JPS62263939A - Manufacture of alloy target material - Google Patents
Manufacture of alloy target materialInfo
- Publication number
- JPS62263939A JPS62263939A JP10805686A JP10805686A JPS62263939A JP S62263939 A JPS62263939 A JP S62263939A JP 10805686 A JP10805686 A JP 10805686A JP 10805686 A JP10805686 A JP 10805686A JP S62263939 A JPS62263939 A JP S62263939A
- Authority
- JP
- Japan
- Prior art keywords
- target material
- alloy target
- rare earth
- powder
- transition metal
- 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.)
- Pending
Links
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 31
- 239000000956 alloy Substances 0.000 title claims abstract description 31
- 239000013077 target material Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 14
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 239000010409 thin film Substances 0.000 claims abstract description 9
- 238000007711 solidification Methods 0.000 claims abstract description 8
- 230000008023 solidification Effects 0.000 claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 150000003624 transition metals Chemical class 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 2
- 238000007906 compression Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000005056 compaction Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000009694 cold isostatic pressing Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 3
- 229910017061 Fe Co Inorganic materials 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 238000009924 canning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
-
- 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
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、光磁気記録用磁性膜をＰＶＤ（物理蒸着）の
−手法であるスパッタリングによって基盤上に形成する
ために使用される合金ターゲット材を製造する方法に関
するもので、特に板状の合金ターゲット材を製造するの
に有効な製造法である。Detailed Description of the Invention [Industrial Application Field] The present invention relates to an alloy target material used for forming a magnetic film for magneto-optical recording on a substrate by sputtering, which is a method of PVD (physical vapor deposition). This method is particularly effective for manufacturing plate-shaped alloy target materials.
希土類元素（Ｔｂ、Ｇｄ、Ｄｙ等）−遷移金属よりなる
合金は、近年光磁気メモリー媒体として有望視され、開
発が進められている。光磁気メモリーは、磁性材料に光
によって記録するものであり、薄膜として基盤上に蒸着
される。これらの薄膜は、前記の希土類元素−遷移金属
合金として、例えば、Ｔｂ−Ｆｅ−Ｃｏ、Ｇｄ−Ｆｅ−
Ｔｂのようなものが用いられている。Alloys made of rare earth elements (Tb, Gd, Dy, etc.) and transition metals have recently been seen as promising as magneto-optical memory media, and are being developed. Magneto-optical memory uses light to record on magnetic materials and is deposited as a thin film onto a substrate. These thin films are made of rare earth element-transition metal alloys such as Tb-Fe-Co, Gd-Fe-
Materials such as Tb are used.
前記の合金系を用いてエポキシ系樹脂等からなる基盤に
スパッタリングにより薄膜を形成するには、真空容器中
に板状のターゲット材を設置し、それに対向して磁性薄
膜を形成しようとする基盤を配置する。１Ｏ−２Ｔｏｒ
ｒのＡｒ分圧下で、高周波（１３，７６８ＩＩ２）によ
りＡｒを電離させてプラズマを発生させ、Ａｒ”イオン
を合金ターゲット材に衝突させ、希土類元素と遷移金属
をたたき出し、基盤上にデポジットさせ薄膜を形成させ
る。To form a thin film by sputtering on a substrate made of epoxy resin or the like using the above-mentioned alloy system, a plate-shaped target material is placed in a vacuum container, and the substrate on which the magnetic thin film is to be formed is placed opposite to it. Deploy. 1O-2 Tor
Under an Ar partial pressure of r, Ar is ionized by high frequency (13,768II2) to generate plasma, and the Ar'' ions collide with the alloy target material to knock out rare earth elements and transition metals, which are deposited on the substrate to form a thin film. Let it form.
従来より、希土類元素−遷移金属合金ターゲット材は、
合金構成元素の１種類を用いて基盤を作り、その−にに
残りの合金成分よりなる合金チップまたはシー１へを張
り付けて、ターゲット材とする製造法（モザイク法）が
用いられている。さらに、所定の合金成分となるように
配合した原料を真空溶解・鋳造しインゴットを作り、機
械加工により製造される方法が利用されている。しかし
ながら、前記の２つの方法のうち、モザイク法において
は、スパッタリングにより形成した膜が成分的に不均一
になり易く、酸素址も１１０００ｐｐ以上であり、安定
して良好な膜を得ることは困難である。真空溶解法によ
るインゴットの製造では、低酸素の高品位な合金ターゲ
ット材が得られるが、インゴットの偏析に起因する膜の
成分不均一および、希土類元素−遷移金属系の合金は非
常にもろいため、ターゲットの形状を出すための機械加
工が困難である。これらの欠点を解決するために、粉末
冶金による手法が考えられ、Ｔ（Ｉ Ｐ法の応用も試み
られているが、ＨＩ Ｐ法の場合カプセルの変形によっ
て、合金に割れが発生する。また、カプセル除去等の工
数が増加する。また、希土類元素のような活性元素を含
む合金粉末の処理、すなわち分級やキャンニング等の工
程で酸化したり、汚染される恐れがある。ＨＩＰにおい
ては、一度粉末が汚染されると、ＨＩ Ｐ工程で除去・
無害化することはできない。実際にスパッタリングに供
される合金ターゲラ］・材は、厚さが約３〜５１ｎの程
度の板状のものであり、ＨＩＰ法によって板状の形状を
得ることは上述の理由により困難である。Traditionally, rare earth element-transition metal alloy target materials are
A manufacturing method (mosaic method) is used in which a substrate is made using one type of alloy constituent element, and an alloy chip or sheet 1 made of the remaining alloy components is attached to the base to form a target material. Furthermore, a method is used in which raw materials blended to have predetermined alloy components are vacuum melted and cast to form an ingot, and the ingot is manufactured by machining. However, among the above two methods, in the mosaic method, the film formed by sputtering tends to be non-uniform in terms of composition, and the oxygen content is more than 11,000 pp, making it difficult to obtain a stable and good film. be. Manufacturing ingots using the vacuum melting method yields a low-oxygen, high-quality alloy target material, but the composition of the film is non-uniform due to ingot segregation, and rare earth element-transition metal alloys are extremely brittle. Machining to obtain the target shape is difficult. To solve these drawbacks, methods using powder metallurgy have been considered, and attempts have also been made to apply the T(IP method), but in the HIP method, cracks occur in the alloy due to deformation of the capsule. The number of man-hours required for capsule removal, etc. increases.Also, there is a risk of oxidation and contamination during processing of alloy powders containing active elements such as rare earth elements, that is, classification and canning processes.In HIP, once If the powder becomes contaminated, it can be removed and removed during the HIP process.
It cannot be made harmless. The alloy targela material actually used for sputtering is a plate-like material with a thickness of about 3 to 51 nm, and it is difficult to obtain a plate-like shape by the HIP method for the reasons described above.
本発明は、前述の問題点を解決するためになされたもの
で、粉末成形法と真空プラズマ溶解法およびスプラット
凝固法により板状で低酸素含有量（１０００ｐｐｍ以下
）の高品位な合金ターゲット材を製造する方法を提供す
るものである。すなわち、希土類粉末と遷移金属粉末を
所定の合金組成となるように配合し、不活性ガス雰囲気
下で混合する。The present invention was made to solve the above-mentioned problems, and produces a plate-shaped high-grade alloy target material with a low oxygen content (1000 ppm or less) using a powder compaction method, a vacuum plasma melting method, and a splat solidification method. The present invention provides a method for manufacturing. That is, rare earth powder and transition metal powder are blended to have a predetermined alloy composition and mixed under an inert gas atmosphere.
これらの原料粉末を得る方法としては、不活性ガス下に
おける機械的粉砕法（クラッシャー、振動ミル、アトラ
イター等）や真空溶解−不活性ガスアトマイズ法が利用
できる。混合方法としては、ボールミルやＶ型ブレンダ
ー等が使用できる。所定の組成に配合され、混合により
均一となった予合金化されていない粉末を冷間等方圧縮
により真空プラズマ溶解用の電極を成形する。当該電極
を用いて真空プラズマ溶解し、スプラット凝固させる。As a method for obtaining these raw material powders, a mechanical pulverization method under an inert gas (crusher, vibration mill, attritor, etc.) or a vacuum melting-inert gas atomization method can be used. As a mixing method, a ball mill, a V-type blender, etc. can be used. The non-prealloyed powder, which is blended into a predetermined composition and made uniform by mixing, is molded into an electrode for vacuum plasma melting by cold isostatic compression. The electrode is used for vacuum plasma melting and splat solidification.
スプラット凝固法は、溶滴を連続的に冷却基盤上に落下
させ、薄い板状に凝固させたものを積み重ねて、バルク
材料を得る技術であり、特に板状のものを製造するのに
適した手法である。さらに、冷却基盤形状を変えること
により種々の形状のものが得られる。したがって、本発
明によれば、成分の均一な電極が製造でき、その電極を
用いて真空プラズマ溶解法により高純度化することがで
きる。さらに、スプラット凝固法により板状の合金ター
ゲット材が得られる。The splat solidification method is a technology that obtains bulk materials by continuously dropping droplets onto a cooling base and stacking the solidified thin plates.It is particularly suitable for manufacturing plate-shaped items. It is a method. Furthermore, various shapes can be obtained by changing the shape of the cooling base. Therefore, according to the present invention, an electrode with uniform components can be manufactured, and the electrode can be used to achieve high purity by vacuum plasma melting. Furthermore, a plate-shaped alloy target material is obtained by the splat solidification method.
以下、本発明を実施例に基づき説明する。合金系は、Ｔ
ｂ−Ｆｅ−Ｃｏを用いた。Hereinafter, the present invention will be explained based on examples. The alloy system is T
b-Fe-Co was used.
Ｔｂ粉末を得るために、１１φ×１“ＱのプロンりをＡ
ｒ雰囲気下でクラッシャーにより粉砕した。In order to obtain Tb powder, a 11φ x 1"Q prong was
It was crushed by a crusher under an atmosphere of r.
このＴｂ粉末にＦｅ粉末、Ｇｏ粉末（Ａｒガスアトマイ
ズ粉）を重量で５３，０％Ｔｂ、 ７．０％ｃｏ、４０
．０％Ｆｅとなるように配合し、Ｖ型ブレンダーを使用
しＡｒ雰囲気下で４Ｈｒ混合した。この粉末をラバーケ
ースに充填し、冷間静水圧プレスに装入、成形圧６ｔ／
ｃｄ、加圧保持１０分間で電極の形状に成形した。To this Tb powder, Fe powder and Go powder (Ar gas atomized powder) were added by weight to 53.0% Tb, 7.0% co, 40%
．． They were blended so as to have 0% Fe and mixed for 4 hours in an Ar atmosphere using a V-type blender. This powder was filled into a rubber case and charged into a cold isostatic press, with a molding pressure of 6t/
cd, and was molded into an electrode shape by holding pressure for 10 minutes.
本工程で合金化されていない電極が得られた。次に、真
空プラズマ溶解炉に、当該電極を装着し、真空排気を行
なった。１Ｏ−４Ｔｏｒｒ到達後、Ａｒ流量２Ｑ ／ｍ
ｉｎで（０，６ＴｏｒｒＡｒ圧）、出力２０ＫＷ−５０
ＫＷで真空プラズマ溶解を行なった。電極から直径φ３
〜φ５ｍの合金化された溶湯が連続的に下部の設置され
たモールドに落下し、スプラット凝固される。モールド
は、２５０＋＋ｍφのものを使用し、スプラット凝固体
の厚さ５画、６肛、７ｗｍ、８ｍのものを製造した。An unalloyed electrode was obtained in this step. Next, the electrode was attached to a vacuum plasma melting furnace, and the furnace was evacuated. After reaching 1O-4Torr, Ar flow rate 2Q/m
in (0.6 TorrAr pressure), output 20KW-50
Vacuum plasma melting was performed at KW. Diameter φ3 from electrode
The alloyed molten metal with a diameter of ~φ5m continuously falls into the mold installed at the bottom and is splat solidified. A mold of 250++ mφ was used to produce splat solidified bodies with a thickness of 5 mm, 6 mm, 7 wm, and 8 m.
表−１
製造した円板状合金ターゲット材は、表面粗度１０〜１
５μｍに機械研磨により仕−１−げた。表−１に本発明
によって製造した合金ターゲット材の密度と不純物に関
する調査結果をまとめた。表より、本発明によるターゲ
ット材は、密度的には従来法に比較して低いが、不純物
に関しては大幅に改善されていることがわかる。また、
本発明によるターゲットを用いて、スパッタリングによ
り薄膜を基盤」二に形成し、薄膜を調査したところ従来
法と比較して均質で特性の良い膜が得られた。Table-1 The manufactured disc-shaped alloy target material has a surface roughness of 10 to 1.
Finished by mechanical polishing to 5 μm. Table 1 summarizes the investigation results regarding the density and impurities of the alloy target material manufactured according to the present invention. From the table, it can be seen that although the target material according to the present invention has a lower density than that of the conventional method, impurities are significantly improved. Also,
A thin film was formed on a substrate by sputtering using the target according to the present invention, and when the thin film was investigated, it was found that a film was homogeneous and had better properties compared to conventional methods.
以上のように本発明によれば、高純度で板状の＝７−
希土類元素−遷移金属合金ターゲラ１へ材が得られ、光
磁気記録用媒体の特性向上に寄与する。As described above, according to the present invention, a highly purified plate-shaped =7- rare earth element-transition metal alloy target layer 1 can be obtained, contributing to improving the characteristics of a magneto-optical recording medium.
Claims (1)
ト材の製造において、希土類元素粉末と遷移金属粉末を
混合する工程、冷間等方圧縮によって電極を成形する工
程および当該電極を真空プラズマ溶解法により溶解・ス
プラット凝固させる工程を有し、酸素含有量１０００ｐ
ｐｍ以下の希土類元素−遷移金属合金ターゲット材を製
造することを特徴とする合金ターゲット材の製造法。In the production of an alloy target material for forming thin films made of rare earth elements and transition metals, there are a process of mixing rare earth element powder and transition metal powder, a process of forming an electrode by cold isostatic compression, and a process of melting the electrode by vacuum plasma melting method.・Has a splat solidification process and has an oxygen content of 1000p
1. A method for producing an alloy target material, the method comprising producing a rare earth element-transition metal alloy target material having a particle size of pm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10805686A JPS62263939A (en) | 1986-05-12 | 1986-05-12 | Manufacture of alloy target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10805686A JPS62263939A (en) | 1986-05-12 | 1986-05-12 | Manufacture of alloy target material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62263939A true JPS62263939A (en) | 1987-11-16 |
Family
ID=14474795
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10805686A Pending JPS62263939A (en) | 1986-05-12 | 1986-05-12 | Manufacture of alloy target material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62263939A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63186836A (en) * | 1987-01-27 | 1988-08-02 | Mitsubishi Kasei Corp | Manufacture of rare earth element-containing alloy of low oxygen content |
| CN114941080A (en) * | 2022-05-25 | 2022-08-26 | 宁波江丰电子材料股份有限公司 | Preparation method of aluminum-scandium alloy |
-
1986
- 1986-05-12 JP JP10805686A patent/JPS62263939A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63186836A (en) * | 1987-01-27 | 1988-08-02 | Mitsubishi Kasei Corp | Manufacture of rare earth element-containing alloy of low oxygen content |
| CN114941080A (en) * | 2022-05-25 | 2022-08-26 | 宁波江丰电子材料股份有限公司 | Preparation method of aluminum-scandium alloy |
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