JP2008095149A - Sputtering target for forming film of high-density magnetic recording medium while causing few particles - Google Patents
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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、特に高密度垂直磁気記録方式の媒体に用いられる磁気記録膜を形成するためのパーティクル発生の少ない高密度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 magnetic recording film applied to a high-density magnetic recording medium of a hard disk, particularly a high-density magnetic recording medium film generation with less particles for forming a magnetic recording film used for a medium of a high-density perpendicular magnetic recording system. The present invention relates to a sputtering target for use.
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高密度磁気記録方式が注目されてきた。この高密度磁気記録方式は、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、すでに実用化が開始されている。この高密度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一つとしてＣｏＣｒＰｔ−ＴｉＯ２グラニュラ磁気記録膜が使用されており、このＣｏＣｒＰｔ−ＴｉＯ２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チタン相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法により作製することが知られている。
このスパッタリングターゲットは、市販のＣｒおよびＰｔを含むＣｏ基合金粉末または急冷凝固して作製したＣｒおよびＰｔを含むＣｏ基合金粉末と二酸化チタン粉末を、二酸化チタン：２〜１５モル％、Ｃｒ：２〜２０モル％、Ｐｔ：４〜３０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、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。そして、このターゲットは、素地中にＴｉＯ２が均一分散している組織を有している（特許文献１、特許文献２などを参照）。さらに、一般に、ターゲットの密度が高く真密度に近い焼結体からなるターゲットほどスパッタリングに際してパーティクルの発生が少なくなることも知られている。
This sputtering target is composed of a commercially available Co-based alloy powder containing Cr and Pt or a Co-based alloy powder containing Cr and Pt produced by rapid solidification and titanium dioxide powder, titanium dioxide: 2 to 15 mol%, Cr: 2 It is known that it is prepared by blending and mixing so as to have a composition consisting of ˜20 mol%, Pt: 4-30 mol%, and the balance: Co, and then vacuum hot pressing or hot isostatic pressing. It has been. The target has a structure in which TiO 2 is uniformly dispersed in the substrate (see Patent Document 1, Patent Document 2, and the like). Furthermore, it is generally known that a target made of a sintered body having a high target density and close to a true density reduces the generation of particles during sputtering.
しかし、従来の素地中に二酸化チタンを均一分散させた磁気記録媒体膜形成用スパッタリングターゲットは、マグネトロンスパッタリングを行なうに際し、パーティクルが多く発生することから、パーティクル発生の少ない磁気記録媒体膜形成用スパッタリングターゲットが求められていた。 However, a conventional sputtering target for forming a magnetic recording medium film in which titanium dioxide is uniformly dispersed in a base material generates many particles when performing magnetron sputtering. Was demanded.
そこで、本発明者らは、マグネトロンスパッタリングを行なうに際し、パーティクル発生の少ない磁気記録媒体膜形成用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、
（ａ）酸素：０．５〜４０原子％、Ｃｒ：２〜２０原子％、Ｐｔ：４〜３０原子％、Ｔｉ：０．５〜２０原子％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焼結体からなる高密度磁気記録媒体膜形成用スパッタリングターゲットにおいて、Ｃｒ、Ｔｉおよび酸素からなる酸化物粒子を素地中に均一分散させたターゲットは、マグネトロンスパッタリングに際しパーティクルの発生が格段に少なくなる
（ｂ）前記Ｃｒ、Ｔｉおよび酸素からなる酸化物粒子は、Ｃｒ、Ｔｉおよび酸素の合計を１００原子％とした場合、Ｃｒ：３〜１０原子％、Ｔｉ：２５〜３５原子％を含有し、残部が酸素からなる酸化物粒子である、
（ｃ）前記素地中に均一分散しているＣｒ、Ｔｉおよび酸素からなる酸化物粒子は微細であるほど好ましく、絶対最大長（粒子の輪郭線上の任意の２点間の距離の最大値）が２５μｍを超える酸化物粒子数が５％以下の粒度分布を有することが好ましい、
（ｄ）前記高密度磁気記録媒体膜形成用スパッタリングターゲットは、前記焼結体の密度が理論密度に近いほど好ましく、相対密度が９５％以上を有する焼結体からなることがいっそう好ましい、などの知見を得たのである。
Accordingly, the present inventors have studied to obtain a sputtering target for forming a magnetic recording medium film with less generation of particles when performing magnetron sputtering. as a result,
(A) Oxygen: 0.5 to 40 atomic%, Cr: 2 to 20 atomic%, Pt: 4 to 30 atomic%, Ti: 0.5 to 20 atomic%, balance: Co and inevitable impurities In a sputtering target for forming a high-density magnetic recording medium film composed of a sintered body having a component composition, a target in which oxide particles composed of Cr, Ti and oxygen are uniformly dispersed in a substrate has a remarkable generation of particles during magnetron sputtering. (B) The oxide particles composed of Cr, Ti, and oxygen have a Cr: 3-10 atomic%, Ti: 25-35 atomic% when the total of Cr, Ti, and oxygen is 100 atomic%. Containing oxide particles with the balance being oxygen,
(C) The finer the oxide particles consisting of Cr, Ti and oxygen that are uniformly dispersed in the substrate, the more preferably the absolute maximum length (the maximum value of the distance between any two points on the particle outline). The number of oxide particles exceeding 25 μm preferably has a particle size distribution of 5% or less.
(D) The high-density magnetic recording medium film-forming sputtering target is preferably such that the density of the sintered body is closer to the theoretical density, more preferably a sintered body having a relative density of 95% or more. I gained knowledge.
この発明は、かかる知見に基づいてなされたものであって、
（１）酸素：０．５〜４０原子％、Ｃｒ：２〜２０原子％、Ｐｔ：４〜３０原子％、Ｔｉ：０．５〜２０原子％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焼結体からなるターゲットにおいて、前記ターゲット素地中にＣｒ、Ｔｉおよび酸素からなる酸化物粒子が均一分散している組織を有しており、前記Ｃｒ、Ｔｉおよび酸素からなる酸化物粒子は、Ｃｒ、Ｔｉおよび酸素の合計を１００原子％とした場合、Ｃｒ：３〜１０原子％、Ｔｉ：２５〜３５原子％を含有し、残部が酸素からなる酸化物粒子であるパーティクル発生の少ない高密度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Ｃｒ、Ｔｉおよび酸素からなる酸化物粒子は、絶対最大長が２５μｍを超える酸化物粒子数が５％以下の粒度分布を有する前記（１）記載のパーティクル発生の少ない高密度磁気記録媒体膜形成用スパッタリングターゲット、
（３）前記焼結体は相対密度が９５％以上を有する焼結体である前記（１）または（２）記載のパーティクル発生の少ない高密度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。
なお、前記（３）記載の焼結体の相対密度は、焼結体の嵩密度を理論密度で割って１００をかけた値であり、焼結体の理論密度は、各元素、分子が均一に混合し、反応、拡散などが起こらないものと仮定して以下のようにして計算した値である。すなわち、焼結体の組成がＣｏａＣｒｂＰｔｃ（ＴｉＯ２）ｄ（ａ，ｂ，ｃ，ｄは重量％）と表されるとき、焼結体の理論密度ρｔは、
ρｔ＝１００／（ａ／ρＣｏ＋ｂ／ρＣｒ＋ｃ／ρＰｔ＋ｄ／ρＴｉＯ２）（ここでρＣｏ＝８．９２、ρＣｒ＝７．１９、ρＰｔ＝２１．４５、ρＴｉＯ２＝４．２５でこれらは各元素、酸化物の理論密度である）で求められる。
したがって、焼結体の相対密度Ｒは、焼結体の嵩密度ρと理論密度ρｔからＲ＝ρ／ρｔ×１００により求められる。
This invention has been made based on such knowledge,
(1) Oxygen: 0.5 to 40 atom%, Cr: 2 to 20 atom%, Pt: 4 to 30 atom%, Ti: 0.5 to 20 atom%, balance: Co and inevitable impurities In the target composed of a sintered body having a component composition, the target substrate has a structure in which oxide particles composed of Cr, Ti and oxygen are uniformly dispersed, and the oxide composed of Cr, Ti and oxygen When the total of Cr, Ti and oxygen is 100 atomic%, the particles contain Cr: 3 to 10 atomic%, Ti: 25 to 35 atomic%, and the remainder is oxide particles composed of oxygen. A sputtering target for forming a low-density magnetic recording medium film,
(2) The oxide particles comprising Cr, Ti, and oxygen have a particle size distribution in which the number of oxide particles having an absolute maximum length exceeding 25 μm is 5% or less, and high density magnetic recording with less generation of particles according to (1). Sputtering target for medium film formation,
(3) The sintered body is characterized by the sputtering target for forming a high-density magnetic recording medium film with less generation of particles according to (1) or (2), wherein the sintered body has a relative density of 95% or more. Is.
The relative density of the sintered body described in (3) above is a value obtained by dividing the bulk density of the sintered body by the theoretical density and multiplying by 100. The theoretical density of the sintered body is uniform for each element and molecule. It is a value calculated as follows assuming that no reaction or diffusion occurs. That is, when the composition of the sintered body is expressed as Co a Cr b Pt c (TiO 2 ) d (where a, b, c, and d are weight%), the theoretical density ρ t of the sintered body is
ρ t = 100 / (a / ρ Co + b / ρ Cr + c / ρ Pt + d / ρ TiO2 ) (where ρ Co = 8.92, ρ Cr = 7.19, ρ Pt = 21.45, ρ TiO2 = 4.25, these are the theoretical densities of each element and oxide).
Therefore, the relative density R of the sintered body is obtained by R = ρ / ρ t × 100 from the bulk density ρ and the theoretical density ρ t of the sintered body.
この発明のパーティクル発生の少ない高密度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粉末、Ｐｔ粉末、Ｃｒ粉末、ＴｉＯ２粉末を用意し、まず、Ｃｒ粉末の一部とＴｉＯ２粉末をボールミルで混合し、得られた混合粉末を真空中、８００〜１３００℃の温度にて熱処理後、粉砕することによりＣｒ、Ｔｉおよび酸素の合計を１００原子％とした場合、Ｃｒ：３〜１０原子％、Ｔｉ：２５〜３５原子％を含み、残部が酸素からなる酸化物粉末を作製し、この酸化物粉末にＣｏ粉末、Ｐｔ粉末およびＣｒ粉末を酸素：０．５〜４０原子％、Ｃｒ：２〜２０原子％、Ｐｔ：４〜３０原子％、Ｔｉ：０．５〜２０原子％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ように配合し、混合して混合粉末を作製し、得られた混合粉末を温度：１０００〜１２５０℃、圧力：１５０ＭＰａ以上、１時間以上保持することにより作製することができる。 In order to manufacture the sputtering target for forming a high density magnetic recording medium film with less generation of particles according to the present invention, Co powder, Pt powder, Cr powder, TiO 2 powder are prepared as raw powders. When TiO 2 powder is mixed with a ball mill, and the obtained mixed powder is heat-treated in a vacuum at a temperature of 800 to 1300 ° C. and then pulverized to make the total of Cr, Ti, and oxygen 100 atomic%, Cr: An oxide powder containing 3 to 10 atom%, Ti: 25 to 35 atom%, and the balance being oxygen is prepared. Co oxide, Pt powder and Cr powder are added to this oxide powder with oxygen of 0.5 to 40 atoms. %, Cr: 2 to 20 atomic%, Pt: 4 to 30 atomic%, Ti: 0.5 to 20 atomic%, and the balance: a component composition consisting of Co and inevitable impurities Mixing a mixed powder prepared, obtained mixed powder temperature: 1000 to 1250 ° C., pressure: 150 MPa or more, can be prepared by holding over 1 hour.
この発明のパーティクル発生の少ない高密度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均一分散しているＣｒ、Ｔｉおよび酸素からなる酸化物粒子に含まれるＣｒの含有量を、Ｃｒ、Ｔｉおよび酸素の合計を１００原子％とした場合、Ｃｒ：３〜１０原子％とした理由は、Ｃｒが３原子％未満ではパーティクルの発生数が多くなるので好ましくなく、一方、１０原子％を越えると得られたスパッタリング膜の磁気特性が低下するので好ましくない理由によるものである。
また、Ｔｉ：２５〜３５原子％とした理由は、Ｔｉが２５原子％未満ではスパッタリング膜の磁気特性が低下するので好ましくなく、一方、Ｔｉが３５原子％を越えると、パーティクルの発生数が多くなるので好ましくないからである。
ターゲット中に分散させる酸化物粒子をＴｉＯ２からＣｒとＴｉを含む酸化物とすることによりパーティクルの発生が少なくなる理由は、酸化物粒子がＣｒを含むことにより、母相であるＣｒを含有するＣｏ合金との密着性が改善され、酸化物粒子がスパッタ中に剥離、脱落しにくくなるためと推測される。
そして、ターゲットの素地中に均一分散しているＣｒ、Ｔｉおよび酸素からなる酸化物粒子は微細な粒子で分散しているほど好ましく、絶対最大長が２５μｍを超える酸化物粒子数が５％以下であることが好ましい。絶対最大長が２５μｍを超える酸化物粒子数が５％を超えると粒径の大きな酸化物粒子が多くなりすぎてパーティクルの発生が多くなるので好ましくないからである。
The content of Cr contained in oxide particles composed of Cr, Ti and oxygen uniformly dispersed in the base material of the sputtering target for forming a high-density magnetic recording medium film with less generation of particles of the present invention is expressed by Cr, Ti and oxygen. In the case where the total amount of Cr is 100 atomic%, the reason for Cr: 3 to 10 atomic% is not preferable because the number of particles generated increases if Cr is less than 3 atomic%. This is because the magnetic properties of the sputtered film deteriorate, which is not preferable.
Moreover, the reason for Ti: 25 to 35 atomic% is not preferable if Ti is less than 25 atomic%, because the magnetic properties of the sputtering film deteriorate. On the other hand, if Ti exceeds 35 atomic%, the number of particles generated is large. This is because it is not preferable.
The reason why the generation of particles is reduced by changing the oxide particles dispersed in the target from TiO 2 to an oxide containing Cr and Ti is that the oxide particles contain Cr and contain Cr as a mother phase. It is presumed that the adhesion with the Co alloy is improved and the oxide particles are less likely to be peeled off and dropped off during sputtering.
The oxide particles composed of Cr, Ti and oxygen uniformly dispersed in the target substrate are preferably dispersed as fine particles, and the number of oxide particles having an absolute maximum length exceeding 25 μm is 5% or less. Preferably there is. This is because if the number of oxide particles having an absolute maximum length exceeding 25 μm exceeds 5%, the number of oxide particles having a large particle diameter increases and the generation of particles increases, which is not preferable.
なお、高密度磁気記録媒体膜形成用スパッタリングターゲットの成分組成として、酸素：０．５〜４０原子％、Ｃｒ：２〜２０原子％、Ｐｔ：４〜３０原子％、Ｔｉ：０．５〜２０原子％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ことはすでに知られている成分組成であるので、その限定理由の説明は省略する。 In addition, as a component composition of the sputtering target for high-density magnetic recording medium film formation, oxygen: 0.5-40 atomic%, Cr: 2-20 atomic%, Pt: 4-30 atomic%, Ti: 0.5-20 Since it is already known to have a component composition containing atomic% and the balance: Co and unavoidable impurities, description of the limitation reason is omitted.
この発明の高密度磁気記録媒体膜形成用スパッタリングターゲットは、マグネトロンスパッタリングに際してパーティクルの発生が少なくなるので、高密度磁気記録媒体膜の不良品を少なくすることができ、コストを削減することができて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 sputtering target for forming a high-density magnetic recording medium film of the present invention reduces the generation of particles during magnetron sputtering, thereby reducing the number of defective high-density magnetic recording medium films and reducing the cost. It can greatly contribute to the development of industries such as computers and digital home appliances.
実施例
原料粉末として、市販の５０％粒径：６μｍのＣｏ粉末、５０％粒径：２０μｍのＰｔ粉末、５０％粒径：３０μｍのＣｒ粉末、５０％粒径：３μｍのＴｉＯ２粉末を用意した。
さらに前記Ｃｒ粉末の一部とＴｉＯ２粉末をボールミルで混合し、得られた混合粉末を真空中、１０００℃の温度にて２４時間加熱の熱処理を行なったのち、さらに粉砕することにより、表１に示される成分組成および粒度を有する酸化物粉末Ａ〜Ｋを作製し用意した。
Example Commercially available 50% particle size: 6 μm Co powder, 50% particle size: 20 μm Pt powder, 50% particle size: 30 μm Cr powder, 50% particle size: 3 μm TiO 2 powder as raw material powder did.
Further, a part of the Cr powder and TiO 2 powder were mixed with a ball mill, and the obtained mixed powder was heat-treated at 1000 ° C. for 24 hours in a vacuum, and then further pulverized. The oxide powders A to K having the component composition and particle size shown in FIG.
これら用意した原料粉末を表２に示される割合で配合し、得られた配合粉末を酸化ジルコニウムのボールとともに１０リットルの容器に投入し、この容器の雰囲気をＡｒガスで置換したのち容器を密封した。この容器を１６時間ボールミルにより回転させ、混合することにより混合粉末を作製し、この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：１２００℃、圧力：１５ＭＰａ、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加工により直径：１５２．４ｍｍ、厚さ：５ｍｍの板にしたのち、銅製のバッキングプレートに接合し、本発明ターゲット１〜１０および比較ターゲット１〜３を作製した。
These prepared raw material powders were blended in the proportions shown in Table 2, and the obtained blended powder was put into a 10-liter container together with zirconium oxide balls, and the atmosphere of this container was replaced with Ar gas, and then the container was sealed. . This container is rotated by a ball mill for 16 hours and mixed to prepare a mixed powder, and this mixed powder is filled in a vacuum hot press apparatus, and is maintained in a vacuum atmosphere at a temperature of 1200 ° C., a pressure of 15 MPa, and a 3 hour holding condition. A plate-like hot press body having the component composition shown in Table 2 was produced by vacuum hot pressing.
The plate-like hot press body was cut into a plate having a diameter of 152.4 mm and a thickness of 5 mm, and then joined to a copper backing plate to prepare the inventive targets 1 to 10 and comparative targets 1 to 3.
従来例
さらに、実施例で用意したＣｏ粉末、Ｐｔ粉末、Ｃｒ粉末、ＴｉＯ２粉末を表２に示される割合で配合し、酸化ジルコニウムのボールとともに１０リットルの容器に投入し、この容器の雰囲気をＡｒガスで置換したのち容器を密封した。この容器を１６時間ボールミルにより回転させ、混合することにより混合粉末を作製した。このようにして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：１２００℃、圧力：１５ＭＰａ、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板状ホットプレス体を作製し、この板状ホットプレス体の相対密度を測定し、その結果を表２に示した。次に、この板状ホットプレス体を切削加工により直径：１５２．４ｍｍ、厚さ：５ｍｍの板にしたのち、銅製のバッキングプレートに接合し、従来ターゲットを作製した。
Conventional Example Furthermore, Co powder, Pt powder, Cr powder, and TiO 2 powder prepared in the examples were blended in the proportions shown in Table 2, and put into a 10 liter container together with zirconium oxide balls. After replacing with Ar gas, the container was sealed. The container was rotated by a ball mill for 16 hours and mixed to prepare a mixed powder. The mixed powder obtained in this way was filled into a vacuum hot press apparatus, and the component composition shown in Table 2 was obtained by vacuum hot pressing in a vacuum atmosphere under conditions of temperature: 1200 ° C., pressure: 15 MPa, and 3 hours. A plate-like hot press body having a thickness of 10 was prepared, and the relative density of the plate-like hot press body was measured. The results are shown in Table 2. Next, this plate-like hot press body was cut into a plate having a diameter of 152.4 mm and a thickness of 5 mm, and then joined to a copper backing plate to produce a conventional target.
このようにして作製した本発明ターゲット１〜１０、比較ターゲット１〜３および従来ターゲットの相対密度（＝嵩密度／理論密度×１００）を測定し、その結果を表２に示した。さらにこれら本発明ターゲット１〜１０、比較ターゲット１〜３および従来ターゲットの一部を切断し、これを樹脂に埋め込み、研磨し、この研磨面を走査電子顕微鏡（ＳＥＭ）により断面組織観察を行い、断面から１０００倍の倍率で無作為に１０箇所選んでＳＥＭ写真（ＣＯＭＰＯ像）を撮影し、このＳＥＭ写真を画質を落とさないようにパソコンにビットマップ形式の画像ファイルとして取り込み、この画像を別途画像処理ソフト（三谷商事社製、Ｗｉｎ Ｒｏｏｆ）に読み込んで二値化し、ＳＥＭ写真において黒く写っているすべての酸化物粒子について、絶対最大長を計測した。二値化の際の条件は元の酸化物粒子の形状にできるだけ近くなるように注意した。計測時の長さのキャリブレーションについてはＳＥＭ像のスケールバーを使用した。計測されたすべての酸化物粒子の絶対最大長を統計処理し、２５μｍ以上の粒子の割合を測定し、その結果を表２に示した。
さらに、素地中に均一分散している酸化物粒子の成分組成についてフィールドエミッションＥＰＭＡ（日本電子社製ＪＸＡ−８５００Ｆ）により、加速電圧：１５ｋＶ、照射電流：５×１０−８Ａ、分析スポット径の設定値：０（実質的な電子線径は約０．５μｍ）の条件にてＣｒ、Ｔｉ、Ｏの組成定量分析を行い、その結果を表２に示した。
The relative densities (= bulk density / theoretical density × 100) of the inventive targets 1 to 10, the comparative targets 1 to 3 and the conventional target thus prepared were measured, and the results are shown in Table 2. Further, the present invention targets 1 to 10, the comparative targets 1 to 3 and a part of the conventional target are cut, embedded in resin, polished, and the polished surface is observed with a scanning electron microscope (SEM). Take 10 SEM photographs (COMPO images) at random from the cross section at a magnification of 1000 times, and import these SEM photographs as bitmap format image files into a personal computer so as not to degrade the image quality. The absolute maximum length was measured for all the oxide particles that were read and binarized by the processing software (Mitani Corporation, Win Roof) and black in the SEM photograph. Care was taken that the binarization conditions were as close as possible to the shape of the original oxide particles. For calibration of the length at the time of measurement, a scale bar of an SEM image was used. The absolute maximum lengths of all the measured oxide particles were statistically processed and the proportion of particles of 25 μm or more was measured. The results are shown in Table 2.
Further, the component composition of the oxide particles uniformly dispersed in the substrate was subjected to field emission EPMA (JXA-8500F manufactured by JEOL Ltd.), acceleration voltage: 15 kV, irradiation current: 5 × 10 −8 A, analysis spot diameter The composition quantitative analysis of Cr, Ti, and O was performed under the condition of set value: 0 (substantially electron beam diameter is about 0.5 μm), and the results are shown in Table 2.
これら本発明ターゲット１〜１０、比較ターゲット１〜３および従来ターゲットを市販のスパッタリング装置に装着し、
到達真空度：＜５×１０−５Ｐａ、
電力：直流８００Ｗ、
Ａｒガス：６．０Ｐａ、
ターゲット−基板間距離：６０ｍｍ、
基板加熱：なし、
の条件で５時間プレスパッタを行い、ターゲット表面の表面加工層を除去したのち、一旦チャンバーを開放して防着板などのチャンバー部材の清掃を行い、その後、再び上記真空度に達するまで真空引きを行なった。真空引き後、３０分のプレスパッタを行なって、ターゲット表面の大気吸着成分や金属酸化層の除去を行なった後、４インチＳｉウエハ上に高密度磁気記録媒体膜を成膜した。成膜後、のウエハについて市販の異物検査装置によりウエハ表面に付着した１μｍ以上のパーティクルの数を計測し、その結果を表２に示した。
These inventive targets 1 to 10, comparative targets 1 to 3 and conventional targets are mounted on a commercially available sputtering apparatus,
Ultimate vacuum: <5 × 10 −5 Pa,
Power: DC 800W,
Ar gas: 6.0 Pa,
Target-substrate distance: 60 mm,
Substrate heating: None,
Pre-sputtering is performed for 5 hours under the conditions described above, and after removing the surface processing layer on the target surface, the chamber is once opened to clean the chamber members such as the deposition prevention plate, and then the vacuum is drawn until the above vacuum degree is reached again. Was done. After evacuation, pre-sputtering was performed for 30 minutes to remove the atmospheric adsorption components and the metal oxide layer on the target surface, and then a high-density magnetic recording medium film was formed on a 4-inch Si wafer. After the film formation, the number of particles of 1 μm or more adhering to the wafer surface was measured with a commercially available foreign substance inspection apparatus, 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１〜１０は、従来ターゲットに比べて、スパッタリングに際してパーティクルの発生が格段に少ないことが分かる。しかし、この発明の範囲から外れた条件の比較法１〜３で作製したターゲットはパーティクルの発生がやや多くなるのでなどして好ましくないことが分かる。 From the results shown in Table 2, it can be seen that the targets 1 to 10 of the present invention generate significantly fewer particles during sputtering than the conventional target. However, it can be seen that the target produced by Comparative Methods 1 to 3 under conditions outside the scope of the present invention is not preferable because the generation of particles is slightly increased.
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| JP2012252768A (en) * | 2011-05-09 | 2012-12-20 | Mitsubishi Materials Corp | Sputtering target for magnetic recording medium film formation and manufacturing method thereof |
| JP2013033581A (en) * | 2011-07-05 | 2013-02-14 | Mitsubishi Materials Corp | Sputtering target for magnetic recording medium film formation and method of manufacturing the same |
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| JP2001236643A (en) * | 2000-02-23 | 2001-08-31 | Fuji Electric Co Ltd | Sputtering target for manufacturing magnetic recording medium, method of manufacturing magnetic recording medium by using the same, and magnetic recording medium |
| JP2001250222A (en) * | 2000-03-01 | 2001-09-14 | Hitachi Ltd | Magnetic recording medium, its producing method and magnetic recorder using the method |
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| JP2001250222A (en) * | 2000-03-01 | 2001-09-14 | Hitachi Ltd | Magnetic recording medium, its producing method and magnetic recorder using the method |
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| JP2012252768A (en) * | 2011-05-09 | 2012-12-20 | Mitsubishi Materials Corp | Sputtering target for magnetic recording medium film formation and manufacturing method thereof |
| JP2013033581A (en) * | 2011-07-05 | 2013-02-14 | Mitsubishi Materials Corp | Sputtering target for magnetic recording medium film formation and method of manufacturing the same |
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