるＣｏ−Ｃｒ−Ｐｔ三元系合金相を素地とし、この素地中にＳｉＯ２などの非磁性酸化物が均一分散している組織を有しており、通常の非磁性体ターゲットと比較して磁束がターゲット内部を通過する割合が大きく、ターゲット上空に漏れ出る磁束が極めて少ない。このことはターゲット下部に磁気回路を配置し、ターゲット上空に漏れ出る磁束を利用して希ガスの電離効率を高めることで放電を安定化させ、成膜速度を向上させているマグネトロンスパッタリング法にとっては大きな問題となる。すなわち、ターゲット上空に漏れ出る磁束が少ない漏洩磁束密度の低いターゲット（すなわち比透磁率の高いターゲット）を用いてマグネトロンスパッタリングを行なうと、放電が安定しないかあるいは放電できても成膜速度が極端に遅くなるなどの問題を引き起こすからである。
この問題点を解消するための手段の一つとして、ターゲットの厚さを薄くして磁束をターゲット上空へ抜けやすくする方法が取られている。しかし、ターゲットを薄くすると、ターゲットの交換頻度が頻繁になるので成膜効率が悪くなり、コスト的に好ましくない。
また、漏洩磁束密度の低いターゲットは、一旦マグネトロンスパッタリングを行ってエロージョンが形成されると、エロージョン部分から磁束が集中的に漏洩し、その部分だけが益々集中的にスパッタされていくためにターゲットの利用効率が低下したり、成膜速度が経時変化したり、基板面内に膜厚のばらつきが生じたり、さらにターゲット上への再デポ膜の大量付着が生じるなどといった問題を引き起こしやすい。
This conventional sputtering target for forming a magnetic recording medium film uses a Co—Cr—Pt ternary alloy phase, which is a ferromagnetic alloy, as a base, and nonmagnetic oxides such as SiO 2 are uniformly dispersed in the base. It has a structure, and the proportion of magnetic flux passing through the inside of the target is larger than that of a normal nonmagnetic target, and the magnetic flux leaking over the target is extremely small. This is for magnetron sputtering, which has a magnetic circuit placed under the target and stabilizes the discharge by increasing the ionization efficiency of the noble gas by utilizing the magnetic flux leaking over the target, thereby improving the deposition rate. It becomes a big problem. In other words, if magnetron sputtering is performed using a target having a low leakage magnetic flux density (ie, a target having a high relative permeability) with a small amount of magnetic flux leaking over the target, the deposition rate is extremely high even if the discharge is not stable or can be discharged. This is because it causes problems such as slowness.
As one of means for solving this problem, a method is adopted in which the thickness of the target is reduced so that the magnetic flux easily escapes over the target. However, if the target is made thin, the replacement frequency of the target becomes frequent, so that the film formation efficiency is deteriorated, which is not preferable in terms of cost.
In addition, a target with low leakage magnetic flux density is once the erosion is formed by performing magnetron sputtering, magnetic flux leaks intensively from the erosion part, and only that part is intensively sputtered. It tends to cause problems such as a decrease in utilization efficiency, a change in deposition rate over time, a variation in film thickness within the substrate surface, and a large amount of redeposition film deposited on the target.
そこで、本発明者らは、ターゲットの厚さを薄くすることなく比透磁率の低いスパッタリングターゲットを得るべく研究を行なった。
その結果、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％を含有し、残部：Ｃｏおよび不可避不純物からなる成分組成を有するスパッタリングターゲットにおいて、その組織をＣｏ−Ｃｒ−Ｐｔ三元系合金相とＰｔ相および非磁性酸化物相からなる混合相とにより構成することによりターゲットの比透磁率を低下させることができ、前記Ｃｏ−Ｃｒ−Ｐｔ三元系合金相は前記Ｐｔ相および非磁性酸化物相からなる混合相により包囲されている組織とすることによりターゲットの比透磁率を一層低下させることができる、という研究結果が得られたのである。
Therefore, the present inventors have studied to obtain a sputtering target having a low relative permeability without reducing the thickness of the target.
As a result, in a sputtering target having a component composition comprising nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, and the balance: Co and inevitable impurities The structure can be composed of a Co—Cr—Pt ternary alloy phase and a mixed phase composed of a Pt phase and a nonmagnetic oxide phase to reduce the relative magnetic permeability of the target, and the Co—Cr— Research results have been obtained that the relative permeability of the target can be further reduced by making the Pt ternary alloy phase a structure surrounded by a mixed phase composed of the Pt phase and the nonmagnetic oxide phase. It is.
この発明は、これら研究結果に基づいてなされたものであって、
（１）非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％を含有し、残部：Ｃｏおよび不可避不純物からなる成分組成を有するスパッタリングターゲットであって、このスパッタリングターゲットの組織は、Ｃｏ−Ｃｒ−Ｐｔ三元系合金相と、Ｐｔ相および非磁性酸化物相からなる混合相とからなる組織を有する比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲット、
（２）前記Ｃｏ−Ｃｒ−Ｐｔ三元系合金相は、Ｐｔ相および非磁性酸化物相からなる混合相により包囲されている前記（１）記載の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲット、に特徴を有するものである。
This invention was made based on these research results,
(1) Nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, a sputtering target having a component composition composed of Co and inevitable impurities The structure of the sputtering target is a perpendicular magnetic recording medium film having a low relative permeability having a structure composed of a Co—Cr—Pt ternary alloy phase and a mixed phase composed of a Pt phase and a nonmagnetic oxide phase. Forming sputtering target,
(2) The Co—Cr—Pt ternary alloy phase is surrounded by a mixed phase composed of a Pt phase and a nonmagnetic oxide phase, and the perpendicular magnetic recording medium film formation having a low relative permeability as described in (1) above is performed. The sputtering target has a feature.
この発明の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲットに含まれる前記非磁性酸化物は、二酸化珪素の他に、酸化タンタル、酸化チタン、酸化アルミニウム、酸化マグネシウム、酸化トリウム、酸化ジルコニウム、酸化セリウムおよび酸化イットリウムなどを使用することができる。このことはすでに知られている。したがって、この発明は、
（３）前記非磁性酸化物は、二酸化珪素、酸化タンタル、酸化チタン、酸化アルミニウム、酸化マグネシウム、酸化トリウム、酸化ジルコニウム、酸化セリウムおよび酸化イットリウムのうちのいずれか一種である前記（１）または（２）記載の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲット、に特徴を有するものである。
In addition to silicon dioxide, the nonmagnetic oxide contained in the sputtering target for forming a perpendicular magnetic recording medium film having a low relative permeability according to the present invention is tantalum oxide, titanium oxide, aluminum oxide, magnesium oxide, thorium oxide, zirconium oxide. In addition, cerium oxide and yttrium oxide can be used. This is already known. Therefore, the present invention
(3) The nonmagnetic oxide is any one of silicon dioxide, tantalum oxide, titanium oxide, aluminum oxide, magnesium oxide, thorium oxide, zirconium oxide, cerium oxide, and yttrium oxide. 2) A sputtering target for forming a perpendicular magnetic recording medium film having a low relative magnetic permeability described in 2).
この発明の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲットを製造するには、原料粉末としてＣｏ−Ｃｒ−Ｐｔ三元系合金粉末、Ｐｔ粉末および非磁性酸化物粉末を用意し、これら原料粉末を非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％を含有し、残部：Ｃｏおよび不可避不純物からなる成分組成となるように配合し、混合し、得られた混合粉末を通常のホットプレス温度（１１００℃以上）より低い温度（７００〜１０５０℃）でホットプレスすることにより作製する。この通常より低い温度（７００〜１０５０℃）ホットプレスするのは原料粉末であるＣｏ−Ｃｒ−Ｐｔ三元系合金粉末に含まれるＣｏおよびＣｒがＰｔ相に拡散することを阻止し、さらに素地のＰｔがＣｏ−Ｃｒ−Ｐｔ三元系合金相に拡散してＰｔ相が減少または消滅するのを阻止するためである。 In order to produce a sputtering target for forming a perpendicular magnetic recording medium film having a low relative magnetic permeability according to the present invention, Co—Cr—Pt ternary alloy powder, Pt powder and non-magnetic oxide powder are prepared as raw powders. The raw material powder contains non-magnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, and the balance: a component composition consisting of Co and inevitable impurities. The mixed powder obtained is hot-pressed at a temperature (700 to 1050 ° C.) lower than the normal hot press temperature (1100 ° C. or higher). This hot pressing at a lower temperature (700 to 1050 ° C.) prevents Co and Cr contained in the Co—Cr—Pt ternary alloy powder, which is a raw material powder, from diffusing into the Pt phase. This is to prevent Pt from diffusing into the Co—Cr—Pt ternary alloy phase and decreasing or disappearing.
この発明の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲットを製造する際に使用するＣｏ−Ｃｒ−Ｐｔ三元系合金粉末はＣｒ：４．２〜３３．３モル％、Ｐｔ：０．０１〜１モル％を含有し、残部がＣｏからなる組成を有することが好まく、したがって、この発明の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲットの素地中に分散しているＣｏ−Ｃｒ−Ｐｔ三元系合金相もＣｒ：４．２〜３３．３モル％、Ｐｔ：０．０１〜１モル％を含有し、残部がＣｏからなる組成を有している。 The Co—Cr—Pt ternary alloy powder used in manufacturing the sputtering target for forming a perpendicular magnetic recording medium film having a low relative permeability according to the present invention is Cr: 4.2 to 33.3 mol%, Pt: 0. It is preferable that it has a composition of 0.01 to 1 mol% and the balance is Co, and is therefore dispersed in the base material of the sputtering target for forming a perpendicular magnetic recording medium film having a low relative magnetic permeability according to the present invention. The Co—Cr—Pt ternary alloy phase also contains Cr: 4.2 to 33.3 mol%, Pt: 0.01 to 1 mol%, and the balance is Co.
この発明の比透磁率の低い垂直磁気記録媒体膜形成用スパッタリングターゲットを用いると、マグネトロンスパッタリングを効率よく行なうことができ、コンピューター並びにデジタル家電等の産業の発展に大いに貢献し得るものである。 When the sputtering target for forming a perpendicular magnetic recording medium film having a low relative magnetic permeability according to the present invention is used, magnetron sputtering can be performed efficiently, which can greatly contribute to the development of industries such as computers and digital home appliances.
原料粉末として、表１に示される成分組成を有する平均粒径：２０μｍのＣｏ−Ｃｒ−Ｐｔ三元系合金粉末Ａ〜Ｄ、平均粒径：２５μｍのＰｔ粉末、平均粒径：５μｍのＣｏ粉末、平均粒径：５μｍのＣｒ粉末を用意し、さらに非磁性酸化物粉末としていずれも平均粒径：３μｍのＳｉＯ２粉末、ＴｉＯ２粉末、Ｔａ２Ｏ５粉末およびＡｌ２Ｏ３粉末を用意した。 As raw material powders, average particle size: 20 μm Co—Cr—Pt ternary alloy powders A to D having the composition shown in Table 1, average particle size: 25 μm Pt powder, average particle size: 5 μm Co powder , average particle size: providing a Cr powder of 5 [mu] m, further both the average particle size as the non-magnetic oxide powder: was prepared 3 [mu] m SiO 2 powder, TiO 2 powder, a Ta 2 O 5 powder and Al 2 O 3 powder .
実施例１
表１に示されるＣｏ−Ｃｒ−Ｐｔ三元系合金粉末Ａ、Ｐｔ粉末およびＳｉＯ２粉末を、Ｃｒ：１０．８％、Ｐｔ：１５．３％、ＳｉＯ２：１０．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１２時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：９００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する本発明ターゲット１を作製した。さらにこの本発明ターゲット１を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｐｔ相、ＳｉＯ２相およびＣｏ−Ｃｒ−Ｐｔ三元系合金相が見られ、Ｃｏ−Ｃｒ−Ｐｔ三元系合金相の周囲にＰｔ相とＳｉＯ２相の混合相が見られた。
この本発明ターゲット１についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Example 1
Co—Cr—Pt ternary alloy powder A, Pt powder and SiO 2 powder shown in Table 1 contain Cr: 10.8%, Pt: 15.3%, SiO 2 : 10.0%, The balance is blended so as to have a component composition consisting of Co and inevitable impurities, and the obtained blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, and the atmosphere in the container is replaced with an Ar gas atmosphere. Then, the container was sealed. This container was rotated with a ball mill for 12 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus, and a plate-like hot press body was produced by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 900 ° C., pressure: 35 MPa, and 3 hours.
The target 1 of the present invention having a diameter of 152.4 mm and a thickness of 5 mm was produced by cutting the plate-like hot press body. Further cutting the invention the target 1, observation of the cut surface by a surface analysis of an electron beam microprobe analyzer (EPMA), Pt phase, the SiO 2 phase and Co-Cr-Pt ternary alloy phase As a result, a mixed phase of Pt phase and SiO 2 phase was observed around the Co—Cr—Pt ternary alloy phase.
The maximum relative magnetic permeability in the target in-plane direction was measured for the target 1 of the present invention, and the results are shown in Table 2.
従来例１
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＳｉＯ２粉末を、Ｃｒ：１０．８％、Ｐｔ：１５．３％、ＳｉＯ２：１０．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：１１００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する従来ターゲット１を作製した。さらにこの従来ターゲット１を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｃｏ−Ｃｒ−Ｐｔ合金相中にＳｉＯ２粒子が均一分散している組織が見られた。この従来ターゲット１についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Conventional example 1
The previously prepared Co powder, Cr powder, Pt powder and SiO 2 powder contain Cr: 10.8%, Pt: 15.3%, SiO 2 : 10.0%, and the remainder from Co and inevitable impurities The resulting blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, the atmosphere in the container is replaced with an Ar gas atmosphere, and then the container is sealed. did. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus and vacuum hot pressed in a vacuum atmosphere under conditions of temperature: 1100 ° C., pressure: 35 MPa, and 3 hours to prepare a plate-like hot press body.
By cutting this plate-like hot press body, a conventional target 1 having a diameter of 152.4 mm and a thickness of 5 mm was produced. Further, when this conventional target 1 was cut and the cut surface was observed by an electron beam microprobe analyzer (EPMA) surface analysis method, a structure in which SiO 2 particles were uniformly dispersed in the Co—Cr—Pt alloy phase. It was observed. The maximum relative permeability in the target in-plane direction of this conventional target 1 was measured, and the results are shown in Table 2.
実施例２
表１に示されるＣｏ−Ｃｒ−Ｐｔ三元系合金粉末Ｂ、Ｐｔ粉末およびＴｉＯ２粉末を、Ｃｒ：９．９％、Ｐｔ：１３．５％、ＴｉＯ２：９．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：９００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する本発明ターゲット２を作製した。さらにこの本発明ターゲット２を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｐｔ相、ＴｉＯ２相およびＣｏ−Ｃｒ−Ｐｔ三元系合金相が見られ、Ｃｏ−Ｃｒ−Ｐｔ三元系合金相の周囲にＰｔ相とＴｉＯ２相とからなる混合相が見られた。この本発明ターゲット２についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Example 2
Co—Cr—Pt ternary alloy powder B, Pt powder and TiO 2 powder shown in Table 1 contain Cr: 9.9%, Pt: 13.5%, TiO 2 : 9.0%, The balance is blended so as to have a component composition consisting of Co and inevitable impurities, and the obtained blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, and the atmosphere in the container is replaced with an Ar gas atmosphere. Then, the container was sealed. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus, and a plate-like hot press body was produced by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 900 ° C., pressure: 35 MPa, and 3 hours.
By cutting this plate-like hot press body, the target 2 of the present invention having a diameter of 152.4 mm and a thickness of 5 mm was produced. Further, the target 2 of the present invention was cut, and the cut surface was observed by an electron beam microprobe analyzer (EPMA) surface analysis method. As a result, a Pt phase, a TiO 2 phase, and a Co—Cr—Pt ternary alloy phase were found. As a result, a mixed phase composed of a Pt phase and a TiO 2 phase was observed around the Co—Cr—Pt ternary alloy phase. The maximum relative permeability in the target in-plane direction was measured for the target 2 of the present invention, and the results are shown in Table 2.
従来例２
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＴｉＯ２粉末を、Ｃｒ：９．９％、Ｐｔ：１３．５％、ＴｉＯ２：９．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：１１００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する従来ターゲット２を作製した。さらにこの従来ターゲット２を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｃｏ−Ｃｒ−Ｐｔ合金相中にＴｉＯ２粒子相が分散している組織が見られた。この従来ターゲット２についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Conventional example 2
The previously prepared Co powder, Cr powder, Pt powder and TiO 2 powder contain Cr: 9.9%, Pt: 13.5%, TiO 2 : 9.0%, and the balance from Co and inevitable impurities The resulting blended powder is put into a 10 liter container together with zirconia balls as a grinding medium, the atmosphere in the container is replaced with an Ar gas atmosphere, and then the container is sealed. did. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus and vacuum hot pressed in a vacuum atmosphere under conditions of temperature: 1100 ° C., pressure: 35 MPa, and 3 hours to prepare a plate-like hot press body.
By cutting this plate-like hot press body, a conventional target 2 having a diameter of 152.4 mm and a thickness of 5 mm was produced. Furthermore, when this conventional target 2 was cut and the cut surface was observed by an electron beam microprobe analyzer (EPMA) surface analysis method, a structure in which the TiO 2 particle phase was dispersed in the Co—Cr—Pt alloy phase. It was observed. The maximum relative permeability in the target in-plane direction of this conventional target 2 was measured, and the results are shown in Table 2.
実施例３
表１に示されるＣｏ−Ｃｒ−Ｐｔ三元系合金粉末Ｃ、Ｐｔ粉末およびＴａ２Ｏ５粉末を、Ｃｒ：１６．０％、Ｐｔ：１５．４％、Ｔａ２Ｏ５：５．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：９００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する本発明ターゲット３を作製した。さらにこの本発明ターゲット３を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｐｔ相、Ｔａ２Ｏ５相およびＣｏ−Ｃｒ−Ｐｔ三元系合金相が見られ、Ｃｏ−Ｃｒ−Ｐｔ三元系合金相の周囲にＰｔ相とＴａ２Ｏ５相からなる混合相が見られた。この本発明ターゲット３についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Example 3
Co—Cr—Pt ternary alloy powder C, Pt powder, and Ta 2 O 5 powder shown in Table 1 are Cr: 16.0%, Pt: 15.4%, Ta 2 O 5 : 5.0% In which the balance is a component composition consisting of Co and inevitable impurities, and the resulting blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, and the atmosphere in the container is filled with Ar gas. The atmosphere was replaced, and then the container was sealed. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus, and a plate-like hot press body was produced by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 900 ° C., pressure: 35 MPa, and 3 hours.
By cutting this plate-like hot press body, the target 3 of the present invention having a diameter of 152.4 mm and a thickness of 5 mm was produced. Further cutting the invention target 3, was observed with the cut surface in the surface analysis of the electron beam microprobe analyzer (EPMA), Pt phase, Ta 2 O 5 phase and Co-Cr-Pt ternary alloy A phase was observed, and a mixed phase composed of a Pt phase and a Ta 2 O 5 phase was observed around the Co—Cr—Pt ternary alloy phase. The maximum relative permeability in the in-plane direction of the target 3 of the present invention was measured, and the results are shown in Table 2.
従来例３
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＴａ２Ｏ５粉末を、Ｃｒ：１６．０％、Ｐｔ：１５．４％、Ｔａ２Ｏ５：５．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：１１００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する従来ターゲット３を作製した。さらにこの従来ターゲット３を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｃｏ−Ｃｒ−Ｐｔ合金相中にＴａ２Ｏ５粒子相が分散している組織が見られた。この従来ターゲット３についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Conventional example 3
Co powder prepared in advance, Cr powder, Pt powder and Ta 2 O 5 powder, Cr: 16.0%, Pt: 15.4%, Ta 2 O 5: it contains 5.0%, the balance being Co And the resulting blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, and the atmosphere in the container is replaced with an Ar gas atmosphere. The container was sealed. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus and vacuum hot pressed in a vacuum atmosphere under conditions of temperature: 1100 ° C., pressure: 35 MPa, and 3 hours to prepare a plate-like hot press body.
By cutting this plate-like hot press body, a conventional target 3 having a diameter of 152.4 mm and a thickness of 5 mm was produced. Furthermore, when this conventional target 3 was cut and the cut surface was observed by an electron beam microprobe analyzer (EPMA) surface analysis method, Ta 2 O 5 particle phase was dispersed in the Co—Cr—Pt alloy phase. Some organizations were seen. The maximum relative permeability in the target in-plane direction of this conventional target 3 was measured, and the results are shown in Table 2.
実施例４
表１に示されるＣｏ−Ｃｒ−Ｐｔ三元系合金粉末Ｄ、Ｐｔ粉末およびＡｌ２Ｏ３粉末を、Ｃｒ：１０．７％、Ｐｔ：１４．７％、Ａｌ２Ｏ３：６．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：９００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する本発明ターゲット４を作製した。さらにこの本発明ターゲット４を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｐｔ相、Ａｌ２Ｏ３相およびＣｏ−Ｃｒ−Ｐｔ三元系合金相が見られ、Ｃｏ−Ｃｒ−Ｐｔ三元系合金相の周囲にＰｔ相とＡｌ２Ｏ３相からなる混合相が見られた。この本発明ターゲット４についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Example 4
Co—Cr—Pt ternary alloy powder D, Pt powder and Al 2 O 3 powder shown in Table 1 are Cr: 10.7%, Pt: 14.7%, Al 2 O 3 : 6.0% In which the balance is a component composition consisting of Co and inevitable impurities, and the resulting blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, and the atmosphere in the container is filled with Ar gas. The atmosphere was replaced, and then the container was sealed. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus, and a plate-like hot press body was produced by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 900 ° C., pressure: 35 MPa, and 3 hours.
By cutting this plate-like hot press body, the target 4 of the present invention having a diameter of 152.4 mm and a thickness of 5 mm was produced. Further cutting the invention target 4, was observed with the cut surface in the surface analysis of the electron beam microprobe analyzer (EPMA), Pt phase, Al 2 O 3 phase and Co-Cr-Pt ternary alloy A phase was observed, and a mixed phase composed of a Pt phase and an Al 2 O 3 phase was observed around the Co—Cr—Pt ternary alloy phase. The maximum relative permeability in the target in-plane direction of this target 4 of the present invention was measured, and the results are shown in Table 2.
従来例４
先に用意したＣｏ粉末、Ｃｒ粉末、Ｐｔ粉末およびＡｌ２Ｏ３粉末を、Ｃｒ：１０．７％、Ｐｔ：１４．７％、Ａｌ２Ｏ３：６．０％を含有し、残部がＣｏおよび不可避不純物からなる成分組成となるように配合し、得られた配合粉末を粉砕媒体となるジルコニアボールと共に１０リットルの容器に投入し、この容器内の雰囲気をＡｒガス雰囲気中で置換し、その後、容器を密閉した。この容器をボールミルで１６時間回転させ、混合粉末を作製した。得られた混合粉末を真空ホットプレス装置に充填し、真空雰囲気中、温度：１１００℃、圧力：３５ＭＰａ、３時間保持の条件で真空ホットプレスすることにより板状ホットプレス体を作製した。
この板状ホットプレス体を切削することによりいずれも直径：１５２．４ｍｍ、厚さ：５ｍｍの寸法を有する従来ターゲット４を作製した。さらにこの従来ターゲット４を切断し、その切断面を電子線マイクロプローブアナライザ（ＥＰＭＡ）の面分析法にて観察したところ、Ｃｏ−Ｃｒ−Ｐｔ合金相中にＡｌ２Ｏ３粒子相が均一分散している組織が見られた。この従来ターゲット４についてターゲット面内方向の最大比透磁率を測定し、その結果を表２に示した。
Conventional example 4
Co powder prepared in advance, Cr powder, Pt powder and Al 2 O 3 powder, Cr: 10.7%, Pt: 14.7%, Al 2 O 3: contains 6.0%, the balance being Co And the resulting blended powder is put into a 10-liter container together with zirconia balls as a grinding medium, and the atmosphere in the container is replaced with an Ar gas atmosphere. The container was sealed. This container was rotated with a ball mill for 16 hours to produce a mixed powder. The obtained mixed powder was filled in a vacuum hot press apparatus and vacuum hot pressed in a vacuum atmosphere under conditions of temperature: 1100 ° C., pressure: 35 MPa, and 3 hours to prepare a plate-like hot press body.
By cutting this plate-like hot press body, the conventional target 4 having a diameter of 152.4 mm and a thickness of 5 mm was produced. Furthermore, when this conventional target 4 was cut and the cut surface was observed by an electron beam microprobe analyzer (EPMA) surface analysis method, the Al 2 O 3 particle phase was uniformly dispersed in the Co—Cr—Pt alloy phase. The organization that has been seen. The maximum relative permeability in the target in-plane direction of this conventional target 4 was measured, and the results are shown in Table 2.
表２に示される結果から、本発明ターゲット１と従来ターゲット１を比較すると、成分組成は同じであるが、素地中にＣｏ−Ｃｒ−Ｐｔ三元系合金相が均一分散しその周囲をＰｔ相および非磁性酸化物相であるＳｉＯ２相からなる混合相により包囲されている本発明ターゲット１は、Ｃｏ−Ｃｒ−Ｐｔ三元系合金相の中に非磁性酸化物相であるＳｉＯ２相が分散している従来ターゲット１に比べて、ターゲット面内方向の最大比透磁率が小さいところから、スパッタリングに際して漏洩磁束密度が大きく、したがって、本発明ターゲット１は従来ターゲット１に比べて効率よくスパッタできることが分かる。同様にして、本発明ターゲット２と従来ターゲット２、本発明ターゲット３と従来ターゲット３、本発明ターゲット４と従来ターゲット４をそれぞれ比較すると、本発明ターゲット２〜４は従来ターゲット２〜４に比べて効率よくスパッタできることが分かる。 From the results shown in Table 2, when the target 1 of the present invention and the conventional target 1 are compared, the composition of the components is the same, but the Co—Cr—Pt ternary alloy phase is uniformly dispersed in the substrate, and the Pt phase surrounds it. and non-magnetic oxide phase present invention targets are surrounded by a mixed phase consisting of SiO 2 phase 1 is the, SiO 2 phase is a non-magnetic oxide phase in the Co-Cr-Pt ternary alloy phase Since the maximum relative permeability in the in-plane direction of the target is smaller than that of the conventional target 1 that is dispersed, the leakage magnetic flux density is large during sputtering. Therefore, the target 1 of the present invention can be sputtered more efficiently than the conventional target 1. I understand. Similarly, when the present invention target 2 and the conventional target 2, the present invention target 3 and the conventional target 3, and the present invention target 4 and the conventional target 4 are respectively compared, the present invention targets 2 to 4 are compared with the conventional targets 2 to 4. It can be seen that sputtering can be performed efficiently.
Claims (3)
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| JP2012036452A (en) * | 2010-08-06 | 2012-02-23 | Tanaka Kikinzoku Kogyo Kk | Target for magnetron sputtering, and method of manufacturing the same |
| JP2012087412A (en) * | 2011-11-17 | 2012-05-10 | Tanaka Kikinzoku Kogyo Kk | Target for magnetron sputtering and method of producing the same |
| WO2012077665A1 (en) * | 2010-12-09 | 2012-06-14 | Jx日鉱日石金属株式会社 | Ferromagnetic material sputtering target |
| US8568576B2 (en) | 2008-03-28 | 2013-10-29 | Jx Nippon Mining & Metals Corporation | Sputtering target of nonmagnetic-particle-dispersed ferromagnetic material |
| US9103023B2 (en) | 2009-03-27 | 2015-08-11 | Jx Nippon Mining & Metals Corporation | Nonmagnetic material particle-dispersed ferromagnetic material sputtering target |
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| US8568576B2 (en) | 2008-03-28 | 2013-10-29 | Jx Nippon Mining & Metals Corporation | Sputtering target of nonmagnetic-particle-dispersed ferromagnetic material |
| US8932444B2 (en) | 2008-03-28 | 2015-01-13 | Jx Nippon Mining & Metals Corporation | Sputtering target of nonmagnetic-particle-dispersed ferromagnetic material |
| US8936707B2 (en) | 2008-03-28 | 2015-01-20 | Jx Nippon Mining & Metals Corporation | Sputtering target of nonmagnetic-particle-dispersed ferromagnetic material |
| WO2010067446A1 (en) * | 2008-12-11 | 2010-06-17 | 三菱マテリアル株式会社 | Sputtering target for forming perpendicular magnetic recording medium film having low relative permeability |
| US9103023B2 (en) | 2009-03-27 | 2015-08-11 | Jx Nippon Mining & Metals Corporation | Nonmagnetic material particle-dispersed ferromagnetic material sputtering target |
| JP2012036452A (en) * | 2010-08-06 | 2012-02-23 | Tanaka Kikinzoku Kogyo Kk | Target for magnetron sputtering, and method of manufacturing the same |
| WO2012077665A1 (en) * | 2010-12-09 | 2012-06-14 | Jx日鉱日石金属株式会社 | Ferromagnetic material sputtering target |
| CN103080368A (en) * | 2010-12-09 | 2013-05-01 | 吉坤日矿日石金属株式会社 | Ferromagnetic material sputtering target |
| JP2012087412A (en) * | 2011-11-17 | 2012-05-10 | Tanaka Kikinzoku Kogyo Kk | Target for magnetron sputtering and method of producing the same |
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