TW201510238A - Sputtering target for magnetic recording medium - Google Patents

Sputtering target for magnetic recording medium Download PDF

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TW201510238A
TW201510238A TW103117278A TW103117278A TW201510238A TW 201510238 A TW201510238 A TW 201510238A TW 103117278 A TW103117278 A TW 103117278A TW 103117278 A TW103117278 A TW 103117278A TW 201510238 A TW201510238 A TW 201510238A
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powder
target
particle diameter
average particle
sputtering target
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TWI593808B (en
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Atsushi Sato
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Jx Nippon Mining & Metals Corp
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0466—Alloys based on noble metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%

Abstract

A sintered-body sputtering target having as the main components an L10-type ordered-lattice Fe-Pt alloy and a non-magnetic material, the sputtering target being characterized in containing Co and/or Ni in an amount of 0.05 to 0.5%, expressed as the ratio of the number of atoms in the metal component of the sputtering target. The present invention addresses the problem of providing a sputtering target comprising a non-magnetic material and an Fe-Pt-based alloy in which the amount of particles generated during sputtering is significantly reduced.

Description

磁記錄媒體用濺鍍靶 Sputter target for magnetic recording media

本發明係關於一種用於形成磁記錄媒體中之磁性薄膜的濺鍍靶。 The present invention relates to a sputtering target for forming a magnetic thin film in a magnetic recording medium.

於硬碟驅動機所代表之磁記錄領域，磁記錄媒體之磁性薄膜的材料，一直使用以強磁性金屬Co、Fe或Ni作為基底之材料。例如，於採用水平磁記錄方式之硬碟的磁性薄膜，係使用以Co作為主成分之Co-Cr系或Co-Cr-Pt系的強磁性合金。 In the field of magnetic recording represented by a hard disk drive machine, a material of a magnetic film of a magnetic recording medium has been mainly made of a material having a ferromagnetic metal Co, Fe or Ni as a base. For example, a magnetic film of a hard disk using a horizontal magnetic recording method is a Co-Cr-based or Co-Cr-Pt-based ferromagnetic alloy containing Co as a main component.

又，採用近年來已實用化之垂直磁記錄方式之硬碟的磁性薄膜，多使用由主成分為Co之Co-Cr-Pt系強磁性合金與氧化物構成的複合材料。而且，由於生產性高，上述磁性薄膜大多係以磁控濺鍍裝置對以上述材料作為成分之濺鍍靶進行濺鍍來製作。 Further, a magnetic material of a hard disk having a perpendicular magnetic recording method which has been put into practical use in recent years is often a composite material composed of a Co-Cr-Pt-based ferromagnetic alloy having a main component of Co and an oxide. Further, since the magnetic properties are high, the magnetic thin film is often produced by sputtering a sputtering target having the above-mentioned material as a component by a magnetron sputtering apparatus.

另一方面，硬碟之記錄密度逐年迅速的增大，正在超越1Tbit/in2。若記錄密度達到1Tbit/in2，則記錄bit之尺寸會低於10nm，可預料於該情形時由熱波動所引起之超順磁性化將成為問題。且可預料就現在所使用之磁記錄媒體的材料例如於Co基合金添加Pt以提高結晶磁異向性的材料而言並不足夠。其原因在於：尺寸在10nm以下穩定地以強磁性動作之磁性粒子需具有更高之結晶磁異向性。 On the other hand, the recording density of hard disks has increased rapidly year by year, surpassing 1Tbit/in 2 . If the recording density reaches 1 Tbit/in 2 , the size of the recording bit will be less than 10 nm, and it is expected that superparamagnetization caused by thermal fluctuations in this case will become a problem. It is also expected that the material of the magnetic recording medium used today, for example, a material in which Pt is added to a Co-based alloy to increase crystal magnetic anisotropy is not sufficient. The reason for this is that magnetic particles which are stably magnetized with a size of 10 nm or less are required to have higher crystal magnetic anisotropy.

由於上述理由，具有L10結構之Fe-Pt合金作為超高密度記 錄媒體用材料而受到注意。具有L10結構之Fe-Pt合金不僅具有高的結晶磁異向性，且耐蝕性、抗氧化性優異，因此被期待為適合應用作為磁記錄媒體的材料。 For the above reasons, an Fe-Pt alloy having an L1 0 structure has been attracting attention as a material for an ultrahigh-density recording medium. The Fe-Pt alloy having the L1 0 structure not only has high crystal magnetic anisotropy, but also has excellent corrosion resistance and oxidation resistance, and therefore is expected to be suitable as a material for a magnetic recording medium.

又，於將具有L10結構之Fe-Pt合金使用作為超高密度記錄媒體用材料之情形時，要求開發如下之技術：使規則化於L10結構之Fe-Pt磁性粒子於磁孤立之狀態下儘量高密度地方向一致且分散。 Further, when a Fe-Pt alloy having an L1 0 structure is used as a material for an ultrahigh-density recording medium, development of a technique for forming a Fe-Pt magnetic particle having a L1 0 structure in a magnetically isolated state is required. The direction is as high as possible and the direction is uniform and dispersed.

因此，以C(碳)或氧化物等非磁性材料將具有L10結構之Fe-Pt磁性粒子孤立的粒狀(granular)結構磁性薄膜，被提出來作為採用熱輔助磁記錄方式之次世代硬碟的磁記錄媒體用。此粒狀結構磁性薄膜具有下述結構：藉由使非磁性材料包圍磁性粒子，以遮斷磁性粒子間之磁相互作用。 Therefore, a granular magnetic film having an isolated structure of Fe-Pt magnetic particles having an L1 0 structure is proposed as a non-magnetic material such as C (carbon) or oxide, and is proposed as a next generation hard using a thermally assisted magnetic recording method. The magnetic recording medium of the disc is used. The granular magnetic film has a structure in which a magnetic interaction between magnetic particles is blocked by surrounding a magnetic particle with a non-magnetic material.

具有粒狀結構之磁性薄膜的磁記錄媒體及與其相關的公知文獻，可列舉專利文獻1、專利文獻2、專利文獻3、專利文獻4、專利文獻5。 A magnetic recording medium having a magnetic film having a granular structure and a related document related thereto include Patent Document 1, Patent Document 2, Patent Document 3, Patent Document 4, and Patent Document 5.

上述具有具L10結構之Fe-Pt磁性粒子的粒狀結構磁性薄膜，含有C作為非磁性材料之磁性薄膜，由於其磁特性特別高，因此受到矚目。然而，若欲對由Fe-Pt合金與C構成之濺鍍靶進行濺鍍，則會有下述問題：在濺鍍時發生C不慎脫離而產生大量顆粒(particle)(附著於基板上之塵埃)。為了解決此問題，需要提供Fe-Pt合金與C之密合性經提高的濺鍍靶。又，雖使用含有代替C之碳化物或氮化物之靶，亦可得到優異之磁性薄膜，但於該情形時亦會有在濺鍍時產生大量顆粒之問題。 The granular magnetic thin film having the Fe-Pt magnetic particles having the L1 0 structure described above, and the magnetic thin film containing C as a non-magnetic material is attracting attention because of its particularly high magnetic properties. However, if a sputtering target composed of an Fe-Pt alloy and C is to be sputtered, there is a problem in that C is inadvertently detached during sputtering to generate a large amount of particles (attached to the substrate). dust). In order to solve this problem, it is necessary to provide a sputtering target in which the adhesion of the Fe-Pt alloy to C is improved. Further, although a magnetic thin film containing a carbide or a nitride instead of C is used, an excellent magnetic thin film can be obtained, but in this case, there is also a problem that a large amount of particles are generated at the time of sputtering.

專利文獻1：日本特開2000-306228號公報 Patent Document 1: Japanese Laid-Open Patent Publication No. 2000-306228

專利文獻2：日本特開2000-311329號公報 Patent Document 2: Japanese Laid-Open Patent Publication No. 2000-311329

專利文獻3：日本特開2008-59733號公報 Patent Document 3: Japanese Laid-Open Patent Publication No. 2008-59733

專利文獻4：日本特開2008-169464號公報 Patent Document 4: Japanese Laid-Open Patent Publication No. 2008-169464

專利文獻5：日本特開2004-152471號公報 Patent Document 5: Japanese Patent Laid-Open Publication No. 2004-152471

專利文獻6：日本特開2012-214874號公報 Patent Document 6: Japanese Laid-Open Patent Publication No. 2012-214874

上述Fe-Pt合金雖然在1：1組成附近會形成L10型規則晶格，但會有下述問題：一般而言結晶結構為規則晶格之材料缺乏延展性，此種材料即便使用加壓燒結裝置進行燒結亦難以提高燒結體之密度。特別是含有難燒結材料之C(碳)之Fe-Pt-C系極難獲得緻密的燒結體。因此若對此種密度低的燒結體濺鍍靶進行濺鍍，則會有下述問題：發生非磁性材料不慎脫離而產生大量顆粒(附著於基板上之塵埃)。 Although the above-mentioned Fe-Pt alloy forms a regular lattice of L1 0 type in the vicinity of the 1:1 composition, there is a problem that the material having a crystal structure of a regular crystal lattice generally lacks ductility, and even if such a material is pressurized It is also difficult to increase the density of the sintered body by sintering the sintering device. In particular, the Fe-Pt-C system containing C (carbon) which is a hard-to-sinter material is extremely difficult to obtain a dense sintered body. Therefore, if such a low-density sintered sputtering target is sputtered, there is a problem in that a large amount of particles (dust adhering to the substrate) are generated by inadvertently removing the non-magnetic material.

又，Fe-Pt合金之L10規則晶格若加熱至1300℃以上，雖然會從規則狀態轉移成不規則狀態而增加延展性，但會有根據其中所含有之非磁性材料的種類而於1300℃以上的溫度分解的情況。而且有下述問題：在1300℃以上之高溫域中，會有發生晶粒成長導致之燒結體組織粗大化之情形，此種粗大的晶粒會成為濺鍍時異常放電(電弧)之起點，而產生顆粒。 Further, when the L1 0 regular crystal lattice of the Fe-Pt alloy is heated to 1300 ° C or higher, the ductility is changed from a regular state to an irregular state, but the ductility is increased depending on the kind of the non-magnetic material contained therein. The temperature is decomposed above °C. Further, there is a problem in that in the high temperature region of 1300 ° C or higher, the sintered body structure is coarsened due to grain growth, and such coarse crystal grains become the starting point of abnormal discharge (arc) at the time of sputtering. And produce particles.

因此，本發明其課題在於提供一種大幅減低濺鍍時所產生之顆粒量的燒結體濺鍍靶，其係由Fe-Pt系合金與非磁性材料構成。 Accordingly, an object of the present invention is to provide a sintered body sputtering target which is capable of greatly reducing the amount of particles generated during sputtering, and is composed of an Fe-Pt-based alloy and a non-magnetic material.

本發明人著眼於：雖然Co或Ni與Fe-Pt合金一樣於1：1組成附近會形成L10型規則晶格，但由規則狀態轉移至不規則狀態之溫度為CoPt中約825℃、NiPt中約645℃，與FePt之約1300℃相比顯著降低，而得到下述知識見解：藉由使Fe-Pt系合金中含有此種元素，即便於比先前技 術低之燒結溫度亦表現不規則結構，合金之延展性增加，可製作高密度之燒結體，此種燒結體濺鍍靶可大幅減低濺鍍時所產生之顆粒量。 The present inventors focused on the fact that although Co or Ni forms a L1 0 type regular lattice in the vicinity of the 1:1 composition as well as the Fe-Pt alloy, the temperature from the regular state to the irregular state is about 825 ° C in CoPt, NiPt. At about 645 ° C, it is significantly lower than about 1300 ° C of FePt, and the following knowledge is obtained: by making such an element in the Fe-Pt-based alloy, even if the sintering temperature is lower than that of the prior art, the sintering temperature is irregular. The structure, the ductility of the alloy is increased, and a high-density sintered body can be produced. This sintered body sputtering target can greatly reduce the amount of particles generated during sputtering.

再者，專利文獻6中記載有一種濺鍍靶，其含有Fe、Pt及C，進一步含有Fe、Pt以外之金屬元素，作為Fe、Pt以外之金屬元素，含有比0at%多且20at%以下之Cu、Ag、Mn、Ni、Co、Pd、Cr、V、B。然而，專利文獻6中僅有含有10at%之Cu之一例，與後述之本發明的添加元素之種類及含量差異很大。 In addition, Patent Document 6 discloses a sputtering target containing Fe, Pt, and C, and further contains a metal element other than Fe or Pt, and contains more than 0 at% and 20 at% or less as a metal element other than Fe or Pt. Cu, Ag, Mn, Ni, Co, Pd, Cr, V, B. However, in Patent Document 6, only one example of 10% by weight of Cu is contained, and the type and content of the additive element of the present invention described later are largely different.

根據此種見解，本發明提供：1)一種濺鍍靶，其係以L10型規則晶格之Fe-Pt合金與非磁性材料為主成分的燒結體濺鍍靶，其特徵在於：以濺鍍靶之金屬成分中之原子數比率計，含有0.05~0.5%之Co或Ni中之任一者或兩者；2)如上述1)記載之濺鍍靶，其除了Fe、Pt、Co、Ni以外，含有選自Ag、Au、B、Cr、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Pd、Re、Rh、Ru、Si、Sn、Ta、W、V、Zn中之任一種以上元素作為金屬成分；3)如上述1)或2)記載之濺鍍靶，其含有碳、碳化物、氧化物、氮化物中之任一種以上作為非磁性材料。 According to such findings, the present invention provides: 1) A sputtering target, a sintered body in which the lattice lines L1 0 type rules Fe-Pt alloy and non-magnetic material as a main component sputtering target, wherein: the sputtering Any one or both of 0.05 to 0.5% of Co or Ni in the metal component of the target metal component; 2) the sputtering target according to the above 1), except for Fe, Pt, Co, Other than Ni, it contains any one selected from the group consisting of Ag, Au, B, Cr, Cu, Ga, Ge, Ir, Mn, Mo, Nb, Pd, Re, Rh, Ru, Si, Sn, Ta, W, V, and Zn. A sputtering target according to the above 1) or 2), which contains at least one of carbon, a carbide, an oxide, and a nitride as a non-magnetic material.

根據本發明，可提供於濺鍍時大幅減低所產生之顆粒量的濺鍍靶。藉此，具有可顯著提高成膜時之產率此優異效果。 According to the present invention, it is possible to provide a sputtering target which greatly reduces the amount of particles generated during sputtering. Thereby, there is an excellent effect that the yield at the time of film formation can be remarkably improved.

本發明之濺鍍靶，其係以L10型規則晶格之Fe-Pt合金與非 磁性材料為主成分的燒結體濺鍍靶，且以濺鍍靶之金屬成分中之原子數比率計，含有0.05~0.5%之範圍的Co或Ni中之任一者或兩者。 The sputtering target of the present invention is a sintered body sputtering target mainly composed of a Fe-Pt alloy of a L1 0 type regular lattice and a non-magnetic material, and is based on an atomic ratio in a metal component of the sputtering target. It contains either or both of Co or Ni in the range of 0.05 to 0.5%.

Fe-Pt合金之組成，一般可使用以原子數比率中Pt為35%以上且55%以下，剩餘部份為Fe之比例進行摻合者，但若為可維持有效之作為磁記錄媒體的特性之範圍內，則無特別限制。 The composition of the Fe-Pt alloy can be generally used in a ratio of Pt of 35% or more and 55% or less in the atomic ratio, and the remainder is Fe. However, if it is a magnetic recording medium which can be effectively maintained There are no special restrictions within the scope.

本案發明中特別重要的是，作為濺鍍靶之金屬成分，以上述金屬成分中之原子數比率計，以0.05~0.5%之範圍含有Co或Ni中之任一者或兩者。 In the present invention, it is particularly important that the metal component of the sputtering target contains either or both of Co or Ni in a range of 0.05 to 0.5% in terms of the atomic ratio of the metal component.

雖然Co或Ni與Fe-Pt合金一樣於1：1組成附近會形成L10型規則晶格，但由此規則狀態轉移至不規則狀態之溫度為CoPt中約825℃、NiPt中約645℃，與FePt之約1300℃相比顯著降低，因此藉由使Fe-Pt系合金中含有此等元素，即便於低燒結溫度亦可得到高密度之燒結體，可抑制顆粒之產生。 Although Co or Ni forms a L1 0 type regular lattice in the vicinity of the 1:1 composition like Fe-Pt alloy, the temperature at which the regular state is transferred to the irregular state is about 825 ° C in CoPt and about 645 ° C in NiPt. Since it is remarkably lowered by about 1300 ° C of FePt, by containing these elements in the Fe-Pt-based alloy, a sintered body having a high density can be obtained even at a low sintering temperature, and generation of particles can be suppressed.

上述之Co或Ni之含量，以上述金屬成分中之原子數比率計設為0.05%以上且0.5%以下。若含量未達0.05%，則由於自規則狀態轉移至不規則狀態之溫度無法充分降低，因此無法期待密度之提高，另一方面，若含量超過0.5%，則可能變得無法得到作為磁性薄膜之充分的磁特性。 The content of Co or Ni described above is 0.05% or more and 0.5% or less in terms of the atomic ratio of the metal component. When the content is less than 0.05%, the temperature from the regular state to the irregular state cannot be sufficiently lowered, so that the density cannot be expected to be improved. On the other hand, if the content exceeds 0.5%, the magnetic film may not be obtained. Full magnetic properties.

含有Co或Ni之任一者或兩者皆可獲得相同的效果。於含有兩者之情形時，必須將其合計含量設為以濺鍍靶之金屬成分中之原子數比率計為0.05%以上且0.5%以下。 The same effect can be obtained by either or both of Co or Ni. In the case where both are contained, the total content thereof is required to be 0.05% or more and 0.5% or less in terms of the atomic ratio of the metal component of the sputtering target.

再者，本案發明可添加Co、Ni作為金屬粉，由於在濺鍍靶之金屬成分中含有上述既定量即可，因此不用特別探討其添加手段。 Further, in the present invention, Co and Ni may be added as the metal powder, and since the metal component of the sputtering target may be contained in the above-mentioned specific amount, it is not particularly necessary to add the means for addition.

本發明之濺鍍靶除了Fe、Pt、Co、Ni以外，可含有選自Ag、Au、B、Cr、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Pd、Re、Rh、Ru、Si、Sn、Ta、W、V、Zn中之任一種以上元素作為金屬成分。 The sputtering target of the present invention may contain, besides Fe, Pt, Co, and Ni, may be selected from the group consisting of Ag, Au, B, Cr, Cu, Ga, Ge, Ir, Mn, Mo, Nb, Pd, Re, Rh, Ru, Any one or more of Si, Sn, Ta, W, V, and Zn is used as a metal component.

此等金屬元素係於經濺鍍之薄膜中，主要為了降低用於表現L10結構之熱處理溫度而添加者。其摻合比例只要為可維持有效之作為磁記錄媒體之特性的範圍內，則無特別限制，添加比例較理想為以上述金屬成分中之原子數比率計設為1at%以上且12at%以下。 These metal elements are incorporated into the sputtered film and are primarily added to reduce the heat treatment temperature used to characterize the L1 0 structure. The blending ratio is not particularly limited as long as it is in a range in which the magnetic recording medium can be effectively used. The addition ratio is preferably 1 at% or more and 12 at% or less in terms of the atomic ratio of the metal component.

又，本發明之濺鍍靶可含有碳、碳化物、氮化物、氧化物作 為非磁性材料。自此種濺鍍靶製得之磁性膜，由於碳、碳化物、氮化物、氧化物具有使磁性粒子彼此之磁相互作用絕緣的結構，故可期待良好之磁特性。特別是於含有碳之情形，從密度提高之觀點而言，含有上述Co或Ni具有效果。非磁性材料之摻合量，只要是可維持有效之作為磁記錄媒體的特性之範圍內，則無特別限制，較佳為設為以靶中之體積比率計為20vol%以上且40vol%以下。 Moreover, the sputtering target of the present invention may contain carbon, carbide, nitride, oxide as It is a non-magnetic material. Since the magnetic film obtained from such a sputtering target has a structure in which magnetic particles are magnetically insulated from each other by carbon, carbides, nitrides, and oxides, good magnetic properties can be expected. In particular, in the case of containing carbon, it is effective to contain Co or Ni as described above from the viewpoint of density improvement. The blending amount of the non-magnetic material is not particularly limited as long as it is a property of the magnetic recording medium that can be effectively maintained, and is preferably 20 vol% or more and 40 vol% or less in terms of the volume ratio in the target.

本發明之濺鍍靶係使用粉末燒結法，例如可藉由下述方法來製作。 The sputtering target of the present invention is produced by a powder sintering method, for example, by the following method.

首先，準備Fe粉、Pt粉、Co粉、Ni粉、Cu粉等作為金屬粉。作為金屬粉，不僅可使用單一元素之金屬粉，亦可使用合金粉。此等金屬粉宜使用粒徑在1~10μm之範圍者。若粒徑在1~10μm，則可更均勻混合，可防止偏析與粗大結晶化。當金屬粉末之粒徑大於10μm之情形時，有時非磁性材料會無法均勻地分散，又，當小於1μm之情形時，有時會發生下述問題：因金屬粉氧化之影響，而導致靶組成不是想要之組成。另，此粒徑 範圍僅為較佳範圍，應理解脫離此範圍並非否定本案發明之條件。 First, Fe powder, Pt powder, Co powder, Ni powder, Cu powder, or the like is prepared as a metal powder. As the metal powder, not only a single element metal powder but also an alloy powder can be used. These metal powders should preferably be used in a particle size range of 1 to 10 μm. When the particle diameter is 1 to 10 μm, it can be more uniformly mixed, and segregation and coarse crystallization can be prevented. When the particle diameter of the metal powder is larger than 10 μm, sometimes the non-magnetic material may not be uniformly dispersed, and when it is less than 1 μm, the following problem sometimes occurs: the target is caused by the oxidation of the metal powder. Composition is not the desired composition. In addition, this particle size The scope is only a preferred range, and it is to be understood that the scope of the invention is not to be construed as a limitation.

又，準備C粉、碳化物粉、氮化物粉等作為非磁性材料粉末。非磁性材料粉末宜使用粒徑在1~30μm之範圍者。若粒徑為1~30μm，則在與前述之金屬粉混合時，非磁性材料粉彼此不易凝聚，而可使之均勻地分散。關於非磁性材料中之C粉，具有如石墨(graphite)或奈米管般具有結晶結構者與以碳黑所代表之非晶質者，可使用任一種之C粉。 Further, C powder, carbide powder, nitride powder or the like is prepared as a nonmagnetic material powder. The non-magnetic material powder should preferably be used in a particle size range of 1 to 30 μm. When the particle diameter is 1 to 30 μm, the non-magnetic material powders are less likely to aggregate with each other when mixed with the metal powder described above, and can be uniformly dispersed. As the C powder in the non-magnetic material, those having a crystal structure such as graphite or a nanotube and amorphous ones represented by carbon black may be used.

接著，將上述原料粉秤量成想要的組成，使用球磨機等公知方法進行混合兼粉碎。此時，宜在粉碎容器內裝入非活性氣體，儘可能地抑制原料粉氧化。 Next, the raw material powder is weighed into a desired composition, and mixed and pulverized by a known method such as a ball mill. At this time, it is preferred to incorporate an inert gas into the pulverization container to suppress oxidation of the raw material powder as much as possible.

於真空環境或非活性氣體環境，以熱壓法對以上述方式得到之混合粉末進行成型、燒結。又，除了前述熱壓以外，亦可使用電漿放電燒結法等各種加壓燒結方法。尤其是熱靜水壓燒結法對提升燒結體密度是有效的。燒結時的保持溫度，雖然亦取決於靶之構成成分，但大多數的情形是在800~1500℃的溫度範圍。 The mixed powder obtained in the above manner is molded and sintered by a hot press method in a vacuum atmosphere or an inert gas atmosphere. Further, in addition to the above-described hot pressing, various pressure sintering methods such as a plasma discharge sintering method can also be used. In particular, the hot hydrostatic sintering method is effective for increasing the density of the sintered body. The holding temperature at the time of sintering depends on the constituent components of the target, but most of the cases are in the temperature range of 800 to 1500 °C.

然後，以車床將所製得之燒結體加工成想要的形狀，藉此可製作本發明之濺鍍靶。 Then, the sintered body obtained is processed into a desired shape by a lathe, whereby the sputtering target of the present invention can be produced.

藉由上述方式可製造本發明之濺鍍靶。以此方式製得之濺鍍靶，具有下述優異之效果：可降低濺鍍時產生之顆粒量，提升成膜時之產率。 The sputtering target of the present invention can be produced by the above method. The sputtering target produced in this manner has an excellent effect of reducing the amount of particles generated at the time of sputtering and improving the yield at the time of film formation.

實施例 Example

以下，根據實施例及比較例來說明。另，本實施例僅為一例示，並不受到此例示的任何限制。亦即，本發明僅受到申請專利範圍的限 制，包含本發明所含之實施例以外的各種變形。 Hereinafter, it demonstrates based on an Example and a comparative example. In addition, this embodiment is merely an example and is not limited by this illustration. That is, the invention is limited only by the scope of the patent application. The system includes various modifications other than the embodiment included in the present invention.

(實施例1) (Example 1)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑10μm之C粉(石墨粉)作為原料粉。然後以下述組成比，秤量成合計重量為2600g。再者，實施例1中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於0.25%之量的Co。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,600 g. Further, in Example 1, the amount of Co corresponding to 0.25% of the metal component in the sputtering target was measured.

秤量組成(分子數比率)：29.85Fe-0.15Co-30Pt-40C Weighing composition (number of molecules): 29.85Fe-0.15Co-30Pt-40C

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋(ball mill pot)，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1500℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill pot having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1500 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co含量為以濺鍍靶之金屬成分中的原子數比率計為0.25%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Co were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Co content was 0.25% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：30.20Fe-0.15Co-29.97Pt-39.68C Analytical composition (number of molecules): 30.20Fe-0.15Co-29.97Pt-39.68C

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。將此靶安裝於磁控濺鍍裝置(佳能安內華(CANON ANELVA)製C-3010濺鍍系統)進行濺鍍。使濺鍍條件為輸 入電功率1kW、Ar氣壓1.7Pa，實施2kWhr的預濺鍍後，在4吋直徑的矽基板上成膜20秒。然後以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為166個。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. This target was mounted on a magnetron sputtering apparatus (CON-10 AN-C-3010 sputtering system) for sputtering. Make the sputtering condition a loss The electric power was 1 kW, the Ar gas pressure was 1.7 Pa, and after 2 kWhr of pre-sputtering, film formation was performed on a 4 吋 diameter ruthenium substrate for 20 seconds. The number of particles attached to the substrate is then measured with a particle counter. The number of particles at this time was 166.

(比較例1) (Comparative Example 1)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑10μm之C粉(石墨粉)作為原料粉。然後以下述組成比，秤量成合計重量為2600g。再者，於比較例1中未添加Co粉。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,600 g. Further, in Comparative Example 1, Co powder was not added.

秤量組成(分子數比率)：30Fe-30Pt-40C Weighing composition (number of molecules): 30Fe-30Pt-40C

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1500℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1500 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe and Pt were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows.

分析組成(分子數比率)：30.25Fe-30.05Pt-39.70C Analytical composition (number of molecules): 30.25Fe-30.05Pt-39.70C

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為 324個，較實施例1增加。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time is 324, which is increased compared with Embodiment 1.

(比較例2) (Comparative Example 2)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑10μm之C粉(石墨粉)作為原料粉。然後以下述組成比，秤量成合計重量為2600g。再者，比較例2中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於10.0%之量的Co。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, and C powder (graphite powder) having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,600 g. Further, in Comparative Example 2, the amount of Co was equivalent to 10.0% by the atomic ratio of the metal component of the sputtering target.

秤量組成(分子數比率)：24Fe-6Co-30Pt-40C Weighing composition (number of molecules): 24Fe-6Co-30Pt-40C

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1500℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1500 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co含量為以濺鍍靶之金屬成分中的原子數比率計為10.05%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Co were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Co content was 10.05% based on the atomic ratio of the metal component of the sputtering target.

分析組成(分子數比率)：24.33Fe-6.07Co-29.98Pt-39.62C Analytical composition (number of molecules): 24.33Fe-6.07Co-29.98Pt-39.62C

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為 153個，較實施例1減少。另一方面，若與實施例1相比，無法得到充分的磁特性。認為此係由於Co的含量多，故飽和磁化或結晶磁異向性能量降低。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time is 153, which is less than that of Example 1. On the other hand, when compared with Example 1, sufficient magnetic characteristics could not be obtained. It is considered that since the content of Co is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(實施例2) (Example 2)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Ni粉、平均粒徑1μm之SiO2粉作為原料粉。然後以下述組成比，秤量成合計重量為2100g。再者，實施例2中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於0.075%之量的Ni。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Ni powder having an average particle diameter of 3 μm, and SiO 2 powder having an average particle diameter of 1 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,100 g. Further, in Example 2, the amount of Ni corresponding to 0.075% in terms of the atomic ratio of the metal component of the sputtering target was measured.

秤量組成(分子數比率)：39.94Fe-0.06Ni-40Pt-20SiO2 Weighing composition (number of molecules): 39.94Fe-0.06Ni-40Pt-20SiO 2

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1200℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Ni、Si係使用ICP-AES裝置進行測定。SiO2之含量係根據Si之測定值使用化學計算比率來計算。根據作為測量結果而得之重量比率來計算分子數比率的結果，此靶之組成如下所述。此時，Ni含量為以濺鍍靶之金屬成分中的原子數比率計為0.075%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Ni, and Si were measured using an ICP-AES apparatus. The content of SiO 2 was calculated from the measured value of Si using a stoichiometric ratio. The result of calculating the ratio of the number of molecules based on the weight ratio obtained as a result of measurement, the composition of this target is as follows. At this time, the Ni content was 0.075% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：39.92Fe-0.06Ni-40.05Pt-19.97SiO2 Analytical composition (number of molecules): 39.92Fe-0.06Ni-40.05Pt-19.97SiO 2

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進 行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為21個。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, the same conditions as in Example 1 were carried out. The sputtering is performed, and the number of particles attached to the substrate is measured by a particle counter. The number of particles at this time was 21.

(比較例3) (Comparative Example 3)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑1μm之SiO2粉作為原料粉。然後以下述組成比，秤量成合計重量為2100g。又，比較例3中並未添加Ni粉。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and SiO 2 powder having an average particle diameter of 1 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,100 g. Further, in Comparative Example 3, Ni powder was not added.

秤量組成(分子數比率)：40Fe-40Pt-20SiO2 Weighing composition (number of molecules): 40Fe-40Pt-20SiO 2

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1200℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Si係使用ICP-AES裝置進行測定。SiO2之含量係根據Si之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Si were measured using an ICP-AES apparatus. The content of SiO 2 was calculated from the measured value of Si using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows.

分析組成(分子數比率)：40.05Fe-39.92Pt-20.03SiO2 Analytical composition (number of molecules): 40.05Fe-39.92Pt-20.03SiO 2

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為35個，較實施例2增加。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 35, which was larger than that of Example 2.

(比較例4) (Comparative Example 4)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Ni粉、平均粒徑1μm之SiO2粉作為原料粉。然後以下述組成比，秤量成合計重量為2100g。再者，比較例4中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於2.0%之量的Ni。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Ni powder having an average particle diameter of 3 μm, and SiO 2 powder having an average particle diameter of 1 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,100 g. Further, in Comparative Example 4, the amount of Ni was equivalent to 2.0% by the atomic ratio of the metal component of the sputtering target.

秤量組成(分子數比率)：38.4Fe-1.6Ni-40Pt-20SiO2 Weighing composition (number of molecules): 38.4Fe-1.6Ni-40Pt-20SiO 2

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1200℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Ni、Si係使用ICP-AES裝置進行測定。SiO2之含量係根據Si之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Ni含量為以濺鍍靶之金屬成分中的原子數比率計為2.01%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Ni, and Si were measured using an ICP-AES apparatus. The content of SiO 2 was calculated from the measured value of Si using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Ni content was 2.01% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：38.34Fe-1.61Ni-39.98Pt-20.07SiO2 Analytical composition (number of molecules): 38.34Fe-1.61Ni-39.98Pt-20.07SiO 2

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為25個，與實施例2幾乎為相同程度。另一方面，若與實施例2相比，無法 得到充分的磁特性。認為此係由於Ni的含量多，故飽和磁化或結晶磁異向性能量降低。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 25, which was almost the same as in Example 2. On the other hand, if compared with the second embodiment, it is impossible to A sufficient magnetic property is obtained. It is considered that since the content of Ni is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(實施例3) (Example 3)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑10μm之BN粉作為原料粉。然後以下述組成比，秤量成合計重量為2400g。再者，實施例3中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於0.2%之量的Co。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, and BN powder having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,400 g. Further, in Example 3, the amount of Co corresponding to 0.2% by the atomic ratio of the metal component of the sputtering target was measured.

秤量組成(分子數比率)：34.86Fe-0.14Co-35Pt-30BN Weighing composition (number of molecules): 34.86Fe-0.14Co-35Pt-30BN

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1200℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co、B係使用ICP-AES裝置進行測定。BN之含量係根據B之測定值使用化學計算比率來計算。根據作為測量結果而得之重量比率來計算分子數比率的結果，此靶之組成如下所述。此時，Co含量為以濺鍍靶之金屬成分中的原子數比率計為0.21%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Co, and B were measured using an ICP-AES apparatus. The content of BN is calculated based on the measured value of B using a stoichiometric ratio. The result of calculating the ratio of the number of molecules based on the weight ratio obtained as a result of measurement, the composition of this target is as follows. At this time, the Co content was 0.21% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：35.10Fe-0.15Co-35.03Pt-29.72BN Analytical composition (molecular ratio): 35.10Fe-0.15Co-35.03Pt-29.72BN

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，安裝於磁控濺鍍裝置進行濺 鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為87個。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Use this target to mount on a magnetron sputtering device Plating, using a particle counter to measure the number of particles attached to the substrate. The number of particles at this time was 87.

(比較例5) (Comparative Example 5)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑10μm之BN粉作為原料粉。然後以下述組成比，秤量成合計重量為2400g。再者，於比較例5中並未添加Co粉。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and BN powder having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,400 g. Further, in Comparative Example 5, Co powder was not added.

秤量組成(分子數比率)：35Fe-35Pt-30BN Weighing composition (molecular ratio): 35Fe-35Pt-30BN

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1200℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、B係使用ICP-AES裝置進行測定。BN之含量係根據B之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and B were measured using an ICP-AES apparatus. The content of BN is calculated based on the measured value of B using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows.

分析組成(分子數比率)：35.37Fe-34.75Pt-29.88BN Analytical composition (number of molecules): 35.37Fe-34.75Pt-29.88BN

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，安裝於磁控濺鍍裝置，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為235個，較實施例3增加。認為此係由於合金與BN之密合性不足，因此BN為容易於濺鍍中脫粒之狀態。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, it was mounted on a magnetron sputtering apparatus, and sputtering was performed under the same conditions as in Example 1, and the number of particles attached to the substrate was measured by a particle counter. The number of particles at this time was 235, which was increased compared with Example 3. It is considered that this is because the adhesion between the alloy and BN is insufficient, so BN is in a state of being easily threshed during sputtering.

(比較例6) (Comparative Example 6)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑10μm之BN粉作為原料粉。然後以下述組成比，秤量成合計重量為2400g。再者，比較例6中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於20.0%之量的Co。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, and BN powder having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,400 g. Further, in Comparative Example 6, the amount of Co corresponding to 20.0% of the atomic ratio in the metal component of the sputtering target was measured.

秤量組成(分子數比率)：21Fe-14Co-35Pt-30BN Weighing composition (number of molecules): 21Fe-14Co-35Pt-30BN

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1200℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1200 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co、B係使用ICP-AES裝置進行測定。BN之含量係根據B之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co含量為以濺鍍靶之金屬成分中的原子數比率計為19.91%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Co, and B were measured using an ICP-AES apparatus. The content of BN is calculated based on the measured value of B using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Co content was 19.91% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：21.21Fe-13.99Co-35.05Pt-29.75BN Analytical composition (number of molecules): 21.21Fe-13.99Co-35.05Pt-29.75BN

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為101個，與實施例3幾乎同程度。另一方面，若與實施例3相比，無法得到 充分的磁特性。認為此係由於Co的含量多，故飽和磁化或結晶磁異向性能量降低。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 101, which was almost the same as in Example 3. On the other hand, if compared with the third embodiment, it is not available. Full magnetic properties. It is considered that since the content of Co is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(實施例4) (Example 4)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Ni粉、平均粒徑5μm之Cu粉、平均粒徑5μm之TaC粉作為原料粉。然後以下述組成比，秤量成合計重量為3400g。再者，實施例4中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於0.4%之量的Ni。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Ni powder having an average particle diameter of 3 μm, Cu powder having an average particle diameter of 5 μm, and TaC powder having an average particle diameter of 5 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 3,400 g. Further, in Example 4, the amount of Ni corresponding to 0.4% by the atomic ratio of the metal component of the sputtering target was measured.

秤量組成(分子數比率)：37.28Fe-0.32Ni-37.6Pt-4.8Cu-20TaC Weighing composition (number of molecules): 37.28Fe-0.32Ni-37.6Pt-4.8Cu-20TaC

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1150℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1150 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Cu、Ni係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。TaC之含量係根據C之測定值使用化學計算比率來計算。根據作為測量結果而得之重量比率來計算分子數比率的結果，此靶之組成如下所述。此時，Ni含量為以濺鍍靶之金屬成分中的原子數比率計為0.40%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Cu, and Ni were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of TaC is calculated based on the measured value of C using a stoichiometric ratio. The result of calculating the ratio of the number of molecules based on the weight ratio obtained as a result of measurement, the composition of this target is as follows. At this time, the Ni content was 0.40% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：37.25Fe-0.32Ni-37.62Pt-4.78Cu-20.03TaC Analytical composition (number of molecules): 37.25Fe-0.32Ni-37.62Pt-4.78Cu-20.03TaC

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度 5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為487個。 Further using a lathe, the sintered body is machined into a diameter of 180.0 mm, thickness The shape of 5.0 mm gives a disc-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 487.

(比較例7) (Comparative Example 7)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑5μm之Cu粉、平均粒徑5μm之TaC粉作為原料粉。然後以下述組成比，秤量成合計重量為3400g。再者，於比較例7中並未添加Ni粉。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Cu powder having an average particle diameter of 5 μm, and TaC powder having an average particle diameter of 5 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 3,400 g. Further, in Comparative Example 7, Ni powder was not added.

秤量組成(分子數比率)：37.6Fe-37.6Pt-4.8Cu-20TaC Weighing composition (number of molecules): 37.6Fe-37.6Pt-4.8Cu-20TaC

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1150℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1150 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Cu係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。TaC之含量係根據C之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Cu were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of TaC is calculated based on the measured value of C using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows.

分析組成(分子數比率)：37.60Fe-37.57Pt-4.76Cu-20.07TaC Analytical composition (number of molecules): 37.60Fe-37.57Pt-4.76Cu-20.07TaC

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，安裝於磁控濺鍍裝置，以與 實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為590個，較實施例4增加。認為此係由於合金與TaC之密合性不足，因此TaC為容易於濺鍍中脫粒之狀態。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Use this target to mount on a magnetron sputtering device to Sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured by a particle counter. The number of particles at this time was 590, which was increased compared with Example 4. This is considered to be because the adhesion between the alloy and TaC is insufficient, and therefore TaC is in a state of being easily threshed during sputtering.

(比較例8) (Comparative Example 8)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Ni粉、平均粒徑5μm之Cu粉、平均粒徑5μm之TaC粉作為原料粉。然後以下述組成比，秤量成合計重量為3400g。再者，比較例8中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於17.0%之量的Ni。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Ni powder having an average particle diameter of 3 μm, Cu powder having an average particle diameter of 5 μm, and TaC powder having an average particle diameter of 5 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 3,400 g. Further, in Comparative Example 8, the amount of Ni was equivalent to 17.0% in terms of the atomic ratio of the metal component of the sputtering target.

秤量組成(分子數比率)：24Fe-13.6Ni-37.6Pt-4.8Cu-20TaC Weighing composition (number of molecules): 24Fe-13.6Ni-37.6Pt-4.8Cu-20TaC

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為真空環境、升溫速度300℃/小時、保持溫度1150℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a vacuum atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1150 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Cu、Ni係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。TaC之含量係根據C之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co含量為以濺鍍靶之金屬成分中的原子數比率計為17.05%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Cu, and Ni were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of TaC is calculated based on the measured value of C using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Co content was 17.05% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：23.98Fe-13.63Ni-37.56Pt-4.79Cu-20.04TaC Analytical composition (number of molecules): 23.98Fe-13.63Ni-37.56Pt-4.79Cu-20.04TaC

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為425個，較實施例4減少。另一方面，若與實施例4相比，無法得到充分的磁特性。認為此係由於Ni的含量多，故飽和磁化或結晶磁異向性能量降低。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 425, which was smaller than that of Example 4. On the other hand, when compared with Example 4, sufficient magnetic characteristics could not be obtained. It is considered that since the content of Ni is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(實施例5) (Example 5)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑10μm之C粉、平均粒徑1μm之SiO2粉作為原料粉。然後以下述組成比，秤量成合計重量為2500g。再者，實施例5中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於0.5%之量的Co。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, C powder having an average particle diameter of 10 μm, and SiO 2 powder having an average particle diameter of 1 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,500 g. Further, in Example 5, the amount of Co corresponding to 0.5% by atomic ratio in the metal component of the sputtering target was measured.

秤量組成(分子數比率)：34.65Fe-0.35Co-35Pt-25C-5SiO2 Weighing composition (number of molecules): 34.65Fe-0.35Co-35Pt-25C-5SiO 2

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為氮環境、升溫速度300℃/小時、保持溫度1100℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1100 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co、Si係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。SiO2之含量係根據Si之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co含量為以濺鍍 靶之金屬成分中的原子數比率計為0.50%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Co, and Si were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of SiO 2 was calculated from the measured value of Si using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Co content was 0.50% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：34.98Fe-0.35Co-34.98Pt-24.72C-4.97SiO2 Analytical composition (number of molecules): 34.98Fe-0.35Co-34.98Pt-24.72C-4.97SiO 2

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為117個。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 117.

(比較例9) (Comparative Example 9)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑10μm之C粉、平均粒徑1μm之SiO2粉作為原料粉。然後以下述組成比，秤量成合計重量為2500g。再者，於比較例9中並未添加Co粉。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, C powder having an average particle diameter of 10 μm, and SiO 2 powder having an average particle diameter of 1 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,500 g. Further, in Comparative Example 9, Co powder was not added.

秤量組成(分子數比率)：35Fe-35Pt-25C-5SiO2 Weighing composition (number of molecules): 35Fe-35Pt-25C-5SiO 2

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為氮環境、升溫速度300℃/小時、保持溫度1100℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1100 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Si係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。SiO2之含量係根據Si之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, and Si were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of SiO 2 was calculated from the measured value of Si using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows.

分析組成(分子數比率)：34.95Fe-35.27Pt-24.80C-4.98SiO2 Analytical composition (number of molecules): 34.95Fe-35.27Pt-24.80C-4.98SiO 2

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為164個，較實施例5增加。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 164, which was larger than that of Example 5.

(比較例10) (Comparative Example 10)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑10μm之C粉、平均粒徑1μm之SiO2粉作為原料粉。以下述組成比，秤量成合計重量為2200g。再者，比較例10中，秤量以濺鍍靶之金屬成分中的原子數比率計相當於2.0%之量的Co。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, C powder having an average particle diameter of 10 μm, and SiO 2 powder having an average particle diameter of 1 μm were prepared as raw material powders. The total weight was 2,200 g in the following composition ratio. Further, in Comparative Example 10, the amount of Co was equivalent to 2.0% by the atomic ratio of the metal component of the sputtering target.

秤量組成(分子數比率)：33.6Fe-1.4Co-35Pt-25C-5SiO2 Weighing composition (number of molecules): 33.6Fe-1.4Co-35Pt-25C-5SiO 2

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為氮環境、升溫速度300℃/小時、保持溫度1100℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1100 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co、Si係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。SiO2之含量係根據Si之測定值使用化學計算比率來計算。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co含量為以濺鍍 靶之金屬成分中的原子數比率計為1.98%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Co, and Si were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. The content of SiO 2 was calculated from the measured value of Si using a stoichiometric ratio. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the Co content was 1.98% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：33.89Fe-1.39Co-34.87Pt-24.82C-5.03SiO2 Analytical composition (number of molecules): 33.89Fe-1.39Co-34.87Pt-24.82C-5.03SiO 2

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為121個，與實施例5幾乎同程度。另一方面，若與實施例5相比，無法得到充分的磁特性。認為此係由於Co的含量多，故飽和磁化或結晶磁異向性能量降低。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 121, which was almost the same as in Example 5. On the other hand, when compared with Example 5, sufficient magnetic characteristics could not be obtained. It is considered that since the content of Co is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

(實施例6) (Example 6)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑3μm之Ni粉、平均粒徑10μm之C粉作為原料粉。然後以下述組成比，秤量成合計重量為2600g。再者，實施例6中，秤量以濺鍍靶之金屬成分中的原子數比率計合計量相當於0.5%之量的Co與Ni。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, Ni powder having an average particle diameter of 3 μm, and C powder having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,600 g. Further, in Example 6, the amount of Co and Ni in an amount corresponding to 0.5% of the total number of atoms in the metal component of the sputtering target was measured.

秤量組成(分子數比率)：34.65Fe-0.05Co-0.30Ni-35Pt-30C Weighing composition (number of molecules): 34.65Fe-0.05Co-0.30Ni-35Pt-30C

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為氮環境、升溫速度300℃/小時、保持溫度1400℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co、Ni係使用ICP-AES裝置進行測定，C係利用採用高頻感 應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時，Co與Ni之合計含量為以濺鍍靶之金屬成分中的原子數比率計為0.50%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Co, and Ni are measured using an ICP-AES device, and C is used in a high-frequency sense. The measurement was carried out by a carbon analyzer of a furnace combustion-infrared absorption method. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. At this time, the total content of Co and Ni was 0.50% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：34.70Fe-0.05Co-0.30Ni-35.08Pt-29.87C Analytical composition (number of molecules): 34.70Fe-0.05Co-0.30Ni-35.08Pt-29.87C

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為121個。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 121.

(比較例11) (Comparative Example 11)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑10μm之C粉作為原料粉。然後以下述組成比，秤量成合計重量為2600g。再者，於比較例11中並未添加Co粉與Ni粉之任一者。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, and C powder having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,600 g. Further, in Comparative Example 11, neither of the Co powder nor the Ni powder was added.

秤量組成(分子數比率)：35Fe-35Pt-30C Weighing composition (number of molecules): 35Fe-35Pt-30C

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為氮環境、升溫速度300℃/小時、保持溫度1400℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。根據以此方式獲得之重量比 率來計算分子數比率而得之結果，此靶之組成如下所述。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe and Pt were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. Weight ratio obtained in this way As a result of calculating the ratio of the number of molecules, the composition of this target is as follows.

分析組成(分子數比率)：35.04Fe-35.07Pt-29.89C Analytical composition (number of molecules): 35.04Fe-35.07Pt-29.89C

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為164個，較實施例6增加。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 164, which was larger than that of Example 6.

(比較例12) (Comparative Example 12)

準備平均粒徑3μm之Fe粉、平均粒徑3μm之Pt粉、平均粒徑3μm之Co粉、平均粒徑3μm之Ni粉、平均粒徑10μm之C粉作為原料粉。然後以下述組成比，秤量成合計重量為2600g。再者，比較例12中，秤量以濺鍍靶之金屬成分中的原子數比率計合計量相當於1.0%之量的Co與Ni。 Fe powder having an average particle diameter of 3 μm, Pt powder having an average particle diameter of 3 μm, Co powder having an average particle diameter of 3 μm, Ni powder having an average particle diameter of 3 μm, and C powder having an average particle diameter of 10 μm were prepared as raw material powders. Then, the following composition ratio was weighed to a total weight of 2,600 g. In addition, in Comparative Example 12, the amount of Co and Ni in an amount corresponding to 1.0% of the total number of atoms in the metal component of the sputtering target was measured.

秤量組成(分子數比率)：34.3Fe-0.40Co-0.30Ni-35Pt-30C Weighing composition (number of molecules): 34.3Fe-0.40Co-0.30Ni-35Pt-30C

接著將秤量之全部粉末與粉碎媒體之SUS磨球一起放入容量10公升的球磨鍋，於Ar環境中，旋轉16小時進行混合、粉碎。然後，將自鍋中取出之粉末填充於碳製模具，使用熱壓裝置進行成型、燒結。使熱壓的條件為氮環境、升溫速度300℃/小時、保持溫度1400℃、保持時間2小時，自升溫開始時至保持結束以30MPa進行加壓。保持結束後直接在腔室內自然冷卻。 Next, the entire amount of the powder was placed in a ball mill having a capacity of 10 liters together with a SUS grinding ball of a pulverizing medium, and the mixture was rotated and pulverized in an Ar atmosphere for 16 hours. Then, the powder taken out from the pot was filled in a carbon mold, and it was molded and sintered using a hot press apparatus. The conditions of the hot pressing were a nitrogen atmosphere, a temperature increase rate of 300 ° C / hour, a holding temperature of 1400 ° C, and a holding time of 2 hours, and the pressure was applied at 30 MPa from the start of the temperature rise to the end of the holding. After the end of the stay, it is naturally cooled directly in the chamber.

接著使用自所製作之燒結體採集而得一部份，實施組成分析。Fe、Pt、Co、Ni係使用ICP-AES裝置進行測定，C係利用採用高頻感應加熱爐燃燒-紅外線吸收法之碳分析裝置進行測定。根據以此方式獲得之重量比率來計算分子數比率而得之結果，此靶之組成如下所述。此時， Co與Ni之合計含量為以濺鍍靶之金屬成分中的原子數比率計為0.98%。 Then, a part of the sintered body produced was used to carry out a composition analysis. Fe, Pt, Co, and Ni were measured using an ICP-AES apparatus, and C was measured by a carbon analyzer using a high-frequency induction heating furnace-infrared absorption method. As a result of calculating the molecular number ratio based on the weight ratio obtained in this manner, the composition of this target is as follows. at this time, The total content of Co and Ni was 0.98% in terms of the atomic ratio in the metal component of the sputtering target.

分析組成(分子數比率)：34.32Fe-0.40Co-0.29Ni-34.97Pt-30.02C Analytical composition (number of molecules): 34.32Fe-0.40Co-0.29Ni-34.97Pt-30.02C

進一步使用車床，將燒結體切削加工成直徑180.0mm、厚度5.0mm之形狀，而得到圓盤狀之靶。使用此靶，以與實施例1相同之條件進行濺鍍，以顆粒計數器測量附著於基板上的顆粒個數。此時的顆粒個數為126個，與實施例6幾乎同程度。另一方面，若與實施例6相比，無法得到充分的磁特性。認為此係由於Co與Ni的合計含量多，故飽和磁化或結晶磁異向性能量降低。 Further, using a lathe, the sintered body was cut into a shape having a diameter of 180.0 mm and a thickness of 5.0 mm to obtain a disk-shaped target. Using this target, sputtering was carried out under the same conditions as in Example 1, and the number of particles attached to the substrate was measured with a particle counter. The number of particles at this time was 126, which was almost the same as in Example 6. On the other hand, sufficient magnetic properties could not be obtained as compared with Example 6. It is considered that since the total content of Co and Ni is large, the saturation magnetization or the crystal magnetic anisotropy energy is lowered.

如以上所述，於任一實施例中，藉由添加既定量之Co或Ni，而可降低濺鍍時產生之顆粒量，可提升成膜時之產率。因此，可知含有Co或Ni，對於抑制產生顆粒具有非常重要的作用。 As described above, in any of the embodiments, by adding a predetermined amount of Co or Ni, the amount of particles generated at the time of sputtering can be reduced, and the yield at the time of film formation can be improved. Therefore, it is understood that the inclusion of Co or Ni has a very important effect on suppressing generation of particles.

產業利用性 Industrial utilization

本發明之濺鍍靶，具有下述優異之效果：可減低濺鍍時產生之顆粒量，提升成膜時之產率。因此，適用作為用以形成粒狀結構型磁性薄膜之濺鍍靶。 The sputtering target of the present invention has an excellent effect of reducing the amount of particles generated at the time of sputtering and improving the yield at the time of film formation. Therefore, it is suitable as a sputtering target for forming a granular structure type magnetic thin film.

Claims (3)

一種濺鍍靶，其係以L10型規則晶格之Fe-Pt合金與非磁性材料為主成分的燒結體濺鍍靶，其特徵在於：以濺鍍靶之金屬成分中之原子數比率計，含有0.05~0.5%之Co或Ni中之任一者或兩者。 A sputtering target which is a sintered body sputtering target mainly composed of a Fe-Pt alloy of a L1 0 type regular lattice and a non-magnetic material, and is characterized by an atomic ratio in a metal component of a sputtering target Containing 0.05 to 0.5% of either Co or Ni or both. 如申請專利範圍第1項之濺鍍靶，其除了Fe、Pt、Co、Ni以外，含有選自Ag、Au、B、Cr、Cu、Ga、Ge、Ir、Mn、Mo、Nb、Pd、Re、Rh、Ru、Si、Sn、Ta、W、V、Zn中之任一種以上元素作為金屬成分 A sputtering target according to the first aspect of the patent application, which comprises, besides Fe, Pt, Co, and Ni, is selected from the group consisting of Ag, Au, B, Cr, Cu, Ga, Ge, Ir, Mn, Mo, Nb, Pd, Any one or more of Re, Rh, Ru, Si, Sn, Ta, W, V, Zn as a metal component 如申請專利範圍第1或2項之濺鍍靶，其含有碳、碳化物、氧化物、氮化物中之任一種以上作為非磁性材料。 A sputtering target according to claim 1 or 2, which contains any one or more of carbon, carbide, oxide, and nitride as a nonmagnetic material.
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