JP3534264B2 - Target material for magnetic thin film and method for manufacturing the same - Google Patents
Target material for magnetic thin film and method for manufacturing the sameInfo
- Publication number
- JP3534264B2 JP3534264B2 JP27444694A JP27444694A JP3534264B2 JP 3534264 B2 JP3534264 B2 JP 3534264B2 JP 27444694 A JP27444694 A JP 27444694A JP 27444694 A JP27444694 A JP 27444694A JP 3534264 B2 JP3534264 B2 JP 3534264B2
- Authority
- JP
- Japan
- Prior art keywords
- target material
- thin film
- compound
- magnetic
- less
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000013077 target material Substances 0.000 title claims description 57
- 239000010409 thin film Substances 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 238000000034 method Methods 0.000 title description 9
- 150000001875 compounds Chemical class 0.000 claims description 47
- 229910052715 tantalum Inorganic materials 0.000 claims description 30
- 229910045601 alloy Inorganic materials 0.000 claims description 23
- 239000000956 alloy Substances 0.000 claims description 23
- 229910052742 iron Inorganic materials 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 22
- 238000005266 casting Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- 239000010408 film Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 4
- 230000008520 organization Effects 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000004544 sputter deposition Methods 0.000 description 11
- 230000005496 eutectics Effects 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 238000005204 segregation Methods 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005546 reactive sputtering Methods 0.000 description 5
- 229910002056 binary alloy Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910017086 Fe-M Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- UNILWMWFPHPYOR-KXEYIPSPSA-M 1-[6-[2-[3-[3-[3-[2-[2-[3-[[2-[2-[[(2r)-1-[[2-[[(2r)-1-[3-[2-[2-[3-[[2-(2-amino-2-oxoethoxy)acetyl]amino]propoxy]ethoxy]ethoxy]propylamino]-3-hydroxy-1-oxopropan-2-yl]amino]-2-oxoethyl]amino]-3-[(2r)-2,3-di(hexadecanoyloxy)propyl]sulfanyl-1-oxopropan-2-yl Chemical compound O=C1C(SCCC(=O)NCCCOCCOCCOCCCNC(=O)COCC(=O)N[C@@H](CSC[C@@H](COC(=O)CCCCCCCCCCCCCCC)OC(=O)CCCCCCCCCCCCCCC)C(=O)NCC(=O)N[C@H](CO)C(=O)NCCCOCCOCCOCCCNC(=O)COCC(N)=O)CC(=O)N1CCNC(=O)CCCCCN\1C2=CC=C(S([O-])(=O)=O)C=C2CC/1=C/C=C/C=C/C1=[N+](CC)C2=CC=C(S([O-])(=O)=O)C=C2C1 UNILWMWFPHPYOR-KXEYIPSPSA-M 0.000 description 1
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 1
- 229910001339 C alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910001362 Ta alloys Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Landscapes
- Magnetic Heads (AREA)
- Physical Vapour Deposition (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は磁気ヘッド等に用いられ
る磁気薄膜を提供するターゲット材およびその製造方法
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a target material for providing a magnetic thin film used for a magnetic head or the like and a method for manufacturing the target material.
【０００２】[0002]
【従来の技術】近年磁気記録技術の進歩は著しく、磁気
ディスク等の大容量化、あるいはＶＴＲ装置の小型軽量
化のために記録密度の高密度化が進められている。この
高密度の記録のために使用される磁気ヘッドには、高保
磁力を有する記録媒体に十分書き込むことが可能な記録
磁界を有する磁性膜を磁気ヘッドに構成することが要求
されている。また、磁気ヘッド用の材料は、記録や再生
の効率の向上の点から高透磁率を有することが必要であ
り、記録再生特性の安定化のためには、磁歪定数を零近
傍に制御することが望ましい。さらに、磁気ヘッドの製
造プロセスにおいては、信頼性を確保するためにガラス
溶着等を用いることが多いので、加熱処理により特性が
劣化しないように高温における安定性向上も必要であ
る。2. Description of the Related Art In recent years, the progress of magnetic recording technology has been remarkable, and the recording density has been increased in order to increase the capacity of magnetic disks and the like, or to reduce the size and weight of VTR devices. The magnetic head used for this high-density recording is required to have a magnetic film having a recording magnetic field capable of sufficiently writing on a recording medium having a high coercive force. Also, the material for the magnetic head needs to have a high magnetic permeability from the viewpoint of improving the efficiency of recording and reproduction, and the magnetostriction constant should be controlled to near zero in order to stabilize the recording and reproduction characteristics. Is desirable. Further, in the manufacturing process of the magnetic head, glass welding or the like is often used in order to ensure reliability, so it is also necessary to improve stability at high temperature so that the characteristics are not deteriorated by heat treatment.
【０００３】このような材料としては、従来からＦｅ−
Ａｌ−Ｓｉ系合金（いわゆるセンダスト）やＣｏ系アモ
ルファス合金等が開発されており、磁気ヘッドに適用さ
れている。（特開昭６０−７４１１０号公報等参照）。
また、最近では特開平３−２０４４４号公報には、優れ
た磁気特性を有する磁気ヘッド用薄膜としてＦｅ−（Ｔ
ｉ，Ｚｒ，Ｈｆ，Ｎｂ，Ｔａから選ばれた一種以上の元
素：以下Ｍと言う）−Ｃ系合金が示されている。また、
特開平４−６８０９号公報には優れた磁気特性が得られ
る磁気ヘッド用薄膜としてＦｅ−（Ｍ）−Ｎ系合金が示
されている。特開平３−２０４４４号公報および特開平
４−６８０９号公報に記載されるように、Ｆｅ−（Ｍ）
−（Ｃ，Ｎ）系の薄膜は、微結晶組織とすることが可能
であり、保磁力が小さく透磁率も高いことに加え、磁気
特性が熱的に安定であるという優れた特性を有してお
り、磁気ヘッド用薄膜として非常に有望な材料と言え
る。As such a material, Fe--
Al-Si alloys (so-called sendust), Co amorphous alloys, etc. have been developed and applied to magnetic heads. (See JP-A-60-74110, etc.).
Recently, Japanese Patent Laid-Open No. 3-20444 discloses Fe- (T) as a thin film for a magnetic head having excellent magnetic characteristics.
One or more elements selected from i, Zr, Hf, Nb and Ta: hereinafter referred to as M) -C based alloys are shown. Also,
Japanese Unexamined Patent Publication (Kokai) No. 4-68009 discloses a Fe- (M) -N-based alloy as a thin film for a magnetic head that provides excellent magnetic characteristics. As described in JP-A-3-20444 and JP-A-4-6809, Fe- (M)
The (C, N) -based thin film can have a microcrystalline structure, has a small coercive force, a high magnetic permeability, and has excellent characteristics that the magnetic characteristics are thermally stable. Therefore, it can be said that it is a very promising material for thin films for magnetic heads.
【０００４】上述した磁気ヘッド用薄膜の内Ｆｅ−
（Ｍ）−Ｃ系合金膜を得る場合には、特開平３−２０４
４４号公報に記載されるように、Ｆｅ−Ｍ系のターゲッ
ト材の上にグラファイトを配置したターゲット材とする
か、あるいはＦｅ−Ｍ系のターゲット材をメタン含有雰
囲気で反応性スパッタリングを行ない膜中に炭素を導入
する方法が知られている。またＦｅ−（Ｍ）−Ｎ系合金
膜を得る場合には、特開平４−６８０９号公報に記載さ
れるように、Ｆｅ上に金属Ｍのペレットを配置したスパ
ッリングターゲット材を用いて窒素含有雰囲気下で反応
性スパッタリングを行うことにより、Ｆｅ−Ｍ−Ｎ系の
合金薄膜を得ていた。Of the above thin films for magnetic heads, Fe-
In order to obtain a (M) -C alloy film, the method disclosed in JP-A-3-204
As described in Japanese Patent Publication No. 44-44, a target material in which graphite is arranged on an Fe-M based target material is used, or the Fe-M based target material is subjected to reactive sputtering in a methane-containing atmosphere in a film. A method of introducing carbon into is known. Further, when an Fe- (M) -N-based alloy film is obtained, as described in JP-A-4-68009, a spalling target material in which pellets of metal M are arranged on Fe is used to contain nitrogen. By carrying out reactive sputtering in an atmosphere, an Fe-MN system alloy thin film was obtained.
【０００５】[0005]
【発明が解決しようとする課題】上述したＦｅ−（Ｍ）
−（Ｃ，Ｎ）系合金の薄膜の製造方法のうち、反応性ス
パッタリング法を用いる方法は、炭素や窒素の導入量を
制御しやすいという利点があり、生産方法の主力になる
ものと考えられる。本発明者は上記の反応性スパッタリ
ング法に適用するため、上記に提案されている合金系の
うち特に高い熱安定性を有し、優れた磁気特性が得られ
るとされるＦｅ−Ｔａ系を選択し、反応性スパッタリン
グによって磁気薄膜を得ることを目的としてＦｅとＴａ
の２元合金のターゲット材を鋳造法によって得ることを
試みた。The above-mentioned Fe- (M)
Among the methods for producing a thin film of a (C, N) -based alloy, the method using the reactive sputtering method has an advantage that it is easy to control the introduction amount of carbon and nitrogen, and is considered to be a main production method. . Since the present inventor applies it to the above-mentioned reactive sputtering method, among the alloy systems proposed above, the Fe-Ta system, which is said to have particularly high thermal stability and excellent magnetic properties, is selected. And Fe and Ta for the purpose of obtaining a magnetic thin film by reactive sputtering.
An attempt was made to obtain the target material of the binary alloy of No. 1 by the casting method.
【０００６】ところが、ＦｅとＴａの合金は鋳造時にＦ
ｅとＴａの化合物を形成するため、鋳造時に大きな偏析
部を有する組織となり、この偏析部がスパッタリングに
よって形成する薄膜の組成のばらつきの原因となること
が判明した。本発明の目的は、スパッタリングによって
得られる膜の組成のばらつきを低減できるＦｅ−Ｔａ系
の磁気薄膜用ターゲット材およびその製造方法を提供す
ることである。However, the alloy of Fe and Ta is F during casting.
It was found that since a compound of e and Ta is formed, the structure has a large segregation portion at the time of casting, and this segregation portion causes variation in the composition of the thin film formed by sputtering. An object of the present invention is to provide an Fe—Ta based target material for a magnetic thin film, which can reduce variations in composition of a film obtained by sputtering, and a method for producing the same.
【０００７】[0007]
【課題を解決するための手段】本発明者は、Ｆｅ−Ｔａ
系合金ターゲット材において、組成をＴａ量を５〜１５
原子％の範囲とすることで、ＦｅとＴａの２元系の状態
図における共晶点近傍の組成とし、さらに鋳造温度を合
金の融点直上とすることにより鋳造時の冷却を早めるこ
とによって、ＦｅとＴａの化合物が微細に分散したター
ゲット材を得ることができ、この組織を有するターゲッ
ト材を用いてスパッタリングすれば、組成分布のばらつ
きの少ない薄膜が得られることを見いだし、本発明に到
達した。The inventor of the present invention has found that Fe--Ta
In the system-based alloy target material, the composition is set to Ta amount of 5 to
By setting the content to be in the atomic% range, the composition near the eutectic point in the phase diagram of the binary system of Fe and Ta can be obtained. Further, by setting the casting temperature just above the melting point of the alloy, the cooling during casting is accelerated, It was found that a target material in which the compound of Ta and Ta is finely dispersed can be obtained, and that a thin film having a small variation in composition distribution can be obtained by sputtering using a target material having this structure, and the present invention was reached.
【０００８】すなわち本発明は、合金組成としてＴａを
５〜１５原子％含有し、残部Ｆｅおよび不可避的不純物
からなるターゲット材であって、Ｆｅを主体とするマト
リックスに、最大粒径が５０μｍ以下のＦｅとＴａの塊
状化合物と、最大長５０μｍ以下のＦｅとＴａの長粒状
化合物とが分散した組織を有することを特徴とする磁気
薄膜用ターゲット材である。また、本発明は、合金組成
としてＴａを５〜１５原子％、Ｃｒを１０原子％以下含
有し、残部Ｆｅおよび不可避的不純物からなるターゲッ
ト材であって、Ｆｅを主体とするマトリックスに、最大
粒径が５０μｍ以下のＦｅとＴａの塊状化合物と、最大
長５０μｍ以下のＦｅとＴａの長粒状化合物とが分散し
た組織を有することを特徴とする磁気薄膜用ターゲット
材である。 That is, the present invention contains Ta as an alloy composition in an amount of 5 to 15 atomic%, and balances Fe and unavoidable impurities.
Which is a target material composed of Fe, and a lumpy compound of Fe and Ta having a maximum particle diameter of 50 μm or less and a long-granular compound of Fe and Ta having a maximum length of 50 μm or less. A target material for a magnetic thin film having a dispersed structure. Further, the present invention is an alloy composition
5 to 15 atomic% Ta and 10 atomic% or less Cr
And a target consisting of the balance Fe and unavoidable impurities.
It is a tough material and has a maximum content of Fe-based matrix.
Fe and Ta lumps with particle size less than 50 μm
Fe particles with a length of 50 μm or less and long granular compounds of Ta are dispersed.
Target for magnetic thin film characterized by having different texture
It is a material.
【０００９】また、その他の本発明は、上記組成の合金
溶湯を前記合金の液相温度を超え融点＋５０℃の鋳造温
度にて鋳造を行なうことを特徴とする本発明の磁気薄膜
用ターゲット材の製造方法である。 Another aspect of the present invention is to provide a target material for magnetic thin film according to the present invention, which is characterized in that the molten alloy having the above composition is cast at a casting temperature of a melting point + 50 ° C. which is higher than the liquidus temperature of the alloy. it is a manufacturing method.
【００１０】[0010]
【作用】本発明のターゲット材の特徴の一つは、Ｆｅと
Ｔａの２元系の状態図における共晶付近の組成であるＴ
ａ５〜１５原子％に規定したことである。ＦｅとＴａの
２元系状態図によれば、共晶点はＴａ７．９原子％であ
り、Ｔａ２．５〜２８原子％の範囲で共晶組織を発現可
能である。ターゲット材の組織を均一微細にするために
は共晶点に一致する組成が好ましいが、共晶点組成の近
傍でも微細な組織を得ることが可能であり、本発明にお
いては、Ｔａを５〜１５原子％に規定した。好ましく
は、Ｔａ７−１０％である。One of the characteristics of the target material of the present invention is that the composition near the eutectic in the phase diagram of the binary system of Fe and Ta is T
It is defined to be 5 to 15 atom%. According to the binary phase diagram of Fe and Ta, the eutectic point is Ta 7.9 atom%, and the eutectic structure can be expressed in the range of Ta 2.5 to 28 atom%. A composition matching the eutectic point is preferable in order to make the structure of the target material uniform and fine, but it is possible to obtain a fine structure even in the vicinity of the eutectic point composition. It was defined as 15 atom%. Preferably, it is Ta7-10%.
【００１１】なお、Ｔａの下限を５原子％としたのは、
５原子％未満では磁気ヘッド等に用いられる磁気薄膜と
した場合に結晶粒の微細化等の磁気特性の向上が達成で
きないためであり、また５％未満ではＴａ量が少ないこ
とから、ＦｅとＴａの化合物自体が少なくなり、化合物
の偏析による薄膜組成のばらつきの問題が生じにくいた
めである。一方１５原子％を超えると、共晶組成から離
れるとともにＦｅとＴａの金属間化合物が多量に生成し
てターゲット材組織を微細化できなくなるため、１５原
子％以下と規定した。The lower limit of Ta is 5 atomic%
If it is less than 5 atomic%, it is not possible to achieve improvement in magnetic properties such as grain refinement in the case of a magnetic thin film used for a magnetic head or the like, and if it is less than 5%, the Ta content is small, so Fe and Ta This is because the compound itself becomes less and the problem of variation in thin film composition due to segregation of the compound is less likely to occur. On the other hand, if it exceeds 15 atomic%, it is separated from the eutectic composition and a large amount of an intermetallic compound of Fe and Ta is generated and the target material structure cannot be refined.
【００１２】本発明においては、ＦｅとＴａの２元系を
基本にするものであるが、Ｔａと同様に薄膜形成時に炭
化物あるいは窒化物となって微細な組織を形成する作用
を持つ元素として知られているＴｉ，Ｚｒ，Ｈｆ，Ｖ，
ＮｂをＴａの一部と置換して含有することを除外するも
のではない。これらの元素は、Ｔａに比べて形成する薄
膜の耐熱性の点で劣るため、Ｔａの含有量よりも少なく
する必要がある。In the present invention, although it is based on a binary system of Fe and Ta, it is known as an element having a function of forming a fine structure by becoming a carbide or a nitride at the time of forming a thin film like Ta. Ti, Zr, Hf, V,
It does not exclude that Nb is substituted with a part of Ta and contained. Since these elements are inferior to Ta in heat resistance of the thin film to be formed, it is necessary to make the content less than Ta.
【００１３】また、本発明においては、薄膜に耐食性を
確保するためＣｒ，Ａｌ，Ｐｔ，Ｒｕ等の耐食性元素の
添加が望ましい。本発明のターゲット材はスパッタリン
グ期間中に炭素あるいは窒素と反応されるものであり、
炭素や窒素と強力に結合する４Ａ，５Ａ属元素であるＴ
ｉ，Ｚｒ，Ｈｆ，Ｖ，Ｎｂは、薄膜状態で炭化物あるい
は窒化物として存在することになるため、薄膜の耐食性
の向上の効果が少ない。 したがって、これ以外のＦｅ
に対して耐食性を高める元素を添加することが望ましい
のである。特にＣｒは、磁気特性の劣化が少ない元素と
して有効である。上述した耐食性元素は、多量に添加す
ると磁気特性を劣化するため、添加量は制限する必要が
あり、１０原子％以下とすることが望ましい。Further, in the present invention, it is desirable to add a corrosion-resistant element such as Cr, Al, Pt, Ru or the like in order to ensure the corrosion resistance of the thin film. The target material of the present invention is one that is reacted with carbon or nitrogen during the sputtering period,
T, which is a 4A, 5A group element that strongly binds to carbon and nitrogen
Since i, Zr, Hf, V, and Nb exist as a carbide or a nitride in a thin film state, the effect of improving the corrosion resistance of the thin film is small. Therefore, other Fe
Therefore, it is desirable to add an element that enhances corrosion resistance. In particular, Cr is effective as an element with little deterioration in magnetic characteristics. The above-mentioned corrosion-resistant element deteriorates the magnetic characteristics when added in a large amount, so the addition amount needs to be limited, and is preferably 10 atomic% or less.
【００１４】また、本発明はＦｅを主体とするマトリッ
クスに、最大粒径が５０μｍ以下のＦｅとＴａを主体と
する塊状化合物と、最大長５０μｍ以下のＦｅとＴａを
主体とする長粒状化合物とが分散した組織に規定した。
磁気ヘッド等に用いられるＦｅ−Ｔａ−（Ｃ，Ｎ）系の
合金薄膜においては、、ターゲット材から導入されるＴ
ａがスパッタリングにより気相から導入されるＣあるい
はＮと結合して炭化物あるいは窒化物を形成し、薄膜組
織において結晶の成長を抑える核として作用している。
この作用により薄膜が微細組織となり優れた磁気特性が
得られるものである。したがって、均一な微細組織であ
り、磁気特性の変動の少ない薄膜を安定して得るために
は、ターゲット材中の組織のばらつきを少なく抑える必
要がある。Further, according to the present invention, in a matrix containing Fe as a main component, an agglomerate compound containing Fe and Ta as a main component having a maximum particle size of 50 μm or less and a long-granular compound containing Fe and Ta as a main component having a maximum length of 50 μm or less as a main component. Defined in a dispersed organization.
In the Fe—Ta— (C, N) -based alloy thin film used for a magnetic head or the like, T introduced from the target material is used.
a combines with C or N introduced from the vapor phase by sputtering to form a carbide or a nitride, and acts as a nucleus for suppressing crystal growth in the thin film structure.
By this action, the thin film becomes a fine structure and excellent magnetic properties are obtained. Therefore, in order to stably obtain a thin film having a uniform fine structure and little variation in magnetic characteristics, it is necessary to suppress the variation in the structure in the target material.
【００１５】一方ターゲット材を構成する元素であるＴ
ａはＦｅとの化合物を形成してターゲット材中に存在す
る。この化合物はマトリックスとなるＦｅとスパッタリ
ング速度およびスパッタリング方向が異なるため、偏析
があるとＴａ濃度が大きく変動し、得られる薄膜の磁気
特性を大きく変動することになる。本発明では、ターゲ
ット材中の偏析を少なくし、組織の微細化を試み、組成
を共晶組成付近に限定するとともに、鋳造を該合金の液
相温度を越え＋５０℃の範囲内で行うことで、偏析の少
ない微細組織を得たものである。その微細組織は、具体
的には最大粒径が５０μｍ以下のＦｅとＴａを主体とす
る塊状化合物と、最大長５０μｍ以下のＦｅとＴａを主
体とする長粒状化合物とが分散した組織である。なお塊
状化合物と長粒状化合物の存在比は、Ｔａ量によって変
えることができるため、Ｔａ量によってスパッタリング
装置の特性に合わせたスパッタリング速度、Ｔａ濃度分
布の調製が可能である。On the other hand, T which is an element constituting the target material
a forms a compound with Fe and exists in the target material. Since this compound has a sputtering rate and a sputtering direction different from those of Fe that is a matrix, if Ta is segregated, the Ta concentration greatly changes, and the magnetic characteristics of the obtained thin film greatly change. In the present invention, segregation in the target material is reduced, microstructure refinement is attempted, the composition is limited to the vicinity of the eutectic composition, and casting is performed within the range of + 50 ° C. above the liquidus temperature of the alloy. A microstructure with less segregation was obtained. Specifically, the fine structure is a structure in which a lump compound mainly composed of Fe and Ta having a maximum particle size of 50 μm or less and a long granular compound mainly composed of Fe and Ta having a maximum length of 50 μm or less are dispersed. Since the abundance ratio of the lump compound and the long particulate compound can be changed by the Ta amount, it is possible to adjust the sputtering rate and the Ta concentration distribution according to the characteristics of the sputtering device by the Ta amount.
【００１６】本発明の製造方法における重要な特徴は、
液相温度を超え融点＋５０℃の鋳造温度にて鋳造を行な
うことである。本発明においては、鋳造温度を融点直上
とし、注湯後にすばやく凝固が始まるようにすることに
よって、ＦｅとＴａの化合物の微細な晶出が起こるとと
もに、鋳造工程中で晶出するＦｅとＴａの化合物とマト
リックスとの比重差に起因する偏析を防止することがで
き、上述した本発明の組織のターゲット材を得ることが
できるものである。また、本発明の製造方法において
は、他の偏析を防止する手段を併用することを除外する
ものではない。例えばより微細な組織とするための強制
冷却を行ったり、１１００〜１３００℃に加熱して１時
間以上保持するソーキングを行っても良い。An important feature of the manufacturing method of the present invention is that
Casting is performed at a casting temperature of the melting point + 50 ° C, which exceeds the liquidus temperature. In the present invention, the casting temperature is set just above the melting point so that solidification starts quickly after pouring, whereby fine crystallization of the Fe and Ta compounds occurs, and at the same time the Fe and Ta compounds crystallized during the casting process. Segregation due to the difference in specific gravity between the compound and the matrix can be prevented, and the target material having the structure of the present invention described above can be obtained. Further, in the production method of the present invention, it is not excluded that another means for preventing segregation is also used. For example, forced cooling may be performed to obtain a finer structure, or soaking may be performed by heating to 1100 to 1300 ° C. and holding for 1 hour or more.
【００１７】[0017]
（実施例１）原子％でＦｅ＝９２．１％、Ｔａ ７．９
％の共晶点組成の合金を１０マイナス３乗Torr下で融点
温度である１４４２℃に対して ＋２０〜２５℃に制御
しながら鋳造を行なった。このターゲット材を光学顕微
鏡で組織観察した。図１にその４００倍の金属ミクロ組
織写真を示す。図１を見ると明かなように、ターゲット
材のミクロ組織は組織断面に占める１個の粒子の面積が
大きい塊状化合物と、微細な長粒状化合物が分散した組
織となっていることがわかる。この組織の観察により塊
状化合物の最大粒径は２１μｍ、長粒化合物の最大長は
２４μｍであった。またＸ線回折分析により、塊状化合
物および長粒化合物ともＦｅ3Ｔａ7の化合物であること
が確認された。また比較例として同一組成の合金を鋳造
温度を融点＋７０〜８０℃に制御して鋳造を行なった。
得られた比較例のターゲット材の４００倍の金属ミクロ
組織写真を図２に示す。比較例のターゲット材中に存在
するＦｅとＴａの塊状化合物の最大粒径は６４μｍであ
った。(Example 1) Fe = 92.1% in atomic%, Ta 7.9
% Alloy having a eutectic point composition was cast at 10 to the third power Torr while controlling the melting point temperature of 1442 ° C. to +20 to 25 ° C. The structure of this target material was observed with an optical microscope. FIG. 1 shows a 400 times metal microstructure photograph. As is clear from FIG. 1, the microstructure of the target material has a structure in which a lump compound in which one particle occupies a large area in the cross section of the structure and a fine long granular compound are dispersed. Observation of this structure revealed that the maximum particle size of the lump compound was 21 μm and the maximum length of the long compound was 24 μm. In addition, it was confirmed by X-ray diffraction analysis that both the lump compound and the long-grain compound were Fe 3 Ta 7 compounds. As a comparative example, an alloy having the same composition was cast by controlling the casting temperature to a melting point +70 to 80 ° C.
FIG. 2 shows a photograph of the metal microstructure of the obtained target material of Comparative Example at 400 times. The maximum particle size of the massive compound of Fe and Ta present in the target material of the comparative example was 64 μm.
【００１８】次にこれらのターゲット材を使用して窒素
とアルゴンの混合雰囲気下でスパッタリングを行ない、
１６原子％の窒素の導入を行った。他の条件は以下の通
りである。
排気到達真空度 ＜ １× １０マイナス６乗
投入電力 ４．５Ｗ／ｃｍ2
基板 結晶化ガラス
膜厚 ２μｍプラス・マイナス０．２μｍ
ターゲット材を４０時間スパッタリングして、得られた
薄膜中のＴａ濃度のばらつきは本発明のターゲット材で
０．１原子％であったが、比較例のターゲット材では
０．９原子％と大きなものとなり、本発明のターゲット
材の方が磁気薄膜を安定して得ることができることがわ
かった。Next, using these target materials, sputtering is performed in a mixed atmosphere of nitrogen and argon,
Introduction of 16 atomic% nitrogen was performed. Other conditions are as follows. Degree of exhausted vacuum <1 × 10 minus 6th power input 4.5 W / cm 2 Substrate Crystallized glass film thickness 2 μm plus / minus 0.2 μm Target material was sputtered for 40 hours to obtain Ta concentration in the obtained thin film. The variation was 0.1 atom% in the target material of the present invention, but was as large as 0.9 atom% in the target material of the comparative example, and the target material of the present invention can obtain a magnetic thin film more stably. I found that
【００１９】（実施例２）
原子％でＦｅ＝８８．０％、Ｔａ＝１２．０％の組成の
合金を１０マイナス３乗Torr下で液相線温度である１５
２０℃に対して＋２０〜２５℃に制御しながら鋳造を行
なった。このターゲット材を光学顕微鏡で組織観察し
た。図３にその４００倍の金属ミクロ組織写真を示す。
図３を見ると明かなように、実施例１と同様にターゲッ
ト材のミクロ組織は組織断面に占める１個の粒子の面積
が大きい塊状化合物と、微細な長粒状化合物が分散した
組織となっていることがわかる。この組織の観察により
塊状化合物の最大粒径は２６μｍ、長粒状化合物の最大
長は１３μｍであった。またＸ線回折分析により、塊状
化合物および長粒状化合物ともＦｅ3Ｔａ7の化合物であ
ることが確認された。なお、実施例１と比較すると塊状
化合物の割合が増加していた。(Example 2) An alloy having a composition of Fe = 88.0 % and Ta = 12.0% in atomic% has a liquidus temperature of 15 under 10 ^ 3 Torr.
Casting was performed while controlling at +20 to 25 ° C with respect to 20 ° C. The structure of this target material was observed with an optical microscope. Fig. 3 shows a photograph of the metal microstructure of 400 times.
As is clear from FIG. 3, as in Example 1, the microstructure of the target material has a structure in which a lump compound having a large area of one particle occupying the structure cross section and a fine long granular compound are dispersed. You can see that Maximum particle size of the bulk compound the tissue observation 26 .mu.m, the maximum length of long grain-like compound was 13 .mu.m. The addition X-ray diffraction analysis, it was confirmed with mass compounds and Nagatsubu like compound is a compound of Fe 3 Ta 7. In addition, as compared with Example 1, the ratio of the lump compound was increased.
【００２０】図３に示すように１２原子％のＴａを含有
する場合でも、本発明のターゲット材組織は極めて微細
であり、偏析のないものであることがわかる。得られた
ターゲット材を実施例１と同様にスパッタリングを行
い、組成のばらつきを測定したところ０．３原子％であ
り、本発明のターゲット材により、１２原子％のＴａを
含有する本発明のターゲット材においても磁気薄膜を安
定して得ることができることがわかった。As shown in FIG. 3, it can be seen that the target material structure of the present invention is extremely fine and has no segregation even when it contains 12 atomic% of Ta. The obtained target material was sputtered in the same manner as in Example 1 and the compositional variation was measured to be 0.3 atom%. With the target material of the present invention, the target of the present invention containing 12 atom% of Ta was used. It was found that the magnetic thin film can be stably obtained even in the material.
【００２１】（実施例３）
原子％でＦｅ＝９２．１％、Ｔａ＝７．９％で１００％
とし、前記ＦｅとＴａの合計に対して、Ｃｒ＝５．７％
を添加した合金を１０マイナス３乗Torr下でＦｅとＴａ
の共晶点温度である１４４２℃に対して＋２０〜２５℃
に制御しながら鋳造を行った。このターゲット材は耐食
性元素としてＣｒを添加したものである。ターゲット材
組織を光学顕微鏡で組織観察した。図４にその４００倍
のターゲット材の金属ミクロ組織写真を示す。図４を見
ると明かなように、実施例１と同様にターゲット材のミ
クロ組織は組織断面に占める１個の粒子の面積が大きい
塊状化合物と、微細な長粒状化合物が分散した組織とな
っていることがわかる。この組織の観察により塊状化合
物の最大粒径は２０μｍ、長粒状化合物の最大長は１３
μｍであった。またＸ線回折分析により塊状化合物およ
び長粒状化合物としてＦｅ3Ｔａ7の化合物が確認され
た。ターゲット材中のＣｒは、化合物としては検出でき
ず、マトリックス部分のＣｒ濃度が化合物部分のよりも
高いことが確認された。(Example 3) Fe = 92.1% in atomic% and 100% in Ta = 7.9 %
And Cr = 5.7% with respect to the total of Fe and Ta.
Fe and Ta alloy under 10 minus cube Torr with the addition of
+20 to 25 ° C against 1442 ° C which is the eutectic point temperature of
Casting was performed while controlling the temperature. This target material has Cr added as a corrosion resistant element. The structure of the target material was observed with an optical microscope. FIG. 4 shows a photograph of a metal microstructure of the target material at a magnification of 400 times. As is clear from FIG. 4, as in Example 1, the microstructure of the target material has a structure in which a lump compound in which one particle occupies a large area in the structure cross section and a fine long grain compound are dispersed. You can see that Maximum particle size of the bulk compound the tissue observation 20 [mu] m, the maximum length of long grain-like compound 13
was μm. The compounds of Fe 3 Ta 7 as mass compounds and Nagatsubu like compound was confirmed by X-ray diffraction analysis. Cr in the target material could not be detected as a compound, and it was confirmed that the Cr concentration in the matrix portion was higher than that in the compound portion.
【００２２】図４に示すようにＣｒ含有する場合でも、
本発明のターゲット材組織は極めて微細であり、偏析の
ないものであることがわかる。得られたターゲット材を
実施例１と同様にスパッタリングを行い、組成のばらつ
きを測定したところ０．１原子％であり、耐食性改善元
素としてＣｒを含有する本発明のターゲット材において
も磁気薄膜を安定して得ることができることがわかっ
た。Even when Cr is contained as shown in FIG.
It can be seen that the target material structure of the present invention is extremely fine and has no segregation. Sputtering was performed on the obtained target material in the same manner as in Example 1, and the variation in composition was measured to be 0.1 atom%, and the magnetic thin film was stable even in the target material of the present invention containing Cr as a corrosion resistance improving element. I found that I can get it.
【００２３】[0023]
【発明の効果】本発明によれば、ＦｅとＴａの化合物を
均一に分散させることができ、組成ばらつきの少ない薄
膜の形成が可能になる。したがって、極めて精度の高い
記録あるいは再生特性を要求される磁気ヘッド用薄膜の
成形のために使用されるターゲット材として極めて有効
である。According to the present invention, the compound of Fe and Ta can be uniformly dispersed, and a thin film with little composition variation can be formed. Therefore, it is extremely effective as a target material used for forming a thin film for a magnetic head that requires extremely accurate recording or reproducing characteristics.
【図１】本発明のターゲット材の金属ミクロ組織写真の
例である。FIG. 1 is an example of a metal microstructure photograph of a target material of the present invention.
【図２】比較例のターゲット材の金属ミクロ組織写真の
例である。FIG. 2 is an example of a metal microstructure photograph of a target material of a comparative example.
【図３】Ｔａ量の多い本発明のターゲット材の金属ミク
ロ組織写真の例である。FIG. 3 is an example of a metal microstructure photograph of a target material of the present invention having a large amount of Ta.
【図４】Ｃｒを含有する本発明のターゲット材の金属ミ
クロ組織写真の例である。FIG. 4 is an example of a metal microstructure photograph of a target material of the present invention containing Cr.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｇ１１Ｂ 5/31 Ｇ１１Ｂ 5/31 Ｃ ─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. 7 Identification code FI G11B 5/31 G11B 5/31 C
Claims (3)
有し、残部Ｆｅおよび不可避的不純物からなるターゲッ
ト材であって、Ｆｅを主体とするマトリックスに、最大
粒径が５０μｍ以下のＦｅとＴａの塊状化合物と、最大
長５０μｍ以下のＦｅとＴａの長粒状化合物とが分散し
た組織を有することを特徴とする磁気薄膜用ターゲット
材。1. A target material containing 5 to 15 atomic% of Ta as an alloy composition , the balance being Fe and unavoidable impurities, and having a Fe-based matrix with a maximum particle size of 50 μm. the following Fe and Ta bulk compound and a magnetic thin film target material and length particulate compound of the maximum length 50μm or less of Fe and Ta are characterized by having a distributed organization.
Ｃｒを１０原子％以下含有し、残部Ｆｅおよび不可避的
不純物からなるターゲット材であって、Ｆｅを主体とす
るマトリックスに、最大粒径が５０μｍ以下のＦｅとＴ
ａの塊状化合物と、最大長５０μｍ以下のＦｅとＴａの
長粒状化合物とが分散した組織を有することを特徴とす
る磁気薄膜用ターゲット材。2. An alloy composition of 5 to 15 atomic% Ta,
Cr content of 10 atomic% or less, balance Fe and unavoidable
A target material composed of impurities , in which a Fe-based matrix has a maximum grain size of 50 μm or less and Fe and T
bulk compound a and the target material for a magnetic film characterized by having a structure in which the <br/> length particulate compounds of the maximum length 50μm or less of Fe and Ta are dispersed.
成の合金溶湯を該合金の液相温度を超え＋５０℃の範囲
の鋳造温度にて鋳造を行なうことを特徴とする磁気薄膜
用ターゲット材の製造方法。3. The set according to claim 1 or 2.
The method of manufacturing a magnetic thin film target material, characterized in that the molten alloy adult performing casting at casting temperature in the range of greater than + 50 ℃ liquidus temperature of the alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27444694A JP3534264B2 (en) | 1994-10-13 | 1994-10-13 | Target material for magnetic thin film and method for manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27444694A JP3534264B2 (en) | 1994-10-13 | 1994-10-13 | Target material for magnetic thin film and method for manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08109470A JPH08109470A (en) | 1996-04-30 |
| JP3534264B2 true JP3534264B2 (en) | 2004-06-07 |
Family
ID=17541806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27444694A Expired - Fee Related JP3534264B2 (en) | 1994-10-13 | 1994-10-13 | Target material for magnetic thin film and method for manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3534264B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001271161A (en) * | 2000-01-20 | 2001-10-02 | Mitsui Mining & Smelting Co Ltd | Method for manufacturing sputtering target |
| US9034153B2 (en) | 2006-01-13 | 2015-05-19 | Jx Nippon Mining & Metals Corporation | Nonmagnetic material particle dispersed ferromagnetic material sputtering target |
| JP5348661B2 (en) * | 2009-01-22 | 2013-11-20 | 山陽特殊製鋼株式会社 | Soft magnetic target material |
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1994
- 1994-10-13 JP JP27444694A patent/JP3534264B2/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| JPH08109470A (en) | 1996-04-30 |
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