JP2009108336A - MANUFACTURING METHOD OF Co-BASE SINTERED ALLOY SPUTTERING TARGET FOR FORMING MAGNETIC RECORDING FILM OF LOW RELATIVE MAGNETIC PERMEABILITY - Google Patents
MANUFACTURING METHOD OF Co-BASE SINTERED ALLOY SPUTTERING TARGET FOR FORMING MAGNETIC RECORDING FILM OF LOW RELATIVE MAGNETIC PERMEABILITY Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 120
- 239000000956 alloy Substances 0.000 title claims abstract description 120
- 230000035699 permeability Effects 0.000 title claims abstract description 40
- 238000005477 sputtering target Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 187
- 239000000203 mixture Substances 0.000 claims abstract description 58
- 229910000684 Cobalt-chrome Inorganic materials 0.000 claims abstract description 45
- 239000010952 cobalt-chrome Substances 0.000 claims abstract description 45
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 24
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 16
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000007731 hot pressing Methods 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001513 hot isostatic pressing Methods 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 4
- 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
- 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 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
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 239000011651 chromium Substances 0.000 description 66
- 238000000034 method Methods 0.000 description 19
- 239000011812 mixed powder Substances 0.000 description 16
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 238000007796 conventional method Methods 0.000 description 13
- 238000005520 cutting process Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 238000009689 gas atomisation Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- -1 Ta 2 O 5 Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000002265 prevention Effects 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スパッタリングターゲットの製造方法に関するものである。 The present invention relates to a method of manufacturing a sputtering target 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.
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、超高密度の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磁気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、この磁気記録膜は高性能な磁気記録膜であることが必要である。これに適用可能な磁気記録膜の一つとして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ＣｒおよびＰｔを含むＣｏ基焼結合金相と二酸化珪素相の混合相を有するＣｏ基焼結合金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法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Ｃｏ基焼結合金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：２〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜３０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、ホットプレスまたは熱間静水圧プレスなどの方法で加圧焼結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、二酸化珪素：２〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜３０モル％を含有し、残部：Ｃｏからなる組成にさらにＢ：０．５〜８モル％を含有するターゲットも知られている（特許文献５参照）。
さらに、前記非磁性酸化物はＳｉＯ２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 Co-based sintered alloy sputtering target is usually composed of silicon dioxide powder, Cr powder, Pt powder and Co powder, silicon dioxide: 2 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 30 mol%. It is known that it is prepared by mixing and mixing so as to have a composition consisting of Co: the balance: Co, and then pressure sintering by a method such as hot pressing or hot isostatic pressing (patent) (See Reference 1, Patent Reference 2, etc.).
Further, silicon dioxide: 2 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 30 mol%, and the balance: Co further contained B: 0.5 to 8 mol% A target is also known (see Patent Document 5).
Furthermore, the non-magnetic oxide is TiO Besides SiO 2, 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 It is known that nonmagnetic oxides such as 3 can be used (see Patent Documents 3 and 4).
しかし、前記従来の方法で作製したＣｏ基焼結合金スパッタリングターゲットは比透磁率が高いために、ターゲット上空に漏れ出る磁束が少ないマグネトロンスパッタリングに適用した際には成膜速度が低下しさらにターゲットの利用効率が低下するという問題点があった。したがって、一層比透磁率の低いＣｏ基焼結合金からなるスパッタリングターゲットが求められていた。 However, since the Co-based sintered alloy sputtering target produced by the conventional method has a high relative magnetic permeability, when applied to magnetron sputtering where the magnetic flux leaking over the target is small, the film formation rate decreases and the target There was a problem that the utilization efficiency decreased. Therefore, a sputtering target made of a Co-based sintered alloy having a lower relative permeability has been demanded.
そこで、本発明者は、比透磁率の一層低いＣｏ基焼結合金スパッタリングターゲットを得るべく研究を行なったところ、
原料粉末としてＣｒ：５０〜７０原子％を含有し、残部がＣｏからなる成分組成を有するＣｒ含有量が多いＣｏＣｒ合金粉末（以下、第一ＣｏＣｒ合金粉末という）と、Ｃｒ：５〜１５原子％を含有し、残部がＣｏからなる成分組成を有する前記第一ＣｏＣｒ合金粉末よりもＣｒ含有量の少ないＣｏＣｒ合金粉末（以下、第二ＣｏＣｒ合金粉末という）、Ｐｔ粉末および非磁性酸化物粉末を、
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、混合したのち加圧焼結することにより得られた磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットは、従来法である二酸化珪素粉末、Ｃｒ粉末、Ｐｔ粉末およびＣｏ粉末を、二酸化珪素：２〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜３０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、ホットプレスまたは熱間静水圧プレスなどの方法で加圧焼結することにより作製されたＣｏ基焼結合金スパッタリングターゲットに比べて、成分組成が同じであっても比透磁率が低くなる、というという研究結果が得られたのである。
Therefore, the present inventor conducted research to obtain a Co-based sintered alloy sputtering target having a lower relative permeability.
CoCr alloy powder (hereinafter referred to as the first CoCr alloy powder) containing Cr: 50 to 70 atom% as raw material powder and having a component composition consisting of Co as the balance, and Cr: 5 to 15 atom% CoCr alloy powder (hereinafter referred to as second CoCr alloy powder), Pt powder and non-magnetic oxide powder having a Cr content lower than that of the first CoCr alloy powder having a component composition consisting of Co.
Nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, with the balance being a component composition consisting of Co and inevitable impurities, mixed and mixed After that, the Co-based sintered alloy sputtering target for forming a magnetic recording film obtained by pressure sintering is obtained by using conventional silicon dioxide powder, Cr powder, Pt powder and Co powder with silicon dioxide: 2-15. After containing and mixing so as to have a composition consisting of mol%, Cr: 4 to 20 mol%, Pt: 5 to 30 mol% and the balance: Co, by a method such as hot pressing or hot isostatic pressing. As a result, it has been found that the relative permeability is low even when the component composition is the same as compared with the Co-based sintered alloy sputtering target produced by pressure sintering.
この発明は、かかる研究結果に基づいてなされたものであって、
（１）Ｃｒ：５０〜７０原子％を含有し、残部がＣｏからなる成分組成を有する第一ＣｏＣｒ合金粉末、Ｃｒ：５〜１５原子％を含有し、残部がＣｏからなる成分組成を有する第二ＣｏＣｒ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、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、混合したのち加圧焼結する比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、に特徴を有するものである。
The present invention has been made based on the results of such research,
(1) First CoCr alloy powder containing Cr: 50 to 70 atomic%, with the balance being composed of Co, and Cr: No. 5 having 15 to 15 atomic% and the balance being composed of Co. 2 CoCr alloy powder, Pt powder and non-magnetic oxide powder containing non-magnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, the balance being Co And a method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative magnetic permeability, which is compounded so as to have a component composition consisting of inevitable impurities, mixed and then subjected to pressure sintering. .
一般に、磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットは、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、残部がＣｏおよび不可避不純物からなる成分組成を有することが知られているが、これにさらにＢ：０．５〜８モル％含有する成分組成を有しても良く、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、残部がＣｏおよび不可避不純物からなる成分組成を有する磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットも知られている。
このＢを含有する磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットは、前記第一ＣｏＣｒ合金粉末および前記第二ＣｏＣｒ合金粉末のいずれか一方または両方の粉末に、さらにＢ：０．５〜８原子％を含有する成分組成を有する粉末にＰｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結することにより比透磁率の一層低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットを製造することができる。
Generally, a Co-based sintered alloy sputtering target for forming a magnetic recording film contains nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, with the balance being It is known to have a component composition consisting of Co and inevitable impurities, but it may further have a component composition containing B: 0.5 to 8 mol%, and nonmagnetic oxide: 0.5 to Also known is a Co-based sintered alloy sputtering target for forming a magnetic recording film having a component composition containing 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, and the balance consisting of Co and inevitable impurities. ing.
The Co-based sintered alloy sputtering target for forming a magnetic recording film containing B includes either or both of the first CoCr alloy powder and the second CoCr alloy powder, and B: 0.5 to 8 Pt powder and nonmagnetic oxide powder are added to powder having a component composition containing atomic%, nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, B: A magnetic recording film having a lower relative magnetic permeability is formed by blending so as to contain 0.5 to 8 mol%, with the balance being a component composition consisting of Co and inevitable impurities, mixing, and then pressure sintering. Co-based sintered alloy sputtering target can be produced.
したがって、この発明は、
（２）前記第一ＣｏＣｒ合金粉末および前記第二ＣｏＣｒ合金粉末のいずれか一方または両方の粉末は、さらにＢ：０．５〜８原子％を含有する成分組成を有する粉末であり、これら粉末にＰｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結する前記（１）記載の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、に特徴を有するものである。
Therefore, the present invention
(2) Either one or both of the first CoCr alloy powder and the second CoCr alloy powder are powders having a component composition further containing B: 0.5 to 8 atomic%, Pt powder and nonmagnetic oxide powder containing nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, B: 0.5 to 8 mol% In addition, the Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative magnetic permeability according to the above (1), wherein the remainder is blended so as to have a component composition comprising Co and inevitable impurities, mixed and then pressure-sintered The manufacturing method is characterized.
一層具体的には、原料粉末として、前記Ｃｒ含有量の多い第一ＣｏＣｒ合金粉末にさらにＢ：０．５〜８原子％を含有する成分組成を有する粉末（以下、第一ＣｏＣｒＢ合金粉末という）および前記第一ＣｏＣｒ合金粉末に比べてＣｒ含有量の少ない前記第二ＣｏＣｒ合金粉末にさらにＢ：０．５〜８原子％を含有する成分組成を有する粉末（以下、第二ＣｏＣｒＢ合金粉末という）を更に用意し、これら原料粉末を、
（イ）前記第一ＣｏＣｒ合金粉末、前記第二ＣｏＣｒＢ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結することにより得られた磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲット、
（ロ）前記第一ＣｏＣｒＢ合金粉末、前記第二ＣｏＣｒ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結することにより得られた磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲット、並びに
（ハ）前記第一ＣｏＣｒＢ合金粉末、前記第二ＣｏＣｒＢ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結することにより得られた磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットは、
従来の純Ｃｏ粉末、純Ｃｒ粉末、Ｐｔ粉末、Ｂ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結することにより得られた磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットに比べて比透磁率が一層低くなる、という研究結果が得られ、この発明は、かかる研究結果に基づいてなされたものであって、
（ａ）第一ＣｏＣｒ合金粉末、第二ＣｏＣｒＢ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結する比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、
（ｂ）第一ＣｏＣｒＢ合金粉末、第二ＣｏＣｒ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結する比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、
（ｃ）第一ＣｏＣｒＢ合金粉末、第二ＣｏＣｒＢ合金粉末、Ｐｔ粉末および非磁性酸化物粉末を、非磁性酸化物：０．５〜１５モル％、Ｃｒ：４〜２０モル％、Ｐｔ：５〜２５モル％、Ｂ：０．５〜８モル％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、混合したのち加圧焼結する比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、に特徴を有するものである。
More specifically, as a raw material powder, a powder having a component composition containing B: 0.5 to 8 atomic% in the first CoCr alloy powder having a high Cr content (hereinafter referred to as the first CoCrB alloy powder). And a powder having a component composition further containing B: 0.5 to 8 atomic% in the second CoCr alloy powder having a smaller Cr content than the first CoCr alloy powder (hereinafter referred to as a second CoCrB alloy powder). And preparing these raw material powders
(A) The first CoCr alloy powder, the second CoCrB alloy powder, the Pt powder and the nonmagnetic oxide powder are mixed with nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, B: 0.5 to 8 mol%, with the balance being a component composition consisting of Co and unavoidable impurities, mixed, mixed and then pressure sintered Co-based sintered alloy sputtering target for recording film formation,
(B) The first CoCrB alloy powder, the second CoCr alloy powder, the Pt powder and the nonmagnetic oxide powder are mixed with nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, B: 0.5 to 8 mol%, with the balance being a component composition consisting of Co and unavoidable impurities, mixed, mixed and then pressure sintered Co-based sintered alloy sputtering target for recording film formation, and (c) the first CoCrB alloy powder, the second CoCrB alloy powder, the Pt powder, and the nonmagnetic oxide powder, nonmagnetic oxide: 0.5 to 15 It is mixed and mixed so that it contains a mole composition, Cr: 4 to 20 mole%, Pt: 5 to 25 mole%, B: 0.5 to 8 mole%, and the balance is composed of Co and inevitable impurities. Then pressurize and sinter More obtained magnetic recording film forming Co sintered alloy sputtering target,
Conventional pure Co powder, pure Cr powder, Pt powder, B powder and non-magnetic oxide powder are mixed with non-magnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol. %, B: 0.5 to 8 mol%, with the balance being a component composition consisting of Co and inevitable impurities, mixed and mixed, and then subjected to pressure sintering to form a magnetic recording film A research result that relative permeability is further lower than that of a Co-based sintered alloy sputtering target was obtained, and the present invention was made based on the research result,
(A) First CoCr alloy powder, second CoCrB alloy powder, Pt powder and non-magnetic oxide powder are mixed with non-magnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 5 A magnetic recording film having a low relative magnetic permeability containing 25 mol%, B: 0.5 to 8 mol%, blended so that the balance is a component composition of Co and inevitable impurities, mixed and then pressure sintered Method for producing Co-based sintered alloy sputtering target for formation,
(B) First CoCrB alloy powder, second CoCr alloy powder, Pt powder and non-magnetic oxide powder are mixed with non-magnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 5 A magnetic recording film having a low relative magnetic permeability containing 25 mol%, B: 0.5 to 8 mol%, blended so that the balance is a component composition of Co and inevitable impurities, mixed and then pressure sintered Method for producing Co-based sintered alloy sputtering target for formation,
(C) First CoCrB alloy powder, second CoCrB alloy powder, Pt powder and non-magnetic oxide powder are mixed with non-magnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 5 A magnetic recording film having a low relative magnetic permeability containing 25 mol%, B: 0.5 to 8 mol%, blended so that the balance is a component composition of Co and inevitable impurities, mixed and then pressure sintered It is characterized by a method for producing a forming Co-based sintered alloy sputtering target.
この発明の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法で使用する非磁性酸化物粉末は、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であり、特に二酸化珪素、酸化タンタル、酸化チタン、酸化アルミニウムのうちのいずれかであることが好ましいことはすでに知られている。したがって、この発明は、
（３）前記非磁性酸化物粉末は、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である前記（１）または（２）記載の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、に特徴を有するものである。
The nonmagnetic oxide powder used in the method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative permeability according to the present invention is silicon dioxide, tantalum oxide, titanium oxide, aluminum oxide, magnesium oxide, thorium oxide. It is already known that any one of zirconium oxide, cerium oxide, and yttrium oxide is preferable, and any of silicon dioxide, tantalum oxide, titanium oxide, and aluminum oxide is particularly preferable. Therefore, the present invention
(3) The nonmagnetic oxide powder is any one of (1) or (1), which 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 method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative magnetic permeability described in 2).
前記加圧焼結は、具体的には、ホットプレスまたは熱間静水圧プレスであることが好ましい。したがって、この発明は、
（４）前記加圧焼結は、ホットプレスまたは熱間静水圧プレスである前記（１）、（２）または（３）記載の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法、に特徴を有するものである。
Specifically, the pressure sintering is preferably hot pressing or hot isostatic pressing. Therefore, the present invention
(4) The pressure sintering is a hot press or a hot isostatic press. Co-based sintered alloy sputtering for forming a magnetic recording film having a low relative magnetic permeability according to (1), (2) or (3). It has the characteristic in the manufacturing method of a target.
この発明の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法において原料粉末として第一ＣｏＣｒ合金粉末、第二ＣｏＣｒ合金粉末、第一ＣｏＣｒＢ合金粉末および第二ＣｏＣｒＢ合金粉末を使用する理由は、第一ＣｏＣｒ合金粉末および第一ＣｏＣｒＢ合金粉末はＣｏとＣｒが非磁性体の金属間化合物を生成する組成域であることから低透磁率化に有効であり、なおかつ金属間化合物中のＣｒは酸化しにくくなってパーティクルの原因となるＣｒの酸化凝集体を生じにくくすることから、出発原料粉末として非常に有効であるからである。しかし、この高Ｃｒ含有の第一ＣｏＣｒ合金粉末または第一ＣｏＣｒＢ合金粉末を使用する際に、目標のターゲット組成を得るためには残量のＣｏを純Ｃｏ粉末で供給すると透磁率が上昇する。これを抑制するためにＣｏに少量のＣｒを加えて、ある程度透磁率を下げた低Ｃｒ組成の第二ＣｏＣｒ合金粉末または第二ＣｏＣｒＢ合金粉末からＣｏを供給することが有効であるからである。 First CoCr alloy powder, second CoCr alloy powder, first CoCrB alloy powder and second CoCrB alloy powder as raw material powders in the method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative permeability according to the present invention The first CoCr alloy powder and the first CoCrB alloy powder are effective in reducing the magnetic permeability because Co and Cr are composition regions in which Co and Cr form a non-magnetic intermetallic compound. This is because Cr in the compound is very effective as a starting raw material powder because it is difficult to oxidize and it is difficult to produce an oxidized aggregate of Cr that causes particles. However, when using this high Cr-containing first CoCr alloy powder or first CoCrB alloy powder, the magnetic permeability increases if the remaining amount of Co is supplied as pure Co powder in order to obtain the target composition. In order to suppress this, it is effective to supply Co from the second CoCr alloy powder or the second CoCrB alloy powder having a low Cr composition by adding a small amount of Cr to Co and lowering the magnetic permeability to some extent.
次に、この発明の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法において使用する第一ＣｏＣｒ合金粉末および第一ＣｏＣｒＢ合金粉末のＣｒを５０〜７０原子％とし、一方、第二ＣｏＣｒ合金粉末および第二ＣｏＣｒＢ合金粉末のＣｒを５〜１５原子％に限定した理由を説明する。
第一ＣｏＣｒ合金粉末および第一ＣｏＣｒＢ合金粉末のＣｒ含有量を５０〜７０原子％としたのは、この範囲を外れると、粉末中のＣｏＣｒの金属間化合物が少なくなり、Ｃｒ酸化防止効果が小さくなるので好ましくないからであり、一方、第二ＣｏＣｒ合金粉末および第二ＣｏＣｒＢ合金粉末のＣｒを５〜１５原子％としたのは、５原子％未満ではＣｏ合金粉末の透磁率が高くなりすぎるので好ましくなく、１５原子％を超えて含有するとターゲット全体としてＣｒが高Ｃｒ含有の第一ＣｏＣｒ合金粉末よりも低Ｃｒ含有の第二ＣｏＣｒ合金粉末の方に多く存在することとなり、低透磁率化およびＣｒ酸化防止の観点から好ましくない理由によるものである。一層好ましくは、７〜１２原子％である。
また、Ｂを第一ＣｏＣｒ合金粉末および第二ＣｏＣｒ合金粉末に添加して第一ＣｏＣｒＢ合金粉末および第二ＣｏＣｒＢ合金粉末として添加するのは、Ｂを単独粉末で加えると、製造工程中にＢ粉末が酸化し易いために好ましくなく、Ｂの酸化防止のためにはＢを合金粉末として添加するのが好ましいからである。
Next, Cr of the first CoCr alloy powder and the first CoCrB alloy powder used in the method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative permeability according to the present invention is 50 to 70 atomic%, On the other hand, the reason why Cr in the second CoCr alloy powder and the second CoCrB alloy powder is limited to 5 to 15 atomic% will be described.
The reason why the Cr content of the first CoCr alloy powder and the first CoCrB alloy powder is 50 to 70 atomic% is that if it is outside this range, the amount of CoCr intermetallic compounds in the powder decreases, and the Cr oxidation prevention effect is small. On the other hand, the Cr content of the second CoCr alloy powder and the second CoCrB alloy powder is set to 5 to 15 atomic% because the magnetic permeability of the Co alloy powder is too high if it is less than 5 atomic%. Undesirably, if the content exceeds 15 atomic%, the Cr as a whole will be present more in the second CoCr alloy powder having a lower Cr content than in the first CoCr alloy powder having a higher Cr content. This is because it is not preferable from the viewpoint of preventing Cr oxidation. More preferably, it is 7 to 12 atomic%.
In addition, B is added to the first CoCr alloy powder and the second CoCr alloy powder and added as the first CoCrB alloy powder and the second CoCrB alloy powder. This is because it is not preferable because it is easily oxidized, and it is preferable to add B as an alloy powder in order to prevent oxidation of B.
この発明の比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法において使用する第一ＣｏＣｒ合金粉末、第二ＣｏＣｒ合金粉末、第一ＣｏＣｒＢ合金粉末および第二ＣｏＣｒＢ合金粉末は、５０％粒径が１５０μｍを越えると混合粉砕時に粉砕が十分に進まないことから、粒径は５０％粒径が１５０μｍ以下であることが好ましく、微細であるほど好ましいところから分級などにより５０％粒径が７５μｍ以下にすることが一層好ましく、さらに５０％粒径が４５μｍ以下とすることがさらに一層好ましい。前記原料粉末の混合は不活性ガス雰囲気中で行なうことが好ましい。これは混合中にＣｒが酸素と結合してクロム酸化物凝集体が形成されるのをより一層防止するからである。 The first CoCr alloy powder, the second CoCr alloy powder, the first CoCrB alloy powder, and the second CoCrB alloy powder used in the method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative permeability according to the present invention are: When the 50% particle size exceeds 150 μm, the pulverization does not sufficiently proceed during the mixing and pulverization. Therefore, the 50% particle size is preferably 150 μm or less, and the finer the particle size is, the more preferable 50% by classification or the like. The particle size is more preferably 75 μm or less, and further preferably the 50% particle size is 45 μm or less. The raw material powder is preferably mixed in an inert gas atmosphere. This is because it further prevents Cr from being combined with oxygen to form chromium oxide aggregates during mixing.
この発明は、一層比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットまたは磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットを提供することができ、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。 The present invention can provide a Co-based sintered alloy sputtering target for forming a magnetic recording film or a Co-based sintered alloy sputtering target for forming a magnetic recording film having a lower relative permeability. It can greatly contribute to development.
市販の５０％粒径：１０μｍのＣｏ粉末、５０％粒径：１５μｍのＰｔ粉末、５０％粒径：５μｍのＢ粉末を用意し、さらに非磁性酸化物粉末として５０％粒径：３μｍのＳｉＯ２粉末、５０％粒径：３μｍのＴｉＯ２粉末、５０％粒径：３μｍのＴａ２Ｏ５粉末および５０％粒径：３μｍのＡｌ２Ｏ３粉末を用意し、さらに５０％粒径：１５μｍのＣｒ粉末を用意した。 Commercially available 50% particle size: 10 μm Co powder, 50% particle size: 15 μm Pt powder, 50% particle size: 5 μm B powder, and 50% particle size: 3 μm SiO as nonmagnetic oxide powder 2 powder, 50% particle size: 3 μm TiO 2 powder, 50% particle size: 3 μm Ta 2 O 5 powder and 50% particle size: 3 μm Al 2 O 3 powder, 50% particle size: 15 μm Cr powder was prepared.
実施例１
さらに、第一ＣｒＣｏ合金粉末としてＣｏ５０Ｃｒ５０合金粉末、第二ＣｏＣｒ合金粉末としてＣｏ８８Ｃｒ１２合金粉末（但し、Ｃｏ５０Ｃｒ５０合金粉末およびＣｏ８８Ｃｒ１２合金粉末の組成比は原子％を示す）をガスアトマイズ法により作製し、これらにＰｔ粉末およびＳｉＯ２粉末を表１に示される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、この容器をボールミルで１２時間回転させることにより混合粉末を作製した。
Example 1
Furthermore, the Co 50 Cr 50 alloy powder as the first CrCo alloy powder and the Co 88 Cr 12 alloy powder as the second CoCr alloy powder (provided that the composition ratio of the Co 50 Cr 50 alloy powder and the Co 88 Cr 12 alloy powder is atomic%. Are prepared by a gas atomization method, and Pt powder and SiO 2 powder are blended so as to have the composition shown in Table 1, and the obtained blended powder is put into a 10-liter container together with zirconia balls as a grinding medium. Then, the atmosphere in the container was replaced with an Ar gas atmosphere, and then the container was sealed, and this container was rotated with a ball mill for 12 hours to produce a mixed powder.
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：１０００℃、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表１に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切削加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより本発明法１を実施し、前記本発明法１で作製したターゲットの面内方向の最大比透磁率を測定し、その結果を表１に示した。 The obtained mixed powder is filled into a vacuum hot press apparatus, and hot press having the component composition shown in Table 1 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. The present invention method 1 was carried out by cutting the hot press body to produce a target having dimensions of diameter: 152.4 mm and thickness: 6 mm. The maximum relative permeability in the in-plane direction of the target was measured, and the result is shown in Table 1.
従来例１
先に用意したＣｏ粉末、Ｐｔ粉末、ＳｉＯ２粉末およびＣｒ粉末を表３に示される割合で配合し、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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表１に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切削加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより従来法１を実施し、従来法１で得られたターゲットの面内方向の最大比透磁率を測定し、その結果を表１に示した。
Conventional example 1
The previously prepared Co powder, Pt powder, SiO 2 powder and Cr powder are blended in the proportions shown in Table 3, and the resulting blended powder is put into a 10 liter container together with zirconia balls as a grinding medium. The atmosphere inside was replaced with an Ar gas atmosphere, and then the container was sealed, and this container was rotated with a ball mill for 12 hours to prepare a mixed powder.
The obtained mixed powder is filled into a vacuum hot press apparatus, and hot press having the component composition shown in Table 1 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. A conventional method 1 is carried out by producing a target and cutting the hot press body to prepare a target having a diameter of 152.4 mm and a thickness of 6 mm. The maximum relative permeability in the in-plane direction was measured and the results are shown in Table 1.
表１に示される結果から、本発明法１で作製したターゲットと従来法１で作製したターゲットを比較すると、得られたターゲットの成分組成は同じであっても、本発明法１で作製したターゲットは従来法１で作製したターゲットよりも面内方向の最大比透磁率が低いことがわかる。 From the results shown in Table 1, when comparing the target prepared by the method 1 of the present invention with the target prepared by the conventional method 1, the target prepared by the method 1 of the present invention was obtained even though the component composition of the obtained target was the same. Shows that the maximum relative permeability in the in-plane direction is lower than that of the target produced by the conventional method 1.
実施例２
第一ＣｏＣｒ粉末としてＣｏ５５Ｃｒ４５合金粉末、第二ＣｏＣｒＢ合金粉末としてＣｏ９０．５Ｃｒ６．０Ｂ３．５合金粉末（但し、Ｃｏ５５Ｃｒ４５合金粉末およびＣｏ９０．５Ｃｒ６．０Ｂ３．５合金粉末の組成比は原子％を示す）をガスアトマイズ法により作製し、これらにＰｔ粉末およびＴｉＯ２粉末を表２に示される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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表２に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切削加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより本発明法２を実施し、前記本発明法２で作製したターゲットの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 55 Cr 45 alloy powder as the first CoCr powder and Co 90.5 Cr 6.0 B 3.5 alloy powder as the second CoCrB alloy powder (provided that Co 55 Cr 45 alloy powder and Co 90.5 Cr 6.0) B 3.5 alloy powder shows atomic%) by a gas atomization method, and Pt powder and TiO 2 powder are blended so as to have the composition shown in Table 2, and the resulting blended powder is obtained. It 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, and the mixed powder is obtained by rotating the container with a ball mill for 12 hours. Produced.
The obtained mixed powder is filled into a vacuum hot press apparatus, and is hot pressed having the component composition shown in Table 2 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. The present invention method 2 was carried out by cutting the hot press body to produce a target having dimensions of diameter: 152.4 mm and thickness: 6 mm. The maximum relative permeability in the in-plane direction of the target was measured, and the result is shown in Table 2.
従来例２
先に用意したＣｏ粉末、Ｐｔ粉末、ＴｉＯ２粉末、Ｂ粉末およびＣｒ粉末を表４に示される割合で配合し、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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表２に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切削加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより従来法２を実施し、前記従来法２で作製したターゲットの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, Pt powder, TiO 2 powder, B powder and Cr powder are blended in the proportions shown in Table 4, and the obtained blended powder is put into a 10 liter container together with zirconia balls as a grinding medium. The atmosphere in the container was replaced with an Ar gas atmosphere, and then the container was sealed, and this container was rotated with a ball mill for 12 hours to prepare a mixed powder.
The obtained mixed powder is filled into a vacuum hot press apparatus, and is hot pressed having the component composition shown in Table 2 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. A conventional method 2 is carried out by cutting the hot-pressed body to produce a target having a diameter of 152.4 mm and a thickness of 6 mm. The maximum relative permeability in the in-plane direction was measured and the results are shown in Table 2.
表２に示される結果から、本発明法２で作製したターゲットと従来法２で作製したターゲットを比較すると、得られたターゲットの成分組成は同じであっても、本発明法２で作製したターゲットは従来法２で作製したターゲットよりも面内方向の最大比透磁率が低いことがわかる。 From the results shown in Table 2, when the target produced by the method 2 of the present invention and the target produced by the conventional method 2 are compared, even if the component composition of the obtained target is the same, the target produced by the method 2 of the present invention Shows that the maximum relative magnetic permeability in the in-plane direction is lower than that of the target produced by the conventional method 2.
実施例３
第一ＣｏＣｒＢ粉末としてＣｏ２８Ｃｒ６５Ｂ７合金粉末、第二ＣｏＣｒ合金粉末としてＣｏ９０Ｃｒ１０合金粉末（但し、Ｃｏ２８Ｃｒ６５Ｂ７合金粉末およびＣｏ９０Ｃｒ１０合金粉末の組成比は原子％を示す）をガスアトマイズ法により作製し、これらにＰｔ粉末およびＴａ２Ｏ５粉末を表３に示される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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表５に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切削加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより本発明法３を実施し、前記本発明法３で作製したターゲットの面内方向の最大比透磁率を測定し、その結果を表３に示した。
Example 3
Co 28 Cr 65 B 7 alloy powder as the first CoCrB powder and Co 90 Cr 10 alloy powder as the second CoCr alloy powder (provided that the composition ratio of the Co 28 Cr 65 B 7 alloy powder and the Co 90 Cr 10 alloy powder is atomic%. Is prepared by a gas atomizing method, and Pt powder and Ta 2 O 5 powder are blended so as to have the composition shown in Table 3, and the obtained blended powder is mixed with 10 liters of zirconia balls as grinding media. The mixture was put into a container, and the atmosphere in the container was replaced with an Ar gas atmosphere. After that, the container was sealed, and this container was rotated with a ball mill for 12 hours to prepare a mixed powder.
The obtained mixed powder is filled into a vacuum hot press apparatus, and hot press having the component composition shown in Table 5 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. The method of the present invention 3 was carried out by cutting the hot-pressed body to produce a target having a diameter of 152.4 mm and a thickness of 6 mm. The maximum relative permeability in the in-plane direction of the target was measured, and the results are shown in Table 3.
従来例３
先に用意したＣｏ粉末、Ｐｔ粉末、Ｔａ２Ｏ５粉末、Ｂ粉末およびＣｒ粉末を表３に示される割合で配合し、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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表３に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより従来法３を実施し、前記従来法３で作製したターゲットの面内方向の最大比透磁率を測定し、その結果を表３に示した。
Conventional example 3
The previously prepared Co powder, Pt powder, Ta 2 O 5 powder, B powder and Cr powder were blended in the proportions shown in Table 3, and the resulting blended powder was placed in a 10 liter container together with zirconia balls serving as grinding media. Then, the atmosphere in the container was replaced with an Ar gas atmosphere, and then the container was sealed, and this container was rotated with a ball mill for 12 hours to prepare a mixed powder.
The obtained mixed powder is filled into a vacuum hot press apparatus, and hot press having the component composition shown in Table 3 by vacuum hot pressing in a vacuum atmosphere under the conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. A conventional method 3 is carried out by cutting the hot-pressed body to produce a target having a diameter of 152.4 mm and a thickness of 6 mm. The maximum relative permeability in the in-plane direction was measured, and the results are shown in Table 3.
表３に示される結果から、本発明法３で作製したターゲットと従来法３で作製したターゲットを比較すると、得られたターゲットの成分組成は同じであっても、本発明法３で作製したターゲットは従来法３で作製したターゲットよりも面内方向の最大比透磁率が低いことがわかる。 From the results shown in Table 3, when the target produced by the method 3 of the present invention and the target produced by the conventional method 3 were compared, the target produced by the method 3 of the present invention was obtained even though the component composition of the obtained target was the same. Shows that the maximum relative magnetic permeability in the in-plane direction is lower than that of the target produced by the conventional method 3.
実施例４
第一ＣｏＣｒＢ粉末としてＣｏ４１Ｃｒ５５Ｂ４合金粉末、第二ＣｏＣｒＢ合金粉末としてＣｏ８７Ｃｒ６Ｂ７合金粉末（但し、Ｃｏ４１Ｃｒ５５Ｂ４合金粉末およびＣｏ８７Ｃｒ６Ｂ７合金粉末の組成比は原子％を示す）をガスアトマイズ法により作製し、これらにＰｔ粉末並びにＡｌ２Ｏ３粉末を表４に示される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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表４に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切削加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより本発明法４を実施し、前記本発明法４で作製したターゲットの面内方向の最大比透磁率を測定し、その結果を表４に示した。
Example 4
Co 41 Cr 55 B 4 alloy powder as the first CoCrB powder and Co 87 Cr 6 B 7 alloy powder as the second CoCrB alloy powder (provided that the composition of the Co 41 Cr 55 B 4 alloy powder and the Co 87 Cr 6 B 7 alloy powder is The ratio is atomic%) is prepared by a gas atomizing method, and Pt powder and Al 2 O 3 powder are blended so as to have the composition shown in Table 4, and the resulting blended powder is used as a grinding medium. The mixture was put into a 10-liter container, and the atmosphere in the container was replaced with an Ar gas atmosphere. Thereafter, the container was sealed, and this container was rotated with a ball mill for 12 hours to prepare a mixed powder.
The obtained mixed powder is filled into a vacuum hot press apparatus, and hot press having the component composition shown in Table 4 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. The present invention method 4 was carried out by cutting the hot press body to produce a target having dimensions of diameter: 152.4 mm and thickness: 6 mm. The maximum relative permeability in the in-plane direction of the target was measured, and the result is shown in Table 4.
従来例４
先に用意したＣｏ粉末、Ｐｔ粉末、Ａｌ２Ｏ３粉末、Ｂ粉末およびＣｒ粉末を表４に示される割合で配合し、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、この容器をボールミルで１２時間回転させることにより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：１０００℃、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表４に示される成分組成を有するホットプレス体を作製し、このホットプレス体を切加工して直径：１５２．４ｍｍ、厚さ：６ｍｍの寸法を有するターゲットを作製することにより従来法４を実施し、前記従来法４で作製したターゲットの面内方向の最大比透磁率を測定し、その結果を表４に示した。
Conventional example 4
The previously prepared Co powder, Pt powder, Al 2 O 3 powder, B powder and Cr powder are blended in the proportions shown in Table 4, and the resulting blended powder is placed in a 10 liter container together with zirconia balls as a grinding medium. Then, the atmosphere in the container was replaced with an Ar gas atmosphere, and then the container was sealed, and this container was rotated with a ball mill for 12 hours to prepare a mixed powder.
The obtained mixed powder is filled into a vacuum hot press apparatus, and hot press having the component composition shown in Table 4 by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1000 ° C., pressure: 35 MPa, and 3 hours. A conventional method 4 is carried out by cutting the hot pressed body to produce a target having a diameter of 152.4 mm and a thickness of 6 mm. The maximum relative permeability in the in-plane direction was measured and the results are shown in Table 4.
表４に示される結果から、本発明法４で作製したターゲットと従来法４で作製したターゲットを比較すると、得られたターゲットの成分組成は同じであっても、本発明法４で作製したターゲットは従来法４で作製したターゲットよりも面内方向の最大比透磁率が低いことがわかる。 From the results shown in Table 4, when the target produced by the method 4 of the present invention and the target produced by the conventional method 4 are compared, even if the component composition of the obtained target is the same, the target produced by the method 4 of the present invention Shows that the maximum relative permeability in the in-plane direction is lower than that of the target produced by the conventional method 4.
Claims (4)
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、混合したのち加圧焼結することを特徴とする比透磁率の低い磁気記録膜形成用Ｃｏ基焼結合金スパッタリングターゲットの製造方法。 A first CoCr alloy powder having a component composition containing Cr: 50 to 70 atomic% and the balance being made of Co, and a second CoCr alloy having a composition composition of Cr: 5 to 15 atomic% and the balance being made of Co Powder, Pt powder and non-magnetic oxide powder,
Nonmagnetic oxide: 0.5 to 15 mol%, Cr: 4 to 20 mol%, Pt: 5 to 25 mol%, with the balance being a component composition consisting of Co and inevitable impurities, mixed and mixed A method for producing a Co-based sintered alloy sputtering target for forming a magnetic recording film having a low relative magnetic permeability, which is then subjected to pressure sintering.
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| JP2011021254A (en) * | 2009-07-16 | 2011-02-03 | Solar Applied Materials Technology Corp | Method for producing boron-containing sputtering target, thin film and magnetic recording medium |
| CN105256174A (en) * | 2015-10-22 | 2016-01-20 | 东北大学 | Biotic bone composite material and preparing method thereof |
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| JP2000282229A (en) * | 1999-03-29 | 2000-10-10 | Hitachi Metals Ltd | CoPt SPUTTERING TARGET, ITS PRODUCTION, MAGNETIC RECORDING FILM AND CoPt MAGNETIC RECORDING MEDIUM |
| WO2007116834A1 (en) * | 2006-03-31 | 2007-10-18 | Mitsubishi Materials Corporation | METHOD FOR MANUFACTURING Co-BASE SINTERED ALLOY SPUTTERING TARGET FOR FORMATION OF MAGNETIC RECORDING FILM WHICH IS LESS LIKELY TO GENERATE PARTICLES, AND Co-BASE SINTERED ALLOY SPUTTERING TARGET FOR FORMATION OF MAGNETIC RECORDING FILM |
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| JPH04297572A (en) * | 1991-03-26 | 1992-10-21 | Hitachi Metals Ltd | Co-cr-pt series target for magnetic recording medium |
| JP2000038661A (en) * | 1998-07-21 | 2000-02-08 | Hitachi Metals Ltd | Co ALLOY TARGET, ITS PRODUCTION, APPARATUS FOR SPUTTERING, MAGNETIC RECORDING FILM AND DEVICE FOR MAGNETIC RECORDING |
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| JP2011021254A (en) * | 2009-07-16 | 2011-02-03 | Solar Applied Materials Technology Corp | Method for producing boron-containing sputtering target, thin film and magnetic recording medium |
| CN105256174A (en) * | 2015-10-22 | 2016-01-20 | 东北大学 | Biotic bone composite material and preparing method thereof |
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